Geometry Characterization of AISI 4
Geometry Characterization of AISI 4
67 (2022), 2, 645-652
DOI: https://doi.org/10.24425/amm.2022.137801
Laser-generated surface patterns provide the means for local mechanical interlocking between the joined materials, tunes
the wettability of surfaces that come in contact, and generally are the main factor for bonding strength enhancement, especially
between dissimilar materials. This paper presents the influence of different patterning overlays generated with a pulsed laser on
the surface of stainless-steel sheets. For all experiments, an overlapping degree of 90% has been chosen between three different
patterns, while the engraving speed, pulse frequency and number of passes have varied. The textured surfaces’ morphology was
assessed through optical microscopy, and the roughness of the surfaces was correlated with the corresponding experimental pa-
rameters. The results have indicated promising insights for joining stainless steel to plastic materials, which is otherwise difficult
to assess through usual welding techniques.
Keywords: microstructuring; laser; ferritic stainless steel; surface patterning
1. Introduction on the surface of material and at the same time to reduce the
possible defects, it is of upmost importance to consider the fol-
Direct laser surface texturing (DLST) is a method that al- lowing parameters: laser wavelength, intensity, energy per pulse,
lows the surface improvement of an engineered material in terms frequency of the laser pulses, the angle of incidence, number
of performance, for task-specific applications. It is a cutting-edge of cycles, polarization, repetition number and rate, scanning
technique, having the advantage of obtaining surface features speed, focal distance, pulse overlapping, number of overlapped
in micro and nano sizes, precise and reproducible textures, both scanning layers [20].
on hard and brittle components. It is possible to be implemented Czotscher et al. [21] investigated 0.2 mm Al sheets with
on different categories of materials, such as metallic (stainless an YLP-HP laser (1065 nm laser beam) considering pulse dura-
steel, titanium and its alloys, cobalt-chromium alloys, magne- tion 120 ns, power average 20…45 W, pulse energy 0.6…1 mJ,
sium alloys, aluminum and alloys, copper, etc.), plastic (PP, scanning speed 1m/s, repetition rate 20…60 KHz. The hole
PE, PEEK, PMMA, PLLA, etc.), ceramic (Al2O3, ZrO2, etc.) depth increases constantly after each pulse, also the hole diam-
and composite (glass fiber reinforced PP/aluminum, magne- eter. A positive influence for lower pulse overlaps and smaller
sium alloy/PET, AISI 304/PA6, C/SiC, SiC/SiC, etc). Usually, distances between the scanning lines were observed, that lead
the pattern can be regular or irregular, in the form of grooves, to a better mesh structure. Salstela et al. [22] studied the ad-
dimples, bumps or other models. DLST is applied on joining of hesion improvement of 5754-aluminum alloy substrate with
dissimilar materials [1,2], biomedical devices [3-9], tribological epoxy resin. On the aluminum substrate, three different types
improvements [10-12], heat exchangers [13], surfaces wetting of micro patterns were applied: microstructuring with micro-
[14], photovoltaics industry [15,16], semiconductors patterning meshes, hierarchical sandblasting + micro-mesh printing and
[17], painting [18]. hierarchical micro-mesh printing + sandblasting. The objective
The last five years have shown an increased research inter- was achieved by increasing the surface area with the number of
est in the DLST technique [19,20]. To obtain the desired texture locking points in substrate material; the hierarchical microstruc-
1
Transilvania University of Brasov, Brasov, Romania
2
BSH Electrodomésticos España S.A., Zaragoza, Spain
3
Universidad Politecnica de Madrid, Madrid, Spain
* Corresponding author: mtierean@unitbv.ro
© 2022. The Author(s). This is an open-access article distributed under the terms of the Creative Commons Attribution-NonCom-
mercial License (CC BY-NC 4.0, https://creativecommons.org/licenses/by-nc/4.0/deed.en which permits the use, redistribution of
the material in any medium or format, transforming and building upon the material, provided that the article is properly cited, the
BY NC use is noncommercial, and no modifications or adaptations are made.
646
turing providing the best solution. The condition is that mesh 2. Experiment
size should be large enough to allow filling with epoxy resin.
Rauh et al. [23] analyzed the effect of micro-conically structured 2.1. Material
aluminum surface obtained by femtosecond laser ablation with
60 fs laser pulses in nitrogen atmosphere, and 6 ns laser pulses The proposed material for microstructuring is the ferritic
in an iodine/air atmosphere, by means of Nd:YAG laser with stainless steel AISI 430 (ACX 500, EN 1.4016) provided by
wavelength λ = 1064 nm, a maximal pulse energy of E = 50 mJ Acerinox SA, Madrid, Spain (TABLE 1, TABLE 2). The material
and f = 20 Hz pulse repetition rate. The best results concerning is ductile and can be shaped using rolling, bending, and emboss-
surface texturing was obtained in the case of femtosecond laser ing. It has a quite good corrosion resistance to various saline or
microstructuring, but iodine atmosphere also yielded satisfactory acidic environments. As the base alloy of the ferritic group, this
results. Knapp et al. [24] investigated three type of polymers: grade 430 ferritic stainless steel is only readily available in sheet
PP, PE and PEEK samples 30×70×8 (mm) in order to improve and coil (up to 1.2 mm thick) most commonly in BA (bright
the adhesion with an Al-thin film. The laser source used in annealed) or 2B (moderately reflective) finishes. Samples were
microstructuring the substrate had a wavelength of λ = 355 nm, cut from a large sheet with 80 mm×25 mm×0.5 mm dimensions.
a repetition rate of 10 kHz, a pulse duration of 33 ± 10 ns
and a pulse energy of 10 W. The pattern type was 30×30 mm TABLE 1
square grid with 0°/90° straight lines spaced by 50 μm or 200 Chemical composition according to EN 10088-2 and ASTM A-240
μm. Experimental results showed that for PE and PEEK, laser
texturing largely increases the adhesion if laser parameters are Element
C Si Mn P S Cr N
(%)
well adjusted. For PP, roughening of the surface seems to be
Concen- 16.00-
more important. Mechanical adhesion mechanisms could also tration
≤0.08 ≤1.00 ≤1.00 ≤0.040 ≤0.015
18.00
≤0.045
be optimized, being better controlled with precise and focalized
laser ablation.
TABLE 2
The improvement of PP tensile adhesive strength was
Mechanical properties as per EN 10088-2 and ASTM A-240
studied by Matsuzaki et al. [25] through roll imprinting of
undercut micropatterns on PP plates samples (30×20×1.5 mm). Material Rp0.2 [MPa] Rm [MPa] ASO [%] HRB
The undercut angle was found to be 25o, and the tensile adhesive AISI 430 ˃260 450-600 ˃20 ˂185
strength was 1.7 times higher than that of the specimen without
surface modification. The aim of Cardoso et al. [14] was to
increase the hydrophobicity of polymeric poly(1-methoxy-4-(O- 2.2. Design of AISI 430 samples
disperse Red 1)-2,5-bis(2-methoxyethyl) benzene) surface film
through laser microstructuring with an Nd:YAG laser operating For this study three design patterns were used, presented
at 850 Hz repetition rate, 70…532 nm pulses, 17…65 nJ energy, in Fig. 1. The surface of microstructured area is 20×19.5 mm
and 1mm/s translation speed. Square-shaped-pillars morpholo- (design type A), 18×16 mm (design type B) and 19.5×17 mm
gies with distinct periodicities, from 5.0 μm to 500 μm were (design type C).
applied. A roughness increasing from Ra = 100 nm to Ra = 450
nm was observed, from non microstructured to microstructured
samples. These results permited the fabrication of surfaces with 2.3. Microstructuring of AISI 430 ferritic stainless steel
contact angle higher than 150o.
Hybrid joints between dissimilar materials, such as metals The microstructuring has been performed with an infrared
and non-metals (polymers, ceramics) [26] represent a widely Nd Fiber Diode-Pumped TruMark 5020 laser made by Trumpf.
customizable approach used in automotive industry [2,27], The equipment has an average power of 20 W, wavelength of
industrial manufacturing [28,29], as well as in biomedical [30], 1062 nm, pulse frequency from 5 to 1000 kHz, integrated with
packing [31], aerospace [32], and households [19] industries, a highly dynamic scanner module. The experiments have been
aiming lightweight structures that are optimized in terms of carried out using a standard design of experiments, in which
production costs and strength [32-34]. Microstructuring can be a parameter was kept constant, while the others were varied. The
used before joining dissimilar materials as pre-treatment in laser constant parameters were: the pulsed peak power of 3.8 kW at
processing to achieve a better mechanical interlocking [28,31] 20 kHz, number of impulses per point (1), defocus 0 mm, 100 µm
and to control the physical, chemical and mechanical properties diameter spot, and a focal distance of 254 mm. An angle align-
of hybrid joints [35]. ment of 3 degrees of the laser beam axis with the perpendicular
The goal of this research paper is to study of the influence to the sample surface was adopted, to prevent damaging the
of different patterning overlays prepared by DLST with differ- laser optical fiber due to specular reflection on the surface of the
ent processing parameters on the surface’s geometry, having as samples. Variable parameters are the frequency (30÷100 kHz),
potential application metal-to-polymer joining. speed (300÷1000 mm/s) and number of passes-repetition (1÷20).
Fig. 2 shows the variation of the pulse duration as a function
647
a)
a)
b) c)
Fig. 1. Sample types: (a) design A, hexagonal shape 2×2 mm (center to center), (b) design B, elliptical shape 2×2 mm (center to center), (c)
design C, circle diameter ϕ0.1 mmb) c)
of speed. Before applying the microstructuring process, the ness of the layer on the height was set for 1 µm in automatic
samples were cleaned with isopropanol for cleaning and de- processes). For measuring the roughness of the microstructured
greasing the samples. All the microstructured samples were surface a roughness tester ISR-100 was used, with a traverse
encoded depending on the speed, frequency and the number of speed of 5 mm/s, measuring force 4 mN, and accuracy ±10%.
repetitions. A minimum overlapping (Ov) ≥ 90% of the succes-
sive laser spots was considered for the beam integrity. From the
obtained samples, only representative ones have been chosen and 3. Results and discussion
discussed.
The microstructuring is performed due to the laser beam
local ablation of the material, generating grooves with a certain
depth and width, as a function of the operational parameters.
Also, a part of the ablated material can be deposited near the
groove as recast material dimples (Fig. 3). Amend et al. [29]
highlighted that the groove width (linear distance of the cavity,
measured between the redeposited material dimples) has a sig-
nificant influence on the surface properties of the material. Also,
Rodríguez-Vidal et al. point out that tensile-shear mechanical
performance is the changing factor as represented by geometry
and cavity aspect ratio [33].
The cross-section optical micrographs of sample A (speed
300 mm/s, frequency 30 kHz, pulse duration 170 ns) are pre-
Fig. 2. Pulse duration correlation with the scanning speed during mi- sented in Fig. 4. The 3D optical microscopy maps of sample
crostructuring
a) b)
a) b)
a) b)
c) d)
c) d)
c) d)
e) f)
Fig. 4. Cross section views of microstructurede)AISI 430 stainless steel, design type A, speed 300
f) [mm/s], frequency 30 [kHz] and number of
repetitions 2 (a), 5 (b), 7 (c), 10 (d), 13 (e), 17 e)
(f) f)
a) b)
Fig. 5. 3D images of microstructured AISI 430 stainless steel, design type A, speed 300 [mm/s], frequency 30 [kHz] and number of repeti-
tions 2 (a) and 17 (b)
649
the width of the groove tends to decrease. This tendency occurs
because in the case of increased repetition the expelled mate-
rial can no longer reach the surface of the workpiece as recast
material, and instead will be deposited on the walls of the hollow
narrowing the width of the groove. The deposited recast mate-
rial is influenced by the laser beam angle alignment, resulting
in one part of the recast material to be larger than the other side,
depending on the laser beam direction.
The difference is visible when it comes to the number of
repetitions in the case of laser passing and in the increasing of
speed. At low speed and a maximum number of repetitions,
it can be observed that groove material is mainly expulsed as
recast material, and the micro-grooves have the pulsed beam
Fig. 6. Variation of the microgrooves’ dimensions of microstructured laser shape. At lower number of repetitions, a small deformation
stainless steel AISI 430 for design type A of the stainless steel can be noted. In the case of type B design
a) b)
a) b)
c) d)
Fig. 7. Cross section views of microstructured AISI 430 stainless steel, design type B, frequencyd)
c) 30 [kHz], speed 300 [mm/s], number of repeti-
tions 10 (a); 20 (b); frequency 40 [kHz], speed 400 [mm/s], number of repetitions 20 (c); frequency 50 [kHz], speed 500 [mm/s], number of
repetitions 10 (d)
a) b)
Fig. 8. 3D images of microstructure frequency 30 [kHz], speed 300 [mm/s], number of repetitions 10 (a) and 20 (b)
650
(Fig. 7 and Fig. 8), the grooves are wider and shallower than Even if the same speed, frequency, and number of repeti-
for the other two designs. This is a consequence of the expelled tions were used for designs A, B and C, the geometry of applied
material that has been deposited inside the groove at a lower microstructure has an important role. From the cross-section
position than in design type A. optical micrographs (Figs. 4, 7 and 10) and profile histograms
In Fig. 9 the results indicate an increase in width with the (Figs. 6, 9 and 11), it can be observed that the material displace-
scanning speed increasing, while the recast material elevation ment is less pronounced for design type B, comparing with
and area of depth displaying a relatively constant tendency. designs type A and C. The same observation can be made in the
In the case of design type C (Fig. 10) the lack of elevation case of design type C in comparison with design type B and A
of the recast material can be noticed. Due to this fact, the eleva- (after 13 no. of repetition of microstructuring operation) regard-
tion’s height is missing from Fig. 11. With the increase in speed, ing the expulsed material.
depth, width and area decreasing has been remarked. The analyzed roughness parameters (Fig. 12) are Ra (the
arithmetic average, the absolute values of the profile within base
length), Rz (the height average, absolute values of heights of
the top five prominences and of the bottom, or peak-to-valley
heights) and Rt (total height of profile, from the lowest point to
the highest peak).
Comparing the roughness after microstructuring with the
roughness of the raw surface (Ra = 0.681 µm, Rz = 2.253 µm,
Rt = 8.828 µm), it can be seen that design A possibly generates
a better anchoring of the welded joints in terms of shear strength
in the directions of the sheet surface.
4. Conclusions
Fig. 9. Variation of the microgrooves’ dimensions of microstructured The pulsed laser offers a fast, easy and clean operation in
stainless steel AISI 430 for design type B metal microstructuring. Microstructuring is essential in different
a) b)
a) b)
c) d)
c) d)
Fig. 10. Cross section views of microstructured AISI 430 stainless steel, design type C: frequency 30 [kHz], speed 300 [mm/s], number of repeti-
tions 10 (a); 15 (b); frequency 50 [kHz], speed 500 [mm/s], and number of repetitions 15 (c); frequency 80 [kHz], speed 800 [mm/s], number
of repetitions 15 (d)
651
From the three studied micropatterning designs, hexagonal,
elliptical and circular, it has been observed that the hexagonal
pattern generates the highest surface roughness (also the highest
depth of the grooves), followed by the circular one, which could
prove beneficial for joining operations. On the other hand, shal-
lower and wider grooves (such as those obtained for the ellipti-
cal pattern) could provide a better crevice corrosion resistance
for coated assemblies. Further studies will be performed on the
characterization of the micropatterned materials surface proper-
ties and behavior in metal-plastic hybrid joints.
References
Fig. 11. Variation of the microgrooves’ dimensions of microstructured
stainless steel AISI 430 for design type C [1] K. Shimamoto, Y. Sekiguchi, C. Sato, Int. J. Adhes. Adhes. 67,
31-37 (2016).
[2] K. Vand der Straeten, I. Burkhardt, A. Olowinsky, A. Gillner,
application domains, ranging from biomaterials to hybrid joints Physcs. Proc. 83, 1137-1144 (2016).
between dissimilar materials, due to the formation and interlock- [3] R.A. Delgado-Ruız, J.L. Calvo-Guirado, P. Moreno, J. Guardia,
ing of grooves, which are cavities (in cross-section) ablated by G. Gomez-Moreno, J.E. Mate-Sanchez, P. Ramirez-Fernandez,
the laser, a part of the ablated material being redeposited on F. Chiva, J. Biomed. Mater. Res. B Appl. Biomater. 96 (1), 91-100
the groove edges as small dimples. The results presented in the (2011).
paper have indicated that the parameters of the laser micropat- [4] W. Liu, S. Liu, L. Wang, Coatings 9 (4), 249 (2019).
terning have a marked influence on the grove morphology, and [5] M. de la Cruz Lorenzo, M. Portillo, A. Albaladejo, Photon Lasers
consequently on the surface or joining properties of the materials. Med. 1 (3), 171-182 (2012).
a)
b) c)
Fig. 12. Roughness results on microstructured AISI 430 stainless steel: (a) design A, (b) design B, (c) design C
652
[6] G. Hu, K. Guan, L. Lu, J. Zhang, N. Lu, Y. Guan, Engineering 4 [19] E. Rodriguez-Vidal, C. Sanz, C. Soriano, J. Leunda, G. Verhaeghe,
(6), 822-830 (2018). J. Mater. Process. Tech. 229, 668-677 (2016).
[7] A. Carvalho, L. Grenho, M.H. Fernandes, A. Daskalova, A. Tri- [20] A. De Zanet, V. Casalegno, M. Salvo, Ceram. Int. 47, 7307-7320
fonov, I. Buchvarov, F.J. Monteiro, Ceram. Int. 46 (2), 1383-1389 (2021).
(2020). [21] T. Czotscher, F. Vollertsen, Physcs. Proc. 83, 53-61 (2016).
[8] R. Ortiz, I. Aurrekoetxea-Rodríguez, M. Rommel, I. Quintana, [22] J. Salstela, M. Suvanto, T.T. Pakkanen, Int. J. Adhes. Adhes. 66,
M. dM Vivanco, J.L. Toca-Herrera, Polymers 10 (12), 1337 (2018). 128-137 (2016).
[9] N. Sirdeshmukh, G. Dongre, Mater. Today-Proc. 44, 2348-2355 [23] S. Rauh, K. Wöbbeking, M. Li, W. Schade, E.G. Hübner, ChemP-
(2021). hysChem 21, 1644-1652 (2020).
[10] A.T.T. Nguyen, M. Brandt, A.C. Orifici, S. Feih, Int. J. Adhes. [24] W. Knapp, D. Djomani, J.F. Coulon, R. Grunchec, Physcs. Proc.
Adhes. 66, 81-92 (2016). 56, 791-800 (2014).
[11] E. Rodriguez-Vidal, C. Sanz, J. Lambarri, J. Renard, V. Gant [25] R. Matsuzaki, N. Tsukamoto, J. Taniguchi, Int. J. Adhes. Adhes.
chenko, Physcs. Proc. 83, 1110-1117 (2016). 68, 124-132 (2016).
[12] G. Dumitru, V. Romano, H.P. Weber, H. Haefke, Y. Gerbig, [26] E. Moldovan, M.H. Tierean, E.M. Stanciu, B. Transilvania Univ.
E. Pflüger, Appl. Phys. A 70, 485-487 (2000). 10 (1) 39-46 (2017).
[13] M. Adjim, R. Pillai, A. Bensaoula, D. Starikov, C. Boney, A. Sai- [27] J.P. Bergmann, M. Stambke, Physcs. Proc. 39, 84-91(2012).
dane, J. Heat Transfer. 129 (7), 798-804 (2007). [28] A. Cenigaonaindia, F. Liébana, A. Lamikiz, Z. Echegoyen, Physcs.
[14] M.R. Cardoso, V. Tribuzi, D.T. Balogh, L. Misoguti, C.R. Men- Proc. 39, 92-99 (2012).
donc, Appl. Surf. Sci. 257, 3281-3284 (2011). [29] P. Amend, S. Pfindel, M. Schmidt, Physcs. Proc. 41, 98-105 (2013).
[15] S. Itapu, D.G. Georgiev, V. Devabhaktuni, J. Electromagnet. Wave, [30] X. Wang, P. Li, Z. Xu, X. Song, H. Liu, J. Mater. Process. Tech.
29 (12), 1547-1556 (2015). 210, 1767-1771 (2010).
[16] J.E. Carey, PhD thesis, Femtosecond-laser Microstructuring of [31] A. Roesner, S. Scheik, A. Olowinsky, A. Gillner, U. Reisgen,
Silicon for Novel Optoelectronic Devices, Harvard University, M. Schleser, Physcs. Proc. 12, 370-377 (2011).
Cambridge, Massachusetts, USA (2004). [32] F.L. Palmieri, M.A. Belcher, C.J. Wohl, K.Y. Blohowiak, J.W. Con-
[17] C. Samoila, D. Ursutiu, A. Tavkhelidze, L. Jangidze, Z. Taliashvili, nell, Int. J. Adhes. Adhes. 68, 95-101 (2016).
G. Skhiladze, M. Tierean, Nanotechnology 31 (3), 035301 (2020). [33] E. Rodriguez-Vidal, J. Lambarri, C. Soriano, C. Sanz, G. Verhae-
[18] A. Guarnaccio, C. Belviso, P. Montano, F. Toschi, Sx. Orlando, ghe, Physcs. Proc. 56, 835-844 (2014).
G. Ciaccio, S. Ferreri, D. Trevisan, D. Mollica, G.P. Parisi, [34] K. Schricker, M. Stambke, J.P. Bergmann, K. Bräutigam, P. Henck-
P. Dolce, A. Bellucci, A. De Stefanis, D.M. Trucchi, V. Valentini, ell, Physcs. Proc. 56, 782-790 (2014).
A. Santagata, F. Cavalcante, A. Lettino, L. Medici, P.P. Ragone, [35] A.V. Brover, L.D. D’yachenko, Met. Sci. Heat Treat. 51 (5-6),
V.G. Lambertini, Surf. Coat. Tech. 406, 126727 (2021). 292-296 (2009).