ASTM D4473-08(2016)
(Test Method)Standard Test Method for Plastics: Dynamic Mechanical Properties: Cure Behavior
Standard Test Method for Plastics: Dynamic Mechanical Properties: Cure Behavior
SIGNIFICANCE AND USE
5.1 This test method provides a simple means of characterizing the cure behavior of thermosetting resins using very small amounts of material (fewer than 3 to 5 g). The data obtained may be used for quality control, research and development, and establishment of optimum processing conditions.
5.2 Dynamic mechanical testing provides a sensitive method for determining cure characteristics by measuring the elastic and loss moduli as a function of temperature or time, or both. Plots of cure behavior and tan delta of a material versus time provide graphical representation indicative of cure behavior under a specified time-temperature profile.
5.3 This test method can be used to assess the following:
5.3.1 Cure behavior, including rate of cure, gel, and cure time.
5.3.2 Processing behavior, as well as changes as a function of time/temperature.
Note 3: The presence of the substrate prevents an absolute measure, but allows relative measures of flow behavior during cure.
5.3.3 The effects of processing treatment.
5.3.4 Relative resin behavioral properties, including cure behavior and damping.
5.3.5 The effects of substrate types on cure.
Note 4: Due to the rigidity of a supporting braid, the gel time obtained from dynamic mechanical traces will be longer than actual gel time of the unsupported resin measured at the same frequency. This difference will be greater for composites having greater support-to-polymer rigidity ratios.3
5.3.6 Effects of formulation additives that might affect processability or performance.
5.4 For many materials, there may be a specification that requires the use of this test method, but with some procedural modifications that take precedence when adhering to the specification. Therefore, it is advisable to refer to that material specification before using this test method. Table 1 of Classification System D4000 lists the ASTM materials standards that currently exist.
SCOPE
1.1 This test method covers the use of dynamic-mechanical-oscillation instrumentation for gathering and reporting the thermal advancement of cure behavior of thermosetting resin. It may be used for determining the cure properties of both unsupported resins and resins supported on substrates subjected to various oscillatory deformations.
1.2 This test method is intended to provide a means for determining the cure behavior of supported and unsupported thermosetting resins over a range of temperatures by free vibration as well as resonant and nonresonant forced-vibration techniques, in accordance with Practice D4065. Plots of modulus, tan delta, and damping index as a function of time/temperature are indicative of the thermal advancement or cure characteristics of a resin.
1.3 This test method is valid for a wide range of frequencies, typically from 0.01 to 100 Hz. However, it is strongly recommended that low-frequency test conditions, generally below 1.5 Hz, be utilized as they generally will result in more definitive cure-behavior information.
1.4 This test method is intended for resin/substrate composites that have an uncured effective elastic modulus in shear greater than 0.5 MPa.
1.5 Apparent discrepancies may arise in results obtained under differing experimental conditions. These apparent differences from results observed in another study can usually be reconciled, without changing the observed data, by reporting in full (as described in this test method) the conditions under which the data were obtained.
1.6 Due to possible instrumentation compliance, especially in the compressive mode, the data generated may indicate relative and not necessarily absolute property values.
1.7 Test data obtained by this test method are relevant and appropriate for use in engineering design.
1.8 The values stated in SI units are to be regarded as the standard.
1.9 This standard does not purport to address all of the safety concerns, if any, associated with its use....
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Designation:D4473 −08 (Reapproved 2016)
Standard Test Method for
Plastics: Dynamic Mechanical Properties: Cure Behavior
This standard is issued under the fixed designation D4473; 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 1.8 The values stated in SI units are to be regarded as the
standard.
1.1 This test method covers the use of dynamic-mechanical-
1.9 This standard does not purport to address all of the
oscillation instrumentation for gathering and reporting the
safety concerns, if any, associated with its use. It is the
thermal advancement of cure behavior of thermosetting resin.
responsibility of the user of this standard to establish appro-
It may be used for determining the cure properties of both
priate safety and health practices and determine the applica-
unsupported resins and resins supported on substrates sub-
bility of regulatory limitations prior to use. Specific precau-
jected to various oscillatory deformations.
tionary statements are given in Note 5.
1.2 This test method is intended to provide a means for
determining the cure behavior of supported and unsupported NOTE 1—There is no known ISO equivalent to this standard.
thermosetting resins over a range of temperatures by free
2. Referenced Documents
vibration as well as resonant and nonresonant forced-vibration
techniques, in accordance with Practice D4065. Plots of
2.1 ASTM Standards:
modulus, tan delta, and damping index as a function of D4000 Classification System for Specifying Plastic Materi-
time/temperature are indicative of the thermal advancement or
als
cure characteristics of a resin. D4065 Practice for Plastics: Dynamic Mechanical Proper-
ties: Determination and Report of Procedures
1.3 Thistestmethodisvalidforawiderangeoffrequencies,
D4092 Terminology for Plastics: Dynamic Mechanical
typically from 0.01 to 100 Hz. However, it is strongly
Properties
recommended that low-frequency test conditions, generally
ASTM/IEEE SI–10 Standard for Use of the International
below 1.5 Hz, be utilized as they generally will result in more
System of Units (SI): The Modern Metric System
definitive cure-behavior information.
1.4 This test method is intended for resin/substrate compos-
3. Terminology
ites that have an uncured effective elastic modulus in shear
3.1 Definitions—For definitions applicable to this test
greater than 0.5 MPa.
method refer to Terminology D4092.
1.5 Apparent discrepancies may arise in results obtained
4. Summary of Test Method
under differing experimental conditions. These apparent differ-
ences from results observed in another study can usually be
4.1 A known amount of thermosetting liquid resin or resin-
reconciled, without changing the observed data, by reporting in
impregnated substrate is placed in mechanical oscillation at
full (as described in this test method) the conditions under
either a fixed or natural resonant frequency or by free vibration
which the data were obtained.
and at either isothermal conditions, with a linear temperature
increase or using a time-temperature relation simulating a
1.6 Due to possible instrumentation compliance, especially
processing condition. The elastic or loss modulus, or both, of
in the compressive mode, the data generated may indicate
the composite specimen are measured in shear or compression
relative and not necessarily absolute property values.
as a function of time. The point in time when tan delta is
1.7 Test data obtained by this test method are relevant and
maximum, and the elastic modulus levels off after an increase,
appropriate for use in engineering design.
is calculated as the gel time of the resin under the conditions of
the test.
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.10 on Mechanical Properties. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Nov. 1, 2016. Published November 2016. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1985. Last previous edition approved in 2008 as D4473 - 08. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D4473-08R16. the ASTM website.
*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
D4473−08 (2016)
NOTE 2—The particular method for measuring the elastic and loss
moduli and tan delta depends upon the individual instrument’s operating
principles.
5. Significance and Use
5.1 This test method provides a simple means of character-
izingthecurebehaviorofthermosettingresinsusingverysmall
amounts of material (fewer than 3 to 5 g). The data obtained
maybeusedforqualitycontrol,researchanddevelopment,and
establishment of optimum processing conditions.
5.2 Dynamic mechanical testing provides a sensitive
method for determining cure characteristics by measuring the
elastic and loss moduli as a function of temperature or time, or
both. Plots of cure behavior and tan delta of a material versus
time provide graphical representation indicative of cure behav-
ior under a specified time-temperature profile.
5.3 This test method can be used to assess the following:
5.3.1 Cure behavior, including rate of cure, gel, and cure
time.
5.3.2 Processing behavior, as well as changes as a function
of time/temperature.
FIG. 1 Typical Temperature Profile
NOTE 3—The presence of the substrate prevents an absolute measure,
but allows relative measures of flow behavior during cure.
5.3.3 The effects of processing treatment.
drivenoscillatoryshearordynamiccompressionsystem.These
5.3.4 Relative resin behavioral properties, including cure
dynamic mechanical instruments operate in one or more of the
behavior and damping.
followingmodesformeasuringcurebehaviorintorsionalshear
5.3.5 The effects of substrate types on cure.
or dynamic compression:
NOTE 4—Due to the rigidity of a supporting braid, the gel time obtained
7.1.1 Forced, constant amplitude, fixed frequency,
from dynamic mechanical traces will be longer than actual gel time of the
7.1.2 Forced, constant amplitude, resonant oscillation,
unsupported resin measured at the same frequency. This difference will be
3 7.1.3 Freely decaying oscillation.
greater for composites having greater support-to-polymer rigidity ratios.
7.2 The apparatus shall consist of the following:
5.3.6 Effects of formulation additives that might affect
7.2.1 Test Fixtures, a choice of the following:
processability or performance.
7.2.1.1 Polished Cone and Plate (Having a Known Cone
5.4 For many materials, there may be a specification that
Angle)—Usually a 25 or 50-mm diameter cone and plate or
requires the use of this test method, but with some procedural
parallel plates are recommended for neat resins. Variations of
modifications that take precedence when adhering to the
this tooling, such as bottom plates with concentric overflow
specification. Therefore, it is advisable to refer to that material
rims, may be used as necessary.
specification before using this test method. Table 1 of Classi-
7.2.1.2 Parallel Plates, having either smooth, polished, or
fication System D4000 lists theASTM materials standards that
serrated surfaces are recommended for neat resins or prepregs
currently exist.
having less than 6 % volatiles.
7.2.1.3 Clamps—Aclamping arrangement that permits grip-
6. Interferences
ping of the composite sample.
6.1 Since small quantities of resin are used, it is essential
7.2.2 Oscillatory Deformation (Strain Device)—A device
that the specimens be representative of the polymeric material
for applying a continuous oscillatory deformation (strain) to
being tested.
the specimen. The deformation (strain) may be applied and
then released, as in free-vibration devices, or continuously
6.2 The result is a response of the thermal advancement or
applied, as in forced-vibration devices (see Table 1 of Practice
cure behavior of the resin in combination with any substrate
D4065).
used to support the resin.
7.2.3 Detectors—A device or devices for determining de-
7. Apparatus
pendent and independent experimental parameters, such as
force (stress or strain), frequency, and temperature. Tempera-
7.1 The function of the apparatus is to hold a neat (unmodi-
ture should be measurable with a precision of 61°C, frequency
fied) resin or uncured supported composite formulation or
to 61 %, and force to 61%.
coated substrate of known volume and dimensions. The mate-
7.2.4 Temperature Controller and Oven—A device for con-
rialactsastheelasticanddissipativeelementinamechanically
trolling the temperature, either by heating (in steps or ramps),
cooling (in steps or ramps), maintaining a constant specimen
Hedvat, S., Polymer Engineering and Science, Vol 21, No. 3, February 1981. environment,oracombinationthereof.Fig.1illustratestypical
D4473−08 (2016)
time-temperature profiles. A temperature controller should be materials are being evaluated using cone and plate test fixtures,
sufficiently stable to permit measurement of sample tempera- the recommended minimum gap setting is equipment-
ture to within 1°C. dependent and reference should be made to the manufacturer’s
operational manual for correct gap setting.
7.3 Nitrogen, or other inert gas supply for purging purposes.
10.3.3.2 Cone and plate experiments should be run only at
8. Test Specimens one temperature. Any changes in the temperature setting will
require adjusting the gap setting to the manufacturer’s recom-
8.1 The neat resin or the self-supporting composition, or
mended value.
both, should be representative of the polymeric material being
10.3.4 Conduct cure characterization of the submitted ma-
tested.
terial in accordance with the desired time and temperature
8.2 Due to the various geometries that might be used for
parameters recording the appropriate property values.
dynamic mechanical curing of thermosetting resins/
composites, specimen size is not fixed by this test method. 10.4 Procedure B—Supported Compositions:
Cure rates may be influenced by specimen thickness, so equal
10.4.1 For self-supporting compositions in prepreg-type
volumes of material should be used for any series of compari-
form using cone and plate or parallel plate fixturing, be certain
sons.
that there is sufficient material to fill the sample volume on the
lower plate completely.
8.3 For convenience, low-viscosity neat resins can be stud-
ied using a supporting substrate. 10.4.2 Insert the substrate between the plates of the test
instrument. A sample disk (usually 25 mm in diameter) of the
8.4 The substrate on which the resin is supported is nor-
self-supporting composition can be die-cut, or several plies of
mally in the form of a woven-glass cloth or tape or a
prepreg can be compressed into a sheet (for example, for 3 min
braided-glass cord. The substrate should have negligible stiff-
at 77°C at 75 atmospheres, 1000 psi) and then a disk die-cut.
ness when compared to the cured resin sample in both a
The orientation of unidirectional reinforcements may affect
flexural and torsional mode of deformation. Other substrates
cure behavior and the orientation should be reported in 12.1.4.
can be used if their effect on cure mechanisms were of interest.
10.4.3 For three to five plies, the recommended gap setting
The composition should be representative of the polymeric
is 1 to 2 mm.This gap setting is arbitrary and dependent on the
material being tested.
type of material and the number of plies being characterized.A
8.4.1 To standardize the pH of the supporting substrates,
gap setting of 0.5 mm would be minimum. Cone and plate test
soak the cloth or braid overnight in distilled water and
fixtures are not recommended for supported compositions.
vacuum-dry. This will avoid any extraneous results with resins
that are pH-sensitive. 10.4.4 For self-supporting substrates where either a bare
substrate is to be impregnated with liquid resin (rectangular or
9. Calibration
cylindrical form) or where a similar prepreg-type specimen
forms a rectangular specimen, clamp the substrate in place
9.1 Calibratetheinstrumentusingproceduresrecommended
utilizing the instrument’s grip system.
by the manufacturer for that specific make and model.
10.4.5 Conduct the cure characterization of the submitted
10. Procedure
material in accordance with the desired time and temperature
NOTE 5—Precaution: Toxic or corrosive effluents, or both, may be
parameters recording the appropriate property values.
released when heating the resin specimen to its cured state and could be
harmful to personnel or to the instrumentation.
10.5 Procedure C—Dynamic Compression:
10.1 Apply the resin or uncured, self-supporting composite
10.5.1 Prepare the test specimen in accordance with the
onto the test fixture. In the case of two-part room-temperature
procedure described in 10.4.2 and 10.4.3.
cureresins,mixingshouldbecarriedoutinlessthan1 %ofthe
10.5.2 Compress slightly the specimen disk and monitor
expected gel time.
and record the preload force by observing the normal force
10.2 Out-time effects and moisture-effect data must be gage or indicator.Adjust the gap as necessary to accommodate
recorded and reported. any material expansion or contraction during the thermal
advancement.
10.3 Procedure A—Unsupported Resin:
10.5.3 Conduct the cure characterization of the submitted
10.3.1 Allow the sample to equilibrate to room temperature
material in accordance with the desired time and temperature
in a desiccator. In case of a solid sample, place it in an oven at
parameters recording the appropriate property values.
100°C for 5 to 10 min in order to soften. Use a vacuum oven
to degas, if necessary. Use 50-mm diameter test plates for low
10.6 Remove excess material by flushing or trimming the
minimum-viscosity systems and 25-mm diameter plates for
testfixtures,usingarazorblade,spatula,knife,orhotsoldering
higher minimum-viscosity materials.
gun.
10.3.2 For neat resins, be certain that there is sufficient
10.7 Isothermal Curing at Elevated Temperature:
material to cover the bottom plate uniformly.
10.3.3 Lower the upper test fixture so that it is touching the 10.7.1 In cases where the specimen can be introduced
material to be cured. directly into the test chamber at elevated temperatures, preheat
10.3.3.1 Thedistancebetweenthetwoparallelplatesshou
...
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: D4473 − 08 D4473 − 08 (Reapproved 2016)
Standard Test Method for
Plastics: Dynamic Mechanical Properties: Cure Behavior
This standard is issued under the fixed designation D4473; 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*Scope
1.1 This test method covers the use of dynamic-mechanical-oscillation instrumentation for gathering and reporting the thermal
advancement of cure behavior of thermosetting resin. It may be used for determining the cure properties of both unsupported resins
and resins supported on substrates subjected to various oscillatory deformations.
1.2 This test method is intended to provide a means for determining the cure behavior of supported and unsupported
thermosetting resins over a range of temperatures by free vibration as well as resonant and nonresonant forced-vibration
techniques, in accordance with Practice D4065. Plots of modulus, tan delta, and damping index as a function of time/temperature
are indicative of the thermal advancement or cure characteristics of a resin.
1.3 This test method is valid for a wide range of frequencies, typically from 0.01 to 100 Hz. However, it is strongly
recommended that low-frequency test conditions, generally below 1.5 Hz, be utilized as they generally will result in more definitive
cure-behavior information.
1.4 This test method is intended for resin/substrate composites that have an uncured effective elastic modulus in shear greater
than 0.5 MPa.
1.5 Apparent discrepancies may arise in results obtained under differing experimental conditions. These apparent differences
from results observed in another study can usually be reconciled, without changing the observed data, by reporting in full (as
described in this test method) the conditions under which the data were obtained.
1.6 Due to possible instrumentation compliance, especially in the compressive mode, the data generated may indicate relative
and not necessarily absolute property values.
1.7 Test data obtained by this test method are relevant and appropriate for use in engineering design.
1.8 The values stated in SI units are to be regarded as the standard.
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 standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use. Specific precautionary statements are given in Note 5.
NOTE 1—There is no known ISO equivalent to this standard.
2. Referenced Documents
2.1 ASTM Standards:
D4000 Classification System for Specifying Plastic Materials
D4065 Practice for Plastics: Dynamic Mechanical Properties: Determination and Report of Procedures
D4092 Terminology for Plastics: Dynamic Mechanical Properties
ASTM/IEEE SI–10 Standard for Use of the International System of Units (SI): The Modern Metric System
3. Terminology
3.1 Definitions—For definitions applicable to this test method refer to Terminology D4092.
This test method 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 March 1, 2008Nov. 1, 2016. Published April 2008November 2016. Originally approved in 1985. Last previous edition approved in 20032008
as D4473 – 03.D4473 - 08. DOI: 10.1520/D4473-08.10.1520/D4473-08R16.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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
D4473 − 08 (2016)
4. Summary of Test Method
4.1 A known amount of thermosetting liquid resin or resin-impregnated substrate is placed in mechanical oscillation at either
a fixed or natural resonant frequency or by free vibration and at either isothermal conditions, with a linear temperature increase
or using a time-temperature relation simulating a processing condition. The elastic or loss modulus, or both, of the composite
specimen are measured in shear or compression as a function of time. The point in time when tan delta is maximum, and the elastic
modulus levels off after an increase, is calculated as the gel time of the resin under the conditions of the test.
NOTE 2—The particular method for measuring the elastic and loss moduli and tan delta depends upon the individual instrument’s operating principles.
5. Significance and Use
5.1 This test method provides a simple means of characterizing the cure behavior of thermosetting resins using very small
amounts of material (fewer than 3 to 5 g). The data obtained may be used for quality control, research and development, and
establishment of optimum processing conditions.
5.2 Dynamic mechanical testing provides a sensitive method for determining cure characteristics by measuring the elastic and
loss moduli as a function of temperature or time, or both. Plots of cure behavior and tan delta of a material versus time provide
graphical representation indicative of cure behavior under a specified time-temperature profile.
5.3 This test method can be used to assess the following:
5.3.1 Cure behavior, including rate of cure, gel, and cure time.
5.3.2 Processing behavior, as well as changes as a function of time/temperature.
NOTE 3—The presence of the substrate prevents an absolute measure, but allows relative measures of flow behavior during cure.
5.3.3 The effects of processing treatment.
5.3.4 Relative resin behavioral properties, including cure behavior and damping.
5.3.5 The effects of substrate types on cure.
NOTE 4—Due to the rigidity of a supporting braid, the gel time obtained from dynamic mechanical traces will be longer than actual gel time of the
unsupported resin measured at the same frequency. This difference will be greater for composites having greater support-to-polymer rigidity ratios.
5.3.6 Effects of formulation additives that might affect processability or performance.
5.4 For many materials, there may be a specification that requires the use of this test method, but with some procedural
modifications that take precedence when adhering to the specification. Therefore, it is advisable to refer to that material
specification before using this test method. Table 1 of Classification System D4000 lists the ASTM materials standards that
currently exist.
6. Interferences
6.1 Since small quantities of resin are used, it is essential that the specimens be representative of the polymeric material being
tested.
6.2 The result is a response of the thermal advancement or cure behavior of the resin in combination with any substrate used
to support the resin.
7. Apparatus
7.1 The function of the apparatus is to hold a neat (unmodified) resin or uncured supported composite formulation or coated
substrate of known volume and dimensions. The material acts as the elastic and dissipative element in a mechanically driven
oscillatory shear or dynamic compression system. These dynamic mechanical instruments operate in one or more of the following
modes for measuring cure behavior in torsional shear or dynamic compression:
7.1.1 Forced, constant amplitude, fixed frequency,
7.1.2 Forced, constant amplitude, resonant oscillation,
7.1.3 Freely decaying oscillation.
7.2 The apparatus shall consist of the following:
7.2.1 Test Fixtures, a choice of the following:
7.2.1.1 Polished Cone and Plate (Having a Known Cone Angle)—Usually a 25 or 50-mm diameter cone and plate or parallel
plates are recommended for neat resins. Variations of this tooling, such as bottom plates with concentric overflow rims, may be
used as necessary.
7.2.1.2 Parallel Plates, having either smooth, polished, or serrated surfaces are recommended for neat resins or prepregs having
less than 6 % volatiles.
7.2.1.3 Clamps—A clamping arrangement that permits gripping of the composite sample.
Hedvat, S., Polymer Engineering and Science, Vol 21, No. 3, February 1981.
D4473 − 08 (2016)
FIG. 1 Typical Temperature Profile
7.2.2 Oscillatory Deformation (Strain Device)—A device for applying a continuous oscillatory deformation (strain) to the
specimen. The deformation (strain) may be applied and then released, as in free-vibration devices, or continuously applied, as in
forced-vibration devices (see Table 1 of Practice D4065).
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 should be measurable with a precision of 61°C, frequency to 61 %, and force
to 61 %.
7.2.4 Temperature Controller and Oven—A device for controlling the temperature, either by heating (in steps or ramps), cooling
(in steps or ramps), maintaining a constant specimen environment, or a combination thereof. Fig. 1 illustrates typical
time-temperature profiles. A temperature controller should be sufficiently stable to permit measurement of sample temperature to
within 1°C.
7.3 Nitrogen, or other inert gas supply for purging purposes.
8. Test Specimens
8.1 The neat resin or the self-supporting composition, or both, should be representative of the polymeric material being tested.
8.2 Due to the various geometries that might be used for dynamic mechanical curing of thermosetting resins/composites,
specimen size is not fixed by this test method. Cure rates may be influenced by specimen thickness, so equal volumes of material
should be used for any series of comparisons.
8.3 For convenience, low-viscosity neat resins can be studied using a supporting substrate.
8.4 The substrate on which the resin is supported is normally in the form of a woven-glass cloth or tape or a braided-glass cord.
The substrate should have negligible stiffness when compared to the cured resin sample in both a flexural and torsional mode of
deformation. Other substrates can be used if their effect on cure mechanisms were of interest. The composition should be
representative of the polymeric material being tested.
8.4.1 To standardize the pH of the supporting substrates, soak the cloth or braid overnight in distilled water and vacuum-dry.
This will avoid any extraneous results with resins that are pH-sensitive.
9. Calibration
9.1 Calibrate the instrument using procedures recommended by the manufacturer for that specific make and model.
10. Procedure
NOTE 5—Precaution: Toxic or corrosive effluents, or both, may be released when heating the resin specimen to its cured state and could be harmful
to personnel or to the instrumentation.
10.1 Apply the resin or uncured, self-supporting composite onto the test fixture. In the case of two-part room-temperature cure
resins, mixing should be carried out in less than 1 % of the expected gel time.
10.2 Out-time effects and moisture-effect data must be recorded and reported.
D4473 − 08 (2016)
10.3 Procedure A—Unsupported Resin:
10.3.1 Allow the sample to equilibrate to room temperature in a desiccator. In case of a solid sample, place it in an oven at
100°C for 5 to 10 min in order to soften. Use a vacuum oven to degas, if necessary. Use 50-mm diameter test plates for low
minimum-viscosity systems and 25-mm diameter plates for higher minimum-viscosity materials.
10.3.2 For neat resins, be certain that there is sufficient material to cover the bottom plate uniformly.
10.3.3 Lower the upper test fixture so that it is touching the material to be cured.
10.3.3.1 The distance between the two parallel plates should be approximately 0.5 mm. However, when low viscosity materials
are being evaluated using cone and plate test fixtures, the recommended minimum gap setting is equipment-dependent and
reference should be made to the manufacturer’s operational manual for correct gap setting.
10.3.3.2 Cone and plate experiments should be run only at one temperature. Any changes in the temperature setting will require
adjusting the gap setting to the manufacturer’s recommended value.
10.3.4 Conduct cure characterization of the submitted material in accordance with the desired time and temperature parameters
recording the appropriate property values.
10.4 Procedure B—Supported Compositions:
10.4.1 For self-supporting compositions in prepreg-type form using cone and plate or parallel plate fixturing, be certain that
there is sufficient material to fill the sample volume on the lower plate completely.
10.4.2 Insert the substrate between the plates of the test instrument. A sample disk (usually 25 mm in diameter) of the
self-supporting composition can be die-cut, or several plies of prepreg can be compressed into a sheet (for example, for 3 min at
77°C at 75 atmospheres, 1000 psi) and then a disk die-cut. The orientation of unidirectional reinforcements may affect cure
behavior and the orientation should be reported in 12.1.4.
10.4.3 For three to five plies, the recommended gap setting is 1 to 2 mm. This gap setting is arbitrary and dependent on the type
of material and the number of plies being characterized. A gap setting of 0.5 mm would be minimum. Cone and plate test fixtures
are not recommended for supported compositions.
10.4.4 For self-supporting substrates where either a bare substrate is to be impregnated with liquid resin (rectangular or
cylindrical form) or where a similar prepreg-type specimen forms a rectangular specimen, clamp the substrate in place utilizing
the instrument’s grip system.
10.4.5 Conduct the cure characterization of the submitted material in accordance with the desired time and temperature
parameters recording the appropriate property values.
10.5 Procedure C—Dynamic Compression:
10.5.1 Prepare the test specimen in accordance with the procedure described in 10.4.2 and 10.4.3.
10.5.2 Compress slightly the specimen disk and monitor and record the preload force by observing the normal force gage or
indicator. Adjust the gap as necessary to accommod
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