ASTM D4473-03

Standard Test Method for Plastics: Dynamic Mechanical Properties: Cure Behavior

SIGNIFICANCE AND USE
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.
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.
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.
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 D 4000 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 unsupported resins and resins supported on substrates and subjected to various oscillatory deformations. These deformations may be in shear or the dynamic compression of supported resins using a dynamic mechanical instrument.
1.2 This test method is intended to provide means for determining the cure behavior of supported and unsupported thermosetting resins over a range of temperatures by free vibration and resonant and nonresonant forced-vibration techniques, in accordance with Practice D 4065. Plots of modulus, cure behavior, 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, will generate 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 ...

General Information

• Status: Historical
• Publication Date: 09-Jul-2003
• ICS: 83.080.10 - Thermosetting materials
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.10 - Mechanical Properties

Relations

• Replaces: ASTM D4473-01 - Standard Test Method for Plastics: Dynamic Mechanical Properties: Cure Behavior
• Effective Date: 10-Jul-2003
• Replaced By: ASTM D4473-08 - Standard Test Method for Plastics: Dynamic Mechanical Properties: Cure Behavior
• Effective Date: 01-Mar-2008
• Referred By: ASTM D4762-18 - Standard Guide for Testing Polymer Matrix Composite Materials
• Effective Date: 10-Jul-2003
• Referred By: ASTM D7750-23 - Standard Test Method for Cure Behavior of Thermosetting Resins by Dynamic Mechanical Procedures using an Encapsulated Specimen Rheometer
• Effective Date: 10-Jul-2003
• Referred By: ASTM E3277-23 - Standard Test Method for Determining the Liquid or Solid State of a Material by Rheometry
• Effective Date: 10-Jul-2003
• Referred By: ASTM D3532/D3532M-19 - Standard Test Method for Gel Time of Carbon Fiber-Epoxy Prepreg
• Effective Date: 10-Jul-2003
• Referred By: ASTM D5592-94(2018) - Standard Guide for Material Properties Needed in Engineering Design Using Plastics
• Effective Date: 10-Jul-2003

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D 4473 – 03
Standard Test Method for
1
Plastics: Dynamic Mechanical Properties: Cure Behavior
This standard is issued under the fixed designation D 4473; 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* 1.9 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 This test method covers the use of dynamic-mechanical-
responsibility of the user of this standard to establish appro-
oscillation instrumentation for gathering and reporting the
priate safety and health practices and determine the applica-
thermal advancement of cure behavior of thermosetting resin.
bility of regulatory limitations prior to use. Specific precau-
It may be used for determining the cure properties of unsup-
tionary statements are given in Note 5.
ported resins and resins supported on substrates and subjected
to various oscillatory deformations. These deformations may
NOTE 1—There is no similar or equivalent ISO standard.
be in shear or the dynamic compression of supported resins
2. Referenced Documents
using a dynamic mechanical instrument.
2
1.2 This test method is intended to provide means for
2.1 ASTM Standards:
determining the cure behavior of supported and unsupported
D 4000 Classification System for Specifying Plastic Mate-
thermosetting resins over a range of temperatures by free
rials
vibration and resonant and nonresonant forced-vibration tech-
D 4065 Practice for Plastics: Dynamic Mechanical Proper-
niques, in accordance with Practice D 4065. Plots of modulus,
ties: Determination and Report of Procedures
cure behavior, tan delta, and damping index as a function of
D 4092 Terminology for Plastics: Dynamic Mechanical
time/temperature are indicative of the thermal advancement or
Properties
cure characteristics of a resin.
ASTM/IEEE SI–10 Standard for Use of the International
1.3 Thistestmethodisvalidforawiderangeoffrequencies,
System of Units (SI): The Modern Metric System
typically from 0.01 to 100 Hz. However, it is strongly
3. Terminology
recommended that low-frequency test conditions, generally
below 1.5 Hz, will generate more definitive cure-behavior
3.1 Definitions—For definitions applicable to this test
information. method refer to Terminology D 4092.
1.4 This test method is intended for resin/substrate compos-
4. Summary of Test Method
ites that have an uncured effective elastic modulus in shear
greater than 0.5 MPa. 4.1 A known amount of thermosetting liquid or resin-
1.5 Apparent discrepancies may arise in results obtained impregnated substrate is placed in mechanical oscillation at
under differing experimental conditions. These apparent differ- fixed or natural resonant frequencies at either isothermal
ences from results observed in another study can usually be conditions, with a linear temperature increase or a time-
reconciled, without changing the observed data, by reporting in temperature relation simulating a processing condition. The
full (as described in this test method) the conditions under elastic or loss modulus, or both, of the composite specimen are
which the data were obtained. measuredinshearasafunctionoftime.Thepointintimewhen
1.6 Due to possible instrumentation compliance, especially tan delta is maximum, and the elastic modulus levels after an
in the compressive mode, the data generated may indicate increase, is calculated as the gel time of the resin under the
relative and not necessarily absolute property values. conditions of the test.
1.7 Test data obtained by this test method are relevant and
NOTE 2—The particular method for measuring the elastic and loss
appropriate for use in engineering design.
moduli and tan delta depends upon the individual instrument’s operating
1.8 The values stated in SI units are to be regarded as the
principles.
standard.
1 2
This test method is under the jurisdiction ofASTM Committee D20 on Plastics For referenced ASTM standards, visit the ASTM website, www.astm.org, or
and is the direct responsibility of Subcommittee D20.10 on Mechanical Properties. contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Current edition approved July 10, 2003. Published September 2003. Originally Standards volume information, refer to the standard’s Document Summary page on
approved in 1985. Last previous edition approved in 2001 as D 4473 – 01. the ASTM website.
*A Summary of Changes section appears at the end of this standard.
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