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Design of Heat Treatment Cycles: A Case Study for Salt Bath Hardening of Tool Steel

Dr. Satyam Sahay | Tata Research Development & Design Centre | Pune 411013 India
November 10, 2000

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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 austenitizing 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 austenizing 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.

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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.

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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 cross-
section 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 (820 C)

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Salt Bath Temperature of 1508 F (820 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.

ACKNOWLEDGMENTS

The author gratefully acknowledges Mr. Aditya Salunkhe and Mr. P.B. Sumant of Accurate Engineering for providing
resources during the execution of this project and also for permission of publishing this work. IH

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