1、Designation: E2113 09E2113 13Standard Test Method forLength Change Calibration of Thermomechanical Analyzers1This standard is issued under the fixed designation E2113; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of las
2、t revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method describes calibration of the length change (deflection) measurement or thermal expansion ofthermomechani
3、cal analyzers (TMA)(TMAs) within the temperature range from -150150 to 1000 C 1000C using the thermalexpansion of a suitable reference material.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This test method differs f
4、rom ISO 11359-1 by providing an alternative calibration procedure.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof whoever uses this standard to consult and establish appropriate safety and health practices and dete
5、rmine the applicability ofregulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E473 Terminology Relating to Thermal Analysis and RheologyE831 Test Method for Linear Thermal Expansion of Solid Materials by Thermomechanical AnalysisE1142 Terminology Relating to Thermophysical
6、 PropertiesE1363 Test Method for Temperature Calibration of Thermomechanical AnalyzersE2161 Terminology Relating to Performance Validation in Thermal Analysis2.2 Other Standards:ISO 11359-1 PlasticsThermomechanical analysis (TMA)Part 1: General principles33. Terminology3.1 Specific technical terms u
7、sed in this test method are described in Terminologies E473, E1142, and E2161 includecalibration, Celsius, coefficient of linear thermal expansion, Kelvin, reference material, repeatability, reproducibility andthermomechanical analysis.4. Summary of Test Method4.1 Thermomechanical analyzers (TMAs) o
8、r related devices are commonly used to determine coefficient of linear thermalexpansion of solid materials (for example, Test Method E831). The test specimen is heated at a linear rate over the temperaturerange of interest and the change in length (dimension) is electronically recorded.4.2 Performan
9、ce verification or calibration of the length change measurement is needed to obtain accurate coefficient of thermalexpansion data.4.3 The thermal expansion of a reference material is recorded using a thermomechanical analyzer. The recorded thermalexpansion is compared to the known value of the refer
10、ence material. The resultant ratio, a calibration coefficient, may then beapplied to the determination of unknown specimens to obtain accurate results.1 This test method is under the jurisdiction ofASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.10 on
11、Fundamental,Statistical and Mechanical Properties.Current edition approved Sept. 1, 2009Aug. 1, 2013. Published October 2009August 2013. Originally approved in 2000. Last previous edition approved in 20042009 asE2113 04.E2113 09. DOI: 10.1520/E2113-09.10.1520/E2113-13.2 For referencedASTM standards,
12、 visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, Ne
13、w York, NY 10036, http:/www.ansi.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM re
14、commends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Signific
15、ance and Use5.1 Performance verification or calibration is essential to the accurate determination of quantitative dimension changemeasurements.5.2 This test method may be used for instrument performance validation, regulatory compliance, research and development andquality assurance purposes.6. App
16、aratus6.1 Thermomechanical Analyzer (TMA)The essential instrumentation required to provide the minimum thermomechanicalanalytical or thermodilatometric capability for this test method includes:6.1.1 A Rigid Specimen Holder, of inert, low expansivity material 0.5 m m-1 K-1 to center the specimen in t
17、he furnace andto fix the specimen to mechanical ground.6.1.2 A Rigid Expansion Probe, of inert, low expansivity material 0.5 m m-1 K1-1 which contacts the specimen with anapplicable compressive or tensile force.6.1.3 A Sensing Element, linear over a minimum of 2 mm, to measure the displacement of th
18、e rigid probe to within 6 10 610nm resulting from changes in length/height of the specimen.6.1.4 A Weight or Force Transducer , to generate a constant force between 1 and 100 mN (0.1 and 10 g) applied through therigid probe to the specimen.6.1.5 A Furnace, capable of providing uniform controlled hea
19、ting (cooling) of a specimen to a constant temperature or at aconstant rate within the applicable temperature range of this test method.6.1.6 A Temperature Controller, capable of executing a specific temperature program by operating the furnace over any suitabletemperature range between -150150 and
20、1000 C 1000C at a rate of temperature change of 5 K/min constant to within 6 0.160.1 K/min.6.1.7 A Temperature Sensor, that can be attached to, in contact with, or reproducibly positioned in close proximity to thespecimen to provide an indication of the specimen/furnace temperature to within 6 0.1 6
21、0.1 K.6.1.8 A means of sustaining an environment around the specimen of an inert purge gas at a rate of 10 to 50 6 5 mL/min.NOTE 1Typically, 99.9+% 99.9+ % pure nitrogen, helium or argon is employed, when oxidation in air is a concern. Unless effects of moisture areto be studied, use of dry purge ga
22、s is recommended and is essential for operation at subambient temperatures.6.1.9 A Data Collection Device, to provide a means of acquiring, storing, and displaying measured or calculated signals, or both.The minimum output signals required are dimension (length) change, temperature, and time.6.2 Mic
23、rometer, calipers or other length measurement device capable of measuring linear dimensions up to 10 mm withreadability of 6 25 625 m.6.3 While not required, the user may find useful software that performs the calculations described in this test method.6.4 Thermal expansion reference material of 8 6
24、 2 mm length, the linear coefficient of expansion of which is known to 6 0.160.1 m m-1 K-1. The coefficient of thermal expansion should be between 9 and 40 m m-1 K-1.6.4.1 Reference materials of known value traceable to a National Reference laboratory are available from a number of suppliers.Contact
25、 ASTM Headquarters for list of such potential suppliers.46.4.1 In the absence of primary or secondary reference materials, high purity aluminum or platinum may be used along withthe values for coefficient of thermal expansion presented in Table 1.NOTE 2The linear expansion of high purity aluminum, c
26、ommonly supplied by instrument manufactures, is useful as a working reference material.Coefficient of thermal expansion values for pure aluminum are presented in Table 1 along with those for platinum.7. Test Specimen7.1 Specimens shall be between 6 and 10 mm in length and have flat and parallel ends
27、 to within 6 25 625 m. Lateraldimensions shall be between 3 and 9 mm. Other lengths and widths may be used but shall be noted in the report.8. Calibration8.1 Perform any calibration procedures described in the manufacturers operations manual.8.2 Calibrate the temperature sensor using Test Method E13
28、63.9. Procedure9.1 Measure the initial specimen length in the direction of the expansion test to within 6 25 625 m at 23 6 2 C.2C.4 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:E37-1033. Contact ASTM CustomerService at servic
29、eastm.org.E2113 1329.2 Place the specimen on the specimen holder under the probe. Place the specimen temperature sensor within 2 mm but nottouching the test specimen.9.3 Move the furnace to enclose the specimen holder. If measurements at subambient temperatures are to be made, cool the testspecimen
30、to at least 20 C 20C below the lowest temperature of interest.The refrigerant used for cooling shall not come into directcontact with the specimen.NOTE 3The refrigerant used for cooling shall not come into direct contact with the specimen.9.4 Apply an appropriate load force to the sensing probe to e
31、nsure that it is in contact with the specimen. A force between 1and 50 mN (0.1 and 5 g) is adequate. The actual incremental force, mass or stress above that required to make contact with thezero force shall be noted in the report.9.5 Heat the specimen at a rate of 5 6 0.1 C/min 0.1C/min over the des
32、ired temperature range and record the change inspecimen length and temperature to all available decimal places. Other heating rates may be used but shall be noted in the report.NOTE 4Other heating rates may be used but shall be noted in the report.NOTE 5For best results, specimen temperature gradien
33、ts should be small. High heating rates, large specimen size and low specimen thermalconductivity may lead to large specimen temperature gradients.NOTE 4Intralaboratory testing indicates that no detectable increase in imprecision is observed for specimens size 2 to 20 mm in length, for heatingrates b
34、etween 2 and 10 C min-1 and for thermal conductivities between 0.2 and 400 Wm-1 K1, if only one parameter is changed.9.6 Determine the measurement instrument baseline by repeating steps 9.2 9.5 using the same test parameters but without atest specimen. The measured change of length (L) of the specim
35、en should normally be corrected by curve subtraction for thisbaseline (that is, the probe is placed on the empty specimen holder) especially for low expansion materials.9.7 Select a temperature change range (T) from a smooth portion of the thermal curve in the desired temperature range. Thenobtain t
36、he L for this temperature range as depicted in Fig. 1.9.8 Record the change in length (L) for the test specimen over a corresponding change in temperature (T). See Fig. 1.TABLE 1 Thermal Expansion CoefficientsAAluminum BCDEF Platinum GHIJTemperature, C Mean Coefficient of Linear Thermal Expansion,m/
37、(m C) Mean Coefficient of Linear Thermal Expansion,m/(m C)1100 12.331000 11.87900 11.26800 11.08700 10.75600 10.45550 35.3 10.31500 33.2 10.18450 31.8 10.05400 30.5 9.92350 29.2 9.80300 27.8 9.67250 26.8 9.64200 26.2 9.45150 25.5 9.38100 24.5 9.1850 23.6 9.010 22.6 8.8550 20.9 8.59100 18.8 8.19150 7
38、.37A Mean coefficient of linear thermal expansion values are calculated for 50 C 50C from the indicated temperature except in the case of platinum where values arefor 100 C 100C of the indicated temperature for the range of 200 to 700 C.700C.B Nix, F. C., and MacNair D., MacNair, D., “The Thermal Ex
39、pansion of Pure Metals: Copper, Gold, Aluminum, Nickel, and Iron,” Physical Review, Vol 60, 1941, p. 597.pp.597605.C Simmons, R. O., and Balluffi R. W., Balluffi, R. W., “Measurments of Equilibrium Vacancy Concentrations inAluminum,” Physical Review, Vol 117, 1960, p. 52.pp. 5231.D Fraser, D. B., an
40、d Hollis Hallet, A. C., “The Coefficient of Linear Expansion and Gruneisen of Cu, Ag, Au, Fe, Ni, and Al from 4K to 300K,” Proceedings of the 7thInternational Conference on Low-Temperature Physics, 1961, p. 689.pp. 689692.E Altman, H. W., Rubin, T., and Johnson, H. L., Ohio State University, Cryogen
41、ic Laboratory Report OSU-TR-26427 (1954) AD 26970.F Hidnert, P., and Krider, H. S., “Thermal Expansion ofAluminum and SomeAluminumAlloys,” Journal of Research National Bureau of Standards, Vol 48, 1952, p. 209.pp.209220.G Nix, F. C., and MacNair, D., “The Thermal Expansion of Pure metals. II: Molybd
42、enum, Palladium, Silver, Tantalum, Tungsten, Platinum, and Lead,” Physical Review, Vol61, 1942, p. 74.pp. 7478.H White, G. K., “Thermal Expansion of Platinum at Low Temperature,” Journal of Physics, Vol 2F, 1972, p. 130.pp. L30L31.I Hahn, T. A., and Kirby, R. K., “Thermal Expansion of Platinum from
43、293 to 1900 K,” AIP American Institute of Physics Conference Proceedings, No. 3, Vol 87, 1972.3,1972, pp. 8795.J Kirby, R. K., “Platinum AThermal Expansion Reference Material,” Thermal Conductivity 24/Thermal Expansion 12,12, Technomic Publishing, Lancaster, PA 1997, pp.655661.E2113 133NOTE 6For the
44、 best calibration results, values for T should range between 50 and 100 C. 100C.10. Calculation10.1 Calculate the mean coefficient of linear thermal expansion for the desired temperature range and calibration coefficientretaining all available significant figures.k 5LT/L (1)where: = mean coefficient
45、 of linear thermal expansion for the reference material at the midpoint of the T range, in m m-1 C-1k = calibration coefficient, dimensionlessL = length of the reference material at room temperature, in mL = change in length of the reference material due to heating, in mT = temperature difference ov
46、er which the change in specimen length is measured, in C.NOTE 7The mean coefficient of linear thermal expansion described here is an approximation to the traditional coefficient of linear thermal expansionwhere the reference length is taken at the test temperature of interest. This approximation cre
47、ates a bias on the order of about 0.015%.10.2 The true length change (Lt) of an unknown may be derived by multiplication of the observed length change (Lo) by thecalculation coefficient (k).Lt 5kLo (2)11. Report11.1 Designation of the Reference Material for coefficient of linear thermal expansion in
48、cluding its source, lot number andchemical composition.FIG. 1 Specimen Expansion Versus TemperatureE2113 13411.2 Dimensions of the specimen and any physical, mechanical or thermal pre-treatment and orientation with respect to theoriginal part (if cut to size).11.3 Designation of the thermomechanical
49、 analyzer by model number, serial number and specimen holder stage and probe type.11.4 Experimental conditions including temperature range of test, heating rate, purge gas type and flow rate.11.5 The calibration coefficient value determined the mid-point of the temperature range of calibration. For example: k = 1.001at 100 C.100C.11.6 The specific dated version of this test method used.12. Precision and Bias12.1 Precision:12.1.1 Precision of the calibration constant v
