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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