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JOURNAL OF IRON AND STEEL RESEARCH, INTERNATIONAL. 2011, 18(11) : 60-66

Effect of Heat Treatment on Microstructure and Property of

Cr13 Super Martensitic Stainless Steel
LIU Y u-rong 1 , YE Dong 1 , YONG Qi-long 2 , SU Jie 2 , ZHAO Kun-yu 1 , JIANG Wen 1
( 1. College of Materials Science and Engineering, Kunming University of Science and Technology, Kunming 650093,
Yunnan, China; 2. Institute of Structural Materials, Central Iron and Steel Research Institute, Beijing 100081, China)

Abstract: The microstructures and mechanical properties of Cr13 super martensitic stainless steel afterdifferent heat
treatments were studied. The results show that the structures of the steel after queuehing are of lath martensite
mixed with a small amount of retained austenite. With the raising queuehing temperature, the original austenite grain
size increases and the lath martensite gradually becomes thicker. The structures of the tempered steel are mixtures of
tempered martensite and reversed austenite dispersed in the martensite matrix. The amount of reversed austenite is
from 7. 54% to 22. 49%. After different heat treatments, the tensile strength, the elongation and the HRC hardness
of the steel are in the range of 813-1070 MPa, 10. 1%-21. 2% and 21. 33-32. 37, respectively. The steel displays the
best comprehensive mechanical properties after the sample is quenched at 1 050 ·c followed by tempering at 650 ·c.
Key words: super martensitic stainless steel; quenching; tempering; structure; property; reversed austenite

Cr13 alloyed martensitic stainless steels have will vary with the raising of tempering tempera-
been widely used in many applications owing to their ture[s-Io]. In this work, the reversed austerrite in a
superior mechanical properties and corrosion resist- new type of Cr13 super martensitic stainless steel
ance[IJ. However, brittle chromium carbide precipi- has been studied and the effect of heat treatment on
tation at the grain boundaries during welding has re- microstructure and property is discussed.
stricted the use of high carbon martensitic stainless
1 Experimental
steeJCZ- 3J. Recently, super martensitic stainless
steels have been developed to solve this prob- The material used in the study was low carbon
lem[I-4]. In these steels, carbon content is reduced martensitic stainless steel which was produced in a
to less than 0. 07% and the contents of nicke! vacuum induction-melting furnace and the ingots
(3. 5%-4. 5%) and molybdenum ( 1. 5%-2. 5%) were forged into bars with air hammer. The bar was
are increased. Thus, the steel not only has high cut to dimensions of ~15 mm X 10 mm and used for
strength, good plasticity and weldability, but also the heat treatment specimens. The chemical compo-
has good corrosion resistance, processability and sitions of the tested steels are shown in Table 1.
lower economic costs, which are particularly attrac- The phase transformation temperatures are also
tive to the oil industry. shown in Table 1, which were measured by Formas-
Several studies on the super martensitic stain- ter-FII thermal dilatometer under a regime of heating
less steel have indicated that heat treatments have a to 1100 ·c for 15 min at a rate of 0. 05 'C/s and then
significant effect on microstructures and properties cooling to room temperature at a rate of 100 'CIs. All
of steeJ[s-'l]. After quenching and tempering, reversed specimens were quenched at the temperature range
austerrite is formed in super martensitic stainless of 800- 1100 ·c for 0. 5 h and then oil quenched.
steel. The reversed austerrite is fine and dispersed in Tempering was carried out at the temperature range
martensite matrix. The existence of the reversed of 550-750 ·c for 2 h. Microstructures were studied
austerrite improves the comprehensive properties of by optical microscopy, scanning electron microscope
the materials, and the amount of reversed austerrite (SEM) and transmission electron microscope (TEM).

Biography,LIU Yu-rong0985-), Female, Master; E-mail: liuyurong0771@163. com; Received Date, October 31, 2010
Issue 11 Effect of Heat Treatment on Microstructure and Property of Crl3 Super Martensitic Stainless Steel • 61 •

Table 1 Chemical composition and phase transformation temperature of tested steels

Chemical composition/% Phase transformation temperature/ ·c
Sampie
c Mn Si Cr Ni Mo w Cu A, Ar M, Mr
0. 019 0.40 o. 16 11. 69 4. 94 2.04 585 730 310 170
2 0.022 0.41 0. 17 11. 86 5. 14 2. 17 1. 00 1. 39 650 775 255 125
Note: A,-Reversed austenite start tansformation temperature; Ar-Reversed austenitefinal tansformation temperature;
M,-Martensite start tansformation temperature; Mr-Martensite final tansformation temperature.

The volume fraction of austenite was determined rate of austenite dramatically. Simultaneously, the
from peaks of X-ray diffraction patterns using CoKa insoluble carbide in austenite at a certain quenching
radiation from 30° to 120°. Hardness variations were temperature can inhibit grain growth of austenite
measured with a rockweil hardness tester with a Ioad and Iimit the growth rate of austenite effectively by
of 1500 N. Tensile strength and elongation were means of pinning the austenitic grain boundaries.
carried out with an electric universal testing ma- When quenching below 1 000 ·c , the carbide and
chine. Every HRC hardness is measured six times other second phase particles can effectively prevent
and averaged, and the tensile strength and elonga- the grain growth of austenite. However, when the
tion are measured three times and averaged. quenching temperature is higher than 1 000 the ·c ,
effect of preventing grain growth of austenite will be
2 Results and Discussion
reduced gradually because of re-dissolution of the in-
2. 1 Effect of heat treatment on microstructure soluble carbide in austenite. As a result, the austen-
2. 1. 1 Quenching temperatures itegrainwill grow remarkably when quenching tem-
The microstructures of the steel quenched at perature is in the range of 1000-1050 ·c. However,
800, 850, 900, 950, 1 000, 1 050 and 1100 show ·c when the quenching temperature is 1050-1100 ·c, the
quenched martensite. The carbon content in tested growth rate of austenite is slow, which indicates
steel is very low ( only 0. 02%) , so that the quenched that the carbide and other second phases in austenite
martensite is lath martensite. The typical martensite have been dissolved fully, demonstrating that the
rnicrostructures are shown in Fig. 1. The grain grades quenching temperature of 1 050-1100 ·c
is benefi-
of original austenite crystal are ranging from 5 to 9 cial to refine the matrix microstructure and improve
CTable 2), which are increased from 16. 8 to 56. 88 J.Lm the comprehensive properties of tested steel. The
with an increase in quenching temperatures. lt is size of martensite platelet increases with increasing
found that grains grow slowly when quenching tem- quenching temperatures. As known, lath martensite
peratures are 900- 1 000 ·c
and 1 050- 1100 ·c, is formed in the original austenite grains and the
whereas grain coarsens when quenching tempera- number of lath is certain in austenite grains. How-
tures are 1 000 - 1 050 ·c.
The elements in tested ever, the width and distribution of lath are not af-
steel, W, Mo and Cr, which have great affinity for fected by austenite grains. Thus, the size of the
carbon and can combine carbon to form a few kinds martensite platelet increases with increasing austen-
of carbides in austenite, can decrease the formation ite grain size[IIJ.

(a) Steel No.1; (b) Steel No. 2.

Fig. 1 Microstructure of tested steel quenched at 1 050 'C
 • 62 • Journal of lron and Steel Research, International Vol. 18

Table 2 Grain sizes of austenite crystal at different queuehing temperatures

Quenching temperature 9oo ·c 950 'C 1 ooo ·c 1 oso ·c 11oo ·c

Steel No. 1 Austenite grain grade 9 (8. 7) 8 (7. 5) 7 (7. 42) 6 (5. 54) 5 (5.43)
Austenite grain size/ ,_.m 17. 4 25. 9 27.04 51. 95 53. 78
Steel No. 2 Austenite grain grade 9 (8.8) 7 (7. 46) 7 (6. 93) 5 (5. 31) 5 (5. 27)
Austenite grain size/ ,_.m 16.8 26.65 32.08 56.03 56. 88

2. 1. 2 Tempering TEM after tempering. Thus, the microstructure of

After samples are tempered at 650 'C , the thick tempered steel is fine tempered martensites combined
lath martensites obtained after quenching at 900, 950, with reversed austenites. Grain sizes of austenite
1 000, 1 050 and 1100 'C become fine tempered mar- crystal increase with increasing quenching tempera-
tensites. The microstructures observed by optical tures and grains grow up rapidly when quenching
microscope are shown in Fig. 2 , and there are fine temperatures are 1 000 - 1 050 'C, which has the
M 23 C 6 carbides precipitation in the martensite ma- same grain growth tendency of the quenched steel.
trix. After tempering, the saturation Ievel of the su- Therefore, tempering temperature has little effect on
persaturated a-ferrite decreases continuously owing the austenite grain growth and the process of tempe-
to the precipitation of carbide. The small amount of ring is the process of microstructure refinement and
:retained austenite will also decompose, and the de- carbide precipitation. The detailed microstructures
composition products are a dual-phase structure of of the samples observed by SEM are shown in
supersaturated a-ferrite and M 23 C 6 carbide, which is Fig. 3. Although the tempering temperatures are
equivalent to the tempered martensite. There is also high, the tempered martensite still retains the quenched
the formation of reversed austenites observed by martensite, which indicates that the sample has high

Fig. 2 Microstructure of steel No. 1 (a) and No. 2 (b) quenched at 1050 "C followed by tempering at 650 "C

Fig. 3 SEM microstructure of steel No. 1 (a) and No. 2 (b) quenched at 1050 "C followed by tempering at 650 "C

thermal stability. tensile strength and elongation with quenching tem-

perature. With increased quenching temperature,
2. 2 Effect of heat treatment on mechanical property the tensile strength of steel decreases. According to
2. 2. 1 Quenching temperature +
Hall-Petch formula R. = C1; KYD- 112 ( where, R. is
Fig. 4 shows the variation of HRC hardness, the yield strength of material; C1; is the resistance of
Issue 11 Effect of Heat Treatment an Microstructure and Property of Cr13 Super Martensitic Stainless Steel • 63 •

28 (a) • Steel No.1 (b)

fl40
"'StPel No.2
920 25

~~.
2ß ~
~ 900
,g~
..
~880
a.;

t; 860
20
~

E
.9:
fJ
~ 840 ~ ~ 15
820 ·~
800
20~------~----~------~----~ ~----~~----~----~------~10
900 950 1000 1050 1100 900 950 1000 1050 1100
Quenching tPmpPraturP/'t

Fig. 4 Effect of quenching temperature on HRC hardness (a) and tensile strength and elongation (b) of steel

disloeation slip; K is a eonstant; and D is the aver- maximum value when the queuehing temperature ts
age grain diameter)[JzJ, it is shown that the smaller 1 050 "C. This is beeause a large number of reversed
the grain size is, the grea ter the effeet of strengthe- austenites form when the steel is tempered at 650 "C
ning and plastie deformation resistanee will be. This after quenehed at 1050 "C (shown in Table 3). The
is beeause the finer the grain size is, the bigger the reversed austenite locates along the boundaries of o-
grain boundaries will be, thereby effeetively preven- riginal austenite crystals and lath boundaries, which
ting the movement of the disloeation. This is ealled displays good toughness and exeellent thermal sta-
grain refining strengthening. When the grain and bility, but very low mechanieal stabilityl 14 J. The re-
lath expand, the strength of steels declines gradual- versed austenite will not transform into martensite
lyl13J. The Hall-Peteh formula also applies to the even at very low temperatures. However, once plas-
lath martensite, beeause there are large angle grain tic deformation oceurs, the reversed austenite will
boundaries between martensite laths. The modified absorb the deformation work and transform to mar-
+
formula[Iz] is R. =cr; KYD;;; 1 , where Drn is the mar- tensite partially. Thereby, the plastieity and tough-
tensite lath bundle diameter and is determined by the ness of material at low temperatures ean be en-
length (dP) and width (w) of martensite. Drn ean be hanced. In addition, the tempered martensite con-
ealculated by sists of lath martensite with a high dislocation density

Drn = !{ wln tan areeo; [ ~] + ~ + ; dP-

and the lath martensite is very fine with the width of
100-200 nm. This is the reason that the eompre-
hensive meehanical properties ean be improved after
tempering. Thus, the integrated analysis of me-
dPareeos [ ~] } (1)
chanieal properties shows that the strength of steel
Based on the modified formula, the tensile assorts well with toughness when samples are tem-
strength varies inversely to the martensite lath bun- pered at 650 "C after queuehing at 1 050 "C. Compa-
dle diameter. Therefore, the smaller martensite lath ring the mechanieal properties of steel No. 1 and
is, the greater the effeet of strengthening will be. No. 2 after the same heat treatment, the tensile
As shown in Fig. 4, the tensile strength of samples strength, hardness and elongation of steel No. 2 is
deereases strongly when queuehing temperatures are always better than those of steel No. 1, which indicates
900-1 050 "C , while the tensile strength of samples that the addition of W and Cu can significantly im-
deereases slightly when queuehing temperatures are
1 050-1 100 "C. The ehange of the tensile strength Table 3 Amount of austenite at-different heat treatments
is just the same as the tendeney of the grain growth Austenite content/%
Heat treatment
(shown in Table 2), whieh indieates that the miero- Steel No. 1 Steel No. 2
strueture and property of the tested steel have a 1 ooo ·c, 1h 0. 49 0.38
strong eorrelation. When queuehing temperatures 1 ooo ·c, 1 h+65o ·c, 2 h 7.54 22.49
are 900- 1100 "C, the elongation and hardness of 1 o5o ·c , o. 5 h 0.34 0.30
the steels ehange in a eertain range and display the 1o5o ·c, o.5 h+65o ·c, 4 h 8. 35 20. 70
 • 64 • Journal of Iran and Steel Research, International Vol. 18

prove the mechanical properties of the tested steel. The change of mechanical properties matches with
2. 2. 2 Tempering temperature the amount of reversed austenite, which indicates
Fig. 5 shows the changes of the HRC hardness, the good correlation between microstructure and me-
tensile strength and elongation with tempering tem- chanical properties of tested steels.
perature for 2 h. The HRC hardness and tensile As shown in Table 3, the amount of austenite
strength decrease rapidly when tempering tempera- in steel No. 1 is much higher than that in steel No. 2
ture is 550- 600 Oe. However, above 600 Oe , the after quenching, while after tempering, the volume
HRC hardness and tensile strength decrease slightly fraction of the reversed austenite of steel No. 2 is al-
as temperature is increased to 650 Oe, and then in- most triple compared with steel No. 1. The fine re-
creases with elevated temperature. The elongations versed austenite dispersed in martensite matrix can
of steel No. 1 and steel No. 2 increase with raised improve the mechanical properties by means of ab-
temperature and display the maximum values of sorbing deformation work when the plastic deforma-
20. 2% and 21. 2%, respectively, at a temperature tion of material occurs[JoJ. Thus, under the same
of 650 Oe. Above 650 Oe , the elongation decreases heat treatment conditions, the comprehensive me-
sharply, so it is not appropriate to temper a sample chanical properties of steel No. 2 are much better
above 650 Oe. In summary, it is observed that with than steel No. 1.
an increase in tempering temperature, the changes
3 ~icrostructure
of HRC hardness and tensile strength have a strong
positive correlation, and they have contrary correla- The austenite contents of specimens after dif-
tion with that of elongation length, which indicates ferent heat treatments tested by XRD are shown in
that the strength, hardness and elongation of tested Table 3. The volume fraction of austenite in quenched
steel have a good correlation. As mentioned before, steels varies slightly from 0. 3% to 0. 49% , all of which
reversed austenites are formed when the steel is tem- is retained austenite. Consequently, the microstruc-
pered. The amount of reversed austenite firstly in- tures of samples after quenching are quenched mar-
creases and then decreases with raised temperature tensite and retained austenite. However, after tempe-
and displays a maximum value at the temperature of ring, the volume fraction of austenite rises rapidly up to
600- 650 oec
9 15 19
' - J. The reversed austenite has good 22. 49%, and these austenite are the reversed aus-
plasticity and toughness, but its strength and HRC tenite. It is found that the reversed austenite can only
hardness is low. That is why the tensile strength be generated when tempering temperature ranges
and hardness of tested steels decrease firstly and from A, to A 1 and the amount of reversed austenite in-
then escalate with the increase in tempering temper- creases with raised temperature and displays a maximum
ature, while the plasticity has a quite opposite change. value at the temperature of 600- 650 oec9 15 19
' - J. The
increase in volume fraction of reversed austenite is
34 (a) o Steel No.1 caused by the increase in driving force of martensite
32
(M) / austenite ( A) transformation with raised tem-
~
30 perature. Furthermore, when the tempering tem-
~
...::: perature is low, the thermal stability of reversed
28
~ austenite is good because of the enrichment of auste-
:I:
26
nitic elements in reversed austenite. Thus, it is dif-
24 ficult for the reversed austenite formed in the
1100 22
process of tempering to transform to martensite again
~

i 1000 18 ~
.::;
during coolingl 15 J. Above the temperature of 650 Oe ,
the volume fraction of austenite decreases. This de-
i 14
ä
.§ crease has been attributed to the transformation of
=s::
~

UJ
~
900
r..l
the reversed austenite into martensite during cool-
E-<
800 mg. When tempering temperatures increase, the
10
550 600 650 700 750 volume fraction of austenite arises and the amount of
Tempering temperature/'C
the austenite forming elements in the reversed aus-
Fig.S Effect of tempering temperature on HRC tenite decreases. Thus, the martensitic transforma-
hardness ( a) and tensile strength and tion is easily induced owing to the decrease of ther-
elongation (b) of steel mal instability of austenite[ 17J. Ultimately, the amount
Issue 11 Effect of Heat Treatment an Microstructure and Property of Crl3 Super Martensitic Stainless Steel • 65

of reversed austenite in specimen at room tempera- pattern and schematic diagram for Fig. 6 ( d) are
ture lowers. shown in Fig. 6 ( e) and ( f) , respecti vely. The re-
Fig. 6 shows the TEM micrographs of specimen versed austenite was formed firstly along the bound-
tempered at 650 'C after quenching at 1 050 ·c. A aries of original austenite crystals and lath bounda-
typical martensite microstructure observed by TEM ries. These places present high defect density, which
is shown in Fig. 6 ( a), which consists of lath mar- can provide the energy of austenite nucleation and the
tensite with a high dislocation density, and the cor- quick diffusion access for nicke! atom[Is.zo-ziJ, Accord-
responding selected area electron diffraction (SAED) ingly, the reversed austenite can easily form along
pattern and schematic diagram are shown in Fig. 6 ( b) the martensite lath or grain boundaries, since they
and (c), respectively. The lath martensite is fine with are beneficial for the formation and growth of aus-
the width of 100-200 nm. That is why the compre- territe grain. The existence of the reverse austerrite
hensive mechanical properties can be improved after can not only prevent the crack propagation along the
tempering. The reversed austenites with a strip martensite laths but also relieve the stress concen-
shape are observed by TEM shown in Fig. 6 ( d). tration caused by dislocations along the martensite
Their length is measured about 10 2 -10 3 nm and the laths. Thus, the toughness of material can be en-
width is about 100 ,nm. The corresponding SAED hanced consequently.

(a) Lath martensite1 (b) SAED pattern for (a); (c) Schematic diagram for (b);
( d) Reversed austenite 1 ( e) SAED pattern for ( d) ; ( f) Schematic diagram of ( e).
Fig. 6 TEM images of sample tempered at 650 "C after quenching at 1 050 "C

similar to that of steel No. 2 after quenching at the

4 Conclusions same temperature.
1) The microstructures of steel No. 1 and No. 2 3) The microstructures of steel No. 1 and No. 2
after quenching at 900-1100 ·c
consist of quenched after tempering at 650 ·c are fine tempered martens-
martensite and retained austenite with the volume ite with the width of 100- 200 nm. After tempe-
fraction of retained austenite from 0. 3% to 0. 49%. ring, the grain size of austenite crystal increases
2) Martensite platelet coarsens and the size of with increasing quenching temperatures and the
original austerrite grains increases from 16. 8 to growth tendency of austerrite crystal is the same to
56. 88 p.m with the rising quenching temperature. that of the quenched samples.
The size of original austenite grains of steel No. 1 is 4) After different heat treatments, the tensile
 • 66 • Journal of Iran and Steel Research, International Vol. 18

strength, elongation and hardness of steel are 813- [10] LI Xiao-yu, WANG Ya, DU Bing, et al. Effect of Retained
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