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J Jmatprotec 2006 03 119
J Jmatprotec 2006 03 119
J Jmatprotec 2006 03 119
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
∗ 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
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)
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
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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