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EffectofThermoPlasticTreatmenton
StructureandCorrosionPropertiesofHigh
NitrogenCrSteelsVeraV.Berezovskaya
Instituteofmaterialscienceandmetallurgy,UralFederalUniversitynamedafterthefirstPresidentofRussiaB.N.
Yeltsin/Professor
ul.Mira,19,Yekaterinburg,620002,Russia
AbstractEffectofagingonstructureandcorrosionpropertiesinhighstrength austenitic Crsteels alloying with nitrogen Cr21N1
andCr18Ni2N1hasbeeninvestigated.Structureofthesteels
and kinetics of austenite decomposition during the
treatment was studiedby Xray diffraction, TEManalyses
and electric resistance measurements. The highest valuesof
strength, micro hardness, corrosion rate and relative
strength reduction as far as brittle intergranular fracture
wereobservedattheearlystageofaustenitedecomposition
at the aging. The formation of nitrides CrN as well
martensitestressinducedtookplaceinthesteels.According
to resistormeter investigationsofnitrogen steelsincompare
withcarbonsteelCr18C1attheearlystageofaging(350C)the metastable ordered clusters enriched with chromium
and nitrogen were formed. Growths of aging temperature
up to 500C led to dissolve the carbides or nitridesbut at
600 C discontinuous precipitations were observed nearby
thegrainboundaries.
Effectofagingcombinedwithcoldplasticdeformation(CPD)
at an 824 % reductionby two schemes,before and after
aging at 350C, on structure and related corrosion
propertiesofsteelCr18Ni2N1hasbeenstudied.CPDatan8
12 % reductionbefore aging at 350C was shown to thrice
decreasing of corrosion rate of the steel as compared to the
undeformed state.A thermoplastic treatmentby thesecondscheme with using CPD at an 20% reduction after aging at
350 C is found to be more effective: the corrosion rate
decreased by an order and strength reduction decreased
morethanbyfourfoldascomparedtotheundeformedstate.
KeywordsAustenite Decomposition; Ordered Clusters; StressMartensite;
Lattice Parameter; Stress Corrosion Cracking; Cold Plastic
Deformation.
Introduction
Highnitrogensteels(HNS)duetotheirmorestrength
and corrosion resistant than in other austenitic steels
with carbon are widely used in power machine
building,shipbuildingandotherfieldsofengineering.In the nearest future [19] after perfecting their
manufacturing technology they are expected willbe
applied in abigger industrial scale. One of the main
directions of investigations to solve these problems is
searching a way to increase their resistance to stress
corrosioncracking(SCC)bothbyefficientalloyingand
optimizationofstrengtheningprocedure.
Well known that nitrogen includes a significant
contribution in hardening of solid solution and grain
boundaries as well as in strain and precipitation
hardening. According to data from work [2],
realization of these factors at appropriate degree of
coldplasticdeformation(CPD)canprovideextremely
high strength for this class of steels up to 3600 MPa.
However in a certain structural state they are
subjected to SCC in corrosive environment [10, 11] so
in this case expedient to use them after strengthening
notmorethenupto0.2=1400MPa.
Materials and Procedure
The highstrength lowcarbon steels with highnitrogen content (0.91.0%) Cr21N1 and Cr18Ni2N1
have been investigated to study mechanism and
kinetics of austenite decomposition and clearing up
CPD influence on structure and corrosion properties
of steels. Kinetics of decomposition of the
oversaturatedsolidsolutioninHNSwascarriedout
as compared with high carbon steel Cr18C1. Their
chemicalcompositionispresentedinTable1,firsttwo
of them were producedby nitrogen pressure casting,
homogenization at 1250 C and rolling with further
quenching in water afterbeing exposed for one and
half an hour at 1200 C. The high carbon steel was
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manufacturedby standard technology and quenched
from the same temperature in oil to put the austenite
structure. The specimens prepared for testing were
agedat300500Cfortwohoursandat600Cforan
hour.
TABLEICHEMICALCOMPOSITIONOFSTEELS
The general corrosion and SCC tests were performed
ina3.5%NaClaqueoussolutionasitdescribedinthe
work [10]. Fractographic studies of fracture surface
after SCC were examined on a JSM35C scanning
electronmicroscopeandmetallographicexamination
onaNeophot32opticalmicroscope.
Theelectricresistancemeasurementswerecarriedout
to investigate the kinetics of solid solution
decomposition [12]. Xray diffraction analysis was
carried out on a DRON3 diffractometer with cobalt
radiation and a radiation filter. The austenite andmartensitecontentsinthesteelswereestimatedusing
the method of homologous pairs by comparing the
integratedintensitiesofthe(110)and(111)lines[13].
The structure of austenite and the type, morphology,
and size of additional phases were investigated by
transmission electron microscopy on an EMV100L
electronmicroscope.
Results and Discussion
Mechanical properties of high nitrogen steels werefollowing: yield strength (0.2) is 650 and 610 MPa;
specific elongation () is 21 and 18% after quenching
and0.2=780 and 820 MPa; =5 and 9% in aged state
respectively in Cr21N1 and Cr18Ni2N1 steels. The
highest growth of strength, corrosion rate and
susceptibilitytoSCCin3.5%NaClwasobservedafter
aging at 350 C [14]. The fracture of specimens was
brittle and intergranular in this case (Fig. 1, a) while
the destruction was not associated with nitrides,
located along the grainboundaries. After overaging
the resistance to SCC increased and the intergranularfracture was replaced to quasicleavage including
related to colonies of discontinuous decomposition of
solid solution (Fig. 1,b). Theinvestigatedsteels had
a good passivity in all structural states due to high
contentofchromiuminsolidsolution,howeveratthe
stage of active corrosion the sharp acceleration of
corrosion was observed after aging at 350 C ininvestigatedsteels(Table2,line2).
FIG.1FRACTURESURFACEAFTERSCCOFCR18NI2N1STEEL
SUBJECTEDOFAGINGAT350(a)AND600C(b)
After quenching from 1200 C an austenite and
carbideswithsurfacemartensite werenotedincarbon
steel as well as in nitrogen steels (Fig. 2, a,b). The
structure of high nitrogen steels varied with rising of
aging temperature identically with some more
stability of austenite in nickelfree steel. The
microstructure of nitrogen steels aged at 350 C was
almost similar to quenched one (Fig. 2, c),but after
agingat600Citwasratherdifferent(Fig.2,d).
Martensitesoftwomorphologieswithdifferentlattice
parameters aT=0.287 nm and a=0.291 nm was
discovered in steel Cr18Ni2N1. As it was shown
earlier [15] it was the thin dispersive martensite (T)
onthegrainboundariesandannealingtwins(Fig.2,b,
c) and lensformed stressinduced martensite () in
the middle of grain (Fig.2, d), which formed
respectively from austenite depleted and enriched
with chromium and nitrogen. The same picture was
found after SCC. The results of Xray diffractionanalysesareshowninTable2.
Steel
grade
Contentinthesteel,wt%
C N Mn Si P S Cr Ni
Cr21N1 0.020 1.021 0.19 0.42 0.015 0.010 21.45
Cr18Ni2N1 0.008 0.899 0.30 0.27 0.020 0.010 17.86 2.00
Cr18C1 0.920 0.63 0.79 0.025 0.023 18.30
30 m
15 m b
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TABLEIIPHASECOMPOSITIONANDCORROSIONPROPERTIESOFTHECR18NI2N1STEELAFTERVARIOUSTREATMENT
of
treatmentSchemeoftreatment
Contentofphases,%*
m,
g/m2h st,%Intheinitialstate AtthesurfaceoffractureafterSCC
AgingwithoutCPD
1 Quenchingfrom1200 95 5 0 62 26 12 2,0 352 1200 +350,2h 95 5 0 58 22 20 30,0 37
3 1200 +400 95 5 0 62 22 16 8,0 34
4 1200 +600 50 44 6 28 64 8 1,0 29
5 1200 +700 0 100 0 0 100 0 0,5 21
CPD
before
aging
6 1200 +8%CPD+350,2h 89 5 6 10,0
7 1200 +12%CPD+350,2h 87 5 8 11,0
8 1200 +20%CPD+350,2h 50 15 35 40 15 45 55,0 42
9 1200 +24%CPD+350,2h 80 7 13 50,0
10 1200 +20%CPD 95 5 0 0,3
CPD
afteraging 11 1200 +350,2h+20%CPD 95 5 0 95 5 0 2,5 10
12 1200 +400 +20%CPD 95 5 0 0,3
13 1200 +600 +20%CPD 50 50 0 0,8
14 1200 +700 +20%CPD 0 100 0 0,4
*Withoutexcessphases.
FIG.2 ICROSTRUCTUREOFSTEELSCR18C1(),CR21N1(B)QUENCHEDANDCR18NI2N1(C,D)AGEDAT350AND600C
30 m
30 m d
c30 m
20 m b
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According to comparison of SCC tests and Xray
diffractionresultsthecorrelationbetweenthevalueof
relative strength reduction (/K) and quantity of
stressinduced martensite, formed directly during the
tests, is observed in high nitrogen steels. Thebiggest
portionofmartensiteinstructureofsteelwasnotedafteragingat350C.
By transmission electron microscopy of thin foils the
evolution of structure in steel Cr18Ni2N1 under the
aging was studied. The structure of quenching steel
consisted of austenite (Fig. 3, ac), ratherbig particles
ofnitridesCr2Nretainedafterheatingalongthegrain
boundaries and not more than 5% of Tphase as a
result of martensitic transformation in depleted
austenite near the nitrides (Fig. 3, df). The nitride
Cr2Nhasahexagonalcrystallinestructurewithlattice
parametersa=0.4805nm,c=0.4480nm. Thecrystalsof
surface martensite formed at electrolytic polishing of
foilcouldbeseenaswell(Fig. 3,g).
After aging at 350 and 400Cbesides andphase
ultra dispersive nitrides CrN with FCC crystalline
ordered structure and lattice parameteraCrN=0.415 nm
formed from a supersaturated solid solution due to
homogeneous isomorphic decomposition were
observed (Fig.4,ac). The crystals of martensite
were found as well. Both phases CrN and were
noticednearbytheextinctioncontoursintheplacesoffoilbending(Fig. 4, df). After 2hour aging at 500C
besides Tphase in the settlement of discontinuous
decompositiononthegrainboundaries(Fig.5,ac)the
singlecrystalsofmartensitewerediscovered(Fig.5,
d). At temperature 600 C fresh portions of
discontinuousdecompositionsettlementsconsistingof
nitridesCr2NandTmartensitewasobserved(Fig.6).
The electric resistance of the steels Cr21N1,
Cr18Ni2N1 and Cr18C1 has been measured
depending on time of aging in isothermal conditions
at 300, 400 and 500 C (Fig. 7). These dependences
wereshowntobethesameforhighnitrogenandhigh
carbonsteels.Attheinitialstagesofprocess(36h)we
can see a sharp electric resistance decrease which
becomesbigger as the temperature of aging grows.
The effect of aging depends on a super saturation
degreebyinterstitialatomsofaustenitequenchedbut
at the same content of carbon and nitrogen (about
0.9%) its displayed stronger in high nitrogen steels.
Withtheincreasingofthetemperatureatthisstageof
aging a differencebetween the curves reduced and
they practically coincided at 500 C. The stress
recoveryattheheatingwasresponsiblefordecreaseof
electricresistanceofthesteels(sharpdecreaseofR/R
preagingstage).
At a longer time of heating it was an increase of
electric resistance most pronounced at 300C. This
stage continued not more than 7 hours at 300 C, 4
hoursat400Cand1hourat500Candassociatedwith the separation of the solid solution with
chromium (as well carbon in carbon steel) during
these exposuresbecause of the conductivity electrons
are scatteredby these enriched in chromium clusters
[16](sharpincreaseofR/Rstage1).
Longer aging influenced on the curves character
differently depending on the temperature of aging. It
is necessary notice a stabilizing of decomposition of
austenite in carbon steel at 300 and 400 C and in
nitrogensteels
only
at
300
C.
It
is
connected
with
the
formingofcarbidesincarbonsteel,butnotcompleting
of nitrides formation in nitrogen steels. It needs to
continue the heatingand further slow increasing of
electric resistance which observed at 400 C in these
steels confirmed it. This process associated with the
orderinginchromiumenrichedclusterswithnitrogen
that was able at an exposure at this temperature or
understresses(nearbytheextinctioncontoursFig.4,
a) if exposure was not enough. Thus the formation of
carbides or nitrides characterized with unchanging or
slowincreasing
of
R/R
stage
2.
Decreasing of electric resistance at 500 C hasbeen
shown in all investigated steels and was connected
with dissolving of clusters enriched in chromium
(slow decreasing of R/R accordingly in carbon and
nitrogensteelsstage3).
Effectofcoldplasticdeformationonthephasecontent
and corrosion properties of the steel Cr18Ni2N1 is
presented in Table 2. CPD at an 824% reduction was
combined with aging at 350 Cby two ways:before
(lines 610 in Table 2) and after aging (lines 1114) as
compared to the undeformed state (lines 15). It
follows from Tab. 2 that CPD at 812% reduction
before aging at 350C decreases to thrice a corrosion
rate in spite of some increasing of martensite
content. On the contrary CPD at 20% reduction
increases nearly twice the corrosion ratebecause of
considerable depleting of austenite and as
consequence increasing ofTmartensite content after
strain aging. Furthermore this treatment condition
negativelyinfluencedontheSCCofthisnitrogensteel
and increased ofmartensite content if to compare
withundeformedstate(lines2and8).Itisknown[17]
thatalowlevelofstresses(trthresholdstress)
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FIG.3STRUCTUREOFQUENCHEDSTEEL CR18NI2N1:ASUBGRAINSTRUCTUREOFAUSTENITE;BSELECTEDAREAELECTRON
DIFFRACTIONPATTERNTAKENFROMREGION(A);CKEYPATTERN;DSTRUCTUREOFGRAINBOUNDARY;ESELECTED
AREAELECTRONDIFFRACTIONPATTERNTAKENFROMREGION(D);FKEYPATTERN;GSURFACEMARTENSITE
FIG.4.STRUCTUREOFAGEDAT350 STEELCR18NI2N1:AHOMOGENEOUSDECOMPOSITIONOFAUSTENITE;BSELECTED
AREAELECTRONDIFFRACTIONPATTERNTAKENFROMREGION(D);CKEYPATTERN;DEXTINCTIONCONTOURSANDMARTENSITE;ESELECTEDAREAELECTRONDIFFRACTIONPATTERNTAKENFROMREGION(D);FKEYPATTERN
Zone axis [ 433
]
e
a
313
133
000
422
220Zone axis [
111 ]
202
c
d
110 , 200Cr2N
211
321
310
020
121, 220Cr2N
Zone axis [
201 ]
Zone axis [001]Cr2N
Zone axis [ 131
]
fg
111
a b
111CrN111
200
200CrN
111 rN
200
200CrN
111
111 CrN
131 CrN
131
Zone axis [ 110
] CrN Zone axis [
101 ] CrN
c
000
d e
112
Zone axis [ 521
]
Zone axis [ 010
]Cr2N004
204
200113
202
321
112
Zone axis [
111 ]
Zone axis [113]
110131
000
f420 Zone axis [ 521
]
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FIG. 5 STRUCTURE OF AGED AT 500 STEEL CR18NI2N1: A GRAIN BOUNDARY; B SELECTED-AREA ELECTRON DIFFRACTION
PATTERN TAKEN FROM REGION (A); C KEY PATTERN; D MARTENSITE ; E SELECTED-AREA ELECTRON DIFFRACTION PATTERNTAKEN FROM REGION (D); F KEY PATTERN
FIG. 6 STRUCTURE OF AGED AT 600 STEEL CR18NI2N1: GRAIN BOUNDARY; B SELECTED-AREA ELECTRON DIFFRACTION
PATTERN TAKEN FROM REGION (A); C KEY PATTERN
does not considerably increase the corrosion current
atSCCofironbutahighlevelofthem(tr)causes
a significant growth of this one (Fig. 8). And taking
intoconsiderationthesametodelayedfailure[18,19]
mechanism of SCC, when the main depolarization
process is hydrogen ions (H+) discharge on the
ordered clusters to atoms (H), they become the
effective sub micro cathodes in electrochemical
process on the surface of the steel. The atoms of
hydrogen can join to molecules (H2) significantly
increasing their size and level of stresses in the
clusters. That is why the stressmartensite can be
formedfromthoselocalareasofstructure.
After 24% reduction the austenite has more stabilitythan after 20% reductionbecause of strain recovery,
thats confirmedby dependence of micro hardnessfrom deformation degree (Fig.9). Fig. 10 shows the
structure of deformedbefore aging at 350 C steel
with the electron diffraction pattern where
martensitecanbenoted.
Zone axis [
101 ]
Zone axis [
811 ]
a b c
011, 110
211 200, 002
211
202
120
401000
Zone axis
[ 011
]
Zone axis [010]Cr2N
202
,
211
331
151
011
200
531
022
711
Zone axis [
101 ]
Zone axis
[
611 ]
000
d ef
a b c
200
011
211
110
203Cr2N, 112
222, 404Cr2N
Zone axis [ 110
]
Zone axis [ 011
]
102
Zone axis [ 010
]Cr2N
000
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FIG.7.KINETICSOFELECTRICRESISTANCECHANGEININVESTIGATEDSTEELSCR21N1(1),CR18NI2N1(2) CR18C1(3)DURING
THEAGINGAT:A300;B400;C500
a
b
c
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FIG.10STRUCTUREOFDEFORMEDATAN8%REDUCTIONBEFOREAGINGAT350 STEELCR18NI2N1: MARTENSITE;B
SELECTEDAREAELECTRONDIFFRACTIONPATTERNTAKENFROMREGION(A);CKEYPATTERN
FIG. 8 POLARIZATION DIAGRAM OF CORROSION AT SCC:
O2ABC CATHODE CURVE; FE/FE2+X11 AND FE/FE2+X22 ANODECURVESATADIFFERENTSTRESS
200
250
300
350
400
450
500
0 11 20 24
, %
HV100
FIG.9
DEPENDENCE
OF
THE
MICRO
HARDNESS
ON
THE
DEGREEOFCPDPRECEDEDTHEAGINGAT350 INSTEEL
CR18NI2N1
Treatment with CPD at 20% reduction after aging at
350Cisfoundtobemoreeffective:thecorrosionrate
decreasedbyanorderandthereductionofstrengthat
SCC was about a quarter of magnitudes of
undeformed state. This positive influence of CPD is
probably connected with breaking the order in
metastable clusters which could be acceptors of
discharged hydrogen and nucleus of stressinduced
martensiteatSCC.
Conclusion
The structure of quenched steels Cr21N1, Cr18Ni2N1
andCr18C1
with
high
content
of
nitrogen
and
carbon,
respectively 1.021, 0.899 and 0.920% consists of
metastable austenite with nitrides or carbides settled
downthegrainboundaries.Alsoasmallcontentof
phase takes place near the nitrides/carbides or as a
resultofpolishing.
Twostagesofdecompositionofausteniteattempering
were shown to be in nitrogen steels by electric
resistance: separation of the solid solution with
chromiumfollowedbyorderingoftheseclusterswith
nitrogenwhichinducedbytimeexposureorstresses.
The highest hardness, corrosion rate and stress
corrosion cracking susceptibility in HNS were
observed at the second stage of aging. This structural
state characterized of ordered enriched with
chromium and nitrogen clusters which had an ability
totransformintoastressinducedmartensite.
Coldplasticdeformationat812%reductionpreceding
the aging at 350 C is shown to decrease three times
thecorrosionrateofthesteelCr18Ni2N1ascompared
to the undeformed state. The role of CPD at this
degree consists of accelerating of nitrides CrNprecipitation without intermediate stage of ordering
i
-Fe/Fe2+
i1 i2
1 - tr
2 - tr
-O2
-H+/HA
B
Cx2
1
2
1
310
200
110, 020
002
222
220
113
000
Zone axis [100 ]
Zone axis [ 011
]
Zone axis [ 031
]
311
a b c
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clusters. A thermoplastic treatmentby 20% CPD after
agingat350Cismoreeffectivebecauseofdestroying
already formed ordered clusters, which are the main
reasonofhighsusceptibilitytoSCC.
ACKNOWLEDGMENT
TheauthorwishestothankMansurS.Khadyevforhis
helpinexperimentalprocedure.
This work was carried out and is running now with
the financial support of Russian Foundation for Basic
Research,grantsN070300062aandN110300065.
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in Environment. Advances in Chemistry Research.
Volume 6. Editors: James C. Taylor.Chapter 7. N.Y.,
USA,NovaSciencePublishersInc.2011:219244.
Vera. V. Berezovskaya was born
04.04.1949.
Engineer, Physics of Metals, Ural
Polytechnic Institute (Sverdlovsk,
USSR),1971;
PhD,MetalScienceandHeatTreatment,
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28
UralPolytechnicInstitute,1985;
Assoc. of Prof., Metallurgical Department of Ural State
Technical University, Yekaterinburg (former Ural
PolytechnicInstitute,Sverdlovsk),1996;
Doctorofscience,MetalScienceandHeatTreatment,Baikov
Institute of Metallurgy and Materials Science, RussianAcademyofScience,Moscow,Russia,2004;
Professor, Metallurgical Department of Ural State Technical
University,Yekaterinburg,2005;
Currently Professor, Institute of Metal Science and
Metallurgy of Ural Federal University named after the first
PresidentofRussiaB.N.Yeltsin.
The main area of scientific interest is relationshipbetween
structureandfractureofstainlessandhighstrengthsteelsat
cavitations,delayedfailureandstresscorrosioncracking.
She is a LECTURER at the Ural Federal University onfollowing subjects: Material Science; Theory of corrosion,
corrosionresistant materials and coatings, from 1991 and
Advanced Materials and Technologies from 2010. She has
about200publications,themainofthemare:
Berezovskaya V. V. Structural Factors Governing Steel
ResistanceduringOperationinCorrosiveMediaunder
Cavitation Conditions. Metallovedenie i Termicheskaya
ObrabotkaMetallov,1987,11:5056[MetalScienceandHeat
Treatment. 1987. V.29,I.1112:863869].
Berezovskaya V. V. Delayed Failure of Maraging Steels in
Environment. Advances in Chemistry Research. Volume 6.
Editors: James C. Taylor. Chapter 7. N.Y., USA, Nova
SciencePublishersInc.2011.219244.
Berezovskaya V. V., Savrai R. A., Merkushkin E. A.,
Makarov A. V. Structure and Mechanical Properties of newhighnitrogen CrMn Steels Containing Molybdenum. Izv.
Ross. Akad. Nauk, Ser. Met., 2012, 3: 3139. [Russian
Metallurgy(Metally),2012,5:380388].
Her current research interests lie in the area of High
Nitrogen Steels, their structure, mechanical, physical and
chemicalproperties.
Dr. Berezovskaya supervises the contracts and grants,
preparedtwoMasters(2010,2011)andthePhD(2002).Sheis
Member of New York Academy of Sciences (New York,
USA,1996);
Member of Association of Russian Metallurgists (Moscow,
Russia2002).
Shehas
Honorary title Hero of Labor of regional importance
(Sverdlovskayaarea,Russia,2003);
Diploma of the Ministry of Education and Science for her
significant contribution to the training of highly qualified
specialists(Russia,2011).
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