Fransua Thomas

Glenn Research Center, Cleveland, Ohio

The Effect of Various Quenchants on the Hardness 

and Microstructure of 60-NITINOL

NASA/TM—2015-218463

January 2015
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Fransua Thomas

Glenn Research Center, Cleveland, Ohio

The Effect of Various Quenchants on the Hardness 

and Microstructure of 60-NITINOL

NASA/TM—2015-218463

January 2015

National Aeronautics and

Space Administration

Glenn Research Center

Cleveland, Ohio 44135
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NASA/TM—2015-218463 1 

The Effect of Various Quenchants on the Hardness and 

Microstructure of 60-NITINOL 

Fransua Thomas 

National Aeronautics and Space Administration 

Glenn Research Center 

Cleveland, Ohio 44135 

Abstract 

The effect of various quenching media on the hardness and microstructure of 60 NITINOL (60 NiTi) 

were evaluated. Specimens of 60 NiTi were heat treated in air at 1000 qC for 30 min or 2 hr, then quench 

cooled by one of seven different methods. The microstructure and hardness of this material was examined 

post heat treatment. The results indicated that the quench method had little effect on the resulting 

hardness and microstructure of 60 NiTi. 

Introduction 

There is an increasing interest in 60 NITINOL (60 NiTi) as an alternative material for bearing and 

gear applications (Ref. 1). In spacecraft systems, bearings must withstand transient loading from the 

vibration of launch and resist wear-accelerating corrosion from the operating environment as well as from 

the corrosive ambient marine environment of many of the U.S. spaceports. Consisting of 60 wt% Ni and 

40 wt% Ti, 60 NiTi is characterized by its excellent hardness, wear resistance, dimensional stability, 

corrosion resistance and tribological properties (Ref. 2). 

Heat treatment is an important process to attain maximum hardness in NiTi alloys like 60 NiTi. The 

process includes heating the material to high temperatures followed by rapid cooling. The heating step is 

referred to as solution treating. During this process the material is heated to a temperature above the 

solvus point and held there for sufficient time to permit the formation of a uniform NiTi phase. For, 

60 NiTi this temperature is 900 to 1050 qC and the soak period is 30 to 120 min. The next step is 

quenching or rapid cooling. Quenching is then used to retain the generally preferable austenitic phase of 

the 60 NiTi. Unlike bearing steels in which the martensitic phase is desired due to its high hardness, in 

NiTi alloys it is the austenitic phase that is hard and sought after in bearing applications. 

Rapid cooling during heat treatment can, however, produce internal residual stresses that can lead to 

dimensional distortion and, in extreme cases, quench cracking, where thermally-induced stresses exceed 

the tensile strength of the material (Ref. 3). Oftentimes, the heat treatment process must be adjusted to 

strike a balance between hardness and residual stress levels. The principle objective of this study is to 

understand the effect of the cooling rate of various quechants on the hardness and microstructure of 

60 NiTi and to improve our understanding of the overall heat treatment process. 

Materials and Procedures 

The 60 NiTi (60 wt% Ni – 40 wt% Ti) was obtained from commercial sources. Specimens were cut 

from an ingot of the material made by hot isostatically pressing atomized Ni - Ti powder in a steel 

container. The specimens used for this heat treatment investigation were approximately 45.7u3u4 mm. 

The specimens were sectioned from the ingot by electrical-discharge machining (EDM), placed in 

different quenchant groups then heat treated in air using a tube furnace. Specimens were heat treated for 

either 30 min or 2 hr at 1000 °C then quenched with one of the seven different quenching media. The 

quenchants used in this study represent commonly used quenchants: room temperature water, boiling 

water, ice water, compressed air, vegetable oil, glycol, and liquid nitrogen (LN2). 
NASA/TM—2015-218463 2 

Figure 1.—Picture showing specimen and location of thermocouple. 

Each specimen was fitted with a type K high temperature thermocouple, which was securely placed in 

the center of each specimen in a 1.50 mm bored hole (Fig. 1). The cooling curve data was recorded using 

a custom high speed acquisition program in which the millivolt signal from the embedded thermocouple 

was routed into the computer with an ICPDAS I-7019R data acquisition module. The program captured 

the data at a rate of approximately 30 Hz and exported it to a tab delimited text file. 

After the solution treating step, the specimens were quickly removed from the furnace and subjected 

to the selected quenchant. To determine the hardness of the specimen, a standard Rockwell C indentation 

tester with a load of 150 kg was used. Prior to checking hardness, the thin oxide layer that formed during 

the heat treatment was removed by manual surface grinding. Four measurements were made on each 

specimen and the average of these measurements is reported. The metallographic process used to prepare 

the specimen consisted of a wet polished by hand using SiC abrasive paper starting with 320 grit abrasive 

and ending with 800 grit abrasive. Secondly a final polish used colloidal silica on a vibratory polisher 

which resulted in a near mirror. Lastly the polished surface was etched in a solution of 5 ml HF + 2.5 ml 

HNO3 + 43 ml deionized water. The microstructure was observed by optical microscopy. 

Results and Discussion 

The average Rockwell hardness values obtained with each quenchant after heat soaks of either 

30 min or 2 hr are shown in Tables 1 and 2, respectively. For the test conditions encompassed by this 

research, each quenchant yielded very similar results in hardness. The average hardness in each of the 

groups ranged from 59 to 61 HRC and the standard deviation was small, less than 1 hardness point. In 

other words, neither the solution treatment duration, nor the quenching media significantly affected the 

hardness for the variables considered in this study. 

To obtain bearing quality hardness, specimens are rapidly cooled by quenching. This process is quite 

severe and may cause thermal cracking or distortion and this phenomena is the primary motivation for 

this study. The 60 NiTi specimens tested appear to be insensitive to the quenching media. The quenchants 

tested have varying thermal properties, leading to differences in the initial cooling rate. A comparison of 

the cooling curves obtained from seven different quenchants is shown in Figure 2. 

To determine if the varying quenching media had any effect on the microstructure, metallographic 

characterization was conducted. Optical microscopy of cross sections of the specimens were carried out to 

compare the microstructures. The microstructure of the specimens after simple heat treatment that 

included solution heating at 1000 qC followed by rapid quench, shows second phase (Ni3Ti) found 

throughout grains and grain boundaries. Figure 3 shows photomicrographs of the similar microstuctures 

of heat treated specimens quenched in the different quenchants. These similarities in microstructure and 

hardness are achieved through the rate in which the specimens are cooled in the fore-mentioned figure. 
NASA/TM—2015-218463 3 

TABLE 1.—SUMMARY OF INDENTATION OF NITINOL SPECIMEN 

IN VARIOUS QUENCHANTS, SOLUTION TREATED FOR 30 MIN 

Rockwell (C) hardness at 30 min 

Quenchant type Average hardness (HRC) 

RT water 61േ0.5 

Shop air 60േ0.6 

Boiling water 60േ0.3 

Ice bath 60േ0.1 

Oil 60േ0.4 

Glycol 60േ0.2 

LN2 60േ0.5 

TABLE 2.—SUMMARY OF INDENTATION OF NITINOL SPECIMEN IN 

VARIOUS QUENCHANTS, SOLUTION TREATED FOR 2 HR 

Rockwell (C) hardness at 2 hr 

Quenchant type Average hardness (HRC) 

RT water 60േ0.2 

Shop air 59േ0.3 

Boiling water 60േ0.5 

Ice bath 59േ0.6 

Oil 60േ0.4 

Glycol 60േ0.1 

LN2 59േ0.5 

Figure 2.—Cooling curves for 60-NITINOL specimen in various quenchants. 

 
NASA/TM—2015-218463 4 

Figure 3.—Optical micrographs showing the microstructure of 60-NITINOL after heat treatment and 

various quenching mediums: (a) room temperature water, (b) boiling water, (c) ice water, (d) shop air, 

(e) vegetable oil, (f) glycol, and (g) liquid nitrogen (LN2). 
NASA/TM—2015-218463 5 

Figure 3.—Concluded. 

Summary and Closing Remarks 

The objective of this study is to understand the effect of various quenchants on the hardness and 

microstructure of 60 NiTi. Based on this study, the results show 60 NiTi exhibits high hardness 

(58 to 61 Rockwell C scale) when heat treated at 1000 qC for 30 min or 2 hr, regardless of which of the 

studied quenchants used for this specimen geometry. These results show that cooling rate is a factor in the 

hardness, when compared to earlier studies of larger specimens, suggesting that additional testing on 

larger specimens will have to be done to further this investigation. 

References 

1. Dellacorte, Christopher, “Intermetallic Nickel-Titanium Alloys for Oil-Lubricated Bearing 

Applications,” NASA/TM—2009-215646, March 2009. 

2. Stanford, Malcolm, “Processing Issues for Preliminary Melts of the Intermetallic Compound 

60-NITINOL,” NASA/TM—2012-216044, November 2012, National Technical Information Service, 

Springfield, VA. 

3. Charles E. Bates, George E. Totten, and Robert L. Brennan, “Quenching of Steel,” Metals Handbook, 

Vol. 4: Heat Treating, ASM International, 1991.