ASTM E1640-2004 Standard Test Method for Assignment of the Glass Transition Temperature By Dynamic Mechanical Analysis《用动态力学分析测定玻璃转变温度的标准试验方法》.pdf
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1、Designation: E 1640 04Standard Test Method forAssignment of the Glass Transition Temperature ByDynamic Mechanical Analysis1This standard is issued under the fixed designation E 1640; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,
2、the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the assignment of a glasstransition temperature (Tg) of materials using dynamic m
3、e-chanical analyzers.1.2 This test method is applicable to thermoplastic poly-mers, thermoset polymers, and partially crystalline materialswhich are thermally stable in the glass transition region.1.3 The applicable range of temperatures for this testmethod is dependent upon the instrumentation used
4、, but, inorder to encompass all materials, the minimum temperatureshould be about 150C.1.4 This test method is intended for materials having anelastic modulus in the range of 0.5 MPa to 100 GPa.1.5 Electronic instrumentation or automated data analysisand data reduction systems or treatments equivale
5、nt to this testmethod may also be used.NOTE 1The user bears the responsibility for determining the preci-sion, accuracy, and validity of the techniques and measurements madeusing dynamic mechanical analyzers in accordance with this standard.1.6 SI units are the standard.1.7 This standard is similar
6、to IEC 61006 except thatstandard uses the peak temprature of the mechanical loss peakas the glass transition temperature while this standard uses theextrapolated onset temperature of the loss modulus change.1.8 This standard does not purport to address all of thesafety concerns, if any, associated w
7、ith its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 4092 Terminology Relating to Dynamic MechanicalMeasurements in
8、PlasticsE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE 1142 Terminology Relating to Thermophysical PropertiesE 1363 Test Method for Temperature Calibration of Ther-momechanical AnalyzersE 1545 Test Method for the Determination of Glass Transi-tion
9、Temperatures by Thermomechanical AnalysisE 1867 Test Method for Temperature Calibration of Dy-namic Mechanical AnalyzersE 2254 Test Method for Storage Modulus Calibration ofDynamic Mechanical Analyzers2.2 Other Standards:SRM 18R-94 Recommended Method for Glass TransitionTemperature (Tg) Determinatio
10、n by DMA of OrientedFiber-Resin Composites3IEC 61006 Methods of Test for the Determiantion of theGlass Transition Temperatue of Electrical Insulating Ma-terials43. Terminology3.1 Definition:3.1.1 Specific technical terms used in this document aredefined in Terminology D 4092 and E 1142.3.1.2 dynamic
11、 mechanical analyzerany of various com-mercial or experimental devices used to study the viscoelasticresponse of a specimen under a forced or free resonantoscillatory load. The force may be applied in torsion, flexure,or a combination of tension and compression.4. Summary of Test Method4.1 Aspecimen
12、 of known geometry is placed in mechanicaloscillation at either fixed or resonant frequency and changes inthe viscoelastic response of the material are monitored as afunction of temperature. Under ideal conditions, the glasstransition region is marked by a rapid decrease in the storagemodulus and a
13、rapid increase in the loss modulus. The glass1This test method is under the jurisdiction ofASTM Committee E37 on ThermalMeasurements and is the direct responsibility of Subcommittee E37.01 on TestMethods and Recommended Practices.Current edition approved June 1, 2004. Published July 2004. Originally
14、 approvedin 1994. Last previous edition approved in 1999 as E 1640992For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM w
15、ebsite.3Available from Cuppliers of Advanced Composite Materials Association,Arlington, VA.4Available from American National Standards Institute (ANSI), New York, NY.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.transition of the t
16、est specimen is indicated by the extrapolatedonset of the decrease in storage modulus which marks thetransition from a glassy to a rubbery solid.5. Significance and Use5.1 This test method can be used to locate the glasstransition region and assign a glass transition temperature ofamorphous and semi
17、-crystalline materials.5.2 Dynamic mechanical analyzers monitor changes in theviscoelastic properties of a material as a function of tempera-ture and frequency, providing a means to quantify thesechanges. In ideal cases, the temperature of the onset of thedecrease in storage modulus marks the glass
18、transition.5.3 A glass transition temperature ( Tg) is useful in charac-terizing many important physical attributes of thermoplastic,thermosets (see SRM 18R-94), and semi-crystalline materialsincluding their thermal history, processing conditions, physicalstability, progress of chemical reactions, d
19、egree of cure, andboth mechanical and electrical behavior. Tgmay be determinedby a variety of techniques and may vary in accordance with thetechnique.5.4 This test method is useful for quality control, specifica-tion acceptance, and research.6. Interferences6.1 Because the specimen size will usually
20、 be small, it isessential that each specimen be homogeneous and/or represen-tative of the material as a whole.6.2 An increase or decrease in heating rates from thosespecified may alter results.6.3 A transition temperature is a function of the experimen-tal frequency, therefore the frequency of test
21、must always bespecified. (The transition temperature increases with increasingfrequency.) Extrapolation to a common frequency may beaccomplished using a predetermined frequency shift factor orassuming the frequency shift factor of about 8C per decade offrequency.57. Apparatus7.1 The function of the
22、apparatus is to hold a specimen ofuniform dimension so that the sample acts as the elastic anddissipative element in a mechanically oscillated system. Dy-namic mechanical analyzers typically operate in one of severalmodes. See Table 1.7.2 The apparatus shall consist of the following:7.2.1 Clamps, a
23、clamping arrangement that permits grippingof the specimen. Samples may be mounted by clamping at bothends (most systems), one end (for example, torsional pendu-lum), or neither end (free bending between knife edges).7.2.2 Oscillatory Stress (Strain), for applying an oscillatorydeformation (strain) o
24、r oscillatory stress to the specimen. Thedeformation may be applied and then released, as in freelyvibrating devices, or continuously applied, as in forced vibra-tion devices.7.2.3 Detector, for determining the dependent and indepen-dent experimental parameters, such as force (or stress), dis-placem
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