Experimental Heat Transfer

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ISSN: 0891-6152 (Print) 1521-0480 (Online) Journal homepage: http://www.tandfonline.com/loi/ueht20

Comparative Study of Wetting and Cooling

Performance of PolymerSalt Hybrid Quench
Medium With Conventional Quench Media
G. Ramesh & K. N. Prabhu
To cite this article: G. Ramesh & K. N. Prabhu (2015) Comparative Study of Wetting and
Cooling Performance of PolymerSalt Hybrid Quench Medium With Conventional Quench
Media, Experimental Heat Transfer, 28:5, 464-492, DOI: 10.1080/08916152.2014.913088
To link to this article: http://dx.doi.org/10.1080/08916152.2014.913088

Accepted author version posted online: 16

May 2014.
Published online: 16 May 2014.
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Date: 28 September 2016, At: 09:33

Experimental Heat Transfer, 28:464492, 2015

Copyright q Taylor & Francis Group, LLC
ISSN: 0891-6152 print/1521-0480 online
DOI: 10.1080/08916152.2014.913088

COMPARATIVE STUDY OF WETTING AND COOLING

PERFORMANCE OF POLYMER SALT HYBRID QUENCH
MEDIUM WITH CONVENTIONAL QUENCH MEDIA
G. Ramesh and K. N. Prabhu
Department of Metallurgical and Materials Engineering, National Institute of
Technology Karnataka, Srinivasnagar, Mangalore, India
Wetting kinetics, kinematics, and cooling performance of a polymer salt hybrid quenchant
were investigated. The rewetting phenomenon for brine, water, polymer, and polymersalt
hybrid solutions was characterized as rapid uniform, fast non-uniform, slow uniform, and
fast uniform processes, respectively. A dimensionless rewetting time was proposed to assess
the nature of the wetting front. The hybrid quenchant showed higher heat transfer during
vapor and transition boiling and lower heat transfer during nucleate boiling and convective
cooling. The presence of salt in the hybrid solution resulted in early destabilization of the
vapor film and an increase in wetting front velocity and rewetting temperature. The polymer
constituent delayed the rewetting phenomenon.
Keywords quenching, cooling curve analysis, wetting, brine solution, polymer solution,
heat flux transients

INTRODUCTION
Quench heat treatment of steel involves heating the material to the austenitizing
temperature followed by quenching (rapid cooling) in a suitable liquid medium. The
process imparts steel a wide spectrum of microstructures and mechanical properties [1].
Wetting and heat transfer are the two phenomena that occur during immersion quenching
and control the final metallurgical and mechanical properties of components. When hot
metal is immersed into a liquid pool, heat transfer is controlled by different cooling stages
known as the vapor blanket, nucleate boiling, and convective or liquid cooling stages.
Quenching from a high temperature produces a stable vapor film around the surface
of a component. The vapor blanket develops when the supply of heat from the interior to
the surface exceeds the amount of heat needed to evaporate the quenchant. During this
vapor blanket stage, the rate of heat transfer is very slow, as the vapor film acts as an
insulator. The heat flow occurs by radiation and conduction through the vapor phase.
Received 27 September 2013; accepted 20 March 2014.
Address correspondence to Dr. K. Narayan Prabhu, Department of Metallurgical and Materials
Engineering, National Institute of Technology Karnataka, Srinivasnagar, Mangalore, 575025, India. E-mail:
prabhukn_2002@yahoo.co.in
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/ueht
464

POLYMERSALT HYBRID QUENCHANT

465

NOMENCLATURE
z, r
f
T
Cp
t
T
l
r
m
A
DT
u

coordinate direction, m
azimuth angles, 8
temperature, K
specific heat, J/Kg K
time, s
Dimensionless time
thermal conductivity, W/m2K
density, kg/m3
mass, kg
area, m2
temperature difference, K
contact angle, 8

g
CR

surface energy, mN/m

cooling rate, 8C/s

Subscripts
s
solid
l
liquid
v
Vapor
e
equilibrium
wet
wetting
avg
average
max
maximum

Nucleate boiling begins when the surface temperature of the component drops slowly
where when the vapor film starts to collapse, and allowing the liquid to come into contact
with the surface of the component. The liquid in contact with the hot surface boils
immediately, and vapor bubbles leave the work-piece surface. This stage is characterized
by violent bubble boiling, as heat is rapidly removed from the part surface by strong
convection, leading to a significantly higher cooling rate. The final stage of the quenching
(convective cooling) occurs when the temperature of the metal surface is reduced below
the boiling point of the quenchant. During this stage, boiling stops and the heat is
transferred by the direct contact between the surface and the liquid because the metal
surface is completely wetted by the fluid [1 3].
The change from the vapor phase to the nucleate boiling stage is not abrupt, and a
transition occurs when the surface heat transfer coefficient and the amount of liquid/solid
contact increases. This leads to the formation of a wetting front on the component surface.
The wetting front is the interface between film boiling and nucleate boiling. The wetting
front moves on the surface of the component with a significant velocity, resulting in
simultaneous occurrence of all three stages of quenching on the hot metal surface [4]. The
cooling mechanism is strongly influenced by the quench medium used to extract the heat
from the component. Different kinds of quenchants, such as water, brine solutions,
polymer solutions, and mineral oils, are used in heat treating industries. During water
quenching, wetting begins at the lower edge of the sample, and the wetting front ascends to
the top in an almost annular manner. Similar to water, mineral oil also exhibits the same
rewetting phenomenon but with an additional wetting front at the upper edge of the metal
[5]. The cooling mechanisms of brine and polymer quenchant are different. When a piece
of hot metal is quenched in a brine solution, deposition of minute salt crystals and violent
fragmentation of this salt layer occurs on the hot metal surface. This creates turbulence at
the metal/quenchant interface, which destroys the vapor phase, resulting in a very high
cooling rate and uniform rewetting (re-contact of liquid with solid surface by collapse of
vapor film occurs when the supply of heat at the surface is less than the amount of heat
needed to evaporate the quenchant) [6]. However, brine quenching is restricted to
quenching of a simple shaped and low hardenable steel because of intolerable distortion
and quench cracking. During polymer quenching, a polymer-enriched film is formed
around the hot metal, which stabilizes the vapor blanket. As the temperature of the hot
surface decreases approximately to the rewetting temperature (temperature at which the

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G. RAMESH AND K. N. PRABHU

vapor film collapses and the surface is wetted by the liquid; some of the important factors
that influence rewetting temperature during quench hardening are work-piece
characteristics, quenchant characteristics, and quenching facility), the vapor blanket
explosively ruptures, resulting in a pseudo-nucleate boiling process [7,8]. Polymer
quenching results in a longer vapor film stage and uniform cooling. However, lower
cooling rates are obtained with a polymer quenching compared to water and brine
quenching. The extent of distortion of the component is expected to be within the tolerable
limit with polymer quenching. The combined effect of salt and polymer solution additions
on a cooling mechanism during quenching has not yet been investigated.
The cooling performance of the quenchant can be evaluated by a Quenchometer
(magnetic) test, hot-wire test, hardenability test, interval 5-sec test, and cooling curve test [9].
Of these methods, cooling curve analysis has been identified as the most meaningful method
of characterizing the cooling performance of a quench medium. It provides continuous
cooling information throughout the three stages of the quenching process. A cooling curve
analysis involves controlled heating of an instrumented test piece, with thermocouples
embedded at certain locations to about 8608C, followed by its immersion in the quenchant.
The temperature recorded in discrete time increments provides a record of the actual cooling
performance [10]. The wetting kinetics of the quenchant on the surface of the component is
generally assessed by measuring the contact angle formed at the three-phase interface. If a
liquid spreads spontaneously on a given solid surface, it is said to be wetting the solid. If the
liquid beads up into a droplet on a surface, then it is considered to be non-wetting the solid
surface [11]. The experimental technique to characterize wetting kinematics of a quenchant is
generally based on measurement of the thermal response at several locations along a
cylindrical probe near the surface. This information can be used to determine local transitions
from slow to fast cooling, which can then be used to estimate the velocity of the wetting front
[12]. Similarly, high-speed video imaging of the cooling process during probe quenching
gives information about the nature of the wetting front and the type of wetting process [2,13].
The objective of the present work is to carry out a comparative study of wetting kinetics,
kinematics, and cooling behavior of a hybrid solution (water polymer salt) with water,
brine, and polymer solution during immersion quenching of an Inconel 600 probe.
EXPERIMENTAL
Water, brine, polymer, and hybrid solutions were used as quenching media in the
present work. The brine quenchant was prepared by additions of 10 wt% of NaCl salt
(NICE CHEMICALS Pvt. Ltd., Kochi, India) into water. Similarly, the polymer quenchant
was prepared by the addition of 20 vol% of glycol-based Aqua Quench 20 solution (PSG
Intentional, Faridabad, India) in water. The hybrid quenchant was prepared by the addition
of 20 vol% of the Aqua Quench 20 solution and 10 wt% of NaCl salt in water. The
viscosity and thermal conductivity of quenchants were measured using a Brookfield
LVDV-IIIU rheometer (Brookfield Engineering Laboratories, USA) and a KD2 Pro
thermal property analyzer, (Decagon Devices, USA), respectively. A pendant drop method
was used to determine the surface tensions of quenchants. A 2.5-mL syringe with a 0.9 mm
diameter needle having a precision flow control valve was used for this purpose. For
spreading studies, a droplet of quenchant (43 46 mL) was dispensed on to the Inconel 600
substrate. The spreading phenomenon was recorded using a dynamic contact angle
analyzer (Korus Steels, India) (FTA 200; First Ten Angstroms, Virginia, USA). Captured

POLYMERSALT HYBRID QUENCHANT

467

images were analyzed using the FTA 200 image analysis software to determine the
interfacial tension, contact angle, droplet base diameter, and spread area. The standard
deviation for contact angle measurements is less than 18, and the standard deviation for
surface tensions is less than 0.5 mN/m. The surface texture (Ra , 0.684 mm and Rz ,
4.711 mm) of the Inconel 600 substrate was similar to the Inconel 600 probe used for
quenching experiments. The surface texture of the Inconel 600 substrate was similar to the
Inconel 600 probe used for quenching experiments. Both the liquid droplet and Inconel
substrate were maintained at room temperature of 288C during the wetting kinetics
experiment. Humidity and atmospheric condition were maintained using air conditioner.
For cooling curve analysis, two quench probes of 12.5 mm diameter and 60 mm length
were prepared from Inconel 600 material. To assess the axial variations in heat flux transients,
holes of 1 mm diameter were drilled using Electric discharge machining (EDM) at different
heights located at 2 mm from the surface (probe I) as shown in Figure 1a. Holes designated as
A1, A2, A3, A4, A5, A6, A7 and A8 were located at 7.5, 15, 22.5, 30, 37.5, 45, 52.5 and 40
mm ^ 1 mm from the top surface of the quench probe respectively. For determination of heat
flux variations in the radial direction, holes of 1 mm were drilled at different azimuth angles to a
depth of 30 mm ^ 1 mm and were located at 2 mm from the surface (probe II) as shown in
Figure 1b. These holes, designated as R1, R2, R3, R4, R5, R6, R7 and R8, were located at angles
of 08, 458, 908, 1358, 1808, 2258, 2708 and 3158 respectively. Holes of diameter 1 mm (A9 for
probe I and R9 for probe II) were drilled at geometric centers of both probes. Quench probes
were conditioned by heating and quenching in quench oil for several times to obtain reproducible
results. Calibrated mineral insulated K-type Inconel 600 thermocouples (model 219-4450, RS
Components & Controls (India) Ltd, India) of 1 mm diameter and 1 m length were used for
measurement of thermal histories of quench probe. The accuracy of the thermocouple
is ^ 0.58C. The hot junction of thermocouples was tightly fitted into the probe; care was taken to
ensure exact positioning of the hot junction of the thermocouple in the probe by marking the
distance on thermocouple. The other ends of thermocouples were connected to a PC-based
temperature data acquisition system (NI 9213, National Instruments Corp. TX, USA), which has
a 24-bit analog-to-digital converter (ADC) for up to 0.028C measurement sensitivity. The probe
was heated to 8508C in a vertical tubular electric resistance furnace open at both ends and then
transferred quickly to a vessel containing 2 L of quenchant placed directly underneath the

Figure 1. Schematic: (a) quench probe I and (b) quench probe II.

468

G. RAMESH AND K. N. PRABHU

Figure 2. Schematic of experimental set-up.

furnace. The probe temperatures were recorded at a time interval of 0.1 sec during quenching.
The schematic of the experimental set-up is shown in Figure 2. A high performance smart
camera (NI 1774C, National Instruments Corp. TX, USA) was used for online video monitoring
of the quenching process. The scanning rate was three images per second.
The metal/quenchant interfacial heat flux transients were estimated from the
measured temperature histories and thermo-physical properties of the probe material by
solving the inverse heat conduction problem (IHCP). The equations that govern the twodimensional transient heat conduction is given below:
for an axial location:







T
T
;
lr
l

r Cp
r
z
r
z
t





1
T
1
T
T
l
;
lr
r Cp
2
r r
r f
r
f
t

for a radial location:

where r and z are the radial and axial coordinates of the quench probe; l, r, and Cp are the
thermal conductivity, density, and specific heat capacity of the probe material; w is the
radial angle; and T and t are temperature and time, respectively.

POLYMERSALT HYBRID QUENCHANT

469

Figure 3. Solution domain used in IHCP: (a) quench probe I and (b) quench probe II.

The above equations were solved inversely with appropriate initial and boundary
conditions [14] using the finite-element-based TmmFE inverse solver software (TherMet
Solutions Pvt. Ltd., Bangalore, India) for estimating metal/quenchant heat transients.
The mathematical description of the serial solution to the IHCP is given in [15]. Figure 3a
shows the solution domain of the half-symmetrical shape of quench probe I used for
estimation of heat flux components in the axial direction. The geometry was discretized
using four-node quadrilateral and four-side linear uniform mesh. The total number of
elements used was 3,000 (25 120). Figure 3b shows the solution domain of quench probe
II used for estimation of heat flux components in the radial direction. The geometry was
discretized using three-node triangle and three-side curved uniform mesh. The total number
of elements in this case was 5,000. The thermo-physical properties of the probe material
used in the inverse model are given in Table 1 [16]. For both probes, the metal in contact with
the liquid surface was divided into eight segments that were assigned an unknown heat flux
boundary. The convergence limit for Gauss Siedel iterations was set at 1026.
RESULTS AND DISCUSSION
The measured thermal conductivity and viscosity of quenchants are presented in
Table 2. Water shows a thermal conductivity of 0.594 W/mK and a viscosity of 0.973 cP.
The addition of 10 wt% of NaCl salt and 20 vol% of Aqua Quench solution to water
resulted in a decrease of thermal conductivity and an increase in viscosity; this is due to the
stiffening/thickening of water upon the addition of salt and polymer. The thermal
conductivity of water was decreased by about 9.6, 46, and 45% upon the addition of 10 wt
% of NaCl salt, 20 vol% of Aqua Quench solution, and 20 vol% of Aqua Quench
solution 10 wt% NaCl salt, respectively. The corresponding increase in viscosity of
water was about 20, 182, and 201%, respectively. The surface tensions (glv) of the water
and brine solution were higher than the polymer and hybrid solutions. The results indicate
that the change in the thermo-physical properties of water was significant upon the addition
of the glycol-based Aqua Quench solution and minimal upon the addition of NaCl salt.

Thermal conductivity (W/mK)

Specific heat (J/kgK)
Density (kg/m3)

Temperature (K)

13.4
451
8,400

323
14.2
467
8,370

373
15.1

423
16
491
8,340

473

Table 1. Thermo-physical properties of Inconel 600 used in IHCP [16]

16.9

523
17.8
509
8,300

573
18.7

623
19.7
522
8,270

673
20.7

723

21.7
533
8,230

773

591
8,190

873

25.9
597
8,150

973

597
8,100

1,073

30.1
611
8,060

1,173

470
G. RAMESH AND K. N. PRABHU

POLYMERSALT HYBRID QUENCHANT

471

Table 2. Thermal conductivity, viscosity, and surface tension of quenchants at 308C

Properties

Water

Brine quenchant

Polymer quenchant

Hybrid quenchant

Thermal conductivity (W/mK)

Viscosity (cP)
Surface tension (mN/m)

0.594
0.973
72.42

0.537
1.171
74.45

0.320
2.741
56.15

0.326
2.931
52.50

The spreading behavior of quenchants on the Inconel 600 substrate is shown in

Figure 4. A droplet forms a triple-phase contact point, also known as the contact line front/
advancing front, and upon dispensing, starts to move from its initial position as spreading
proceeds. Figure 5 shows the relaxation of the contact angle and spread area of droplets of
the quench media on the Inconel substrate. The relaxation of the contact angle of the water
and brine solution was gradual, and the rate of change in the contact angle was very slow.
On the other hand, the relaxation of the contact angles of the polymer and hybrid solutions
was sharp during the initial stage, and it became gradual as the system approached
equilibrium. The spread areas of droplets of water and brine solution were nearly constant,
whereas droplets of the polymer and hybrid solutions show rapid increase in the spread
area during the initial stage and become constant during the later stages of spreading. This
indicates that the spreading kinetics of the water and brine solution was very slow, whereas
the spreading kinetics was faster for the polymer and hybrid solutions on the Inconel
substrate. Further, higher contact angles were observed for the water and brine solution,
which indicates poor wettability. On the other hand, improved wettability was observed for
the polymer and hybrid solutions, as indicated by their lower contact angles. The
equilibrium contact angle ue (defined as the value of u beyond which ddtu # 0:0018/ms) of
88 ^ 0.348, 88 ^ 0.188, 68 ^ 0.298, and 69 ^ 0.448 were obtained for water, brine,
polymer, and hybrid solutions, respectively. Equilibrium contact angles were used to
determine the quantity glv cos ue, which gives an idea about solid liquid interface tension
(gsl). The values of parameter glv cos ue were found to be 2.53, 2.60, 21.03, and 18.81 mN/
m for water, brine, polymer, and hybrid solutions, respectively. It indicates that polymer
and hybrid solutions exhibit lower solid liquid interface tension on the Inconel 600
substrate compared to the water and brine solution. The results clearly indicate the minimal
effect of salt addition and the significant effect of polymer solution addition on the
spreading of water; this was mainly due to the significant increase in density and decrease
in the surface tension of water upon the addition of the Aqua Quench solution as compared
to the addition of NaCl salt.
The video images captured during quenching of the Inconel probe are shown in
Figure 6. Water quenching shows the formation of vapor film around the probe and the
occurrence of a wetting front at the bottom surface of quench probe. The wetting front
then ascends to the top surface. Brine solution quenching shows no clear indication of
the occurrence of vapor film and the wetting front, which implies rapid rewetting. It
also shows the formation of mist on the quench probe surface during rewetting due to
the re-dissolution of the salt layer formed at the early stage of quenching. Similarly to
water quenching, polymer quenching shows the clear occurrence of vapor film
formation and a wetting front on the quench probe surface. The duration to complete
the rewetting was longer than water quenching, indicating slow movement of the
wetting front for the polymer quenchant. However, it was observed that the nature of

472

G. RAMESH AND K. N. PRABHU

Figure 4. Images showing contact angle relaxation spreading on Inconel 600 substrate: (a) water, (b) brine,
(c) polymer, and (d) hybrid solutions.

the wetting front with polymer quenching was uniform compared to water quenching,
which showed a non-uniform front. The formation of vapor mist during rewetting was
observed for polymer quenching. This is due to the re-dissolution of the polymer film
formed on the quench probe surface at the early stage of quenching. Further, the
formation of numerous bubbles during nucleate boiling was observed for polymer
quenching. Quenching of the probe in the hybrid solution showed the formation of
vapor film and a wetting front, as for water and polymer quenching. The duration to
complete rewetting was shorter than water quenching, indicating fast movement of the

POLYMERSALT HYBRID QUENCHANT

473

Figure 5. (a) Contact angle relaxation and (b) spread area of quenchants droplet during spreading on Inconel 600
substrate.

wetting front for the hybrid solution. The nature of the wetting front was uniform, as for
polymer quenching. Further, it shows strong mist formation with a longer duration
during rewetting. During nucleate boiling, the occurrences of numerous bubbles on the
quench probe surface were observed for hybrid solution quenching, as for polymer
quenching.
Figure 7 shows the cooling curves measured at the geometric center of the probe
quenched in the reference fluid between quenching experiments with different quenchants.
A maximum cooling rate difference of 2.88C/s was observed. The experiments confirmed
that the quench probe was not affected significantly after quenching. The repeatability of
experiments with a quench probe was good. Similarly, Figure 8 shows a comparison of
cooling rate curves measured at the geometric centers of probe I and probe II. The

474

G. RAMESH AND K. N. PRABHU

Figure 6. Photographs of Inconel probe heated to 8508C quenched in: (a) water, (b) brine, (c) polymer, and
(d) hybrid quenchants.

maximum cooling rate difference of 2.68C/s was observed, indicating that cooling curve
analysis results of both probes were comparable. The thermal histories measured at various
axial and radial locations (Figures 9 and 10) were used to determine the wetting front
velocities, rewetting temperatures, and nature of wetting fronts. In the case of brine
quenching, rewetting occurs at nearly the same time (about 0.2 0.4 sec) on different axial
locations. This is due to the explosive-like fragmentation of salt on the quench probe

POLYMERSALT HYBRID QUENCHANT

475

Figure 7. Comparison of cooling rate curves of quench probe measured at geometric center in reference oil
before and after quenching experiments.

surface, which resulted in uniform wetting. The average rewetting temperature of 8418C
was observed for brine quenching. Figure 11 shows the variation of wetting front velocity
and rewetting temperature at axial locations of the probe for water, polymer, and hybrid
quenchants. Polymer quenching shows decreased wetting front velocity than does water

Figure 8. Comparison of cooling rate curves of probe I and probe II measured at geometric center in reference oil.

476

G. RAMESH AND K. N. PRABHU

Figure 9. Thermal histories of quench probe measured at different axial locations during quenching in: (a) water,
(b) brine, (c) polymer, and (d) hybrid quenchants.

POLYMERSALT HYBRID QUENCHANT

477

Figure 9. (Continued).

quenching due to longer duration of the vapor film. On the other hand, hybrid quenching
shows increased wetting front velocity and higher rewetting temperature than does water
quenching. However, movement of the wetting front was slower than for brine quench
medium. The average wetting front velocities of 17.48, 13.00, and 23.97 mm/s were
observed for water, polymer, and hybrid solutions, respectively. The corresponding
average rewetting temperatures were found to be 7568C, 7558C, and 8008C. Figure 12
gives the time required for the transition from vapor film to nucleate boiling stage at
different radial locations. The variation of rewetting times at different radial locations was
found to be less for brine, polymer, and hybrid solutions quenching and significant for
water quenching. The following simple dimensionless wetting time parameter was
proposed to quantify the nature of the wetting front. Implementation of Eq. (3) is described
in Appendix A:
q
P1
2
1
n tavg 2 tn
n
twet 1 2
;
3
1 tmax 2 tmin
where
twet is the dimensionless rewetting time,
n is the number of radial locations,
tn is the rewetting time at the nth radial location (sec),
tavg is the average rewetting time (sec),
tmax is the maximum rewetting time (sec), and
tmin is the minimum rewetting time (sec).
The nature of the wetting front is more uniform as twet approaches the value of 1. twet
values of 0.82, 0.96, 0.87, and 0.92 were obtained for water, brine, polymer, and hybrid
solutions, respectively. This clearly indicates that the nature of the wetting front was more

478

G. RAMESH AND K. N. PRABHU

Figure 10. Thermal histories of quench probe measured at different radial locations during quenching in:
(a) water, (b) brine, (c) polymer, and (d) hybrid quenchants.

POLYMERSALT HYBRID QUENCHANT

479

Figure 10. (Continued).

uniform with brine, hybrid, and polymer solutions quenching and non-uniform with water
quenching.
Figure 13 compares cooling curves and cooling rates at the geometric center of the
probe obtained with water, brine, polymer, and hybrid quench media. The duration of the
vapor phase stage was found to be 2.2 sec for water quenching. Short duration (about
0.4 sec) of the vapor phase stage was observed for brine quenching due to fragmentation of
the salt layer that was formed on quench probe surface. This resulted in rapid transition
from the vapor phase to the nucleate boiling stage. On the other hand, polymer quenching
shows longer vapor phase stage on the quench probe surface due to the formation of a thick
polymer film during quenching, which stabilizes the vapor film. This resulted in gradual
transition from the vapor phase to nucleate boiling stage and slow movement of the wetting

Figure 11. Variation of rewetting temperature (line with symbol) and wetting front velocity (line without
symbol) on axial locations of quench probe surface during quenching.

480

G. RAMESH AND K. N. PRABHU

Figure 12. Variation of rewetting time at different radial locations of probe during quenching in water, brine,
polymer, and hybrid quenchants.

front for polymer quenching. The duration of the vapor phase stage for hybrid quenching
was about 1 sec. The different duration of the vapor film stage is due to the change in
solid liquid interfacial tensions of quenchants. Fluid having higher wettability and lower
solid liquid interface tension can easily form a vapor film around the probe surface. The
glv cos u values of water (2.53 mN/m) and brine (2.60 mN/m) were increased to 21.03 and

Figure 13. Cooling curves (line without symbol) and cooling rate curves (line with symbol) of quench probe at
the geometric center during quenching.

POLYMERSALT HYBRID QUENCHANT

481

18.81mN/m upon the addition of polymer; this resulted in easier formation of a vapor film
in polymer and hybrid quenchants. Further, the improved wettability and decrease in the
solid liquid interface tension of polymer and hybrid quenchants during rewetting
increases the spreading of fluid on the Inconel substrate, resulting in the evolution of
copious amount of bubbles during the nucleate boiling regime. Even though the hybrid
solution contains 20 vol% of glycol-based polymer solution, it shows faster transition from
the vapor phase to nucleate boiling stage compared to water and polymer quenchants.
A possible reason could be the formation of a polymer film containing the salt on the hot
probe surface during quenching. The heat flow at the metal/quenchant interface causes
fragmentation of the salt layer, resulting in early rewetting of the fluid at a higher
temperature than the water and polymer quenchant. This leads to fast movement of the
wetting front for the hybrid solution compared to water and polymer quenchant. However,
the presence of a polymer in the hybrid solution delays the fragmentation of salt, which
resulted in lower rewetting temperature and wetting front velocities of the hybrid solution
than the brine solution.
Critical cooling curve parameters, such as peak cooling rate (CRpeak), temperature of
the peak cooling rate (TCRpeak), cooling rate at 7058C (CR705), cooling rate at 3008C
(CR300), cooling rate at 2008C (CR200), and time taken to cool from 7308C to 2608C, were
determined from the cooling curves measured at the geometric center of the probe and are
presented in Table 3. Grum et al. [17] reported a maximum cooling rate of around 2008C/s,
and the temperature at which the peak occurred was in the interval between 6508C 5008C
at the center of an Inconel 600 probe heated to 8508C during water quenching. In the
present study, the corresponding values were found to be 2028C/s and 6048C, respectively.
This indicates that experimental results are comparable with the data available in the
literature. The peak cooling rate and cooling rate at 7058C (temperature at which austenite
transformation starts to occur for most of the carbon steels) were found to be 2028C/s and
1668C/s, respectively, for water. These parameters increased upon the addition of NaCl salt
and decreased upon the addition of a glycol polymer solution. The hybrid solution
quenching showed nearly same cooling rate at 7058C (1638C/s) and decreased peak
cooling rate (1688C/s) compared to water. However, the temperature at which the peak
cooling occurs was found to be higher for the hybrid solution than other quenchants.
Similarly, the temperature at which the peak cooling rate occurs for water increased upon
additions of salt or a polymer solution. Cooling rates at 3008C and 2008C (temperatures
that are in the region of the martensitic transformation for many steels) of water were
nearly the same upon additions of salt or a polymer solution. These values decreased for
the hybrid quenchant.

Table 3. Cooling curve parameters determined for various quenchants

Critical cooling parameters

Water

Brine quenchant

Polymer quenchant

Hybrid quenchant

CRpeak (8C/s)
TCRpeak (8C)
CR705 (8C/s)
CR300 (8C/s)
CR200 (8C/s)
t730 200 (sec)

202
604
166
85
35
3.39

228
666
222
82
35
3.26

172
644
120
83
39
3.86

168
732
163
72
29
4.36

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G. RAMESH AND K. N. PRABHU

To simplify the analysis of cooling curves, a characterization parameter should be

devised that would provide a summary of the cooling process. The integration of the area
under a cooling rate curve between two temperatures T1 and T2 involves an entire
quenching period. Although the selection of T1 and T2 depends on the steel alloy, it was
concluded that the best general range was 6008C to 3008C. Thelning found that the area
under the curve increased with the average quenching speed [1]. The quench speeds of
quenchants were compared using the Thenlning method, which involves determination of
area under the cooling rate curve in the temperature range of 6008C to 3008C (A600 300).
The A600 300 values of 46,431, 47,175, 39,457, and 32,5228C2/s were observed for water,
brine, polymer, and hybrid solutions quenching, respectively. Higher quench speeds were
observed for water and brine solutions due to their higher thermal conductivities and lower
viscosities, whereas lower quench speeds were observed for polymer and hybrid
quenchants due to their lower thermal conductivities and higher viscosities. The lower
values of A600 300, peak cooling rate, and cooling rates at 3008C and 2008C indicated lower
cooling performance for the hybrid quenchant during nucleate boiling and convective
cooling stages. Even though rewetting of the probe occurs at a higher temperature in a
hybrid solution (8008C), the probe surface temperature was still higher than the rewetting
temperature (7558C) of the polymer solution. This leads to the formation of a thick
polymer mist on the probe surface, which prevails for a longer duration. As a result, the
cooling performance of the hybrid quenchant was lower during nucleate boiling and
convective cooling stages.
The time temperature data measured at different axial locations except at A8
(40 mm from the top surface) were input to the inverse program for estimating the metal/
quenchant interfacial heat flux transients and surface temperatures of the quench probe.
The temperatures measured at the A8 location were used to compare the temperatures
estimated by the inverse program at the same location. Figure 14 shows good agreement
between the measured and estimated time temperature data at the A8 location. In the case
of radial locations, all thermal histories measured were input to the inverse program.

Figure 14. Measured and estimated temperature profile of quench probe I at A8 location.

POLYMERSALT HYBRID QUENCHANT

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Figure 15. Estimated metal/quenchant heat flux transients at axial locations of probe surface during quenching
in: (a) water, (b) brine, (c) polymer, and (d) hybrid quenchants.

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G. RAMESH AND K. N. PRABHU

Figure 15. (Continued).

Figures 15 and 16 show the spatially dependent metal/quenchant interfacial heat flux
transients estimated at axial and radial locations of the quench probe surface. The average
peak heat flux values of 4,748, 5,740, 3,648, and 4,366 kW/m2 were obtained for water,
brine, polymer, and hybrid solutions quenching, respectively. The corresponding average
heat flux values were 4,255, 5,490, 3,400, and 3,841 kW/m2 at 7058C; 1,141, 1,170, 1,257,
and 1,021 kW/m2 at 3008C; and 441, 477, 533, and 347 kW/m2 at 2008C. The peak heat
flux and heat flux at 7058C were higher for brine and water quenching, whereas they were
lower for polymer and hybrid solutions. It was observed that the hybrid solution showed
higher values of peak heat flux and heat flux at 7058C compared to polymer quenching. The
heat flux values of hybrid solution quenching were lower at 3008C and 2008C than for other
quenchants. Figure 17 shows the variations of heat flux values at critical temperatures on
different locations of quench probe surfaces for all quenchants. Heat flux variations at axial
locations were found to be higher than at radial locations for all quenchants; this is due to
the dynamic nature of the wetting front. The variations of heat flux values at 3008C and
2008C were found to be nearly same for all quenchants. The variations of heat flux values
at peak and 7058C were found to be higher with brine and water quenching and lower with
polymer and hybrid solutions quenching.
The amount of heat removed during quenching was determined by plotting the
integral heat flux curve for all quench media. Figure 18 shows the heat removed during
quenching in water, brine, polymer, and hybrid solutions at different segments of the
probe. The amounts of heat removed by quenchants were nearly the same: be 10.55, 10.57,
10.64, and 10.58 MJ/m2 for water, brine, polymer, and hybrid solutions quenching,
mC DT
respectively. The heat content of the probe was calculated using the formula Ap (where
m, Cp, A, and DT are mass, specific heat capacity, area of the probe, and temperature
difference, respectively) and was found to be 10.59 MJ/m2. The heat removed by the
quenchants and heat content of the quench probe were nearly same, indicating validity of
the inverse model used in the present work.
For a better understanding of the heat transfer characteristics of each quenchant, the
time required for heat removal as a fraction of the probe heat content was plotted. Figure 19

POLYMERSALT HYBRID QUENCHANT

485

Figure 16. Estimated metal/quenchant heat flux transients at radial locations of probe surface during quenching
(a) water, (b) brine, (c) polymer, and (d) hybrid quenchants.

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G. RAMESH AND K. N. PRABHU

Figure 16. (Continued).

shows the average time for the known fraction of heat removal during quenching in water,
brine, polymer, and hybrid solutions. The time for the known fraction of heat removal was
lower for brine quenching, higher for polymer quenching, and intermediate for water and
hybrid solution quenching. Hybrid quenching shows a lower time, up to 40% heat removal,
and a higher time for the remaining percent of heat removal than water quenching. The
results indicated that the rate of heat transfer was higher with brine, lower with polymer,
and intermediate with water and hybrid solutions. The heat removal ability of the hybrid
solution was better than water in the initial stages. It should be noted that although cooling
curve analyses showed lower cooling performance during nucleate and convective cooling
for the hybrid solution compared to the polymer quenchant, the fraction of heat removed
was higher for the hybrid quench medium; this is due to the early destabilization of the
vapor film and increased wetting front velocity. The presence of salt in the hybrid medium
had a significant effect on destabilization of the vapor film, rewetting temperature, and
wetting front velocity, whereas the polymer constituent had a significant effect on the
cooling rate of components.
The results of the investigation indicated rapid uniform rewetting, fast nonuniform rewetting, slow uniform rewetting, and fast uniform rewetting processes with
brine, water, polymer, and hybrid solutions quenching, respectively. The rapid rewetting
of the brine solution is beneficial; however, the increased heat flux/quench speed may
result in distortion and cracking of components during quenching, especially in high
hardenable steels and thin section components. The non-uniform nature of wetting
during water quenching may result in non-uniform evolution and distribution of
microstructure and residual stress. The lower cooling performance of polymer is
beneficial in minimizing distortion and cracking during quenching, but the slow
movement of wetting may result in gradual variation of properties of components. The
hybrid solution combines the beneficial effects of both the brine and polymer
quenchants. Quenching in this medium resulted in faster rewetting, higher rewetting

POLYMERSALT HYBRID QUENCHANT

487

Figure 17. Spatially dependent heat flux at critical temperatures on the probe surface during quenching: (a) axial
location and (b) radial location.

temperature, and a uniform nature of the wetting front. It helps in attaining uniform
microstructure and mechanical properties. In general, a higher peak cooling rate and a
cooling rate at 7058C and a lower cooling rate at 3008C and 2008C are beneficial for
steel quenching. It was observed that heat flux/cooling rate at the peak and 7058C were
found to be higher for the hybrid medium than for the polymer quenchant. This is
beneficial in steel quenching to avoid transformation of austenite to pearlite. Similarly,
lower heat flux/cooling rates at 3008C and 2008C of hybrid quenching were beneficial in
the reduction of distortion and cracking during steel quenching, and also in aluminum
alloys, to avoid heat treatment damage.
To assess the effect of cooling performance of quench media on the microstructure in
steel, cooling curves measured at the geometric center were superimposed on the
continuous cooling transformation (CCT) diagram of steel. Figure 20 shows the CCT
diagram of AISI 1045 steel obtained using JMatPro software. (Sente Software, UK). The

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G. RAMESH AND K. N. PRABHU

Figure 18. Heat removed per unit area of probe during quenching in water, brine, polymer, and hybrid
quenchants: (a) bottom segment, (b) middle segment, and (c) top segment.

POLYMERSALT HYBRID QUENCHANT

489

Figure 19. Time required for removal heat as a fraction of probe heat content.

Figure 20. Cooling curves obtained with water, brine, polymer, and hybrid quenching superimposed on CCT
diagram of AISI 1045 steel.

resultant micro-constituent of steel consists of varying amounts of ferrite, bainite, and

martensite, as given in Table 4. The higher cooling rate in the brine solution resulted in a
higher amount of martensite and a lower amount of ferrite. On the other hand, polymer
quenching showed a lower amount of martensite and a higher amount of ferrite than other
quenchants due to slow cooling. Although cooling performance of the hybrid solution was
Table 4. Effect of quenchants on estimated volume percent of micro-constituent in AISI 1045

Ferrite
Bainite
Martensite

Water

Brine quenchant

Polymer quenchant

Hybrid quenchant

15
17
68

10
5
85

23
65
12

16
23
61

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G. RAMESH AND K. N. PRABHU

lower during the nucleate and convective cooling stages, it shows micro-constituents
similar to that obtained with water. With varying cooling rates obtained with different
quench media used in the present work, the resultant hardness of the steel estimated from
the CCT diagram was found to be 305, 323, 230, and 295 VPN for water, brine, polymer,
and hybrid quenching, respectively. The study shows that the wetting and cooling
performance of the polymer salt hybrid solution was superior to the polymer solution and
comparable with water.
CONCLUSIONS
Wetting kinetics, kinematics, and cooling performance of a hybrid solution
containing a polymer solution and salt were investigated, and results were compared with
water, brine, and polymer solutions. The presence of polymer had a significant effect on
the thermo-physical properties of the quench medium, whereas the presence of salt had a
minimal effect. Water and brine show higher contact angles on the Inconel substrate,
indicating poor wettability; polymer and hybrid solutions show lower contact angles,
indicating improved wettability. Spreading kinetics of the hybrid and polymer solutions
were faster than water and brine solutions. A dimensionless rewetting time was proposed
to assess the nature of the wetting front during quenching. The nature of the wetting front
was more uniform with brine, hybrid, and polymer solutions quenching and non-uniform
with water quenching. The rewetting phenomenon was characterized as rapid uniform, fast
non-uniform, slow uniform, and fast uniform processes for brine, water, polymer, and
polymer salt hybrid solutions, respectively. The rewetting temperature and wetting front
velocity were found to be higher with brine quenching, lower with polymer quenching, and
intermediate with water and hybrid quenching. Higher cooling rates at 7058C, peak
cooling, 3008C and 2008C were observed for brine and water quenching than for polymer
quenching. Hybrid solution quenching showed nearly the same cooling rate of water but
was higher than polymer quenching at 7058C and lower at other critical temperatures.
Higher heat flux values were obtained with brine and water quenching, and lower heat flux
values were obtained for polymer and hybrid solution quenching. Quenching with the
hybrid solution showed higher peak heat flux and higher heat flux at 7058C than for
polymer quenching and lower heat flux values at 3008C and 2008C than for other
quenchants. The variations of heat flux values at different locations of probe surface were
found to be higher with brine and water and lower with polymer and hybrid quench media.
The hybrid quenchant combines the beneficial effects (wetting kinetics, kinematics, and
heat transfer characteristics) of both brine and polymer quench media.
FUNDING
One of the authors (KNP) gratefully acknowledges the financial support provided by
the Science and Engineering Research Board (SERB), Department of Science and
Technology (DST), Government of India, New Delhi, India under an R&D project.
REFERENCES
1. G. E. Totten, C. E. Bates, and N. A. Clinton, Handbook of Quenchants and Quenching
Technology, ASM International, Materials Park, OH, 1993.

POLYMERSALT HYBRID QUENCHANT

491

2. B. Liscic, H. M. Tensi, L. C. F. Canale, and G. E. Totten, Quenching Theory and Technology,

CRC Press, Boca Raton, FL, 2010.
3. C. E. Bates, G. E. Totten, and R. L. Brennan, Quenching of Steel, ASM Handbook Heat Treating,
vol. 4, ASM International, Materials Park, OH, pp. 160, 1991.
4. C. Simsir and C. H. Gur, Simulation of Quenching, in C. H. Gur and J. Pan (Eds.), Handbook of
Thermal Process Modeling Steels, CRC Press, Boca Raton, FL, chap. 9, 2008.
5. H. M. Tensi, A. Stich, and G. E. Totten, Quenching and Quenching Technology, in G. E. Totten
(Ed.), Steel Heat Treatment: Metallurgy and Technologies, CRC Press, Boca Raton, FL, chap. 9,
2007.
6. H. Chandler, Heat Treaters Guide: Practices and Procedures for Irons and Steels, ASM
International, Materials Park, OH, 1995, p. 84.
7. G. E. Totten, B. Liscic, N. I. Kobasko, S. W. Han, and Y. H. Sun, Advances in Polymer
Quenching Technology, in Proceedings of the First International Automotive Heat Treating
Conference, ASM International, Materials Park, OH, pp. 37 44, 1998.
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International Induction Heat Treating Seminar, Clearwater, FL, May, 10 12, 2000.
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Media for Hardening, in P. Hodgson (Ed.), Quenching and Carburizing, The Institute of
Materials, London, 1993.
10. K. N. Prabhu and P. Fernandes, Heat Transfer during Quenching and Assessment of Quench
SeverityA Review, J. ASTM Int., vol. 6, JAI101784, 2009.
11. K. N. Prabhu and P. Fernandes, Determination of Wetting Behavior, Spread Activation Energy,
and Quench Severity of Bioquenchants, Metall. Mater. Trans. B, vol. 38, pp. 631 640, 2007.
12. T. H. Kunzel, H. M. Tensi, and G. Welzel, Rewetting RateThe Decisive Characteristic of a
Quenchant, Fifth International Congress on Heat Treatment of Materials, Budapest, Hungary,
pp. 1806 1813, October 20 24, 1986.
13. G. E. Totten and H. M. Tensi, Using Conductance Data to Characterize Quenchants, Heat Treat
Progress, vol. 2, pp. 39 42, 2002.
14. G. Ramesh and K. N. Prabhu, Spatial Dependence of Heat Flux Transients and Wetting Behavior
During Immersion Quenching of Inconel 600 Probe in Brine and Polymer Media, Metall. Mater.
Trans. B, DOI:10.1007/s11663-014-0038-7
15. T. S. P. Kumar, A Serial Solution for the 2-D Inverse Heat Conduction Problem for Estimating
Multiple Heat Flux Components, Numer. Heat Tr. B-Fund., vol. 45, pp. 541 563, 2004.
16. R. N. Penha, L. C. F. Canale, G. E. Totten, G. S. Sarmiento, and J. M. Ventura, Simulation of
Heat Transfer and Residual Stresses from Cooling Curves Obtained in Quenching Studies,
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APPENDIX A
When hot metal is submerged into the liquid pool, heat transfer is controlled by different cooling
stages, known as the vapor blanket stage/film boiling stage, the nucleate boiling stage, and the
convective or liquid cooling stage. Quenching is a non-stationary process where the change from the
vapor blanket stage to nucleate boiling is not abrupt; a transition occurs when the surface heat
transfer coefficient and the amount of liquid/solid contact increases. The occurrence of these local
boiling phenomena is a function of time and position along the surface of the component, and this
behavior leads to the occurrence of a wetting front. The wetting front is the loci of the boundary
between the vapor film and the occurrence of bubbles [4]. The nature of the wetting front and its

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G. RAMESH AND K. N. PRABHU

Figure 21. Wetting front on quench probe surface: (a) non-uniform nature and (b) uniform nature.

movement on the quench probe has significant effect on the formation of a microstructure and
distribution of hardiness over the component.
Consider (a) non-uniform and (b) uniform wetting front formation on the probe surface during
quenching, as shown in Figure 21. For a particular time, wetting front edge locations occur at
different depth (axial) locations of the probe. Conversely, for a particular depth (axial location) of the
quench probe, transition from the vapor blanket to nucleate boiling occurs at different times on
different radial locations. Let t1, t2, t3, and t4 be the rewetting times for four radial locations A, B, C,
and D, respectively, at a particular depth (axial location) E, as shown in Figure 21. The rewetting
times for locations A, B, C, and D occur at different times (in the increasing order of
t1 , t3 , t4 , t2) for non-uniform wetting, while they occur at nearly the same time
(t1 < t2 < t3 < t4) for a uniform wetting front. Measurement of rewetting times at different radial
locations at a particular axial location of the probe can therefore be used to assess the nature of the
wetting front. The wetting front is more uniform if the variation of rewetting times on different radial
locations is less, while it is more non-uniform when rewetting time variation is significant. In the
present study, the rewetting times measured on different radial locations of the probe at a depth of
30 mm were used to quantify the nature of the wetting front. The following dimensionless wetting
time parameter was proposed to quantify the nature of the wetting front:
q
P1
2
1
n tavg 2 t n
n
twet 1 2
;
1 t max 2 t min
where
twet is the dimensionless rewetting time,
n is the number of radial locations,
tn is the rewetting time at the nth radial location (sec),
tavg is the average rewetting time (sec),
tmax is the maximum rewetting time (sec), and
tmin is the minimum rewetting time (sec).

The numerator of the above equation is the standard deviation of rewetting time, which
determines the variation of rewetting times. The value of the standard deviation of
rewetting time was normalized with the range of rewetting time (tmax tmin) to make
it dimensionless. The nature of the wetting front is more uniform as twet approaches the
value of 1.