ASTM D4102-82(2008)

Standard Test Method for Thermal Oxidative Resistance of Carbon Fibers

SIGNIFICANCE AND USE
The test is used to determine the oxidative resistances of carbon fibers as a means of selecting the most stable fibers for incorporation in high-temperature fiber-reinforced composite systems. It can be used for quality control, material specification, and for research and development of improved carbon fibers. Factors that influence the oxidative resistance and should be reported are fiber identification, precursor type, fiber modulus, and any information on impurities, particularly metals. Also note that the presence of finish on the fiber can affect the oxidative resistance, and thus, alternative specimen preparations that enable the evaluation of finish effects are included.
SCOPE
1.1 This test method covers the apparatus and procedure for the determination of the weight loss of carbon fibers, exposed to ambient hot air, as a means of characterizing their oxidative resistance.
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversions to inch-pound units which are provided for information only and are not considered standard.
1.3 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. For specific hazard information, see Section 8.

General Information

• Status: Historical
• Publication Date: 31-Oct-2008
• ICS: 59.100.20 - Carbon materials
• Technical Committee: D30 - Composite Materials
• Drafting Committee: D30.03 - Constituent/Precursor Properties

Relations

• Replaces: ASTM D4102-82(2004) - Standard Test Method for Thermal Oxidative Resistance of Carbon Fibers
• Effective Date: 01-Nov-2008
• Referred By: ASTM D4762-18 - Standard Guide for Testing Polymer Matrix Composite Materials
• Effective Date: 01-Nov-2008

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4102 − 82(Reapproved 2008)
Standard Test Method for
Thermal Oxidative Resistance of Carbon Fibers
This standard is issued under the fixed designation D4102; 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 4. Summary of Test Method
1.1 This test method covers the apparatus and procedure for 4.1 The test method is composed of two parts. The first one
the determination of the weight loss of carbon fibers, exposed specifies exposure conditions for an accelerated measurement,
to ambient hot air, as a means of characterizing their oxidative determining weight loss of the carbon fiber after 24 h in air at
resistance. 375°C (707°F). The second part specifies conditions for an
extended measurement, determining the weight loss resulting
1.2 The values stated in SI units are to be regarded as
from 500-h exposure in air at 315°C (600°F).
standard. The values given in parentheses are mathematical
conversions to inch-pound units which are provided for infor-
5. Significance and Use
mation only and are not considered standard.
5.1 The test is used to determine the oxidative resistances of
1.3 This standard does not purport to address all of the
carbon fibers as a means of selecting the most stable fibers for
safety concerns, if any, associated with its use. It is the
incorporation in high-temperature fiber-reinforced composite
responsibility of the user of this standard to establish appro-
systems. It can be used for quality control, material
priate safety and health practices and determine the applica-
specification, and for research and development of improved
bility of regulatory limitations prior to use. For specific hazard
carbon fibers. Factors that influence the oxidative resistance
information, see Section 8.
and should be reported are fiber identification, precursor type,
fiber modulus, and any information on impurities, particularly
2. Referenced Documents
metals. Also note that the presence of finish on the fiber can
2.1 ASTM Standards:
affect the oxidative resistance, and thus, alternative specimen
C613/C613M Test Method for Constituent Content of Com-
preparations that enable the evaluation of finish effects are
posite Prepreg by Soxhlet Extraction
included.
3. Definitions
6. Apparatus
3.1 carbon fibers—fibers containing at least 90 % carbon by
6.1 Balance, capable of weighing to the nearest 0.1 mg.
weight made by pyrolysis from synthetic polymeric or pitch
6.2 Vacuum Oven, capable of providing vacuum of 10 torr
fibers and having moduli ≥70 GPa (≥10 psi).
(1.3 kPa) or less at 80°C (177°F).
3.2 precursor—organic fiber from which carbon fibers are
6.3 Circulating Air Oven, with sufficient flow rate and
prepared via pyrolysis. Polyacrylonitrile (PAN), rayon, and
capability to change the ambient air in the chamber once a
pitch are commonly used.
minute, while maintaining the temperature within 10°C (18°F)
3.3 fiberfinish—surfacecoatingappliedtofiberstofacilitate
over the 25°C (77°F) to 375°C (707°F) range.
handling or provide better wetting and compatibility of fiber
6.4 Glass Beakers, borosilicate, 250-mL (8.45 oz) or other
and matrix, or both.
size, appropriate for the oven (one per sample).
6.5 Wire Mesh Covers, for the beakers to reduce excessive
1 3
This test method is under the jurisdiction of ASTM Committee D30 on
air turbulence during the exposure.
Composite Materialsand is the direct responsibility of Subcommittee D30.03 on
6.6 Boiling Flasks or Erlenmeyer Flasks, borosilicate glass,
Constituent/Precursor Properties.
Current edition approved Nov. 1, 2008. Published December 2008. Originally
250- or 500-mL (8.45- or 16.91-oz) size, with standard-taper
approved in 1982. Last previous edition approved in 2004 as D4102 – 82 (2004).
joint.
DOI: 10.1520/D4102-82R08.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on 20-mesh nickel-chromium wire gauze from Fisher Scientific Co. has been
the ASTM website. found satisfactory for this purpose.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4102 − 82 (2008)
6.7 Glass Condensers, borosilicate for the above flasks. 11.2 If finish is to be removed (see 9.3), then either use a
Soxhlet extraction as recommended in Test Method C613/
6.8 Hot Plate.
C613M or follow Steps 11.3.1 – 11.3.4. If finish is not to be
6.9 Tweezers, stainless steel.
removed, skip Steps 11.3.1 – 11.3.4 and proceed with Step
11.4.
7. Reagents and Materials
11.3 Removal of the Finish:
7.1 Methyl Ethyl Ketone (2-butanone) 99.5 % pure, boiling
11.3.1 Put the specimen in a dry flask and cover with 100 to
range 70.0 to 81.0°C (158 to 177.8°F), or other suitable
200 mL(3.38 to 6.76 oz) of methyl ethyl ketone solvent. Place
solvents recommended in Test Method C613/C613M.
the condenser onto the flask and start the cooling water. Heat
8. Hazards the flask on the hot plate or heating bath to bring the solvent to
boil. Soak the specimen in the boiling solvent for 15 min. Take
8.1 The methyl ethyl ketone, classified as an irritant and a
off the condenser, decant the solvent, and remove the speci-
fire hazard, should be handled in a well-ventilated area and
men.
should not be exposed to direct heat or open flame.
11.3.2 Dry the specimen in the vacuum oven at 77°C
(170°F) at a reduced pressure of 10 torr (1.3 kPa) or less for 30
9. Test Specimen and Sampling
min.
9.1 Using clean gloves to prevent any contamination, par-
11.3.3 Weigh the dried specimen to the nearest 0.1 mg.
ticularly with salt, unwrap the outer layers, which may have
Record the weight.
been contaminated by previous handling or environmental
11.3.4 Repeat Steps 11.3.1 – 11.3.3 until the weight remains
exposure, from the test package of carbon-fiber yarn and
constant, within 60.1 mg. Record the final weight, W .
e
discard. Form a small coil of fresh fiber weighing approxi-
11.4 Drying:
mately 2 g around two gloved fingers and tuck the ends in to
11.4.1 Dry each specimen for 16 h in a vacuum oven at
obtain a specimen in the form of an easily handleable loop.
77°C (170°F) at a reduced pressure of 10 torr (1.3 kPa)
...