1、Designation: D4065 12Standard Practice forPlastics: Dynamic Mechanical Properties: Determination andReport of Procedures1This standard is issued under the fixed designation D4065; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、 year 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This practice is for genera
3、l use in gathering and report-ing dynamic mechanical data. It incorporates laboratory prac-tice for determining dynamic mechanical properties of plasticspecimens subjected to various oscillatory deformations on avariety of instruments of the type commonly called dynamicmechanical analyzers or dynami
4、c thermomechanical analyzers.1.2 This practice is intended to provide means of determin-ing the transition temperatures, elastic, and loss moduli ofplastics over a range of temperatures, frequencies, or time, byfree vibration and resonant or nonresonant forced vibrationtechniques. Plots of elastic a
5、nd loss moduli are indicative of theviscoelastic characteristics of a plastic. These moduli arefunctions of temperature or frequency in plastics, and changerapidly at particular temperatures or frequencies. The regionsof rapid moduli change are normally referred to as transitionregions.1.3 The pract
6、ice is primarily useful when conducted over arange of temperatures from 160C to polymer degradationand is valid for frequencies from 0.01 to 1000 Hz.1.4 This practice is intended for materials that have anelastic modulus in the range from 0.5 MPa to 100 GPa (73 psito 1.5 107psi).1.5 Discrepancies in
7、 results are known to arise when ob-tained under differing experimental conditions. Without chang-ing the observed data, reporting in full (as described in thispractice) the conditions under which the data were obtainedwill enable apparent differences observed in another study tobe reconciled.An ass
8、umption of this technique is that testing isconducted in the region of linear viscoelastic behavior.1.6 Different modes of deformation, such as tensile, bendingand shear, are used, as listed in the referenced test methods.1.7 Test data obtained by this practice are relevant andappropriate for use in
9、 engineering design.1.8 The values stated in SI units are to be regarded asstandard. The values given in parentheses are for informationonly.1.9 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this practice
10、to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific hazardsstatements are given in Section 8.NOTE 1This practice is equivalent to ISO 67211.2. Referenced Documents2.1 ASTM Standards:2D618 Practice for Conditioning Pl
11、astics for TestingD4000 Classification System for Specifying Plastic Materi-alsD4092 Terminology for Plastics: Dynamic MechanicalPropertiesD4440 Test Method for Plastics: Dynamic Mechanical Prop-erties Melt RheologyD5023 Test Method for Plastics: Dynamic Mechanical Prop-erties: In Flexure (Three-Poi
12、nt Bending)D5024 Test Method for Plastics: Dynamic Mechanical Prop-erties: In CompressionD5026 Test Method for Plastics: Dynamic Mechanical Prop-erties: In TensionD5279 Test Method for Plastics: Dynamic Mechanical Prop-erties: In TorsionD5418 Test Method for Plastics: Dynamic Mechanical Prop-erties:
13、 In Flexure (Dual Cantilever Beam)E1867 Test Method for Temperature Calibration of DynamicMechanical AnalyzersE2254 Test Method for Storage Modulus Calibration ofDynamic Mechanical AnalyzersE2425 Test Method for Loss Modulus Conformance ofDynamic Mechanical Analyzers1This practice is under the juris
14、diction ofASTM Committee D20 on Plastics andis the direct responsibility of Subcommittee D20.10 on Mechanical Properties.Current edition approved Aug. 1, 2012. Published September 2012. Originallyapproved in 1982. Last previous edition approved in 2006 as D4065 - 06. DOI:10.1520/D4065-12.2For refere
15、nced 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 website.*A Summary of Changes section appears at the end of this standardCopyrig
16、ht ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12.2 ISO Standard:ISO 67211 Plastics Determination of Dynamic Mechani-cal Properties, Part 1, General Principles33. Terminology3.1 DefinitionsFor definitions of terms relating to thispractice, s
17、ee Terminology D4092.4. Summary of Practice4.1 Aspecimen of known geometry is placed in mechanicaloscillation either at fixed or natural resonant frequencies.Elastic or loss moduli, or both of the specimen are measuredwhile varying time, temperature of the specimen or frequencyof the oscillation, or
18、 both the latter. Plots of the elastic or lossmoduli, or both, are indicative of viscoelastic characteristics ofthe specimen. Rapid changes in viscoelastic properties atparticular temperatures, times, or frequencies are normallyreferred to as transition regions.NOTE 2The particular method for measur
19、ement of elastic and lossmoduli depends upon the operating principle of the instrument used.4.2 D5023, D5024, D5026, D5279, and D5418 describespecific methods for determining dynamic mechanical proper-ties.5. Significance and Use5.1 Dynamic mechanical testing provides a method fordetermining elastic
20、 and loss moduli as a function oftemperature, frequency or time, or both. A plot of the elasticmodulus and loss modulus of material versus temperatureprovides a graphical representation of elasticity and dampingas a function of temperature or frequency.5.2 This procedure can be used to locate transi
21、tion tempera-tures of plastics, that is, changes in the molecular motions of apolymer. In the temperature ranges where significant changesoccur, elastic modulus decreases rapidly with increasing tem-perature (at constant or near constant frequency) or increaseswith increasing frequency (at constant
22、temperature). A maxi-mum is observed for the loss modulus, as well as for the tandelta curve, in the transition region.5.3 This procedure can be used, for example, to evaluate bycomparison to known reference materials or control materials:5.3.1 Degree of phase separation in multicomponentsystems,5.3
23、.2 Filler type, amount, pretreatment, and dispersion, and5.3.3 Effects of certain processing treatment.5.4 This procedure can be used to determine the following:5.4.1 Stiffness of polymer composites, especially as a func-tion of temperature,5.4.2 Degree of polymer crystallinity, and5.4.3 Magnitude o
24、f triaxial stress state in the rubber phase ofrubber modified polymers.5.5 This procedure is useful for quality control, specifica-tion acceptance, and research.5.6 Procedural modifications in material specifications takeprecedence to this practice. Therefore, consult the appropriatematerial specifi
25、cation before using this practice. Table 1 ofClassification System D4000 lists the ASTM materials stan-dards that currently exist.6. Interferences6.1 Since small quantities of specimen are used, it isessential that the specimens be homogeneous or representative,or both.7. Apparatus7.1 The function o
26、f the apparatus is to hold a plasticspecimen of uniform cross section, so that the specimen acts asthe elastic and dissipative element in a mechanically oscillatedsystem. Instruments of this type are commonly called dynamicmechanical or dynamic thermomechanical analyzers. Theytypically operate in on
27、e of seven oscillatory modes: (1) freelydecaying torsional oscillation, (2) forced constant amplitude,resonant, flexural oscillation, (3) forced constant amplitude,fixed frequency, compressive oscillation, (4) forced constantamplitude, fixed frequency, flexural oscillation, (5) forced,constant ampli
28、tude, fixed frequency, tensile oscillation, (6)forced constant amplitude, fixed frequency, torsional oscilla-tion and (7) forced constant amplitude, fixed frequency, orvariable frequency dual cantilever.7.2 The apparatus shall consist of the following:7.2.1 ClampsA clamping arrangement that permits
29、grip-ping of the sample.7.2.2 Oscillatory Deformation (Strain)Adevice for apply-ing an oscillatory deformation (strain) to the specimen. Thedeformation (strain) shall be applied and then released, as infree-vibration devices, or continuously applied, as in forced-vibration devices (see Table 1).7.2.
30、3 DetectorsA device or devices for determining de-pendent and independent experimental parameters, such asforce (stress or strain), frequency, and temperature. Tempera-ture shall be measurable with an accuracy of 61C, frequencyto 61 %, and force to 61%.7.2.4 Temperature Controller and OvenA device f
31、or con-trolling the specimen temperature, either by heating (in steps orramps), cooling (in steps or ramps), or maintaining a constantspecimen environment. Any temperature programmer shouldbe sufficiently stable to permit measurement of sample tem-perature to 60.5C.7.3 Nitrogen or other gas supply f
32、or purging purposes.7.4 Calipers or other length-measuring device capable ofmeasuring to an accuracy of 60.01 mm.8. Hazards8.1 Precautions:8.1.1 Certain materials, when heated near their decomposi-tion point, can release potentially toxic, or corrosive effluents,or both that can be harmful to person
33、nel or to the apparatus.8.1.2 Buckling of the clamped specimen due to thermalexpansion during the test.3Available from American National Standards Institute, 25 W. 43rd St., NewYork, NY 10036.D4065 1229. Test Specimens9.1 Specimens are of any uniform size or shape but areordinarily analyzed in recta
34、ngular form. If some heat treatmentis applied to the specimen to obtain this preferred analyticalform, this treatment shall be noted in the report.9.2 Due to the numerous types of dynamic mechanicalinstruments, specimen size is not fixed by this practice. Inmany cases, a specimen of 0.75 by 9.4 by 5
35、0 mm (0.03 by 0.38by 2.0 in.) is found to be usable and convenient.NOTE 3It is important to select a specimen size consistent with themodulus of the material under test and capabilities of the measuringapparatus. For example, while thick specimens of low modulus materialsare suitable for measurement
36、, thin specimens of high modulus materialsare required.9.3 Unless otherwise specified in the appropriate materialspecification, condition the specimen at a set temperature of23C (73F) that is maintained 62C (64F) and at a setrelative humidity of 50 % that is maintained 610 % for notless than 40 h pr
37、ior to test in accordance to Procedure A ofPractice D618, for those tests where conditioning is required. Ifother specimen conditioning is used, it should be noted in thereport.10. Calibration10.1 Using the same heating rate or schedule to be used forspecimens, calibrate the instrument temperature a
38、xis, using theinstrument manufacturers procedures with either or both of thefollowing substances. Refer to E1867, E2254, and E2425 foradditional details on calibration.Standard Transition Temperature, C Type of TransitionWater 0.0 fusionIndium 156.6 fusion11. Procedure11.1 Measure the length, width,
39、 and thickness of the speci-men to an accuracy of 61%.11.2 Maximum strain amplitude shall be within the linearviscoelastic range of the material. Strains of less than 1 % arerecommended.11.3 If temperature is to be the independent variable:11.3.1 The test frequency shall be from 0.01 to 500 Hz,fixed
40、 or changing as the dependent variable.TABLE 1 Summary of Techniques and Calculations Used to Determine Dynamic Mechanical PropertiesTechnique Input Excitation Mode of OscillationFrequency Range,HzSpecimen Size,mmCalculationsOscillatingStrainElasticComponentDampingComponentDynamicmechanicalanalyzerS
41、inusoidal/fixed orresonancefrequencyForced constant amplitude-fixed or resonance frequencyflexural oscillation0.001 to 60 Hz t = 0.011.6b = 0.0213L = 18, 25, or 333tA (2 D +L)/L2RRectangular:Tan d = JV/f2E854p2f2I2H2bsL/21Dd2fL/tg3Circular:E8 =4p2f2I-H/3r4(2D + L)22L3Visco-elastometerASinusoidalfixe
42、dfrequencyForced constant amplitude-fixed frequency-tensile oscillation(see Fig. 4)3.5, 11, 35,110L =7cmT =0.05cmB =0.4cmDL/L Rectangular crosssection:E8 = NL:/ btD Lcos dCircular crosssection:E9 = NL/ tbDLsin dTan d directly readDL/LE8 = NL cosd/p r2DLE9 = NL sind/p r2DLTan d directly readMechanica
43、lspectrometerB,CSinusoidalfixed orForced constant amplitude;fixed or variable0.0016 to 80 t = 0.0251.0b = 12.7DL/L Rectangular crosssection:variablefrequencyfrequency-tensileoscillation (see Fig. 5)L = 63.5 E8 = NL cos d/btD/ LE9 = NL sind/tbD LCircular crosssection:Tan d directly readD4065 123TABLE
44、 1 ContinuedTechnique Input Excitation Mode of OscillationFrequency Range,HzSpecimen Size,mmCalculationsOscillatingStrainElasticComponentDampingComponentr = 1.6, 2.35,3.15L = 63.5DL/LE8 = NL cosd/p r2D/LE9 = NL sind/p r2D/LTan d directly readMechanicalspectrometerB,CSinusoidalfixed orvariablefrequen
45、cyForced constant amplitude;fixed or variablefrequency-compressiveoscillation (see Fig. 6)0.001680 Up to 38 38:t =38b =38L = 110DL/L Rectangular crosssection:E8 = NL cosd/tbDLE9 = NL sind/tbD LTan d directly readr = 850t = 110Circular crosssection:E8 = NL cosd/p r2DLE9 = NL sind/pr2D LTan d directly
46、 readMechanicalspectrometerB,CSinusoidalfixed orvariablefrequencyForced constant amplitude;fixed or variablefrequency-flexuraloscillation (see Fig. 7)0.001680 t = 0.56.4b = 12.7L = 63.53 ta/L2Rectangular crosssection:E8 NL3cos d/2 bt3aE9 = NL3sind/2bt3aTan d directly readr = 0.253.2L = 63.53 ra/L2Ci
47、rcular crosssection:E8 =4NL3cos d/3r4aE9 =4NL3sind/3 r4aTan d directly readDynamicMechanicalSinusoidalfixed orConstant forceamplitude;0.0150 t =upto2.0b =upto10DL/L Rectangular crosssection:AnalyzerB,Dvariablefrequencyfixed or variablefrequency-tensileL =upto24 E8 = NL cosd/ btD/ LE9 = NL sin d/tbD
48、Loscillation (see Fig. 5) Tan d directly readr =upto2.0L =upto24DL/L Circular crosssection:E8 = NL cosd/p r2D/LE9 = NL sind/p r2D/LTan d directly readDynamic Sinusoidal Constant force amplitude; 0.0150 Up to 3 20 DL/L Rectangular crossMechanical fixed or fixed or variable t = up to 20 section:Analyz
49、erB,Dvariable frequency-compression b =upto20 E8 = NL cosd/ tb E9 = NL sind/frequency oscillation (see Fig. 6) L = 0.001-24 DLtbD Lr = 120 Tan d directly readt =upto20DL/ L Circular crosssection:E8 = NL cosd/p r2DLE9 = NL sind/pr2DLTan d directly readDynamicMechanicalAnalyzerB,DSinusoidalfixed orvariablefrequencyConstant force amplitude;fixed or variablefrequency-flexuraloscillation (see Fig. 7)0.0150 t =upto24b =upto10L =upto203 ta/L2Rectangular crosssection:D4065 124TABLE 1 ContinuedTechnique Input Excitation Mode of OscillationFreque
