1、Designation: D 4065 06Standard Practice forPlastics: Dynamic Mechanical Properties: Determination andReport of Procedures1This standard is issued under the fixed designation D 4065; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, t
2、he 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This practice is for gen
3、eral 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 dyn
4、amic 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 elasti
5、c and 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 pr
6、actice 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 3 107psi.1.5 Discrepancies
7、 in 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
8、assumption 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
9、 in engineering design.1.8 The values stated in SI units are to be regarded asstandard. The values given in brackets are for information only.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:2D 618 Practice for Conditioning
11、Plastics for TestingD 4000 Classification System for Specifying Plastic Mate-rialsD 4092 Terminology for Plastics: Dynamic MechanicalPropertiesD 4440 Test Method for Plastics: Dynamic MechanicalProperties Melt RheologyD 5023 Test Method for Plastics: Dynamic MechanicalProperties: In Flexure (Three-P
12、oint Bending)D 5024 Test Method for Plastics: Dynamic MechanicalProperties: In CompressionD 5026 Test Method for Plastics: Dynamic MechanicalProperties: In TensionD 5279 Test Method for Plastics: Dynamic MechanicalProperties: In TorsionD 5418 Test Method for Plastics: Dynamic MechanicalProperties: I
13、n Flexure (Dual Cantilever Beam)E 1867 Test Method for Temperature Calibration of Dy-namic Mechanical AnalyzersE 2254 Test Method for Storage Modulus Calibration ofDynamic Mechanical AnalyzersE 2425 Test Method for Loss Modulus Conformance of1This practice is under the jurisdiction ofASTM Committee
14、D20 on Plastics andis the direct responsibility of Subcommittee D20.10 on Mechanical Properties.Current edition approved Dec. 1, 2006. Published December 2006. Originallyapproved in 1982. Last previous edition approved in 2001 as D 4065 - 01.2For referenced ASTM standards, visit the ASTM website, ww
15、w.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.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive,
16、 PO Box C700, West Conshohocken, PA 19428-2959, United States.Dynamic Mechanical Analyzers2.2 ISO Standard:ISO 67211 Plastics Determination of Dynamic Me-chanical Properties, Part 1, General Principles33. Terminology3.1 DefinitionsFor definitions of terms relating to thispractice, see Terminology D
17、4092.4. Summary of Practice4.1 A specimen 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 both the latte
18、r. 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 measurement of elasti
19、c and lossmoduli depends upon the operating principle of the instrument used.4.2 D 5023, D 5024, D 5026, D 5279, and D 5418 describespecific methods for determining dynamic mechanical proper-ties.5. Significance and Use5.1 Dynamic mechanical testing provides a method fordetermining elastic and loss
20、moduli as a function of tempera-ture, frequency or time, or both. A plot of the elastic modulusand loss modulus of material versus temperature provides agraphical representation of elasticity and damping as a functionof temperature or frequency.5.2 This procedure can be used to locate transition tem
21、pera-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 temperat
22、ure). 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 multicomponent sys-tems,5.3.2 Fil
23、ler 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 of tria
24、xial 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 specification
25、 before using this practice. Table 1 ofClassification System D 4000 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 of the
26、 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 one of
27、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 amplitude,
28、 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 grip-
29、ping of the sample.7.2.2 Oscillatory Deformation (Strain)A device for ap-plying 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).7.2.3 De
30、tectorsA 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 for c
31、on-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 for p
32、urging 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 personnel
33、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.D40650629. Test Specimens9.1 Specimens are of any uniform size or shape but areordinarily analyzed in rectangula
34、r 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 50 mm
35、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, thin
36、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 65 % for not lessthan 40 h prior to test
37、in accordance to ProcedureAof PracticeD 618, for those tests where conditioning is required. If otherspecimen conditioning is used, it should be noted in the report.10. Calibration10.1 Using the same heating rate or schedule to be used forspecimens, calibrate the instrument temperature axis, using t
38、heinstrument manufacturers procedures with either or both of thefollowing substances. Refer to E 1867, E 2254, and E 2425 foradditional details on calibration.Standard Transition Temperature, C Type of TransitionWater 0.0 fusionIndium 156.6 fusion11. Procedure11.1 Measure the length, width, and thic
39、kness 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 or chang
40、ing 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,mmCalculationsOscillatingStrainElasticComponentDampingComponentDynamicmechanicalanalyzerSinusoidal
41、/fixed orresonancefrequencyForced constant amplitude-fixed or resonance frequencyflexural oscillation0.001 to 60 Hz t = 0.011.6b = 0.0213L = 18, 25, or 336 3tA (2D +L)/L2RRectangular:Tan d = JV/f2E8 54p2f2I2H2bL/2 1 D!2L/t#3Circular:E8 =4p2f2I-H/3r4(2D + L)22L3Visco-elastometerASinusoidalfixedfreque
42、ncyForced 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 readMechanicalspectrom
43、eterB,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/tbDLCircular crosssection:Tan d directly readD4065063TABLE 1 Continued
44、Technique 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 orvariablefrequencyForced con
45、stant amplitude;fixed or variablefrequency-compressiveoscillation (see Fig. 6)0.001680 Up to 38 3 38:t =38b =38L = 110DL/L Rectangular crosssection:E8 = NL cosd/tbDLE9 = NL sind/tbDLTan d directly readr = 850t = 110Circular crosssection:E8 = NL cosd/p r2DLE9 = NL sind/pr2D LTan d directly readMechan
46、icalspectrometerB,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/2bt3aE9 = NL3sind/2bt3aTan d directly readr = 0.253.2L = 63.53 ra/L2Circular cross
47、section:E8 =4NL3cos d/3r4aE9 =4NL3sind/3r4aTan 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/tbDLoscillation (s
48、ee 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 3 20 DL/L Rectangular crossMechanical fixed or fixed or variable t = up to 20 section:AnalyzerB,Dvariable
49、 frequency-compression b =upto20 E8 = NL cosd/ tb E9 = NL sin d/frequency oscillation (see Fig. 6) L = 0.001-24 DLtbDLr = 120 Tan d directly readt =upto20DL/L Circular crosssection:E8 = NL cosd/p r2DLE9 = NL cosd/pr2DLTan d directly readDynamicMechanicalAnalyzerB,DSinusoidalfixed orvariablefrequencyConstant force amplitude;fixed or variablefrequency-flexuraloscillation (see Fig. 7)0.0150 t =upto24b =upto10L =upto203 ta/L2Rectangular crosssection:D4065064TABLE 1 ContinuedTechnique Input Excitation Mode of OscillationFrequency Range,HzSpec
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