ASTM D4065-95
(Practice)Standard Practice for Plastics: Dynamic Mechanical Properties: Determination and Report of Procedures
Standard Practice for Plastics: Dynamic Mechanical Properties: Determination and Report of Procedures
SCOPE
1.1 This practice is for general use in gathering and reporting dynamic mechanical data. It incorporates laboratory practice for determining dynamic mechanical properties of specimens subjected to various oscillatory deformations on a variety of instruments of the type commonly called dynamic mechanical analyzers or dynamic thermomechanical analyzers.
1.2 This practice is intended to provide means of determining the transition temperatures, elastic, and loss moduli of plastics over a range of temperatures, frequencies, or time, by free vibration and resonant or nonresonant forced vibration techniques. Plots of elastic and loss moduli are indicative of the viscoelastic characteristics of a plastic. These moduli are functions of temperature or frequency in plastics, and change rapidly at particular temperatures or frequencies. The regions of rapid moduli change are normally referred to as transition regions.
1.3 The practice is primarily useful when conducted over a range of temperatures from -160°C to polymer degradation and is valid for frequencies from 0.01 to 1000 Hz.
1.4 This practice is intended for materials that have an elastic modulus in the range from 0.5 MPa to 100 GPa (73 psi to 1.5 x 10 7 psi).
1.5 Apparent discrepancies may arise in results obtained under differing experimental conditions. Without changing the observed data, reporting in full (as described in this practice) the conditions under which the data were obtained will enable apparent differences observed in another study to be reconciled.
1.6 Test data obtained by this practice are relevant and appropriate for use in engineering design.
1.7 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this practice to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 8.
Note 1—This practice is technically equivalent to ISO 6721, Part 1.
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Designation: D 4065 – 95 An American National Standard
Standard Practice for
Determining and Reporting Dynamic Mechanical Properties
of Plastics
This standard is issued under the fixed designation D 4065; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript 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 priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazards
1.1 This practice is for general use in gathering and report-
statements are given in Section 8.
ing dynamic mechanical data. It incorporates laboratory prac-
tice for determining dynamic mechanical properties of speci-
2. Referenced Documents
mens subjected to various oscillatory deformations on a variety
2.1 ASTM Standards:
of instruments of the type commonly called dynamic mechani-
D 618 Practice for Conditioning Plastics and Electrical
cal analyzers or dynamic thermomechanical analyzers.
Insulating Materials for Testing
1.2 This practice is intended to provide means of determin-
D 4000 Classification System for Specifying Plastic Mate-
ing the transition temperatures, elastic, and loss moduli of
rials
plastics over a range of temperatures, frequencies, or time, by
D 4092 Terminology Relating to Dynamic Mechanical
free vibration and resonant or nonresonant forced vibration
Measurements on Plastics
techniques. Plots of elastic and loss moduli are indicative of the
viscoelastic characteristics of a plastic. These moduli are
3. Terminology
functions of temperature or frequency in plastics, and change
3.1 Definitions—For definitions of terms relating to this
rapidly at particular temperatures or frequencies. The regions
practice, see Terminology D 4092.
of rapid moduli change are normally referred to as transition
regions.
4. Summary of Practice
1.3 The practice is primarily useful when conducted over a
4.1 A specimen of known geometry is placed in mechanical
range of temperatures from −160°C to polymer degradation
oscillation either at fixed or natural resonant frequencies.
and is valid for frequencies from 0.01 to 1000 Hz.
Elastic or loss moduli, or both of the specimen are measured
1.4 This practice is intended for materials that have an
while varying time, temperature of the specimen or frequency,
elastic modulus in the range from 0.5 MPa to 100 GPa (73 psi
7 or both, of the oscillation. Plots of the elastic or loss moduli, or
to 1.5 3 10 psi).
both, are indicative of viscoelastic characteristics of the speci-
1.5 Apparent discrepancies may arise in results obtained
men. Rapid changes in viscoelastic properties at particular
under differing experimental conditions. Without changing the
temperatures, times, or frequency are normally referred to as
observed data, reporting in full (as described in this practice)
transition regions.
the conditions under which the data were obtained will enable
apparent differences observed in another study to be recon- NOTE 1—The particular method for measurement of elastic and loss
moduli depends upon the operating principle of the instrument used.
ciled.
1.6 Test data obtained by this practice is relevant and
5. Significance and Use
appropriate for use in engineering design.
5.1 Dynamic mechanical testing provides a method for
1.7 The values stated in SI units are to be regarded as the
determining elastic and loss moduli as a function of tempera-
standard. The values given in parentheses are for information
ture, frequency or time, or both. A plot of the elastic modulus
only.
and loss modulus of material versus temperature provides a
1.8 This standard does not purport to address all of the
graphical representation of elasticity and damping as a function
safety concerns, if any, associated with its use. It is the
of temperature or frequency.
responsibility of the user of this practice to establish appro-
5.2 This procedure can be used to locate transition tempera-
tures of plastics, that is, changes in the molecular motions of a
This practice is under the jurisdiction of ASTM Committee D-20 on Plastics polymer. In the temperature ranges where significant changes
and is the direct responsibility of Subcommittee D20.10 on Mechanical Properties.
Current edition approved Oct. 10, 1995. Published December 1995. Originally
published as D 4065 – 82. Last previous edition D 4065 – 94. Annual Book of ASTM Standards, Vol 08.01.
This edition includes revisions to Table 1 and the addition of 1.6. Annual Book of ASTM Standards, Vol 08.02.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 4065
occur, elastic modulus decreases rapidly with increasing tem- 7.2.4 Temperature Controller and Oven—A device for con-
perature (at constant or near constant frequency) or increases trolling the specimen temperature, either by heating (in steps or
with increasing frequency (at constant temperature). A maxi- ramps), cooling (in steps or ramps), or maintaining a constant
mum is observed for the loss modulus. specimen environment. Any temperature programmer should
5.3 This procedure can be used, for example, to evaluate by be sufficiently stable to permit measurement of sample tem-
comparison to known reference materials: perature to 60.5°C.
5.3.1 Degree of phase separation in multicomponent sys- 7.3 Nitrogen or other gas supply for purging purposes.
tems, 7.4 Calipers or other length-measuring device capable of
5.3.2 Filler type, amount, pretreatment, and dispersion, and measuring to an accuracy of 0.01 mm.
5.3.3 Effects of certain processing treatment.
8. Hazards
5.4 This procedure can be used to determine the following:
5.4.1 Stiffness of polymer composites, especially as a func-
8.1 Precautions:
tion of temperature,
8.1.1 Toxic or corrosive effluents, or both, may be released
5.4.2 Degree of polymer crystallinity, and
when heating the specimen near its decomposition point and
5.4.3 Magnitude of triaxial stress state in the rubber phase of
can be harmful to personnel or to the apparatus.
rubber modified polymers.
8.1.2 Take care to prevent buckling of the clamped speci-
5.4.4 This procedure is useful for quality control, specifica-
men due to thermal expansion during the test.
tion acceptance, and research.
5.5 For many materials, there may be a specification that
9. Test Specimens
requires the use of this practice, but with some procedural
9.1 Specimens may be any uniform size or shape but are
modifications that take precedence when adhering to the
ordinarily analyzed in rectangular form. If some heat treatment
specification. Therefore, it is advisable to refer to that material
is applied to the specimen to obtain this preferred analytical
specification before using this practice. Table 1 of Classifica-
form, this treatment should be noted in the report.
tion System D 4000 lists the ASTM materials standards that
9.2 Due to the numerous types of dynamic mechanical
currently exist.
instruments, specimen size is not fixed by this practice. In
many cases, a specimen of 0.75 by 9.4 by 50 mm (0.03 by 0.38
6. Interferences
by 2.0 in.) is found to be usable and convenient.
6.1 Since small quantities of specimen are used, it is
NOTE 2—It is important to select a specimen size consistent with the
essential that the specimens be homogeneous or representative,
modulus of the material under test and capabilities of the measuring
or both.
apparatus. For example, thick specimens of low modulus materials may be
suitable for measurement, while thin specimens of high modulus materials
7. Apparatus
may be required.
7.1 The function of the apparatus is to hold a plastic
9.3 Condition the specimen at 23 6 2°C (736 4°F) and 50
specimen of uniform cross section, so that the specimen acts as
6 5 % relative humidity for not less than 40 h prior to test in
the elastic and dissipative element in a mechanically oscillated
accordance to Procedure A of Practice D 618, for those tests
system. Instruments of this type are commonly called dynamic
where conditioning is required. If other specimen conditioning
mechanical or dynamic thermomechanical analyzers. They
is used, it should be noted in the report.
typically operate in one of seven oscillatory modes: (1) freely
decaying torsional oscillation, (2) forced constant amplitude,
10. Calibration
resonant, flexural oscillation, (3) forced constant amplitude,
10.1 Using the same heating rate or schedule to be used for
fixed frequency, compressive oscillation, (4) forced constant
specimens, calibrate the instrument temperature axis, using the
amplitude, fixed frequency, flexural oscillation, (5) forced,
instrument manufacturer’s procedures with either or both of the
constant amplitude, fixed frequency, tensile oscillation, (6)
following substances.
forced constant amplitude, fixed frequency, torsional oscilla-
Standard Transition Temperature, °C Type of Transition
tion and (7) forced constant amplitude, fixed frequency, or
Water 0.0 fusion
variable frequency dual cantilever.
Indium 156.6 fusion
7.2 The apparatus shall consist of the following:
10.2 Calibrate the instrument using procedures recom-
7.2.1 Clamps—A clamping arrangement that permits grip-
mended by the manufacturer.
ping of the sample.
7.2.2 Oscillatory Deformation (Strain)—A device for ap-
11. Procedure
plying an oscillatory deformation (strain) to the specimen. The
deformation (strain) may be applied and then released, as in 11.1 Measure the length, width, and thickness of the speci-
free-vibration devices, or continuously applied, as in forced- men to an accuracy of 61%.
vibration devices (see Table 1). 11.2 Maximum strain amplitude should be within the linear
7.2.3 Detectors—A device or devices for determining de- viscoelastic range of the material. Strains of less than 1 % are
pendent and independent experimental parameters, such as recommended.
force (stress or strain), frequency, and temperature. Tempera- 11.3 If temperature is to be the independent variable:
ture should be measureable with an accuracy of 61°C, 11.3.1 The test frequency may be from 0.01 to 500 Hz, fixed
frequency to 61 %, and force to 61%. or changing as the dependent variable.
D 4065
TABLE 1 Summary of Techniques and Calculations Used to Determine Dynamic Mechanical Properties
Calculations
Input Frequency Range, Specimen Size,
Technique Mode of Oscillation
Oscillating Elastic Damping
Excitation Hz mm
Strain Component Component
Dynamic Sinusoidal/ Forced constant amplitude- 0.001
...
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