ASTM D4065-20

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. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4065 − 12 D4065 − 20
Standard Practice for
Plastics: Dynamic Mechanical Properties: Determination and
Report of Procedures
This standard is issued under the fixed designation D4065; 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 (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. 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 plastic 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°Cfrom −140°C to polymer
degradationsoftening 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 × 10
psi).
1.5 Discrepancies in results are known to arise when 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. An assumption of this technique is that testing is conducted in the
region of linear viscoelastic behavior.
1.6 Different modes of deformation, such as tensile, bending and shear, are used, as listed in the referenced test methods.
1.7 Test data obtained by this practice are relevant and appropriate for use in engineering design.
1.8 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.9 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 practicestandard to establish appropriate safety safety, health, and healthenvironmental practices and determine
the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 8.
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.10 on Mechanical Properties.
Current edition approved Aug. 1, 2012Sept. 1, 2020. Published September 2012September 2020. Originally approved in 1982. Last previous edition approved in 20062012
as D4065 - 06.D4065 - 12. DOI: 10.1520/D4065-12.10.1520/D4065-20.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4065 − 20
NOTE 1—This practice is equivalent to ISO 6721–1.
1.10 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D618 Practice for Conditioning Plastics for Testing
D4000 Classification System for Specifying Plastic Materials
D4092 Terminology for Plastics: Dynamic Mechanical Properties
D4440 Test Method for Plastics: Dynamic Mechanical Properties Melt Rheology
D5023 Test Method for Plastics: Dynamic Mechanical Properties: In Flexure (Three-Point Bending)
D5024 Test Method for Plastics: Dynamic Mechanical Properties: In Compression
D5026 Test Method for Plastics: Dynamic Mechanical Properties: In Tension
D5279 Test Method for Plastics: Dynamic Mechanical Properties: In Torsion
D5418 Test Method for Plastics: Dynamic Mechanical Properties: In Flexure (Dual Cantilever Beam)
E1867 Test Methods for Temperature Calibration of Dynamic Mechanical Analyzers
E2254 Test Method for Storage Modulus Calibration of Dynamic Mechanical Analyzers
E2425 Test Method for Loss Modulus Conformance of Dynamic Mechanical Analyzers
E3142 Test Method for Thermal Lag of Thermal Analysis Apparatus
2.2 ISO Standard:
ISO 6721–1 Plastics— Determination of Dynamic Mechanical Properties, Part 1, General Principles
3. Terminology
3.1 Definitions—For definitions of terms relating to this practice, see Terminology D4092.
4. Summary of Practice
4.1 A specimen of known geometry is placed in mechanical oscillation either at fixed or natural resonant frequencies. Elastic or
loss moduli, or both of the specimen are measured while varying time, temperature of the specimen or frequency of the oscillation,
or both the latter. Plots of the elastic or loss moduli, or both, are indicative of viscoelastic characteristics of the specimen. Rapid
changes in viscoelastic properties at particular temperatures, times, or frequencies are normally referred to as transition regions.
NOTE 2—The particular method for measurement of elastic and loss moduli depends upon the operating principle of the instrument used.
4.2 D5023, D5024, D5026, D5279, and D5418 describe specific methods for determining dynamic mechanical properties.
5. Significance and Use
5.1 Dynamic mechanical testing provides a method for determining elastic and loss moduli as a function of temperature, frequency
or time, or both. A plot of the elastic modulus and loss modulus of material versus temperature provides a graphical representation
of elasticity and damping as a function of temperature or frequency.frequency, respectively.
5.2 This procedure can be used to locate transition temperatures of plastics, that is, changes in the molecular motions of a polymer.
In the temperature ranges where significant changes occur, elastic modulus decreases rapidly with increasing temperature (at
constant or near constant frequency) or increases with increasing frequency (at constant temperature). A maximum is observed for
the loss modulus, as well as for the tan delta curve, in the transition region.
5.3 This procedure can be used, for example, to evaluate by comparison to known reference materials or control materials:
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D4065 − 20
5.3.1 Degree of phase separation in multicomponent systems,
5.3.2 Filler type, amount, pretreatment, and dispersion, and
5.3.3 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 function of temperature,
5.4.2 Degree of polymer crystallinity, and
5.4.3 Magnitude of triaxial stress state in the rubber phase of rubber modified polymers.
5.5 This procedure is useful for quality control, specification acceptance, and research.
5.6 Procedural modifications in material specifications take precedence to this practice. Therefore, consult the appropriate material
specification before using this practice. Table 1 of Classification System D4000 lists the ASTM materials standards that currently
exist.
6. Interferences
6.1 Since small quantities of specimen are used, it is essential that the specimens be homogeneous or representative, or both.
7. Apparatus
7.1 The function of the apparatus is to hold a plastic specimen of uniform cross section, so that the specimen acts as the elastic
and dissipative element in a mechanically oscillated system. Instruments of this type are commonly called dynamic mechanical
or dynamic thermomechanical analyzers. They typically operate in one of seven oscillatory modes: (1) freely decaying torsional
oscillation, (2) forced constant amplitude, resonant, flexural oscillation, (3) forced constant amplitude, fixed frequency,
compressive oscillation, (4) forced constant amplitude, fixed frequency, flexural oscillation, (5) forced, constant amplitude, fixed
frequency, tensile oscillation, (6) forced constant amplitude, fixed frequency, torsional oscillation and (7) forced constant
amplitude, fixed frequency, or variable frequency dual cantilever.
7.2 The apparatus shall consist of the following:
7.2.1 Clamps—A clamping arrangement that permits gripping of the sample.
7.2.2 Oscillatory Deformation (Strain)—A device for applying an oscillatory deformation (strain) to the specimen. The
deformation (strain) shall be applied and then released, as in free-vibration devices, or continuously applied, as in forced-vibration
devices (see devices.Table 1).
7.2.3 Detectors—A device or devices for determining dependent and independent experimental parameters, such as force (stress
or strain), frequency, and temperature. Temperature shall be measurable with an accuracy of 61°C, readable to 61 °C, frequency
to 61 %, and force to 61 %.
7.2.4 Temperature Controller and Oven—A device for controlling the specimen temperature, either by heating (in steps or ramps),
cooling (in steps or ramps), or maintaining a constant specimen environment. Any temperature programmer should be sufficiently
stable to permit measurement of sample temperature to 60.5°C.60.5 °C.
7.3 Nitrogen or other gas supply for purging purposes.
7.4 Calipers or other length-measuring device capable of measuring to an accuracy of 60.01 mm.
D4065 − 20
8. Hazards
8.1 Precautions:
8.1.1 Certain materials, when heated near their decomposition point, can release potentially toxic, or corrosive effluents, or both
that can be harmful to personnel or to the apparatus.
8.1.2 Buckling of the clamped specimen due to thermal expansion during the test.
9. Test Specimens
9.1 Specimens are of any uniform size or shape but are ordinarily analyzed in rectangular form. If some heat treatment is applied
to the specimen to obtain this preferred analytical form, this treatment shall be noted in the report.
9.2 Due to the numerous types of dynamic mechanical 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 by 2.0 in.) is found to be usable and convenient.The selection of sample size
depends on material modulus, and DMA geometry used. A general recommendation is that length divided by thickness is greater
than or equal to 10.
NOTE 3—It is important to select a specimen size consistent with the modulus of the material under test and capabilities of the measuring apparatus. For
example, while thick specimens of low modulus materials are suitable for measurement, thin specimens of high modulus materials are required.Instrument
manufacturers often provide sample size recommendations based on material modulus.
9.3 Unless otherwise specified in the appropriate material specification, condition the specimen at a set temperature of 23°C
(73°F)23 °C (73 °F) that is maintained 62°C (64°F)62 °C (64 °F) and at a set relative humidity of 50 % that is maintained 610
% 610 % for not less than 40 h prior to test in accordance to Procedure A of Practice D618, for those tests where conditioning
is required. If other specimen conditioning is used, it should be noted in the report.
10. Calibration
10.1 Using the same heating rate or schedule to be used for specimens, calibrate the instrument temperature axis, using the
instrument manufacturer’s procedures with either or both of the following substances. Refer to and recommended materials (refer
to standards E1867, E2254, and E2425 for additional details on calibration.).
Standard Transition Temperature, °C Type of Transition
Water 0.0 fusion
Indium 156.6 fusion
11. Procedure
11.1 Measure the length, width, and thickness of the specimen to an accuracy of 61 %.
11.2 Maximum strain amplitude shall be within the linear viscoelastic range of the material. Strains of less than 1 % are
recommended.
11.3 If temperature is to be the independent variable:
11.3.1 The test frequency shall be from 0.010.01 Hz to 500 Hz, 500 Hz, fixed or changing as the dependent variable.
TABLE 1 Summary of Techniques and Calculations Used to Determine Dynamic Mechanical Properties
Calculations
Frequency Range, Specimen Size,
Technique Input Excitation Mode of Oscillation
Oscillating Elastic Damping
Hz mm
Strain Component Component
Dynamic Sinusoidal/ Forced constant amplitude- 0.001 to 60 Hz t = 0.01–1.6 ± 3tA (2 D + Tan δ = JV/f
mechanical fixed or fixed or resonance frequency b = 0.02–13 L)/L R
analyzer resonance flexural oscillation L = 18, 25, or 33
frequency Rectangular:
D4065 − 20
TABLE 1 Continued
Calculations
Frequency Range, Specimen Size,
Technique Input Excitation Mode of Oscillation
Oscillating Elastic Damping
Hz mm
Strain Component Component
E'
2 2
4π f I2H
5 L/t
f g
2b L/21D
s d
Circular:
2 2 4
E' = 4π f I-H/3r
2 3
(2D + L) [2L ]
Visco- Sinusoidal Forced constant amplitude- 3.5, 11, 35, L = 7 cm ΔL/L Rectangular cross E9 = NL/ tbΔL·sin δ
A
elastometer fixed fixed frequency- 110 T = 0.05 cm section: Tan δ directly read
frequency tensile oscillation B = 0.4 cm E' = NL:/ btΔ L
(see Fig. 4) cos δ
Circular cross
section:
2 2
ΔL/L E' = NL cosδ/π r E9 = NL sinδ/π r
ΔL ΔL
Tan δ directly read
Mechanical Sinusoidal Forced constant amplitude; 0.0016 to 80 t = 0.025–1.0 ΔL/L Rectangular cross
B,C
spectrometer fixed or fixed or variable b = 12.7 section:
variable frequency-tensile L = 63.5 E' = NL cos δ/bt E9 = NL sinδ/
frequency oscillation (see Fig. 5) Δ/ L tbΔ L
Circular cross Tan δ directly read
section:
2 2
r = 1.6, 2.35, ΔL/L E' = NL cosδ/π r E9 = NL sinδ/π r
3.15 Δ/L Δ/L
L = 63.5 Tan δ directly read
Mechanical Sinusoidal Forced constant amplitude; 0.0016–80 Up to 38 × 38: ΔL/L Rectangular cross E9 = NL sinδ/
B,C
spectrometer fixed or fixed or variable t = 38 section: tbΔ L
variable frequency-compressive b = 38 E' = NL cosδ/tb Tan δ directly read
frequency oscillation (see Fig. 6) L = 1–10 ΔL
r = 8–50 Circular cross E9 = NL sinδ/
t = 1–10 section: πr Δ L
E' = NL cosδ/π r Tan δ directly read
ΔL
Mechanical Sinusoidal Forced constant amplitude; 0.0016–80 t = 0.5–6.4 3 ta/L Rectangular cross
B,C
spectrometer fixed or fixed or variable b = 12.7 section:
variable frequency-flexural L = 63.5
frequency oscillation (see Fig. 7)
3 3
E' NL cos δ/ E9 = NL sinδ/
3 3
2 bt a 2bt a
Tan δ directly read
2 3
r = 0.25–3.2 3 ra/L Circular cross E9 = 4NL sinδ/
L = 63.5 section: 3 r a
E' = 4NL Tan δ directly read
cos δ/3r a
D4065 − 20
TABLE 1 Continued
Calculations
Frequency Range, Specimen Size,
Technique Input Excitation Mode of Oscillation
Oscillating Elastic Damping
Hz mm
Strain Component Component
Dynamic Sinusoidal Constant force 0.01–50 t = up to 2.0 ΔL/L Rectangular cross
Mechanical fixed or amplitude; b = up to 10 section:
B,D
Analyzer variable fixed or variable L = up to 24 E' = NL cosδ/ bt E9 = NL sin δ/
frequency frequency-tensil
...