Current Opinion in Solid State and Materials Science 27 (2023) 101106

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Current Opinion in Solid State & Materials Science

journal homepage: www.elsevier.com/locate/cossms

Recent research progress in hydrogen embrittlement of additively

manufactured metals – A review
Ju Yao, Qiyang Tan *, Jeffrey Venezuela *, Andrej Atrens, Ming-Xing Zhang *
School of Mechanical and Mining Engineering, The University of Queensland, St. Lucia, QLD 4072, Australia

A R T I C L E I N F O A B S T R A C T

Keywords: Hydrogen is considered as a primary energy carrier for the hydrogen economy. However, hydrogen embrittle­
Additive manufacturing ment (HE) is an inescapable problem that needs to be solved because metals, particularly steels, are commonly
Hydrogen embrittlement used in the transportation and storage of hydrogen, and because HE occurs in high-performance structural
Metals
components in contact with moisture or hydrogen. In particular, HE concerns of additively produced alloys
Microstructure
Mechanical properties
should be addressed, because additive manufacturing (AM) can provide significant advantages in the
manufacturing of such structural components. This review overviews the recent research progress in HE of metals
fabricated using AM. This review introduces AM and HE and summarises and discusses (i) the factors that in­
fluence the HE of AM metals, (ii) possible mechanisms of HE, (iii) the differences and similarities of HE behaviour
between metals processed by AM and those produced through conventional manufacturing processes, and (iv)
the current challenges and research gaps of HE in AM metals. The review covers structural steels, titanium alloys,
tool steels, nickel-based superalloys, stainless steels and high-entropy alloys.

1. Introduction revolutionary manufacturing technology due to its advantages over

traditional subtractive processes, including faster part delivery from
Hydrogen embrittlement (HE) [1,2] is associated with high perfor­ concept to market, the ability to create objects with high geometric
mance metallic materials widely used in industry, including steels, ti­ complexity, and reduced waste generation during fabrication [7,8]. In
tanium alloys and superalloys. HE manifests as the deterioration in the last decade, there has been considerable research in the AM of
structural properties [3], like tensile and fatigue properties [4], and can metallic materials with two frontier AM technologies: direct energy
lead to unexpected catastrophic failure [5]. The ubiquitous nature of deposition (DED) and powder bed fusion (PBF). The latter can be further
hydrogen means that the ingress of hydrogen atoms is typically difficult divided into the major techniques: selective laser melting (SLM) or
to avoid. HE has been extensively studied for over 100 years since it was sintering (SLS) and electron beam melting (EBM) [8]. These AM pro­
first documented by Johnson in 1875 [5,6]. It is now widely agreed that cesses use either powder or wire as the feedstock and use layer-by-layer
HE of high-performance structural components is an unavoidable issue, fabrication to shape and consolidate the feedstock into arbitrary con­
particularly for components exposed to environments that can liberate figurations with complex geometries possible [9]. At present, AM can
hydrogen, such as sea water, hydrogen gas, or moist air. Thus, it is a fabricate highly dense metal parts with acceptable mechanical proper­
long-term challenge to select the right material or to develop new ma­ ties for industrial applications from steels, aluminium (Al) alloys, tita­
terials for hydrogen production, storage, and transportation. nium (Ti) alloys, nickel-based (Ni-based) superalloys, and cobalt-
Additive manufacturing (AM), also known as 3D printing, is a chrome (CoCr) alloys[10,11]. In addition, modelling and simulation

Abbreviations: AM, Additive manufacturing; ASS, Austenitic stainless steel; BCC, Body centred cubic; BCT, Body centred tetragonal; DMD, Direct metal deposition;
DED, Directed energy deposition; EBM, Electron beam melting; FCC, Face centred cubic; FEA, Finite element analysis; GB, Grain boundary; HAC, Hydrogen-assisted
cracking; HCP, Hexagonal close-packed; HEA, High-entropy alloys; HE, Hydrogen embrittlement; HEDE, Hydrogen enhanced decohesion; HELP, Hydrogen enhanced
localised plasticity; HEE, Hydrogen environment embrittlement; HRE, Hydrogen reaction embrittlement; IHE, Internal hydrogen embrittlement; LAM, Laser additive
manufacturing; LENS, Laser engineered net shaping; LMD, Laser metal deposition; PBF, Powder bed fusion; SEM, Scanning electron microscope; SLM, Selective laser
melting; SS, Stainless steel; SSRT, Slow strain rate tensile; TDS, Thermal desorption spectroscopy; TEM, Transmission electron microscopy; UTS, Ultimate tensile
strength; XRD, X-ray diffraction; YS, Yield strength.
* Corresponding authors.
E-mail addresses: q.tan@uq.edu.au (Q. Tan), j.venezuela@uq.edu.au (J. Venezuela), mingxing.zhang@uq.edu.au (M.-X. Zhang).

https://doi.org/10.1016/j.cossms.2023.101106
Received 25 July 2023; Received in revised form 13 September 2023; Accepted 13 September 2023
Available online 21 September 2023
1359-0286/© 2023 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

can indicate how process variables affect the quality of AM components. Table 1
Modelling and simulation can assist with a fundamental understanding Applications for common AM metals [10,11].
of the underlying physical processes and rapid design can shorten the Alloys Applications
qualification cycle of the AM part [12]. In summary, AM is already
Aluminium Aerospace
widely used to create high-quality products and there is much AM has Stainless steel Corrosion resistance; Aerospace; Energy, oil and gas; Medical;
focused on generating products with superior mechanical properties. Automotive; Marine; Machinability and weldability; Tools
Hydrogen embrittlement (HE) of AM products has received relatively and moulds; Consumer products; High temperature
less attention. The earliest report by Baek et al. in 2017 [13] compared Structural steel Tools and moulds
Titanium Corrosion resistance; Aerospace; Automotive; Marine;
the HE behaviour of 304L stainless steel (SS) fabricated by direct metal Machinability and weldability; High temperature; Medical
tooling (DMT), one of the AM methods, with that of the cold rolled. The Cobalt chrome Corrosion resistance; Aerospace; Medical
DMT 304L SS had higher HE resistance than the rolled specimen in Nickel-Based Corrosion resistance; Aerospace; Marine; Machinability and
gaseous hydrogen, and the strain-induced martensitic transformation superalloys weldability; High temperature
Precious metals Medical; Consumer products
did not occur in the DMT specimen. This study concluded that the DMT
AM technology was capable of creating products for use in hydrogen
[13]. Subsequently, HE research of AM metallic materials has received is necessary to investigate their HE susceptibility.
increasing attention, including research on 304L SS [13–16], 316L SS
[17–20], Inconel 718 [21–28] and Ti-6Al-4 V [29–37]. These studies
confirmed that the HE behaviour of metals fabricated with AM differs 2.2. AM processes
from those made through conventional processes.
Reviews on hydrogen embrittlement (HE) and on metal additive The ASTM F2792-12a standard defines two major methods of AM,
manufacturing (AM) have been published in the past few years powder bed fusion (PBF) (as shown in Fig. 1 (a)), and direct energy
[8,9,11,38–44]. The reviews on HE emphasised mechanisms and deposition (DED) (as shown in Fig. 1 (b)). PBF uses a high-energy beam
microstructure [38–40,45–47]. Those on metal AM emphasised pro­ (laser or electron beam) to sinter or melt the pre-spread powder layer on
cesses, microstructure and properties [8,9,11,48,49]. These reviews the bed into the desired profile, followed by spreading and sintering/
have provided the background of HE and AM. However, the HE melting subsequent layers in a repeat fashion until the whole part is
knowledge generated from conventional alloys cannot be fully applied built-up. In contrast, DED builds up layer profiles utilizing a focused
to AM metals because HE is sensitive to microstructure, and generally high-energy beam to simultaneously melt and deposit the feedstock
microstructure of AM alloys differs from their counterparts produced metal that can be either powder (injected by single or multiple nozzles)
through conventional processes. Thus, understanding the HE behaviour or wire (directly feed in) on a substrate plate or on existing layers [8,9].
of the AM metals is essential for extending the AM technology to All metal AM methods basically operate in a similar manner although
hydrogen related industries. However, there is a lack of an integrated different terminologies have been used over the last two decades [8]. All
review on the intersection area of the HE susceptibility of AM metals. AM methods feature fast heating, rapid cooling, a high thermal gradient
Thus, this review will provide valuable insights into the current state within a small melt pool and complicated thermal history [8,11,61,62]
of knowledge regarding HE of metals fabricated using AM, effectively which leads to the different microstructure and properties of parts
building critical reviews and discussions on previous research results. processed by AM compared with those produced with traditional
The present work aims to overview the current understanding of HE of manufacturing processes. In addition, AM has many more processing
AM metals, providing the most up-to-date knowledge in this area. The variables or parameters that influence the microstructure and properties
review starts with the characteristics and applications of AM metals in of the products [8,11]. Table 2 lists the most prevalent parameters.
Section 2, followed by briefing the two typical mechanisms of HE and Lambrakos and Cooper [69,70] identified the most important pro­
the influence of material microstructures on HE in Section 3. Section 4, cess parameters in metal AM as (i) powder or wire feed rate, (ii) laser or
the major part of this review, focuses on the mechanisms and primary electron-beam power density, (iii) traverse and scanning speed, (iv)
influencing factors of HE on the properties of various AM metals, hatch spacing, and (v) layer thickness. Considerable effort has been
including Ti alloys, Ni-based superalloys, stainless steels, high-entropy devoted to investigate the influences on the microstructure and prop­
alloys, and ultrahigh strength steels. This review summarises the re­ erties of AM alloys [71–78], and there have been several review papers
ported HE mechanisms in the literature. The evaluation of those HE [8,11,43,79–84].
mechanisms is beyond the scope of this paper. But, comparisons of the Generally, DED requires higher energy density because coarser
HE susceptibility of AM metals with conventionally produced metals are powders or wires are used, which results in larger melt pools (around 1
provided, together with suggestions for future studies. mm in diameter), a faster build rate, and a relatively slower cooling rate.
Hence, DED is also associated with poorer surface finish and lower
2. Metal additive manufacturing geometric accuracy. Subsequent machining is required [48,85] to ach­
ieve the final shape and size. Many DED techniques have been devel­
2.1. Introduction oped. Commercially available systems include laser direct metal forming
(LDMF) [23,86], laser engineered net shaping (LENS) [87–90], direct
The ASTM defined additive manufacturing (AM) as “a process of light fabrication (DLF) [91,92], and direct metal deposition (DMD)
joining materials to make objects from 3D model data, usually layers [93,94].
upon layer, as opposed to subtractive manufacturing methodologies” In comparison, PBF uses lower beam energy density with a smaller
[50]. Currently, there are large number of AM technologies for metals spot size, resulting in smaller melt pools, (generally ~100 μm in diam­
[8,51,52], such as selective laser melting (SLM) eter), greater resolution, better surface finish and much higher dimen­
[15,22,26,30,34,35,53–57], electron beam melting (EBM) sional accuracy [8,9,95]. Hence, PBF is more suitable for manufacturing
[29,31–34,58–60], and directed energy deposition (DED) [14,15,18]. components with highly complex geometry at a small production vol­
These technologies have strong potential to revolutionise the production ume, such as those in the medical and aerospace sectors [9]. In addition,
paradigm in a variety of industries, including aerospace, automotive, PBF is related to much faster heating and cooling and a larger thermal
energy, medicine, tooling, and consumer goods [51]. Applications for gradient within the melt pools than DED. Hence, for the same alloy, the
common metals fabricated by AM are listed in Table 1. microstructure and properties, including HE, of parts fabricated with
Most of these metals are sensitive to hydrogen or are used as critical PBF differ from those made by DED. Based on the type of power source,
components in environments where hydrogen may be produced. Thus, it PBF can be further divided into two principal processes: (i) selective

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 1. Schematic illustration of the (a) LPBF process and (b) LDED process. Reproduced from Yin [8] with permission from Taylor & Francis, and Tan is the author of
the paper.

The distinguishing microstructural features of AM metals include (i)

Table 2
the finer microstructure due to the fast cooling, (ii) metallurgical defects
Summary of key processing parameters in AM processes [8,11,63–68].
resulting from improper processing settings, (iii) anisotropic micro­
Parameters DED PBF structures with elongated grains owing to the directional solidification
Feedstock Powder Wire Powder characteristics, and (iv) non-equilibrium microstructures including
Nomenclature LDED EDED LPBF EPBF metastable phases, solute trapping, and non-equilibrium compositions
as a result of fast cooling [98]. Common defects include (i) unmelted or
Heat source Laser Electron Laser Electron
beam beam
partially melted particles of powders, (ii) lack of fusion, (iii) keyholes,
Power 100 ~ 3000 W 500 ~ 50 ~ 1000 W (iv) cracking, (v) deposited layers, (vi) delamination, (vii) ejecting
2000 W molten droplets, and (viii) porosity [51,99]. Fig. 3 shows examples of
Beam spot size up to millimetres N/A ≤ 100 μm defects that form in SLM alloys, including the porosity that resulted from
Scan speed 5 ~ 20 mm/s 1 ~ 10 10 ~ 1000 mm/s
either insufficient energy input or excessive energy use, the balling ef­
mm/s
Powder 50 ~ 150 μm N/A 10 ~ 60 μm 60 ~ 105 fect due to excess energy, and hot cracking caused by stress at elevated
particle size μm temperatures [51]. Remelting is a way to improve the microstructure
Hatch distance ≤ 1 mm N/A ≤ 400 μm 200 mm and mechanical properties of AM parts by reheating and resolidifying
Layer thickness ≤ 500 μm N/A ≤ 100 μm 50 ~ 100 the material, which can help to achieve higher densification, improve
μm
Atmosphere Protective, e.g., Vacuum Protective, e.g., Vacuum
surface finish, and increase strength and toughness [100,101].
Air, Argon and Argon and AM parts often have an epitaxial columnar grain morphology
nitrogen nitrogen because of the fast directional solidification with an extremely high
* Typical value.
thermal gradient (approximately 106 K/m). This corresponds to micro­
structural texture and inhomogeneity, leading to undesired anisotropic
properties. Additionally, due to their elongated shape, columnar struc­
laser melting (SLM) or sintering (SLS) and (ii) electron beam melting
tures are susceptible to intergranular hot-cracking when exposed to high
(EBM). Both processes require a platform to hold the powders [96].
thermal shocks during the AM process [11,102–104]. An example of the
However, EBM also requires high vacuum in order to focus the electron
epitaxial columnar grain morphology in SLM Co-Cr-Mo alloy is pre­
beam.
sented in Fig. 4 [105]. Inoculation treatment is an effective method for
refining and homogenizing the microstructure, converting the columnar
2.3. Microstructure characteristics structure into equiaxed grains. This is achieved by introducing nucle­
ants, which can be either externally added or in-situ formed, to promote
As mentioned above, the AM processes are associated with a high heterogeneous nucleation [106]. In the past years, inoculation treat­
cooling rate and directional solidification within small melt pools. Thus, ments to promote heterogeneous nucleation has been widely utilised in
microstructures and properties of metals processed using AM differ from metal AM to process high-performance Ti alloys [107–109], Al alloys
those produced by conventional methods [8,51]. For example, Fig. 2 [102,104,110–112], and steels [106,113–116].
shows that the as-built SLM 316L stainless steel has cellular dendritic Different materials produced with AM exhibit varying microstruc­
structures and columnar grain structures that are not present in the tural characteristics. For example, retained γ austenitic films along the
wrought 316L [97]. building direction is common in most AM steels [117]. Fig. 5 (a) and (b)

Fig. 2. Optical microscope microstructure of (a) wrought 316L and (b) as-built SLM 316L. Reproduced from Tascioglu [97] with permission from Springer.

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 3. Defects in SLM Ti-6Al-4 V: (a) porosity, (b) balling, and (c) hot-tearing cracks. [51].

Moreover, Fig. 6 shows that the microstructure in the AM steels is

sensitive to the cooling rate and the temperature gradient, which are
controllable via the energy input by changing the feeding mechanism
such as laser power or/and scanning speed. Therefore, the mechanical
characteristics of steels produced through AM can be deliberately cus­
tomised by considering the specific correlation between the micro­
structure and the desired property [8].
The microstructural features of various metals fabricated by AM have
been comprehensively summarised in previous reviews on metal AM
[8,9,11,48] and are not detailed herein since the present work focuses
on HE.

2.4. Mechanical properties

Metals produced with different AM methods have different micro­

structures that result in distinct properties. For example, the micro­
structure of metals produced with the laser PBF process is much finer as
a result of the fast-cooling, resulting in better tensile strength but lower
ductility when compared to other processing methods [66]. Table 3 lists
the tensile properties, yield strength (YS), ultimate tensile strength
(UTS) and elongation, of the mostly studied metals fabricated with AM.
For comparison, properties of the counterpart metals produced with the
typical conventional manufacturing processes are also listed. Other
mechanical properties such as impact toughness, fatigue resistance, and
creep resistance, are not included in this review since they have been
investigated and reviewed previously [8,103,122–125].
Fig. 7 compares the mechanical properties of AM alloys and the
conventionally produced alloys with processes such as casting, forging,
and other forging processes for the properties (UTS, YS and elongation).
The X-axis representing data obtained from the traditional methods, and
the Y-axis representing data obtained from AM metals.
The reported property data for the alloys fabricated by AM is more
scattered due to the obvious anisotropy in the mechanical properties,
especially elongation [8,51,117,175]. Nevertheless, the tensile proper­
ties of AM metals are comparable with those made using conventional
Fig. 4. (a) SEM micrograph of the cross section of a Co-29Cr-6Mo alloy fabri­ methods. This is attributed to the relatively high cooling rates achieved
cated via the SLM process. (b) The corresponding crystal orientation map of the in AM, which reduces the partitioning and favours finer microstructure
micrograph showing the epitaxial columnar grain morphology in the metal AM than conventional production [176]. This implies that AM has strong
part. Reproduced from Takaichi [105] with permission from Elsevier. and practical potential for industry applications in producing high-
quality parts with complex geometries.
show the ultrafine cellular-dendritic substructure in the SLM H13 steel.
Most of the cells present a pancake-like morphology along the building 3. Hydrogen embrittlement
direction, and there are extremely thin retained austenite (γ) films in-
between the cells. This microstructure is formed from directional so­ Hydrogen embrittlement (HE) is the deterioration of mechanical
lidification during AM and solute segregation [118–121]. The inter­ properties of solid metals due to the presence of hydrogen [3], which can
dendritic segregation of solutes, carbon in particular, stabilised the local degrade tensile and fatigue properties [4], and can even cause cata­
austenite by decreasing its martensitic transformation point below room strophic failure [5]. The pervasive nature of hydrogen makes the entry
temperature and suppressed the subsequent martensitic transformation of hydrogen atoms into a substance typically difficult to avoid. Thus, HE
in these areas, forming austenitic films. Fig. 5 (d) presents the retained is an inevitable problem, particularly for high-performance structural
austenitic films amongst the martensite blocks [117]. components.
The causes of HE can be explained from different aspects, including

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 5. (a) SEM micrograph of the SLM H13 steel, with the dashed lines representing the melt pool boundaries; (b) high magnification SEM micrograph, showing
extremely fine cell-like substructures in the sample. (c) EBSD phase map and the corresponding EDS maps of the main constituent elements of the area marked in (b).
(d) TEM bright-field (upper) and high-angle annular dark field scanning-TEM (lower) micrographs viewed along the [100]γ, with the inset showing the SAED pattern
of the marked area. Reproduced from Tan [117] with permission from Elsevier, and Tan is the author of the paper.

Fig. 6. (a & b) SEM microstructure, (c) tensile strength & (d) elongation of LDED deposited 316L alloys with different scan speeds; (e-h) SEM images from the etched
surfaces of the LPBF built 316L samples built with different laser scanning speeds. Reproduced from Yin [8] with permission from Taylor & Francis, and Tan is the
author of the paper.

the sources of hydrogen and the types of embrittlement. Generally, HE is processing or fabrication. The severity of hydrogen embrittlement in­
divided in the literature into three categories: internal hydrogen creases with hydrogen concentration, and depends on temperature and
embrittlement (IHE), hydrogen reaction embrittlement (HRE), and the state of stress [178,181]. HRE is caused by the high pressures
hydrogen environment embrittlement (HEE) [3,177–180]. IHE is caused resulting from the chemical reaction of hydrogen inside the metal, for
by hydrogen in the metal lattice, typically introduced during prior example the production of methane by the reaction of hydrogen and

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Table 3
Mechanical properties of metals by additive manufacturing (AM) and traditional (TR) methods.
Materials AM UTS (MPa) YS (MPa) Elongation Hardness Ref. TR UTS YS Elongation Hardness Ref.
(%) (HV) (MPa) (MPa) (%) (HV)

316L SS LPBF 480 ~ 760 350 ~ 640 10 ~ 30 220 ~ 279 [66] Cast 596 ± 16 365 ± 69 ± 9 [126]
22
670 ± 30 520 ± 70 47.5 ± 11.5 [127] Forged 450 ~ 150 ~ 50 ~ 62 133 ~ 140 [66]
818 230
653 ± 3.4 534 ± 5.7 16.2 ± 0.8 [128] 450 170 40 [129]
704.1 ± 2.5 581.1 ± 54.8 ± 2.3 239.6 ± 6.6 [130] 480 170 40 [129]
7.3
E- 437 ~ 580 253 ~ 396 10 ~ 59 165 ~ 173 [66] 620 310 30 [129]
PBF
DED 533 ~ 685 235 ~ 485 12 ~ 43 180 ~ 210 [66] 485 170 40 218 [129]
900 580 6.5 [131] Wrought 887 382 [132]
770 415 4 [131] 935 390 [132]
430 ~ 510 400 ~ 440 14 ~ 20 [89]
639 558 21 [133]
536 352 46 [133]
304L SS LPBF 706.7 ± 6.2 454.7 ± 50.3 ± 1.4 217.5 ± 3.7 [130] Cast 295 125 23 [129]
11.5
530 ± 24 430 ± 12 32 ± 11 [134] Forged 450 170 40 [129]
660 ± 20 540 ± 15 36 ± 12 [134] 480 170 40 [129]
DED 609 ± 18 337 ± 29 48.2 ± 2.5 [78] 620 310 30 [129]
606 ± 13 314 ± 6 56.4 ± 5.8 [78]
685 ± 5 490 ± 8 51 ± 2 [135]
580 ± 10 280 ± 6 62 ± 5 [135]
Ti-6Al-4 LPBF 973 ~ 1407 885 ~ 5 ~ 19 381 ~ 479 [66] Cast 950 940 23.1 [66]
V 1333
1000.4 803.6 7.9 [136] Forged 1380 1192 19.1 [66]
1013 836.6 9.5 [136] 926 ± 2 878 ± 4 20 ± 1 [137]
911.1 738.6 4.2 [136] 1030 970 16 [138]
1011.5 783.2 5.2 [136] 980 865 13.5 [139]
1219 ± 20 1143 ± 30 4.89 ± 0.6 [140] Wrought 1008 962 19 [141]
1269 ± 9 1195 ± 19 5 ± 0.5 [140] 870 ± 10 790 ± 18.1 ± 0.8 [142]
20
1246 ± 134 1150 ± 67 1.4 ± 0.5 [143] 933 ± 7 832 ± 13 ± 1.5 [143]
10
1273 ± 53 1421 ± 3.2 ± 0.5 [143] 942 ± 8 836 ± 9 12.5 ± 1.2 [143]
120
E- 915 ~ 1200 830 ~ 13 ~ 25 360 ~ 460 [66]
PBF 1150
979 905 10 [144]
971 910 10 [144]
1066 1006 15 [138]
1073 1001 11 [138]
1032 973 12 [138]
1032.9 ± 984.1 ± 9 ± 2.9 [145]
12.9 8.5
1008.6 ± 961 ± 7.1 7.1 ± 3.4 [145]
15.2
1029.7 ± 7 982.9 ± 12.2 ± 0.8 [145]
5.7
966.5 ± 5.3 1017.4 ± 12.2 ± 2 [145]
4.9
DED 920 ~ 1163 850 ~ 4 ~ 17 [66]
1105
1099 ± 2 976 ± 24 4.9 ± 0.1 [146]
1025 ± 2 950 ± 2 5±1 [137]
1063 ± 20 960 ± 26 10.9 ± 1.4 [147]
IN 718 LPBF 1400 1180 16.9 [148] Cast 950 940 23.1 [148]
1440 1186 18.5 [148] 1090 915 11 [129]
1450 1190 20.4 [148] Forged 1380 1192 19.1 [148]
1126 849 22.8 [149] Wrought 1350 1105 [129]
1143 ± 5 995 ± 10 23 ± 3 [150] 1435 1185 [129]
1085 ± 11 816 ± 24 19.1 ± 0.7 [151] 1530 1365 [129]
1010 ± 10 737 ± 4 20.6 ± 2.1 [151] 1407 1172 21 [151]
E- 1207 669 21 [152]
PBF
1060 ± 26 822 ± 25 22 [153]
929 ± 20 744 ± 44 5.5 [153]
1138 ± 24 925 ± 20 15.7 ± 4.3 [154]
1061 ± 83 894 ± 24 11.5 ± 6.9 [154]
AISI 4340 LPBF 1207 ~ 1076 ~ 16 ~ 18 [155] Forged 1315 1250 8.2 393 [129]
1227 1110
1386 ~ 1276 ~ 19 [155] 1315 1240 14.6 393 [129]
1434 1311
(continued on next page)

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Table 3 (continued )
Materials AM UTS (MPa) YS (MPa) Elongation Hardness Ref. TR UTS YS Elongation Hardness Ref.
(%) (HV) (MPa) (MPa) (%) (HV)

DED 480 ~ 681 [94] Wrought 1862 1517 11 [155]

H13 LPBF 1712 ± 103 1236 ± 4.1 ± 1.2 [156] Forged 1580 1365 14.4 458 [129]
178
1620 ± 215 835 ± 23 4.1 ± 2.3 [156] 1960 1570 13.0 549 [129]
1965 ± 145 1073 ± 72 3.7 ± 1.7 [156] Wrought 1999 1569 7.5 [157]
2005 ± 68 1190 ± 50 3.8 ~ 6.9 [117]
1370 ± 1003 ± 1.7 ± 0.6 [158]
175.1 8.5
1440 ± 892 ± 1.5 ± 0.2 [159]
34.6 55.2
1704 ± 30 1342 ± 67 1.55 [160]
1321 ± 11 1167 ± 73 0.35 [160]
1227 ± 46 1133 ± 42 0.3 [160]
DED 1820 1505 6 [93]
2064 ± 51 1288 ± 54 6 ± 2.2 [157]
2033 ± 38 1564 ± 24 5.0 ± 2.8 [157]
17––4 PH LPBF 1103.8 ~ 633.8 ~ 20.5 ~ 21.3 259 [161] Forged 795 515 18 252 [129]
1105.8 666.2
980 500 7 340 [162] 930 725 16 271 [129]
1100 500 12 340 [162] 965 795 14 292 [129]
1370 1190 8.3 380 [163] 1000 860 13 303 [129]
1060 650 14.5 [164] 1070 1000 12 332 [129]
940 580 5.8 [164] 1170 1070 10 361 [129]
1188 1160 4.8 [165] 1310 1170 10 388 [129]
1203 1170 4.8 [165] Wrought 1018 992 13.4 430 [166]
DED 900 ± 200 400 ± 100 5±3 441 [167] 1450 1370 9 [168]
18Ni 300 LPBF 1290 ± 114 1214 ± 99 13.3 ± 1.9 388 [169] Cast 1750 1650 8 [129]
1050 930 5 350 [170] Wrought 1000 ~ 760 ~ 6 ~ 15 332 [169]
1170 895
1187.6 ± 914.9 ± 6.14 ± 1.33 371 [171]
10.4 12.5
1050 ± 45 903 ± 98 8 ± 1.2 371 [172]
1165 ± 7 915 ± 7 12.44 ± 0.14 332 ~ 342 [173]
1260.1 ± 768.0 ± 13.9 ± 2 [174]
79 29
825.9 ± 96 1324.7 ± 14.0 ± 1.5 [174]
51

carbon in the steel [178,182]. HEE is caused by hydrogen that can enter operative mechanism in AM steels. HEDE assumes that hydrogen causes
the material (initially hydrogen free) during service or during mechan­ brittle cleavage of metal bonds, whereas hydrogen is associated with
ical testing, such as during mechanical testing in gaseous hydrogen [3]. plastic deformation in HELP [23]. In addition, some studies suggested
HEE takes place in hydrogen-containing atmospheres. During testing in that there may be synergistic effects between the HE mechanisms and
hydrogen gas, some hydrogen molecules are adsorbed on the surface, that the details of the HE fracture process are more complicated than
the hydrogen molecules dissociate into hydrogen atoms, and some assumed in these mechanisms [23,44,191,192].
hydrogen atoms enter the metal [178,183]. Alternatively, if hydrogen is
released by a chemical reaction at the steel surface, as in acid pickling to 3.1.1. Hydrogen enhanced decohesion (HEDE)
remove mill scale after hot working of an ingot, the hydrogen activity The HEDE mechanism proposes that hydrogen reduces the cohesive
can be extremely large, so large that the hydrogen can deposit at internal strength of an alloy [184–186]. The decohesion mechanism was origi­
defects like inclusions and produce sufficient pressures to exceed the nally proposed in 1926 by Pfeil, who stated that “hydrogen decreased
ultimate strength of the steel and cause blisters. Hydrogen in excess of the cohesion across cubic cleavage planes and grain boundaries” [193].
the hydrogen solubility causes the precipitation of hydrides in hydride A refined version proposed that the presence of hydrogen reduces the
forming metals such as Ti and Al (but typically not in steels). cohesive strength of interface boundaries or lattice planes [194,195].
The HE sensitivity depends on the microstructure and properties of Troiano suggested that the underlying mechanism of HEDE is that the
the metal. Consequently, it is expected that the HE sensitivities of metals electron from a hydrogen atom dissolved in steel enters the unfilled 3D
manufactured by AM differ from those produced by conventional shell of the atom comprising the steel (e.g. Fe atoms as suggested by
methods because microstructures and properties of parts fabricated with Troiano in his study of pure Fe), and that these extra electrons in the d-
AM are different from those produced with conventional methods. shell increase the interatomic repulsive forces, and result in decreasing
Before reviewing the HE of AM alloys, major HE mechanisms are sum­ cohesive strength [5,195]. The schematic of the HEDE mechanism is
marised in the following. shown in Fig. 8 [196], which shows another way to explain the HEDE
model. The entry of hydrogen causes the crystal lattice to expand,
weakening the atomic bonds at the tip of a crack. As a result, the energy
3.1. HE mechanisms required to enable crack propagation is lowered, resulting in a macro­
scopic brittle fracture [197,198].
The following mechanisms have been usually used to explain the Few studies have provided evidence that HEDE is the sole HE
observed manifestations of HE in metals: (i) hydrogen-enhanced deco­ mechanism in AM metals, but often HEDE is assumed in combination
hesion (HEDE) [184–186], (ii) hydrogen-enhanced localised plasticity with the HELP mechanism. For example, Li et al. [23] reported that the
(HELP) [187,188], (iii) adsorption-induced dislocation emission (AIDE) HE of IN 718 was caused by the synergistic effect of the HELP and HEDE
[40], and (iv) hydride formation and cleavage (HFC) [189,190]. HEDE mechanism, while Wan et al. [199] proposed that the HE of the
and HELP are the mechanisms most often considered [13] to be the

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 7. Comparison between the UTS, YS & elongation of traditional methods (x-axis) and AM methods (y-axis).

AlCoCrFeNi2.1 eutectic high-entropy alloy (HEA) was due to the acti­

vation of the HEDE and HELP mechanisms.

3.1.2. Hydrogen enhanced localised plasticity (HELP)

The HELP mechanism considers that hydrogen facilitates local
dislocation nucleation and motion at the crack tip, resulting in local
dislocation pile-ups near slip band intersections, causing premature
failure [187,188]. The schematic diagram of the HELP mechanism is
shown in Fig. 9 [196]. In 1971, Beachem first proposed the mechanism
of hydrogen-enhanced localised plasticity by analysing fracture surfaces
in quenched and tempered steels. HE was assessed as a function of the
stress intensity factor, and compared flow stresses with and without
hydrogen [200]. Later, Birnbaum, Robertson and other researchers
refined the model, using elasticity theory combined with observations
using in-situ transmission electron microscopy (TEM) [201–203].
The HELP model assumes that the diffusible hydrogen increases the
mobility of dislocations, causing a reduction in the material’s shear
strength. Such reduction in the shear strength enables the formation of
micro voids that connect along preferential slip planes, resulting in
highly localised fracture [197,198].
Fig. 8. Schematic of the HEDE mechanism, including tensile separation of Some research on materials processed using AM has identified HELP
atoms owing to weakening of interatomic bonds by (i) hydrogen in the lattice, as the primary mechanism of HE [21,23,34,199,204–206]. More details
(ii) adsorbed hydrogen, and (iii) hydrogen at particle–matrix interfaces. are presented in the subsequent sections.
Reproduced from Lynch [196] with permission from Elsevier.

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 9. Schematic of the HELP mechanism, including a micro void-coalescence process, with plasticity localised and facilitated in regions of high hydrogen con­
centration. Reproduced from Lynch [196] with permission from Elsevier.

3.1.3. Hydride formation and cleavage (HFC) mediated HE mechanisms (e.g., HELP, AIDE or HESIV) together with
Embrittlement of hydride-forming metals is primarily attributed to the decohesion-based (HEDE) mechanism are responsible for the HE.
the brittle nature of the hydride phase and/or the failure along the The dominance of a specific mechanism is contingent upon factors such
metal/hydride phase, known as the HFC mechanism [207]. This as hydrogen concentration, material stress state, and environmental
mechanism was first proposed by Westlake in 1969 [208] and is conditions.
important in hydride forming metals such as Ti and Al The concurrent operation of both HELP and HEDE mechanisms, in
[190,207,209–211]. The schematic diagram of the HFC mechanism is accordance with the HELP + HEDE model, has recently been substan­
shown in Fig. 10 [196], which involves repetitive processes of (i) tiated across a range of materials, including various types of steels
hydrogen diffusion towards areas with elevated hydrostatic stress in [212,215], nickel-based alloys [216,217], aluminium alloys [218–220],
advance of cracks, (ii) nucleation and growth of a hydride phase, (iii) the and high-entropy alloys [221,222]. These mechanisms also apply to
fracturing of the hydride upon reaching a critical size, and (iv) arrest of some metals fabricated through AM processes [13,16,23,28,199,223].
crack propagation at the interface between the hydride and the matrix Further discussion of the synergistic action of HE mechanisms in AM
[40]. metals will be provided in the subsequent sections.
The HFC has been identified as the main mechanism of HE in Ti al­
loys processed using various AM techniques, including SLM and EBM
[31,32,34]. Additional information regarding this mechanism is pre­ 3.2. Microstructure influence
sented in the subsequent sections.
HE is sensitive to microstructure, even for the same alloy. Micro­
3.1.4. The synergistic action of HE mechanisms structural alteration may result in an improvement in the resistance to
Numerous investigations of HE primarily focused on the dominance HE [34]. For example, Jeong et al. [224] considered that the lath-type of
of only one particular mechanism. However, recent advancements in retained austenite in steels has a more positive effect in relieving
modelling and experimental studies have shed light on the collaborative hydrogen susceptibility than the equiaxed retained austenite at a similar
interplay of multiple HE mechanisms [44,212–214]. Djukic et al. [44] volume fraction and mechanical stability. It has been verified that lath-
indicated that the cooperative action of multiple HE mechanisms in type retained austenite slows hydrogen diffusion as the lath boundaries
steels and iron could be classified into two categories (i) HELP-mediated inhibit hydrogen migration. Venezuela et al. [225] considered that
HEDE model and (ii) HELP + HEDE model. The HELP-mediated HEDE martensite is known to be the most susceptible to hydrogen compared
model focuses on the activation of the HEDE mechanism through pre­ with other ferrous microstructures such as pearlite and bainite.
vious activity of the HELP mechanism, while the HELP + HEDE model Martensite possesses a highly strained nano-structure because of lattice
involves the synergistic effect of both plasticity-mediated HE mecha­ distortions induced by the interstitial carbon atoms [226]. The presence
nisms and the HEDE mechanism. The summary of the unified model for of a high dislocation density and a high density of interface defects in­
synergistic interplay of HE mechanisms in steels is illustrated in Fig. 11. troduces higher residual stress in the lattice. Hydrogen can interact with
The HELP-mediated HEDE model assumes that the governing mecha­ these inherent stresses in martensite, causing embrittlement [225]. The
nism of HE in steels and other materials is primarily the HELP mecha­ order of HE susceptibility of microstructure is ranked as follows from
nism. In this case, HE is initiated by HELP and is a prerequisite for the low to high: fine-grained massive ferrite and acicular ferrite < fine-
eventual activation of the decohesion-based (HEDE) mechanism at grained granular bainite and massive ferrite < coarse-grained granular
specific microstructural locations. On the other hand, the HELP + HEDE bainite and bainite ferrite embedded with martensite-austenite consti­
describes the simultaneous action of hydrogen-enhanced plasticity and tute < untempered martensite [227]. Hydrogen trapping and diffusion
decohesion. According to this model, some or multiple plasticity- are closely related to the microstructure of materials and are critical to
assessing HE susceptibility. This is further discussed in the following
sections [39].

3.2.1. Hydrogen trapping

Lynch [40] proposed that solute hydrogen occupies and diffuses
across interstitial lattice sites in metals and occupies to varying degrees
the lower potential-energy sites than normal interstitial sites. Schematic
illustrations of sites and traps for hydrogen in materials are shown in
Fig. 12. These sites are generally listed in terms of hydrogen trapping
strength from low to high: solute atoms < locations between the first
Fig. 10. Schematic presenting subcritical crack growth involving hydrogen several atomic layers beneath surfaces and free surfaces < vacancies <
diffusion to hydrostatically stressed regions, then formation and fracture of a strain fields and dislocation cores < grain boundaries < inclusion or
brittle hydride at a crack tip. Reproduced from Lynch [196] with permission matrix interfaces < internal cracks and voids.
from Elsevier. Traps influence the solubility and diffusivity of hydrogen. Thus,

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 11. Summary of the unified model for synergistic interplay of HE mechanisms in steels: localised plasticity and decohesion (HELP + HEDE model). Reproduced
from Djukic [44] with permission from Elsevier.

Fig. 12. Schematic illustrations of sites and traps for hydrogen in materials (a) on the atomic scale, and (b) on a microscopic scale. Reproduced from Lynch [196]
with permission from Elsevier.

trapping can either enhance or weaken the material’s HE susceptibility HEE, hydrogen gas dissociates and is adsorbed at crack tips. In contrast,
[39,228]. A thorough investigation of trapping mechanisms in metals is in IHE, solute hydrogen diffuses to interior fracture-tip surfaces and is
necessary because it is important for understanding the complicated adsorbed there. Solute hydrogen can also precipitate as hydrogen gas in
interactions between metals and hydrogen and could aid in the design of voids and at delaminated non-porous plating/substrate interfaces,
hydrogen-induced failure prevention methods [39]. sometimes resulting in high pressures, which can then be reabsorbed
The location of hydrogen trapping influences the dynamics of HE. In and then diffuse under applied stresses. In normal interstitial lattice

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

sites, hydrogen concentration occurs ahead of notches and fractures, dislocations for low carbon martensite, which reduces hydrogen diffu­
where strong hydrostatic stresses lead to a slightly enlarged lattice [40]. sivity. As increasing the carbon content, hexagonal close packed (HCP)
Furthermore, crystalline defects such as grain boundaries (GBs) and structure martensite may form with lower stacking fault energy
dislocations play a significant role in HE of metals [215,229]. A GB is a [242,250]. HCP structure is closer packed than BCC. Thus, the diffusion
planar defect that can trap hydrogen. Similarly, the dislocation is a line rate of hydrogen in HCP martensite is lower than in ferrite [242]. In
defect with a stress field surrounding the dislocation core that can general, Deff of hydrogen is 4 to 5 orders of magnitude greater in BCC
interact with hydrogen [39]. Wan and co-workers [215] have shown metals than in FCC and HCP metals at 20 ◦ C [249]. However, there are
that the reaction of GBs with dislocations is a key component in HE exceptions, for instance, palladium (FCC) and cobalt (HCP) which have
mechanism for polycrystalline metals. The dislocation-GB reaction can Deff of several orders of magnitude higher than most other FCC and HCP
cause a locally activated state of the GB with a more disordered atom­ metals, likely due to quantum effects overriding lattice-packing effects
istic structure, introducing a local dilative stress concentration. When [40]. Besides, Deff quoted in the literature span 4 to 5 orders of magni­
GB is segregated with hydrogen atoms, the cohesion of the GB is tude at 20 ◦ C for some metals such as steels and Al, presumably because
significantly weakened when it is activated. At present, numerous of experimental difficulties related to controlling surface conditions (e.g.
studies demonstrated the importance of GBs in HE, especially in the oxide films) that influence hydrogen ingress and egress [40,251]. A
following aspects: decrease in Deff indicates an increase in hydrogen trapping in metals. In
further, some studies have found that the reduction in Deff increases with
(i) Hydrogen atoms tend to segregate on GBs [230]; the strength of metals, which means the higher-strength metals are more
(ii) The quasi-cleavage-like fracture predominates in materials with susceptible to HE [244].
moderate hydrogen concentrations, and the micro-scale facets on
the quasi-cleavage fracture surface, as well as the sites of micro- 4. HE characteristics of AM metals
cracks within the material, usually correlate to GBs [231–233];
while the intergranular fracture is common in materials charged This section reviews major reported results on HE characteristics of
with relatively high hydrogen content [234–236]; different AM metals, including titanium (Ti) alloys (4.1), nickel (Ni)-
(iii) HE suppression can be achieved by grain structure refinement based superalloys (4.2), steels (4.3), and high-entropy alloys (4.4). In
[237–239]. addition, some metals are also known to be sensitive to hydrogen. But,
the HE susceptibility of their counterparts fabricated by AM has not been
3.2.2. Hydrogen diffusion studied, such as AISI 4340 and H13. These metals will also be briefed in
Previous studies have indicated that HE is generally caused by local this section.
hydrogen enrichment due to hydrogen trapping at dislocations, GBs, and Table 4 lists the metals processed by AM, for which HE was studied.
other defects. A high density of hydrogen traps would reduce the Among the extensively studied materials are Ti-6Al-4 V, IN 718, AISI
hydrogen diffusion coefficient [240,241]. The principal mechanism for 304L stainless steel, and AISI 316L stainless steel. It is noteworthy that
hydrogen diffusion in steel is lattice diffusion via interstitial jumps the bulk of the research on HE of AM-fabricated metals is currently
[242]. Metals with relatively low hydrogen diffusion coefficients have concentrated on powder-based AM, while research in wire-arc AM re­
been found to be more susceptible to HE [229,240,243]. mains relatively limited [252]. In light of this, the forthcoming sections
Due to hydrogen diffusion is sensitive to trapping in lattice imper­ of this review will primarily focus on the HE characteristics of metals
fections, diffusion models have been proposed to quantify trapping pa­ processed by powder-based AM.
rameters, which could be utilised to determine HE susceptibility
[39,244]. This information may be acquired using several approaches,
with the most common being the hydrogen permeation test [39]. Ac­ 4.1. Titanium alloys
cording to Oriani [245], the McNabb-Foster model solutions can be
resolved by assuming a dynamic local hydrogen equilibrium between Titanium (Ti) alloys are widely utilised as structural and functional
traps and lattice sites. Several constitutive equations linking the diffu­ materials in automotive, aerospace, medical and chemical sectors
sion coefficient (Deff) to trap parameters result from this assumption. For because of their high corrosion resistance, high strength, good
instance, by assuming low trap occupancy, the effective diffusion coef­ biocompatibility and lightweight. The problem of hydrogen penetration
ficient can be obtained using the equation [246,247]:
Table 4
DL AM metals for which HE was studied.
Deff = ( )
NT Eb (1)
1+ exp Materials Material type AM processes Ref.
NL RT
AISI 304L Austenitic stainless DED (LENS and [13–16]
where NT is the number of trap sites (cm3), NL is the number of lattice steel DMT), PBF (SLM)
AISI 316L Austenitic stainless DED (LENS), PBF [17–20]
sites (cm3), R is the gas constant, and T is the absolute temperature. steel (SLM)
Another method to assess Deff from permeation experiments is to use Nb-alloyed Austenitic steel PBF (EBM) [60]
either the time lag or the breakthrough method [248]: 17-4PH Precipitation PBF (SLM) [55]
( ) ( ) hardening stainless
NT DL Eb steel
ln = ln − 1 − (2)
NL Deff RT AerMet100 Low-alloy high PBF (SLM) [204,253]
strength martensite
Aside from vacancies, different microstructural features can influ­ steel
ence hydrogen diffusion in metals, including dislocations, GBs and 18Ni 300 Maraging steel PBF (SLM) [57,254–256]
Ti-6Al-4 V Ti & Ti alloy PBF (SLM and [29–37]
crystal structure. For example, for pure metals at ambient temperatures,
EBM)
hydrogen diffusion mainly depends on the crystal structure [249]. A Ti-6.5Al-3.5Mo- Ti & Ti alloy PBF (EBM) [59]
body-centred cubic (BCC) structured ferrite allows a high diffusion rate 1.5Zr-0.3Si
and a low solubility because of its open lattice structure. Conversely, the IN 718 Nickel super-alloy DED (DMF), PBF [21–28]
face-centred cubic (FCC) structured austenite has a lower diffusion rate (SLM)
AlCoCrFeNi2.1 High-entropy alloy DED (LENS) [199]
and a higher solubility because of the close-packed lattice. Martensite is CoCrFeNiMn High-entropy alloy PBF (SLM) [223,257,258]
primarily a body-centred tetragonal structures (BCT), with high density Pure copper Copper PBF (EBM) [58]

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

and accumulation in Ti alloys arises at different stages of manufacturing produced by different AM methods, including DED (e.g., DMD and
(e.g. pickling treatment) and service (e.g. in a highly corrosive media). LENS) and PBF (e.g., SLM/DMLS and EBM). The AM products exhibited
Hydrogen dissolves in the Ti lattice through penetration, causing sig­ comparable performance with the cast and wrought products, as pre­
nificant changes in physical–chemical properties, microstructure [259], sented in Fig. 13. The HE behaviours of various AM Ti alloys have also
mechanical properties [211,260], and defect structure [261]. In many been studied and reported [29–32,34,205,206,262]. The following
cases, the influence of hydrogen on Ti alloys can lead to a disastrous section discusses HE of the most typical AM Ti alloys.
accident. The risk of hydrogen-induced failure is more hazardous due to
the fact that it is difficult to detect the defects at the beginning of the 4.1.1. Ti-6Al-4V
process [262]. Ti-6Al-4 V alloy is the working horse of Ti alloys. But, Ti-6Al-4 V
The production of hydrides is the most common cause of embrittle­ alloy has low machinability because of poor thermal conductivity [277],
ment in Ti alloys [210,211]. Hardie and Ouyang [263] reported that high chemical reactivity to oxygen [278], and proclivity for strain
hydrogen absorption causes embrittlement, as evidenced by a decrease hardening [279,280]. Traditional methods for producing Ti-6Al-4 V
in elongation. In α + β Ti alloys with a high fraction of β phase, hydrogen parts are forging, casting and rolling, followed by machining to final
tends to migrate within the β lattice and react with the α-phase along the shape and dimension. These methods invariably result in significant
α/β boundaries, leading to the formation of hydrides. This scenario ex­ material waste, expensive manufacturing costs, and long lead times.
acerbates degradation, and the severity of embrittlement depends on the [281]. In such cases, AM is beneficial to production of Ti-6Al-4 V
hydrogen pressure and the hydrogen mobility in the β phase [211]. The components with geometrical complexity [83,281,282].
interaction of hydrogen with metals and the HE is influenced by a va­ Due to the fast cooling, SLM Ti-6Al-4 V alloy generally has an acic­
riety of parameters, such as environment, microstructure, chemical ular α’-martensite phase, but EBM Ti-6Al-4 V, which is associated with a
composition and phase composition [211,264–267]. relatively slow cooling, is characterised by prior β grains with a trans­
In some cases, Ti alloys may benefit from hydrogen interaction [59]. formed α/β microstructure, as shown in Fig. 14 [34,83]. Moreover,
A combination of reversible hydrogenation and thermal effects on hy­ Fig. 15 presents micrographs of hydrogenated SLM and EBM Ti-6Al-4 V
drogenated Ti alloys is known as thermo-hydrogen processing (THP). [34]. The interaction of hydrogen with defects of Ti-6Al-4 V manufac­
The use of THP allows the microstructure to be refined, the process­ tured by different AM methods is expected to be varying. A few papers
ability to be improved and the mechanical properties of Ti alloys to be have been published [29–32,34].
enhanced. [268–270]. Furthermore, Ti-H systems can be utilised as Metalnikov et al. [31,34] observed hydrogen-assisted cracking
promising hydrogen storage materials [271,272]. (HAC) in EBM Ti-6Al-4 V with fine duplex α + β phases. They suggested
The microstructure has a strong influence on the HE susceptibility of that EBM Ti-6Al-4 V had better resistance to HAC in electrochemical and
Ti alloys. Ti alloys with more α phase have better resistance to HE due to gaseous environments than the conventionally manufactured wrought
the close packed HCP lattice. In the α phase, the maximum solubility of alloys because EBM Ti-6Al-4 V has a lower amount of discontinuous
hydrogen is 0.18 wt% at around 300 ◦ C. Hydrogen solubility reduces β-phase, absorbing less hydrogen than the wrought alloy. They also re­
with temperature, leading to the formation of hydrides. In the β phase of ported that, compared with EBM Ti-6Al-4 V, the SLM alloy demon­
Ti, the hydrogen solubility is approximately 5 times higher than that in strated a higher trend of hydrogen absorption and hydride precipitation
the α phase at the eutectoid temperature and achieves a maximum of because of the α’-martensite microstructure. This means that Ti-6Al-4 V
1.98 wt% at 640 ◦ C. However, the hydrogen solubility at room tem­ processed by SLM is more susceptible to hydrogen than that processed
perature is still unknow because the embrittlement mechanism that by EBM [34]. Fig. 16 shows a series of thermal desorption spectroscopy
operates in highly β stabilised alloys has not been determined [273,274]. (TDS) results, showing the desorption peaks in hydrogenated SLM and
Various AM technologies have been used to produce Ti alloy samples EBM Ti-6Al-4 V. There were three desorption peaks in the spectra for the
or/and engineering parts [59,275,276]. Actually, Ti alloy is the mostly SLM samples, which implied the presence of three different hydrogen
studied metal for AM. Dutta and Froes [276] reviewed Ti alloys traps. The first desorption peak appeared at low temperatures. The

Fig. 13. Tensile behaviour comparison of AM, cast and wrought Ti-6Al-4 V at room temperature. Reproduced from Dutta [276] with permission from Elsevier.

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 14. SEM images showing the microstructure of Ti–6Al–4 V alloy processed by (a & c) SLM and (b & d) EBM. Reproduced from Metalnikov [34] with permission
from Elsevier.

Fig. 15. Micrographs of electrochemical hydrogen charged (a) SLM and (b) EBM Ti–6Al–4 V. Reproduced from Metalnikov [34] with permission from Elsevier.

activation energy was 31 ± 5 kJ/mol, which indicated a reversible trap samples. The brighter areas indicate a higher concentration of hydrogen,
that could be assigned to dislocations (~30 kJ/mol) [32,283]. The and the dark areas were related to the less hydrogenated α phase. The
second hydrogen trap was also reversible and could be assigned to GBs hydrides were aligned parallel to the interphase boundaries, and the
(~50 kJ/mol) [31,32]. The third peak appeared at high temperatures higher structural complexity with more Ti hydrides was present in the
and was characterised by the activation energy of 85 ± 9 kJ/mol, which EBM alloy. In addition, the discontinuous β-phase also resulted in faster
indicated a strong irreversible trap with Ti hydrides (approx. 90 ~ 125 hydrogen desorption in the EBM Ti-6Al-4 V than the wrought alloy
kJ/mol) [283,284]. In contrast, the EBM sample had only two peaks, because the BCC β-phase was associated with the higher solute oxygen
which were associated with two hydrogen traps: (i) a relatively low content (see Fig. 18).
activation energy (53 ± 3 kJ/mol) at low temperatures, which corre­ The contradiatory conclusion between Matalninkov et al. and Navi
sponded to GB reversible trapping, and (ii) a high activation energy (88 et al.’s might be attributed to Metalnikov et al.’s [34] underestimation of
± 5 kJ/mol) at higher temperatures, which indicates irreversible trap­ the influence of hydrides and microvoid formation on the HE suscepti­
ping by Ti hydrides. Thus, based on the TDS spectra in Fig. 14, the main bility. Metalnikov et al. only compared the microstructure difference
trap was irreversible in the SLM Ti-6Al-4 V, whereas in the EBM between wrought and EBM Ti-6Al-4 V, without other direct comparative
Ti–6Al–4 V, it was reversible [34]. experimental results. In addition, the TDS spectra in these two studies
In contrast, Navi et al. [32] reported that the HE susceptibility of were different. Only one H-trap was identified in the TPD/TDS spectra
EBM Ti-6Al-4 V was greater than that of the wrought alloy because of the for the EBM sample in Navi et al.’s [32] work. This was probably
larger amount of α/β interfaces, and the discontinuous β-phase particles attributed to the difference in heating rate or/and different instruments
along the short-horizontal direction in the EBM Ti-6Al-4 V. Both factors used because Navi and co-workers used their home made system rather
promoted the formation of hydrides and microvoids, inducing HAC than a commercially available machine. Thus, further studies are
along the interphase boundaries. Fig. 17 presents the time-of-flight necessary to clarify the accuracy of these data and conclusions.
secondary ion mass spectrometry image mapping of the total Additionally, Silverstein and Eliezer [30] reported that the suscep­
hydrogen intensity and the Ti-hydride intensity in wrought and EBM tibility of AM Ti-6Al-4 V to HE strongly depended on the printing

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 16. (a & b) TDS spectra of electrochemical hydrogen charged and (c & d) determination of the activation energies of each hydrogen desorption peaks (a & c)
SLM and (b & d) EBM Ti–6Al–4 V. Reproduced from Metalnikov [34] with permission from Elsevier.

direction. The vertical direction (SLM1) had a lower resistance to HE 4.2. Nickel-based superalloys
compared with the horizontal direction (SLM2), as shown in Fig. 19. The
higher HE susceptibility of the SLM1 sample was attributed to the higher Nickel-based (Ni-based) superalloys are commonly used at temper­
amount of Ti-hydrides as indicated in Fig. 20 and a lower trapping en­ atures above 500 ◦ C when high creep and/or fatigue resistance is
ergy of TiH (Fig. 21). In contrast, the SLM2 printing direction may have required. These alloys usually contain up to 10 alloying elements,
created a high-stress intensity environment that reduced the probability including light elements such as carbon or boron, aluminium and heavy
of the stress-induced hydride mechanism (see Fig. 22, Fig. 23, Fig. 24). refractory elements such as tantalum, rhenium or tungsten [288].
Although the alloys were designed for turbine engine application, they
4.1.2. Ti-6.5Al-3.5Mo-1.5Zr-0.3Si are also increasingly applied to other sectors, such as ultra-supercritical
Ti-6.5Al-3.5Mo-1.5Zr-0.3Si is another typical α + β Ti alloy that is power plants, nuclear power plants and fossil fuel-fired diesel engines,
used in compressor disks and blades of jet engines because of high creep and fuel cells. The applications are most prevalent over 750 ◦ C because
resistance, and thermal stability at high temperatures [59,285]. There the characteristics of ferritic steels deteriorate dramatically above this
are two studies on the hydrogenation of this alloy manufactured using temperature [289].
AM [59,286]. Due to the geometrical complexity of energy generation and aero­
Stepanova et al. [59] investigated the HE of Ti-6.5Al-3.5Mo-1.5Zr- space components, AM of Ni-based superalloys has attracted increasing
0.3Si processed by EBM and found that the microstructure has a sub­ interest from scientists and engineers. At present, different AM tech­
stantial impact on the hydrogen sorption kinetics during gas-phase hy­ niques have been used to process both solid solution and precipitate-
drogenation at 650 ◦ C. The average rate of hydrogen sorption was higher strengthened Ni-based superalloys [290]. Comprehensive details of Ni-
in the EBM samples produced with lower electron beam current (3 mA), based superalloys processed by AM, including SLM, EBM and DED,
which corresponded to smaller melt pools [287], faster cooling and can be found in recently published review papers [81,84,291]. Table 5
therefore finer secondary α precipices, than those produced with higher summarises the reported commercial Ni-based superalloys processed
electron beam current (4 mA), which was associated with slower cooling through the powder-based fusion approach. Inconel 718 (also called Ni-
and coarser α. Further increasing the electron beam current to 6 mA based 718 or IN 718) is the mostly studied alloy compared with others as
caused GB cracking due to high internal stresses in the material during it is the most widely used [290].
solidification, which increased the rate of hydrogen sorption and the Chemical, microstructure and property inhomogeneities are major
hydrogen [59]. In addition, no other research has been done to directly concerns in AM Ni-based superalloys. Such inhomogeneities result from
measure the HE of AM Ti-6.5Al-3.5Mo-1.5Zr-0.3Si. the rapid and repeated thermal gyrations during AM, which are related
Up to now, the research on HE of AM Ti alloys is limited. Although a to non-equilibrium phase formation, spatially dependent microstructure
few papers were published on Ti-6Al-4 V, inconsistent results were re­ gradients and multi-length scale microstructure inhomogeneities [292].
ported. Due to the more processing variables in AM compared with Although superalloys have good high-temperature oxidation and creep
traditional manufacturing routes, the microstructure of AM alloys is resistance and good corrosion resistance at room temperature, it does
more complicated, which leads to the complexity of HE behaviour of AM not mean that the alloys are immune to HE and/or water vapour effects
Ti alloys. Hence, to enable the wider applications of AM of Ti alloys, in high-pressure hydrogen environments [293]. It has been found that
more and in-depth study on HE of AM Ti alloys needs to be done. HE occurs over a much wider temperature range in many superalloys.
More significant HE has been evidenced at substantially higher

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 17. Time-of-flight secondary ion mass spectrometry image mapping of (a & c) the total hydrogen intensity and (b & d) the Ti-hydride intensity in (a & b)
wrought and (c & d) EBM samples. (a & b) Reveal the whole cross-section, whereas (c & d) reveal the upper side of the cross-section. Brighter areas indicate higher
concentration of hydrogen. Arrows mark the hydrides aligning parallel to the interphase boundaries. Reproduced from Navi [32] with permission from Elsevier.

is necessary [21–23,26,185,295,296].
Precipitation-hardenable IN 718 has high strength and is conse­
quently hard to machine [290,297]. Hence, AM has received a lot of
attention for fabricating IN 718 components in the last decade [26,298].
At present, AM of IN 718 alloy has been well established, and high-
quality AM IN 718 parts can be produced with SLM [151,299] and
EBM [154,300]. Hosseini and Popovich [301] reviewed the micro­
structural features, tensile strength, hardness, fatigue strength, and
high-temperature creep behaviour of IN 718 alloy fabricatred with
different AM techniques, different processing and post-processing
conditions.
The HE susceptibility of IN 718 alloy produced with conventional
processing has been studied by several researchers. Hirose et al. [302]
reported that IN 718 alloy has a high sensitivity to HE, with hydrogen-
induced cracking predominantly occurring at stress-concentrated re­
gions on the surface of the alloy. They noted that reducing the local
hardness of these surface regions can effectively prevent such cracking.
It has been verified that the laser surface solutionizing technique is
effective in reducing the HE susceptibility of IN 718. Tarzimoghadam
Fig. 18. TDS spectra for wrought and EBM specimens precharged with
hydrogen for four days. The spectra were measured at a heating rate of 15 ◦ C/
et al. [184] studied the effects of γ and δ phases on the HE sensitivity of
min. Reproduced from Navi [32] with permission from Elsevier. IN 718. They found that rapid and preferential desorption of diffusible
hydrogen occurs in the γ-matrix, while δ/matrix interface decohesion
serves as the primary damage mechanism in the presence of hydrogen.
temperatures compared with lower temperatures. This is different from
The role of the δ-phase in HE is attributed to hydrogen accumulation at
steels, which are more sensitive to HE at relatively lower temperatures
the δ/matrix interfaces during loading, resulting in reduced bonding
ranging from − 200 ◦ C to 200 ◦ C. Hence, HE is an important factor to
strength and concurrent decohesion upon straining. Furthermore, Li
consider for safe design in a hydrogen environment since most super­
et al. [216] investigated the HE behaviour of IN 718 at room tempera­
alloys are often used at high temperatures [294]. Thus, HE study of the
ture, and reported that hydrogen charging deteriorates the mechanical
Ni-based alloys, including fabricating by AM and conventional methods,

15
J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 19. Two different SLM-building directions: (a) SLM1 and (b) SLM2. Reproduced from Silverstein [30] with permission from Elsevier.

hydrogen-induced brittle zone [303].

However, fewer work has been done on the HE susceptibility of IN
718 alloy processed by AM and no review paper has been published.
Kolesov and Alekseeva [22] first reported that hydrogen accumulated
around GBs in an SLM IN 718 sample after hydrogen charging, which
compensated for the effect of high micro stresses. X-ray diffraction
spectra taken from the SLM IN 718 samples and traditional manufac­
tured IN 718 indicated that hydrogen charging in the SLM samples
partially eliminated the residual stress/strain as the H-charged peaks in
these samples were narrower than the initial as-built SLM samples
without H-charging. In contrast, H-charging of the conventionally pro­
duced samples led to slightly peak widening. This can be considered as
the result of hydrogen dissolution in the lattice, which decreased the
micro-strain.
Li et al. [23] reported that hydrogen reduced the UTS, YS, and
elongation of AM IN 718 samples, including both as-built (as-deposited)
samples along both perpendicular to and parallel with the building di­
rections, and heat-treated horizontal samples. Fig. 26 (c & d) show the
results of tensile properties originated from their stress–strain curves.
For uncharged specimens, YS and UTS of the as-built horizontal plane
(HP), as-built vertical plane (VP) and heat-treated-HP samples were 737
MPa and 1078 MPa, 678 MPa and 975 MPa, 1260 MPa and 1475 MPa,
respectively. High YS and UTS of the heat-treated-HP samples were
attributed to the formation of the γ′ and γ′′ strengthening precipitates
[304,305]. After hydrogen charging, both YS and UTS in the as-built VP
specimens were not greatly affected but reduced by approximately 100
MPa in the as-built HP samples and heat-treated samples.
Additionally, for comparison of the hydrogen-induced degradation
in mechanical properties, Li and his co-workers [23] used the index of
HE (HEI) which was calculated using Eq. 3 [306] to calculate the relative
fracture strain loss of the specimens:
εf (uncharged) − εf (charged)
HEI = (3)
εf (uncharged)

where εf(uncharged) and εf(charged) are the fracture strain of hydrogen un­
charged and hydrogen charged specimens, respectively.
The HEI value in the as-built VP specimens was 23%, which was the
Fig. 20. X-ray diffractometer (XRD) pattern of Ti-6Al-4 V (a) SLM1 & (b) SLM2. lowest compared to the as-built HP specimens at 27% and heat-treated
Black: Uncharged & Red: gas phase hydrogen charged 10 h at 500 ◦ C and 0.5 HP specimens at 37%. This indicated that the as-built VP specimens
MPa. Reproduced from Silverstein [30] with permission from Elsevier. (For
exhibited the highest resistance to HE. The synergistic effect of HELP
interpretation of the references to colour in this figure legend, the reader is
and HEDE were used to explain the cracking of the AM IN 718 samples in
referred to the web version of this article.)
this study. The presence of high-density dislocations in the hydrogen-
induced brittle zone of both the as-built and heat-treated samples in­
properties, as shown in Fig. 25 (a & b). They observed a partial Portevin- dicates that plastic deformation is a contributing factor to HE failure,
Le Chatelier (PLC) effect for hydrogen charging current density of 220 aligning with the HELP mechanism. Concurrently, in the as-built sam­
mA/cm2 and 590 mA/cm2. PLC is a type of plastic instability manifested ples, γ-matrix/Laves phase interface decohesion, and in the heat-treated-
as stress serrations during deformation. Additionally, they detected HP samples, intergranular cracking, both support the HEDE mechanism.
plastic deformation features characterised by dislocation cells in the

16
J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 21. Hydrogen thermal desorption curve and determination of the activation energies for two fitted hydrogen desorption peaks of the TDS spectra from hy­
drogenated Ti-6Al-4 V (a) SLM1 & (b) SLM2. Reproduced from Silverstein [30] with permission from Elsevier.

Fig. 27 shows that, for the as-built HP and VP samples, crack initiation in a straight cracking feature. Thus, the vertical samples had a stronger
sites were located at γ-matrix/Laves phase interfaces, but the crack resistance to HE than the horizontal samples due to the suppression of
propagation path in both as-built samples was different. The as-built HP hydrogen entrance by columnar dendrites. For the heat-treated HP
samples had a zigzag crack propagation path, whereas the VP samples samples, hydrogen-induced cracking initiated from γ-matrix/δ phase
had a straight crack propagation path. In the as-built HP sample, the interfaces and propagated along GBs. As a result, the heat-treated hor­
crack growth was in the form of decohesion along the interfaces. izontal samples had a higher susceptibility to HE due to their GB pre­
Because the intersection angle between the maximum shear stress di­ cipitates and high strength level. Hesketh et al. [24] reported similar
rection and tensile direction was 45◦ , the cracks extended to the γ-matrix results in the effect of printing direction to those of Li et al. [23].
along a specific direction. In contrast, in the as-built VP sample, the long Xu et al. [27] also investigated the HE behaviour of the as-built SLM
axis direction of Laves phases was almost vertical to the tensile direc­ and post-heat-treated IN 718 in terms of microstructural evolution and
tion, and this orientation was conducive to crack growth via void coa­ crack characterization using a low strain rate tensile (SSRT) tests under
lescence along long-chained γ-matrix/Laves phase interfaces, resulting in situ electrochemical hydrogen charging. The solution treatment (ST)

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

( )
σfH 1 + δfH
IHE = 1 − ( ) (5)
σ fa 1 + δfa

where σfa and σfH are the fracture strengths obtained in air and
hydrogen, respectively, and δfa and δfH are the uniform plasticity strains
obtained in air and hydrogen, respectively.
The SAT samples had the largest IHE index of 0.87, followed by the as-
built SLM and ST samples, which indicated that the SAT samples had the
highest HE susceptibility. This was attributed to the high dislocation
density and local strain along the cellular structure walls in the as-built
SLM sample, which increased the local hydrogen concentration and
resulted in cracking along the cell walls. The ST process led to the
dissolution of the Laves phase and a reduction in the dislocation density,
which slowed down the diffusion of hydrogen along the cell walls.
Subsequent aging of the SAT samples caused precipitation of the γ′, γ″
and δ phases. The formation of the δ phase along the GBs and the cell
walls led to δ/γ interface cracking. Consequently, the SAT samples
Fig. 22. The kinetic curves of hydrogen sorption of EBM Ti-6.5Al-3.5Mo-1.5Zr-
exhibited the highest strength as well as the highest susceptibility to HE
0.3Si parts produced by EBM with different electron beam current: (1 – 3 mA, 2
– 6 mA & 3 – 4 mA). Reproduced from Stepanova [59] with permission
among these samples [27].
from Elsevier. However, Yoo et al. [25] proposed that if the temperature of heat
treatment was sufficiently high, the hydrogen diffusivity of LPBF IN 718
was comparable to that of conventional IN 718. At the sufficiently high
and solution-aging treatment (SAT) were carried out as post-heat
temperature of heat-treatment conditions, continuous γ’’ precipitation
treatments. There was a substantial impact of post-heat treatment on
along the sub-GB can reduce the density of vacancies and dislocations,
the hydrogen content of the SLM IN 718. The hydrogen atoms preferred
weakening the role of grain/sub-GBs in hydrogen transport as well as in
to diffuse in the ST samples compared to the as-built or SA samples due
hydrogen trapping.
to the higher hydrogen desorption rate (as shown in Fig. 28 (a)), which
Additionally, Kevinsannya et al. [26] discovered that the fatigue
revealed that the ST samples had the lowest HE susceptibility. Fig. 28 (b
limit and fatigue life of the AM IN 718 was not influenced by hydrogen,
- d) show the SSRT test results obtained in air and under in-situ hydrogen
which was similar to the observation for forged IN 718, because
charging. The results indicate that post-heat treatment significantly
hydrogen had little influence on the crack growth threshold. However,
affected the tensile properties of both conditions. Compared with the as-
the mechanism for determining whether hydrogen deteriorates the
built SLM samples, the ST process decreased the fracture strength from
crack growth threshold in IN 718 has not yet been clarified in their work.
1053 to 904 MPa in air and 858 to 679 MPa in hydrogen, while the SAT
Based on the current studies on HE of Ni-based superalloys fabricated
process increased the fracture strength to 1357 and 1154 MPa in air and
by AM, two main HE mechanisms can be suggested, namely, HEDE and
hydrogen, respectively. Li et al. [23] ascribed the improvement in
HELP [23,184–188,308]. There is a synergistic effect between these two
strength to the precipitation strengthening of γ′/γ″ phases [304,305].
mechanisms [23]. Many studies have also been conducted on the in­
To understand the hydrogen-induced degradation of the tensile
fluence of printing direction [23,24] and post-heat treatment [23,25,27]
properties, Xu and his co-workers [27] used IHE susceptibility index
on AM Ni-based alloys. However, the main knowledge gap on HE of AM
which was calculated using Eq. 4 [307] to evaluate the effect of
Ni-based superalloys exists in the comparison of alloys fabricated by AM
hydrogen on strength and plasticity.
with those fabricated through conventional routes. Furthermore, the

Fig. 23. SEM images of the surface of EBM Ti-6.5Al-3.5Mo-1.5Zr-0.3Si at different electron beam currents (a & d) 3 mA, (b & e) 4 mA, (c & f) 6 mA; (a-c) as-built (d-
f) after hydrogenation. Reproduced from Stepanova [59] with permission from Elsevier.

18
J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 24. Portions of diffraction patterns of the Ti-6.5Al-3.5Mo-1.5Zr-0.3Si samples produced by EBM a different electron beam current (1 – 6 mA, 2 – 4 mA & 3 – 3
mA) (a) before and (b) after hydrogenation. Reproduced from Stepanova [59] with permission from Elsevier.

current studies are limited to the IN 718 alloy, and the HE susceptibility
Table 5
of other AM Ni-based superalloys is still unknown.
Summary of Ni-based superalloys processed through powder-based AM modal­
ities [290].
Alloys AM processes 4.3. Stainless steels
Inconel 625 BJ, DED, EBM, SLM
Hastelloy X EBM, SLM Stainless steel (SS) contains at least 12% chromium to ensure high
Inconel 718 BJ, DED, EBM, SLM corrosion resistance [309]. SS is often used for applications in envi­
Haynes 282 DED, EBM ronments that may contain hydrogen or moisture. Thus, HE of this type
Inconel 738 SLM, EBM
Mar-M247/CM274 * related to chemistry SLM, EBM
of steels is often a concern. There are several comprehensive books and
Rene 142 EBM reviews on the HE of SSs [310–312].
Rene N5 EBM Most SSs have good AM processability, and therefore AM of SS is an
CMSX-4 DED, EBM active topic. Table 6 lists typical SSs that are commonly processable with
AM. There are a few integrated reviews summarizing the research
progress in this field [8,313–316]. In addition, Laleh et al. [317]
compared the mechanisms of corrosion behaviour of AM SSs with their
conventionally produced counterparts, including the deleterious effect
of hydrogen. AM SS products generally have finer microstructure

Fig. 25. (a) Engineering stress–strain curves of hydrogen free and hydrogen charged samples; (b) High magnification image of red rectangle region in (a).
Reproduced from Li [216] with permission from Elsevier. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version
of this article.)

19
J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 26. (a) Stress–strain curves of IN 718 alloy with and without hydrogen; (b) high magnification image of signed region in (a); (c) YS and UTS of samples; (d)
fracture strain and HEI of samples. HU: hydrogen uncharged; HC: hydrogen charged. Reproduced from Li [23] with permission from Elsevier.

Fig. 27. Hydrogen-assisted cracking of frac­

tured samples along lateral surfaces (a-a’’) as-
built HP sample; (b-b’’) as-built VP sample; (c-
c’’) heat-treated-HP sample (a) crack initiation
at the matrix/discrete Laves phase interfaces;
(a’) crack growth along matrix/Laves phase
interfaces; (a’’) cracks propagation through
the γ-matrix; (b) crack initiation at matrix/
long-chained Laves phase interfaces; (b’)
crack growth; (b’’) cracks propagation
through the coalescence of voids along ma­
trix/Laves interfaces; (c) crack initiation at
GBs; (c’) crack growth along GBs; (c’’) cracks
propagation along GBs. TD: tensile direction.
Reproduced from Li [23] with permission from
Elsevier.

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 28. (a) Hydrogen desorption curves – pre-charged at 5 mA/cm2 for 24 h, (b) engineering stress–strain curves, (c) fracture strength, and (d) uniform plasticity for
various processed IN 718. as-SLM: as-built SLM, ST: solution treatment, and SAT: solution aging treatment. [27].

enrichment at critical sites of the microstructure, such as the micro­

Table 6
mechanically stress concentrated regions in front of hetero-interfaces,
Summary of stainless steels processed using powder-based AM [8,316].
and thus leading to H-assisted cracking [329,330]. For the AM ASS,
Alloys Microstructure Type AM processes the fast cooling may lead to solute segregation or the incompletion of the
304L Austenite Austenitic SS DED, PBF δ to γ transformation during AM. The small amount of δ ferrite retained
316L Austenite Austenitic SS DED, PBF in metastable ASSs may increase the HE susceptibility, providing crack
17-4PH Martensite PH SS PBF initiation sites [16,331,332]. The current research on HE of AM ASS
AISI 420 Martensite Martensitic SS DED, PBF
AISI 431 Martensite Martensitic SS DED
focuses on AISI 304L SS [13–16] and AISI 316L SS [4,17,54]. he re­
AISI 441 Ferrite Ferritic SS PBF ported results are discussed in the following sections.
2507 Duplex Duplex SS PBF
2205 Duplex Duplex SS PBF 4.3.1.1. AISI 304L. AISI 304, the most common ASS, has low cost,
mechanical properties similar to construction steel, good corrosion
because of the high cooling rate. But they are also highly anisotropic due resistance and high weldability [333]. The austenitic microstructure in
to the formation of columnar grains, which differs from their wrought 304L SS is subject to strain-induced transformation during service or
counterparts [95,318–321]. Thus, the HE susceptibility of AM SS is ex­ forming due to the relatively low stacking fault energy [334]. This
pected to be different from the wrought alloy [55]. Studies on HE of AM transformation is also dependent on microstructure, particularly texture
SS are limited. The existing studies have focused on austenitic SS and [335] and grain size [336]. Highly dense AM 304L SS exhibits tensile
precipitation hardening (PH) SS. and fatigue performance that are comparable to the wrought counter­
part in both ambient and severe hydrogen environments. Generally,
4.3.1. Austenitic stainless steels internal hydrogen causes tensile ductility loss in both PBF and DED-
Austenitic stainless steel (ASS), particularly the AISI (American Iron manufactured 304L SS. Furthermore, defects, and the micro-
and Steel Institute) 300 series, are the most common [322]. Hydrogen segregation in the AM parts can promote microcrack coalescence,
diffusivity in the FCC crystal structure of the ASS is lower than in the leading to a more severe reduction in ductility [15].
BCC lattice, which makes austenitic SS potentially more resistant to HE In 2017, Baek et al. [13] first reported the dependency of HE resis­
than ferritic stainless steels, particularly resistant to environment tance on AM processing of 304L SS. They compared the HE behaviour of
hydrogen embrittlement (EHE) [16]. Thus, ASS is commonly used to 304L processed using direct metal tooling (DMT) with the rolled coun­
make parts exposed to gaseous hydrogen, such as gaseous hydrogen terpart and found that the DMT processed 304L had higher HE resistance
storage and gaseous hydrogen transportation applications than the conventionally processed 304L. Fig. 29 shows that the elon­
[16,323–325]. Thermodynamically stable ASS, such as the AISI 316S, is gation to fracture of the DMT 304L was similar in air (52%) and with
less susceptible to HE even though severe HE has been reported in hydrogen (50%). In contrast, the strain to failure of the rolled 304L was
metastable ASSs, such as AISI 304 in which strain-induced α′ martensite significantly reduced (68% reduced to 19%). In addition, the DMT
forms during deformation [326–328]. The strain-induced α′ martensite specimens showed the same ductile fracture behaviour in both air
provides a fast diffusion path for hydrogen, resulting in hydrogen (Fig. 30 (a)) and hydrogen (Fig. 30 (b)): ductile fracture with small

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 29. Stress–strain curves of (a) type 304L STS DMT manufactured specimen, (b) type 304L STS rolled plate specimen. Reproduced from Baek [13] with
permission from Elsevier.

Fig. 30. Fractography of 304L SS specimens tested in different atmospheres (a) DMT manufactured specimen (air), (b) DMT manufactured specimen (10 MPa
hydrogen), (c) rolled plate specimen (air), rolled plate specimen (10 MPa hydrogen). Reproduced from Baek [13] with permission from Elsevier.

uniform dimples and no evidence of cleavage or secondary cracks. The fracture surfaces (a-c), and the measured HE susceptibility of steel for
rolled 304L also exhibited ductile fracture in air, characterised by a cup- each condition (d). The HE susceptibility of the 304L was closely related
cone fracture mode (Fig. 30 (c)), but brittle cleavage fracture in to the production route. For the casting and annealed (CA) 304L, H-
hydrogen (Fig. 30 (d)). The HELP and HEDE mechanisms can be used to charging resulted in a significant loss of ductility. For the LPBF and
elucidate HE in this material. According to the HELP model, a locally thermomechanical treatment (TMT) CA samples, hydrogen had a minor
elevated hydrogen concentration (such as the local tip) augments influence on ductility. EBSD analysis indicated that the volume fraction
dislocation activity, resulting in localized stress concentration and the of strain-induced α′ martensite was higher in the CA samples (~16%)
initiation of failure at planar defects [177,337]. Fig. 31 presents the than in the LPBF and CA-TMT samples (respectively ~ 3% and ~ 1%) at
EBSD images and phase maps of the fractured surfaces of both the DMT the same strain level of 60%. This suggests that the low resistance of the
and rolled 304L. The strain-induced martensitic transformation did not CA sample to HE could be attributed to the low local mechanical sta­
occur in the DMT specimen in the gaseous hydrogen environment. In bility of the austenite. This instability resulted from chemical in­
contrast, there was BCC strain-induced martensite in the rolled 304L. homogeneity in the austenite regions, notably around the retained δ
The finer microstructure of the DMT 304L might be responsible for the zones in the initial state. The application of TMT after CA improved the
higher mechanical stability of the austenite. This study concluded that chemical homogeneity of the microstructure. This effectively restored
AM technology could be more suitable for creating 304L SS products for the stability of the austenite and consequently enhanced the HE resis­
hydrogen usage and service [13]. tance of the CA-TMT sample. In contrast, the LPBF sample exhibited a
Lee et al. [16] also investigated the microstructure and HE suscep­ completely austenitic structure due to the high cooling rate, which also
tibility of 304L SS manufactured using different processes. Fig. 32 shows resulted in a finer and more homogenous microstructure with a
the typical engineering stress- strain curves, the SEM images of the distinctive solidification cellular structure. These features increased the

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 31. EBSD images of fractured surface for DMT specimen (a –d) and rolled plate specimen (e –h); (a) DMT origin (inverse pole figure image), (b) DMT origin
(phase map), (c) DMT specimen (air), (d) DMT specimen (hydrogen), (e) rolled (inverse pole figure image), (f) rolled plate origin (phase map), (g) rolled plate
specimen (air), (h) rolled plate specimen (hydrogen). Reproduced from Baek [13] with permission from Elsevier.

Fig. 32. Typical engineering stress-engineering strain curves of the (a) LPBF, (b) CA, and (c) CA-TMT samples with and without hydrogen. The SEM images show the
surface of samples after tensile testing at the fracture site. (d) Quantification of HE susceptibility for each condition. Reproduced from Lee [16] with permission
from Elsevier.

strength, stabilised the austenite, and enhanced the resistance to HE. Lee enrichment at the γ-α′ interface.
and co-workers [16] also found that the majority of the H-assisted cracks
were initiated in the α′ martensite in all samples, further indicating the 4.3.1.2. AISI 316L. 316L SS is commonly used in demanding applica­
importance of strain-induced α′ martensitic transformation in the HE of tions like heat exchangers, jet engines, military applications, and
304L. Thus, the presence of δ and chemical inhomogeneity within the γ biomedical services. But, 316L has limitations in some environments
matrix were revealed to promote HE by causing the deformation- [338,339] due to its relatively low wear resistance and strength,
induced martensitic transformation and the concomitant hydrogen particularly at elevated temperatures as SS components are susceptible

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

to oxidation, corrosion, carburization, sensitization, and HE [4,340]. level of strain [236,341,342].

AM can be used to fabricate 316L parts. The strength is typically higher The resulted published so far indicate that the HE susceptivity of AM
because of the finer microstructure produced by AM processing [82]. 316L SS is closely related to the initial microstructure, such as the
The corrosion behaviour of the AM 316L SS has been well documented morphology and density of dislocations. While, the deformation twin­
[4,17,54]. In contrast, there is less research on HE, although it is ex­ ning, dendritic segregation, and precipitates are considered to have little
pected that the HE sensitivity of AM 316L SS would be different to 316L effect. Further detailed studies on HE in the as-built DED 316L is still
produced by conventional methods. needed to fully elucidate the mechanisms that are responsible for the
Miller et al. [17] investigated the HE of 316L fabricated by AM. embrittlement [18]. In addition, previous results suggested that SLM
Fig. 33 shows that the LPBF 316L had lower ductility (due to the high 316L SS can be a candidate for use in hydrogen environments because of
residual stress and higher porosity) and higher HE susceptibility than the its relatively high YS and resistance to HE.
thermomechanical (TM) 316L. The LPBF 316L showed lower strength
and lower strain to fracture after exposure to the air for 2184 h, whereas, 4.3.2. Precipitation-Hardening stainless steels
both strength and ductility were increased for the TM 316L. It was Precipitation-hardening stainless steel (PHSS) has ultrahigh strength
considered that the faster diffusion of hydrogen in the LPBF 316L was and good corrosion resistance [8] and is prevalently used in aerospace,
responsible for the HE. Nevertheless, it is hard to understand the in­ oil and gas industries, chemical plants, and the marine industries. AM of
crease in tensile properties of the TM 316L after exposure to air, and PHSS has attracted significant interest from researchers [8,343], with
clarification work is needed (see Fig. 34). greatest attention devoted to 17-4PH and 15-5PH
Bertsch et al. [18] also studied the HE behaviour AM 316L produced [164,168,319,344–346]. Both steels are strengthened by precipitation
using SLM and DED. Fig. 32 shows that hydrogen charging reduced the of extensively dispersed Ni3Al, Ni3Ti, Ni3Mo, B2A Laves phase and other
ductility of the as-built SLM and DED 316L. In contrast, post-processing intermetallic precipitates in the martensite matrix [347,348]. 17-4PH SS
heat treatment (HT) eliminated the hydrogen sensitivity of the SLM contains 15 ~ 17.5 wt% Cr, 3 ~ 5 wt% Ni and 3 ~ 5 wt% Cu and is
samples and weakened the HE sensitivity for the DED samples. The typically aged at 480 to 620 ◦ C after solid solution heat treatment, which
hydrogen sensitivity of the DED 316L seemed higher than for SLM 316L. achieves a YS of 1370 MPa, a UTS of 1450 MPa and an elongation of 9%
It was considered that the HT reduced or even eliminated the AM defects for the wrought alloy [168,347,349,350]. Research has indicated that
such as porosity and residual stress, and therefore enhanced the HE- the solid solution treated wrought 17-4PH steel has higher HE resistance
resistance. The smaller melt pools and faster cooling of the SLM pro­ than the peak-aged steel [351]. This indicates that the hydrogen sensi­
cess compared with the DED process may be responsible for the lower tivity of this steel also depends on the microstructure.
HE susceptivity of SLM 316L compared with the DED 316L. Research has studied the susceptibility of AM 17-4PH to pitting,
Fig. 35 shows that the hydrogen charging did not change the mi­ environmentally assisted cracking (EAC) [352,353], and stress corrosion
crostructures of as-built SLM and DED 316L SS. However, the deformed cracking (SCC) [354]. Guennouni et al. [352] found that AM 17-4PH
microstructures varied with hydronation as shown in Fig. 36. The steel exhibited improved resistance to pit initiation due to the pres­
microstructure of the SLM 316L remained unchanging after deformation ence of finer and fewer NbC particles. However, they found that stable
and hydrogen charging. In contrast, equiaxed dislocation cells were pits propagated faster for AM 17-4PH steel due to the larger amount of
present during the later stages of the deformation of DED 316L and retained austenite. Stress was found to stabilize metastable pits, but to
hydrogen charging promoted the development of texture within twin- accelerate the propagation of stable pits, resulting in an increased sus­
free regions. This indicated that the DED 316L may be more sensitive ceptibility to EAC in AM 17-4PH. Shoemaker et al. [354] reported that
to hydrogen. Hydrogen has the ability to be attracted to the stress fields the SCC performance of AM 17-4PH was consistently inferior to wrought
surrounding dislocations due to the HELP mechanism, resulting in a steel, with crack growth rates up to 5 times higher. This degradation was
decrease in the spacing between dislocations and an increase in their attributed to an elevated oxygen content, porosity induced by argon
mobility [201]. Several studies have demonstrated that when materials processing, and fast cooling rate during AM processing.
are subjected to strain, hydrogen can expedite the formation of dislo­ Alnajjar et al. [55] comparative the HE of SLM and wrought 17-4PH.
cation microstructures. This is accomplished by reducing the average The SLM processed 17-4PH has a δ-ferritic microstructure with rela­
size of dislocation cells in various materials such as Ni and Fe at a given tively fine grains (as shown in Fig. 37) due to the rapid cooling during

Fig. 33. Stress-Strain graphs for traditional manufacturing (TM) and LPBF samples before exposure (control) and after 2184 h of exposure. Reproduced from Miller
[17] with permission from Elsevier.

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 34. Engineering stress–strain curves for specimens of (a) SLM and (b) DED 316L. Thin curves represent as-built 316L (black for uncharged, red for hydrogen-
charged), and thicker curves represent heat-treated 316L (grey for uncharged, pink for hydrogen-charged), for both a and b. Reproduced from Bertsch [18] with
permission from Elsevier. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

Fig. 35. Bright-field STEM micrographs of dislocation structures at 15% elongation in (a & b) as-built SLM, and (c & d) as-built DED 316L SS. Dashed line in (b)
parallel to deformation twins, dotted lines in (c & d) indicate dislocation cell walls with dendritic segregation profiles. Reproduced from Bertsch [18] with permission
from Elsevier.

SLM, which suppressed the formation of austenite and retained δ ferrite testing (pre + charged). These results allow identification of the dif­
at room temperature. Aging both the wrought and SLM 17-4PH steels at ference in HE susceptibility. Both the wrought and the SLM steels were
580 ◦ C for 4 h caused precipitation of nanoscale Cu-containing pre­ susceptible to HE evidenced by a significant reduction in elongation of
cipitates in both steels. SSRT tests were used to study the HE behaviour the H-charged samples. Nevertheless, the SLM ferritic steel showed
in an acidic chloride solution at room temperature with cathodic higher strength and better ductility for all testing conditions (uncharged,
charging. Fig. 38 presents the slow strain rate stress–strain curves of pre-charged, and pre-charged with continually charging during testing
specimens in the following conditions: (i) uncharged, (ii) pre-charged and different strain rate) than the martensitic wrought steel. This was
and (iii) pre-charged plus continually charging during the tensile attributed to the fine microstructure of the SLM alloy.

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 36. Bright-field STEM micrographs of dislocation structures up to 250 μm away from the fracture surfaces in (a & b) uncharged & (c & d) hydrogenated as-built
SLM (left) and DED (right) 316L. Arrows indicate voids formed along dislocation walls. Reproduced from Bertsch [18] with permission from Elsevier.

Fig. 37. EBSD data obtained on the SLM 17-4PH

steel aged 4 h at 580 ◦ C. (a) phase map of the X-
Z plane. The BCC and FCC phases are in blue and
black respectively. The non-indexed areas are in
white. (b) orientation map of the X-Z plane (IPF Z,
where Z is the building direction), (c) phase map of
the X–Y plane. (d) orientation map of the X–Y
plane. Reproduced from Alnajjar [55] with
permission from Elsevier. (For interpretation of the
references to colour in this figure legend, the reader
is referred to the web version of this article.)

4.4. Ultrahigh strength steels additive manufacturing of ultrahigh strength steels provides advantages
for integrated part production. Work on AM has focused on maraging
Ultrahigh-strength steels are predominantly used in aerospace, steels, 4340 steel, and tool steel. High strength steels are associated with
defence and marine industries to fabricate engineering components high susceptibility to hydrogen because of their high strength. There­
subjected to high load and with high geometrical complexity. Hence, fore, investigation and understanding of the HE behaviour of these AM

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 38. Stress–strain curves of (a) wrought and (b) SLM smooth 17-4PH specimens. Reproduced from Alnajjar [55] with permission from Elsevier.

steels are essential before they can be practically used. HE of wrought produced during SLM or casting because these defects can accumulate
ultrahigh strength steels has been comprehensively studied. However, hydrogen and promote crack propagation and brittle fracture [225].
research on HE of AM steels is limited. The following sections review the The HE behaviours of grade 300 maraging steel processed by SLM
currently published results on maraging steels, 4340 steel, and tool steel. were investigated by Li et al. [254] and Kwon et al. [57]. Li et al. [254]
examined the microstructures and mechanical properties of the grade
4.4.1. Maraging steels 300 maraging steel, processed by SLM, before and after hydrogen
Maraging steels contain almost no carbon but a high content of other charging. The hydrogen charged specimen suffered severe HE as the
alloying elements, including nickel, cobalt, and molybdenum. The ul­ strength and plasticity decreased significantly. In situ high energy X-ray
trahigh strength is achieved through precipitation of intermetallic diffraction (XRD) and EBSD were used to study the mechanism of the
compounds, such as Ni3Ti, Ni3Mo Fe2Mo and Fe7Mo6, that form during fracture mode transition from ductile fracture to brittle fracture after
aging after the steels are quenched to martensite [355]. Maraging steels hydrogen charging. The results are shown in Fig. 39. The SLM 300
combine ultrahigh strength and high toughness, which is critically maraging steel has a martensitic matrix similar to that of a conventional
important in the aerospace sector. The most typical maraging steel is the grade 300 maraging steel, with irregular coarse plate martensite [361].
18Ni, which can achieve tensile strength over 2000 MPa after proper Hydrogen charging did not cause any phase transformation. Compared
heat treatment. to the uncharged sample, the hydrogen charged steel has significantly
Several studies have shown that SLM processing can produce fully lower tensile strength and elongation at break and no apparent plastic
dense maraging steel, which showed mechanical properties comparable deformation at failure. They found that the ductile to brittle fracture
to those produced utilizing traditional manufacturing [356–359]. mode transition in the SLM maraging steel was induced by hydrogen
However, maraging steels produced either using traditional routes charging. There were non-uniform dimples, a typical feature of ductile
[54,57,356,360] or using AM [225] are very susceptible to HE, mani­ fracture, on the fracture surface of the uncharged specimen, whereas the
festing as a reduction in mechanical properties [54,57,356,360]. In hydrogen charged specimen showed a brittle fracture mode with a
addition, HE of maraging steel is increased by the presence of pores mixture of dimples and cleavage planes, as presented in Fig. 40. They

Fig. 39. (a) OM and (b) IPF micrographs of the studied AM grade 300 maraging steel, and (c) high energy XRD profiles of the hydrogen-free and hydrogen-charged
specimens before deformation. Reproduced from Li [254] with permission from Elsevier.

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 40. The macroscopic and microscopic morphologies of the fracture surfaces of the uncharged and hydrogenated samples showing the obvious HE. Reproduced
from Li [254] with permission from Elsevier.

proposed that the ductile to brittle fracture mode transition in SLM traditional methods [57,356,357].
maraging steel in the presence of hydrogen was due to the locally pre­ However, there is still no systematic comparison and analysis be­
mature martensitic transformation (as in Fig. 41) and cracking along the tween maraging steels fabricated by AM and conventional methods.
{1 1 1} retained austenite plane that was perpendicular to the loading Thus, further investigation is necessary.
direction. The microcracks released the localised stress fields in retained
austenite and thus inhibited the further phase transformation from 4.4.2. AISI 4340 – High strength low alloy steel
retained austenite to the newly formed martensite. These microcracks AISI 4340 steel is a typical medium carbon low alloy ultra-high
coalesced and propagated rapidly under the applied stress, leading to strength steel with YS over 1860 MPa [94]. The shape complexity of
the brittle fracture of the hydrogen charged specimen. engineering parts made of this steel drives the research of AM of 4340
In addition, Kwon et al. [57] also studied how post-heat treatment steel. Currently, the LAM techniques used for 4340 steel include laser
affected the HE of the SLM 18Ni 300. They found the reduction in the welding and laser cladding for repair. The current major research effort
amount of retained austenite that was replaced with martensite at the is undertaken to evaluate the microstructure evolution during the repair
borders of the solidification cells. Compared to the hydrogen charged as- of some high-value AISI 4340 steel components by the DMD process
built counterparts, the hydrogen charged heat-treated samples had a [155,362–364]. However, there are only a few studies that investigated
smaller number of trapped hydrogen atoms and showed improved the mechanical properties and microstructure of 4340 steel processing
ductility in the tensile tests. The reduction of the austenite content and by the PBF methods [155,362,363,365].
the dislocation density after heat treatment led to the decrease in AISI 4340 steel is prone to HE, which is a common cause of failure
hydrogen susceptibility of the steels. Furthermore, they reported that [197,366,367]. Generally, higher strength steels are more susceptible to
isothermal aging improved the strength of the uncharged steel, but HE [367]. During the steel manufacturing process, hydrogen is easily
resulted in more hydrogen trapped and thus reduced HE resistance. absorbed by liquid Fe, which results in IHE C +H2 O ↔ CO +H2 and
Thus, it was concluded that artificial aging had a negative effect on the Fe +H2 O ↔ FeO +H2 [197]. Internal hydrogen has a substantial influ­
HE resistance of steel, whereas heat treatment had a positive effect. The ence on high-strength steels. Because of the ease of microcrack growth,
same tendency was observed in maraging steels manufactured using IHE by the mechanism of high-pressure bubble formation might be

Fig. 41. Lattice strain evolution of the martensite and retained austenite in the (a) uncharged and (b) hydrogenated specimens with the applied stress along the
loading direction. Reproduced from Li [254] with permission from Elsevier.

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

extremely severe [366]. From the diffusion perspective, the major H- martensite matrix, a small amount of retained austenite, and
trap sites in low alloy carbon steels are most likely associated with composition-dependent carbides [157,160,373–375]. Such a micro­
dislocations, within the interfaces of the martensite nano-structure, and structure also occurs in laser-welded or laser-cladding parts [376,377].
with the interface between the matrix and particles including carbides, The microstructure of AM H13 steel is characterised by ultrafine cellular
nitrides and carbonitrides. In the AISI 4340 steel, dislocations are sug­ or dendritic sub-grain structures due to the fast cooling (103 ~ 106 K/s).
gested as the major H-trap sites [368,369]. These microstructures are not common in cast H13 [119]. In PBF H13
Liu and co-workers [369] reported two-stage permeation and trap­ steel, the intrinsic heat treatment can decompose martensite into fine
ping of hydrogen in as-received commercial 4340 steel attributed to the ferrite and Fe3C precipitates, which is similar to traditional tempering
presence of two types of hydrogen trapping sites, which were identified [160]. DED H13 steel specimens had strengths similar to their wrought
as ferrite GBs and dislocations (trap 1) and ferrite/cementite interfaces counterparts [93,157], but, the elongation (approx. 5% ~ 6%) was
(trap 2). Fig. 42 shows that the apparent diffusivity of hydrogen in trap 1 lower than traditionally manufactured parts (approx. 9%) [378]. The
was higher than that in trap 2, while the saturation concentration of ductility for the PBF H13 steel (<4%) was even lower than that for the
hydrogen for trap 1 was lower than that for trap 2. DED-built components. The high brittleness of AM H13 is related to the
Fig. 43 shows that the representative microstructure from the high content of carbon martensite, and high residual stress, up to 1420
research of Liu and co-workers [369] of as-received commercial 4340 MPa, because of the fast-cooling of the AM process [379–381]. The YS
steel (in the hot rolled and slow cooled condition) consisted of ferrite and UTS of H13 vary from about 830 to 1564 MPa and from 900 to 2064
and pearlitic (lamellar cementite), while the microstructure of the PBF MPa, respectively, indicating the high fluctuation of mechanical prop­
4340 steel was predominantly martensitic with fine microstructure erties in the AM H13 components [8].
because of the rapid cooling of the melt pools [155]. It should also be HE is not a major cause of failure for tool steels in service. Thus, there
mentioned that 4340 is typically used in the quenched and tempered is a lack of research on the HE properties of tool steels [382]. However,
condition, for which the microstructure is tempered martensite. As as previously stated, high-strength steels are highly susceptible to HE
mentioned before, HE is sensitive to microstructure, and microstructural [244]. This high hydrogen sensitivity is often linked to the presence of
alteration may lead to improvement in resistance to HE [34]. Thus, it martensite in the microstructure [227]. For example, AISI H13 is a high-
could be expected that the interaction of hydrogen with microstructural strength martensitic steel, and thus is likely to be sensitive to HE. The
defects of 4340 manufactured by AM is different to that produced using AM can impart better properties to H13 steel, including high strength,
conventional methods. Although the HE of AISI 4340 fabricated by good anisotropy performance and high design freedom, which expands
conventional methods has been considerably investigated the application range of this steel. To date, highly dense H13 steel parts
[197,366,367,369–371], no literature has been dedicated to the study of have been successfully produced using AM by optimizing the processing
HE of AM AISI 4340. In order to advance the research of AM 4340 steel parameters [117]. However, there is no literature dedicated to the study
and realise its industrial applications, it is necessary and essential to of the HE of AM H13 steel, even in commercial H13 steel processed by
investigate the HE performance (see Fig. 44) conventional methods. For the development of industrial applications of
AISI H13 steel, it is necessary to systematically and comprehensively
4.4.3. AISI H13 – Tool steel investigate the HE performance.
Tool steel refers to a variety of carbon and alloy steels that are In summary, the studies on the HE performance of AM steels has
particularly well-suited to make tools, such as cutting tools, dies, and mostly focussed on austenitic stainless steels, including AISI 304L and
moulds (TDM). Complicated TDM manufacturing can take months or AISI 316L. Precipitation-hardening stainless steel such as 17-4PH and
even years and entails high costs. AM offers a new tool-making route, grade 300 maraging steel have also received some attention. The effect
which can shorten the production cycle by around 40%. In addition, AM of post-heat treatment [16–18,55,57] and different AM processes [18]
methods can also directly fabricate geometrically complex shapes, such on the HE properties of AM steels have been investigated. Most studies
as internal cooling channels, enhancing the design function [8]. showed that the strength and plasticity of steel specimens decrease after
AISI H13 steel is one of the most common tool steels, and is char­ charging with hydrogen [13,55,254]. But, the majority of steels fabri­
acterised with high strength, high toughness, high hardenability and cated by SLM have better resistance to HE than steels produced by
good resistance to thermal softening. AISI H13 has been extensively conventional fabrication methods [18,55]. Further research is necessary
studied after production by both the PBF and DED processes due to the insufficient number of studies that systematically compare
[8,93,158,372,373]. The typical microstructure is characterised by a and analyse the HE performance of steels fabricated using conventional

Fig. 42. (a) Calculated variation of hydrogen concentration, CH, with electrochemical charging time, t, in the two traps present in 4340 steel, (b) comparison of
calculated (cal) and experimentally (exp) measured variation of total hydrogen concentration, CH, with electrochemical charging time, t. [369].

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 43. Micrographs of (a) as-received commercially AISI 4340 steel (hot rolled and slow cooled) [369] and (b) as-built PBF AISI 4340 steel. [363].

Fig. 44. (a, b & c) SEM images on the cross-section of an LPBF-built H13 steel; (d) TEM image of another LPBF-built H13 steel showing the lath martensite and M23C6
carbide; EBSD phase map (e) and orientation colour map (f) of an LPBF fabricated H13 steel; (g) Low magnification image of the microstructures in an LDED built
H13 sample; (h & i) SEM image of microstructure of the as-built LDED H13 sample: (h) the top, (i) the middle. Reproduced from Yin [8] with permission from Taylor
& Francis, and Tan is the author of the paper.

methods and AM methods. Moreover, there is a lack of studies on using [199,388–392].

AM methods to manufacture hydrogen-sensitive high-strength AISI AM of HEA has attracted considerable attention [393]. Compared
4340 steel, and H13 steel. with conventional techniques for making HEAs, such as the plasma arc
melting, AM of HEA allows the creation of non-equilibrium micro­
structures and may produce comparable or better mechanical properties
4.5. High-Entropy alloys (HEAs) [394,395]. The current mainstream AM processing methods for HEAs
are DLD (also known as LMD, DMD, LENS and laser cladding), SLM (also
High-entropy alloys (HEAs) are a relatively new alloy class with five known as LBM, DMLS, LMF) and EBM, as listed in Table 7 [80,393]. A
or more principal elements [383]. The concentration of each element in few HEAs [199], including CoCrFeNiMn [396–398], CrMnFeCoNi
the HEA is 5 ~ 35 atomic% [384]. This innovative alloy design method [396,399], CrFeCoNi [400], AlCoCrFeNi [401,402], AlCoCrFeNiTi0.5
has resulted in several HEA systems with good properties, including [403], compositionally graded HEAs [404,405], and laminated HEAs
good corrosion resistance [385], good fracture toughness at cryogenic [406], have been successfully produced with AM using either pre-
temperatures [386], and high strength at elevated temperatures [387]. alloyed HEA powders or mixed metallic powders. Moghaddam et al.
Thus, HEAs may find much potential in harsh environment applications. [80] published a review of HEAs processed using AM, including the
Several detailed review papers on HEAs have been published

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Table 7 [258,414]. The rapid cooling also causes a significant accumulation of

Summary of HEAs processed through powder-based AM methods dislocation groups, leading to the formation of a cellular structure with a
[80,393]. high density of dislocations at cell walls [415–417]. In addition, tradi­
Alloys AM processes tional manufacturing methods such as casting, melting, and powder
CoCrFeNiMn (Cantor)-based LMD, SLM
metallurgy cannot achieve the production of precise parts with complex
AlxCoCrFeNi-based LMD, DMD, SLM structures. Typically, products manufactured through traditional
MoNbTaW LMD methods require additional machining before they can be put into ser­
FeCoCrAlCu LMD vice. This not only leads to material wastage but also increases costs,
TiZrNbWMo Laser Cladding
thereby restricting the development and application of HEAs [258].
CrMoTaWZr Laser Cladding
AlTiVMoNb Laser Cladding Currently, the AM processes have been successfully applied to prepare
MoNbTaW SLM the CoCrFeMnNi [396–398].
Ni6Cr4WFe9Ti SLM Due to the superior HE resistance of conventionally produced
CoCrFeNi SLM CoCrFeNiMn HEAs, several studies have investigated the HE perfor­
AlxCoCrFeNi LENS, SLM, EBM
CoCrFeNiTi-based EBM
mance of AM CoCrFeNiMn HEAs. Fu et al. [257] investigated the HE
Al0.5CrMoNbTa0.5 EBM behaviour of the as-built SLM and post-annealed equiatomic CoCr­
FeMnNi HEA samples using SSRT (initial strain rate of 1 × 10− 5s− 1) tests
under in situ electrochemical hydrogen charging. The testing results in
feedstock requirements, common processing methods (LMD, SLM and air (as shown in Fig. 45) showed that annealing at 900 ℃ for 1 h
EBM), microstructures features along with their properties and under­ increased the uniform plasticity from 20% of the as-built SLM sample to
lying mechanisms, and a conclusion of the current state and prospects of 3%, but slightly reduced the UTS from 751 to 707 MPa. However, the
AM HEAs. This review summarises the responses of HEAs to hydrogen. UTS of the annealed sample was still significantly higher than that of the
traditional manufactured CoCrFeMnNi. Hydrogen charging remarkably
4.5.1. CoCrFeNiMn reduced the plasticity, indicating the high hydrogen susceptivity of this
The equiatomic CoCrFeNiMn HEA alloy has a single-phase FCC alloy. The stress–strain curves with in situ hydrogen charging (Fig. 45
crystal structure, which has a good combination of strength-ductility at (a)) showed only 3.3% uniform plasticity of as-built SLM samples. In
room and cryogenic temperatures. CoCrFeNiMn HEA was reported as contrast, annealed samples exhibited about 10% uniform plasticity. This
having a HE susceptibility lower than that of the 304 and 316 ASSs implied that annealing improved the HE resistance. The annealed SLM
[407–411]. Moreover, the HE resistance of CoCrFeNiMn HEA can be CoCrFeNiMn had delayed initiation and propagation of cracks after
increased by increasing the nano-twin density [412]. hydrogen charging, which effectively improved the HE resistance of the
However, the strength of this alloy, when processed using traditional SLM samples. Investigations on both as-built SLM and annealed proto­
methods, is relatively low, with an YS of approximately 300 MPa and type CoCrFeMnNi HEA samples suggested that annealing preserved the
UTS of approximately 530 MPa. This limitation has drawn the attention cellular structures while effectively reduced the dislocation densities.
of many researchers aiming to enhance the mechanical properties [413]. Fig. 46 shows that a high dislocation density was distributed along the
AM offers advantages in improving material properties due to the rapid fusion boundary in as-built SLM CoCrFeNiMn, while annealed SLM
cooling, which facilitates the formation of finer microstructure

Fig. 45. Results from the SSRT tests in air and under in situ hydrogen charging of as-built SLM and 900 ℃ for 1 h annealed samples: (a) engineering stress–strain
curves; (b) UTS values; (c) uniform plasticity values; (d) strength loss (σL ) and uniform plasticity loss (δL ). Reproduced from Fu [257] with permission from Elsevier.

31
J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 46. High magnification electron channelling contrast imaging (ECCI) on X-Y plane of the uncharged (a) as-built SLM and (b) annealing at 900 ℃ for 1 h samples.
Reproduced from Fu [257] with permission from Elsevier.

CoCrFeNiMn was associated with a relatively low-density of disloca­ density (VED) evaluated using the following empirical equation (Eq.5)
tions. Thus, annealing slightly reduced the strength, annealing signifi­ [418].
cantly increased the ductility and HE resistance as indicated by the SSRT
P
tests with in situ electrochemical hydrogen charging. VED = (5)
vht
Fu et al. [257] also reported that crack initiation and propagation
were delayed by the HELP mechanism for the same alloy because of the where P is the laser power, v is the scanning speed, t is the layer thick­
formation of nano-twins and dislocation cells in the modified structures. ness, and h is the hatch spacing.
During testing with hydrogen charging, a region with nano-sized It was found that the improper LPBF parameters led to increased
deformation twins and dislocation cells formed beneath the surface of numbers of microcracks and holes, resulting in a slight decrease in the
the annealed sample. This region was also enriched with hydrogen. HE resistance of the material. Fig. 47 shows that the sample processed
Hydrogen can enhance the motion of dislocations, increase their using the medium VED had the highest UTS and elongation before and
mobility, reduce the stacking fault energy and facilitate the formation of after hydrogen charging, which were 663 MPa, 24% and 646 MPa, 24%,
nano-sized twins and dislocation cells. This deformation area delayed respectively. In contrast, the low VED sample had significant processing
the initiation of HE cracks by reducing the hydrogen concentration at defects, had the lowest UTS of 633 MPa, the highest elongation loss ratio
the GBs. However, as deformation and hydrogen concentration of 17% and strength loss ratio of 3% after charging hydrogen. Hydrogen
increased near the sample surface, HE cracks initiated along specific charging did not produce a significant effect on the YS, indicating that
crystal planes and propagated. Along the crack path, GBs captured more hydrogen did not cause solid solution strengthening, which is consistent
hydrogen, leading to the formation of slip bands and dislocation cells with some previous related studies [257,258,412]. Thus, they concluded
that slowed the crack propagation. Thus, it is expected that the HE that proper process parameters can produce better mechanical proper­
resistance of SLM CoCrFeMnNi can be improved by post-processing. ties, and even after hydrogen charging, there can be uniform plastic
Lin et al. [223] also confirmed that a heat treatment of CoCrFeMnNi deformation. In addition, the samples with three different processes
at 900 ◦ C reduced dislocation density at the cell walls, which conse­ have low strength loss and elongation loss ratio, reflecting significant
quently reduced the metal’s ability to trap hydrogen. They attributed the hydrogen embrittlement resistance. In addition, the elongation of the
decrease in trapping capability in the heat-treated SLM sample to both high VED sample was increased after charging hydrogen, which in­
decrease in dislocation density and removal of Mn segregation. They dicates that hydrogen increased ductility for LPBF CoCrFeNiMn [258].
discovered that a change from HE in the as-built SLM sample to In addition, Cheng et al. [258] found that hydrogen charging
hydrogen-induced plasticity in the heat-treated SLM sample was ach­ increased the strain hardening rate of the LPBF CoCrFeNiMn HEA. This
ieved by modifying the cell structure through heat treatment. There increase was associated with a notable increase in the proportion of
were higher amounts of hydrogen in the hydrogen affected region of the deformation twins in the presence of hydrogen. This strengthening
as-built sample compared to that of the heat-treated sample aggravated behaviour became evident after the emergence of the strain hardening
the HEDE mechanism, which consequently enhanced the formation of platform, enabling the strain hardening rate to reach and surpass that of
intergranular cracking with relatively low strain localisation and the sample without hydrogen charging. This phenomenon played a vital
degraded HE resistance. The HELP mechanism is also activated in the as- role in strengthening the material, contributing significantly to the
built HEA sample. Hydrogen amounts were initially higher in the as- strengthening mechanism. In addition, the extra work hardening
built SLM sample, and the hydrogen concentration at the GB could resulting from the presence of deformation twins is commonly associ­
further increase when hydrogen atoms were transported to the GB ated with the “dynamic Hall-Petch” effect [419]. The formation and
intercepted by deformation twins. Therefore, the GBs intercepted by propagation of nanotwins introduced new interfaces that led to grain
deformation twins with high concentrations of hydrogen were more fragmentation, thereby reducing the mean free path of dislocations. In
susceptible to the HEDE mechanism and high stress concentrations, summary, the strengthening effect caused by a significant quantity of
making them the preferential initiation sites and propagation paths for deformation twins increased the HE resistance of LPBF CoCrFeNiMn
intergranular cracking. This combined interplay of the HELP and HEDE HEA, to maintain comprehensive mechanical properties in a hydrogen
mechanisms is referred to as HELP-mediated HEDE model [44,212]. environment. However, this positive effect may be diminished under
Therefore, the pronounced twinability in the as-built SLM CoCrFeMnNi unfavourable process parameters.
sample results in intensified intergranular cracking.
Furthermore, Cheng et al. [258] studied the effect of different pro­ 4.5.2. AlCoCrFeNi2.1
cessing parameters on the HE performance of CoCrFeNiMn HEAs The AlCoCrFeNi2.1 eutectic HEA has gained significant attention due
fabricated by LPBF using SSRT tests with and without hydrogen. They to its distinctive in-situ composite structure, which effectively addresses
characterised the processing parameters using volumetric energy the limitations of inadequate strength in FCC single-phase HEA and

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J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 47. Mechanical properties of LPBF samples under different processes with and without hydrogen processed using VED values of (a) 71 J/mm3, (b) 81 J/mm3 and
(c) 90 J/mm3. Reproduced from Cheng [258] with permission from Elsevier.

insufficient ductility in BCC single-phase HEA [420]. Several researchers suggested an inhomogeneous hydrogen diffusion that was strongly
have successfully produced AlCoCrFeNi2.1 HEA using AM methods, dependent on the local microstructure. Fig. 48 indicates that the inter­
including LMD [421], SLM [420,422,423], and PAAM (powder-bed arc facial cracking of the H-charged specimens can be attributed to a locally
additive manufacturing) [424]. increased hydrogen concentration at the phase boundaries between the
Wan et al. [199] used in-situ small-scale tensile testing with and FCC/L12 and BCC/B2 phases. Fig. 49 shows representative cases of the
without cathodic hydrogen charging to investigate the HE behaviour of phase morphology dependence of the deformation and crack initiation.
the AlCoCrFeNi2.1 eutectic HEA, which was fabricated with LENS using The cracking susceptibility was also influenced by the relative orienta­
pre-alloyed powder. As-cast samples were also tested as a reference. The tion of the phase boundary and the loading direction. When the phase
hydrogen charging led to a drop in the strain to failure of the LENS HEA boundary was nearly perpendicular to the loading direction, fracture
from 10% to 7% with an embrittlement factor of 33%. In comparison, was more easily initiated. In this case, cracks highly likely initiated in
the as-cast sample exhibited a reduction in ductility from 19% to 16%, the BCC/B2 phase. In the phase boundaries of the examined eutectic
with an embrittlement factor of about 20%. Both samples exhibited a HEA, there was a Kudjumov-Sachs (K-S) type orientation relationship
decrease in the UTS (AM sample: from 1214 MPa to 1126 MPa and as- [425] between FCC/L12 and the BCC/B2 phases, which may allow for
cast sample: from 1007 MPa to 959 MPa) but a slight reduction in the slip transfer between the two phases. They concluded that the regular
YS (AM sample: 820 MPa & as-cast sample: 480 MPa). The fractured H- high-angle GBs were more vulnerable to cracking than low-angle GBs
charged specimens showed surface fissures that were not present in the and phase boundaries, according to the EBSD study of hydrogen-induced
hydrogen-free specimens, indicating brittle behaviour. TDS analysis surface cracks in the AM samples. Both the HELP and HEDE mechanisms
indicated a larger concentration of hydrogen (approx. 12 wppm) in the are typically activated in this HEA. Within the FCC/L12 phase, hydrogen
AM specimen than in the as-cast specimen (approx. 9 wppm). Thus, they restricts the deformation to specific slip systems, intensifying local
concluded that the finer microstructure and increased density of deformation and leading to localized necking and failure. This process
boundaries in the AM sample contributed to the larger hydrogen uptake. results in cracking along the slip traces. Whereas hydrogen also di­
In addition, Wan et al. [199] used finite element analysis (FEA) to minishes the bonding energy at boundaries, making them more sus­
simulate the hydrogen diffusion in both AM and as-cast samples and ceptible to opening as cracks approach due to the stress field created by

Fig. 48. Detailed fractography of the tested specimens (H-charged): (a & b) as-cast; (c & d) AM. [199].

33
J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

Fig. 49. Representative cases showing the phase morphology dependence of the deformation and crack initiation. (a1-a3) representative phase morphology; (b1-b3)
exemplary SEM images of the as-cast specimen; (c1-c3) exemplary SEM images of the AM specimen. The global tensile direction is horizontal. [199].

these cracks.
Table 8
Overall, HEAs can be high-strength materials. High-strength mate­
The dominant HE mechanisms of metals by additive manufacturing (AM) and
rials are critical when serving in a hydrogen-containing environment, as
traditional (TR) methods.
they might experience higher mechanical stress and thus a higher sus­
ceptibility to HE owing to their high strength [199,408,409,426]. Materials AM Ref. TR Ref.

Currently, although several attempts to produce high-strength HEAs by Ti-6Al-4 V HFC [29–37] HFC [32]
AM have been successful, the study of HE behaviour of the AM HEAs is IN 718 HELP + HEDE [23,28] HELP + [216,217]
HEDE
still limited. The knowledge gaps of the current research on the effect of
AISI 304L HELP + HEDE [13,16] HELP + [16,427]
the HE performance of HEAs include but are not limited to different HEDE
feeding mechanisms, the type of heat sources, and the direction of AISI 316L HELP [17–20] HELP [217,428]
printing. Therefore, for the development of HEAs’ practical applications, 17-4PH HELP [55] HELP [55,429]
it is necessary to systematically and comprehensively investigate the HE 18Ni 300 HELP [57,254–256] HELP [356,361]
CoCrFeNiMn HELP1 [257,258]1 HELP [407–411]
properties of this material. HELP-mediated [223]2
HEDE2
AlCoCrFeNi2.1 HELP + HEDE [199] HELP + [199]
4.6. Summary HEDE

4.6.1. The dominant HE mechanism of AM metals

Table 8 lists several alloys that have been identified the prevailing some alloys also cite the synergistic action of HELP and HEDE. For Ti
HE mechanisms and have been fabricated using AM and traditional alloys, the mechanism involves HFC.
methods. The predominant HE mechanism for AM metals is HELP. But, Currently, there is no obvious discernible distinction in HE

34
J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

mechanisms between materials manufactured through AM and those a single AM method with traditional methods.
produced using traditional methods. Nevertheless, the susceptibility of
metals to HE remains disparate across various manufacturing methods, 4.6.2.3. Anisotropic properties. In addition to the finer microstructure,
largely attributable to the distinct microstructural characteristics most AM metals also exhibit pronounced anisotropy due to the direc­
inherent in materials produced through AM. tional solidification feature that results in the formation of columnar
grains, distinguishing them from their wrought counterparts
4.6.2. Influences of microstructural features of AM metals on HE [95,318–321]. This inherent anisotropy can introduce variations in
As previously mentioned, AM processes are characterised with rapid susceptibility to HE along different orientations, necessitating a
cooling and directional solidification within small melt pools. Conse­ comprehensive study of the build orientations effects on the hydrogen
quently, the microstructures and properties of metals produced through sensitivity of the AM metals. Currently, several studies have indicated
AM significantly differ from those manufactured using conventional that vertical (i.e., obtained parallel to the printing direction) AM IN718
methods [8,51]. It is widely acknowledged that HE is influenced by a samples exhibit superior HE resistance compared to their horizontal (i.
number of factors, including sample density and microstructural char­ e., obtained normal to the printing direction) counterparts. This
acteristics such as dislocation density, grain boundaries, and internal improved resistance can be attributed to the suppression of hydrogen
cracks and voids [40]. The major differences in microstructural features entrance by columnar dendrites [23,24]. However, tests on AM Ti-6Al-4
between AM metals and conventionally produced metals, and their in­ V showed contrasting results, with vertical samples displaying lower HE
fluence on HE are summarised as follows: resistance compared to samples oriented horizontally. This disparity can
be ascribed to the horizontal direction may have a high-stress intensity
4.6.2.1. Metallurgical defects. AM processes have been known to intro­ environment that reduced the probability of the stress-induced hydride
duce metallurgical defects, including porosities, cracks, and inclusions mechanism [30]. As such, the current body of research cannot defini­
[51,99]. These defects can serve as sites for hydrogen absorption and tively determine whether vertically constructed samples outperform
subsequently promote embrittlement [40]. In addition, defects and horizontally constructed ones in terms of HE resistance. Nonetheless, it
micro-segregation in AM components can promote microcrack coales­ is evident that a strong correlation exists between HE performance and
cence, resulting in a more severe reduction in ductility [15,258]. the anisotropic characteristics of the samples, emphasising the need for
However, the majority of the current research primarily focuses on further investigation in future studies.
evaluating the HE performance of high-density samples, with limited In summary, the microstructural characteristics of AM metals make
consideration to the influence of material defects on HE. Given that their HE susceptibility differing to the counterpart metals produced
defects are a prevalent microstructural feature in AM metals, it is using conventional methods. A comprehensive understanding of AM
imperative to place greater emphasis on investigating their roles in HE. microstructural features that affect HE is essential for advancing the
knowledge and mitigation strategies related to HE in AM metals. Further
4.6.2.2. The finer microstructure. Finer microstructures associated with research is needed to explore these intricate relationships and develop
AM metals also influence HE susceptibility by increasing the boundary effective solutions to enhance the resistance of AM metals to HE.
density [199] and dislocation density [55]. Previous studies have
demonstrated that finer microstructure in AM samples often results in 5. Conclusions and outlook
increased hydrogen uptake [199]. However, in some cases, AM samples
with finer microstructure may exhibit a lower HE susceptibility, such as The present state of research on the HE of metals fabricated using AM
austenite in AM 304L SS [13,16]. The high cooling rate during the AM is presented in this review with a focus on the mechanisms and primary
process generally results in a finer and more homogeneous microstruc­ influencing factors, including Ti alloys, Ni-based superalloys, steels, and
ture with a distinctive solidification cellular structure. This type of high-entropy alloys. This paper also reviews some common materials
microstructure can suppress dislocation slip and deformation twinning that are sensitive to hydrogen but lack research on processing by AM,
during deformation, resulting in the reduction in the nucleation sites of including AISI 4340, and some promising AM metals which lack litera­
α’ martensite. Thus, compared with traditionally fabricated ASSs, the ture dedicated to the study of HE properties, including AlCoCrFeNi2.1
strain-induced α’ martensitic transformation in AM ASSs is suppressed, eutectic HEA and H13.
and the austenitic stability is enhanced [13,16,430]. As martensite is Currently, research on HE of AM metals has primarily identified the
more susceptible to hydrogen in comparison to other ferrous micro­ predominant HE mechanism to be the hydrogen-enhanced localised
structures, and materials undergoing martensitic transformation are plasticity (HELP) mechanism, though others also identified the syner­
notably sensitive to HE [225–227]. Therefore, the utilisation of AM to gistic action of HELP and HEDE. For titanium alloys, the predominant
suppress strain-induced martensitic transformation presents a feasible mechanism involved hydride formation and cleavage (HFC). At present,
approach for enhancing the HE resistance of austenitic steels, deserving there is no discernible distinction in HE mechanisms between materials
further research attention. In addition, extensive research conducted on manufactured through AM and those produced through traditional
typical martensitic steels has consistently demonstrated that materials methods. The most recent studies have found better HE resistance for
produced through AM exhibit substantially finer microstructure, such as AM metals, for example, DMT and SLM 304L SS [13,16] and SLM 17-
smaller martensitic laths and blocks, when compared to materials 4PH [55]. In contrast, some of the researchers have found the oppo­
manufactured using traditional methods [106,117,431]. It can be site, such as EBM Ti-6Al-4 V was more prone to hydrogen-induced
anticipated that this discrepancy in microstructure will also result in cracking at interphase boundaries [32], and DED 316L SS had
discernible differences in their resistance to HE. Nevertheless, the rele­ enhanced HE susceptibility [18]. In addition, the manufacturing
vant research in this topic remains relatively limited, underscoring the methods, including the direction of printing (horizontal or vertical)
need for further extensive investigations. [23,24,30], feeding mechanism (DED or PBF) [15,18], the type of heat
Moreover, materials produced with different AM methods also differ source (laser beam or electron beam) [34] and post-heat treatment
in their microstructures. For instance, EBM Ti-6Al-4 V has a lower conditions [16,23,25,27,57,257], can also significantly affect the HE
amount of discontinuous β-phase, absorbing less hydrogen than the behaviour of the AM alloys.
wrought alloy, while the SLM Ti-6Al-4 V demonstrated a higher trend of However, investigations on the HE susceptibility of numerous ma­
hydrogen absorption and hydride precipitation than the EBM counter­ terials processed by AM remain scarce, with few studies dedicated to
parts because of the α’-martensite microstructure [31,34]. Thus, sub­ understanding the HE characteristics of AM metals [13,32,54,59,286].
sequent research cannot be limited to comparing the HE performance of This review highlights the following research gaps that merit future

35
J. Yao et al. Current Opinion in Solid State & Materials Science 27 (2023) 101106

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interests or personal relationships that could have appeared to influence hydrogen embrittlement, Corros. Eng. Sci. Technol. 56 (6) (2021) 565–574.
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Data availability
18892–18910.
[26] S. Kevinsannya, O. Okazaki, Y. Takakuwa, Y. Ogawa, H. Funakoshi,
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Acknowledgment [27] J. Xu, Z. Hao, Z. Fu, X. He, H. Wang, G. Xu, Hydrogen embrittlement behavior of
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This work was financially supported by the ARC Discovery Project 359–369.
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for funding support (No. DP210103162). The authors are grateful to the Hydrogen embrittlement of Inconel 718 manufactured by laser powder bed fusion
ARC Discovery Project (No. DP210103162) for funding support. Jeffrey using sustainable feedstock: effect of heat treatment and microstructural
Venezuela acknowledges the support of the Advance Queensland In­ anisotropy, Metals 13 (2) (2023) 418.
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