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Characterization

T. S. Prasanna Kumar,1 B. Hernandez-Morales,2 and G. E. Totten3

DOI: 10.1520/MPC20140003

Reference

QuenchProbeAn

Alternative Probe Design

for In-Situ Estimation of

Cooling Rates, Heat Flux,

and Hardenability During

Immersion Quenching of

Hardenable Steels

VOL. 3 / NO. 4 / MONTH 2014

Stage:

Page: 1

Total Pages: 26

Materials Performance and Characterization

doi:10.1520/MPC20140003

Vol. 3

No. 4

Month 2014

Reference QuenchProbeAn

Alternative Probe Design for In-Situ

Estimation of Cooling Rates, Heat Flux,

and Hardenability During Immersion

Quenching of Hardenable Steels

Reference

Kumar, T. S. Prasanna, Hernandez-Morales, B., and Totten, G. E., Reference

QuenchProbeAn Alternative Probe Design for In-Situ Estimation of Cooling Rates, Heat

Flux, and Hardenability During Immersion Quenching of Hardenable Steels, Materials

Performance and Characterization, Vol. 3, No. 4, 2014, pp. 124, doi:10.1520/

MPC20140003. ISSN 2165-3992

ABSTRACT

Manuscript received January 9,

2014; accepted for publication

March 7, 2014; published online xx

xx xxxx.

1

Madras 600036, India.

Department de Ingeniera

Metalu

rgica, Univ. Nacional

Auto

noma de Mexico, 04510

Ciudad de Mexico, Mexico.

Department of Mechanical and

Materials Engineering, Portland

State Univ., Portland, OR 97201.

This article reviews some of the limitations of the standard cooling curve

analysis and the Jominy hardenability test in extending the results to actual

quenching, which can be used by the heat treater in the plant. The specimen is

made of the same grade of steel as the quenched component with section

laboratory tests. The test is carried out in the plant under actual conditions

10

dispensing the need to correlate the standard cooling curve data and end

11

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13

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15

Using the cooling data at the point of measurement, the cooling rates,

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17

C 2014 by ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA 19428-2959

Copyright V

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KUMAR ET AL. ON REFERENCE QUENCHPROBE

18

austenite decomposition models for handling the latent heat liberated during

19

quenching. Several steels ranging from low carbon to medium alloy steels were

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values. The Reference QuenchProbe is thus shown to generate data needed for

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Introduction

27

There are two important techniques for obtaining quantitative information to assist

the heat treater in achieving fully hardened steel during quenching viz., the cooling

curve and the Jominy hardenability test. Both tests have been around for nearly 100

years. A cooling curve is the graph obtained by plotting the measured temperature

of a specimen against time at a known location (usually at the geometric center of

the specimen) when the specimen is quenched in a uid medium [1]. Hardicke [2,3]

reported rst published examples of cooling curve characterization of various

quenching media using Le Chateliers 18 mm diameter by 18 mm cylindrical iron

bar probe with a mass of 37 g and a Pt/Pt-Rh thermocouple inserted to the geometric

center. Data acquisition was performed by connecting the thermocouple to a mirror

galvanometer which intermittently monitored the image of the oscillating pendulum

from the galvanometer on to photographic lm.

There are a number of variants of the specimen shape, size and materials,

though the preferred shape is cylindrical. Many of these have been reviewed previously [46]. In addition to ISO 9950 [7], several standards have been developed

including ASTM D6200-01 [8], ASTM D6482-06 [9], and ASTM D6549-06 [10],

which are all based on a 12.5 mm diameter by 60 mm cylindrical Inconel 600 probe

with a Type K thermocouple inserted at the geometric center. Other standard probes

are constructed using silver with a thermocouple at the geometric center such as

ASTM D7646-10 [11] or with the thermocouple positioned at the surface such as

that described in Method A of JIS K 2242 or method which utilized a silver probe

with a center thermocouple [12]. Currently, there is considerable interest in the

standardization and use of a larger Liscic/Petrofer 50 mm diameter by 200 mm cylindrical Inconel 600 probe with three thermocouples; one is placed at 1 mm below the

surface, another 4 mm below the surface, and the third at the center mid-length of

the probe which is proposed for use to characterize the heat transfer properties steel

materials under plant quenching conditions [13,14]. These probes are used in commercially available quenchant testing equipment that utilize electronic data acquisition systems and numerical analysis to provide an insight into the nature of heat

transfer conditions throughout the quenching process using gas, vaporizable liquids,

and molten salts.

The second tool refers to the hardenability information which is obtained in the

laboratory by end-quenching a cylindrical steel piece of a specic grade as described

Materials Performance and Characterization

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KUMAR ET AL. ON REFERENCE QUENCHPROBE

in ASTM A255-10 [15]. The hardness along the length of the specimen, which is a

function of the cooling rate at the location due to end quenching, is measured after

the test is completed. The distance from the quenched-end which gives a hardness

corresponding to 50 % martensite is taken as the hardenability of the steel grade.

The specimen size and the equipment are standardized to ensure identical quenching severity. Since the austenite decomposition depends on the cooling rate and the

metallurgical characteristics of the steel, the hardenability will reect the ease with

which martensitic structure could be obtained in practice. The test gives an indication of the comparative ability of different steels to undergo martensitic

transformation.

This article addresses some of the limitations of the standard cooling curve analysis procedures and the Jominy hardenability test in extending the analysis to actual

quenching in industrial setups and how by suitable design of a new system, the limitations can be overcome.

ASTM D6200 covers acquisition and interpretation of cooling curves for oil

quenching [8]. An Inconel probe of standard dimensions is heated to the austenitizing temperature and quenched in a vessel containing a specied amount of the oil

sample. The temperature at the center of the specimen is measured by a thermocouple and parameters such as maximum cooling rate, critical times, etc., computed

from the cooling curve thus obtained. The test parameters serve to compare the performance of a given oil with that of another one, a control sample, or previous performance of the same oil. The test will show the effect of oxidation, the presence of

additives and their concentrations, or contamination on the cooling characteristics

of the quenching oil. It is also known that different grades of steels yield different

hardness values under identical quenching conditions. As such, the cooling curves

obtained from the standard Inconel probe or similar ones using a material different

from the material undergoing heat treatment cannot be used as a guideline for

achieving the desired hardness in the part of interest.

The parameters that affect the cooling rates during quenching include agitation

of the quenchant, thermo-physical-chemical properties of the quenchant such as viscosity, ashpoint, composition, etc [16]. Both the latent heat liberated during phase

transformation and the diffusion of heat in the solid also affect the overall heat

transfer process during quenching. Therefore it becomes imperative to develop techniques for estimating the cooling rates, heat transfer coefcients, and other quality

control parameters under plant conditions specic to the process on hand. Cheng

et al. [17] showed that the heat transfer coefcient had a peak value and its corresponding temperature interval varied with the cross section dimension of the work

piece, quenchant type, and axial position of the specimen being quenched. Sedighi

and McMahon [18] studied the effect of quenchant circulation on the heat transfer

rate during quenching of steels. Maniruzzaman et al. [19] studied the effect of agitation on the quench performance of a mineral oil based quenchant by computing the

effective heat transfer coefcients as a function of surface temperature. The effect of

section size on the surface temperature and heat transfer coefcient during quenching of steel cylinders were studied by Heming et al. [20] and Woodard et al. [21].

The effect of start temperature on boiling water heat transfer was studied during

spray quenching and a method was proposed to predict the boiling curves under different start temperatures by Li et al. [22].The effect of initial soaking temperature of

Materials Performance and Characterization

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KUMAR ET AL. ON REFERENCE QUENCHPROBE

quenching was reported by Babu and Prasanna Kumar [23].

In recent years, simulation of heat treatment processes [2430] has gained

grounds as a precursor to consistent quality control and distortion-free quenched

components. An excellent review on the simulation of quenching is available in Simsir and Gur [25], who dealt with the modeling of heat transfer, metallurgy, and

mechanics of phase transformations in steel during quenching. Quenching as a process involves the simultaneous solution of all these phenomena.

The literature cited above emphasizes the dependence of heat transfer rates on

quenchant circulation, surface nish, surface temperature, soaking temperature, and

quenchant type, among other things. As discussed above, the quench probes normally

used by the heat treating industry for determining the cooling curves are constructed

using a standard material, usually a material that does not undergo phase transformation [1]. The cooling curves obtained with such probes cannot, therefore, be directly

used for computing heat ux for other steel/quenchant combinations. For realistic data

on heat transfer during practical quenching operations, one has to take into account all

the factors mentioned above. Therefore, an acceptable method of measurement of heat

transfer characteristics of a quenchant should be steel-quenchant-process specic.

All of the aforesaid observations with regard to heat transfer conditions existing

during industrial practices using agitated quenchants and those existing in laboratory tests are applicable for hardenability tests as well. Since quenching is steel-quenchant-process specic, any quantitative data on the process will have to be generated

by replicating all the three components of the quenching process, while in the

Jominy end quench test, both the process and the quenchant are different from

actual practice, as the quenchant is always water and the specimen is end-quenched

under standard conditions.

In this paper, these issues are addressed by the use of a hand-held equipment

(Reference QuenchProbe) that is designed to make plant measurements under plant

conditions (quenchant agitation, quenchant type and quality, steel grade, etc.). The

Reference QuenchProbe is designed to use a cylindrical specimen, with varying

diameters to match the section thickness of the component. The length of the specimen is made sufciently large to eliminate the end effects during quenching. The

evolution of the cooling rate distribution is obtained by solving the coupled

enthalpy-based inverse heat conduction and austenite decomposition models starting from the composition specic TTT diagram of the steel sample. Simultaneously

with the cooling rate variations across the thickness, surface heat ux, microstructure, and hardness distributions are also computed which give a measure of the steel

hardenability.

As pointed out earlier, there are a number of disadvantages associated with

using the standard quench probe as per ASTM D6200 [8]. A comparison between

that probe and the one described in this paper shows the advantages of the latter

(see Table 1).

Portable, self-contained handheld equipment was designed for acquiring the thermal

response and computing the surface heat ux, cooling rates, hardness, and

Materials Performance and Characterization

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KUMAR ET AL. ON REFERENCE QUENCHPROBE

TABLE 1

A comparison between the ASTM D6200 [8] quench probe and the Reference QuenchProbe.

Sl

Number

Test

(ASTM D6200 [8] and others)

Reference QuenchProbe

(This article)

steel being heat treated. The results will not

be the same as when a component is

quenched

results are exact as when the component is

quenched

Effect of viscosity,

oil contamination,

oxidation, usage factor etc

static conditions; exact inuence of the

properties in practice not known

steel and quenchant combinations; reects

the true inuence of the quenchant

properties

cooling curve analysis

giving only one cooling curve for the entire

sample

multiple cooling curves at any point in the

cross section obtained by advanced heat

transfer calculations; differentiates cooling

rate at center and surface of specimen

Microstructure and

hardness; hardenability

prediction/measurement

Not possible

measure/prediction of hardenability and

microstructure variation

different grades of steel

mediums can be used for designing process

sheets for new products

Effect of agitation

ow velocities

ows

plant. The test equipment, shown in Fig. 1, has two parts: (i) a hand held portable

unit for measuring the temperature of the probe during quenching and (ii) a vertical

tubular electric resistance furnace for heating the probe. The hand held unit is comprised of a hollow handle attached to a stem manufactured from machined and

welded stainless steel rods/tubes, the specimen made of the same grade of steel being

quenched (which is xed at the end of the stem), a K type mineral insulated, stainless steel sheathed thermocouple xed at a radial distance of 4 mm from the surface

of the specimen at mid-height, a mechanical system for ensuring positive contact of

the thermocouple with the specimen, and a data acquisition system. The electrical

resistance heating furnace, mounted on casters is designed for heating the probe to a

maximum temperature of 1000 C under controlled atmosphere with a P.I.D. temperature controller. Once the specimen is heated to the desired temperature and

soaked, the handheld unit is removed from the furnace and the specimen immersed

into the quench tank. The local temperature is recorded during quenching.

Mathematical Models

The estimation of quench parameters such as heat ux, cooling rate, hardness and

microstructure distribution during quenching of an alloy steel specimen is based on

mathematical models which have been published elsewhere [3133]. The procedure

is based on coupling inverse heat conduction analysis with austenite decomposition

Materials Performance and Characterization

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KUMAR ET AL. ON REFERENCE QUENCHPROBE

FIG. 1

The hand held Reference

QuenchProbe showing the

probe attached at one end,

with a thermocouple xed to

the probe for recording the

time temperature data during

quenching(left). Portable

electric resistance furnace for

heating the specimen to the

soaking temperature before

quenching the specimen in the

tank (right).

models. The input to the model is the time-temperature curve measured at a known

position in the specimen. The mathematical model combines the composition

specic TTT diagram of the steel and empirical hardness models based on local

cooling rate.

The heat transfer phenomena on the surface of the component being quenched

in a uid is quite complex, with lm boiling followed by nucleate boiling occurring

at high and medium surface temperatures; at lower surface temperatures, the heat

transfer takes place by pure convection through a boundary layer. A review of methods used for analyzing heat transfer during quenching has been published recently

[34]. Boundary heat ux estimation during any thermal process is an ill-posed

inverse heat conduction problem (IHCP). When a solid body is subjected to heating

or cooling due to a uid, the heat transfer mechanism at the solid/uid boundary

can be extremely complex. Particularly with reference to immersion quenching,

there are different regimes operating at distinct temperature ranges. The IHCP simplies the problem by analyzing the result of any such complex causes in that it

is based on the solution to a specic time-temperature history at a given location

inside the solid body. Prasanna Kumar [35] developed an algorithm for estimating

the unknown boundary heat ux, which was shown to be applicable under diverse

situations [32,33,3537]. A detailed validation of the IHCP algorithm for a 2D

quenching case can be found in Ref. [38].

Estimation of heat transfer coefcients during quenching requires the accurate

measurement of surface temperature also. Due to experimental difculties it is common practice to embed a thermocouple very near the surface. It is quite well known

that the temperature gradients near the surface will be quite steep for high heat

transfer processes like quenching which makes such surface temperature measurements unacceptable. The specialized LiscicNanmac probe also has limitations as

the thermal eld around the point of measurement is inuenced by the construction

of the probe [39]. The inverse algorithm overcomes these difculties mathematically.

Materials Performance and Characterization

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KUMAR ET AL. ON REFERENCE QUENCHPROBE

FIG. 2

The solution domain in

cylindrical axi-symmetric

coordinates showing an

example of the FE mesh.

The solution gives both the unknown heat ux at the surface and the thermal eld

as functions of time at all nodes simultaneously. Thus, the transient surface temperature can be accurately computed, even with a single thermocouple measurement

inside the specimen.

During alloy steel quenching the steels undergo phase change at various rates

which requires concurrent solutions to the two phenomena of heat transfer and austenite decomposition. The details of combining the IHCP with the TTT diagram of

the steel of interest can be found in Refs. [35,36].

AN IMPLICIT ENTHALPY BASED INVERSE HEAT CONDUCTION MODEL

201

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209

The heat transfer in the specimen during immersion quenching was modeled in the

cylindrical coordinate system, assuming symmetry about the longitudinal axis, with

the heat ux at the boundary treated as an unknown quantity. Graded, 4-node isoparametric toroidal elements were used for meshing the middle 10 mm of the specimen, where the thermocouple tip was positioned, at 4 mm depth from the specimen

surface. An example of the FE mesh is shown in Fig. 2.

Initial efforts in modeling the IHCP during quenching were based on treating

the latent heat as a source term [35,36]. It was observed that handling the source

term could lead to instabilities; therefore, the present work incorporates the latent

heat through the implicit non-linear enthalpy model due to Swaminathan and Voller

[40]. Application of a semi-implicit analysis for simulation of freezing of water can

be found in [41], which was extended in this work with a fully implicit formulation

(see the Appendix).

The heat transfer in the specimen during quenching was modeled using the heat

conduction governing equation written in terms of enthalpy:

@

@T

@

@T

@H

k

(1)

@r

@r

@z

@z

@t

210

225

Tr; z; t Tsoak

at t 0

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KUMAR ET AL. ON REFERENCE QUENCHPROBE

@T

qt on S1 ;

k

@r

226

@T

0 on S2

k

@z

Tro ; z0 ; t Tmeas t ;

t 0 < t tend

where:

Tsoak the soaking temperature,

q(t) the unknown heat ux at the boundary during quenching, and

Tmeas (t) the measured thermal response at the thermocouple position dened

by the coordinates (r0,z0).

The unknown heat ux is vectorized into qi; i 1, 2,, m,, n. For a given calculation, the heat ux is treated as constant over a small time interval, Dt. The

inverse algorithm is to estimate qm assuming qi; i 1,, m 1 are known (already

determined). The mth time step is the current time step. Similar to heat ux components, the continuous thermal histories measured during experiments are discretized

and denoted by Yj(i); j 1, 2,, s and i 1, 2,, n, where s is the number of temperature measurement locations, which in the present case is equal to one. Following

Ref. [21], the objective function for minimization is chosen as

(2)

s X

r

X

227

^

Yj;mi1 T

j;mi1

228

229

230

231

232

233

234

235

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237

238

239

240

2

j1 i1

from the expression given below

241

242

s X

r

X

^j;mi1 /j;i

Yj;mi1 T

(3)

Dqm

j1 i1

s X

r

X

/j;i

2

j1 i1

^ T

^j;i

T

j;i

/j;i

(4)

Dqi

^ , is given by

The temperature corresponding to an increment in heat ux, T

j;i

(5)

244

q

qm1

^ Tj;i m;;mr1

T

j;i

q

0

m;;mr1 1 eqm1

^j;i , is dened by

and the temperature corresponding to the base ux, T

(6)

243

245

^j;i Tj;i qm;;mr1 qm1

T

The volumetric enthalpy term, H, was modelled as the sum of the enthalpies of

the mixture of phases present at any time step as follows:

Materials Performance and Characterization

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FIG. 3

A typical graph of enthalpies of

the initial (austenite) and a

product phase (ferrite) for an

alloy steel undergoing phase

change [42].

(7)

Hi

X T

T0

where the superscript refers to the transformation product, T0 is any reference temperature and the subscript tr refers to the fraction transformed.

In the context of modeling alloy solidication [40,41], the enthalpy term would

explicitly involve the latent heat term at temperatures up to solidus. Generally, the

solidication range is determined based on composition and the corresponding

phase diagram with the latent heat modeled as a function of fraction solid. With

solid state transformation, as in alloy steel quenching, the transformation beginning

and end can extend over different ranges depending on cooling rates. The transformation fractions can also vary widely.

As the austenite starts decomposing into other phases, the net enthalpy of the

mixture decreases since the enthalpy of any phase resulting from the decomposition

is smaller than that of austenite at that temperature. The enthalpies of different

phases as a function of temperature are shown in Fig. 3, taken from JMatPro [42],

for a typical steel. Starting from fully austenitic phase with the highest enthalpy, the

enthalpy of the mixture always diminishes, thus accounting for latent heat

liberation.

FINITE ELEMENT FORMULATION

248

249

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252

253

254

255

256

257

258

259

260

261

262

263

264

the enthalpy and the thermal conductivity terms. Following the normal Galerkin

nite element procedures, Eq 1 was discretized as:

K n1 fT gen1 C H_ n1 fF gn1

(8)

265

with iterations within the time step:

268

(9)

Hnm1 Hnm

dHnm m1

Tn Tnm

dT

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10

where:

n the time step, and

m the iteration within the time step.

The global set of equations now take the form for an iteration within the time

step

K m

n

270

271

272

273

274

m

m

1

dH

1

dH

m

m

f

T

g

f

H

g

f

H

g

fT gm1

fF gm

C

C

n

n

n

n

n

Dt

dT n

Dt

dT n

(10)

The matrix [K] and the force vector {F} are computed for each itreation using

the converged values of temperatures at the previous iteration. The iterations were

continued until the end condition dened by the tolerance dened by Eq 11 was

achieved.

!

fH gm

fH gm1

n

n

abs

(11)

< 0:001

fH gm1

n

The heat transfer is coupled with austenite decomposition through the enthalpy

term appearing in Eq 1, which requires the modeling of austenite decomposition. As

a rst step towards this aim, the TTT diagram of the steel was digitized and used in

the software for computation of phase transformation. A schematic of the methodology adopted for tracking the austenite decomposition using well-known formulae

for diffusional [43] and non-diffusional [44] transformations is given in Fig. 4.

Scheils additivity rule was invoked for marking the beginning of measurable

amounts of fraction transformed (0.01), given by

(12)

m

X

Dtj

1

t

Tj

s

j1

FIG. 4

Schematic representation of

the technique applied to obtain

the CCT diagram from the

composition specic TTT

diagram of the steel and

measured/computed cooling

curves.

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11

where m gave the starting point for the computation of real fraction of transformed

product starting from the mth time step, the normalized fraction product was

computed as the ratio of the real fraction transformed until that time step and the

equilibrium fraction of that product at that temperature.

i

Xnorm

Tm

(13)

(14)

291

292

293

294

1

i

ln 1 Xnorm

Tm nTm1

bTm1

i

Xnorm

Tm1

1 exp bTm1

i

teq

Dt

295

296

nTm1

From which, the real fraction of the ith phase forming at the temperature step is

calculated using

(16)

290

The new normalized fraction at the end of the present time step is then calculated by

(15)

289

i

Xreal

Tm1

i

Xeqbrm

T m

fraction at the present time step is computed from an inverse relation of JMAK

equation given by

i

teq

288

297

298

i

i

i

Tm1 Xnorm

Tm1 Xeqbrm

Tm1

Xreal

CRITICAL TEMPERATURES

299

For computing austenite decomposition into its product phases by the aforementioned approach, two important pieces of information are necessary: (i) the critical

temperatures Ae3, Ae1 associated with the TTT diagram, and (ii) those associated

with the equilibrium diagram. It is observed that the critical temperatures obtained

from these two approaches never match. However, for estimating austenite decomposition, it is important to ensure consistency in the critical temperatures obtained

from the TTT diagram and the FeC equilibrium diagram, as the kinetic parameters

in the JMAK equations are linked to the equilibrium phase quantities read from the

FeC equilibrium diagram. To ensure this, the procedure adopted by Prasanna

Kumar [23] for dening the phase boundaries in the FeC equilibrium diagram was

used.

300

MATERIAL PROPERTIES

311

The true fractions of all the phases were summed and the remaining austenite fraction was computed for each element at the end of each time step. The thermal conductivity and enthalpy properties were computed as sums of the contributions of the

individual fractions of phases present in the element at the time step. The properties

of individual phases were taken from the commercial software JMatPro as explained

elsewhere [36].

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HARDNESS MODELING

318

In general, a mixture rule based on the amounts of the phases formed and their

hardness is used for predicting the macro hardness of the quenched steel. Maynier

et al. [45] developed regression equations for the hardness of various phases as function of the chemistry and cooling rates at 700 C. However, their equations depended

only on the nal amounts of the phases. In this work, the hardness w of the phases

that are forming isothermally at each time step during transformation of austenite

was taken from the TTT diagrams for the respective steel grades. A step-wise linear

model was developed from the data as a function of temperature. The hardness due

to continuous cooling was written based on the rule of mixtures as

319

(17)

we

XX

j

320

321

322

323

324

325

326

327

wij DXji

where the hardness of the fractional ith phase at the jth time step was summed continuously to get the macro hardness of the eth element.

The Reference QuenchProbe was used under industrial quenching environments for

a combination of several alloy steels and quenchants. Cylindrical specimens 25 mm

diameter by 100 mm long, made of hardenable grade steels C45, 41Cr4, 100Cr6,

8822 H, SA 542, 52 100, 4140, SUP 9 were heated to normal soaking temperatures

and immersed in agitated tanks containing Servo 707, Castrol 798, Nippon 303, or

Hardcastle Polymer solutions (4.5 %, 6.0 %, 13.5 %, 14.0 %). Some of the results

obtained are given below.

MEASURED COOLING CURVES

probe made of three different grades of steels quenching in aqueous solutions of

polymers of different concentrations are shown in Fig. 5. The complex interaction

between the thermal diffusivity of the steel, the heat transfer characteristics of the

quenchant at different regimes of heat transfer, and the rate of latent heat liberation

affect the cooling curves as shown in the gure.

328

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330

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333

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335

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339

340

341

342

343

344

345

AND CORE

346

The Reference QuenchProbe is used to obtain the cooling curves at the surface and

the core of the specimen which can reveal the differential cooling rates across the

section as well as the surface phenomena. Figure 6 shows the cooling curves obtained

by measurement as well as by computation in a 41Cr4 steel quenched in a polymer

solution under agitation.

The surface temperature brings out clearly the latent heat effects due to martensitic transformation at around 300 C, at which temperature the heat removal rates

of the uid is quite low resulting in slower cooling rates. The cooling rate as a function of the local temperature is shown in Fig. 7. The onset of the convective regime

in the quenchant starts at 300 C.

Materials Performance and Characterization

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FIG. 5

Cooling curves measured at

4 mm depth from the surface of

a cylindrical specimen of

different grades of steel

quenched in different media.

The surface heat ux computed during quenching of three different grades of steel

samples in four types of quenchants shown in Fig. 8 reveals the very complex nature

of heat transfer in the uid media. The surface heat ux during quenching of alloy

steels in agitated tanks is affected by many factors which cannot be duplicated in the

laboratory. It depends on thermal diffusivity of the steel, the thermal dissipation

mechanism on the uid side, the austenite decomposition rates, intensity of agitation, etc. It is therefore obvious that the heat ux is specic to the steel, quenchant,

and plant conditions. This is well brought out in Figs. 8(a)8(c). It must be noted,

however, that each case refers to different plants.

Figure 8(a) shows the heat ux obtained during quenching of C45 and 41Cr4

grades of steel in similar quenchants (13 % aqueous solution of a polymer) in different plants. The maximum heat ux is around 1 MW/m2 in both the cases, but the

occurrence of peak heat ux at different temperatures brings out the differences in

FIG. 6

A typical set of cooling curves

obtained during quenching of a

41Cr4 grade steel in a 6 %

aqueous polymer solution

during an industrial trial.

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14

FIG. 7

Computed cooling rates at the

surface and core corresponding

to the data shown in Fig. 6.

the steel being quenched. In the case of 52 100 and SUP 9 grades quenched in oil

(Fig. 8(b)), the peak heat ux varies from 0.8 to 1.4 MW/m2, while the peak occurs at

about the same temperature. The inuence of lower concentrations of polymer on

peak heat ux is evident in the case of 41Cr4 grade of steel (Fig. 8(c)).

SURFACE COOLING RATES

The surface cooling rates computed simultaneously with the heat ux are shown in

Figs. 9(a)9(c) for the same cases as shown in Figs. 8(a) and 8(c). Similar observations can be made with reference to the cooling rates, as with heat ux. The maximum cooling rate was around 150 C/s for 41Cr4 quenched in 6 % polymer solution,

while it was around 60 C/s when quenched in 13 % polymer solution. While oil

quenching showed a clear convective regime below 420 C, with low cooling rates,

such distinction could not be made with other quenchants.

The occurrence of peak cooling rate during quenching will affect the products

of transformation and is connected with the TTT diagram, which is brought out in

Fig. 9(a), while in the case of C45 steel, the peak occurs at a higher temperature

(780 C compared to 580 C in the case of 41Cr4 steel) thus promoting ferrite/pearlite. In the case of oil quenching of 52 100 and SUP9 grades, the trends were similar,

with the peak ranging from 58 to 98 C/s. The different regimes of heat transfer were

unaffected by the steel grades studied. Similar observations can be made in the case

of 41 Cr4 steel quenched in two different concentrations of polymer solutions, with

the lower concentration quenchant giving higher cooling rate of 150 compared to

60 C/s with higher concentration quenchant.

HARDNESS ESTIMATION

Apart from the immersion quench tests with several steels and quenchant combinations, three grades of steels, En19, C45, and 8627 H, were end quenched to introduce

a large range of cooling rates in the same specimen. The temperature history at a

point 5 mm from the quenched end was recorded during end quenching and used as

input to the model. Using the mathematical models described in this paper, the heat

Materials Performance and Characterization

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FIG. 8

(a).Computed heat ux at the

surface during quenching of

C45 and 41Cr4 grades of steel

quenched in 13 % polymer

solutions. (b).Computed heat

ux at the surface during

quenching of 52 100 and SUP 9

grades of steel quenched in oil.

(c).Computed heat ux at the

surface during quenching of

41Cr4 grades of steel quenched

in aqueous polymer solutions of

different concentrations.

15

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KUMAR ET AL. ON REFERENCE QUENCHPROBE

FIG. 9

(a).Computed cooling rates at

the surface during quenching

of C45 and 41Cr4 grades of

steel quenched in 13 % polymer

solutions. (b).Computed

cooling rates at the surface

during quenching of 52 100 and

SUP 9 grades of steel

quenched in oil. (c).Computed

cooling rates at the surface

during quenching of 41Cr4

grades of steel quenched in

aqueous polymer solutions of

different concentrations.

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17

FIG. 10

Measured and estimated

hardness of several grades of

steel after end quenching

(EndQ) and immersion

quenching in several media.

ux due to water impingement at the end of the cylindrical specimen was computed

along with the cooling rates at several locations along the length of the specimen

and the hardness. The results of the computed and measured hardness in both

the immersion quenched and end quenched samples are shown in Fig. 10. The

computed hardness along the length of the end quenched specimens and across the

section of immersion quenched specimen were shown to be in good agreement with

the measured values which validates the procedure.

ERROR ESTIMATE

Like any numerical technique based on the nite-element method, the accuracy of

the calculation depends both on the domain discretization and time step size. An

estimate of the error in the computation during quenching of a C45 steel specimen

in mineral oil is given in Fig. 11 for the discretization scheme shown in Fig. 2 and two

time steps, viz., 0.5 and 0.1 s. The maximum percentage error in the estimated

temperature at the thermocouple location coincided with the occurrence of the

FIG. 11

Error in the estimation of

recorded temperatures at the

thermocouple location for

different time step values

during quenching of a C45

specimen in mineral oil.

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18

maximum heat ux in all the cases. It was seen that the maximum error could be

brought down to less than 0.5 % with a time step of 0.1 s, while the value was nearly

2.25 % for a time step of 0.5 s. Considering that the calculations were CPU intensive,

a time step of 0.5 s was chosen for all cases.

Summary

Checking the effect of agitation level/ow rate/quenching position in the tank

Checking the effect of contamination and property variations in quenchants

directly in the tank

Estimating the cooling rates at the surface and core of specimens

Predicting microstructure/hardness at the surface and core

Selecting the most suitable quenchant for a given component to achieve the

required hardness range under actual conditions in the plant

Generating data for:

mathematical modeling of heat ux for a specic plant condition,

calculating stresses in quenched component by nite element analysis, and

reducing distortion due to quenching.

Appendix

415

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419

420

421

422

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429

430

431

432

433

434

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440

441

442

The phase change during quenching of hardenable steels involves latent heat liberation, which will have to be considered for quenching simulation. The implicit

enthalpy method, mentioned briey in the section entitled An Implicit Enthalpy

Based Inverse Heat Conduction Model is a very powerful algorithm for taking into

account the liberation of latent heat during quenching. The enthalpy formulation

considers the temperature dependency of all the properties including thermal conductivity. The nite element formulation of the scheme is therefore elaborated

here.

The partial differential equation describing heat transfer during alloy steel

quenching is written in cylindrical axi-symmetric coordinates as

(A1)

414

417

A portable Reference QuenchProbe using specimens of the same grade of steel as the

component of interest has been developed for in situ testing of cooling rates and

hardenability during immersion quenching of hardenable grades of steels. Using the

time-temperature data recorded during quenching of the sample, the surface cooling

rates at the surface and the surface heat ux density during quenching were calculated by combining Inverse Heat Transfer and austenite decomposition models.

Concurrently with the surface conditions, the cooling rate, microstructure, and hardness variations form the surface to the core were calculated. Deploying the Reference

QuenchProbe in industrial heat treatment plants, tests done for several alloy steels

during quenching in several industrial quenchants, it was shown that the Reference

QuenchProbe could be effectively used for:

413

@

@T

@

@T

@T

Q qc

k

k

in X

@r

@r

@z

@z

@t

443

444

445

446

447

448

449

450

451

452

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19

453

T Ti r; z at t 0

and the boundary conditions

@T

@T

k

nr k

nz qr; z

@r

@z

454

where k, q, and c are the thermal conductivity, density, and specic heat of the material, which are functions of the phase and temperature T. The term Q represents the

rate of heat generation due to latent heat release. In what can be considered as the

most general and straight forward treatment of latent heat, the source term in Eq A1

is written as

Q qL

(A2)

457

458

459

460

461

462

463

@

@T

@

@T

@ftr @T

k

k

q cL

@T @t

@r

@r

@z

@z

(A5)

456

@ftr

@ftr @T

qL

@t

@T @t

where:

L the latent heat of transformation of austenite, and

ftr the fraction of austenite transformed into different phases.

We can now write the energy balance equation as:

@

@T

@

@T

@ftr @T

@T

qL

(A3)

k

k

qc

@T @t

@r

@r

@z

@z

@t

(A4)

455

Hi

X T

T0

464

where:

superscript i the transformation product,

subscript fr the transformed amount, and

T0 any reference temperature.

Differentiating the above equation with respect to T, we obtain

@H

@ftr

(A6)

q cL

@T

@T

465

@

@T

@

@T

@H

(A7)

k

@x

@x

@y

@y

@t

470

471

The nite element formulation of the above equation (Eq A7) can be conveniently

obtained from the Galerkin formulation. The distribution of the dependent variable,

472

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473

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20

form

T e r; z; t

s

X

474

475

wi r; zTi t

i1

where:

s the number of nodes assigned to element e, and

Ti the nodal temperatures.

wi are the interpolation or shape functions, the form of which is governed by

the order of the element. With the assumed distribution of the temperature over the

element and following the standard Galerkin procedure, the discretized element

equation is obtained in the form

Ce H_ K e fT ge fF ge

(A8)

476

483

Cij

Kij

Xe

Xe

481

482

484

qwi dC

The set of rst order ordinary differential equations in Eq A8 is rendered into a set

of linear algebraic equations by applying weighted average approximations to the

differentiated quantity. The interpolation is linear, dened by

485

486

487

fH gn1 fH gn

h H_ n1 1 h H_ n

Dt

where the subscript n refers to the time step number. The choice of the value of h

leads us to the various difference schemes. With h 0 and observing that [C] is

independent of temperature, we get the implicit scheme, i.e.,

488

489

490

K n1 fT gen1 C H_ n1 fF gn1

get the global set of equations

K n1 fT gn1 C

491

492

fH gn1 fH gn

fF gn1

Dt

The unknown enthalpy term in Eq A11 is dened by its Taylor series expansion

with iterations within the time step:

(A12)

480

wi wj dX

C1

(A11)

479

@wi @wj

@wi @wj

k

k

dX

@r @r

@z @z

Fi

(A10)

478

and

(A9)

477

Hnm1 Hnm

dHnm m1

Tn Tnm

dT

493

494

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21

Hnm1 Hnm

(A13)

dHnm m1 dHnm m

T

T

dT n

dT n

With this substitution in Eq A10, the global set of equations now take the form for

iteration within the time step:

K m

n

495

496

m

m

1

dH

1

dH

m

m

fF gm

H

H

C

C

fT gm1

f

g

f

g

f

g

n

n

n

n

n

Dt

dT n

Dt

dT n

(A14)

The matrix [K] and the force vector {F} are computed for each iteration using the

converged values of temperatures at the previous iteration. The iterations are continued until the end condition dened by the tolerance.

(A15)

497

498

499

fH gm1

fH gm

n

n

abs

< e

fH gm

n

500

References

501

[1] Totten, G. E., Dossett, J. L., and Kobasko, N. I., Quenching of Steel, ASM

Handbook, Vol. 4A, Steel Heat Treating Fundamentals and Processes, J. L.

Dossett and G. E. Totten, Eds., ASM International, Materials Park, OH, 2013,

pp. 91157.

[2] Le Chatelier, H., Etudes sur la Trempe de Lacier, Rev. Metall., Vol. 1, No. 9,

1904, pp. 473492.

[3] Haedicke, S., Le Chateliers Harteversuche, Stahl Eisen, Vol. 24, No. 21, 1904,

pp. 12391244.

[4] Totten, G. E., Bates, C. E., and Clinton, N. A., Chapter 3Cooling Curve

Analysis, Handbook of Quenchants and Quenching Technology, ASM International, Materials Park, OH, 1993, pp. 69128.

[5] Canale, L., Luo, X., Yao, X., and Totten, G., Quenchant Characterization by

Cooling Curve Analysis, J. ASTM Int., Vol. 6, No. 2, 2009, 101981.

[6] Hernandez-Morales, B., Vergara-Hernandez, H. J., Solorio-Daz, G., and

Totten, G., Experimental and Computational Study of Heat Transfer During

Quenching of Metallic Probes, Evaporatation, Condensation and Heat Transfer, A. Ahsan, Ed., InTech, Rijeka, Croatia, 2011, pp. 4972.

[7] ISO 9950: Industrial Quenching OilsDetermination of Cooling

CharacteristicsNickel-Alloy Probe Test Method, International Organization

for Standardization, Geneva, Switzerland, 1995.

[8] ASTM D6200-01: Standard Test Method for Determination of Cooling Characteristics of Quench Oils by Cooling Curve Analysis, Annual Book of ASTM

Standards, ASTM International, West Conshohocken, PA, 2012.

[9] ASTM D6482-06: Standard Test Method for Determination of Cooling

Characteristics of Aqueous Polymer Quenchants by Cooling Curve Analysis

with Agitation (Tensi Method), Annual Book of ASTM Standards, ASTM International, West Conshohocken, PA, 2012., 2011.

Materials Performance and Characterization

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[10] ASTM D6549-06: Standard Test Method for Determination of Cooling Characteristics of Quenchants by Cooling Curve Analysis with Agitation (Drayton

Unit), Annual Book of ASTM Standards, ASTM International, West Conshohocken, PA, 2012, 2011.

[11] ASTM D7646-10: Standard Test Method for Determination of Cooling Characteristics of Aqueous Polymer Quenchants for Aluminum Alloys by Cooling

Curve Analysis, Annual Book of ASTM Standards, ASTM International, West

Conshohocken, PA, 2010.

[12] JIS K2242: Heat Treat Fluids, Japanese Standards Association, 4-1-24, Akasaka,

Minato-ku, Tokyo 107-8440, Japan, 2012.

[13] Liscic, B. and Filetin, T., Measurement of Quenching Intensity, Calculation of

Heat Transfer Coefcient and Global Database of Liquid Quenchants, MEMI

J., Vol. 19, 2012, pp. 5263.

[14] Liscic, B. and Singer, S., Large Probes for Characterization of Industrial

Quenching Processes, ASM Handbook, Vol. 4A, Steel Heat Treating

Fundamentals and Processes, J. Dossett and G. Totten, Eds., ASM International,

Materials Park, OH, 2013, pp. 176191.

[15] ASTM A255-10: Standard Test Methods for Determining Hardenability of

Steel, Annual Book of ASTM Standards, ASTM International, West Conshohocken, PA, 2010.

[16] ASTM D6710-02: Standard Guide for Evaluation of Hydrocarbon-Based

Quench Oil, Annual Book of ASTM Standards, ASTM International, West

Conshohocken, PA, 2012.

[17] Cheng, M., Cheng, J., Yuan, S. Q., and Zhao, F., Studies on the Heat Transfer

Behaviour of the Interface between Workpiece and Media in the Quenching

Process, Acta Metall. Sinica, Vol. 10, 1997, pp. 479484.

[18] Sedighi, M. and McMahon, C. A., The Inuence of Quenchant Agitation

on the Heat Transfer Coefcient and Residual Stress Development in the

Quenching of Steels, Proc. IMechE Part B, Vol. 214, 2000, pp. 555567.

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