Astm d4065 PDF
Astm d4065 PDF
Astm d4065 PDF
This standard has been approved for use by agencies of the Department of Defense.
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This practice is under the jurisdiction of ASTM Committee D20 on Plastics and Annual Book of ASTM Standards, Vol 08.01.
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is the direct responsibility of Subcommittee D20.10 on Mechanical Properties. Annual Book of ASTM Standards, Vol 08.02.
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Current edition approved September 10, 2001. Published November 2001. Available from American National Standards Institute, 25 W. 43rd St., New
Originally published as D 4065 – 82. Last previous edition D 4065 – 95. York, NY 10036.
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D 4065 – 01
5. Significance and Use 7.2.2 Oscillatory Deformation (Strain)—A device for ap-
5.1 Dynamic mechanical testing provides a method for plying an oscillatory deformation (strain) to the specimen. The
determining elastic and loss moduli as a function of tempera- deformation (strain) may be applied and then released, as in
ture, frequency or time, or both. A plot of the elastic modulus free-vibration devices, or continuously applied, as in forced-
and loss modulus of material versus temperature provides a vibration devices (see Table 1).
graphical representation of elasticity and damping as a function 7.2.3 Detectors—A device or devices for determining de-
of temperature or frequency. pendent and independent experimental parameters, such as
5.2 This procedure can be used to locate transition tempera- force (stress or strain), frequency, and temperature. Tempera-
tures of plastics, that is, changes in the molecular motions of a ture should be measureable with an accuracy of 61°C,
polymer. In the temperature ranges where significant changes frequency to 61 %, and force to 61 %.
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.
5.4 This procedure can be used to determine the following: 8. Hazards
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
6. Interferences 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.
6.1 Since small quantities of specimen are used, it is
essential that the specimens be homogeneous or representative, NOTE 3—It is important to select a specimen size consistent with the
or both. modulus of the material under test and capabilities of the measuring
apparatus. For example, thick specimens of low modulus materials may be
7. Apparatus suitable for measurement, while thin specimens of high modulus materials
may be required.
7.1 The function of the apparatus is to hold a plastic
specimen of uniform cross section, so that the specimen acts as 9.3 Condition the specimen at 23 6 2°C (736 4°F) and 50
the elastic and dissipative element in a mechanically oscillated 6 5 % relative humidity for not less than 40 h prior to test in
system. Instruments of this type are commonly called dynamic accordance to Procedure A of Practice D 618, for those tests
mechanical or dynamic thermomechanical analyzers. They where conditioning is required. If other specimen conditioning
typically operate in one of seven oscillatory modes: (1) freely is used, it should be noted in the report.
decaying torsional oscillation, (2) forced constant amplitude,
resonant, flexural oscillation, (3) forced constant amplitude, 10. Calibration
fixed frequency, compressive oscillation, (4) forced constant 10.1 Using the same heating rate or schedule to be used for
amplitude, fixed frequency, flexural oscillation, (5) forced, specimens, calibrate the instrument temperature axis, using the
constant amplitude, fixed frequency, tensile oscillation, (6) instrument manufacturer’s procedures with either or both of the
forced constant amplitude, fixed frequency, torsional oscilla- following substances.
tion and (7) forced constant amplitude, fixed frequency, or Standard Transition Temperature, °C Type of Transition
variable frequency dual cantilever. Water 0.0 fusion
Indium 156.6 fusion
7.2 The apparatus shall consist of the following:
7.2.1 Clamps—A clamping arrangement that permits grip- 10.2 Calibrate the instrument using procedures recom-
ping of the sample. mended by the manufacturer.
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D 4065 – 01
11. Procedure 11.3 If temperature is to be the independent variable:
11.1 Measure the length, width, and thickness of the speci- 11.3.1 The test frequency may be from 0.01 to 500 Hz, fixed
men to an accuracy of 61 %. or changing as the dependent variable.
11.2 Maximum strain amplitude should be within the linear
viscoelastic range of the material. Strains of less than 1 % are
recommended.
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 to 60 Hz t = 0.01–1.6 6 3tA (2D + Rectangular: Tan d = JV/f2
mechanical fixed or fixed or resonance fre- b = 0.02–13 L)/L2R E8 5
analyzer resonance quency flexural oscillation L = 18, 25, or 33 4p2 f 2 I2H
frequency [L/t#3
2b~L/2 1 D!2
Circular:
E8 = 4p2f2I-H/3r4
(2D + L)2 [2L3]
Visco- Sinusoidal Forced constant amplitude- 3.5, 11, 35, L = 7 cm DL/L Rectangular cross E9 = NL/tbDL·sin d
elastometerA fixed fixed frequency- 110 T = 0.05 cm section: Tan d directly read
frequency tensile oscillation B = 0.4 cm E8 = NL:/btD L
(see Fig. 4) cos d
Circular cross
section:
DL / L E8 = NL cosd/p r2 E9 = NL sind/p r2
DL DL
Tan d directly read
Mechanical Sinusoidal Forced constant amplitude; 0.0016 to 80 t = 0.025–1.0 DL/L Rectangular cross
spectrometerB,C fixed or fixed or variable b = 12.7 section:
variable frequency-tensile L = 63.5 E8 = NL cos d/bt E9 = NL sind/
frequency oscillation (see Fig. 5) D/L tbDL
Circular cross Tan d directly read
section:
r = 1.6, 2.35, DL/L E8 = NL cosd/p r2 E9 = NL sind/p r2
3.15 D/L D/L
L = 63.5 Tan d directly read
Mechanical Sinusoidal Forced constant amplitude; 0.0016–80 Up to 38 3 38: DL/L Rectangular cross E9 = NL sind/
fixed or fixed or variable t = 38 section: tbDL
spectrometerB,C variable frequency-compressive b = 38 E8 = NL cos d/tb Tan d directly read
frequency oscillation (see Fig. 6) L = 1–10 DL
r = 8–50 Circular cross E9 = NL cos d/
t = 1–10 section: pr2D L
E8 = NL cosd/p r2 Tan d directly read
DL
Mechanical Sinusoidal Forced constant amplitude; 0.0016–80 t = 0.5–6.4 3 ta/L2 Rectangular cross
spectrometerB,C fixed or fixed or variable b = 12.7 section:
variable frequency-flexural L = 63.5
frequency oscillation (see Fig. 7)
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D 4065 – 01
TABLE 1 Continued
Calculations
Input Frequency Range, Specimen Size,
Technique Mode of Oscillation Oscillating Elastic Damping
Excitation Hz mm
Strain Component Component
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D 4065 – 01
TABLE 1 Continued
Calculations
Input Frequency Range, Specimen Size,
Technique Mode of Oscillation Oscillating Elastic Damping
Excitation Hz mm
Strain Component Component
F t
K 5 bt 3 16/3 2 3.36 b ~1 2 t4/12b4! G
Mechanical Sinusoidal Forced constant amplitude .01–200 L = 1–46 3 ta/L2 S810 D Tan d directly read
spectrometerB,C fixed fixed frequency flexural t = .1–5 E8 5
2b~t/L!3
frequency oscillation (single or dual b = .1–18
cantilever)
Mechanical Sinusoidal Forced constant amplitude .01–200 t = .1–3 a/t S810 D t Tan d directly read
spectrometerB,C fixed fixed frequency shear G8 5 2A
frequency oscillation
Mechanical Sinusoidal Forced constant amplitude .01–100 t = .005–1 a/L S810DL Tan d directly read
spectrometerB,C fixed fixed frequency tensile b = .01–18 E8 5 wt
frequency oscillation L = 1–20
Mechanical Sinusoidal, Forced constant amplitude 0.00016–16.0 t = up to 1.59 12 tA/L E8 = (NL3/Bt3A)cosd E9 = (NL3/Bt3A)sind
spectrometerB,C fixed fixed or variable frequency in b = up to 6.4
or variable dual cantilever geometry L = up to 44.5
frequency
A
Instruments of this type are available from IMASS, Inc., Box 134, Accord, MA 02018.
B
Instruments of this type are available from TA Instruments, 109 Lukens Drive, New Castle, DE 19720.
C
Instruments of this type are available from Rheometric-Scientific, Inc., One Possumtown Road, Piscataway, NJ 08854.
D
Instruments of this type are available from The Perkin-Elmer Corp., 761 Main Avenue, Norwalk, CT 06859-0256.
Symbols:
I = moment of inertia of the inertial member D = clamping distance
f = frequency of oscillation H = instrument constant
L = specimen length between clamp J = instrument constant
b = specimen width V = instrument provided dependent variable
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D 4065 – 01
t = specimen thickness A = oscillation amplitude
r = specimen radius u = angular displacement
k = constant
a = parallel axes displacement
G8 = elastic modulus in shear
D = logarithmic decrement T = torque,
G9 = loss modulus in shear RR = relative rigidity
DL = change in length n = number of cycles for oscillation to decay a specific amount
E8 = elastic modulus P = period of oscillation
E9 = loss modulus d = phase angle
N = axial force
Z = elapsed time
R = instrument arm length
11.3.2 Vary the temperature of the test specimen from the 13.1.2 Description of the instrument used for test.
lowest to the highest temperature of interest while measuring 13.1.3 Dimensions of the test specimen.
its elastic and viscous properties. 13.1.4 Description of the calibration procedure.
NOTE 4—Preferably, tests conducted over a temperature range should 13.1.5 Identification of the sample atmosphere by gas com-
be performed in incremental steps or at a rate slow enough to allow position, purity, and rate used.
temperature equilibrium throughout the entire specimen. The time to reach 13.1.6 Details of conditioning the specimen prior to test.
equilibrium will depend upon the mass of the particular specimen and the 13.1.7 The temperature program including initial and final
gripping arrangement. Temperature program rates of 1 to 2°C/min or 2 to temperatures as well as rate of linear temperature change or
5°C step intervals held for 3 to 5 min have been found suitable. The effect
of heating rate may be observed by running specimens at two or more
size and duration of temperature steps.
rates and comparing the elastic and viscous property results obtained. 13.1.8 Table of data and results.
NOTE 5—The accuracy required of the temperature measurement will 13.1.9 Number of specimens tested.
depend upon the rate of change of moduli with temperature of the plastic 13.1.10 A plot of the elastic moduli and loss moduli versus
being investigated. In transition regions, experience has indicated that the temperature (or frequency) where tests are conducted at more
specimen temperature should be read to 60.5°C.
than one temperature (or frequency).
11.3.3 Duplicate specimens should be examined, and the 13.1.10.1 Moduli should be plotted on the ordinate with
mean results reported. upward deflections as increase in elasticity and damping. The
11.4 If frequency is to be the independent variable: ordinate should be clearly labeled with title and units of
11.4.1 The test temperature should be fixed at the desired measurement.
value. 13.1.10.2 Temperature, frequency, or time should be plotted
11.4.2 Vary the frequency applied to the test specimen while on the abscissa, increasing from left to right. The abscissa
measuring its elastic and viscous properties. should be clearly labeled with title and units of measurement.
11.4.3 Duplicate specimens should be examined and the 13.1.10.3 Transition temperatures are taken from the peak
mean results reported. values in the loss modulus profile.
12. Calculation 13.1.10.4 Wherever possible, each thermal effect should be
identified and supplementary supporting evidence reported.
12.1 Calculate the dynamic mechanical properties using the 13.1.11 Average values and standard deviations of elastic
equations given in Table 1 or in the manufacturer’s operating (or relative rigidity) and loss modulus (or damping) reported to
manual. two significant figures.
12.1.1 Use the average measured values of specimen length,
13.1.12 Date of test.
width, and thickness.
13.1.13 Maximum strain amplitude and frequency.
13. Report 13.1.14 Equations used to calculate values.
13.1 Report the following information:
13.1.1 Complete identification and description of the mate- 14. Keywords
rial tested including name, stock or code number, date made, 14.1 dynamic mechanical; modulus; rheological; tan delta;
form, source, etc. viscoelastic
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D 4065 – 01
SUMMARY OF CHANGES
This section identifies the location of selected changes to this practice. For the convenience of the user,
Committee D20 has highlighted those changes that may impact the use of this practice. This section may also
include descriptions of the changes or reasons for the changes, or both.
D 4065 – 01: (3) Footnote C in Table 1 has been changed. Company name
(1) Title has been changed. change.
(2) ISO statement has been added. (4) Summary of Changes section added.
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