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A ch. Me all. Ma e . 65 (2020), 2, 727-734
DOI: 10.24425/amm.2020.132812
R. KAWULOK1*, I. SCHINDLER1, H. NAVRÁTIL1, V. ŠEVČÁK1, J. SOJKA1,
K. KONEČNÁ1, B. CHMIEL2
HOT FORMABILITY OF HEAT-RESISTANT STAINLESS STEEL X15C NiSi 20-12
High- empe a u e plas ic p ope ies o hea - esis an s ainless s eel X15C NiSi 20-12 we e assessed on he basis o ho ensile
es s and nil s eng h es s. The esul s we e suppo ed by me allog aphic analyses using SEM and EDX analysis. The o mabili y
o he in es iga ed s eel can be di ided in o oughly h ee empe a u e a eas. In he empe a u e ange o 900°C o abou 1050°C,
o mabili y was nega i ely a ec ed by p ecipi a ion o ca bide pa icles a g ain bounda ies. As he empe a u e ose o 1200°C,
hese pa icles dissol ed, esul ing in an inc ease in o mabili y. Fu he empe a u e inc eases esul ed in a ela i ely s eep d op
in o mabili y caused by o e hea ing o he ma e ial. The nil duc ili y empe a u e o 1280°C and he nil-s eng h empe a u e o
1362°C we e de e mined. The Plas ic and s eng h p ope ies o he in es iga ed ma e ial we e compa ed wi h he de o ma ion
beha io o he e e ence s eel X5C Ni 18-10, which shows a signi ican ly wide ange o sui able o ming empe a u es.
Keywo ds: Hea - esis an s ainless s eel, Ho ension es , Nil s eng h empe a u e, Nil duc ili y empe a u e
1. In oduc ion
Aus eni ic hea - esis an s eels had been de eloped on he
basis o s ainless s eels by he end o he 19 h cen u y and oday,
hey a e widely used in cons uc ion ma e ials o applica ions
such as boile s, eac o s, hea e s, hea exchange s, e c. Thei main
ad an age is he combina ion o ela i ely high s eng h, c eep,
oxida ion and co osion esis ance and ela i ely low p oduc ion
cos s [1-7]. Complica ions in hese s eels a e associa ed wi h
de e io a ion o mechanical p ope ies and o mabili y due o
p ecipi a ion. Unde ope a ing condi ions, a ious seconda y
phases can be o med in aus eni ic s eels, such as MX ca -
boni ides, M23C6 ca bides, Z phases, sigma phases, and La es
phases, which may agglome a e u he due o aging [1,8-11].
Thus, he mic os uc u e o hea - esis an s eels is o med by
aus eni ic g ains, which a e lined wi h p ecipi a es o med in he
empe a u e ange o abou 600-1000 (1050)°C. These pa icles
lead o emb i lemen , and he s eel is subjec ed o dissolu ion an-
nealing, which usually akes place in he ange o 1000-1100°C.
Ano he nega i e e ec is he educed ec ys alliza ion abili y
o aus eni ic hea - esis an s eels [12-18].
MX ca boni ides and M23C6 ype ca bides ha e an cc
la ice and no mally nuclea e u he along he g ain bounda ies
and in loca ions wi h highe disloca ion densi y. This phenom-
enon is associa ed wi h he a e o di usion, which is highe in
hese places han in he emaining olume [19-24]. The M23C6
ca bide oughening a e is much highe han ha o MX ype
ca boni ides, which p omo es high empe a u e c eep. Mic o-
alloying elemen s, such as Ti, Nb and V also con ibu e o he
o ma ion o MX ca boni i ides, and since hey ha e a highe
ca bon a ini y han ch omium, hey a e used o educe and slow
down he o ma ion o M23C6 ca bides. M23C6 ca bides posi ed
along he g ain bounda ies can also cause in e -c ys alline co -
osion [22-24].
The aim o he wo k was o e alua e he ho o mabili y
o ch omium nickel aus eni ic s ainless s eel and hea - esis an
X15C NiSi 20-12. This s eel is used o he cons uc ion o hea
ea men equipmen , pa s o boile s and u nace agg ega es
( i ings, g a es, con eyo s, hinges), hea exchange and an
componen s, o he mally s essed pa s o ce amic and glass
u naces, he mocouple p o ec i e slee es, as hea s essed
as ene s and o he s [1,2]. The de o ma ion beha io s udy will
be based mainly on uniaxial ho ensile es s, a e y sensi i e
me hod due o he p e ailing ensile componen s o he s ess in
o mabili y e alua ion. The pa ame e s e alua ed a e duc ili y,
con ac ion and ul ima e ensile s eng h. The ensile es esul s
can be used o de e mine he NDT (Nil duc ili y empe a u e) a
which he o mabili y o he ma e ial is exhaus ed and ac u e
1 VSB – TECHNICAL UNIVERSITY OF OSTRAVA, FACULTY OF MATERIALS SCIENCE AND TECHNOLOGY, 17. LISTOPADU 15/2172, 708 00 OSTRAVA – PORUBA, CZECH REPUBLIC
2 TŘINECKÉ ŽELEZÁRNY, A.S., PRŮMYSLOVÁ 1000, 739 61 TŘINEC, CZECH REPUBLIC
* Co esponding au ho : os isla [email p o ec ed]
728
occu s unde load wi hou e idence o elonga ion o he es
specimen. Ano he c i ical empe a u e o he high empe a u e
egion o me allic ma e ials is he nil s eng h empe a u e (NST)
a which he ma e ial loses all i s s eng h du ing hea ing due o
he g ain bounda y mel ing, i.e. empe a u e a which he ma e ial
does no ole a e any load. NST is always highe han NDT, bu
bo h o hese c i ical empe a u es a e highly dependen on he
chemical composi ion o he ma e ial [12,25-27].
2. Expe imen al
S eel X15C NiSi 20-12 wi h chemical composi ionin Ta-
ble 1 was supplied in a pos -ho olling condi ion.
TABLE 1
Chemical composi ion o X15C NiSi 20-12 s eel in w .%
X15C NiSi 20-12 CMnSiC NiMoN
0.16 1.01 1.54 20.2 12.3 0.27 0.07
The de o ma ion beha io was in es iga ed on a ho de-
o ma ion simula o Gleeble 3800. Tes s o de e mining he
nil-s eng h empe a u e (NST) we e pe o med on cylind ical
samples wi h a diame e o 6 mm and a leng h o 81 mm. These
samples we e loaded wi h a cons an ensile o ce o 80 kN
h oughou he es ia ai con olled pis on. A he same ime,
he esis i e hea ing o he samples was ca ied ou a a a e o
20°C·s–1 up o a empe a u e 1200°C, and hen he hea ing was
slowed down o 2°C·s–1, while he empe a u e was linea ly in-
c easing o he ac u e o he sample caused by he combina ion
o mel ing e ec g ain bounda ies and e y low ensile o ces. In
o de o elimina e he e ec o possible inhomogenei ies in he
in es iga ed ma e ials and also o s a is ical e alua ion, his es
was epea ed 3 imes – see Fig. 1. The a e age NST was 1362°C
wi h a ela i ely low s anda d de ia ion o ±4°C.
Fig. 1. Reco ds o NST measu emen o s eel X15C NiSi 20-12
Fo ho ensile es ing, cylind ical specimens wi h a di-
ame e o 10 mm and a leng h o 116.5 mm we e p epa ed and
h eaded on he end po ions. Ho -g ips s ainless s eel jaws
(Fig. 2) we e used o uniaxial ension es s, which a e used o
p o ide uni o m hea ing in he 20 mm zone [25,26]. Tensile
es s we e ca ied ou in he empe a u e ange o 900-1280°C.
The esis ance hea ing o he samples was a he a e o 10°C·s–1
di ec ly o he de o ma ion empe a u e, whe e 180 s delay ol-
lowed. The pull o he sample in o he ac u e was a a s oke
a e o 50 mm·s–1.
Fig. 2. Placemen o samples in ho g ips jaw ype o es s on simula-
o Gleeble 3800
Tensile diag ams (see Fig. 3) om which he maximum
o ce alues Fmax (kN) and he sample elonga ion ill ac u e
∆L (mm) we e de e mined. These alues we e subsequen ly
used o calcula e he ul ima e ensile s eng h RmT (MPa) and
he ho duc ili y AT (%):
PD[


mT
F
RS

 (1)


T
L
AL
'
 (2)
Whe e ∆L is elonga ion ill ac u e (mm) and L0 = 20 mm is he
ini ial measu ed leng h.
Fig. 3. G aphical ep esen a ion o he ho ensile es o s eel X15C NiSi
20-12
Con ac ion ZT (%) was exp essed by c oss-sec ional a eas
o es ba s a e b eaking S1 (mm2) and ini ial c oss-sec ion
S0 = 78.5 mm2:
729



T
SS
ZS


 (3)
Selec ed samples we e subjec ed o me allog aphical
analyses (ligh mic oscopy, SEM and EDX). Con en ional
me allog aphic examina ion by ligh mic oscopy was used o
he mic os uc u e analysis. Polishing and g inding was done
by using pape s and SiO2 suspensions. The g ain size calcula-
ion was based on he in e cep leng hs measu emen using
he so wa e Quick PHOTO INDUSTRIAL 3.2. Fo a sample
hea ed o 1050°C, supplemen a y analysis o he p ecipi a es
was pe o med by he SEM me hod on a JEOL JSM-6490LV
scanning elec on mic oscope equipped wi h an INCA x-ac
ene gy dispe sion analyze (Ox o d Ins umen s). Chemical
e ching was ealized wi h a eagen o 10 pa s H2O, 10 pa s
HNO3 and 1 pa HCl.
Fo compa ison, analogous expe imen s we e pe o med on
e e ence aus eni ic s ainless s eel X5C Ni 18-10, he chemical
composi ion o which is gi en in Table 2.
TABLE 2
Chemical composi ion o X5C Ni 18-10 s eel in w .%
X5C Ni 18-10 CMnSiC NiMoN
0.024 1.55 0.37 18.2 8.0 0.25 0.07
3. Resul s and discussion
Ho de o ma ion beha io o s eel X15C NiSi 20-12
Examples o b oken samples a e shown in Fig. 4. Fig. 5
shows he ac u e su aces o he selec ed wo o ming em-
pe a u es. In he case o 1280°C, he signi ican coa sening o he
g ain, which has a mean size o abou 0.4 mm, is clea ly isible.
Signi ican coa sening o he g ain is p obably due o a combina-
ion o se e al causes. Signi ican coa sening o he g ain ends
o be associa ed wi h he p esence o ancho ed s uc u e due
o pa icles o o he phases o a la ge size o he p ima g ain,
including o he c ys allog aphic o ien a ion.
As can be seen om Fig. 3, wi h inc easing empe a u e,
he con ac s eng h dec eases o a empe a u e o abou 1265°C.
This phenomenon is displayed along wi h he duc ili y depend-
ence on de o ma ion empe a u e in Fig. 6. I is also e iden om
his g aph ha he highes o mabili y can be expec ed o he
in es iga ed s eel wi hin a na ow empe a u e ange o abou
1100 o 1200°C, which is in ag eemen wi h au ho s [2,14]. When
he empe a u e was inc eased u he , he o mabili y d opped
sha ply, wi h an NDT o 1280°C being de e mined.
Fig. 6. The mal dependence o duc ili y ill ac u e, con ac ion and
ul ima e ensile s eng h s eel X15C NiSi 20-12
Ini ial s uc u e a ec ed by he hea ing empe a u e
o s eel X15C NiSi 20-12
The ini ial ma e ial s uc u e is cha ac e ized by conside -
able he e ogenei y wi h he appea ance o g ains o he o de o
en hs o a millime e – see Fig. 7.
In o de o cla i y he measu ed da a, u he expe imen s
we e conduc ed aimed a s udying he s uc u e o he samples
be o e de o ma ion. Tensile samples we e hea ed o selec ed
empe a u es o 900°C, 1050°C, 1200°C, o 1280°C, and hei
s uc u e was ixed by quenching. Me allog aphic images o
s uc u es a e hea ing in Fig. 8 documen aus eni ic g ains, o en
wi h cha ac e is ic wins. The o iginal coa se g ains emained
a hea ing empe a u es o 900-1050°C. Da k e ching a i ac s
signal he occu ence o inclusions.
Fig. 4. Selec ed examples o samples a e es
Fig. 5. Examples o ac u e su aces a e sample ailu e
730
Fig. 7. Ini ial s uc u e o X15C NiSi 20-12
I has been e i ied ha he accele a ion o g ain g ow h
occu s abo e a empe a u e o abou 1100°C – see Fig. 9.
In he empe a u e ange o 900-1050°C, small o ma ions
occu in pa icula in he o m o chains (see Fig. 10a), which
a e e y likely o educe o mabili y – his co esponds o he
g aph in Fig. 6. A hese empe a u es, he g ain bounda y di u-
sion akes place much as e han in he emaining olume and
g ain bounda ies p o ide p e e ed nuclea ion si es o ca bide
pa icle p ecipi a ion. A highe empe a u es, hese o ma ions
dissol e a he g ain bounda ies (see Fig. 10b) and hus inc ease
o mabili y. Examples o simila mechanisms a e desc ibed in
se e al pape s [1,28-31].
The d op in o mabili y a empe a u es abo e 1200°C is
mainly due o o e hea ing o he ma e ial, which is associa ed
wi h signi ican coa sening o he g ain.
SEM/EDX analysis
Fig. 11a) illus a es he cha ac e o he backsca e ed
elec on p ecipi a ion pa e n a e polishing he sample. I
is clea ha p ecipi a es o med nea -con inuous mesh a he
g ain bounda ies, and we e ypically in he ange o abou
0.5-2.5 μm and o a small ex en p ecipi a es o up o 5 μm in
leng h we e also obse ed. A small po ion o p ecipi a es was
also p esen wi hin he aus eni ic g ains. Fig. 11b) shows he
cha ac e o p ecipi a ion a e e ching. To cla i y he na u e o
he p ecipi a es, an EDX analysis o hei chemical composi ion
was pe o med. Fig. 12 compa es he esul s o EDX analysis
o he me al ma ix and he p ecipi a e pa icles. The esul s o
a)
c)
b)
d)
Fig. 8. Examples o he mic os uc u e o selec ed hea ing empe a u es o s eel X15C NiSi 20-12; a) 900°C, b) 1050°C, c) 1200°C, d) 1280°C
731
a se ies o analyses showed ha he p ecipi a es a e likely o be
M23C6 ype ca bides con aining p e e ably C bu also inc eased
he con en o molybdenum (54.34% C ; 30.48% Fe; 9.27% C;
3.48% Ni; 1.33% Mo; 0.75% Mn; 0.35% Si). The con en o
Si in he p ecipi a es was always lowe compa ed o he me al
ma ix (19.43% C ; 60.73% Fe; 5.29% C; 11.51% Ni; 0.35%
Mo; 1.07% Mn; 1.62% Si). The p esence o M23C6 ca bides in
he sample hea ed o 1050°C is p obably due o he ac ha
he inc eased p opo ion o silicon in ch omium-nickel s eels
p omo es p ecipi a ion o his ype o ca bide and inc eases he
empe a u e ange a which he ca bide is s able [32]. The delay
ime a 1050°C was p obably no su icien o dissol e he ca bide
p ecipi a es, because hei o ma ion du ing cooling should be
elimina ed due o he quenching o he sample in o wa e . Fo
he s udied s eel, he empe a u e o 1050°C ep esen s he lowe
limi o he ecommended solu ion annealing in e al [1,2]
The same sample, EDX analysis o he chemical composi-
ion o he coa se non-me allic inclusions was also pe o med
– see Fig. 13 and 14. Coa se non-me allic inclusions we e ound
o be complex oxysul ides. Al2O3 – based oxides we e p esen in
he cen e o he inclusions and con ained an inc eased Ca con en
(47.5% Al; 46.1% O; 5.6% Ca; 0.4% C ; 0.4% Fe). The inclu-
sion en elope was a sulphide o he (Mn, Ca)S ype (46.7% Mn;
35.0% S; 7.5% Ca; 5.2% C ; 2.1% Al; 2.1% O; 1.6% Fe).
b)a)
Fig. 10. G ain bounda ies wi h and wi hou ine elemen s in s eel X15C NiSi 20-12; a) 900°C, b) 1200°C
a) b)
Fig. 11. SEM mic oscopy o sample s uc u e wi h pa icles on g ain bounda ies a e hea ing a 1050°C; a) Polished sample, b) E ched sample
wi h local si es o chemical EDX analysis
Fig. 9. In luence o hea ing empe a u e on g ain size X15C NiSi 20-12

732
o 32°C compa ed o s eel X15C NiSi 20-12. This co esponds
o he empe a u e dependence o s eng h and o mabili y in
Fig. 16-17.
Due o he highe con en o C, C and Si, and he expec ed
lowe ec ys alliza ion capaci y, he s eel X15C NiSi 20-12
shows g ea e s eng h especially a low empe a u es, he di -
e ences a e negligible a he empe a u e ange o 1200-1250°C.
This e ec is mos likely due o he highe con en o C, C and Si
since hese elemen s signi ican ly a ec s eng h and plas ici y as
well as ec ys alliza ion kine ics. Silicon has a simila e ec o C
in aus eni ic s eels. The highe silicon con en , which is dissol ed
in aus eni e, g adually dec eases o mabili y h oughou he ho
o ming empe a u e, and his e ec is pa icula ly appa en o
Si con en s abo e 1%. Ch omium in solid solu ion inc eases
s eng h, inc eases ac i a ion ene gy and educes ec ys alliza ion
abili y, especially in high alloy aus eni ic s eels. The Fo ma ion
a) b)
Fig. 12. EDX analysis o sample a 1050°C; a) ma ix (Spec um 1), b) p ecipi a e (Spec um 2)
Fig. 13. Example o inclusion in sample 1050°C
a) b)
Fig. 14. EDX analysis o inclusion o he sample a 1050°C; a) Inclusion en elope o med by (Mn,Ca)S, b) The cen al pa o he Al2O3-based
inclusions wi h inc eased Ca con en
Compa ison o ho de o ma ion beha iou
o X15C NiSi 20-12 and X5C Ni 18-10 s eels
Fo e e ence s eel X5C Ni 18-10, a nil-s eng h em-
pe a u e o 1394°C was de e mined wi h a s anda d de ia ion
o ±1°C (see Fig. 15), indica ing a ela i e educ ion o NST
o ch omium ca bide un a o ably a ec s o mabili y in he lowe
o ming empe a u e ange. The c i ical de o ma ion εc equi ed
o he ini ia ion o dynamic ec ys alliza ion o aus eni ic
ypes o s eels is gene ally highe in he ange 1000-850°C han
εc > 0.5. In pa icula , dynamic eco e y wi h pa ial emo al o
ein o cemen is aking place in o ming such alloyed aus eni ic
733
s eels, bu he decisi e pa o eco e y is due o pos -dynamic
p ocesses [12-14].
Fig. 17 shows ha he ho o mabili y o X15C NiSi 20-12
is i ually lowe o e he en i e empe a u e ange compa ed
o he e e ence less alloyed s eel. The easons a e analogous o
he di e ences in s eng h.
Nil duc ili y empe a u e (NDT) has a alue o app ox.
1374°C o X5C Ni 18-10 s eel; his is 94°C mo e han in he
case o X15C NiSi 20-12, which he e o e shows a much na -
owe ange o sui able o ming empe a u es. The e is a a ie y
o calcula ions o de e mining solidus TS and TL liquidus em-
pe a u e alues, bu only a ew a e sui able o complex alloyed
aus eni ic s ainless s eels [33-35].
The expe imen ally de e mined NDT and NST alues co -
espond o he solidus TS and TL liquidus empe a u e calcula ions
acco ding o o mulas [36]:
   

 
  &  6  6L
 0Q  1L  &U
 $O  3
S
T   



(41)
  
   

  &  6  &X
6L 0Q 0R 1L
&U 7L 9 3
L
T   
  


(4)
A compa ison o all c i ical empe a u es o he high em-
pe a u e egion o he wo in es iga ed s eels is gi en in Table 3.
TABLE 3
C i ical empe a u es o in es iga ed s eels
NDT (°C) NST (°C) TS (°C) [36] TL (°C) [36]
X15C NiSi 20-12 1280 1362 1387 1423
X5C Ni 18-10 1374 1394 1448 1463
The di e ence in NST and NDT alues should be a ound
30°C wi h a ole ance o ±15°C, acco ding o he au ho s o he
pape s [26,27]. This co esponds o a di e ence o 20°C in he
case o s eel X5C Ni 18-10, bu he di e ence o 82°C in s eel
X15C NiSi 20-12 is abno mally la ge and con i ms he unsui -
abili y o applying high o ming empe a u es.
Fig. 16. Compa ison o s eng h o wo s eels X15C NiSi 20-12 and
X5C Ni 18-10
b)a)
Fig. 17. Compa ison o he empe a u e dependence o plas ic p ope ies o s eels X15C NiSi 20-12 and X5C Ni 18-10; a) Duc ili y, b) Reduc-
ion o a ea
Fig. 15. G aph o NST measu emen o s eel X5C Ni 18-10
734
4. Conclusions
C i ical empe a u es associa ed wi h high empe a u e
plas ici y o hea - esis an s ainless s eel X15C NiSi 20-12 was
ound, i.e. NDT = 1280°C and NST = 1362°C. I has been ound
ha he empe a u e ange mos sui able o o ming his s eel
has a e y na ow ange o 1100-1200°C. A lowe empe a u es,
he o mabili y is sligh ly educed due o he ine ca bide mesh
along he g ain bounda ies, mainly o med by M23C6 pa icles.
As he empe a u e ises up o abou 1200°C, hese pa icles
dissol e, esul ing in imp o ed plas ic p ope ies. The ela i ely
s eep d op in o mabili y a empe a u es abo e 1200°C is mainly
due o g ain g ow h in connec ion wi h ma e ial o e hea ing.
A compa ison o he de o ma ion beha io o he in es iga -
ed s eel wi h aus eni ic s ainless s eel X5C Ni 18-10 showed ha
he alloy wi h lowe C, C and Si con en showed lowe s eng h
and o mabili y a i ually all empe a u es abo e 900°C. A he
same ime, he e e ence NDT and NST alues o he e e ence
s eel a e signi ican ly highe han in he case o X15C NiSi 20-12.
Acknowledgemen s
This pape was c ea ed a he Facul y o Ma e ials Science and Technology
wi hin he P ojec No. CZ.02.1.01/0.0/0.0/17_049/0008399 unded by he
Minis y o Educa ion, You h and Spo s o he Czech Republic; and wi hin
he s uden s’ g an p ojec SP2020/88 suppo ed a he VŠB – TU Os a a
by he Minis y o Educa ion o he Czech Republic.
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