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Hydrogen Embrittlement of AISI 316L steel produced by Selective Laser Melting

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Trabajo presentado en: Third European Conference on the Structural Integrity of Additively Manufactures Materials (ESIAM23)

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Hydrogen Embrittlement of AISI 316L steel produced by Selective Laser Melting

Author: Peral, Luis Borja,Díaz Portugal, Andrés,Ebrahimzadeh, P.,Fernández-Pariente, I.,Alegre Calderón, Jesús Manuel,Cuesta Segura, Isidoro Iván
Publisher: Elsevier
Year: 2024
DOI: 10.1016/j.prostr.2024.01.007
Source: https://riubu.ubu.es/bitstream/10259/8863/1/Peral-psi_2024.pdf
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Pee - e iew unde esponsibili y o he scien i ic commi ee o he ESIAM23 chai pe sons
10.1016/j.p os .2024.01.007
10.1016/j.p os .2024.01.007 2452-3216
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h ps://c ea i ecommons.o g/licenses/by-nc-nd/4.0
)
Pee - e iew unde esponsibili y o he scien i ic commi ee o he ESIAM23 chai pe sons
A ailable online a www.sciencedi ec .com
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2452-3216 © 2023 The Au ho s. Published by ELSEVIER B.V.
This is an open access a icle unde he CC BY-NC-ND license (h ps://c ea i ecommons.o g/licenses/by-nc-nd/4.0)
Pee - e iew unde esponsibili y o he scien i ic commi ee o he ESIAM23 chai pe sons
Thi d Eu opean Con e ence on he S uc u al In eg i y o Addi i ely Manu ac u es Ma e ials
(ESIAM23)
Hyd ogen Emb i lemen o AISI 316L s eel p oduced by Selec i e
Lase Mel ing
L.B. Pe ala*, A. Díazb, P. Eb ahimzadeha, I. Fe nández-Pa ien ea, J. Aleg eb, I.I. Cues ab
a Depa men o Ma e ial Science and Me allu gical Enginee ing. Uni e si y o O iedo, Gijón (As u ias), Spain
b Depa men o Cu il Enginee ing. Uni e si y o Bu gos, Bu gos (Cas illa y León), Spain
Abs ac
Selec i e lase mel ing (SLM) is one o he common me hods o addi i e manu ac u ing and i can be employed o
cus omize componen s wi h complex geome y expec ed o wo k in hyd ogen a mosphe es. Howe e , mo e s udies
a e s ill needed o cha ac e ize he beha io o p in ed mechanical componen s in ended o wo k in con ac wi h
hyd ogen. In his s udy, smoo h and no ched ensile samples we e p echa ged in an acid solu ion wi h 8 mA/cm2 o
24h ime. Hyd ogen damage was mo e ma ked in he no ched samples, especially a 0.005 mm/min, whe e ac u e
mic omechanism changed om duc ile in he absence o hyd ogen o quasi-b i le in he p esence o in e nal hyd ogen.
The ole o he s ain-induced ma ensi e is also highligh ed.
© 2023 The Au ho s. Published by ELSEVIER B.V.
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Pee - e iew unde esponsibili y o he scien i ic commi ee o he ESIAM23 chai pe sons
Keywo ds: 316L, SLM, ensile, hyd ogen emb i lemen , s ain-induced ma ensi e
1. In oduc ion
Nowadays, he e is a con inued in e es in de eloping alloys able o wo k in hyd ogen applica ions a high p essu e
hyd ogen gas. In his ega d, aus eni ic s ainless s eels such as 316 o 316L a e good candida es because o hei low
hyd ogen di usi i y and high duc ili y [1–3]. In he con ex o hyd ogen echnologies, he p oduc ion o connec o
* Co esponding au ho :
E-mail add ess: [email p o ec ed]
A ailable online a www.sciencedi ec .com
ScienceDi ec
S uc u al In eg i y P ocedia 00 (2022) 000–000
w
ww.else ie .com/loca e/p ocedia
2452-3216 © 2023 The Au ho s. Published by ELSEVIER B.V.
This is an open access a icle unde he CC BY-NC-ND license (h ps://c ea i ecommons.o g/licenses/by-nc-nd/4.0)
Pee - e iew unde esponsibili y o he scien i ic commi ee o he ESIAM23 chai pe sons
Thi d Eu opean Con e ence on he S uc u al In eg i y o Addi i ely Manu ac u es Ma e ials
(ESIAM23)
Hyd ogen Emb i lemen o AISI 316L s eel p oduced by Selec i e
Lase Mel ing
L.B. Pe ala*, A. Díazb, P. Eb ahimzadeha, I. Fe nández-Pa ien ea, J. Aleg eb, I.I. Cues ab
a Depa men o Ma e ial Science and Me allu gical Enginee ing. Uni e si y o O iedo, Gijón (As u ias), Spain
b Depa men o Cu il Enginee ing. Uni e si y o Bu gos, Bu gos (Cas illa y León), Spain
Abs ac
Selec i e lase mel ing (SLM) is one o he common me hods o addi i e manu ac u ing and i can be employed o
cus omize componen s wi h complex geome y expec ed o wo k in hyd ogen a mosphe es. Howe e , mo e s udies
a e s ill needed o cha ac e ize he beha io o p in ed mechanical componen s in ended o wo k in con ac wi h
hyd ogen. In his s udy, smoo h and no ched ensile samples we e p echa ged in an acid solu ion wi h 8 mA/cm2 o
24h ime. Hyd ogen damage was mo e ma ked in he no ched samples, especially a 0.005 mm/min, whe e ac u e
mic omechanism changed om duc ile in he absence o hyd ogen o quasi-b i le in he p esence o in e nal hyd ogen.
The ole o he s ain-induced ma ensi e is also highligh ed.
© 2023 The Au ho s. Published by ELSEVIER B.V.
This is an open access a icle unde he CC BY-NC-ND license (h ps://c ea i ecommons.o g/licenses/by-nc-nd/4.0)
Pee - e iew unde esponsibili y o he scien i ic commi ee o he ESIAM23 chai pe sons
Keywo ds: 316L, SLM, ensile, hyd ogen emb i lemen , s ain-induced ma ensi e
1. In oduc ion
Nowadays, he e is a con inued in e es in de eloping alloys able o wo k in hyd ogen applica ions a high p essu e
hyd ogen gas. In his ega d, aus eni ic s ainless s eels such as 316 o 316L a e good candida es because o hei low
hyd ogen di usi i y and high duc ili y [1–3]. In he con ex o hyd ogen echnologies, he p oduc ion o connec o
* Co esponding au ho :
E-mail add ess: [email p o ec ed]
2 L.B. Pe al / S uc u al In eg i y P ocedia 00 (2019) 000–000
and elbows equi es speci ic geome ies ha can be op imized h ough addi i e manu ac u ing. I has been epo ed
ha addi i ely manu ac u ed 316L boas s supe io mechanical p ope ies han hose o con en ional s a e [1].
Howe e , g ea e abso p ion o hyd ogen can be induced in he SLMed 316L [2] because o i s highe densi y o
disloca ions, induced due o he apid cooling a es du ing solidi ica ion. In addi ion, he in luence o SLM de ec s
and su ace inishing in hyd ogen di usion mus be be e unde s ood [2,3]. Acco dingly, new p oduc ion echniques,
especially addi i e manu ac u ing, equi e e-e alua ion o hyd ogen suscep ibili y o aus eni ic s ainless s eels. In
his wo k, smoo h and no ched ensile samples ha e been elec ochemically p echa ged. Tensile beha io , wi h
in e nal hyd ogen, was s udied a di e en s ain a es and hyd ogen emb i lemen is discussed in e ms o he
ope a i e ac u e mic omechanisms.
2. Expe imen al p ocedu e
2.1 Ma e ial and p ocessing
AISI 316L was addi i ely manu ac u ed wi h an ALBA 300 machine, ollowing pa ame e s gi en in Table 1. The
chemical composi ion o he p in ed ma e ial is shown in Table 2. Ho ex ac ion samples o de e mine hyd ogen
concen a ion and ensile samples we e p in ed simul aneously on he same pla o m o he ALBA 300 machine.
Table 1. P in ing pa ame e s in ALBA 300 machine
Lase
powe (W) Scanning speed (mm/s) Ha ching dis ance (mm)
225 650 0.1
Table 2. Chemical composi ion in weigh pe cen (w . %)
Fe C C
Ni Mo
b
alance 0.02 18 12 2
2.2 Hyd ogen p echa ging and ho ex ac ion
Hyd ogen was in oduced in samples wi h a geome y o 10 mm x 10 mm x 1 mm. A cu en densi y o 8 mA/cm2
was applied o 24 hou s a oom empe a u e (RT) in 1M H2SO4 solu ion, added wi h 0.25 g/l As2O3 (pHൎ1).
Hyd ogen abso p ion was analyzed by means o he ho ex ac ion echnique. Samples we e hea ed a 1100ºC o 300
s in a LECO DH603 hyd ogen analyse .
Figu e 1. Hyd ogen p echa ging in ensile samples. Expe imen al se up
2.3 Tensile es s and ac u e su aces.
Tensile es s we e ca ied ou in a MTS Se ies 40 machine. In o de o s udy he in luence o hyd ogen a di e en
s ain a es, ensile es s we e done om 0.1 o 0.005 mm/min. Smoo h and no ched samples we e used wi h he ensile
di ec ion pa allel o he p in ing di ec ion o he addi i ely manu ac u ed 316L samples. The wid h and hickness o
ensile samples we e 5 and 1 mm, espec i ely. The gauge leng h o samples was 20 mm. In he case o he no ched
L.B. Pe al e al. / P ocedia S uc u al In eg i y 53 (2024) 52–57 53
A ailable online a www.sciencedi ec .com
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S uc u al In eg i y P ocedia 00 (2022) 000–000
w
ww.else ie .com/loca e/p ocedia
2452-3216 © 2023 The Au ho s. Published by ELSEVIER B.V.
This is an open access a icle unde he CC BY-NC-ND license (h ps://c ea i ecommons.o g/licenses/by-nc-nd/4.0)
Pee - e iew unde esponsibili y o he scien i ic commi ee o he ESIAM23 chai pe sons
Thi d Eu opean Con e ence on he S uc u al In eg i y o Addi i ely Manu ac u es Ma e ials
(ESIAM23)
Hyd ogen Emb i lemen o AISI 316L s eel p oduced by Selec i e
Lase Mel ing
L.B. Pe ala*, A. Díazb, P. Eb ahimzadeha, I. Fe nández-Pa ien ea, J. Aleg eb, I.I. Cues ab
a Depa men o Ma e ial Science and Me allu gical Enginee ing. Uni e si y o O iedo, Gijón (As u ias), Spain
b Depa men o Cu il Enginee ing. Uni e si y o Bu gos, Bu gos (Cas illa y León), Spain
Abs ac
Selec i e lase mel ing (SLM) is one o he common me hods o addi i e manu ac u ing and i can be employed o
cus omize componen s wi h complex geome y expec ed o wo k in hyd ogen a mosphe es. Howe e , mo e s udies
a e s ill needed o cha ac e ize he beha io o p in ed mechanical componen s in ended o wo k in con ac wi h
hyd ogen. In his s udy, smoo h and no ched ensile samples we e p echa ged in an acid solu ion wi h 8 mA/cm2 o
24h ime. Hyd ogen damage was mo e ma ked in he no ched samples, especially a 0.005 mm/min, whe e ac u e
mic omechanism changed om duc ile in he absence o hyd ogen o quasi-b i le in he p esence o in e nal hyd ogen.
The ole o he s ain-induced ma ensi e is also highligh ed.
© 2023 The Au ho s. Published by ELSEVIER B.V.
This is an open access a icle unde he CC BY-NC-ND license (h ps://c ea i ecommons.o g/licenses/by-nc-nd/4.0)
Pee - e iew unde esponsibili y o he scien i ic commi ee o he ESIAM23 chai pe sons
Keywo ds: 316L, SLM, ensile, hyd ogen emb i lemen , s ain-induced ma ensi e
1. In oduc ion
Nowadays, he e is a con inued in e es in de eloping alloys able o wo k in hyd ogen applica ions a high p essu e
hyd ogen gas. In his ega d, aus eni ic s ainless s eels such as 316 o 316L a e good candida es because o hei low
hyd ogen di usi i y and high duc ili y [1–3]. In he con ex o hyd ogen echnologies, he p oduc ion o connec o
* Co esponding au ho :
E-mail add ess: [email p o ec ed]
A ailable online a www.sciencedi ec .com
ScienceDi ec
S uc u al In eg i y P ocedia 00 (2022) 000–000
w
ww.else ie .com/loca e/p ocedia
2452-3216 © 2023 The Au ho s. Published by ELSEVIER B.V.
This is an open access a icle unde he CC BY-NC-ND license (h ps://c ea i ecommons.o g/licenses/by-nc-nd/4.0)
Pee - e iew unde esponsibili y o he scien i ic commi ee o he ESIAM23 chai pe sons
Thi d Eu opean Con e ence on he S uc u al In eg i y o Addi i ely Manu ac u es Ma e ials
(ESIAM23)
Hyd ogen Emb i lemen o AISI 316L s eel p oduced by Selec i e
Lase Mel ing
L.B. Pe ala*, A. Díazb, P. Eb ahimzadeha, I. Fe nández-Pa ien ea, J. Aleg eb, I.I. Cues ab
a Depa men o Ma e ial Science and Me allu gical Enginee ing. Uni e si y o O iedo, Gijón (As u ias), Spain
b Depa men o Cu il Enginee ing. Uni e si y o Bu gos, Bu gos (Cas illa y León), Spain
Abs ac
Selec i e lase mel ing (SLM) is one o he common me hods o addi i e manu ac u ing and i can be employed o
cus omize componen s wi h complex geome y expec ed o wo k in hyd ogen a mosphe es. Howe e , mo e s udies
a e s ill needed o cha ac e ize he beha io o p in ed mechanical componen s in ended o wo k in con ac wi h
hyd ogen. In his s udy, smoo h and no ched ensile samples we e p echa ged in an acid solu ion wi h 8 mA/cm2 o
24h ime. Hyd ogen damage was mo e ma ked in he no ched samples, especially a 0.005 mm/min, whe e ac u e
mic omechanism changed om duc ile in he absence o hyd ogen o quasi-b i le in he p esence o in e nal hyd ogen.
The ole o he s ain-induced ma ensi e is also highligh ed.
© 2023 The Au ho s. Published by ELSEVIER B.V.
This is an open access a icle unde he CC BY-NC-ND license (h ps://c ea i ecommons.o g/licenses/by-nc-nd/4.0)
Pee - e iew unde esponsibili y o he scien i ic commi ee o he ESIAM23 chai pe sons
Keywo ds: 316L, SLM, ensile, hyd ogen emb i lemen , s ain-induced ma ensi e
1. In oduc ion
Nowadays, he e is a con inued in e es in de eloping alloys able o wo k in hyd ogen applica ions a high p essu e
hyd ogen gas. In his ega d, aus eni ic s ainless s eels such as 316 o 316L a e good candida es because o hei low
hyd ogen di usi i y and high duc ili y [1–3]. In he con ex o hyd ogen echnologies, he p oduc ion o connec o
* Co esponding au ho :
E-mail add ess: [email p o ec ed]
2 L.B. Pe al / S uc u al In eg i y P ocedia 00 (2019) 000–000
and elbows equi es speci ic geome ies ha can be op imized h ough addi i e manu ac u ing. I has been epo ed
ha addi i ely manu ac u ed 316L boas s supe io mechanical p ope ies han hose o con en ional s a e [1].
Howe e , g ea e abso p ion o hyd ogen can be induced in he SLMed 316L [2] because o i s highe densi y o
disloca ions, induced due o he apid cooling a es du ing solidi ica ion. In addi ion, he in luence o SLM de ec s
and su ace inishing in hyd ogen di usion mus be be e unde s ood [2,3]. Acco dingly, new p oduc ion echniques,
especially addi i e manu ac u ing, equi e e-e alua ion o hyd ogen suscep ibili y o aus eni ic s ainless s eels. In
his wo k, smoo h and no ched ensile samples ha e been elec ochemically p echa ged. Tensile beha io , wi h
in e nal hyd ogen, was s udied a di e en s ain a es and hyd ogen emb i lemen is discussed in e ms o he
ope a i e ac u e mic omechanisms.
2. Expe imen al p ocedu e
2.1 Ma e ial and p ocessing
AISI 316L was addi i ely manu ac u ed wi h an ALBA 300 machine, ollowing pa ame e s gi en in Table 1. The
chemical composi ion o he p in ed ma e ial is shown in Table 2. Ho ex ac ion samples o de e mine hyd ogen
concen a ion and ensile samples we e p in ed simul aneously on he same pla o m o he ALBA 300 machine.
Table 1. P in ing pa ame e s in ALBA 300 machine
Lase
powe (W) Scanning speed (mm/s) Ha ching dis ance (mm)
225 650 0.1
Table 2. Chemical composi ion in weigh pe cen (w . %)
Fe C C
Ni Mo
b
alance 0.02 18 12 2
2.2 Hyd ogen p echa ging and ho ex ac ion
Hyd ogen was in oduced in samples wi h a geome y o 10 mm x 10 mm x 1 mm. A cu en densi y o 8 mA/cm2
was applied o 24 hou s a oom empe a u e (RT) in 1M H2SO4 solu ion, added wi h 0.25 g/l As2O3 (pHൎ1).
Hyd ogen abso p ion was analyzed by means o he ho ex ac ion echnique. Samples we e hea ed a 1100ºC o 300
s in a LECO DH603 hyd ogen analyse .
Figu e 1. Hyd ogen p echa ging in ensile samples. Expe imen al se up
2.3 Tensile es s and ac u e su aces.
Tensile es s we e ca ied ou in a MTS Se ies 40 machine. In o de o s udy he in luence o hyd ogen a di e en
s ain a es, ensile es s we e done om 0.1 o 0.005 mm/min. Smoo h and no ched samples we e used wi h he ensile
di ec ion pa allel o he p in ing di ec ion o he addi i ely manu ac u ed 316L samples. The wid h and hickness o
ensile samples we e 5 and 1 mm, espec i ely. The gauge leng h o samples was 20 mm. In he case o he no ched
54 L.B. Pe al e al. / P ocedia S uc u al In eg i y 53 (2024) 52–57
L.B. Pe al / S uc u al In eg i y P ocedia 00 (2019) 000–000 3
samples, he geome y o he no ch can be seen in Figu e 5. Smoo h and no ched samples we e elec ochemically
p echa ged, ollowing condi ions p e iously desc ibed. The expe imen al se up is illus a ed in Figu e 1. A e
hyd ogen p echa ging, ensile samples we e es ed in ai a RT. F ac u e su aces we e examined in a scanning elec on
mic oscope JEOL JSM-6460LV, using an accele a ion ol age o 10 kV.
3. Resul s
3.1 Mic os uc u e and hyd ogen up ake
Addi i ely manu ac u ed 316L mic os uc u e is showed in Figu e 2(a). Mic os uc u e shows a laye ed s uc u e
s acked wi h a c shaped mel pools. Columna aus eni e g ains, o ming epi axially along he building di ec ion, can
be obse ed. The cellula s uc u e is also obse ed in he g ains because o he apid cooling [3]. A e he 3D p in ing
p ocess, he XRD analysis e ealed he e a e only di ac ion peaks co esponding o he aus eni e phase, Figu e 2(b).
On he o he hand, om ho ex ac ion es s, hyd ogen concen a ion was de e mined o be �37 w ppm. Howe e ,
due o he low hyd ogen di usi i y o aus eni ic s eels, addi i ely manu ac u ed samples a e no sa u a ed a e 24h,
and his concen a ion is only eached a he subsu ace le el.
(a) (b)
Figu e 2. (a)
M
ic os uc u e o
A
ISI 316L (e ched wi h Kalling’s No. 2 o 125s) a e 3D p in ing. (b) XRD analysis, a e 3D
p in ing, conduc ed wi h a Sei e XRD 3000 TT di ac ome e
Table 3. Tensile p ope ies on smoo h samples. CHS: c oss-
head speed
CHS
(mm/min)
σ
ys
(MPa)
σ
u s
(MPa)
𝜀𝜀
(%)
RA
(%)
Uncha ged 0.1 477 546 39 30
H p echa ged 0.1 490 553 36 28
H p echa ged 0.01 496 557 35 27
Figu e 3. Tensile cu es on smoo h samples
2The a (º)
15 20 25 30 35 40
Coun s
0
1000
2000
3000
4000
5000
6000
316L SLM (As-buil )
{111}
{200}
{220}
building
4 L.B. Pe al / S uc u al In eg i y P ocedia 00 (2019) 000–000
3.2 Tensile es on smoo h samples
Tensile esul s on smoo h samples a e shown in Figu e 3, while ensile p ope ies a e gi en in Table 3. F ac u e
su aces a e compa ed in Figu e 4, o he uncha ged and hyd ogen p echa ged condi ion (0.01 mm/min).
Hyd ogen emb i lemen suscep ibili y was e alua ed by compa ing slow s ain a e ensile cu es o uncha ged and
hyd ogen p echa ged samples. In he p esence o in e nal hyd ogen (ൎ37 w ppm), yield s eng h and ul ima e ensile
s eng h inc eased. This ac migh be associa ed o hyd ogen disloca ion pinning mechanism in aus eni ic s ainless
s eels [4]. Besides, a dec ease o duc ili y was also obse ed in he p esence o in e nal hyd ogen. Dimples indica ing
duc ile ac u e we e obse ed in he uncha ged condi ion, Figu e 4(a). Howe e , a e hyd ogen p echa ging and
especially a 0.01 mm/min, s e ched and shallow dimples we e obse ed nea he su ace egion, Figu e 4(b). The
s e ched and shallow dimples in a H-cha ged 316L s eel ha e also been expe imen ally ound by p e ious au ho s
[5]. S e ched and shallow oids a e a ibu ed o hyd ogen accele a ed nuclea ion o oids ha igge s local shea ing
be ween oids. This mechanisms has also been nume ically cap u ed [6]. Based on he low di usi i y o hyd ogen in
aus eni ic s ainless s eels, i is expec ed ha high hyd ogen concen a ion (ൎ37 w ppm) was in oduced a he
subsu ace le el wha sligh ly modi ied he ac u e mic omechanism in he p esence o in e nal hyd ogen, as can be
seen in Figu e 4.
(a) (b)
Figu e 4. F ac u e su aces. (a) Uncha ged. (b) Hyd ogen p echa ged and es ed a 0.01 mm/min, wi h s e ched and shallow
dimples p oduced by local shea s ain
3.4 Tensile es on no ched samples
Hyd ogen in luence on ensile beha io was also s udied on no ched samples. Tensile esul s co esponding o he
uncha ged and hyd ogen p echa ged condi ion a e displayed in Figu e 5. The ob ained mechanical p ope ies and he
emb i lemen indexes a e summa ized in Table 4 and Table 5, espec i ely. On he o he hand, ac u e su aces a e
shown in Figu e 6. F ac u e su aces obse a ions we e done nea he no ched egion. In he uncha ged sample,
dimples we e obse ed, Figu e 6(a). Ne e heless, ac u e mic omechanism was modi ied in he p esence o
hyd ogen. In sample es ed wi h hyd ogen a 0.005 mm/min, seconda y c acks and quasi-clea ages we e no ed, Figu e
6(b). This ac con ibu es o jus i y he loss o s eng h and duc ili y (Table 4 and Table 5) o ensile es s conduc ed
especially a 0.005 mm/min a e hyd ogen p echa ging (8 mA/cm2 o 24h). Addi ionally, a e ensile es s, XRD
1 mm
L.B. Pe al e al. / P ocedia S uc u al In eg i y 53 (2024) 52–57 55
L.B. Pe al / S uc u al In eg i y P ocedia 00 (2019) 000–000 3
samples, he geome y o he no ch can be seen in Figu e 5. Smoo h and no ched samples we e elec ochemically
p echa ged, ollowing condi ions p e iously desc ibed. The expe imen al se up is illus a ed in Figu e 1. A e
hyd ogen p echa ging, ensile samples we e es ed in ai a RT. F ac u e su aces we e examined in a scanning elec on
mic oscope JEOL JSM-6460LV, using an accele a ion ol age o 10 kV.
3. Resul s
3.1 Mic os uc u e and hyd ogen up ake
Addi i ely manu ac u ed 316L mic os uc u e is showed in Figu e 2(a). Mic os uc u e shows a laye ed s uc u e
s acked wi h a c shaped mel pools. Columna aus eni e g ains, o ming epi axially along he building di ec ion, can
be obse ed. The cellula s uc u e is also obse ed in he g ains because o he apid cooling [3]. A e he 3D p in ing
p ocess, he XRD analysis e ealed he e a e only di ac ion peaks co esponding o he aus eni e phase, Figu e 2(b).
On he o he hand, om ho ex ac ion es s, hyd ogen concen a ion was de e mined o be �37 w ppm. Howe e ,
due o he low hyd ogen di usi i y o aus eni ic s eels, addi i ely manu ac u ed samples a e no sa u a ed a e 24h,
and his concen a ion is only eached a he subsu ace le el.
(a) (b)
Figu e 2. (a)
M
ic os uc u e o
A
ISI 316L (e ched wi h Kalling’s No. 2 o 125s) a e 3D p in ing. (b) XRD analysis, a e 3D
p in ing, conduc ed wi h a Sei e XRD 3000 TT di ac ome e
Table 3. Tensile p ope ies on smoo h samples. CHS: c oss-
head speed
CHS
(mm/min)
σ
ys
(MPa)
σ
u s
(MPa)
𝜀𝜀
(%)
RA
(%)
Uncha ged 0.1 477 546 39 30
H p echa ged 0.1 490 553 36 28
H p echa ged 0.01 496 557 35 27
Figu e 3. Tensile cu es on smoo h samples
2The a (º)
15 20 25 30 35 40
Coun s
0
1000
2000
3000
4000
5000
6000
316L SLM (As-buil )
{111}
{200}
{220}
building
4 L.B. Pe al / S uc u al In eg i y P ocedia 00 (2019) 000–000
3.2 Tensile es on smoo h samples
Tensile esul s on smoo h samples a e shown in Figu e 3, while ensile p ope ies a e gi en in Table 3. F ac u e
su aces a e compa ed in Figu e 4, o he uncha ged and hyd ogen p echa ged condi ion (0.01 mm/min).
Hyd ogen emb i lemen suscep ibili y was e alua ed by compa ing slow s ain a e ensile cu es o uncha ged and
hyd ogen p echa ged samples. In he p esence o in e nal hyd ogen (ൎ37 w ppm), yield s eng h and ul ima e ensile
s eng h inc eased. This ac migh be associa ed o hyd ogen disloca ion pinning mechanism in aus eni ic s ainless
s eels [4]. Besides, a dec ease o duc ili y was also obse ed in he p esence o in e nal hyd ogen. Dimples indica ing
duc ile ac u e we e obse ed in he uncha ged condi ion, Figu e 4(a). Howe e , a e hyd ogen p echa ging and
especially a 0.01 mm/min, s e ched and shallow dimples we e obse ed nea he su ace egion, Figu e 4(b). The
s e ched and shallow dimples in a H-cha ged 316L s eel ha e also been expe imen ally ound by p e ious au ho s
[5]. S e ched and shallow oids a e a ibu ed o hyd ogen accele a ed nuclea ion o oids ha igge s local shea ing
be ween oids. This mechanisms has also been nume ically cap u ed [6]. Based on he low di usi i y o hyd ogen in
aus eni ic s ainless s eels, i is expec ed ha high hyd ogen concen a ion (ൎ37 w ppm) was in oduced a he
subsu ace le el wha sligh ly modi ied he ac u e mic omechanism in he p esence o in e nal hyd ogen, as can be
seen in Figu e 4.
(a) (b)
Figu e 4. F ac u e su aces. (a) Uncha ged. (b) Hyd ogen p echa ged and es ed a 0.01 mm/min, wi h s e ched and shallow
dimples p oduced by local shea s ain
3.4 Tensile es on no ched samples
Hyd ogen in luence on ensile beha io was also s udied on no ched samples. Tensile esul s co esponding o he
uncha ged and hyd ogen p echa ged condi ion a e displayed in Figu e 5. The ob ained mechanical p ope ies and he
emb i lemen indexes a e summa ized in Table 4 and Table 5, espec i ely. On he o he hand, ac u e su aces a e
shown in Figu e 6. F ac u e su aces obse a ions we e done nea he no ched egion. In he uncha ged sample,
dimples we e obse ed, Figu e 6(a). Ne e heless, ac u e mic omechanism was modi ied in he p esence o
hyd ogen. In sample es ed wi h hyd ogen a 0.005 mm/min, seconda y c acks and quasi-clea ages we e no ed, Figu e
6(b). This ac con ibu es o jus i y he loss o s eng h and duc ili y (Table 4 and Table 5) o ensile es s conduc ed
especially a 0.005 mm/min a e hyd ogen p echa ging (8 mA/cm2 o 24h). Addi ionally, a e ensile es s, XRD
1 mm
56 L.B. Pe al e al. / P ocedia S uc u al In eg i y 53 (2024) 52–57
L.B. Pe al / S uc u al In eg i y P ocedia 00 (2019) 000–000 5
analysis was pe o med on he ac u e su aces. XRD analysis e ealed he p esence o s ain-induced ma ensi e nea
he no ched egion (Table 6). I is impo an o highligh , his phase ans o ma ion was no p e iously ound a e he
3D p in ing p ocess (Figu e 2b).
Table 4. Tensile p ope ies on no ched samples. NTS: no ch
ensile s eng h and RA: educ ion o a ea
CHS
(mm/min)
Tes du a ion
(min)
σ
NTS
(MPa)
RA
(%)
Uncha ged 0.1 24 645�8 7.1
H p echa ged 0.01 180 619�4 5.8
H p echa ged 0.005 360 601�1 4.9
Table 5. Emb i lemen indexes on no ched samples
CHS
(mm/min)
EI σ
NTS
(%)
EI RA
(%)
Uncha ged 0.1 - -
H p echa ged 0.01 4 18
H p echa ged 0.005 7 31
Figu e 5. Tensile cu es on no ched samples
Table 6. S ain-induced ma ensi e in {211} wi h 2
θ
=156.4° and {200} wi h 2
θ
=106.1°. XRD esul s nea he no ched egion a e
he ensile es s
CHS (mm/min) S ain-induced ma ensi e (%)
Uncha ged
0.1 3.5
H p echa ged
0.01 4.0
H p echa ged
0.005 4.0
(a) (b)
Figu e 6. F ac u e su aces. (a) Uncha ged. (b) Hyd ogen p echa ged and es ed a 0.005 mm/min
Hyd ogen elec ochemical p echa ging
Enginee ing s ain (mm/mm)
0,000 0,025 0,050 0,075 0,100
Enginee ing s ess (MPa)
0
100
200
300
400
500
600
700
Uncha ged - 0.1 mm/min
H p echa ged - 0.01 mm/min
H p echa ged - 0.005 mm/min
1 mm
6 L.B. Pe al / S uc u al In eg i y P ocedia 00 (2019) 000–000
Since ma ensi e is known o be e y sensi i e o hyd ogen emb i lemen [7,8], his can be an impo an ac o
explaining he inc eased hyd ogen emb i lemen suscep ibili y o he sample es ed a 0.005 mm/min in he p esence
o hyd ogen (ൎ37 w ppm). Thus, in he p esence o in e nal hyd ogen, i is impo an o highligh ha he obse ed
ac u e mic omechanisms nea he no ched egion (Figu e 6b) can be p omo ed by he s ain-induced ma ensi e
o ma ion. I is well known ha hyd ogen a oms a e d i en by he high hyd os a ic s ess exis ing in he icini y o
he no ch and simul aneously, he s ain-induced ma ensi e ac s as a di usion pa h o hyd ogen [7] due o he highe
di usi i y h ough ha phase; his sho -ci cui di usion induced he o ma ion o quasi-clea ages and seconda y
c acks.
4. Conclusions
Hyd ogen ex-si u ensile es s we e employed o e alua e hyd ogen emb i lemen suscep ibili y in an addi i ely
manu ac u ed 316L by selec i e lase mel ing. Based on smoo h ensile esul s, signi ican hyd ogen ha dening (yield
s eng h and ul ima e ensile s eng h inc eased) was obse ed because o he high in e nal hyd ogen (ൎ37 w ppm).
Addi ionally, duc ili y sligh ly dec eased. On he o he hand, in he p esence o a no ch, he no ch ensile s eng h and
especially, he educ ion o a ea we e a ec ed by hyd ogen. In his case, ac u e mic omechanism changed om
duc ile (wi hou hyd ogen) o quasi-b i le (wi h hyd ogen) nea he no ched egion. Hyd ogen damage is also
explained because o he s ain-induced ma ensi e o ma ion nea he no ch ip egion.
Acknowledgemen s
The au ho s would like o hank he Spanish Go e nmen o he inancial suppo ecei ed o pe o m he esea ch
p ojec s PID2021-124768OB-C21 and TED2021-130413B-I00. This wo k was also suppo ed by he Regional
Go e nmen o Cas illa y León (Jun a de Cas illa y León) and by he Minis y o Science and Inno a ion MICIN and
he Eu opean Union Nex Gene a ion EU/PRTR (MR4W.P2 and MR5W.P3).
Re e ences
[1] Li e ani E, Toschi S, Ceschini L, Fo una o A. E ec o selec i e lase mel ing (SLM) p ocess pa ame e s on mic os uc u e and
mechanical p ope ies o 316L aus eni ic s ainless s eel. J Ma e P ocess Technol 2017;249:255–63.
h ps://doi.o g/10.1016/j.jma p o ec.2017.05.042.
[2] Lin J, Chen F, Liu F, Xu D, Gao J, Tang X. Hyd ogen pe mea ion beha io and hyd ogen-induced de ec s in 316L s ainless s eels
manu ac u ed by addi i e manu ac u ing. Ma e Chem Phys 2020;250. h ps://doi.o g/10.1016/j.ma chemphys.2020.123038.
[3] Zhou Z, Zhang K, Hong Y, Zhu H, Zhang W, He Y, e al. The dependence o hyd ogen emb i lemen on hyd ogen anspo in
selec i e lase mel ed 304L s ainless s eel. In J Hyd ogen Ene gy 2021;46:16153–63. h ps://doi.o g/10.1016/j.ijhydene.2021.02.035.
[4] Claeys L, Depo e T, De G ae e I, Ve beken K. Fi s obse a ion by EBSD o ma ensi ic ans o ma ions due o hyd ogen p esence
du ing s aining o duplex s ainless s eel. Ma e Cha ac 2019;156. h ps://doi.o g/10.1016/j.ma cha .2019.109843.
[5] Ma suo T, Yamabe J, Ma suoka S. E ec s o hyd ogen on ensile p ope ies and ac u e su ace mo phologies o Type 316L s ainless
s eel. In J Hyd ogen Ene gy 2014;39:3542–51. h ps://doi.o g/10.1016/j.ijhydene.2013.12.099.
[6] Díaz A, Aleg e JM, Cues a II, Zhang Z. Nume ical s udy o hyd ogen in luence on oid g ow h a low iaxiali ies conside ing ansien
e ec s. In J Mech Sci 2019;164. h ps://doi.o g/10.1016/j.ijmecsci.2019.105176.
[7] Zhang H yun, Zheng L wei, Wang T, L W jie, Shi Q xin, Ma J yao, e al. In e ela ionship be ween hyd ogen and α′-ma ensi e o SUS
304 aus eni ic s ainless s eel e ealed by ensile es s. Ma e ials Science and Enginee ing: A 2022;831.
h ps://doi.o g/10.1016/j.msea.2021.142169.
[8] Fan YH, Zhang B, Yi HL, Hao GS, Sun YY, Wang JQ, e al. The ole o e e sed aus eni e in hyd ogen emb i lemen ac u e o
S41500 ma ensi ic s ainless s eel. Ac a Ma e 2017;139:188–95. h ps://doi.o g/10.1016/j.ac ama .2017.08.011.

L.B. Pe al e al. / P ocedia S uc u al In eg i y 53 (2024) 52–57 57
L.B. Pe al / S uc u al In eg i y P ocedia 00 (2019) 000–000 5
analysis was pe o med on he ac u e su aces. XRD analysis e ealed he p esence o s ain-induced ma ensi e nea
he no ched egion (Table 6). I is impo an o highligh , his phase ans o ma ion was no p e iously ound a e he
3D p in ing p ocess (Figu e 2b).
Table 4. Tensile p ope ies on no ched samples. NTS: no ch
ensile s eng h and RA: educ ion o a ea
CHS
(mm/min)
Tes du a ion
(min)
σ
NTS
(MPa)
RA
(%)
Uncha ged 0.1 24 645�8 7.1
H p echa ged 0.01 180 619�4 5.8
H p echa ged 0.005 360 601�1 4.9
Table 5. Emb i lemen indexes on no ched samples
CHS
(mm/min)
EI σ
NTS
(%)
EI RA
(%)
Uncha ged 0.1 - -
H p echa ged 0.01 4 18
H p echa ged 0.005 7 31
Figu e 5. Tensile cu es on no ched samples
Table 6. S ain-induced ma ensi e in {211} wi h 2
θ
=156.4° and {200} wi h 2
θ
=106.1°. XRD esul s nea he no ched egion a e
he ensile es s
CHS (mm/min) S ain-induced ma ensi e (%)
Uncha ged
0.1 3.5
H p echa ged
0.01 4.0
H p echa ged
0.005 4.0
(a) (b)
Figu e 6. F ac u e su aces. (a) Uncha ged. (b) Hyd ogen p echa ged and es ed a 0.005 mm/min
Hyd ogen elec ochemical p echa ging
Enginee ing s ain (mm/mm)
0,000 0,025 0,050 0,075 0,100
Enginee ing s ess (MPa)
0
100
200
300
400
500
600
700
Uncha ged - 0.1 mm/min
H p echa ged - 0.01 mm/min
H p echa ged - 0.005 mm/min
1 mm
6 L.B. Pe al / S uc u al In eg i y P ocedia 00 (2019) 000–000
Since ma ensi e is known o be e y sensi i e o hyd ogen emb i lemen [7,8], his can be an impo an ac o
explaining he inc eased hyd ogen emb i lemen suscep ibili y o he sample es ed a 0.005 mm/min in he p esence
o hyd ogen (ൎ37 w ppm). Thus, in he p esence o in e nal hyd ogen, i is impo an o highligh ha he obse ed
ac u e mic omechanisms nea he no ched egion (Figu e 6b) can be p omo ed by he s ain-induced ma ensi e
o ma ion. I is well known ha hyd ogen a oms a e d i en by he high hyd os a ic s ess exis ing in he icini y o
he no ch and simul aneously, he s ain-induced ma ensi e ac s as a di usion pa h o hyd ogen [7] due o he highe
di usi i y h ough ha phase; his sho -ci cui di usion induced he o ma ion o quasi-clea ages and seconda y
c acks.
4. Conclusions
Hyd ogen ex-si u ensile es s we e employed o e alua e hyd ogen emb i lemen suscep ibili y in an addi i ely
manu ac u ed 316L by selec i e lase mel ing. Based on smoo h ensile esul s, signi ican hyd ogen ha dening (yield
s eng h and ul ima e ensile s eng h inc eased) was obse ed because o he high in e nal hyd ogen (ൎ37 w ppm).
Addi ionally, duc ili y sligh ly dec eased. On he o he hand, in he p esence o a no ch, he no ch ensile s eng h and
especially, he educ ion o a ea we e a ec ed by hyd ogen. In his case, ac u e mic omechanism changed om
duc ile (wi hou hyd ogen) o quasi-b i le (wi h hyd ogen) nea he no ched egion. Hyd ogen damage is also
explained because o he s ain-induced ma ensi e o ma ion nea he no ch ip egion.
Acknowledgemen s
The au ho s would like o hank he Spanish Go e nmen o he inancial suppo ecei ed o pe o m he esea ch
p ojec s PID2021-124768OB-C21 and TED2021-130413B-I00. This wo k was also suppo ed by he Regional
Go e nmen o Cas illa y León (Jun a de Cas illa y León) and by he Minis y o Science and Inno a ion MICIN and
he Eu opean Union Nex Gene a ion EU/PRTR (MR4W.P2 and MR5W.P3).
Re e ences
[1] Li e ani E, Toschi S, Ceschini L, Fo una o A. E ec o selec i e lase mel ing (SLM) p ocess pa ame e s on mic os uc u e and
mechanical p ope ies o 316L aus eni ic s ainless s eel. J Ma e P ocess Technol 2017;249:255–63.
h ps://doi.o g/10.1016/j.jma p o ec.2017.05.042.
[2] Lin J, Chen F, Liu F, Xu D, Gao J, Tang X. Hyd ogen pe mea ion beha io and hyd ogen-induced de ec s in 316L s ainless s eels
manu ac u ed by addi i e manu ac u ing. Ma e Chem Phys 2020;250. h ps://doi.o g/10.1016/j.ma chemphys.2020.123038.
[3] Zhou Z, Zhang K, Hong Y, Zhu H, Zhang W, He Y, e al. The dependence o hyd ogen emb i lemen on hyd ogen anspo in
selec i e lase mel ed 304L s ainless s eel. In J Hyd ogen Ene gy 2021;46:16153–63. h ps://doi.o g/10.1016/j.ijhydene.2021.02.035.
[4] Claeys L, Depo e T, De G ae e I, Ve beken K. Fi s obse a ion by EBSD o ma ensi ic ans o ma ions due o hyd ogen p esence
du ing s aining o duplex s ainless s eel. Ma e Cha ac 2019;156. h ps://doi.o g/10.1016/j.ma cha .2019.109843.
[5] Ma suo T, Yamabe J, Ma suoka S. E ec s o hyd ogen on ensile p ope ies and ac u e su ace mo phologies o Type 316L s ainless
s eel. In J Hyd ogen Ene gy 2014;39:3542–51. h ps://doi.o g/10.1016/j.ijhydene.2013.12.099.
[6] Díaz A, Aleg e JM, Cues a II, Zhang Z. Nume ical s udy o hyd ogen in luence on oid g ow h a low iaxiali ies conside ing ansien
e ec s. In J Mech Sci 2019;164. h ps://doi.o g/10.1016/j.ijmecsci.2019.105176.
[7] Zhang H yun, Zheng L wei, Wang T, L W jie, Shi Q xin, Ma J yao, e al. In e ela ionship be ween hyd ogen and α′-ma ensi e o SUS
304 aus eni ic s ainless s eel e ealed by ensile es s. Ma e ials Science and Enginee ing: A 2022;831.
h ps://doi.o g/10.1016/j.msea.2021.142169.
[8] Fan YH, Zhang B, Yi HL, Hao GS, Sun YY, Wang JQ, e al. The ole o e e sed aus eni e in hyd ogen emb i lemen ac u e o
S41500 ma ensi ic s ainless s eel. Ac a Ma e 2017;139:188–95. h ps://doi.o g/10.1016/j.ac ama .2017.08.011.