Full text
c ys als
A icle
E ec o S ain on T ans o ma ion Diag ams o
100C 6 S eel
Ros isla Kawulok 1,* , I o Schindle 1, Ja osla Sojka 1, Pe Kawulok 1, Pe Opˇela 1,
Lukáš Pindo 2, Edua d G ycz 2, S anisla Rusz 1and Voj ˇech Še ˇcák1
1VŠB-TU Os a a, Facul y o Ma e ials Science and Technology, VSB-Technical Uni e si y o Os a a,
70800 Os a a, Czech Republic; [email p o ec ed] (I.S.); ja osla [email p o ec ed] (J.S.);
pe [email p o ec ed] (P.K.); pe [email p o ec ed] (P.O.); s anisla [email p o ec ed] (S.R.);
[email p o ec ed] (V.Š.)
2
Tˇ ineck
é
Želez
á
ny, a.s., 73961 Tˇ inec, Czech Republic; [email p o ec ed] (L.P.); [email p o ec ed] (E.G.)
*Co espondence: os isla [email p o ec ed]
Recei ed: 5 Ma ch 2020; Accep ed: 18 Ap il 2020; Published: 21 Ap il 2020
Abs ac :
Based on dila ome ic es s, he e ec o a ious alues o p e ious de o ma ion on he
kine ics o aus eni e ans o ma ions du ing he cooling o 100C 6 s eel has been s udied. Dila ome ic
es s ha e been pe o med wi h he use o he op ical dila ome ic module o he plas ome e Gleeble
3800. The ob ained esul s we e compa ed o me allog aphic analyses and ha dness measu emen s
HV30. Uniaxial comp ession de o ma ions we e chosen as ollows: 0, 0.35, and 1; no e ha hese a e
ue (loga i hmic) de o ma ions. The highly impo an inding was he absence o baini e. In addi ion,
i has been e i ied ha wi h he inc easing amoun o de o ma ion, he e is a u he shi in he
pea li ic egion o highe cooling a es. The p e ious de o ma ion also a ec ed he empe a u e
ma ensi e s a , which dec eased due o de o ma ion. The de o ma ion alue o 1 also shi ed he
c i ical cooling a e equi ed o ma ensi e o ma ion om he 12 ◦C/s o 25 ◦C/s.
Keywo ds: ans o ma ion diag ams; 100C 6 s eel; dila ome ic es
1. In oduc ion
T ans o ma ion diag ams can be di ided in o wo ypes. The i s ype is he ime- empe a u e-
ans o ma ion (TTT) diag am, which desc ibes he aus eni e ans o ma ions du ing an iso he mal
dwell. The second ype is he con inuously cooling ans o ma ion (CCT) diag am ha desc ibes
he e ec o cooling a e on aus eni e ans o ma ion [
1
,
2
]. In addi ion, his ype o diag am can be
modi ied o a de o ma ion con inuously cooling ans o ma ion (DCCT) ype, which also includes
he e ec o p e ious de o ma ion. Such diag ams hen ind hei p ac ical applica ion in he case
o he con olling o s eel o ming p ocesses ( olling, o ging), and hei indings o en lead o an
imp o emen in he economics o he p oduc ion p ocess [3–7].
Aus eni e ans o ma ionkine icsdu ingcoolingisin luencedbymany ac o s.Themos impo an
ac o s a e he chemical composi ion and he a e o cooling o he s eels. Fu he , he ans o ma ion o
supe cooled aus eni e is in luenced by aus eni iza ion empe a u e, ini ial s uc u e, aus eni ic g ain
size, and p e ious de o ma ion [
8
–
17
]. The e ec s o all hese ac o s a e summa ized in he schema ic
CCT diag am in Figu e 1[8].
C ys als 2020,10, 326; doi:10.3390/c ys 10040326 www.mdpi.com/jou nal/c ys als
C ys als 2020,10, 326 2 o 16
C ys als 2020, 10, x FOR PEER REVIEW 2 o 17
.
Figu e 1. In luence o alloying, he momechanical ac o s, and s uc u e s a e on ans o ma ion
kine ic [8].
The e ec o p e ious de o ma ion i sel on di e en ypes o s eel is e alua ed in a numbe o
esea ch s udies [18–28]. F om he ob ained indings, i can be claimed ha he p e ious
de o ma ion, in combina ion wi h he chemical composi ion and o he ac o s, has di e en e ec s
on indi idual ans o ma ions o ans o ma ion p oduc s. The au ho s o hese wo ks assume ha
he de o ma ion accele a es di usion-con olled ans o ma ions, speci ically he ans o ma ion
o aus eni e o e i e and pea li e [18–26]. Due o he de o ma ion, he numbe o la ice de ec s
inc eases, which p omo es he di usion o all a oms in he solid solu ion and leads o a as e
nuclea ion and g ow h o he new phase nuclei— his leads o he accele a ion o bo h
ans o ma ions [23–26]. The accele a ing e ec s o inc easing de o ma ion and s ain a e on e i ic
ans o ma ion a e shown in Figu es 2 and 3, espec i ely (whe e empe a u e A
3
is he
ans o ma ion empe a u e o aus eni e o e i e and A
1
is he ans o ma ion empe a u e o
aus eni e o pea li e by he cooling o hypoeu ec oid s eels). In addi ion, om Figu e 2, i is e iden
ha wi h inc easing de o ma ion (up o abou 0.4), he a ea o e i ic ans o ma ion is
na owed— hus, he pea li ic ans o ma ion is accele a ed [26]. This hesis con i ms ha e en ou
p e ious esea ch de ec ed ha he e ec o p e ious de o ma ion leads o an inc eased ac ion o
pea li e and e i e [11,20].
Figu e 1.
In luence o alloying, he momechanical ac o s, and s uc u e s a e on ans o ma ion
kine ic [8].
The e ec o p e ious de o ma ion i sel on di e en ypes o s eel is e alua ed in a numbe o
esea ch s udies [
18
–
28
]. F om he ob ained indings, i can be claimed ha he p e ious de o ma ion,
in combina ion wi h he chemical composi ion and o he ac o s, has di e en e ec s on indi idual
ans o ma ions o ans o ma ion p oduc s. The au ho s o hese wo ks assume ha he de o ma ion
accele a es di usion-con olled ans o ma ions, speci ically he ans o ma ion o aus eni e o e i e
and pea li e [
18
–
26
]. Due o he de o ma ion, he numbe o la ice de ec s inc eases, which p omo es
he di usion o all a oms in he solid solu ion and leads o a as e nuclea ion and g ow h o he new
phase nuclei— his leads o he accele a ion o bo h ans o ma ions [
23
–
26
]. The accele a ing e ec s
o inc easing de o ma ion and s ain a e on e i ic ans o ma ion a e shown in Figu es 2and 3,
espec i ely (whe e empe a u e A
3
is he ans o ma ion empe a u e o aus eni e o e i e and
A
1
is he ans o ma ion empe a u e o aus eni e o pea li e by he cooling o hypoeu ec oid s eels).
In addi ion, om Figu e 2, i is e iden ha wi h inc easing de o ma ion (up o abou 0.4), he a ea o
e i ic ans o ma ion is na owed— hus, he pea li ic ans o ma ion is accele a ed [
26
]. This hesis
con i ms ha e en ou p e ious esea ch de ec ed ha he e ec o p e ious de o ma ion leads o an
inc eased ac ion o pea li e and e i e [11,20].
C ys als 2020, 10, x FOR PEER REVIEW 2 o 17
.
Figu e 1. In luence o alloying, he momechanical ac o s, and s uc u e s a e on ans o ma ion
kine ic [8].
The e ec o p e ious de o ma ion i sel on di e en ypes o s eel is e alua ed in a numbe o
esea ch s udies [18–28]. F om he ob ained indings, i can be claimed ha he p e ious
de o ma ion, in combina ion wi h he chemical composi ion and o he ac o s, has di e en e ec s
on indi idual ans o ma ions o ans o ma ion p oduc s. The au ho s o hese wo ks assume ha
he de o ma ion accele a es di usion-con olled ans o ma ions, speci ically he ans o ma ion
o aus eni e o e i e and pea li e [18–26]. Due o he de o ma ion, he numbe o la ice de ec s
inc eases, which p omo es he di usion o all a oms in he solid solu ion and leads o a as e
nuclea ion and g ow h o he new phase nuclei— his leads o he accele a ion o bo h
ans o ma ions [23–26]. The accele a ing e ec s o inc easing de o ma ion and s ain a e on e i ic
ans o ma ion a e shown in Figu es 2 and 3, espec i ely (whe e empe a u e A
3
is he
ans o ma ion empe a u e o aus eni e o e i e and A
1
is he ans o ma ion empe a u e o
aus eni e o pea li e by he cooling o hypoeu ec oid s eels). In addi ion, om Figu e 2, i is e iden
ha wi h inc easing de o ma ion (up o abou 0.4), he a ea o e i ic ans o ma ion is
na owed— hus, he pea li ic ans o ma ion is accele a ed [26]. This hesis con i ms ha e en ou
p e ious esea ch de ec ed ha he e ec o p e ious de o ma ion leads o an inc eased ac ion o
pea li e and e i e [11,20].
Figu e 2.
E ec o de o ma ion on he e i ic ans o ma ion o HSLA (High-S eng h Low-Alloy)
s eel [
26
]. The empe a u es o A 1 and A 3 ep esen he empe a u es o he ansi ion du ing cooling.
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.
Figu e 1. In luence o alloying, he momechanical ac o s, and s uc u e s a e on ans o ma ion
kine ic [8].
The e ec o p e ious de o ma ion i sel on di e en ypes o s eel is e alua ed in a numbe o
esea ch s udies [18–28]. F om he ob ained indings, i can be claimed ha he p e ious
de o ma ion, in combina ion wi h he chemical composi ion and o he ac o s, has di e en e ec s
on indi idual ans o ma ions o ans o ma ion p oduc s. The au ho s o hese wo ks assume ha
he de o ma ion accele a es di usion-con olled ans o ma ions, speci ically he ans o ma ion
o aus eni e o e i e and pea li e [18–26]. Due o he de o ma ion, he numbe o la ice de ec s
inc eases, which p omo es he di usion o all a oms in he solid solu ion and leads o a as e
nuclea ion and g ow h o he new phase nuclei— his leads o he accele a ion o bo h
ans o ma ions [23–26]. The accele a ing e ec s o inc easing de o ma ion and s ain a e on e i ic
ans o ma ion a e shown in Figu es 2 and 3, espec i ely (whe e empe a u e A
3
is he
ans o ma ion empe a u e o aus eni e o e i e and A
1
is he ans o ma ion empe a u e o
aus eni e o pea li e by he cooling o hypoeu ec oid s eels). In addi ion, om Figu e 2, i is e iden
ha wi h inc easing de o ma ion (up o abou 0.4), he a ea o e i ic ans o ma ion is
na owed— hus, he pea li ic ans o ma ion is accele a ed [26]. This hesis con i ms ha e en ou
p e ious esea ch de ec ed ha he e ec o p e ious de o ma ion leads o an inc eased ac ion o
pea li e and e i e [11,20].
Figu e 3.
E ec o s ain a e on he e i ic ans o ma ion o HSLA s eel [
26
]. The empe a u es o A 1
and A 3 ep esen he empe a u es o he ansi ion du ing cooling.
In he case o assessing he e ec o plas ic de o ma ion on he ans o ma ion o aus eni e o
baini e and ma ensi e, his e ec is ambiguous and, he e o e, canno be gene alized as in he p e ious
case. When aus eni e is de o med, a dense disloca ion ne wo k is o med and inhibi s he p og ess
o he phase bounda ies, and despi e a la ge numbe o nuclei, he sha e o he new phase is lowe
han ha o non-de o med aus eni e, especially a highe cooling a es. The ole o disloca ion on he
ma ensi e s a empe a u e is mo e con o e sial. The la ge amoun o disloca ions gene a ed by a
la ge plas ic de o ma ion o aus eni e p io o he ma ensi e may s abilize he glissile emb yo–aus eni e
in e ace, leading o a dec ease in ma ensi e (Ms)- empe a u e ( empe a u e o s a ing ma ensi e
ans o ma ion). This is known as he disloca ion s abiliza ion mechanism. Howe e , he e is
some imes an opposi e phenomenon; accumula ed la ice de ec s ini ia e ma ensi e o ma ion and
enable i s o ma ion a highe empe a u es han in he case o non-de o med aus eni e ans o ma ion.
An example o his is he g aph in Figu e 4, which shows ha he Ms empe a u e ises a e a heigh
de o ma ion o 30% and 60% compa ed o he Ms empe a u e o he unde o med specimens o selec ed
s eels [18,23,24,29–36].
C ys als 2020, 10, x FOR PEER REVIEW 3 o 17
Figu e 2. E ec o de o ma ion on he e i ic
ans o ma ion o HSLA (High-S eng h
Low-Alloy) s eel [26]. The empe a u es o
A
1
and A
3
ep esen he empe a u es o he
ansi ion du ing cooling.
Figu e 3. E ec o s ain a e on he e i ic
ans o ma ion o HSLA s eel [26]. The
empe a u es o A
1
and A
3
ep esen he
empe a u es o he ansi ion du ing
cooling.
In he case o assessing he e ec o plas ic de o ma ion on he ans o ma ion o aus eni e o
baini e and ma ensi e, his e ec is ambiguous and, he e o e, canno be gene alized as in he
p e ious case. When aus eni e is de o med, a dense disloca ion ne wo k is o med and inhibi s he
p og ess o he phase bounda ies, and despi e a la ge numbe o nuclei, he sha e o he new phase is
lowe han ha o non-de o med aus eni e, especially a highe cooling a es. The ole o disloca ion
on he ma ensi e s a empe a u e is mo e con o e sial. The la ge amoun o disloca ions
gene a ed by a la ge plas ic de o ma ion o aus eni e p io o he ma ensi e may s abilize he glissile
emb yo–aus eni e in e ace, leading o a dec ease in ma ensi e (Ms)- empe a u e ( empe a u e o
s a ing ma ensi e ans o ma ion). This is known as he disloca ion s abiliza ion mechanism.
Howe e , he e is some imes an opposi e phenomenon; accumula ed la ice de ec s ini ia e
ma ensi e o ma ion and enable i s o ma ion a highe empe a u es han in he case o
non-de o med aus eni e ans o ma ion. An example o his is he g aph in Figu e 4, which shows
ha he Ms empe a u e ises a e a heigh de o ma ion o 30% and 60% compa ed o he Ms
empe a u e o he unde o med specimens o selec ed s eels [18,23,24,29–36].
Figu e 4. In luence o he p e ious de o ma ion on ma ensi e (Ms) empe a u e in selec ed
low-alloyed s eels [23].
All diag am ypes can be cons uc ed on he basis o ma hema ical simula ions using
specialized p og ams (JMa PRO, QTS eel, e c.) o by physical es s on dila ome e s o dila ome ic
modules o uni e sal plas ome e s. In he case o he ma hema ical calcula ion o he diag ams,
he diag ams a e calcula ed on he basis o he equa ions compiled o he selec ed s eel chemical
composi ion ange, bu hei accu acy is no always op imal. Fo his eason, i is ce ainly mo e
app op ia e o design diag ams on he basis o dila ome ic es s ha a e pe o med on specimens o
speci ic quali ies [37–41].
The subjec o his a icle was o e alua e he in luence o he p e ious de o ma ion o wo
di e en ue s ains, loga i hmic de o ma ion (e = 0.35 and 1), on he cons uc ion o (D)CCT
diag ams o 100C 6 s eel, hus con ibu ing o he ex ension o knowledge o he aus eni e
ans o ma ion kine ics du ing cooling o he bea ing s eels. The 100C 6 s eel has good ho
o mabili y, is sui able o di ec quenching, and, in a so annealed condi ion, is easonably
machinable and sui able o componen s wi h a e y ha d and wea - esis an su ace. P ima ily, his
s eel is in ended o he p oduc ion o bea ing balls up o 25 mm in diame e , and olle s and ape
Figu e 4.
In luence o he p e ious de o ma ion on ma ensi e (Ms) empe a u e in selec ed low-alloyed
s eels [23].
All diag am ypes can be cons uc ed on he basis o ma hema ical simula ions using specialized
p og ams (JMa PRO, QTS eel, e c.) o by physical es s on dila ome e s o dila ome ic modules o
uni e sal plas ome e s. In he case o he ma hema ical calcula ion o he diag ams, he diag ams a e
calcula ed on he basis o he equa ions compiled o he selec ed s eel chemical composi ion ange,
bu hei accu acy is no always op imal. Fo his eason, i is ce ainly mo e app op ia e o design
diag ams on he basis o dila ome ic es s ha a e pe o med on specimens o speci ic quali ies [
37
–
41
].
C ys als 2020,10, 326 4 o 16
The subjec o his a icle was o e alua e he in luence o he p e ious de o ma ion o wo di e en
ue s ains, loga i hmic de o ma ion (e =0.35 and 1), on he cons uc ion o (D)CCT diag ams o
100C 6 s eel, hus con ibu ing o he ex ension o knowledge o he aus eni e ans o ma ion kine ics
du ing cooling o he bea ing s eels. The 100C 6 s eel has good ho o mabili y, is sui able o di ec
quenching, and, in a so annealed condi ion, is easonably machinable and sui able o componen s
wi h a e y ha d and wea - esis an su ace. P ima ily, his s eel is in ended o he p oduc ion o
bea ing balls up o 25 mm in diame e , and olle s and ape olle bea ings up o a 16 mm wall
hickness [
42
–
44
]. This expe imen was ealized in o de o e i y he e ec o he p e ious de o ma ion
on he inal s uc u e o he hype eu ec oid s eel.
2. Ma e ials and Me hods
As can be seen om he chemical composi ion o he 100C 6 s eel, which is p esen ed in Table 1,
i is a hype -eu ec oid high-ca bon and low-alloyed s eel.
Table 1. Chemical composi ion o in es iga ed 100C 6 s eel in w .%.
C Mn Si P S C
0.994 0.38 0.324 0.011 0.001 1.45
Fo he pu pose o he expe imen , simple cylind ical specimens wi h a diame e o 6 mm and
leng h o 86 mm we e p epa ed om he 100C 6 s eel. The ini ial s a e o he in es iga ed s eel was
de o med as i was p epa ed om he olled ods 12 mm in diame e .
The dila ome ic expe imen s we e pe o med wi h he use o he op ical dila ome ic module (The
Model 39112 Scanning Non-Con ac Op ical Dila ome e and Ex ensome e Sys em wi h G een LED
Technology (Dynamic Sys ems Inc., Poes enkill, NY, USA) o he Gleeble 3800 plas ome e . This op ical
dila ome ic module is based on he measu emen c oss-sec ion ( adial componen s o s ain) o
samples wi h a epea abili y o
±
0.3
µ
m by a equency o 2400 Hz wi h a maximum empe a u e o
1200 ◦C [18–20].
The i s s ep was o de e mine he empe a u es o A
c1
and A
cm
, which ep esen he empe a u es
o he ansi ion du ing hea ing. In his case, he specimen was hea ed a 5
◦
C/s o 500
◦
C, and he hea ing
a e was hen slowed down o 10
◦
C/min (0.167
◦
C/s) o loca e he ans o ma ion a ea. E alua ion o
he measu ed da a was ca ied ou using he semi-au oma ic CCT so wa e (Dynamic Sys ems Inc.,
Poes enkill, NY, USA), which uses he angen ial me hod in combina ion wi h he de i a ion o he
dila a ion cu e o de e mine he ans o ma ion empe a u es. The esul o his es is shown in
Figu e 5.
C ys als 2020, 10, x FOR PEER REVIEW 4 o 17
olle bea ings up o a 16 mm wall hickness [42–44]. This expe imen was ealized in o de o e i y
he e ec o he p e ious de o ma ion on he inal s uc u e o he hype eu ec oid s eel.
2. Ma e ials and Me hods
As can be seen om he chemical composi ion o he 100C 6 s eel, which is p esen ed in Table 1,
i is a hype -eu ec oid high-ca bon and low-alloyed s eel.
Table 1. Chemical composi ion o in es iga ed 100C 6 s eel in w .%.
C Mn Si P S C
0.994 0.38 0.324 0.011 0.001 1.45
Fo he pu pose o he expe imen , simple cylind ical specimens wi h a diame e o 6 mm and
leng h o 86 mm we e p epa ed om he 100C 6 s eel. The ini ial s a e o he in es iga ed s eel was
de o med as i was p epa ed om he olled ods 12 mm in diame e .
The dila ome ic expe imen s we e pe o med wi h he use o he op ical dila ome ic module
(The Model 39112 Scanning Non-Con ac Op ical Dila ome e and Ex ensome e Sys em wi h G een
LED Technology (Dynamic Sys ems Inc., Poes enkill, NY, USA) o he Gleeble 3800 plas ome e . This
op ical dila ome ic module is based on he measu emen c oss-sec ion ( adial componen s o s ain)
o samples wi h a epea abili y o ± 0.3 µm by a equency o 2400 Hz wi h a maximum empe a u e
o 1200 °C [18–20].
The i s s ep was o de e mine he empe a u es o A
c1
and A
cm
, which ep esen he
empe a u es o he ansi ion du ing hea ing. In his case, he specimen was hea ed a 5 °C/s o 500
°C, and he hea ing a e was hen slowed down o 10 °C/min (0.167 °C/s) o loca e he ans o ma ion
a ea. E alua ion o he measu ed da a was ca ied ou using he semi-au oma ic CCT so wa e
(Dynamic Sys ems Inc., Poes enkill, NY, USA), which uses he angen ial me hod in combina ion
wi h he de i a ion o he dila a ion cu e o de e mine he ans o ma ion empe a u es. The esul
o his es is shown in Figu e 5.
.
Figu e 5. De e mina ion o ans o ma ion empe a u es A
c1
and A
cm
du ing hea ing.
Based on he p e ious expe imen (i.e., de e mina ion o A
c1
and A
cm
empe a u es), o he
specimens we e uni o mly p ehea ed a 850 °C wi h a subsequen 10 min dwell a his empe a u e
in o de o cons uc (D)CCT diag ams. A e ha (in he case o he CCT diag am), he specimens
we e con inuously cooled o oom empe a u e by he cons an cooling a es in he ange o 0.2–150
°C/s. To achie e cooling a es abo e 25 °C/s, he specimens (wi h cooling a es o 60 and 150 °C/s =
only o cons uc ion o CCT diag am) had o ha e a special hollow-head s uc u e o high-speed
Figu e 5. De e mina ion o ans o ma ion empe a u es Ac1 and Acm du ing hea ing.
C ys als 2020,10, 326 5 o 16
Based on he p e ious expe imen (i.e., de e mina ion o A
c1
and A
cm
empe a u es),
o he specimens we e uni o mly p ehea ed a 850
◦
C wi h a subsequen 10 min dwell a his empe a u e
in o de o cons uc (D)CCT diag ams. A e ha (in he case o he CCT diag am), he specimens we e
con inuously cooled o oom empe a u e by he cons an cooling a es in he ange o 0.2–150
◦
C/s.
To achie e cooling a es abo e 25
◦
C/s, he specimens (wi h cooling a es o 60 and 150
◦
C/s=only o
cons uc ion o CCT diag am) had o ha e a special hollow-head s uc u e o high-speed cooling by
ai nozzles. Un o una ely, he disad an age o hese specially designed specimens is he inabili y o
pe o m a de o ma ion [
45
,
46
]. The empe a u e o hea ing a 850
◦
C is no mal o he cons uc ion o
CCT diag ams o 100C 6 s eel [42–44,47,48].
In he case o he cons uc ion o bo h a ian s o DCCT diag ams, he con inuous cooling was
p eceded by he uniaxial comp ession de o ma ion, which was execu ed di ec ly a e he dwell a
he aus eni iza ion empe a u e. The magni ude o he ue (loga i hmic) de o ma ion in he i s and
second case was equal o 0.35 and 1, espec i ely. In bo h cases, he de o ma ion was pe o med a he
s ain a e o 1/s. The limi ing elemen in he case o he cons uc ion o he DCCT diag ams was he
c ea ion o specimens ha could allow a maximum cooling a e o 35
◦
C/s o be achie ed [
45
] a e he
p e ious de o ma ion; hus, in bo h cases o DCCT diag ams, he cooling a es we e selec ed in he
ange o 0.2–35 ◦C/s.
Examples o dila ome ically es ed specimens wi hou de o ma ion and wi h he de o ma ion o
0.35 and 1 a e gi en in Figu e 6.
C ys als 2020, 10, x FOR PEER REVIEW 5 o 17
cooling by ai nozzles. Un o una ely, he disad an age o hese specially designed specimens is he
inabili y o pe o m a de o ma ion [45,46]. The empe a u e o hea ing a 850 °C is no mal o he
cons uc ion o CCT diag ams o 100C 6 s eel [42–44,47,48].
In he case o he cons uc ion o bo h a ian s o DCCT diag ams, he con inuous cooling was
p eceded by he uniaxial comp ession de o ma ion, which was execu ed di ec ly a e he dwell a
he aus eni iza ion empe a u e. The magni ude o he ue (loga i hmic) de o ma ion in he i s and
second case was equal o 0.35 and 1, espec i ely. In bo h cases, he de o ma ion was pe o med a
he s ain a e o 1/s. The limi ing elemen in he case o he cons uc ion o he DCCT diag ams was
he c ea ion o specimens ha could allow a maximum cooling a e o 35 °C/s o be achie ed [45]
a e he p e ious de o ma ion; hus, in bo h cases o DCCT diag ams, he cooling a es we e
selec ed in he ange o 0.2–35 °C/s.
Examples o dila ome ically es ed specimens wi hou de o ma ion and wi h he de o ma ion
o 0.35 and 1 a e gi en in Figu e 6.
Figu e 6. Examples o es ed specimens wi hou de o ma ion and a e he de o ma ion o 0.35 and 1.
The ob ained esul s we e compa ed o me allog aphic analyses—scanning elec on
mic oscopy (SEM), ligh -mic oscopy, and HV30 ha dness measu emen . Samples in ended o
me allog aphic analysis ha e been p epa ed by means o mechanical g inding and polishing. The
mic os uc u e was e ealed ia e ching in he 2% pic ic acid solu ion [20].
As men ioned in he in oduc ion, ans o ma ion o aus eni e depends on he size o aus eni ic
g ains as well; he e o e, o e e y (D)CCT diag am besides chemical composi ion and o he
he momechanical pa ame e s, i should be men ioned o wha size o aus eni ic g ains his
ans o ma ion diag am is alid. The e o e, he in es iga ed s eel was es ed o de e mina ion o he
a e age size o aus eni ic g ains (AGS). O he hea ing pa ame e s, like he hea ing a e and
empe a u e dwell ime, we e he same as in he case o he dila ome ic expe imen , excep he ac
ha ins ead o de o ma ion a e he dwell ime, he samples we e di ec ly wa e -quenched o ix he
o igin aus eni ic s uc u e. The scheme o his hea - ea men expe imen is e iden om Figu e 7a.
In o de o e alua e he aus eni ic g ain size, classical op ical me allog aphy has been applied when
using he me hod o o igin-aus eni ic-g ain e ealing. The esul ing mic os uc u e o his addi ional
expe imen is included in Figu e 7b. I was ound ha all 3 ans o ma ion diag ams, which a e
p esen ed in his a icle, we e cons uc ed o AGS = 9.8 µm. AGS was e alua ed by he means o he
specialized so wa e, Quick PHOTO INDUSTRIAL 3.2 (PROMICRA s. .o., P ague, Czech Republic).
Figu e 6.
Examples o es ed specimens wi hou de o ma ion and a e he de o ma ion o 0.35 and 1.
The ob ained esul s we e compa ed o me allog aphic analyses—scanning elec on mic oscopy
(SEM), ligh -mic oscopy, and HV30 ha dness measu emen . Samples in ended o me allog aphic
analysis ha e been p epa ed by means o mechanical g inding and polishing. The mic os uc u e was
e ealed ia e ching in he 2% pic ic acid solu ion [20].
As men ioned in he in oduc ion, ans o ma ion o aus eni e depends on he size o aus eni ic
g ains as well; he e o e, o e e y (D)CCT diag am besides chemical composi ion and o he
he momechanical pa ame e s, i should be men ioned o wha size o aus eni ic g ains his
ans o ma ion diag am is alid. The e o e, he in es iga ed s eel was es ed o de e mina ion
o he a e age size o aus eni ic g ains (AGS). O he hea ing pa ame e s, like he hea ing a e and
empe a u e dwell ime, we e he same as in he case o he dila ome ic expe imen , excep he ac ha
ins ead o de o ma ion a e he dwell ime, he samples we e di ec ly wa e -quenched o ix he o igin
aus eni ic s uc u e. The scheme o his hea - ea men expe imen is e iden om Figu e 7a. In o de
o e alua e he aus eni ic g ain size, classical op ical me allog aphy has been applied when using he
me hod o o igin-aus eni ic-g ain e ealing. The esul ing mic os uc u e o his addi ional expe imen
is included in Figu e 7b. I was ound ha all 3 ans o ma ion diag ams, which a e p esen ed in
his a icle, we e cons uc ed o AGS =9.8
µ
m. AGS was e alua ed by he means o he specialized
so wa e, Quick PHOTO INDUSTRIAL 3.2 (PROMICRA s. .o., P ague, Czech Republic).
C ys als 2020,10, 326 6 o 16
C ys als 2020, 10, x FOR PEER REVIEW 6 o 17
(a) (b)
Figu e 7. The analysis o he in luence o empe a u e on he aus eni ic g ain size o he 100C 6 s eel.
(a) scheme o aus eni ic g ain size (AGS) expe imen ; (b) Mic os uc u e o aus eni e, AGS = 9.8 µm.
3. Resul s and Discussion
3.1. CCT Diag am
As he in es iga ed s eel is o hype -eu ec oid ype, only aus eni e
–
pea li e and aus eni e
–
ma ensi e ans o ma ions we e dila ome ically de ec ed and localized. The example o he
dila a ion cu es wi h he localized ans o ma ion empe a u es is gi en in Figu e 8.
Figu e 8. Selec ed examples o dila a ion cu es, including de e mina ion o ans o ma ion poin s
by use o he angen ial me hod.
Based on he analysis o he dila a ion cu es, he CCT diag am has been compiled (see Figu e
9). The cons uc ed CCT diag am consis s o only he pea li ic and ma ensi ic egions. O he
s uc u al componen s de ec ed in he samples o he in es iga ed s eel we e ca bides, which do no
ans o m ei he du ing hea ing o du ing cooling. I is clea ha he aus eni e is ans o med o
pea li e a cooling a es up o 18 °C/s. The ans o ma ion o aus eni e o ma ensi e p oceeds abo e
he cooling a e o 12 °C/s.
Figu e 7.
The analysis o he in luence o empe a u e on he aus eni ic g ain size o he 100C 6 s eel.
(a) scheme o aus eni ic g ain size (AGS) expe imen ; (b) Mic os uc u e o aus eni e, AGS =9.8 µm.
3. Resul s and Discussion
3.1. CCT Diag am
As he in es iga ed s eel is o hype -eu ec oid ype, only aus eni e–pea li e and aus eni e–
ma ensi e ans o ma ions we e dila ome ically de ec ed and localized. The example o he dila a ion
cu es wi h he localized ans o ma ion empe a u es is gi en in Figu e 8.
C ys als 2020, 10, x FOR PEER REVIEW 6 o 17
(a) (b)
Figu e 7. The analysis o he in luence o empe a u e on he aus eni ic g ain size o he 100C 6 s eel.
(a) scheme o aus eni ic g ain size (AGS) expe imen ; (b) Mic os uc u e o aus eni e, AGS = 9.8 µm.
3. Resul s and Discussion
3.1. CCT Diag am
As he in es iga ed s eel is o hype -eu ec oid ype, only aus eni e
–
pea li e and aus eni e
–
ma ensi e ans o ma ions we e dila ome ically de ec ed and localized. The example o he
dila a ion cu es wi h he localized ans o ma ion empe a u es is gi en in Figu e 8.
Figu e 8. Selec ed examples o dila a ion cu es, including de e mina ion o ans o ma ion poin s
by use o he angen ial me hod.
Based on he analysis o he dila a ion cu es, he CCT diag am has been compiled (see Figu e
9). The cons uc ed CCT diag am consis s o only he pea li ic and ma ensi ic egions. O he
s uc u al componen s de ec ed in he samples o he in es iga ed s eel we e ca bides, which do no
ans o m ei he du ing hea ing o du ing cooling. I is clea ha he aus eni e is ans o med o
pea li e a cooling a es up o 18 °C/s. The ans o ma ion o aus eni e o ma ensi e p oceeds abo e
he cooling a e o 12 °C/s.
Figu e 8.
Selec ed examples o dila a ion cu es, including de e mina ion o ans o ma ion poin s by
use o he angen ial me hod.
Based on he analysis o he dila a ion cu es, he CCT diag am has been compiled (see Figu e 9).
The cons uc ed CCT diag am consis s o only he pea li ic and ma ensi ic egions. O he s uc u al
componen s de ec ed in he samples o he in es iga ed s eel we e ca bides, which do no ans o m
ei he du ing hea ing o du ing cooling. I is clea ha he aus eni e is ans o med o pea li e a
cooling a es up o 18
◦
C/s. The ans o ma ion o aus eni e o ma ensi e p oceeds abo e he cooling
a e o 12 ◦C/s.
C ys als 2020,10, 326 7 o 16
C ys als 2020, 10, x FOR PEER REVIEW 7 o 17
Figu e 9. Con inuously cooling ans o ma ion (CCT) diag am o he 100C 6 s eel.
The cons uc ed CCT diag am was compa ed o a scanning elec on mic oscopy (SEM) and
HV30 ha dness measu emen . The mic os uc u e o he non-de o med s a e has been documen ed
a ou selec ed cooling a es, namely 1, 12, 25, and 150 °C/s (Figu e 10a–d).
(a) 150 °C/s—M + C + RA (b) 25 °C/s—T(P) + M + C
(c) 12 °C/s—T(P) + M + C (d) 1 °C/s—P + C
Figu e 10. SEM mic os uc u es o selec ed samples, wi hou de o ma ion. M, ma ensi e; C,
ca bides; P, pea li e; T(P), oos i e; RA, e ained aus eni e.
Figu e 9. Con inuously cooling ans o ma ion (CCT) diag am o he 100C 6 s eel.
The cons uc ed CCT diag am was compa ed o a scanning elec on mic oscopy (SEM) and HV30
ha dness measu emen . The mic os uc u e o he non-de o med s a e has been documen ed a ou
selec ed cooling a es, namely 1, 12, 25, and 150 ◦C/s (Figu e 10a–d).
C ys als 2020, 10, x FOR PEER REVIEW 7 o 17
Figu e 9. Con inuously cooling ans o ma ion (CCT) diag am o he 100C 6 s eel.
The cons uc ed CCT diag am was compa ed o a scanning elec on mic oscopy (SEM) and
HV30 ha dness measu emen . The mic os uc u e o he non-de o med s a e has been documen ed
a ou selec ed cooling a es, namely 1, 12, 25, and 150 °C/s (Figu e 10a–d).
(a) 150 °C/s—M + C + RA (b) 25 °C/s—T(P) + M + C
(c) 12 °C/s—T(P) + M + C (d) 1 °C/s—P + C
Figu e 10. SEM mic os uc u es o selec ed samples, wi hou de o ma ion. M, ma ensi e; C,
ca bides; P, pea li e; T(P), oos i e; RA, e ained aus eni e.
Figu e 10.
SEM mic os uc u es o selec ed samples, wi hou de o ma ion. M, ma ensi e; C, ca bides;
P, pea li e; T(P), oos i e; RA, e ained aus eni e.
The p esence o e ained aus eni e was con i med by X- ay di ac ion analysis ha was pe o med
using a Co K
α
sou ce (
λ
=0.17902 nm) by means o he B uke -AXS D8 (B uke GmbH, Ka ls uhe,
Ge many) Ad ance appa a us. The specimen wi h a cooling a e o 150
◦
C/s (Figu e 10a) con ained
app oxima ely 6.3% o e ained aus eni e (RA).
C ys als 2020,10, 326 8 o 16
The mic os uc u e o pea li ic blocks can be conside ed ine-g ained wi h he a e age size o
pea li ic blocks o abou 6
µ
m. Fo measu emen o he size o pea li ic blocks (g ains), specialized
so wa e Quick PHOTO INDUSTRIAL (PROMICRA s. .o., P ague, Czech Republic) was used, as well
as in he de e mina ion o AGS.
In all cases, ca bides o di e en sizes om pa icles smalle han 0.1
µ
m o pa icles eaching
up o a ound 1
µ
m we e obse ed in he mic os uc u e. This con i ms ha he s uc u e o he s eel
a he end o he hea ing dwell consis ed o he aus eni e and ca bides. The mic os uc u e o he
sample, which was cooled by he a e o 1
◦
C/s, consis s o lamella pea li e P and ca bides (Figu e 10d).
P ecipi a ion o ine ca bides C along he bounda ies o o me aus eni ic g ains was obse ed only
o a e y small ex en . The mic os uc u e o he samples, which we e cooled by he in e media e
a es, 12 and 25
◦
C/s, consis s o pea li e. Wi h espec o an in e -lamella dis ance and o ien a ion o
pea li ic colonies, he mo phology o his pea li e can be iden i ied as oos i e T(P) [
49
] (Figu e 10b,c).
The s uc u e o hese samples also con ains ma ensi e M, whose amoun ises wi h he cooling a e.
Ca bides we e obse ed in hese s uc u es as well. The sample cooled by he high a e o 150
◦
C/s
(Figu e 10a) consis s o he mic os uc u e ha is gi en only by ma ensi e wi h a ce ain sha e o
e ained aus eni e RA (see small da ke a eas in Figu e 10a) and ca bides.
By compa ing he expe imen ally ob ained CCT diag am (Figu e 9) o he simila diag ams
ob ained om a ailable li e a u e (Figu es 11 and 12) [
41
,
49
–
51
], i is qui e clea ha he basic di e ence
be ween he compa ed diag ams is he absence o baini e in he expe imen ally ob ained diag am
(Figu e 9), which was con i med by he me allog aphic analyses—see Figu e 10. This inding could be
caused by he inc eased con en o Si in he in es iga ed s eel, which is, in his case, nea maximum o
his g ade o bea ing s eel. I is known ha in he case o high-ca bon s eels wi h inc easing con en o
Si, he kine ics o baini ic ans o ma ion slows down [51–54].
C ys als 2020, 10, x FOR PEER REVIEW 8 o 17
The p esence o e ained aus eni e was con i med by X- ay di ac ion analysis ha was
pe o med using a Co Kα sou ce (λ = 0.17902 nm) by means o he B uke -AXS D8 (B uke GmbH,
Ka ls uhe, Ge many) Ad ance appa a us. The specimen wi h a cooling a e o 150 °C/s (Figu e 10a)
con ained app oxima ely 6.3% o e ained aus eni e (RA).
The mic os uc u e o pea li ic blocks can be conside ed ine-g ained wi h he a e age size o
pea li ic blocks o abou 6 µm. Fo measu emen o he size o pea li ic blocks (g ains), specialized
so wa e Quick PHOTO INDUSTRIAL (PROMICRA s. .o., P ague, Czech Republic) was used, as
well as in he de e mina ion o AGS.
In all cases, ca bides o di e en sizes om pa icles smalle han 0.1 µm o pa icles eaching
up o a ound 1 µm we e obse ed in he mic os uc u e. This con i ms ha he s uc u e o he s eel
a he end o he hea ing dwell consis ed o he aus eni e and ca bides. The mic os uc u e o he
sample, which was cooled by he a e o 1 °C/s, consis s o lamella pea li e P and ca bides (Figu e
10d). P ecipi a ion o ine ca bides C along he bounda ies o o me aus eni ic g ains was obse ed
only o a e y small ex en . The mic os uc u e o he samples, which we e cooled by he
in e media e a es, 12 and 25 °C/s, consis s o pea li e. Wi h espec o an in e -lamella dis ance and
o ien a ion o pea li ic colonies, he mo phology o his pea li e can be iden i ied as oos i e T(P)
[49] (Figu e 10 b,c). The s uc u e o hese samples also con ains ma ensi e M, whose amoun ises
wi h he cooling a e. Ca bides we e obse ed in hese s uc u es as well. The sample cooled by he
high a e o 150 °C/s (Figu e 10a) consis s o he mic os uc u e ha is gi en only by ma ensi e wi h
a ce ain sha e o e ained aus eni e RA (see small da ke a eas in Figu e 10a) and ca bides.
By compa ing he expe imen ally ob ained CCT diag am (Figu e 9) o he simila diag ams
ob ained om a ailable li e a u e (Figu es 11 and 12) [41,49
–
51], i is qui e clea ha he basic
di e ence be ween he compa ed diag ams is he absence o baini e in he expe imen ally ob ained
diag am (Figu e 9), which was con i med by he me allog aphic analyses—see Figu e 10. This
inding could be caused by he inc eased con en o Si in he in es iga ed s eel, which is, in his case,
nea maximum o his g ade o bea ing s eel. I is known ha in he case o high-ca bon s eels wi h
inc easing con en o Si, he kine ics o baini ic ans o ma ion slows down [51
–
54].
F om he poin o iew o he localiza ion o he pea li ic ans o ma ion and he empe a u e o
he beginning o ma ensi e o ma ion on he empe a u e axis, he e was a good ma ch. A good
ma ch was also ob ained when compa ing all h ee CCT diag ams, namely he ime domain o
pea li e o ma ion, also aking in o accoun sligh ly di e en empe a u es o aus eni iza ion (850 °C
s. 860 °C).
Howe e , ma ensi e appea ed in he s uc u e a a cooling a e o 12 °C/s, which is a highe a e
han in he case o he compa ed CCT diag ams om he li e a u e.
Figu e 11. CCT diag am o 100C 6 s eel—acco ding o [51].
C ys als 2020, 10, x FOR PEER REVIEW 9 o 17
Figu e 11. CCT diag am o 100C 6
s eel—acco ding o [51].
Figu e 12. CCT diag am o 100C 6
s eel—acco ding o [42].
3.2. DCCT Diag am – De o ma ion e = 0.35
While i is possible o encoun e a la ge numbe o CCT diag ams o he in es iga ed 100C 6
s eel in he li e a u e [42
–
44,51–54], he e is a minimum o in o ma ion abou he e ec o p io
de o ma ion on his s eel. In he case o he p esen ed esea ch, he in es iga ed s eel was
dila ome ically es ed a e wo le els o he p e ious de o ma ion. The DCCT diag am in Figu e 13
documen s he in luence o he p e ious de o ma ion o e = 0.35.
Only he aus eni e
–
pea li e and aus eni e
–
ma ensi e ans o ma ions we e ound in his DCCT
diag am (Figu e 13). Howe e , i is e iden ha he p e ious de o ma ion accele a ed he pea li ic
ans o ma ion; in o he wo ds, due o he p e ious de o ma ion, he pea li ic nose has been shi ed
o he le , i.e., o sho e imes and hus o highe cooling a es— om 18 °C/s (maximum o CCT
diag am) o 35 °C/s. The ma ensi ic ans o ma ion was in luenced by he p e ious de o ma ion in
he sense o lowe ing he ma ensi e-s a empe a u e by app oxima ely 50 °C ( om 220 °C o CCT
o 170 °C o DCCT 0.35).
.
Figu e 13. De o ma ion con inuously cooling ans o ma ion (DCCT) diag am o he 100C 6
s eel—a e he de o ma ion o e = 0.35.
Figu e 12. CCT diag am o 100C 6 s eel—acco ding o [42].
C ys als 2020,10, 326 9 o 16
F om he poin o iew o he localiza ion o he pea li ic ans o ma ion and he empe a u e
o he beginning o ma ensi e o ma ion on he empe a u e axis, he e was a good ma ch. A good
ma ch was also ob ained when compa ing all h ee CCT diag ams, namely he ime domain o pea li e
o ma ion, also aking in o accoun sligh ly di e en empe a u es o aus eni iza ion (850
◦
C s. 860
◦
C).
Howe e , ma ensi e appea ed in he s uc u e a a cooling a e o 12
◦
C/s, which is a highe a e
han in he case o he compa ed CCT diag ams om he li e a u e.
3.2. DCCT Diag am—De o ma ion e =0.35
While i is possible o encoun e a la ge numbe o CCT diag ams o he in es iga ed 100C 6 s eel
in he li e a u e [
42
–
44
,
51
–
54
], he e is a minimum o in o ma ion abou he e ec o p io de o ma ion
on his s eel. In he case o he p esen ed esea ch, he in es iga ed s eel was dila ome ically es ed
a e wo le els o he p e ious de o ma ion. The DCCT diag am in Figu e 13 documen s he in luence
o he p e ious de o ma ion o e =0.35.
C ys als 2020, 10, x FOR PEER REVIEW 9 o 17
Figu e 11. CCT diag am o 100C 6
s eel—acco ding o [51].
Figu e 12. CCT diag am o 100C 6
s eel—acco ding o [42].
3.2. DCCT Diag am – De o ma ion e = 0.35
While i is possible o encoun e a la ge numbe o CCT diag ams o he in es iga ed 100C 6
s eel in he li e a u e [42
–
44,51–54], he e is a minimum o in o ma ion abou he e ec o p io
de o ma ion on his s eel. In he case o he p esen ed esea ch, he in es iga ed s eel was
dila ome ically es ed a e wo le els o he p e ious de o ma ion. The DCCT diag am in Figu e 13
documen s he in luence o he p e ious de o ma ion o e = 0.35.
Only he aus eni e
–
pea li e and aus eni e
–
ma ensi e ans o ma ions we e ound in his DCCT
diag am (Figu e 13). Howe e , i is e iden ha he p e ious de o ma ion accele a ed he pea li ic
ans o ma ion; in o he wo ds, due o he p e ious de o ma ion, he pea li ic nose has been shi ed
o he le , i.e., o sho e imes and hus o highe cooling a es— om 18 °C/s (maximum o CCT
diag am) o 35 °C/s. The ma ensi ic ans o ma ion was in luenced by he p e ious de o ma ion in
he sense o lowe ing he ma ensi e-s a empe a u e by app oxima ely 50 °C ( om 220 °C o CCT
o 170 °C o DCCT 0.35).
.
Figu e 13. De o ma ion con inuously cooling ans o ma ion (DCCT) diag am o he 100C 6
s eel—a e he de o ma ion o e = 0.35.
Figu e 13.
De o ma ion con inuously cooling ans o ma ion (DCCT) diag am o he 100C 6 s eel—a e
he de o ma ion o e =0.35.
Only he aus eni e–pea li e and aus eni e–ma ensi e ans o ma ions we e ound in his DCCT
diag am (Figu e 13). Howe e , i is e iden ha he p e ious de o ma ion accele a ed he pea li ic
ans o ma ion; in o he wo ds, due o he p e ious de o ma ion, he pea li ic nose has been shi ed
o he le , i.e., o sho e imes and hus o highe cooling a es— om 18
◦
C/s (maximum o CCT
diag am) o 35
◦
C/s. The ma ensi ic ans o ma ion was in luenced by he p e ious de o ma ion in
he sense o lowe ing he ma ensi e-s a empe a u e by app oxima ely 50
◦
C ( om 220
◦
C o CCT
o 170 ◦C o DCCT 0.35).
In o de o ob ain a comple ely ma ensi ic-ca bidic s uc u e, i was necessa y o quench he
specimens a e he de o ma ion by he use o wa e je s. This, howe e , makes i impossible o ins all
he dila ome ic module. The cou se o quenching a e he 0.35 de o ma ion is shown in Figu e 14.
The cooling a e be ween 810 ◦C and 100 ◦C was close o 3500 ◦C/s.
The mic os uc u e o all samples ha we e de o med by he s ain o 0.35 was obse ed by
ligh -mic oscopy and SEM me hods (Figu e 15). Obse ed mic os uc u es coincided wi h hose
desc ibed abo e o he ma e ial s a e wi hou de o ma ion. An inc eased oos i e sha e a he expense
o ma ensi e was obse ed in he case o de o med samples, which we e cooled by in e media e a es.
Documen a ion ia he SEM me hod has been pe o med only in he case o he sample, which was
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