J Jmatprotec 2006 03 119

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Journal of Materials Processing Technology 176 (2006) 140–145

Effects of the surface temperature and cooling rate on the residual


stresses in a flame hardening of 12Cr steel
M.K. Lee ∗ , G.H. Kim, K.H. Kim, W.W. Kim
Nuclear Nanomaterials Development Team, Korea Atomic Energy Research Institute, P.O. Box 105, Yuseong, Taejon 305-353, South Korea
Received 30 July 2004; received in revised form 10 May 2005; accepted 15 March 2006

Abstract
The residual stress properties of low carbon 12Cr steel, currently used as a nuclear steam turbine blade material, generated by flame hardening
have been studied with respect to both the surface temperature and cooling rate. The residual stress state generated by flame hardening was
dominated by two opposite competitive contributions, they are, tensile stress due to a phase transformation and compressive stress due to a thermal
contraction. As both the surface temperature and cooling rate increase at temperatures above Teq␥ , the increment of the tensile stresses was evident.
It was, furthermore, found that the cracks were nucleated and propagated across the prior austenite grain boundaries during too high temperature
(∼1200 ◦ C) and rapid cooling (∼250 m/s) treatments. This can be explained by a stress relaxation phenomenon, implying a generation of large
tensile stress probably with a value close to or higher than the yield stress of the base material. The optimum processing temperatures required for
the desirable residual stress and hardness were found in the range of 870–960 ◦ C on the basis of the specification of GE power engineering.
© 2006 Elsevier B.V. All rights reserved.

Keywords: Surface treatment; Flame hardening; 12Cr steel; Hardness; Residual stress; Martensitic transformation

1. Introduction toughness and fatigue failures [1–4]. From these investigations it


is commonly recognized that both understanding the generation
Flame hardening process is a useful technique for a surface behavior of the elastic residual stress accurately and controlling
modification that can be readily applied to extend the service the elastic residual stress at a moderate level and with uniformity
life of many machine steel parts such as steam and gas turbines, are of great technological importance in thermal hardening of
gears for paper machinery, rolls for printing and steel working steels.
industries, and various automotive components. Such various Despite the technological importance of achieving the desir-
applications are brought about by the ability to harden regions able residual stress state, many studies have been mostly focused
locally, the simple and easy operation, the high-speed and low- on the improvement of hardness on the surfaces and the automa-
cost processing, and the improved mechanical properties. tion of the flame hardening process [5–8]. In this study, the
One of the major requirements to ensure the practical use generation behavior of residual stresses for low carbon 12Cr
of the flame-hardened engineering parts is realizing the desir- steel used as a nuclear steam turbine blade material has been
able residual stresses within the material. This is because the studied systematically with respect to the surface temperature
level and nature of transient and residual stresses greatly affect and cooling rate during flame hardening, since the edges of steam
the mechanical properties and the qualities of the derived parts. turbine blades must be hardened for protection from signifi-
Associated with this, a number of investigations have shown cant erosion–corrosion problems [9–12] and is thus of particular
that the thermal treatment of steels, if not properly monitored, importance in monitoring of residual stresses within the blade
could induce tensile stresses or stress gradients that make it material. The flame hardening conditions for the desirable resid-
sensitive to a range of failure process such as stress corrosion ual stress states have also been optimized.
cracking (SCC), hydrogen cracking, brittle fracture, fracture
2. Experimental

∗ Corresponding author. Tel.: +82 42 868 8565; fax: +82 42 868 8549. The chemical composition of 12Cr steel was 11.5–12.5Cr, 0.25–0.65Mn,
E-mail address: leeminku@kaeri.re.kr (M.K. Lee). 0.20Mo, 0.05–0.20Nb, 0.12–0.15C, 0.025P, 0.025S, 0.50Si, 0.75Ni, balance

0924-0136/$ – see front matter © 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmatprotec.2006.03.119
M.K. Lee et al. / Journal of Materials Processing Technology 176 (2006) 140–145 141

Fe. It was cut into a shape with the dimensions of 10 mm × 10 mm × 20 mm.


The gases used as a source of the flame were 99% O2 and 96.9% propane
(C3 H8 ) with small amounts of 1.0% ethane (C2 H6 ) and 1.9% butane (C4 H10 ),
and their flow rates were controlled to stabilize the flame properties and to
change the flame intensities. The temperature recording equipment including
a dynamic temperature measurement system and a K-type thermocouple was
used to monitor the thermal cycles of 12Cr steel during the flame hardening.
The surface temperature Ts were taken from the hole located at less than 0.1 mm
from the specimen surface, so that the heating and cooling cycles of the surfaces
of 12Cr steel could be controlled with a high accuracy. Details on the flame
hardening apparatus are found in the previous study [13].
In order to study the residual stresses properties after the flame hardening,
the temperature cycles on the surfaces have been controlled with respect to both
the maximum surface temperature Ts,max and the cooling rate Vc . As shown in
Fig. 1, the processing temperatures Ts,max were varied between 500 and 1200 ◦ C
based on the knowledge of the equilibrium phase transformation of Fe–Cr steel
with 0.1 wt.% carbon [14]. Since this temperature range includes an equilibrium
austenitization temperature Teq␥ of about 805 ◦ C in 12Cr steel, monitoring of
both the thermal and transformation stresses can be possible. Various cooling
methods such as air cooling, forced Ar cooling, and water quenching have also
been employed to control the cooling rate Vc . The Vc was determined from
the range between Ts,max and Ms using a relation (Ts,max − Ms )/(tTs,max − tMs ),
where Ms represents the temperature for the martensite transformation during
cooling. For 12Cr steel Ms is approximately 267 ◦ C as given by the following
equation [15]: Fig. 1. Equilibrium phase diagram of Fe–Cr alloy with 0.1 wt.% carbon
(Kc = Fe3 C, K1 = (Fe,Cr)23 C6 = (Fe,Cr)7 C3 ) [14].
Ms (◦ C) = 561 − 474C − 33Mn − 17Cr − 17Ni − 21Mo (1)

In order to investigate the surface hardening properties, Vickers hardness K␣ radiation. The crystallographic plane used for the residual stress measure-
measurements were performed for the flame-hardened surfaces using a micro- ment was (3 1 0). The analysis was based on the sin2 ψ method [16] for which the
hardness tester (HMV 2000, Shimazu) at a load of 200 gf. More than 10 hardness lattice spacing d3 1 0 was measured at seven different ψ-angles up to ±50◦ with
measurements were made to assure a sufficient confidence in the resulting data. respect to the surface normal. A Young’s modulus (E) = 217 GPa and a Poisson’s
All the metallographic samples were prepared by mechanical grinding to a ratio (ν) = 0.26 were used for the calculation of the residual stresses [17]. Prior
0.3 ␮m finish, followed by etching in a solution of picric acid 4 g, ethanol 96 ml, to X-ray diffraction experiments, electrolytic polishing treatment of thin surface
and HCl 3 ml. The residual stress properties in the surface hardened layer were layers of the flame hardened 12Cr steel was done to remove the surface oxide
characterized using an x-ray diffractometer (X’Pert Pro-MNR, Philps) with a Cu and contaminant layers without introducing any mechanical treatments.

Fig. 2. Temperature cycles as a function of Ts,max , and cooling method: (a) Ts,max < Teq␥ , (b) Ts,max > Teq␥ , (c) Ts,max = 760 ◦ C, (d) Ts,max = 1050 ◦ C, and (e)
Ts,max = 1200 ◦ C.
142 M.K. Lee et al. / Journal of Materials Processing Technology 176 (2006) 140–145

Table 1
Determination of the cooling rate Vc with various cooling methods (Vc was
determined from the temperature range between Ts,max and Ms )

Ts,max (◦ C)

760 1050 1200

Vc (◦ C/s)
Air cooling 4.1 4.2 4.6
Forced Ar cooling 14.8 11.3 15.9
23.6 21.1
Water quenching 213.2 239.9 226.4

3. Results and discussion

3.1. Flame hardening of 12Cr steel

During the flame hardening all the developed temperature


cycles are shown in Fig. 2, where Fig. 2(a) and (b) are the ones
controlled as a function of Ts,max at temperatures below Teq␥
and above Teq␥ , respectively, and Fig. 2(c), (d), and (e) are the
ones for various cooling methods when Ts,max = 760, 1050, and
1200 ◦ C, respectively. The cooling rates Vc determined from
the cooling cycles in Fig. 2(c), (d), and (e) are summarized in
Table 1. In general, the temperature cycle shows a discontinu-
ous curve that consists of a relatively rapid heating stage with
the order of ∼102 ◦ C/s up to the designed temperature, a crit-
ical peak point because of a sudden drop of the heat flux, and
finally a cooling stage. This is typical for the thermal character-
istics of the flame hardening process. Those temperature cycles
show that all the surfaces of 12Cr steel were accurately con-
trolled as a function of the designed temperature and cooling
rate.
Fig. 3. (a) Residual stress and (b) hardness properties of 12Cr steel as a function
3.2. Effects of maximum surface temperature (Ts,max ) of Ts,max after flame hardening followed by air cooling.

In the thermal treatment of steels the sign and amount of the


residual stress can be determined by the two competitive con- 12Cr steel showed initially tensile stress of about 100 MPa with
tributions: one is by the thermal stress and the other is by the a hardness of 260HV0.2 as designated in Fig. 3(a) and (b). It
transformation stress. The thermal stress is generated by the tem- is found that such level of tensile stress decreases gradually
perature difference between the surface and the interior of the with increasing Ts,max up to 760 ◦ C and finally almost stress-
material during cooling, which is actually compressive because free state. At the temperatures below Teq␥ all the samples have
the surface is more rapidly cooled with more contraction, com- almost similar hardness with the base value ∼260HV0.2 of the
pared to the interior of the material. On the contrary, the transfor- as-received 12Cr steel. This result shows clearly a dominant
mation stress comes from the phase transformation of austenite contribution of the thermal stress component at these temper-
into martensite during cooling, and is intrinsically tensile. This atures as predicted. Although martensite transformation occurs
is due to the trapped carbon atoms in the set of octahedral sites, with a hardness enhancement (∼430HV0.2 ) for Ts,max = 850 ◦ C
which creates the tetragonality of the martensitic crystal struc- (>Teq␥ ), a generation of a large amount of compressive stress is
ture and substantial tensile strains with displacements of the notable, indicating that the thermal stress component still con-
nearest neighboring iron atoms [15]. Therefore, understanding tributes more dominantly compared to the transformation stress
the influences of these two opposite stress contributions on the component. As Ts,max increases further, however, the residual
final residual stress state are of primary importance in both con- stress shows a transition from a compressive to a tensile stress
trolling the residual stresses and achieving the desirable stress by showing a linear dependence on Ts,max . This can be explained
state in the material. by the enhanced transformation stress effect resulting from dis-
Fig. 3(a) and (b) show the variations of the residual stress and solution of carbides and formation of martensite crystals. The
hardness, respectively, as a function of Ts,max after flame hard- hardness is also linearly increased up to 1150 ◦ C, but a slight
ening of 12Cr steel followed by an air cooling. The as-received decrease in the hardness at Ts,max = 1200 ◦ C can be explained by
M.K. Lee et al. / Journal of Materials Processing Technology 176 (2006) 140–145 143

Fig. 4. SEM views of the flame-hardened surfaces of 12Cr steel as a function of Ts,max (PAGB: prior austenite grain boundary).

the effect of rapid grain growth of austenite crystals after the full 3.3. Effects of cooling rate (Vc )
dissolution of carbides, as will be demonstrated below in Fig. 4.
In this study the optimum flame hardening condition has also Dependence of the cooling rate Vc on the residual stress
been established for achieving the desirable residual stress and and harness properties in a flame hardening of 12Cr steel is
hardness on the surface, as pointed out earlier. For this, the speci- seen in Fig. 5(a) and (b), respectively. The Ts,max has been
fications of GE Power Generation Engineering were introduced, controlled at 760, 1050, and 1200 ◦ C to study the behavior of
where the acceptance criteria suggest a compressive stress range both the thermal and transformation stresses below and above
of 140–550 MPa and a hardness at least more than 390HV [18], Teq␥ . For Ts,max = 760 ◦ C below Teq␥ an increase of the com-
as illustrated in Fig. 3(a) and (b), respectively. According to these pressive stress was remarkable with increasing Vc , but there
criteria, it is found that the flame hardening should be carried was no increase in the hardness with an almost constant value
out in the range of approximately 870–960 ◦ C in Ts,max . (∼260HV). This is due to the effect of a thermal stress contribu-
Fig. 4 shows SEM views for the etched surfaces of 12Cr tion, since the higher the cooling rate, the higher the temperature
steel prepared as a function of Ts,max . For Ts,max < Teq␥ , the as- gradient between the surface and the interior of the material. On
received microstructure exhibiting tempered-martensite struc- the contrary, at the temperatures above Teq␥ the tensile stress
ture with very fine carbides was retained regardless of Ts,max (see increases with increasing Vc . Such behavior can be explained
Ts,max = 530, 760 ◦ C). In the temperatures above Teq␥ , however, by the autotempering effect. In low carbon steels with rela-
a distinct decrease in volume fraction of carbides was observed tively high Ms temperatures above room temperature, carbon
due to dissolution of carbides into matrix. For Ts,max = 1150 and mobility is sufficiently high enough to cause carbide precipita-
1200 ◦ C the carbides were almost dissolved in the matrix but the tion in the martensite even during quenching [15]. Therefore,
existence of small amount of undissolved carbides indicates an the faster cooling rate reduces the autotempering time and the
insufficient time for a full dissolution of the carbides because resultant carbide precipitation. Consequently the tensile stress
of a very short duration of the process. Compared to the sample increases by enhancing the transformation stress component.
at Ts,max = 1150 ◦ C, a growth of the prior austenite grain (PAG) This explanation is also supported by the increase in hardness
at Ts,max = 1200 ◦ C is remarkable, certifying a slight decrease of with Vc in Fig. 5(b). It is worthwhile, however, to note that for
the hardness in Fig. 3(b). the sample prepared at Ts,max = 1200 ◦ C and subsequent water
144 M.K. Lee et al. / Journal of Materials Processing Technology 176 (2006) 140–145

Fig. 5. (a) Residual stress and (b) hardness properties of 12Cr steel as a function of cooling rate Vc after flame hardening at Ts,max = =750, 1050, and 1200 ◦ C.

quenching the tensile stress was decreased drastically down to a value close to or higher than yield stress (∼590 MPa) of 12Cr
a zero level and appears to be almost relieved. Such a stress steel.
relaxation was attributed to the formation of the cracks, as will A decrease in the volume fraction of the carbides with increas-
be demonstrated in Fig. 6. This means a generation of very ing Vc is observed in Fig. 6 for the samples prepared at temper-
large amount of residual tensile stress that probably approaches atures above Teq␥ , while no variation in the microstructure was

Fig. 6. SEM views of 12Cr steel as a function of cooling rate Vc after flame hardening at Ts,max = 750, 1050, and 1200 ◦ C.
M.K. Lee et al. / Journal of Materials Processing Technology 176 (2006) 140–145 145

Fig. 7. Evolution of fracture of 12Cr steel induced by the flame hardening at Ts,max = 1200 ◦ C and subsequently water quenching: (a) micro-cracks (after one process),
(b) PAGB cracks (after two processes), and (c) material failure (after four processes).

observed at Ts,max = 760 ◦ C. As already discussed above, it is engineering, the optimum processing temperatures required for
noted that the micro-cracks were generated at the condition of the desirable residual stress and hardness were found in the range
Ts,max = 1200 ◦ C and Vc = 226 ◦ C/s. These micro-cracks formed of 870–960 ◦ C.
across either the lath boundaries or prior austenite grain bound-
aries (PAGBs), but many of them appeared along the PAGBs Acknowledgement
that seem to be the most sensitive site to a crack initiation and
growth in this material. This is clearly seen in Fig. 7 that shows This work was supported financially by Ministry of Science
the growth behavior of the micro-cracks formed initially along & Technology (MOST) through National Mid- and Long-term
the PAGBs with applying the residual tensile stress by repeat- Atomic Energy R&D Program (Current Issues of NPPG). The
ing the processing cycle at Ts,max = 1200 ◦ C and Vc = 226 ◦ C/s. authors also appreciate Korea Basic Science Institute (KBSI,
The micro-cracks that were formed initially (Fig. 7(a), after one Daegu in South Korea) for measuring the residual stresses by
process) were propagated and merged into each other across the XRD.
PAGBs (Fig. 7(b), after two processes). When the processing
cycle increases further, a catastrophic fracture occurred finally as References
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