Available online at www.sciencedirect.

com

ScienceDirect
Materials Today: Proceedings 5 (2018) 2891–2900 www.materialstoday.com/proceedings

ICAMA 2016

Low Temperature Embrittlement studies on Stainless Steel 304 LN

TIG Welds
G Dilip Maruthia, Purushotham Nb, Rashmi Ra*
a,
Department of Mechanical Engineering, BMSCE, Bangalore, India
b
B/E Engineering Services India Pvt. Ltd., Hyderabad, India

Abstract

Austenitic stainless steel 304LN (SS 304LN) is widely used in nuclear industry. TIG welding is selected here to weld the
stainless steel plates because it offers the possibility of producing high quality and porosity free welds. However, weld metal
experiences hot cracks during welding of austenitic stainless steels. Due to this, austenitic stainless steel welds are designed to
have 3-8% delta ferrite in the weld metal to avoid hot cracks during solidification. With the presence of delta ferrite, when these
materials are exposed to elevated temperature (300 - 5000C) the weld transforms into embrittlement phases such as iron rich α
and chromium rich α, G phase and M23C6. These embrittlement phases deteriorate the mechanical properties of the weld. In this
study, an attempt is made to study the low temperature embrittlement on SS 304LN TIG Welds. The low temperature
embrittlement behaviour on aged samples at (300, 350, 4000C) was evaluated for 10000 hours by mechanical property testing and
micro structural examination. Mechanical testing involves Hardness test and Impact test. Delta ferrite measurement was done to
see any transformation of delta ferrite. Fracture surfaces were characterized using SEM. Increase in hardness with increase in
aging temperature and decrease in delta ferrite content at 3500C and 400 0C clearly indicate that aging temperature affects
kinetics of transformation of delta ferrite. Scanning Electron Microscopy did not show any transformation of delta ferrite. It was
found that aging treatment has a strong influence on impact toughness. Decreases in impact toughness value especially at sub –
zero temperatures indicate kinetics of transformation of delta ferrite is affected by aging temperature during low temperature
aging.
© 2018 Elsevier Ltd. All rights reserved.
Selection and Peer-review under responsibility of International Conference on Advanced Materials and Applications (ICAMA
2016).

Keywords: Stainless steel 304 LN; Welding; TIG Welding; Embrittlement; Impact Test; Hardness Test;

*Rashmi R. Tel.: 9538847737

E-mail address: rashmir.mech@bmsce.ac.in

2214-7853 © 2018 Elsevier Ltd. All rights reserved.

Selection and Peer-review under responsibility of International Conference on Advanced Materials and Applications (ICAMA 2016).
2892 G Dilip Maruthi et.al / Materials Today: Proceedings 5 (2018) 2891–2900

1. Introduction

Stainless steels are essentially alloys of iron,chromium and carbon with Cr content exceeding 12% and carbon
content being small. The term “stainless” implies resistance to staining,rusting and pitting in air, moist and polluted
conditions. This stainless property of all stainless steels is attributed to the chromium addition. Chromium
contributes to a formation of a thin, passive surface film, probably oxide, which protects the steel against corrosive
attack. Thus, stainless steels posses excellent corrosion resistance along with other properties like high strength (at
low as well as high temperature), good workability and abrasion resistance which make them suitable for a variety
of applications.

The primary fabrication method for components made of stainless steel is fusion welding (TIG Welding). Austenitic
stainless steels are fully austenitic in their wrought condition. In welded condition austenitic stainless steel have
duplex microstructure consisting of an austenitic matrix with 3 to 8% delta ferrite. As welding studies have shown
the formation of primary ferrite during solidification reduces the vulnerability of these steels to hot cracking.
Therefore, the composition of weld filler metals and castings are adjusted to promote primary ferrite solidification.
During cooling, most of the primary ferrite transforms to austenite but small residual amount of ferrite is retained at
room temperature. The presence of residual ferrite has additional benefits: the strength is increased and the alloys
resistance to stress corrosion cracking is improved. With the presence of ferrite as a second phase in the welded
steel, the stability of these alloys during elevated temperature applications is of concern. Various studies said that
delta ferrite transforms in to various phases like carbides, sigma, chi and secondary phases etc. When temperature is
greater than about 5500C, these transformed products influence the mechanical and corrosion properties. In the case
of low temperature aging (<550°C) of weld, the five metallurgical process namely, spinodal decomposition,
precipitation of alpha prime, secondary austenite, G-phase and metal carbides are identified as responsible to aging
embrittlement of the ferrite phase.

2. Material Selection

2.1. Material

The 304LN austenitic stainless steel TIG welded rectangular specimens are used to study and the Composition of
304LN stainless steel material is given as follows in table.1, Fig 1 shows the dimensions of weld specimen.

Table 1. Chemical composition of 304LN Stainless steel

C Mn Si P S Cr Ni N

Base 0.024 1.73 0.55 0.022 0.001 18.8 9.25 0.15

Weld 0.048 1.84 0.56 0.021 0.01 18.5 12.4 ------

Fig. 1 Weld specimen

 G Dilip Maruthi et.al/Materials Today: Proceedings 5 (2018) 2891–2900 2893

3. Welding Procedure Specifications

• Welding process: GTAW (Gas tungsten Arc Welding)

• Joint design: V Groove
• Shielded gas: Argon (99.99%)
• Current: DC
• Polarity: straight for GTAW
• Volts: 10V-20V
• Tungsten electrode: Size: 2.5 mm Type: 2% throated

4. Aging Treatment

These furnaces used to set the aging temperatures 300,350 and 4000C. Prepared Specimens were kept in furnace as
shown in Fig.2. for 10000hrs aging time. Timer was connected to the furnace itself to measure time.

Fig. 2. Furnace with time controller

5. Results and Discussions

5.1. Hardness Test

Rockwell Hardness Machine with B scale with a 100 kg major load and a 1/16” inch steel ball indenter was used to
determine the hardness profile of both base as well as weld metals. Specimens aged at 300oC, 350oC and 400oC for
10000 hrs were used for hardness testing. The specimens were polished as per the standard metallographic specimen
preparation. Surface to be tested was made smooth and free from dust, oxides, and defects. Readings were taken
over length of 40 mm at three positions as shown in Fig.3. for 100 Kg load and 10 sec dwell time. Distance between
successive indentations was kept 2 mm. Readings were shown in table.2 and graphs were shown in fig.4, fig.5,
fig.6, fig.7 and fig.8.

Fig. 3. Weld specimen terminology

2894 G Dilip Maruthi et.al / Materials Today: Proceedings 5 (2018) 2891–2900

Table 2. Hardness values table for weld specimens. (12-300oC,10000 hrs; 22-350oC,10000 hrs; 32-400oC,10000 hrs)

Weld Rockwell Hardness Values (HRB)

12 22 32
Distance (mm) from the
Top Middle Bottom Top Middle Bottom Top Middle Bottom
centre of the weld
-20 80 86 82 78 78 84 79.5 79.5 81
-18 82 89 82 79 89 80 81.5 81 79
-16 81 90 88.5 84.5 86 83 79.5 81 84
-14 84 89 92.5 84 86 90 83 85 85
-12 90 89 86 85.5 90 89 84 87 84
-10 92.5 90 90.5 86 88.5 93 82 82.5 88
-8 93 90 95 90 91 91 89 88 86
-6 94.5 93.5 93 92 97 93 84 88 91
-4 89 92.5 92.5 87 94 90 88 89 89
-2 92 92 96 94 88 90 91 98 83
0 90.5 90.5 99 83 89 91 84.5 94.5 85
2 92 92 89 87.5 95 96 90 89 83
4 93 91.5 96 86.5 90 88 93 90 83
6 95 91 94 86 93 88 91.5 84 84
8 95.5 93.5 96 86.5 90 89 92 86 82
10 93.5 92.5 92.5 84 86 85 89.5 88 86.5
12 85.5 89 89 81 83 85 88.5 87 88
14 83.5 87.5 92 86 83 87 86 85.5 82
16 85 90 88 82 89 90 83.5 88.5 79
18 79.5 87.5 86 83 81 84 79 86 81
20 82 87 85 80 79 86 78.5 82.5 79

Distance from weld Distance from weld

Fig. 4 (a) Hardness profile for inner weld specimen aged at 3000C for 10000hrs (b) Hardness profile for inner weld specimen aged at 3500C for
10000hr
 G Dilip Maruthi et.al/Materials Today: Proceedings 5 (2018) 2891–2900 2895

Distance from weld

Fig. 5. Hardness profile for inner weld specimen aged at 4000C for 10000hrs

Fig. 6. Hardness profile for inner weld specimen top portion for all aging conditions for 10000 hrs

Fig. 7. Hardness profile for inner weld specimen middle portion for all aging conditions for 10000h
2896 G Dilip Maruthi et.al / Materials Today: Proceedings 5 (2018) 2891–2900

Fig. 8. Hardness profile for inner weld specimen bottom portion for all aging conditions for 10000hrs

5.2. Impact Test

The Charpy impact tests were carried out for weld specimens at three different testing temperatures -100C, 300C and
1500C. The results were tabulated and graphs were plotted. Impact toughness values of weld specimens aged at 300,
350 and 400oC for 10000 hrs are tabulated in table.3, table.4 and table.5 Fig.9, Fig.10, Fig.11 and Fig.12 shows the
effect of test temperature on impact toughness of specimens aged at 300, 350 and 400oC .

Table.3. Impact toughness of specimens aged at 300°C for 10000 hrs

Test Temperature Impact energy

Type of weld Remarks
(0C) (joules)
-10 Outer Weld 106 Specimen broken

30 Outer Weld 114 Specimen broken

150 Outer Weld 124 Specimen broken

Fig. 9. Effect of test temperature on Impact toughness of specimens aged at 300°C

 G Dilip Maruthi et.al/Materials Today: Proceedings 5 (2018) 2891–2900 2897

Table 4. Impact toughness of specimens aged at 350°C for 10000 hrs

Test Temperature Impact energy

Type of weld Remarks
(0C) (joules)
-10 Outer Weld 90 Specimen broke

30 Outer Weld 93 Specimen broke

150 Outer Weld 123 Specimen broke

Fig. 10. Effect of test temperature on Impact toughness of specimens aged at 350°C

Table.5. Impact toughness of specimens aged at 400 0 C for 10000 hrs.

Test Temperature Impact energy

Type of weld Remarks
(0C) (joules)

-10 Outer Weld 104 Specimen broke

30 Outer Weld 116 Specimen broke
Outer Weld
150 124 Specimen broke

Fig. 11. Effect of test temperature on Impact toughness of specimens aged at 400°C
2898 G Dilip Maruthi et.al / Materials Today: Proceedings 5 (2018) 2891–2900

Fig. 12. Effect of aging temperature on impact toughness of specimen at testing temperature -10°C

5.3. Scanning Electron Microscopy

A scanning electron microscope (SEM) was utilized to observe both higher resolution microstructure of a
sample as well as to identify the types of precipitates that were present.

Fig. 13. SEM photograph showing delta ferrite in austenitic matrix for Fig. 14. Impact specimen aged at 350°C for 10000hrs tested at
304LN stainless steel specimen aged at 400°C for 10000hrs 150°C showing fibrous structure with fine dimples

From the Fig .13 and Fig.14 shows SEM microstructure there is no relevance of transformation of delta ferrite. It
only shows vermicular delta ferrite in austenitic matrix.

5.3.1. Fractography

The fracture surface of the broken Charpy V-notch specimens were all examined using scanning electron
microscopy (SEM). There were observed differences between specimens broken at different testing temperatures -
10°C, 30°C and 150°C. few of the typical fractographs are presented in Fig.13 and Fig.14.

5.4.Delta Ferrite Measurement

The specimens were polished up to diamond finish and etched with marble’s reagent in order to identify the weld
region. The ferrite content of the aged specimens was measured using an Aminco-Bremer Magne-Gage with No.3
magnet which calibrated using NBS coating thickness standards according to the ANSI/AWS A4.2-74. The values
of FN (Ferrite Number) are measured and recorded in Table. 6.
 G Dilip Maruthi et.al/Materials Today: Proceedings 5 (2018) 2891–2900 2899

Table.6. Ferrite Number (FN) Values for 304LN Stainless Steel aged at 300°C, 350°C and 400°C for 10000 hrs

Ageing Trials Weld Parent metal

Temperature, 0C specimen

300 1. 4
2. 3.4
3. 4.6
4. 3.2
5. 3.8 Parent Metal has not registered any
Average 3.8 Ferrite Number value in any ageing
condition.
350 1. 3.4
2. 3.2
3. 2.8
4. 3.4
5. 3.4
Average 3.24
400 1. 1.4
2. 1.2
3. 1.4
4. 1.2
5. 1.2
Average 1.28

6. Conclusion

• The ferrite content of the welded specimens decreases on aging. The drop in ferrite content is more significant
at higher aging temperature.
• The maximum hardness values are observed in the weld metal compared to the base metal because of finer
structure, presence of ferrite and composition.
• As aging temperature increases the hardness values of the welded samples decreases due to increased kinetics
of phase transformation.
• Aging temperature has a strong influence on impact toughness. Aged samples show lower impact toughness
compared to the base metal.
• Fracture surfaces of most of the samples showed fibrous appearance with small percentage of cleavage in a few
cases.
• Fracture surface also indicated presence of spherical precipitates in the dimples which could be the
transformation products.
2900 G Dilip Maruthi et.al / Materials Today: Proceedings 5 (2018) 2891–2900

References

[1] A.A Tavassoli, A.Bisson and P.Soulat, “Ferrite Decomposition in Austenitic stainless steel weld metals” Metal science, 18, (1984) pp 345.
[2] Borland J C,Younger R N 1960 “Some aspects of cracking in welded Cr–Ni austenitic steels”. British.Welding journal, vol. 7: pp22–59.
[3] Bhadeshia H K D H, David SA,Vitek J M 1991 “Solidification sequences in stainless steel dissimilar alloy welds”. Mater. Sci. Technol. 7:
50–61.
[4] B. Raj, V. Shankar, A. K. Bhaduri, 2006, Welding Technology for Engineers, Alpha Science International Ltd. - Oxford, U.K.
[5] C. D. Lundin, D. F. Spond, 1976, “The nature of morphology of fissures in austenitic stainless steel weld metal”, Welding Journal 55(11), pp.
356s-367s.
[6] C. D. Lundin, C. P. D. Chou, 1985, “Fissuring in the “Hazard HAZ” region of austenitic stainless steel welds”, Welding Journal 64(4), pp.
113s-118s.
[7] D Peckner, I M Bernstein,Handbook of Stainless Steels,McGraw-Hill, 1977.
[8] DeLong, W.T. 1974, “Ferrite in Austenitic Stainless Steel Weld Metal”, Welding Journal 53(7): 276-s
[9] Espy, R.H. 1982, “Weldability of Nitrogen-Strengthened Stainless SteeIs”, Welding Journal 61(5), 149-s to 156-s
[10] F.C.Hull, welding journal, vol.46 (12) 1967, p.399s.
[11] F.B.Pickering,” Physical metallurgy and the design of steel” p.202. Gunia, R.B., and Ratz, G.A., “The Measurement of Delta—Ferrite in
Austenitic stainless Steels”, WRC Bulletin 132, New York, N.Y, August 1968, p. 5.
[12] H. B. Cary, S. C. Hezler, 2005, Modern Welding Technology 6th Edition, Pearson Prentice HallTM.
[13] Hull F C 1967 “The effect of δ-ferrite on the hot cracking of stainless steel”. Weld. J. 46: 399s–409s.
[14] H.D.Soloman and L.M.Levinson, Acta metal 26 (1978) 429.
[15] H.M.Chung And O.K.Chopra, “Kinetics And Mechanism Of Thermal Aging Embrittlement Of Duplex Stainless Steels,” Proceedings Of
Third International Symposium On Environmental Degradation Of Materials In Nuclear Power Systems- Water Reactors, August 30-
September 3,1987,Traverse City, MI.
[16] H.M.Chung And O.K.Chopra, “Long Term Embrittlement Of Cast Duplex Stainless Steels In LWR Systems In Material Science And
Technology Division Light-Water-Reactor” Safety Material Engg., Research Programs,Quarterly Progress Report Jan-March 1984,
NUREC/CR,1,ANL-84-60,1,52,Sept.(1984).
[17] ISIJ International, Vol. 42 (2002), No. 4, “Decomposition of Austenite in Austenitic Stainless Steels”, pp. 325–337.
[18] John C. Lippold and Damian J. Kotecki, 2005, Welding Metallurgy and Weldability of Stainless Steels, John Wiley & Sons Inc.
[19] J. A. Brooks, A. W. Thompson, J. C. Williams, 1984, “A fundamental study of the beneficial effects of delta ferrite I reducing weld
cracking”, Welding Journal 63(3), pp. 71s-83s
[20] J. C. Ma, Y. S. Yang, W. H. Tong, Y. Fang, Y. Yu, Z. Q. Hu, 2007, “Microstructural evolution in AISI 304 stainless steel during directional
solidification and subsequent solid-state transformation”, Material Science and Engineering A 444 pp. 64-68
[21] J, Honeycompe, T. G. Gooch, 1972, “Effect of manganese on cracking and corrosion resistance on fully austenitic stainless steel weld
metals”, Metal Construction and British Welding Journal 4(12):456
[22] J.A. Brooks, A.W.Thompson and J.C. Williams, welding journal, vol.63 (3), 1984, p.71s.
[23] J. Bnetly, M.K.Miller, S.S.Brenner and J.A.Spitzonogel, “Thermal aging of Primary coolant Pipe Steels in Proc. 43rd Annual Meeting of
the Electron Microscopy Society of America, G.W.Bailey,ed., San Franncisco Press (1985) 325.
[24] J.M.Viteck, S.A. David, D.J. Alexander, J.R.Keiser and R.K.Nanstad, Acta Mettalurgica, 39 (4) (1991) 503.
[25] J.K.Lai, materials science and engg. 58,(1983)195.
[26] J.W.Elmer and T.W.Eagar, proceedings of the 2nd international conference on trends in welding research, U.S.A., edited by S.A.David and
J.M.Vitek (1990).
[27] Kelly T F, Cohen M,Vandersande J B 1984 Rapid solidification of a droplet-processed stainless steel. Met. Trans. A15: 819–833.
[28] Koseki T, Matsumiya T,YamadaW, Ogawa T 1994 Numerical modeling of solidification and subsequent transformation of Fe–Cr–Ni alloys.
Metall. Mater. Trans. A25: 1309–1321.