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Transformation Temperature of Nickel-Titanium Alloys by Thermal Analysis
Transformation Temperature of Nickel-Titanium Alloys by Thermal Analysis
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: F2004 − 17
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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F2004 − 17
by other test methods due to the effects of strain and load on the of the alloy. For example, bare 25-45 mg samples can be air
transformation. For example, transformation temperatures cooled after solution annealing.
measured in accordance with Test Method F2082 will differ 8.3 Clean the sample of all foreign materials such as cutting
from those measured by the current standard. fluid. If the sample is oxidized during heat treatment, grind,
5.5 The use of this test method for finished or semi-finished polish, or etch the sample to remove the oxide. Take care to
components without annealing (as in 8.2) shall be agreed upon avoid cold working the sample as this will change its thermal
between the purchaser and the supplier. response. Slight oxidation is permissible but remove all heavy
oxide scale.
6. Interferences
9. Calibration
6.1 Make sure the material to be tested is homogeneous
since milligram sample quantities are used. 9.1 Calibrate the temperature axis of the instrument using
the same heating rate, purge gas, and flow rate as those used for
6.2 Take care in preparing the sample (1). Cutting and
analyzing the specimen in accordance with Test Method E967.
grinding can cause localized heating and/or deformation, that
affect the transformation temperature. Oxidation during heat 10. Procedure
treatment can change the thermal conductance of the sample.
10.1 Place the sample on the sample pan and place the pan
6.3 Set the gas flow to provide adequate thermal conductiv- on the test pedestal.
ity in the test cell.
10.2 Place an empty pan on the reference pedestal.
7. Apparatus 10.3 Turn on the purge gas at a flow rate of 10 to 50
7.1 Use a differential scanning calorimeter capable of heat- mL/min.
ing and cooling at rates up to 10°C/min and of automatically 10.3.1 Use helium as the purge gas for the sample chamber.
recording the differential energy input between the specimen 10.3.2 Use a dry air, helium, or nitrogen cover gas. The dry
and the reference to the required sensitivity and precision. gas shall have a dew point below the lowest temperature of the
cooling cycle.
7.2 Use sample capsules or pans composed of aluminum or
other inert material of high thermal conductivity. 10.4 Run the cooling and heating program.
10.4.1 Use the heating and cooling rates of 10 6 0.5°C/min.
7.3 Use helium gas purge supply. See 10.3.1. 10.4.2 Heat the sample from room temperature to a tem-
7.4 Use an analytical balance with a capacity of 100 mg perature of at least Af + 30°C; hold at that temperature for a
capable of weighing to the nearest 0.1 mg. time sufficient to equilibrate the sample with the furnace.
10.4.3 Cool the sample to a temperature of below Mf –
8. Sampling 30°C; hold for a time sufficient to equilibrate the sample with
8.1 Use a sample size of 25 to 45 mg. Cut the sample to the furnace. Then, heat the sample to a temperature of at least
maximize surface contact with the (DSC) sample pan. Af + 30°C.
8.2 Anneal the sample at 800 to 850°C for 15 to 60 min in 10.5 Data Acquisition—Record the resulting curve from the
vacuum or inert atmosphere, or in air with adequate protection heating and cooling program from Af + 30°C to Mf – 30°C.
from oxidation. Rapidly cool the sample to prevent precipita-
11. Graphical Data Reduction
tion of phases that may change the transformation temperature
11.1 Draw the baselines for the cooling and heating portions
of the curve as shown in Fig. 1.
11.2 Draw the tangents to the cooling and heating spikes
through the inflection points as shown in Fig. 1. If a computer
program is used to construct the tangents, care must be taken in
locating the tangent points.
11.3 Obtain Ms, Mf, As, and Af as the graphical intersection
of the baseline with the extension of the line of maximum
inclination of the appropriate peak of the curve as shown in
Fig. 1. Ap is the peak minimum of the endothermic curve, and
Mp is the peak maximum of the exothermic curve. Read Ap and
Mp directly from the graph as shown in Fig. 1.
12. Report
12.1 Report the following information with the test results:
12.1.1 Complete identification and description of the mate-
rial tested including the specification and lot number.
12.1.2 Description of the instrument used for the test.
FIG. 1 DSC Curve for Nickel-Titanium (NiTi) 12.1.3 Statement of mass, dimensions, and geometry.
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F2004 − 17
12.1.4 Material for the specimen pan and temperature pro- TABLE 2 Precision of Mp
gram. Mp, Repeatability Reproducibility
Repeatability Reproducibility
12.1.5 Description of the temperature calibration procedure. Material grand Standard Standard
Limit Limit
mean Deviation Deviation
12.1.6 Identification of the specimen environment by gas,
A -43.8 0.42 2.65 1.2 7.4
flow rate, purity, and composition. B -20.5 1.10 2.21 3.1 6.2
12.1.7 Results of the transformation measurements using C 58.1 0.88 1.05 2.5 2.9
the nomenclature in accordance with Terminology F2005.
Temperature results should be reported to the nearest 1°C.
TABLE 3 Precision of Ms
13. Precision and Bias Ms, Repeatability Reproducibility
Repeatability Reproducibility
Material grand Standard Standard
13.1 An interlaboratory study was conducted in accordance mean Deviation Deviation
Limit Limit
with Practice E691 in seven laboratories with three different A -41.6 0.40 2.35 1.1 6.6
materials, with each laboratory obtaining five results for each B -16.9 0.95 1.24 2.7 3.5
material. There were two rounds of testing. In the first round, C 64.8 0.74 1.15 2.1 3.2
all the test samples were annealed in one laboratory; in the
second round, the samples were annealed by the laboratory that
TABLE 4 Precision of As
conducted the test. The details are given in ASTM Research
Report No. RR:F04-1008.3 As, Repeatability Reproducibility
Repeatability Reproducibility
Material grand Standard Standard
Limit Limit
13.2 The results of round one are summarized in Tables 1-6 mean Deviation Deviation
for each transformation temperature parameter (Mf, Mp, Ms, A -25.3 0.30 1.85 0.8 5.2
B -4.8 0.32 1.58 0.9 4.4
As, Ap, Af). The values are in degrees Celsius. The terms C 72.9 0.65 2.68 1.8 7.5
repeatability limit and reproducibility limit are used as speci-
fied in Practice E177.
13.3 The results of round two are summarized in Tables TABLE 5 Precision of Ap
7-12 for each transformation temperature parameter (Mf, Mp, Ap, Repeatability Reproducibility
Repeatability Reproducibility
Material grand Standard Standard
Ms, As, Ap, Af). The values are in degrees Celsius. The terms mean Deviation Deviation
Limit Limit
repeatability limit and reproducibility limit are used as speci- A -23.4 0.23 2.01 0.6 5.6
fied in Practice E177. B 2.5 0.67 1.39 1.9 3.9
C 91.6 0.80 2.25 2.2 6.3
14. Keywords
14.1 differential scanning calorimeter; DSC; nickel-titanium
alloy; NiTi; Nitinol; shape memory alloy; TiNi; transformation
temperature
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Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:F04-1008. Contact ASTM Customer
Service at service@astm.org.
TABLE 1 Precision of Mf
Mf, Repeatability Reproducibility
Repeatability Reproducibility
Material grand Standard Standard
Limit Limit
mean Deviation Deviation
A -50.0 0.57 3.97 1.6 11.1
B -26.3 0.95 2.62 2.7 7.3
C 48.5 1.02 1.54 3.0 4.3
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F2004 − 17
TABLE 6 Precision of Af
Af, Repeatability Reproducibility
Repeatability Reproducibility
Material grand Standard Standard
Limit Limit
mean Deviation Deviation
A -19.4 0.16 1.94 0.5 5.4
B 5.7 0.57 1.50 1.6 4.2
C 94.7 0.85 3.18 2.4 8.9
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F2004 − 17
TABLE 12 Precision of Af, When Samples are Annealed by
Testing Laboratory
Af, Repeatability Reproducibility
Repeatability Reproducibility
Material grand Standard Standard
Limit Limit
mean Deviation Deviation
A -16.6 0.87 4.95 2.4 13.9
B 6.6 0.69 4.07 1.9 11.4
C 94.7 0.91 2.61 2.5 7.3
APPENDIX
(Nonmandatory Information)
X1. RATIONALE
X1.1 It is well known that slow cooling after annealing of tray and then allow the samples and the foil tray to cool
nickel-rich alloys allows precipitates of the Ni4Ti3 type to together, out of the furnace, in room temperature air.
form, thereby increasing the Ti content of the matrix and the
transformation temperatures. The practice is to avoid slow X1.2 Differences in sample preparation techniques between
cooling and thus preserve the “as annealed” transformation. It laboratories influenced the reproducibility limit. Differences in
is possible, however, to cool the samples too quickly, raising calibration techniques may have also influenced reproducibil-
the transformation temperature, possibly due to stress effects ity. To minimize interlaboratory variations in results, common
that retain residual martensite. One method of achieving the sample preparation and calibration practices must be estab-
desired cooling rate is to heat treat the test specimens on a foil lished.
REFERENCE
(1) Marquez, J., Slater, T., and Sczerzenie, F., “Determining the Trans- Shape Memory and Superelastic Technologies (SMST), edited by A. R.
formation Temperatures of NiTi Alloys using Differential Scanning Pelton, D. Hodgson, S. M. Russell, and T. Duerig, 1997, pp. 13-18.
Calorimetry,” in Proceedings of the 2nd International Conference on
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