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Metal Science and Heat Treatment, Vol. 52, Nos. 11 12, March, 2011 (Russian Original Nos.

. 11 12, November December, 2010)

THERMOCHEMICAL TREATMENT
UDC 669.14.018.298:621.785.062

STRUCTURE AND PROPERTIES OF CARBURIZED COATINGS


WITH REVERTED AUSTENITE ON LOW-CARBON MARTENSITIC STEELS
A. S. Ivanov,1 S. A. Kokovyakina,1 and A. S. Pertsev1
Translated from Metallovedenie i Termicheskaya Obrabotka Metallov, No. 11, pp. 51 56, November, 2010.

The process of creation and subsequent hardening of a gradient carburized layer in low-carbon martensitic
steel 17Kh2G2NMFTB is studied. It is shown that the structure and properties of the carburized layer can be
optimized due to formation of reverted austenite hardened by quenching from the intercritical temperature
range.

Key words: gradient layer, reverted austenite, lath martensite, low-carbon martensitic steels
(LCMS).

In the present work we had an aim to study the formation


of a surface layer in the process of carburizing of low-carbon
martensitic steel 17Kh2G2NMFTB, to determine the structure and properties of the layer, and to estimate the possibility of its hardening by optimizing the modes of subsequent
heat treatment at preserved structure and properties of the
matrix of the metal.

INTRODUCTION
Low-carbon martensitic steels (LCMS) possess a number
of unique features distinguishing them from other structural
steels traditionally used in machine building [1 5]. Rational
alloying and low content of carbon in LCMS promote elevation of the stability of supercooled austenite and yield a martensite structure in large cross sections after comparatively
slow cooling in air.
In order to widen the range of application of LCMS to
operation under conditions of contact friction it is necessary
to develop processes of their surface hardening. LCMS of
grades 07Kh3GNMYuA, 10Kh3GNM, and 08Kh2G2F operating under contact friction (gears, turbodrill parts) are subjected to surface hardening by carburizing and nitriding.
However, grades 12Kh2G2NMFT, 15Kh2G2NMFB, and
17Kh2G2NMFTB having the highest strength are not used in
a surface-hardened state [7 10].
1

METHODS OF STUDY
We studied low-carbon martensitic steel 17Kh2G2NMFTB
and (for comparison) 12Kh2G2NMFT. The chemical compositions, the hardness, and the structures of the steels in the
initial state are presented in Tables 1 and 2.
Gas carburizing of the steels was performed in a Ts-75
shaft furnace at 900 910C for 4 h at benzene feeding rate
of 80 100 drops/min. Subsequent heat treatment was performed in a SNOL-type laboratory furnace. The carburized
specimens were placed into a container with waste carburizer
in order to avoid decarburization.

Perm State Engineering University, Perm, Russia (e-mail:


mto@pstu.ru).

TABLE 1. Chemical Compositions of Steels


Content of elements, wt.%
Steels

17Kh2G2NMFTB
12Kh2G2NMFT

Si

Mn

Cr

Ni

Mo

Nb

Ti

S, at most

P, at most

0.17
0.13

0.37
0.24

2.07
2.24

2.42
2.39

1.50
1.38

0.39
0.45

0.17

0.12
0.10

0.22
0.04

0.011
0.119

0.015
0.004

562
0026-0673/11/1112-0562 2011 Springer Science + Business Media, Inc.

Structure and Properties of Carburized Coatings with Reverted Austenite

563

TABLE 2. Structure and Hardness of the Steels in the Initial Condition


Steel

Initial condition

17Kh2G2NMFTB Hot-rolled bar


12Kh2G2NMFT Hot-rolled sheet,
6 mm

Structure

HRC
hardness

Lath martensite
Lath martensite

37
39

The microstructure of the steels was studied using an


OLYMPUS GX-51 microscope at magnification of 100
1000 and a Video Test-Master. Structure 4-0 software for
image analysis. The hardness was measured by the Rockwell
method in accordance with GOST 901359; the microhardness was measured in accordance with GOST 945076 using
a PMT-3 microhardness meter at a load of 0.5 and 0.2 N.
X-ray diffraction analysis was performed with the help
of a DRON-3 x-ray diffractometer in iron Ka radiation; the
results were recorded using a DRON System for Automation of x-ray Diffractometers.
The content of retained austenite (in %) was determined
using the ratio of the integral intensities of line (311) of austenite and line (211) of martensite, i.e.,
Aret = 100/[1.273(I(211)a /I(311)g ) + 1],

(1)

where I(311)g and I(311)a are the intensities of the lines of retained austenite and martensite, respectively.
The microstresses and the sizes of subgrains in austenite
and martensite were computed by the method of approximation from x-ray lines (110) (211) of martensite and (111)
(311) of austenite. The approximating functions were [6]
y = 1/(1 + ax 2 )

and

y = 1/(1 + ax 2 )2.

(2)

The standards were powders of technically pure iron and


copper.
The process of decomposition of retained austenite was
studied and the critical points of the carburized layers were
determined using a Chevenard dilatometer on specimens
3.5 mm in diameter subjected to through carburizing. The
standard was a piros alloy. Layer-by-layer chemical analysis was performed using an ARL-31.100 emission quantum
meter.
RESULTS AND DISCUSSION
The microstructure of the carburized layer of steels
17Kh2G2NMFTB and 12Kh2G2NMFT is presented in
Fig. 1. The microhardness and the content of retained austenite are presented in Fig. 2a and b.
The structure of the carburized layer on steel
17Kh2G2NMFTB may be divided conventionally into three
zones. In the first (surface) layer martensite and retained austenite are accompanied at a distance of up to h = 0.10 mm by

100 mm

Fig. 1. Microstructure of carburized layer on steels 17Kh2G2NMFTB


(a) and 12Kh2G2NMFT (b ).

a high amount of carbides. In the second (austenite) zone the


content of austenite at a distance h ~ 0.20 0.30 mm from
the surface attains 77% and the microhardness decreases
abruptly to 460 HV (Fig. 2a and b ). At h ~ 0.40 0.45 mm
the content of retained austenite decreases to 40% due to the
decrease in the carbon concentration in the layer. This causes
formation of a third (martensite) zone, where coarse acicular
martensite gradually transforms into lath martensite of the
matrix. The microhardness in this zone increases to 620 HV
in steel 17Kh2G2NMFTB and to 800 HV in steel
12Kh2G2NMFT. As the distance from the surface increases
and the carbon concentration decreases, the microhardness
decreases uniformly and attains 400 HV, which corresponds
to the microhardness of the matrix of the steel. The hardness
of the carburized layer is 58 HRC.
A distinctive feature of the microstructure of the carburized layer of steel 12Kh2G2NMFT is a high content of retained austenite (up to 85%). The distribution of the microhardness and of the amount of retained austenite after carburizing of steels 17Kh2G2NMFTB and 12Kh2G2NMFT has
the same nature (Fig. 2a and b ). The hardness of the carburized layer of steel 12Kh2G2NMFT is only 40 HRC due to
the higher content of retained austenite in it as compared to
steel 17Kh2G2NMFTB.
In order to decrease the content of retained austenite and
to optimize the structure and properties of the carburized

564

A. S. Ivanov et al.
Aret , %
100
90
80
70
60
50
40
30
20
10

Aret , %
17Kh2G2NMFTB
12Kh2G2NMFT

80

17Kh2G2NMFTB
17Kh2G2NMFTB
12Kh2G2NMFT

70
60
50
40
30
20
10

0.05 0.15 0.25

0.35

0.45 0.55 Matrix

0.05

0.15

0.25

h, mm
HV, kgf/mm2

HV, kgf/mm2
1200

17Kh2G2NMFTB
12Kh2G2NMFT

800

600

600

400

400

200

200
0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0

h, mm

Matrix

17Kh2G2NMFTB
17Kh2G2NMFTB
12Kh2G2NMFT

1000

800

0.45

h, mm

1200
1000

0.35

0.1 0.2 0.3

0.4

0.5 0.6 0.7 0.8 0.9 1.0

h, mm

Fig. 2. Distribution of retained austenite and of microhardness over the thickness of surface layer (h is the distance from the surface) in steels 17Kh2G2NMFTB and 12Kh2G2NMFT: a, b ) after carburizing; c, d ) after carburizing and hardening from 810C in oil (:, =) and in air (&).

layer, the carburizing was followed by hardening of the steels


from temperatures of the austenitic and two-phase (a + g)
ranges with oil and air cooling.
Steels 17Kh2G2NMFTB and 12Kh2G2NMFT were
hardened from 810C (0.5 h) in oil and in air by the regime
worked out at the Inkar Company for steel 12Kh2N4A (the
hold time is corrected with allowance for the charge).
After oil cooling of steel 12Kh2G2NMFT the surface
zone of the carburized layer acquires high-carbon martensite,
preserves a carbide zone, and the content of the austenite decreases. Formation of a martensite structure and decrease in
the content of retained austenite cause growth in the hardness
of the carburized layer to 62 HRC. In the case of air cooling
of the steel a carbide zone and a zone of fragmented austenite
are preserved in the structure in addition to the formed
martensite.
Oil cooling and air cooling of steel 17Kh2G2NMFTB
lower considerably the content of retained austenite as compared to the initial carburized state (to 49 and 47%, respectively, Fig. 2c ).
The distribution of the microhardness over the thickness
of the layer for steels 17Kh2G2NMFTB and 12Kh2G2NMFT
after oil and air hardening is the same (Fig. 2d ) and does not
change in the cause of the hardening. The fall in the microhardness in the austenite zone is preserved but becomes
lower. The highest microhardness is observed over the whole
of the thickness of the layer after oil cooling.

It should be noted that the content of austenite in the


austenitic zone of the carburized layer on steel 12Kh2G2NMFT
is considerably higher and the microhardness is lower than in
steel 17Kh2G2NMFTB.
In has been shown in [11, 12] that steel 12Kh2G2NMFT
promises much after hardening from the intercritical temperature range (ITR). Hardening from a temperature exceeding
Ac1 but lower than Ac3 yields a homogeneous structure of
lath martensite. The close levels of mechanical properties after complete and incomplete hardening make it possible to
lower the temperature of heating for hardening, which should
reduce the level of internal stresses in the metal.
We estimated the possibility to use incomplete hardening
for steel 17Kh2G2NMFTB in a carburized state. According
to the data of dilatometric analysis of the carburized layer on
steels 12Kh2G2NMFT and 17Kh2G2NMFTB (we studied
specimens subjected to through carburizing), A1 = 710
720C and A3 = 790 800C. After hardening of carburized
specimens of steel 12Kh2G2NMFT from 740 and 770C
both in air and in oil, the structure and the properties of the
carburized layer remained virtually unchanged. Therefore,
we chose the temperature of 750C for hardening the studied
steels from the ITR.
The structure of the carburized layer on steel
17Kh2G2NMFTB after hardening from the ITR is represented by carbide-martensite, austenite-martensite, and mar-

Structure and Properties of Carburized Coatings with Reverted Austenite

565

Q, mm

Aret , %

0,25

40

35
30

0,20
0,15

25

0,10

20

0,05

15

0.1

0.2

0.3

0.4

10

0.5

h, mm

sm , P

0
0.06

0.16 0.26

0.36

0.46 Matrix

400
350
300
250
200
150
100
50

h, mm
HV, kgf/mm2
1200

b
1000

2
0.1

0.2

0.3

0.4

0.5

h, mm

800

600

Fig. 4. Sizes of blocks (Q ) (a) and microstresses (sm ) (b ) in the


austenitic zone of surface layer on steel 17Kh2G2NMFTB after carburizing and hardening from 750C in air (1 ) and in oil (2 ).

2
400
200
0

0.1 0.2 0.3

0.4 0.5 0.6 0.7 0.8

0.9 1.0

1.2

h, mm

sm , P
500

Fig. 3. Distribution of retained austenite (a) and microhardness (b )


over the thickness of surface layer (h is the distance from the surface) in steel 17Kh2G2NMFTB after carburizing and hardening
from 750C in air (1 ) and in oil (2 ).

400

300
200

2
1

100

tensite zones arranged from the surface to the core of the


specimen, respectively.
After oil cooling of steel 17Kh2G2NMFTB the hardness
of the carburized layer is 61 HRC, which is comparable with
the hardness due to hardening from 810C; the core has a
hardness of 32 HRC. After air cooling the hardness of the
layer is somewhat lower, i.e., 54 HRC; that of the core is
29 HRC. After oil and air cooling from 750C the content of
the retained austenite is lower than after hardening from
810C (compare Figs. 3 and 2c). Its maximum content
(35 36%) is detected at h ~ 0.15 0.25 mm.
The distribution of the microhardness after hardening
from 750 and 810C differs (compare Figs. 3 and 2d ). After
hardening from 750C the dip of the microhardness in the
zone of retained austenite disappears; the microhardness decreases uniformly from about 1100 HV on the surface of the
layer to 300 HV in the matrix. After air cooling the microhardness in the zone of retained austenite at the place of the
dip increases to about 90 HV. It should be noted that in steel
12Kh2G2NMFT similar properties are obtained after treatment in more complex mode, namely, (1 ) carburizing, high
tempering at 620C. hardening from 740 and 770C with oil
or air cooling, respectively, and (2 ) carburizing, hardening
from 740C with 2-h heating at 620C, and oil or air cooling.

0.1

0.2

0.3

0.4

0.5

h, mm
Fig. 5. Microstresses in austenite in steel 17Kh2G2NMFTB after
carburizing and hardening by different regimes: 1 ) from 750C in oil;
2 ) from 819C in oil; 3 ) from 750C in air; 4 ) from 810C in air.

The variation of the parameters of the subgrain structure of the austenite in the carburized layer of steel
17Kh2G2NMFTB after hardening from the ITR (750C)
presents special interest. The sizes of the blocks and the
microstresses in the austenite differ substantially after air
cooling and after oil cooling (Fig. 4).
After air cooling the block sizes are much smaller and
the level of the microstresses is higher than after oil cooling.
This may be connected with the fact that the reverted austenite (the retained austenite not decomposed and newly formed
during heating to the ITR temperature) undergoes precipitation hardening in air, i.e., segregation of dispersed carbides
that harden the austenite and increase in the stresses.
Figure 5 presents the curves of variation of microstresses
in austenite over the thickness of the layer after hardening
from 750 and 810C in oil and in air. After hardening from
750C in air the level of the microstresses is considerably

566

A. S. Ivanov et al.
a, nm

HV, kgf/mm2

0.362

1200

1000

0.361

800

0.360

600
0

0.05

0.10

0.15

1
0.20

0.25

0.30

0.35

0.359

h, mm
Fig. 6. Distribution of microhardness over the thickness of surface
layer (h is the distance from the surface) of steel 17Kh2G2NMFTB
after carburizing and hardening from 650C in air: 1 ) hardness of
austenite (target measurement); 2 ) hardness of austenite and martensite.

2
3
0

0.1

0.2

0.3

0.4

0.5

0.6

h,
a, nm
0.362

0.361

1
0.360

higher than after hardening in oil; in the austenite region


(h ~ 0.20 mm) it even exceeds the level of the microstresses
attained after hardening from 810C. The high compressive
stresses in the surface layer promote increase in the fatigue
resistance and stabilize the austenite.
Precipitation nature of the hardening of reverted austenite is mentioned in [13 15]. Target measurements of the
microhardness of austenite have shown that its hardness is
higher than the integral hardness of the austenite-martensite
structure in the same region of the layer (Fig. 6).
Thus, austenite hardens upon comparatively slow cooling in air and is fragmented forming blocks of a smaller size.
Summarizing the facts mentioned above we may suggest
the following scheme of formation of reverted austenite in
the carburized layer of steel 17Kh2G2NMFTB due to heating in the ITR and subsequent cooling at different rates.
At 750C the carburized layer preserves (acquires) reverted austenite, the behavior of which in the processes of
cooling in air and in oil differs substantially. It could be expected that in oil cooling the stresses in the layer should be
higher than in comparatively slow air cooling. However,
such behavior is observed in martensite, but in austenite the
microstresses after air cooling are considerably higher than
after oil cooling.
It seems that this is explainable by the fact that carbon is
redistributed during air cooling in reverted austenite and
ultrafine carbides of a cementite type are segregated there.
This causes substantial precipitation hardening of the reverted austenite. Simultaneously, there occurs redistribution
of dislocations and formation of nanosize subgrains.
In the case of oil cooling these processes are suppressed,
and the level of the microstresses in the austenite is considerably lower and the block sizes are higher than in air cooling.
This is conformed by the results of a comparison of the
microhardness of the layer after hardening from 750C in air
and in oil (see Fig. 3). In the surface carbide-martensite zone
(h 100 mm), where the content of austenite is comparatively low, the hardness of the layer hardened in oil is higher
than that after cooling in air. In the austenitic zone
(h = 100 200 mm), where we have detected a dip in the
hardness after carburizing and after carburizing followed by

0.359

4
5
0

0.1

0.2

0.3

0.4

0.5

0.6

h,
Fig. 7. Variation of the lattice parameter of austenite over the thickness of hardened layer (h is the distance from the surface) of steel
17Kh2G2NMFTB after carburizing and hardening from 750C (a)
and from 810C (b ): 1 ) after carburizing; 2, 3 ) after carburizing
and hardening from 750C in oil and in air respectively; 4, 5 ) after
carburizing and hardening from 810C in oil and in air respectively.

hardening from 810C, the hardness after air hardening from


750C increases abruptly and remains higher than after air
cooling over the entire layer up to h = 550 mm.
Precipitation hardening of austenite accompanied by rearrangement of its dislocation structure is similar to the process of cell formation. As a result, the blocks are refined
markedly (see Fig. 4). Locking of dislocations in walls
causes growth in the strength and hardness of the austenite. It
can be assumed that fixation of the dislocation structure of
the austenite and increase in its stability are promoted by
segregation of dispersed carbides over boundaries of
subgrains described in works [16, 17].
Variation of the parameters of the crystal structure of
austenite over the thickness of carburized layer after carburizing and after carburizing followed by hardening from 810
and 750C in oil and in air is presented in Fig. 7. In all the
cases the decrease in the content of carbon in the layer results
in decrease in the lattice parameter of the austenite. The
value of the lattice parameter differs somewhat depending on
the heating temperature and on the rate of the hardening
cooling. In the process of hardening from 810C retained
austenite with the same lattice parameter is preserved upon
cooling in oil and in air. After cooling from 750C, the lattice
parameter of the austenite is less after cooling in air than after cooling in oil. It is obvious that this is a consequence of
the earlier described process of segregation of dispersed carbides and carbon depletion of the reverted austenite due to
the comparatively slow air cooling.
Thus, the reverted austenite differs from the retained austenite in carburized layer of steel 17Kh2G2NMFTB by the

Structure and Properties of Carburized Coatings with Reverted Austenite

fact that its precipitation hardening and stabilization occur as


a result of segregation of ultrafine carbides and formation of
a cellular structure with nanometric (25 30 nm) sizes of
subgrains and an elevated level of microstresses.
CONCLUSIONS
1. The complex alloying system of steel 17Kh2G2NMFTB
promotes formation of stable retained austenite in carburized
layer.
2. Retained austenite in carburized layer is distributed by
a law with an extremum; its maximum content (80 85%)
occurs at a distance h = 0.2 0.3 mm from the surface.
3. It is possible to form reverted austenite with a high
carbon content and unusually high hardness in carburized
layer of steel 17Kh2G2NMFTB by hardening from the
intercritical temperature range with cooling in air.
4. The most probable cause of the hardening of the austenite is segregation of ultrafine carbides of a cementite type.
5. Strengthening and stabilization of the reverted austenite is also promoted by rearrangement of its dislocation
structure, formation of nanosize subgrains, and elevation of
the level of microstresses.
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