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Article history: The present research work studies the effect of cryogenic treatment on the residual stress state in
Received 8 April 2010 4140 steel. Two kinds of cryogenic treatment, namely shallow (SCT, 80 C 5 h) and deep cryogenic
Received in revised form 13 October 2010 treatment (DCT, 196 C 24 h) were carried out between quenching and tempering in conventional
Accepted 21 October 2010
heat treatment process. The results evidenced an increase in the compressive residual stress in steel
are subjected to cryogenic treatment before tempering. X-ray diffractometry revealed that residual
stresses are relieved during tempering, according to the redistribution of carbon in martensite and
Keywords:
the precipitation of transition carbides. While conventional heat treatment (CHT) and shallow cryo-
Cryogenic treatment
Residual stress
genic treatment (SCT) promote a tensile state of residual stress, DCT shows a compressive residual
Steel stress.
2010 Elsevier B.V. All rights reserved.
0924-0136/$ see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmatprotec.2010.10.018
D. Senthilkumar et al. / Journal of Materials Processing Technology 211 (2011) 396401 397
During the last decade, cryogenic treatment techniques have RAW MATERIAL CHT
been developed and are now broadly used by industry to improve
the mechanical properties of steel components. Barron Randall
SCT
(1974) and Harish et al. (2009) studied that deep cryogenic treat-
CHEMICAL COMPOSITION ANALYSIS
ment of SAE 52100 bearing steel enhances wear resistance. Collins
DCT
and Dormer (1997) investigated the inuence of deep cryogenic
treatment on D2 cold work tool steel. Dong et al. (1998) stud-
ied the effect of DCT with respect to the microstructure of T1 HARDENING (875C, 1 hour)
high speed steels. It was proved that deep cryogenic treatment
can improve wear resistance by the precipitation of nano-sized DEEP
SHALLOW
eta-carbides in the primary martensite. It was also observed by QUENCHING IN CRYOGENIC
CRYOGENIC
Stratton (2007). Tamas Reti (2002) found that the amount of OIL (30C) TREATMENT
TREATMENT
(-196C, 24
retained austenite present in steel plays a signicant inuence (-80C, 5 hours)
hours)
on the magnitude of the residual stresses and dimensional sta-
bility. They also pointed out that the effect of retained austenite TEMPERING (200C, 1
on component performance is still a controversial issue. Some of hour)
Table 1
Chemical composition of 4140 steel (wt%).
Sample description %C % Si % Mn %P %S % Cr % Mo
56.7
60.3
technique (MOS, Dual 512 pixels) with a gonimeter in modi-
64
66
55
60
5.67
2.59
4.71
5.20
2.80
thick were used for the measurements. The purpose of the
present investigation is to determine surface residual stress after
CHT, SCT and DCT conditions. The residual stresses can be classied
Phi = 90
into three types based on the length scale. These stresses remain
FWHM
4.46
4.47
5.18
5.22
5.19
5.81
5.62
5.58
2.58
2.59
2.79
2.78
2.82
4.69
4.72
4.71
4.50
5.18
5.75
2.54
2.74
4.73
De Oliveira et al. (2007) pointed out that the microstresses are
given by two distincts. The rst one remains homogenous within
one grain and the forces are assumed to be in balance among adjoin-
ing grains. The second one is homogenous over some inter atomic
distances and the internal forces remain in equilibrium around
crystalline defects. Microstresses are formed by non-uniform strain
4.37
4.43
4.43
5.11
5.29
5.16
5.91
5.66
5.67
2.52
2.55
2.54
2.66
2.76
4.76
4.72
4.72
2.80
Phi = 0
FWHM
occurs over short distances. This strain is typically within few grains
or within a single grain of type 2 and type 3, respectively. The
present study measures the micro- and macro-stresses in both lon-
gitudinal and transverse directions with respect to the bar axis
Average longitudinal
+148.76 (tensile)
+49.83 (tensile)
175.00
88.53
classical sin2 ( ) method. The test method for residual stress anal-
ysis by X-ray diffraction is described in SFS-EN 15305 (2008). The
107.9
80.7
67.4
47.7
146.5
208.1
170.4
134.7
159.8
151.8
52.3
45.3
51.9
89.9
86.7
109.0
107.0
(MPa)
89
184.06
69.1
ture analysis on the CHT, SCT and DCT samples (before and after
tempering) were examined by using scanning electron micro-
141.9
134.6
134.2
137.2
123.9
115.9
148.3
193.3
210.6
119.6
107.6
97.1
19.4
18.7
20.2
68.8
66.6
71.9
Residual stress measurements.
scope. Furthermore, the tempered CHT, SCT and DCT samples were
also subjected to Charpy test at room temperature as per ASTM
standards E23 (2002).
Sample description
tempering
tempering
tempering
tempering
tempering
CHT prior
DCT prior
CHT after
DCT after
SCT prior
SCT after
Table 2
3.1. Residual stress (2003) and Vanvlack (1998) have explained that the tempering
reduces hardness and residual stress but it increases ductility
The micro- and macro-stresses measured in both, longitudi- and toughness and also it provides dimensional stability. Data in
nal and transverse directions, for CHT, SCT and DCT samples are Table 2, evidence a progressive reduction in compressive stresses
tabulated in Table 2. from CHT (+245 MPa), to SCT (+145 MPa) and DCT (+115 MPa),
respectively. In the case of CHT and SCT samples, tensile stresses
1. Residual stress after CHT: Compressive stresses after quenching develop after tempering. The same does not occur in DCT sample,
(137 2 MPa). where residual macrostresses remain compressive. It is observed
2. Residual stress after SCT (inuence of 80 C 5 h): No inu- that the different behavior of CHT, SCT and DCT is not caused
ence of SCT in view of the measured experimental scatter by the different amount of retained austenite, because the tem-
(125 10 MPa). pering temperature is too low to cause the transformation of
3. Residual stress after DCT (inuence of 196 C 24 h): The lower this phase into ferrite and cementite. The inuence of cryogenic
temperature and longer soaking time in DCT promote higher treatment on the martensitic microstructure seems to be the
compressive stresses (184 30 MPa). sole factor affecting present value of residual stress after temper-
ing.
Bhadeshia (2002) pointed out that the strains due to phase Huang et al. (2003) pointed out that the substantial relief of
transformations can alter the state of residual stress. It is known compressive residual stress occurred in the SCT and DCT sam-
that the martensitic transformation of a steel component puts the ples after stress relieving or tempering. The reason is due to the
surface under compression. It is argued that this is because of the occurrence of ner carbide precipitates throughout the matrix and
expansion at the surface due to formation of the lower density bct the loss of tetragonality of martensite. However, the stress relief
martensite from fcc austenite. is higher for the CHT sample, which was not subjected to sub
Present results highlight that hardness is higher in SCT and zero treatment. Grachev (2009) explained that the structural and
DCT than in CHT, of 4 and 6HRC, respectively, given in Table 2. As phase transformations can promote the process of shear forma-
proposed by Collins and Dormer (1997), the increase in hardness tion and also raise the shear resistance due to hardening of the
produced by subzero treatment is given by the transformation of alloy in the process of phase transformations that stabilize the
retained austenite to martensite. After studying most reliable the- structure, as in decomposition of super saturated solid solutions.
ories, it is inferred that through the carbon redistribution at low It should be noted that an alloy with less stable structure necessar-
temperature, DCT further promotes the formation of nucleation ily relaxes more intensely than an alloy with more stable structure.
sites for subsequent precipitation of large numbers of very ne The rate of transition of the system to a more stable state has great
carbide particles, during tempering. This effect has been claimed importance. Higher relaxation of stresses corresponds to a higher
as low temperature conditioning of martensite, which was inves- rate of transition to a more stable state. The mechanism of this
tigated by Meng et al. (1994). Our previous study reports about process responsible for stabilization of the structure has substan-
retained austenite present in the samples of 4140 subjected to CHT, tial signicance. This stress is caused by the spatial variation in
SCT and DCT after tempering, respectively, by X-ray diffraction composition and microstructure which leads to different thermal
techniques. It was reported that 6.5% austenite is retained in the contraction and also by the transformation of retained austenite
CHT sample. After SCT, the retained austenite is reduced from 6.5% to martensite. The martensite needs to be cooled below a certain
to 5.1%. Further, after DCT results in a further reduction of retained temperature to develop internal stress high enough to generate
austenite from 6.5% (CHT) to 2.7%. It is found that the SCT and crystal defects. The required long holding time suggests a local-
DCT promoted the transformation of retained austenite to marten- ized carbon distribution occurring by clustering of carbon atoms to
site and cause an increase in compressive residual stresses. The lattice defects (dislocations). The martensite becomes more super-
reduction of retained austenite from CHT samples does not develop saturated with decreasing temperature. This increases the lattice
compressive residual stress in SCT samples (prior and after temper- distortion and thermodynamic instability of the martensite, both
ing) whereas an increase in compressive residual stress is observed of which drive carbon and alloying atoms to segregate nearby
in DCT samples (prior and after tempering). This is contributed to defects. These clusters act as or grow into nuclei for the forma-
the conversion of available retained austenite to martensite. The tion of carbides when tempered subsequently. Fig. 2 shows the
process of treating samples with shallow cryogenic freezer is totally martensite microstructure of CHT, SCT and DCT samples before and
different from deep cryogenic system from the level of temper- after tempering. There are no microstructural changes observed
ature reduction. Cryogenic treatment reduces retained austenite between CHT, SCT and DCT samples before and after tempering.
and the volume decreases as treatment temperature is lowered. No appreciable differences could be detected by scanning electron
The decrease in the temperature of cryogenic treatment will lead to microscopy. However, the changes in lattice parameters are proved
more transformation of austenite to martensite and hence, greater by recent in situ neutron diffraction study indicating that the lattice
compressive residual stress will be developed. The temperature parameters a and c of the martensite behave differently during
to which the metal has been cooled is more important than the the cooling and warming-up processes. The lattice parameter a
holding time, because of the athermal character of the marten- changes with temperature almost linearly, following almost the
sitic transformation. The transformation of retained austenite to same curve during the cooling and warming-up process, indicat-
martensite is depends on the cooling temperature. Bozidar Liscic ing that it is not only a pure thermal effect. This was stated by
(1997) pointed out that the further transformation will take place Huang et al. (2003). It is inferred from the above result that carbon
only if the temperature is lowered further. However, martensite atoms segregation occurred up to 0.2%, during the deep and shallow
nish temperature (Mf ) for 4140 steel should not be lower than treatment process, which was put forward by Mittemeijer and Van
80 C, so that no difference should be observed between SCT and Doorn (1983). Because carbon atoms predominantly occupy the
DCT sample; i.e., both treatment temperatures are lower than Mf . octahedral or tetrahedral site to the defect regions mainly affecting
In light of the present difference stabilization phenomenon has the c lattice parameter. The capacity of carbon atoms to diffuse
to be taken into account. increases as the temperature rises back to room temperature. Dur-
Cryogenic treatment is not a nal heat treatment process since ing this stage carbon atoms move along short distance to segregate
successive stress relieving or tempering is absolutely necessary on the twin crystal surface or on other defects, form ne carbides of
to attain the stress relieving of brittle primary martensite. Avner diameter 2660 A leading to relief of residual stress in cryogenically
400 D. Senthilkumar et al. / Journal of Materials Processing Technology 211 (2011) 396401
Fig. 2. Microstructure of (a) CHT prior tempering, (b) CHT after tempering, (c) SCT prior tempering, (d) SCT after tempering, (e) DCT prior tempering and (f) DCT after
tempering, at 5000 magnication.
treated samples, as explained in Bensely et al. (2008) and Huang 3.2. Impact test
et al. (2003).
Microstresses were also estimated by the prediction of full The impact energy for all the samples is tabulated in Table 3.
width at half-maximum of the peaks (FWHM) from the X-ray In the light of the experimental scatter, CHT, SCT and DCT samples
diffraction patterns of processed samples. FWHM illustrate the have practically the same toughness. However, the slightly higher
microstresses and or hardness and plastic deformation. When toughness of SCT and DCT must be considered in view of the lower
the value of FWHM increases, the hardness of steel also will
be increasing. FWHM values are the average values from psi
angles. The hardness values are also reported in Table 2. The Table 3
Impact energy.
reduction of retained austenite from CHT samples increases both
compressive microstresses and hardness of SCT samples and DCT Conditions Sample Absorbed Average J
samples. This is attributed to the transformation of austenite to identication energy J
martensite. Raw material (Group A) A 31 31 1.5
The untempered samples have the highest microstresses and B 32
hardness in all the cases but the material is more brittle due to C 29
D 32
the untempered martensite. Hence tempering should be done to
reduce the brittleness by sacricing some hardness and tensile CHT (Group B) E 8 8.0 1
strength to relieve internal stress and to increase toughness and F 9
G 7
ductility. During tempering, martensite rejects carbon in the form H 8
of nely divided carbide phases. The end result of tempering is a
SCT (Group C) J 9 9.5 0.5
ne dispersion of carbides in the -iron matrix, which bears little
K 10
structural stability to the original as-quenched martensite. Hence, L 9
the microstresses and hardness of all the samples are reduced after M 10
tempering. It is observed that the SCT and DCT of both tempered and
DCT (Group D) N 10 9.5 0.5
un-tempered samples show increased hardness and microstresses O 9
when compared with the conventionally treated samples, respec- P 10
tively. Q 9
D. Senthilkumar et al. / Journal of Materials Processing Technology 211 (2011) 396401 401
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