1、Designation: E2347 11E2347 16Standard Test Method forIndentation Softening Temperature by ThermomechanicalAnalysis1This standard is issued under the fixed designation E2347; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、of last 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 is applicable to materials that soften upon heating to a modulus less than 6.0 MPa. This test meth
3、oddescribes the determination of the temperature at which the specific modulus of either 6.65 (Method A) or 33.3 MPa (Method B)(equivalent to Test Method D1525) of a test specimen is realized by indentation measurement using a thermomechanical analyzeras the test specimen is heated. This temperature
4、 is identified as the indentation softening temperature. The test may be performedover the temperature range of ambient to 300 C.300C.NOTE 1This test method is intended to provide results similar to those of Test Method D1525 but is performed on a thermomechanical analyzer usinga smaller diameter in
5、denting probe. Equivalence of results to those obtained by Test Method D1525 has been demonstrated on a limited number ofmaterials. Until the user demonstrates equivalence, the results of this Test Method shall be considered to be independent and unrelated to those of TestMethod D1525.1.2 This test
6、method is not recommended for ethyl cellulose, poly (vinyl chloride), poly (vinylidene chloride) and othermaterials having a large measurement imprecision (see Test Method D1525 and 5.3 and Section 14).1.3 The values stated in SI units are to be regarded as standard. No other units of measurement ar
7、e included in this standard.1.4 There is no ISO standard equivalent to this test method.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices
8、 and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1525 Test Method for Vicat Softening Temperature of PlasticsE473 Terminology Relating to Thermal Analysis and RheologyE1142 Terminology Relating to Thermophysical PropertiesE1363 Test M
9、ethod for Temperature Calibration of Thermomechanical AnalyzersE2113 Test Method for Length Change Calibration of Thermomechanical AnalyzersE2206 Test Method for Force Calibration of Thermomechanical Analyzers3. Terminology3.1 Definitions:3.1.1 Specific technical terms used in this standard test met
10、hod are defined in Terminologies E473 and E1142. including Celsius,complex modulus, modulus, strain, stress, storage modulus, thermal analysis, and thermomechanical analysis.3.1.2 penetration softening temperature, C,nthe temperature at which a test specimen has a modulus of either 6.65 or 33.3MPa a
11、s measured in penetration.4. Summary of Test Method4.1 The modulus of a material may be determined by the indentation (penetration) of a circular, flat tipped probe. Therelationship between modulus of a material (stress divided by strain) and penetration depth is given by:1 This test method is under
12、 the jurisdiction of ASTM Committee E37 on Thermal Measurements and is the direct responsibility of Subcommittee E37.10 on Fundamental,Statistical and Mechanical Properties.Current edition approved April 1, 2011April 1, 2016. Published May 2011April 2016. Originally approved in 2004. Last previous e
13、dition approved in 20052011 asE2347 05.E2347 11. DOI: 10.1520/E2347-11.10.1520/E2347-16.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standardsstandards Docume
14、nt Summary page on the ASTM website.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 rec
15、ommends 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 States1E 53F/4D d!
16、(1)where:E = modulus, MPa,F = force, N,D = diameter of a circular, flat tipped probe, mm, andd = penetration depth, mm.NOTE 2Note the identity Pa = N / m2.4.2 Some materials soften upon heating. For such materials, the modulus may be determined by penetration as the sample isheated. This test method
17、 identifies the temperature at which the modulus of the specimen is determined to be 6.65 MPa (MethodA) or 33.3 MPa (Method B).4.3 Specifically, a test specimen is tested in penetration using a circular, flat tipped probe.Aknown stress is applied to the centerof a test specimen as it is heated at a
18、constant rate from ambient temperature to the upper temperature limit for the material. Thepenetration (that is, deflection) of the test specimen is recorded as a function of temperature. The temperature at which the modulusof the specimen is determined to be 6.65 MPa (Method A) or 33.3 MPa (Method
19、B) is determined to be the penetration softeningtemperature.5. Significance and Use5.1 Data obtained by this test method shall not be used to predict the behavior of materials at elevated temperatures except inapplications in which the conditions of time, temperature, method of loading, and stress a
20、re similar to those specified in the test.5.2 This standard test method is particularly suited for quality control and development work. The data are not intended for usein design or predicting endurance at elevated temperatures.5.3 Ruggedness testing indicates that some materials, such as poly (vin
21、yl chloride) exhibit substantially greater imprecision thanthat described in Section 14 for “well behaved” materials.6. Apparatus6.1 A thermomechanical analyzer consisting of:6.1.1 Rigid Specimen Holder, of inert, low expansivity material ( 1 (1 m m-1 C-1) to center the specimen in the furnace andto
22、 fix the specimen to mechanical ground.6.1.2 Rigid Penetration Probe, of inert, low expansivity material ( 1 (1 m m-1 C-1) that contacts the specimen with anapplied compression force (see Fig. 1). The tip shall be 0.1 to 1.0 mm in diameter, free of burrs and be perpendicular to the axisof the probe.
23、 The tip shall protrude at least 0.1 mm from the end of the probe.6.1.3 Deflection Sensing Element, having a linear output over a minimum range of 5 mm to measure the displacement of therigid penetration probe (see 6.1.2) to within 60.1 m.6.1.4 Programmable Force Transducer, to generate a constant f
24、orce (6 2.5 %)(62.5 %) between 0.05 and 1.0 N that is appliedto the specimen through the rigid penetration probe (see 6.1.2).FIG. 1 Penetration ProbeE2347 162NOTE 3Other forces may be used but shall be reported.6.1.5 Temperature Sensor, that can be positioned reproducibly in close proximity to the s
25、pecimen to measure its temperatureover the range of 25 to 300 C 300C to 6 0.1 C.0.1C.6.1.6 Temperature Programmer and Furnace, capable of temperature programming the test specimen from ambient to 300 C300C at a linear rate of at least 2.0 6 0.2 C/min.0.2C/min.6.1.7 Means of Providing a Specimen Envi
26、ronment, of inert gas at a purge rate of 50 mL/min 6 5 %.5 %.NOTE 4Typically, inert purge gas that inhibits specimen oxidation are 99.9+ % pure nitrogen, helium or argon. Dry gases are recommended for allexperiments unless the effect of moisture is part of the study.6.1.8 Data Collection Device, to
27、provide a means of acquiring, storing, and displaying measured or calculated signals, or both.The minimum output signals required are a change in linear dimension to a sensitivity of 60.1 mm, and temperature to a sensitivityof 61 um.m.6.1.9 Calipers, Micrometer, or other length measuring device capa
28、ble of a length measurement of up to 2 mm with a precisionof 61 m.7. Hazards7.1 Toxic or corrosive effluents, or both, may be released when heating some materials and could be harmful to personnel andto apparatus.8. Sampling, Test Specimens, and Test Units8.1 Because the specimen size is small, care
29、 shall be taken to ensure that each specimen is homogeneous and representative ofthe sample as a whole.8.2 The specimen may be cut from sheets, plates or molded shapes, or may be molded to the desired finished dimensions.8.3 A typical test specimen is a rectangle 78 78 7 to 8 7 to 8 mm or a circle 7
30、8 7 to 8 mm in diameter with a thicknessof 1 to 3 mm.8.4 This standard test method assumes that the material is isotropic. Should specimens be anisotropic, such as in reinforcedcomposites, the direction of the reinforcing agent shall be reported relative to the compression (specimen) dimensions.9. P
31、reparation of Apparatus9.1 Perform any setup or calibration procedures recommended by the apparatus manufacturer in the operations manual.10. Calibration and Standardization10.1 Calibrate the temperature display of the apparatus according to Test Method E1363 using a heating rate of 2.0 6 0.2C/min.0
32、.2C/min.10.2 Calibrate the deflection display of the apparatus according to Test Method E2113.10.3 Calibrate the mechanism for applying force to the test specimen according to Test Method E2206.11. Procedure11.1 Measure the diameter of the circular penetration tip of the penetration probe to 61 m an
33、d record this value as D.11.2 Method A:11.2.1 Set the value of Force (F) at 0.15 6 0.004 N.11.2.2 Proceed with steps 11.3.2 11.3.4.611.3.2 to 11.3.4.6.11.3 Method B:11.3.1 Set the value of Force (F) to 0.75 6 0.01 N.11.3.2 Perform Scouting Experiment:11.3.2.1 Using Eq 2 and an estimated value of do
34、= 0, estimate the deflection (dd) to be used as the experimental endpointto three significant figures.11.3.2.2 Center the test specimen on the stage with a surface perpendicular to the loading nose of the penetration probe.11.3.2.3 Load the penetration probe onto the center of the test specimen with
35、 the force determined in 11.2.1 (Method A) or11.3.1 (Method B). Set the deflection signal to zero at ambient temperature.11.3.2.4 Heat the test specimen at 2.0 6 0.2 C 0.2C min-1 from ambient temperature until the deflection d (determined in11.3.2.1) is obtained while recording specimen deflection a
36、nd temperature. Once the deflection value is achieved, terminate thetemperature program and remove the load from the test specimen. Cool the apparatus to ambient temperature.11.3.2.5 Record the temperature at the deflection value d as the estimated indentation softening temperature (T).11.3.2.6 For
37、ease of interpretation, record the thermal curve with penetration displayed on the Y-axis and temperature on theX-axis as illustrated in Fig. 2.E2347 16311.3.3 Determine the Baseline:11.3.3.1 With no sample present, place the tip of the penetration probe onto the center of the sample stage. Load the
38、 probe withthe force determined in 11.2.1 or 11.3.1. Set the deflection scale signal to be zero at ambient temperature.11.3.3.2 Heat the sample area at 2.0 6 0.2 C 0.2C min-1 from ambient temperature to a temperature 5 C 5C higher thanT determined in 11.3.2.5. Once the temperature program is complet
39、e, remove the load from the probe and cool the apparatus toambient temperature.11.3.3.3 Measure the deflection of the baseline at temperature T and record it as do.NOTE 5do is positive for a baseline that expands with temperature and negative if the baseline contracts.11.3.4 Test Specimen:11.3.4.1 U
40、sing Eq 2 and the value for do from 11.3.3.3, determine to three significant figures the deflect (d) to be used as theexperimental endpoint.11.3.4.2 Center the test specimen on the stage with a surface perpendicular to the loading nose of the penetration probe.11.3.4.3 Load the penetration probe ont
41、o the center of the test specimen with the force determined in 11.2.1 (Method A) or11.3.1 (Method B). Set the deflection signal to zero at ambient temperature.NOTE 6During heating, the test specimen may expand (see Fig. 2). Nonetheless, the deflection value is taken from the original dimension of th
42、e testspecimen measured at ambient conditions. This corresponds with the conditions of D1525. Intralaboratory studies show that using the original dimensioncompared to the maximum dimension produces a0.7 C 0.7C increase in the value for T. This is within experimental error (see sectionSection 14).11
43、.3.4.4 Using the appropriate softening temperature determined in 11.3.2.5 start the temperature program 50 C 50C belowthis temperature and heat the test specimen at 2.0 6 0.2 C 0.2C min-1 from ambient temperature until the deflection dFIG. 2 Penetration Curve of PolystyreneE2347 164(determined in 11
44、.3.4.1) is obtained while recording specimen deflection and temperature. Once the deflection value is achieved,terminate the temperature program and remove the load from the test specimen. Cool the apparatus to ambient temperature.11.3.4.5 Record the temperature at the deflection value d as the inde
45、ntation softening temperature (T).11.3.4.6 For ease of interpretation, record the thermal curve with penetration displayed on the Y-axis and temperature on theX-axis as illustrated in Fig. 2.12. Calculation12.1 Calculate the deflection value as follows:E2347 165d 53F/4D E! 2do (2)where:E = modulus,
46、MPa,F = force, N,D = diameter of a circular, flat tipped probe, mm,d = penetration depth, mm, anddo = baseline depth at temperature T, mm.NOTE 7Note the identity Pa = N / m2.12.1.1 For example, if:E = 6.65 MPa,F = 0.15 N,D = 0.889 mm, anddo = 0.0003 mm.13. Report13.1 Report the following information
47、:13.1.1 Complete identification and description of the material tested including source, manufacturer code and any thermal ormechanical pretreatment.13.1.2 Description of the instrument used, including model number and location of the temperature sensor.13.1.3 Details of the procedure used to calcul
48、ate the penetration softening temperature including strain and resulting force, stressand resultant strain, as well as specimen dimensions.13.1.4 Heating rate, C/min, rate and temperature range.13.1.5 A copy of all original records that are presented.13.1.6 The penetration softening temperature (T),
49、 C, and13.1.7 The specific dated version of this test method used.14. Precision and Bias14.1 An interlaboratory study was conducted in 2005 in which polystyrene was tested using MethodA(6.65 MPa modulus) andMethod B (33.3 MPa modulus). Twelve laboratories participated in the test using six instrument models from three manufacturers.33 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:E37-1034. Contact ASTM CustomerService at serviceastm.org
