Design of Heat Treatment Cycles: A Case Study for Salt

Bath Hardening of Tool Steel

Although heat treatment operations have strong bearing on the final
product quality, Heat treatment process parameters are often arrived at
through empirical or trial and error methods. The present work describes
an engineering approach to the design of heat treatment cycles in an
industrial salt bath hardening operation.
Industry accepted heat treatment processing cycles might sometimes lead
to longer product development time, sub-optimal level of operation at
lower process efficiency, and higher energy consumption. This article
elaborates on important engineering issues to be considered in salt bath
hardening such as: selection of austenitising temperature and soaking
time, selection of appropriate salt, rectification of salt, tempering cycle
and quality control measures. This holistic approach was successfully
applied to an industrial scale heat treating operation for the production of
slip gauges.
Accurate Engineering Company Ltd. is leading Indian manufacturer of
precision measuring instruments and machine tools. With its state of art
manufacturing facilities in Pune, India, the company offers a
comprehensive range of measuring equipment including slip gauges; snap
gauges, vernier calipers, air gauges, measuring fixtures, and three
coordinate measuring instruments.
The heat treatment operation is an important step in the manufacturing of
these precision instruments. Proper control during this operation is
essential to obtain product with stringent dimensional control as well as
high wear-resistance. The common heat treatments practiced during the
manufacturing of these precision equipment are:

salt bath hardening operation, where the components are heated in

a salt bath furnace and quenched to room temperature,
cryogenic treatment for stabilization of martensitic microstructure,
and
tempering operation for obtaining a desirable combination of
strength, hardness and toughness.

Accurate Engineering recently procured a large amount of steel from

Germany at a very attractive price. This grade of steel, locally branded as
"Frank Grade," was used by one of the leading German slip gauge
manufacturers. Although, the composition of this grade was provided, the
heat treatment schedule was not revealed. At the Accurate heat
treatment shop, attempts were made to develop the heat treatment cycle

through trial and error method. Wide variations in hardness ranging from
30 to 45 HRC were observed during these trials, well below the required
hardness of 60 HRC.
During the past two decades, the process engineering group of Tata
Research Development & Design Centre (TRDDC) has successfully
executed several industrial projects on model based optimization of
various metallurgical operations. The Frank Grade problem was
undertaken by TRDDC to design a heat treatment cycle for this steel to
obtain uniform hardness of HRC 60 after quenching and tempering
operations.

Fig. 1 Schematic of hardening operation. (Left) Heating to the

austenitizing temperature shown as shaded regime, and (Right)
high cooling rate for hardening.

Approach to Design of the Heat Treatment Cycle

Hardening of steel is achieved by transforming the ferrite+pearlite phases
to austenite phase by heating and subsequently by transforming the
austenite phase to martensite phase by cooling. Under standard
processes, it is difficult to obtain a 100% transformed martensite
structure. There will always be a minimal amount of retained austenite in
the structure. It is desirable to transform this retained austenite to ensure
complete hardness, improve toughness and minimize distortion during the
service.
As depicted in Fig. 1(a), the transformation to austenite requires heating
above Ac3 for hypoeutectoid steel (with %C < 0.8) or above Ac1 for
hypereutectoid steel (with %C > 0.8). During the subsequent quenching
operation, the cooling rate should be high enough to avoid transformation
to softer phases like pearlite and bainite. This is schematically shown in
Fig. 1(b).
The important metallurgical issues in designing a hardening cycle for tool
steels are:

Selection of austenising temperature,

Adequate soaking time for thermal homogenization of the

component,
Selection of appropriate quenching media to obtain required cooling
rate,
Cooling the component to the room temperature,
Tempering temperature and time.

However, several other practical aspects, such as selection of salt and its
neutrality maintenance, need to be addressed for successful industrial
scale hardening. These issues are elaborated in the following section.

Steel Grade
Identification of the steel grade is the most important parameter for
designing a hardening cycle. The nominal and specified composition of the
Frank grade steel are tabulated in Table I. The composition falls in the
AISI Type W2 grade (water-hardening high carbon tool steel). This grade
is a shallow hardening tool steel and in rods above 0.5 inch in diameter
hardens selectively providing a hard, abrasion resistance surface and a
soft and tough core. These characteristics make it desirable for many
tools that are subjected to impact during use. It has a good machinability
and is readily formable by forging. W2 grade responds uniformly to
normal heat treatments and is a widely used steel for many purposes.

Selection of Salt for Process

When selecting a salt for a given application, the following issues must be
considered:

The required heating temperature of the steel part must lie within
the working range of the salt;

The melting point should be low to avoid prolonged heat-up times

for heavy loads;
The salt must be compatible with quenching media; and
The ease with which the salt is washed from the workpiece after
heat treatment and the affinity of salt for moisture must be
considered.

At present, Accurate uses a proprietary MNC-661 heat treatment salt,

supplied by Matador Chemical Industries, India. The specification sheet of
this salt indicates that its melting point is 1220 F (660 C) and
recommended working range is 1508 to 1580 F (820 to 860 C). However,
the heat treatment requirement at Accurate is as high as 1832 F
(1000 C). Using a salt above its recommended working temperature can
result in oxidation of the salt as well as increase the possibility of
oxidation and decarburization in the workpiece. Therefore, a suitable
alternative had to be identified.
Barium chloride-based salts are widely used for salt bath heat treatment
of tool steels. The typical compositions and recommended working
temperatures for these salts are given in Table II. For the Frank Grade
steel, Salt #2 with 70% BaCl2 and 20% NaCl is recommended for
austenitization.

Fig. 2 TTT diagram of AISI W2 grade steel.

Salt Bath Temperature & Soaking Time

Proper control of salt bath temperature in the austenitizing range is
important, as very high bath temperatures will result into grain growth
while lower temperatures will prevent the complete transformation of
pearlite to austenite.
The time-temperature-transformation diagram for this grade is given in
Fig. 2. The Ac1 temperature for this grade of steel is 1345 to 1369 F (732

to 743 C), so the recommended austenitizing temperature (bath

temperature) for this grade of steel should be in the range of 1428 to
1555 F (775 to 845 C). For complex shapes and larger parts, it is
recommended to preheat the workpiece at 1202 F (650 C) for stress
relieving prior to hardening.

Fig. 3 Suggested locations for uniformity survey.

As a best practice, uniformity surveys should be conducted in the salt

baths before charging the load at a given heat treatment temperature.
These surveys are usually made by holding thermocouples in the top,
center and bottom of the bath as illustrated in Fig. 3. The soaking time in
a salt bath should be sufficient to heat the workpiece through its crosssection and enable the complete phase transformation to austenite.
Longer times will result in grain growth and decarburization at the
surface. The recommended soaking time in the salt bath furnace is 20 to
25 seconds per millimeter of workpiece thickness, which translates to a
holding time of approximately 10 to 30 minutes for the parts in this
project.
Salt Rectification
Neutral salts used for austenitizing steel become contaminated with
soluble oxides and dissolved metals during use. As the buildup of these
oxides and dissolved metals renders the bath oxidizing and decarburizing
toward steel, it is necessary to periodically rectify the bath. In the case of
salt bath furnaces with immersed electrodes, daily rectification of the bath
is required. For the recommended barium chloride-based salts (Salt#
1,2,3 in Table II) rectification should be done by adding 125 gm of boric
acid (for each 100 kg of salt) and inserting a 3-inch graphite rod for one
hour for every 4 hours of operation.

Fig. 4 Typical cooling curve for a quenchant with

three different stages of cooling.

Tempering
Tempering modifies the properties of quenched hardened tool steel and
renders a desirable combination of strength, hardness and toughness. In
general, two or more shorter tempering cycles are recommended for
complete transformation of the retained austenite and for tempering the
freshly formed martensite during cool-down after the first tempering
cycle. The suggested double tempering process for the Frank grade steel
calls for a 45 minutes treatment at 392 F (200 C). Water-hardened tool
steels like this steel should be tempered immediately after hardening,
preferably before they reach room temperature, to prevent or minimize
cracking.
EXPERIMENTATION AND RESULTS

Fig. 5 Schematic of hardness test locations.

Fig. 6 Average and standard deviation of central
points and corner for as-heat treated, 0.1 mm and
0.3 mm ground samples.

Based on the items discussed above, the following heat treatment

schedule was selected:

Salt Bath Temperature of 1508 F (850 C)

Holding Time of 15 minutes
Quenching in Water
Tempering at 392 F (200 C) for 45 minutes

Fifteen samples measuring 55 mm x 35 mm x 10 mm were heat treated.

The Rockwell HRC hardness values were measured on the as-heat treated
surface, as well as at depths of 0.1 mm and 0.3 mm. The location where
each hardness measurement was taken is shown schematically in Fig. 5.
The results of the hardness measurements on the fifteen samples are
summarized in Fig. 6.
The mean hardness and standard deviation of the center point and the
corners are plotted for each of the three locations. As is evident from Fig.
6, the corners of the as-heat treated sample had an average hardness
value of 44.8 HRC with a standard deviation of 12.1. Such a low average
hardness value and high degree of variation is not acceptable in the final
product. In the 0.1 mm depth sample, the average hardness value
increased to 51.4 along with a reduction of the standard deviation to 9.8.

The hardness value further improved to an average of 60.6 with a

standard deviation of 1.2 for the 0.3 mm depth. Such a high and uniform
hardness value is highly desirable for the slip gauges. It must be noted
that the hardness value of 30 to 45 HRC was obtained during the in-house
trials at the company.
The low hardness and wide variability of the as-heat treated samples was
primarily due to the surface scale, whereas the improvement in hardness
levels from 0.1 mm to 0.3 mm suggests decarburization in the product. It
is believed that the decarburized layer is due to the non-rectification of
the MNC 661 salt currently being used at Accurate Engineering.
It is interesting to note that in all the three cases, the center points
showed a lower hardness value as compared to the corner points. Such
an effect is believed to be the result of a higher tendency of vapor blanket
formation in the sample center as compared to the sample corner.
Agitation in the quench bath would break the vapor blanket during the
first state of quenching and could improve hardness uniformity.
RECOMMENDATIONS
The summary of recommendations as determined by the process analysis
and the experimental results are given below:

Salt mixture of 70% BaCl2 + 30% NaCl should be used at an

austenitizing temperature of 1508 F (820 C) and soak time of 15
minutes.
Rectification of the above salt must be done every four hours of
operation with 125 gm of boric acid for every 100 Kg of salt and by
inserting 3" graphite rod in the bath for 1 hour.
Uniformity survey of the bath temperature should be conducted
before loading the workpiece at desired temperature.
The workpiece should be cleaned from scale before heating in the
salt bath furnace.
The workpiece should be quickly transferred from the salt bath to
the quench water maintained at a temperature less than 95 F
(35 C).
Quenching water should be agitated in order to achieve hardness
uniformity.
When the part can be held by hand, it should be quickly transferred
to the tempering furnace and held at 392 F (200 C) for 45 minutes.
The tempering cycle should be repeated to achieve better
dimensional stability.
The parts should be cleaned in a solution of 10% NaOH by weight in
water followed by rinsing in plain water.

SUMMARY
By using the suggested heat treatment cycle determined for the Frank
Grade steel, the desired hardness of HRC 60 was achieved.
Decarburization of surface layer was observed and attributed to the use of
salt bath at higher than recommended temperature and the absence of
periodic salt rectification.