AFML-TR-78-64
PA~o2•69 OFFICIAL FILECL UP
THERMOGRAVIMETRIC ANALYSIS OFPOLYMERS IN AIR
Polymer BranchNonmetallic Materials Division
August 1978
TECHNICAL REPORT AFML-TR-78-64
Final Report for Period November 1977 through February 1978
Approved for public release; distribution unlimited.
AIR FORCE MATERIALS LABORATORY IES• O L O 505 1AIR FORCE WRIGHT AERONAUTICAL LABORATORIES OAIR FORCE SYSTEMS COMMANDWRIGHT-PATTERSON AIR FORCE BASE, OHIO 45433
BEST AVAILABLE COPY
NOTICE
When Government drawings, specifications, or other data are used for anypurpose other than in connection with a definitely related Government pro-curement operation, the United States Government thereby incurs no respon-sibility nor any obligation whatsoever; and the fact that the government mayhave formulated, furnished, or in any way supplied the said drawings, speci-fications, or other data, is not to be regarded by implication or otherwiseas in any manner licensing the holder or any other person or corporation, orconveying any rights or permission to manufacture, use, or sell any patentedinvention that may in any way be related thereto.
This report has been reviewed by the Information Office (ASD/OIP) and isreleasable to the National Technical Information Service (NTIS). At NTIS, itwill be available to the general public, including foreign nations.
This technical report has been reviewed and is approved for publication.
ARNOLD tR. L. VAN DEUSEN, Chiefoject Scientist Polymer Branch
Nonmetallic Materials Division
FOR THE DIRECTOR
Nonmetallic Materials Division
"If your address has changed, if you wish to be removed from our mailinglist, or if the addressee is no longer employed by your organization pleasenotify AFML/MBP, W-PAFB, OH 45433 to help us maintain a current mailing list".
Copies of this report should not be returned unless return is required bysecurity considerations, contractual obligations, or notice on a specificdocument.
AIR FORCE/56780/6 June 1979 - 125
SECURITY CLASSIFICATION OF THIS PAGE (When Data E;ntered)
REPORT DOCUMENTATION PAGE [ READ INSTRuc'rIosNBEFORE COMPLETING FORM
1. REPORT NUMBER i2. GOVT ACCESSION No. 3. RECIPIENT'S CATALOG NUMBER
AFML-TR-78-64
4. TITLE (and Subtitle) S. TYPE OF REPORT f PERIOD COVEREDFinal Report
THERMOGRAVIMETRIC ANALYSIS OF POLYMERS IN AIR November 1977 - February 197f6. PERFORMING ORG, REPORT NUMBER
7. AUTHOR(&) S. CONTRACT OR GRANT NUMBER(s)
Gerhard F. L. Ehlers, AFML/MBPEdward J. Soloski, UDRI
S. PERFORMING ORGANIZATION NAME AND ADDRESS 10. PROGRAM ELEMENT, PROJECT, TASK
Air Force Materials Laboratory (AFML/MBP) AREA & WORK UNIT NUMBERS
Air Force Systems Command 62102F/2419/04
Wright-Patterson Air Force Base, OH 45433 24190415
I1. CONTROLLING OFFICE NAME AND ADDRESS 12. REPORT DATE
Air. Force Materials Laboratory (AFML/MBP) August 1978Air Force Systems Command 13. NUMBER OF PAGESWright-Patterson Air Force Base, OH 4543314. MONITORING AGENCY NAME & ADDRESS(tf dlffrrent from Coritrollinp Office) 15. SECURITY CLASS. (of this report)
UNCLASSIFIED15a. DECL ASSI FICATION/ DOWNGRADING
SCHEDULE
16. DISTRIBUTION STATEMENT (of this Report)
Approved for public release, distribution unlimited.
17. DISTRIBLITION STATEMENT (of the eb,tract -ntered In Block 20, If diff•-rnt ftrm Rnportt
18. SUPPLEMENTARY NOTES
19. KEY WORDS (Continue on reverse aide it necessary and identify by bfock number)
Thermogravimetric AnalysisPolymers
20. ABSTRACT (Continue on reverse side if necessary and Identify by hloek urntuber)
This report is concerned with the weight loss curves of 107 polymers, representa-tive of a wide range of systems such as aliphatic, fluoroaliphatic, aromatic,heterocyclic and semiorganic, are presented. The data have been obtained in aDuPont 951 Thermogravimetric Analyzer in air at a heating rate of 20 0 C/min.
DD 1 JAN73 1473 EDiTION OF I N3V 65 IS OBSOLETESECURITY CLASSIFICATION OF THIS PAGE (47hen Data Entered)
AFML-TR-78-64
FOREWORD
This report was prepared by the Polymer Branch, Nonmetallic
Materials Division. The work was initiated under WUD #43, "Structural
Resins". It was administered under the direction of the Air Force
Materials Laboratory, Air Force Wright Aeronatical Laboratories, Air
Force Systems Command,- Wright-Patterson Air Force Base, Ohio, with
Dr. G. F. L. Ehlers (AFML/MBP) as Project Scientist.
The report covers work conducted from November 1977 to February 1978
by G. F. L. Ehlers, Air Force Materials Laboratory and E. J. Soloski,
University of Dayton Research Institute. It was submitted for publication
by the authors in February 1978.
iii
AFML-TR-78-64
TABLE OF CONTENTS
SECTION PAGE
I INTRODUCTION 1
II DISCUSSION 2
III RESULTS 3
AFML-TR- 78-64
LIST OF TGA CURVES
PAGES
Aliphatic (addition type) polymers 4-13
Fl uoroal i phati cs 14-21
Del ri n 22
Nylon 6,6 23
Epoxy resins 24-27
Phenolic resin 28
Pyrolyzed rayon 29
Polyphenyl enes 30-33
Polyphenyl ene oxides 34-40
Polyphenylene sul fones 39-42
Polyphenyl ene s ul foxi de 43
Polyphenylene sulfide 44
Aromatic polyesters 45-48
Polycarbonate 49
Polyxylylenes 50-51
Polyurea 52
Aromatic polyamides 53-56
Polyimides 57-60
Polybenzimidazoles 61-69
Polybenzoxazol es 70-77
Polyoxadiazoles 78-80
Polybenzothi azol es 81-83
Polythiadiazoles 84
Polyqui noxal i nes 85-94
BBB and related structures 95-98
Miscellaneous polyheterocycl i cs 99-104
Silicon containing polymers 105-110
vi
AFML-TR-78-64
SECTION I
INTRODUCTION
Between 1960 and 1977, thermal analysis data have been determined
on approximately 1800 experimental polymers, prepolymers, and oligomers.
The majority of these data consisted of weight loss studies under
programmed and isothermal conditions, and DTA and DSC scans. Some
samples have been subjected to thermomechanical analysis, torsion braid
analysis, and thermal decomposition/mass spectrographic analysis.
As far as thermogravimetric data under programmed conditions are
concerned, the predominant number of samples have been run on a modified
Chevenard Thermobalance at a fixed heating rate of approximately 3°C/min,
and in most cases in a nitrogen atmosphere. These data served for many
years to obtain a quick and first indication about the basic thermal
stability of a polymer system.
However, more recently, these methods and results became inadequate.
The Chevenard balance required relatively large sample sizes (50 - 100 mg).
The fixed heating rate of 3°C/min allowed only one run per day, and the
results could not be compared to DSC or TMA runs on the same polymer;
here, heating rates of 20°C/min are being used in order to obtain
optimal sensitivity and resolution for the detection of glass transition
temperatures. Furthermore, increased need for weight loss data in air
required additional data.
AFML-TR-78-64
SECTION II
DISCUSSION
107 polymer samples, representative of systems such as aliphatic,
fluoroaliphatic, aromatic, heterocyclic and semiorganic structures, were
subjected to programed thermogravimetric analysis in the Dupont 951
Thermogravimetric Analyzer. A heating rate of 20°C/min was used, and
the scans were carried out in an air atmosphere with a flow rate of
72 cc/min.
A number of the weight loss plots showed irregularities of the type
seen on pages 79, 90, 91, 99, and 101. Vigorous gas evolution at this
fast heating rate cools sample and thermocouple, resulting in a shift
of the weight loss curve towards lower temperatures. These irregularities
normally have been eliminated during replotting, with the exception of
the cases on the above pages. An extreme case was Delrin, which had
about a 70°C drop in temperature beyond the last point of the curve
shown on page 21. It was impossible in this case to correct the curve.
2
AFML-TR-78-64
SECTION III
RESULTS
3
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