Influence of Shallow and Deep Cryogenic Treatment on the Residual State of Stress of 4140 Steel

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  • 8/10/2019 Influence of Shallow and Deep Cryogenic Treatment on the Residual State of Stress of 4140 Steel

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    Journal of Materials Processing Technology 211 (2011) 396401

    Contents lists available atScienceDirect

    Journal of Materials Processing Technology

    j o u r n a l h o m e p a g e : w w w . e l s e v i e r . c o m / l o c a t e / j m a t p r o t e c

    Influence of shallow and deep cryogenic treatment on the residual state ofstress of 4140 steel

    D. Senthilkumar a,1, I. Rajendran a,, M. Pellizzari b, Juha Siiriainen c,2

    a Department of Mechanical Engineering, Dr. Mahalingam College of Engineering and Technology, Udumalai Road, Pollachi 642 003, Tamil Nadu, Indiab Department of Materials Engineering and Industrial Technologies, University of Trento 38050, Italyc Stresstech Oy, Tikkutehtaantie 1, 40800 Vaajakoski, Finland

    a r t i c l e i n f o

    Article history:Received 8 April 2010

    Received in revised form 13 October 2010

    Accepted 21 October 2010

    Keywords:

    Cryogenic treatment

    Residual stress

    Steel

    a b s t r a c t

    The present research work studies the effect of cryogenic treatment on the residual stress state in4140 steel. Two kinds of cryogenic treatment, namely shallow (SCT, 80 C5 h) and deep cryogenic

    treatment (DCT, 196 C24 h) were carried out between quenching and tempering in conventional

    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

    the precipitation of transition carbides. While conventional heat treatment (CHT) and shallow cryo-

    genic treatment (SCT) promote a tensile state of residual stress, DCT shows a compressive residual

    stress.

    2010 Elsevier B.V. All rights reserved.

    1. Introduction

    In recent years material scientists and engineers devoted their

    efforts in enhancing the fatigue and impact properties of met-

    als by deliberately producing compressive residual stresses in to

    the surface of engineering materials. Residual stresses are the

    stresses that remain within a part after the original cause of

    the stresses (external forces, heat gradient) has been removed.

    Kalpakjian (1985) pointed out that the residual stresses remain

    along a cross-section of the component, even without the exter-

    nal cause. Samant and Dahotre (2008) described thatthese internal

    stresses become evenly balanced by themselves. They existed in a

    free body that had no external forces or constraints acting on its

    boundary.

    Residual stresses are caused by means of load or thermal

    gradients or both. These stresses are developed during differ-

    ent processes like non uniform plastic deformation during cold

    working, shot peening, surface hammering, grinding, welding,phase transformations, and high thermal gradients. Over the past

    few years, much interest has been shown in the properties and

    improvement of compressive residual stress. Knowledge of resid-

    Corresponding author. Tel.:+91 04259236030/236040; fax:+91 04259236070.

    E-mail addresses:kumarsen [email protected](D. Senthilkumar),

    irus [email protected](I. Rajendran),[email protected]

    (M. Pellizzari),[email protected](J. Siiriainen).1 Tel.: +91 04259 236030/236040; fax: +91 04259 236070.2 Tel.: +358 014 333 0037; fax: +358 014 333 0099.

    ual stress in steels is important in the component design field.

    It not only leads to improve fatigue resistance but also improves

    the dimensional stability. It can also lead to improve the con-

    temporary drop in resistance against stress corrosion cracking.

    In polycrystalline and/or multiphase materials, residual stresses

    can be classified as microstresses and macrostresses. Almer et al.

    (1998)stated that the microstresses are formed due to incompat-

    ibilities between grains or between phases and the macrostresses

    are formed by differential plastic deformation over a large scale

    relative to microstructure. Prevey (1996) explained thatthe macro-

    scopic stresses or macrostresses are extended over large distances

    relative to thegrainsize. Macrostresses vary within the body of the

    component over a range larger than the grain size of the material.

    These stresses are of general interest in design and failure analysis.

    Macrostresses are tensor quantities. These stresses are determined

    for a given location and direction by measuring the strain in that

    directionat a single point. Microscopic stresses or microstresses are

    treated as scalarproperties of the material.These microstresses arerelated to the degree of cold working or hardness, and the result of

    imperfections in the crystal lattice. Microstresses arise from vari-

    ations in strain between the crystallites bound by dislocation

    tangles within the grains. They are acting over distances less than

    the dimensions of the crystals. Hoffmann et al. (1997)pointed out

    that the microstresses vary from point to point within the crystals.

    They are producinga range of lattice spacing andbroadening of the

    diffraction peak. These micro-residual stresses are generated dur-

    ing diffusionless martensitic transformation by dislocations and by

    solute carbon atoms remaining in their octahedral sites without

    diffusion.

    0924-0136/$ see front matter 2010 Elsevier B.V. All rights reserved.

    doi:10.1016/j.jmatprotec.2010.10.018

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    D. Senthilkumar et al. / Journal of Materials Processing Technology211 (2011) 396401 397

    During the last decade, cryogenic treatment techniques have

    been developed and are now broadly used by industry to improve

    the mechanical properties of steel components. Barron Randall

    (1974)andHarish et al. (2009)studied that deep cryogenic treat-

    ment of SAE 52100 bearing steel enhances wear resistance.Collins

    and Dormer (1997) investigated the influence 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

    high speed steels. It was proved that deep cryogenic treatment

    can improve wear resistance by the precipitation of nano-sized

    eta-carbides in the primary martensite. It was also observed by

    Stratton (2007). Tamas Reti (2002) found that the amount of

    retained austenite present in steel plays a significant influence

    on the magnitude of the residual stresses and dimensional sta-

    bility. They also pointed out that the effect of retained austenite

    on component performance is still a controversial issue. Some of

    the key factors influencing the retained austenite transformation

    include grain size,quenching temperature, hardening temperature,

    chemical composition, quenching cooling rates, and stress reliev-

    ing or tempering. Retained austenite causes a decrease in tensile

    and yield strength in steels and reduces the maximum achiev-

    able surface compressive stresses relative to the amount of this

    phase. Tempering at sufficiently high temperature promotes the

    transformation of retained austenite, accompanied by increasedhardness. The contemporary loss in hardness due to the tempering

    of primary martensite partially hides the positive effect of former

    transformation.Alexandru and Bulancea (2002)have pointed out

    that cryogenic treatments have been proposed as a useful method

    to transformretained austeniteprior to temperingand to overcome

    the problems related to austenite stabilization. The transformation

    of retained austenite into martensite influences the residual stress,

    whichwill have an effecton theperformance of thematerial. How-

    ever, Preciado et al. (2006) statedthat because of rather lowamount

    of retainedaustenite (lessthan 15%)left by conventionalquenching

    in the microstructure of alloy steels, it appears that the cryogenic

    cooling would not cause additional microstructure improvements

    comparedto ordinary quenching. So, cryogenic treatments are nec-

    essaryto createa molecularchange in alloy steels, making the mostretained austenite into martensite, a denser, refined mix, smaller

    and a more uniform than austenite. Besides, cryogenic treatment

    would induce the precipitation of very fine carbides of dimensions

    lessthan1m, which occupiesthe microvoids so thatit contributes

    to the increase of both coherence and density within the metal.

    Molinari et al. (2001) studied thatcarbide precipitationoccurs with

    a higher activation energy thus leading to a higher nucleation rate

    which in turn leads to finer dimensions and a more homogenous

    distribution. A new phenomenon referred as tempered martensite

    detwinningoccurred in AISI M2 steel, which showed a reduction

    of twins after soaking at 196 C for 35 h. Deep cryogenic treat-

    ment reduces the wear rate of the hot work tool steel. This result

    was interpreted on the basis of increased toughness, because in

    the presence of delamination, the ability of materials to opposecrack propagation can really increase the mechanical stability on

    the wear surface and load bearing capacity. Therefore, even if the

    deep cryogenic treatment does not influence hardness, it increases

    both toughness and wear resistance. This is usual with no or low

    amount of retained austenite present in steel.

    MohanLal etal. (2001) analyzedthe influenceof cryogenic treat-

    ment on T1 type-high speed steel andconcluded that thecryogenic

    RAW MATERIAL

    CHEMICAL COMPOSITION ANALYSIS

    HARDENING (875C, 1 hour)

    QUENCHING IN

    OIL (30C)

    SHALLOW

    CRYOGENIC

    TREATMENT

    (-80C, 5 hours)

    TEMPERING (200C, 1

    hour)

    DEEP

    CRYOGENIC

    TREATMENT

    (-196C, 24

    hours)

    CHT

    SCT

    DCT

    Fig. 1. Research methodology.

    treatment at 93K, soaking for 24 h, imparts 110% improvement in

    tool life of T1 type high speed steel.

    The main objective of the present work is to evaluate the

    influence of two cryogenic treatments, namely shallow cryogenictreatment (SCT, 80 C for 5 h) and deep cryogenic treatment

    (DCT, 196 C for 24 h) on surface residual stress, hardness and

    impact toughness of 4140 steel. It finds application in axle shafts,

    crankshafts, connecting rods, gears, and many other automotive

    components.

    2. Material and experimental procedure

    The material considered in study was obtained in the form of

    20 mm diameter rod. The composition of the 4140 chrome molyb-

    denum steel was obtained by optical emission spectroscopy (OES).

    The chemical composition of the alloy considered is reported in

    Table 1.The experimental procedure adopted in the present study

    is schematically shown inFig. 1.Samples were subjected to con-

    ventional heat treatment (CHT) consisting of quench hardening in

    oil at 875 C for 1 h. Part of samples was then subjected to shal-

    low cryogenic treatment (SCT)and deep cryogenic treatment(DCT)

    as indicated in Bensely et al. (2007).By shallow cryogenic treat-

    ment the conventionally quench hardened samples were directly

    put in a freezer kept at 80 C and soaked for 5 h to attain ther-

    mal equilibrium. Samples were then extracted and left to reach

    room temperature in air. By deep cryogenictreatment, theconven-

    tionally quench hardened samples were slowly cooled from room

    temperature to196 Cin3h,soakedat196 Cfor24handfinally

    heated back to room temperature in 6 h. All samples were finally

    subjected to tempering or stress relieving at 200 C for 60min.

    X-ray diffraction techniques exploit the fact that when a metal

    is under stress, applied or residual, the resulting elastic strainscause the atomic planes in the metallic crystal structure to change

    their spacing. When a beam of X-rays is incident on a polycrys-

    talline material, crystographic planes diffract X-rays and Braggs

    law n= 2dh k l sinis satisfied, which was put forward by Martinez

    et al. (2003). Here n is an integer indicating the order of diffraction,

    is the X-ray wave length,dh k lis lattice spacing of theh k lplanes,

    and is the diffraction angle on the h k lplanes.

    Table 1

    Chemical composition of 4140 steel (wt%).

    Sample description % C % Si % Mn % P % S % Cr % Mo

    Raw material 0.45 0.35 0.75 0.017 0.019 1.19 0.21

    Uncertainty 0.010 0.013 0.012 0.003 0.007 0.007 0.018

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    Table

    2

    Residualstressmeasurements.

    Sampledescription

    Transversemacrostress

    Phi=0

    (MPa)

    Averagetransverse

    macrostress(MPa)

    Longitudinal

    macrostressPhi=90

    (MPa)

    Averagelongitudinal

    macrostress(MPa)

    FWHM

    Phi=0

    Average

    FWHM

    FWHM

    Phi=90

    AverageFWHM

    Hardness(HRC)

    CHTprior

    tempering

    141.9

    136.9

    107.9

    107.9

    7

    4.3

    7

    4.4

    1

    4.4

    6

    4.4

    8

    60

    134.6

    109.0

    4.4

    3

    4.4

    7

    134.2

    107.0

    4.4

    3

    4.5

    0

    SCTprior

    tempering

    137.2

    125.6

    7

    80.7

    65.2

    6

    5.1

    1

    5.1

    8

    5.1

    8

    5.2

    0

    64

    123.9

    67.4

    5.2

    9

    5.2

    2

    115.9

    47.7

    5.1

    6

    5.1

    9

    DCTprior

    tempering

    148.3

    184.0

    6

    146.5

    175.0

    0

    5.9

    1

    5.7

    5

    5.8

    1

    5.6

    7

    66

    193.3

    208.1

    5.6

    6

    5.6

    2

    210.6

    170.4

    5.6

    7

    5.5

    8

    CHTafter

    tempering

    119.6

    +108.1

    (tensile)

    134.7

    +148.7

    6(tensile)

    2.5

    2

    2.5

    4

    2.5

    8

    2.5

    9

    55

    107.6

    159.8

    2.5

    5

    2.5

    9

    97.1

    151.8

    2.5

    4

    2.6

    0

    SCTafter

    tempering

    19.4

    +19.4

    3(tensile)

    52.3

    +49.8

    3(tensile)

    2.8

    0

    2.7

    4

    2.7

    9

    2.8

    0

    56.7

    18.7

    45.3

    2.6

    6

    2.7

    8

    20.2

    51.9

    2.7

    6

    2.8

    2

    DCTafter

    tempering

    68.8

    69.1

    89.9

    88.5

    3

    4.7

    6

    4.7

    3

    4.6

    9

    4.7

    1

    60.3

    66.6

    89

    4.7

    2

    4.7

    2

    71.9

    86.7

    4.7

    2

    4.7

    1

    In this analysis, X-ray diffraction measurements were car-

    ried out on X-stress 3000 diffractometer (Stresstech Oy/Finland)

    to find out the residual micro- and macro-stresses. This anal-

    ysis has been conducted by using solid-state linear sensor

    technique (MOS, Dual 512 pixels) with a gonimeter in modi-

    fied psi geometry (symmetry side inclination). According to the

    instructions given by Stresstech (2006), X-ray diffraction tests

    were carried out at room temperature in ambient air using

    Cr K radiation for residual micro- and macro-stress measure-

    ments. Cylindrical samples of size 15 mm diameter and 10 mm

    thick were used for the measurements. The purpose of the

    present investigation is to determine surface residual stress after

    CHT, SCT andDCT conditions. Theresidualstresses canbe classified

    into three types based on the length scale. These stresses remain

    homogenous over a large number of grains and equilibrium forces

    are assumed over a large number of crystals. Here uniform strain

    occurs overlarge distances. Macrostresses are stronglyrelated with

    macroscopic structures such as grain boundary area, grain shape,

    grain size, cracks, porosity, and several other features.

    De Oliveira et al. (2007)pointed out that the microstresses are

    given by two distincts. The first one remains homogenous within

    onegrain andtheforces areassumedto bein balance amongadjoin-

    ing grains. The second one is homogenous over some inter atomic

    distances and the internal forces remain in equilibrium aroundcrystalline defects. Microstresses are formed by non-uniform strain

    occurs overshort distances. Thisstrain 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

    by the X-ray diffraction techniques. This technique measures the

    changes in interplanar spacing caused by the residual stress. These

    changes in the crystals (grains) are corresponding to the elastic

    constants and the residual stress of the material. Prevey (1996)

    mentioned that macrostresses produce uniform distortion of many

    crystals simultaneously, shifting the angular position of the diffrac-

    tion peak selected for residual stress measurement.

    The data were obtained at beam angle in the range comprising

    between 45 and 45 and the residual stresses were found outby using the Chi-method (-method) which is derived from the

    classical sin2() method. The test method for residual stress anal-

    ysis by X-ray diffraction is described in SFS-EN 15305 (2008).The

    diffraction peak position was found out by using cross-correlation

    algorithm. Macroscopic stresses are displayed in MPa. Micro-

    scopic stresses are presented as a relative result, by expressing the

    peak broadening. With this kind of measurements, the absolute

    microstress value in MPa would not be obtained. The behavior of

    microstresses is more or less a scalar quantity, apart from vector

    form macroscopic stresses.

    The properties and parameters chosen for the experimen-

    tation are Poissons ratio= 0.3, Youngs modulus = 211,000 MPa,

    diffraction angle = 156.4, and exposure time= 5 s. Due torestricted

    penetration of Cr K radiation in steel (4m), only the stresses inthe outermost surface region could be determined. Hence, stresses

    at 3 locations approximately 120 degree apart were determined

    on the surface of the outer diameter of the samples. Microstruc-

    ture analysis on the CHT, SCT and DCT samples (before and after

    tempering) were examined by using scanning electron micro-

    scope. Furthermore, the tempered CHT, SCT and DCT samples were

    also subjected to Charpy test at room temperature as per ASTM

    standards E23 (2002).

    3. Results and discussions

    The results of the residual stress measurements and the tough-

    ness values for CHT, SCT and DCT conditions are discussed below.

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    3.1. Residual stress

    The micro- and macro-stresses measured in both, longitudi-

    nal and transverse directions, for CHT, SCT and DCT samples are

    tabulated inTable 2.

    1. Residual stress after CHT: Compressive stresses after quenching

    (1372MPa).

    2. Residual stress after SCT (influence of 80 C5 h): No influ-

    ence of SCT in view of the measured experimental scatter

    (12510 MPa).

    3. Residual stress after DCT(influence of196 C24 h): The lower

    temperature and longer soaking time in DCT promote higher

    compressive stresses (18430 MPa).

    Bhadeshia (2002) pointed out that the strains due to phase

    transformations can alter the state of residual stress. It is known

    that the martensitic transformation of a steel component puts the

    surface under compression. It is argued that this is because of the

    expansion at the surface due to formation of the lower density bct

    martensite from fcc austenite.

    Present results highlight that hardness is higher in SCT and

    DCT than in CHT, of 4 and 6HRC, respectively, given inTable 2.As

    proposed byCollins and Dormer (1997),the increase in hardnessproduced by subzero treatment is given by the transformation of

    retained austenite to martensite. After studying most reliable the-

    ories, it is inferred that through the carbon redistribution at low

    temperature, DCT further promotes the formation of nucleation

    sites for subsequent precipitation of large numbers of very fine

    carbide particles, during tempering. This effect has been claimed

    as low temperature conditioning of martensite, which was inves-

    tigated byMeng et al. (1994). Our previous study reports about

    retained austenitepresent in thesamples of 4140 subjectedto CHT,

    SCT and DCT after tempering, respectively, by X-ray diffraction

    techniques. It was reported that 6.5% austenite is retained in the

    CHT sample. After SCT, the retained austenite is reduced from 6.5%

    to 5.1%. Further, after DCT results in a further reduction of retained

    austenite from 6.5% (CHT) to 2.7%. It is found that the SCT andDCT promoted the transformation of retained austenite to marten-

    site and cause an increase in compressive residual stresses. The

    reductionof retained austenitefrom CHTsamples does notdevelop

    compressive residual stressin SCT samples (prior and aftertemper-

    ing) whereas an increase in compressive residual stress is observed

    in DCT samples (prior and after tempering). This is contributed to

    the conversion of available retained austenite to martensite. The

    process of treatingsampleswith shallow cryogenic freezer is totally

    different from deep cryogenic system from the level of temper-

    ature reduction. Cryogenic treatment reduces retained austenite

    and the volume decreases as treatment temperature is lowered.

    Thedecreasein the temperature of cryogenic treatmentwill lead to

    more transformation of austenite to martensite and hence, greater

    compressive residual stress will be developed. The temperatureto which the metal has been cooled is more important than the

    holding time, because of the athermal character of the marten-

    sitic transformation. The transformation of retained austenite to

    martensite is depends on the cooling temperature.Bozidar Liscic

    (1997)pointed out that the further transformation will take place

    only if the temperature is lowered further. However, martensite

    finish temperature (Mf) for 4140 steel should not be lower than

    80 C, so that no difference should be observed between SCT and

    DCT sample; i.e., both treatment temperatures are lower thanMf.

    In light of the present difference stabilization phenomenon has

    to be taken into account.

    Cryogenic treatment is not a final heat treatment process since

    successive stress relieving or tempering is absolutely necessary

    to attain the stress relieving of brittle primary martensite. Avner

    (2003) and Vanvlack (1998) have explained that the tempering

    reduces hardness and residual stress but it increases ductility

    and toughness and also it provides dimensional stability. Data in

    Table 2,evidence a progressive reduction in compressive stresses

    from CHT (+245MPa), to SCT (+145MPa) and DCT (+115MPa),

    respectively. In the case of CHT and SCT samples, tensile stresses

    develop after tempering. The same does not occur in DCT sample,

    where residual macrostresses remain compressive. It is observed

    that the different behavior of CHT, SCT and DCT is not causedby the different amount of retained austenite, because the tem-

    pering temperature is too low to cause the transformation of

    this phase into ferrite and cementite. The influence of cryogenic

    treatment on the martensitic microstructure seems to be the

    sole factor affecting present value of residual stress after temper-

    ing.

    Huang et al. (2003)pointed out that the substantial relief of

    compressive residual stress occurred in the SCT and DCT sam-

    ples after stress relieving or tempering. The reason is due to the

    occurrence of finer carbide precipitates throughout the matrix and

    the loss of tetragonality of martensite. However, the stress relief

    is higher for the CHT sample, which was not subjected to sub

    zero treatment.Grachev (2009)explained that the structural and

    phase transformations can promote the process of shear forma-

    tion and also raise the shear resistance due to hardening of the

    alloy in the process of phase transformations that stabilize the

    structure, as in decomposition of super saturated solid solutions.

    It should be noted that an alloy with less stable structure necessar-

    ily relaxes more intensely than an alloy with more stable structure.

    The rate of transition of the system to a more stable state has great

    importance. Higher relaxation of stresses corresponds to a higher

    rate of transition to a more stable state. The mechanism of this

    process responsible for stabilization of the structure has substan-

    tial significance. This stress is caused by the spatial variation in

    composition and microstructure which leads to different thermal

    contraction and also by the transformation of retained austenite

    to martensite. The martensite needs to be cooled below a certain

    temperature to develop internal stress high enough to generate

    crystal defects. The required long holding time suggests a local-ized carbondistribution occurringby clustering of carbonatoms to

    lattice defects (dislocations). The martensite becomes more super-

    saturated with decreasing temperature. This increases the lattice

    distortion and thermodynamic instability of the martensite, both

    of which drive carbon and alloying atoms to segregate nearby

    defects. These clusters act as or grow into nuclei for the forma-

    tion of carbides when tempered subsequently. Fig. 2 shows the

    martensite microstructure of CHT, SCTand DCTsamples before and

    after tempering. There are no microstructural changes observed

    between CHT, SCT and DCT samples before and after tempering.

    No appreciable differences could be detected by scanning electron

    microscopy. However, the changes in lattice parameters are proved

    by recent in situ neutron diffraction studyindicatingthat the lattice

    parameters a and c of the martensite behave differently duringthe cooling and warming-up processes. The lattice parameter a

    changes with temperature almost linearly, following almost the

    same curve during the cooling and warming-up process, indicat-

    ing that it is not only a pure thermal effect. This was stated by

    Huang et al. (2003). It is inferred from the above result that carbon

    atoms segregation occurredup to 0.2%, during the deepand shallow

    treatment process, which was put forward by Mittemeijer and Van

    Doorn (1983). Because carbon atoms predominantly occupy the

    octahedral or tetrahedral site to the defect regions mainly affecting

    the c lattice parameter. The capacity of carbon atoms to diffuse

    increases as the temperature rises back to room temperature. Dur-

    ingthis stage carbonatoms move along short distance to segregate

    on thetwin crystal surface or on other defects, form fine carbides of

    diameter 2660A leading to relief of residual stress in cryogenically

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    400 D. Senthilkumar et al. / Journal of Materials Processing Technology211 (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 magnification.

    treated samples, as explained inBensely et al. (2008)andHuang

    et al. (2003).

    Microstresses were also estimated by the prediction of full

    width at half-maximum of the peaks (FWHM) from the X-ray

    diffraction patterns of processed samples. FWHM illustrate the

    microstresses and or hardness and plastic deformation. When

    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

    reduction of retained austenite from CHT samples increases both

    compressive microstresses and hardness of SCT samples and DCT

    samples. This is attributed to the transformation of austenite to

    martensite.The untempered samples have the highest microstresses and

    hardness in all the cases but the material is more brittle due to

    the untempered martensite. Hence tempering should be done to

    reduce the brittleness by sacrificing some hardness and tensile

    strength to relieve internal stress and to increase toughness and

    ductility. During tempering, martensite rejects carbon in the form

    of finely divided carbide phases. The end result of tempering is a

    fine dispersion of carbides in the -iron matrix, which bears little

    structural stability to the original as-quenched martensite. Hence,

    the microstressesand hardness of all thesamples are reduced after

    tempering. Itis observedthatthe SCTandDCT ofbothtempered and

    un-tempered samples show increased hardness and microstresses

    when compared with the conventionally treated samples, respec-

    tively.

    3.2. Impact test

    The impact energy for all the samples is tabulated in Table 3.

    In the light of the experimental scatter, CHT, SCT and DCT samples

    have practically the same toughness. However, the slightly higher

    toughness of SCT and DCT must be considered in view of the lower

    Table 3

    Impact energy.

    Conditions Sample

    identification

    Absorbed

    energyJ

    AverageJ

    Raw material (GroupA) A 31 31 1.5B 32

    C 29

    D 32

    CHT (Group B) E 8 8.0 1

    F 9

    G 7

    H 8

    SCT (Group C) J 9 9.5 0.5

    K 10

    L 9

    M 10

    DCT (Group D) N 10 9.5 0.5

    O 9

    P 10

    Q 9

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    D. Senthilkumar et al. / Journal of Materials Processing Technology211 (2011) 396401 401

    amount of austenitein thesesamples,whichcannotbe transformed

    during tempering. Note thatthe transformationof retained austen-

    ite to martensite would eventually cause a reduction in toughness.

    Hence, a compensating effect by cryogenic treatment can be

    hypothesized as, for example, the finer precipitation of transition

    carbidesis promotedby the low temperatureconditioningof marten-

    site. A very interesting result is that very similar impact toughness

    is observed for samples having different HRC. Present results show

    that the higher toughness can be expected after cryogenic treat-

    ment, irrespective from the kind of soaking temperature and/or

    time for SCT and DCT conditions.

    4. Conclusions

    In this work the influence of a post-quench shallow cryogenic

    treatment (SCT, 80 C5 h) and deep cryogenic treatment (DCT,

    196 C24 h) on the residual state of stress of 4140 steel was

    evaluated.

    Similar values of compressive macrostresses were measured

    after quenching and further SCT, while higher stresses devel-

    oped after DCT. The reduction in temperature reduces density

    of lattice defects (dislocations) and thermodynamic instability of

    the martensite, which drives carbon and alloying elements to

    nearby defects. These clusters act as nuclei for the formation offine carbides when stress is relieved or tempered subsequently.

    The precipitation of carbides in tempered SCT and DCT sam-

    ples are responsible for the residual stress relaxation. However,

    the decrease in the temperature of cryogenic treatment will lead

    to more transformation of austenite into martensite and hence,

    greater compressive residual stress willbe developedin the untem-

    peredDCT samples whencompared withSCT andCHT, respectively.

    This study concludes that in 4140 steel maximum compressive

    stresses develop after DCT, before tempering. This was highlighted

    to positively influence the state of stressafterstress relieving. Com-

    pared to tensile stresses observed in CHT andSCT samples, residual

    compressive stresses were found after DCT.

    The toughness of the 4140 steel is not significantly influenced

    by SCTand DCTsampleswithrespect to CHTsamples.However,theexpected drop in toughness for these samples, due to the reduced

    amount of austenite, was not observed. This was interpreted as the

    possible evidence of a low temperature conditioning of martensite,

    leading to a finer transition carbides precipitation during temper-

    ing.

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