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Materials Performance and

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
J_ID: MPC DOI: 10.1520/MPC20140003 Date: 20-March-14
Stage:
Page: 1
Total Pages: 26
PROOF COPY [MPC20140003]

Materials Performance and Characterization
doi:10.1520/MPC20140003
Vol. 3
No. 4
Month 2014
available online at www.astm.org
T. S. Prasanna Kumar,1 B. Hernandez-Morales,2 and G. E. Totten3
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
Indian Institute of Technology,

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 in industrial setups and reports the development of a new portable
toolReference QuenchProbefor estimating cooling rates, hardness, and
microstructure distributions in hardenable steel grades during immersion
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
thickness matching that of the component, which is a departure from standard
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
quench hardenability tests done in the laboratory to industrial practice. To test
12
the suite of mathematical models associated with the Reference QuenchProbe
13
hardware and software, specimens of different grades of steels were
14
instrumented with a single thermocouple near the surface of the specimen.
15
Using the cooling data at the point of measurement, the cooling rates,
16
microstructure, and hardness at other critical locations were computed. An
17
C 2014 by ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA 19428-2959
Copyright V
ID: veeraragavanb Time: 19:39 I Path: S:/3B2/MPC#/Vol00304/140033/APPFile/AT-MPC#140033
Stage:
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KUMAR ET AL. ON REFERENCE QUENCHPROBE
enthalpy-based non-linear inverse heat conduction model was coupled with
18
austenite decomposition models for handling the latent heat liberated during
19
quenching. Several steels ranging from low carbon to medium alloy steels were
20
both end-quenched by water and immersion quenched in several industrial
21
quenchants. The computed hardness of end quenched and immersion
22
quenched specimens were shown to be in good agreement with the measured
23
values. The Reference QuenchProbe is thus shown to generate data needed for
24
heat treatment process design including quenchant selection, which can be
25
directly used in practice.
26
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
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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
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the specimen on the heat uxas a function of surface temperatureduring

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).
Equipment and Test Procedure

Portable, self-contained handheld equipment was designed for acquiring the thermal
response and computing the surface heat ux, cooling rates, hardness, and
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TABLE 1
A comparison between the ASTM D6200 [8] quench probe and the Reference QuenchProbe.
Sl
Number
Test
Standard Quench Probe

(ASTM D6200 [8] and others)
Reference QuenchProbe
(This article)
Cooling Curve Analysis
The probe materials are different from the

steel being heat treated. The results will not
be the same as when a component is
quenched
Same grade of steel as the component. The

results are exact as when the component is
quenched
Effect of viscosity,
oil contamination,
oxidation, usage factor etc
Properties measured in a laboratory under

static conditions; exact inuence of the
properties in practice not known
Done under plant conditions for the specic

steel and quenchant combinations; reects
the true inuence of the quenchant
properties
Data acquisition for

cooling curve analysis
Single thermocouple at center of specimen,

giving only one cooling curve for the entire
sample
Single thermocouple near the surface;

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
Tests done with different thicknesses gives a

measure/prediction of hardenability and
microstructure variation
Selection of quenchant for

different grades of steel
By trial and error based on experience
Data base generated for different quenching

mediums can be used for designing process
sheets for new products
Effect of agitation
Possible with standard apparatus for uniform

ow velocities
Test done under actual, highly turbulent

ows
microstructural variations in the specimen during quench heat treatment in the

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
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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.
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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
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208
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
with the initial condition
225
Tr; z; t Tsoak
at t 0
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and the boundary conditions

@T
qt on S1 ;
k
@r
226

@T
0 on S2
k
@z
Additionally, the thermal history at the thermocouple location is known

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
236
237
238
239
240
2
j1 i1
The incremental ux (Dq)m for updating the heat ux qm is then computed

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
where /j,i is the sensitivity coefcient dened as

^ 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:
246
247
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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
qci dT 1 ftri qLi
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
250
251
252
253
254
255
256
257
258
259
260
261
262
263
264
The heat conduction Eq 1 is nonlinear due to the temperature dependence of both

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
The unknown enthalpy term in Eq 8 is dened by its Taylor series expansion

with iterations within the time step:
268
(9)
Hnm1 Hnm
dHnm m1
Tn Tnm
dT
266
267
269
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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
PHASE TRANSFORMATION MODELING
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.
275
276
277
278
279
280
281
282
283
284
285
286
287
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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
An equivalent time (Fig. 4) which would result in the amount of normalized

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].
312
301
302
303
304
305
306
307
308
309
310
313
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12
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.
Industrial Test Results

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
The cooling curve data obtained at 4 mm from the surface of a 25 mm diameter

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
329
330
331
332
333
334
335
336
337
338
339
340
341
342
343
344
COMPUTED COOLING CURVES AND COOLING RATES AT SURFACE
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.
347
348
349
350
351
352
353
354
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356
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13
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.
SURFACE HEAT FLUX
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.
357
358
359
360
361
362
363
364
365
366
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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
371
372
373
374
375
376
377
378
379
380
381
382
383
384
385
386
387
388
389
390
391
392
393
394
395
396
397
398
Stage:
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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
Stage:
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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.
16
Stage:
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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.
399
400
401
402
403
404
405
406
407
408
409
410
411
412
Stage:
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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
In situ measurement of quenching capacity of different steel/quenching medium combinations

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
416
418
419
420
421
422
423
424
425
426
427
428
429
430
431
432
433
434
435
436
437
438
439
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
Stage:
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19
with the initial condition
453
T Ti r; z at t 0
and the boundary conditions

@T
@T
k
nr k
nz qr; z
@r
@z
454
on the heat flux boundary; S1
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
The net enthalpy of the steel at any temperature is written as

(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
qci dT 1 ftri qLi
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
The energy equation (Eq A4) becomes

@
@T
@
@T
@H
(A7)
k
@x
@x
@y
@y
@t
470
FINITE ELEMENT FORMULATION
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
466
467
468
469
473
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20
T, within the element is assumed to be a linear combination of polynomials of the

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
where the matrix terms are given by
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
Substituting for the differentiated quantity by the linear interpolation function, we

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
is achieved when the temperature eld would converge.
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.
502
503
504
505
506
507
508
509
510
511
512
513
514
515
516
517
518
519
520
521
522
523
524
525
526
527
528
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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
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Materials Performance and

J_ID: MPC DOI: 10.1520/MPC20140003 Date: 20-March-14

PROOF COPY [MPC20140003]

available online at www.astm.org

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

Indian Institute of Technology,

quenching in industrial setups and reports the development of a new portable

toolReference QuenchProbefor estimating cooling rates, hardness, and

microstructure distributions in hardenable steel grades during immersion

thickness matching that of the component, which is a departure from standard

quench hardenability tests done in the laboratory to industrial practice. To test

the suite of mathematical models associated with the Reference QuenchProbe

hardware and software, specimens of different grades of steels were

instrumented with a single thermocouple near the surface of the specimen.

microstructure, and hardness at other critical locations were computed. An

ID: veeraragavanb Time: 19:39 I Path: S:/3B2/MPC#/Vol00304/140033/APPFile/AT-MPC#140033

J_ID: MPC DOI: 10.1520/MPC20140003 Date: 20-March-14

PROOF COPY [MPC20140003]

enthalpy-based non-linear inverse heat conduction model was coupled with

both end-quenched by water and immersion quenched in several industrial

quenchants. The computed hardness of end quenched and immersion

quenched specimens were shown to be in good agreement with the measured

heat treatment process design including quenchant selection, which can be

directly used in practice.

ID: veeraragavanb Time: 19:39 I Path: S:/3B2/MPC#/Vol00304/140033/APPFile/AT-MPC#140033

J_ID: MPC DOI: 10.1520/MPC20140003 Date: 20-March-14

PROOF COPY [MPC20140003]

ID: veeraragavanb Time: 19:39 I Path: S:/3B2/MPC#/Vol00304/140033/APPFile/AT-MPC#140033

J_ID: MPC DOI: 10.1520/MPC20140003 Date: 20-March-14

PROOF COPY [MPC20140003]

the specimen on the heat uxas a function of surface temperatureduring

Equipment and Test Procedure

ID: veeraragavanb Time: 19:39 I Path: S:/3B2/MPC#/Vol00304/140033/APPFile/AT-MPC#140033

J_ID: MPC DOI: 10.1520/MPC20140003 Date: 20-March-14

PROOF COPY [MPC20140003]

Standard Quench Probe

Cooling Curve Analysis

The probe materials are different from the

Same grade of steel as the component. The

Properties measured in a laboratory under

Done under plant conditions for the specic

Data acquisition for

Single thermocouple at center of specimen,

Single thermocouple near the surface;

Tests done with different thicknesses gives a