SAE AMS 3729A-1994 Epoxy Resin Matrix Thermosetting Moderate Temperature Resistant Unfilled《未填充的适度耐高温热固环氧树脂基体》.pdf

1、1. SCOPE:1.1 Form:This specification covers a heat-reactive, thermosetting, epoxy resin matrixin the form of a semi-solid. The resin matrix thermally cures to an epoxypolymer.1.2 Application:This product has been used typically in manufacture of moderate temperature,high strength composite prepreg m

2、aterials, but usage is not limited to suchapplications.1.3 Safety-Hazardous Materials:While the materials, methods, applications, and processes described orreferenced in this specification may involve the use of hazardous materials,this specification does not address the hazards which may be involve

3、d in suchuse. It is the sole responsibility of the user to ensure familiarity withthe safe and proper use of any hazardous materials and to take necessaryprecautionary measures to ensure the health and safety of all personnelinvolved.2. APPLICABLE DOCUMENTS:The following publications form a part of

4、this specification to the extentspecified herein. The latest issue of SAE publications shall apply. Theapplicable issue of other publications shall be the issue in effect on thedate of the purchase order.AEROSPACE MATERIAL SPECIFICATIONAMS3729 REV. A Issued 1985-10Revised 1994-06Reaffirmed 2014-08Su

5、perseding AMS3729Epoxy Resin Matrix, ThermosettingModerate Temperature Resistant, UnfilledRATIONALEAMS3729A has been reaffirmed to comply with the SAE five year review policy._SAE Technical Standards Board Rules provide that: “This report is published by SAE to advance the state of technical and eng

6、ineering sciences. The use of this report is entirely voluntary, and its applicability and suitability for any particular use, including any patent infringement arising therefrom, is the sole responsibility of the user.”SAE reviews each technical report at least every five years at which time it may

7、 be revised, reaffirmed, stabilized, or cancelled. SAE invites your written comments and suggestions.Copyright 2014 SAE InternationalAll rights reserved. No part of this publication may be reproduced, stored in a retrieval system or transmitted, in any form or by any means, electronic, mechanical, p

8、hotocopying, recording, or otherwise, without the prior written permission of SAE.877-606-7323 (inside USA and Canada)TO PLACE A DOCUMENT ORDER: Tel: Tel: +1 724-776-4970 (outside USA)SAE WEB ADDRESS:Fax: 724-776-0790Email: CustomerServicesae.orghttp:/www.sae.orgSAE values your input. To provide fee

9、dbackon this Technical Report, please visithttp:/www.sae.org/technical/standards/AMS3729A2.1 SAE Publications:Available from SAE, 400 Commonwealth Drive, Warrendale, PA 15096-0001.AMS 2825 Material Safety Data SheetsAMS 3099 Curing Agent, Solid Aromatic Amine, 4,4-Diaminodiphenyl SulfoneAMS 3701 Epo

10、xy Resin, Tetraglycidyl Methylenedianiline (TGMDA), 10,000 -14,000 Centipoise ViscosityAMS 3705 Epoxy Resin, Cycloaliphatic LiquidAMS 3728 Epoxy Cresol Novolac Resin, Low Molecular WeightARP1610 Physical-Chemical Characterization Techniques, Epoxy Adhesive andPrepreg Resin Systems2.2 ASTM Publicatio

11、ns:Available from ASTM, 1916 Race Street, Philadelphia, PA 19103-1187.ASTM D 1652 Epoxy Content of Epoxy Resins2.3 U.S. Government Publications:Available from DODSSP, Subscription Services Desk, Building 4D, 700 RobbinsAvenue, Philadelphia, PA 19111-5094.MIL-STD-2073-1 DOD Materiel, Procedures for D

12、evelopment and Application ofPackaging Requirements3. TECHNICAL REQUIREMENTS:3.1 Material:Shall be a thermosetting formulation conforming to the percentages by weightshown in Table 1.TABLE I - CompositionComponent min maxTetraglycidyl Methylenedianiline, AMS 3701 54.5 58.5Epoxy Resin, Cycloaliphatic

13、 Liquid, AMS 3705 8.0 10.0Epoxy Cresol Novolac Resin, AMS 3728 7.5 9.54,4 - Diaminodiphenyl Sulfone, AMS 3099 23.0 27.0Boron Trifluoride Amine Complex 0.8 1.63.2 Impurities:Volatile content shall be not greater than 1.5%, determined in accordancewith 4.5.1:SAE INTERNATIONAL AMS3729A Page 2 of 9 3.3

14、Properties:Resin shall conform to the requirements shown in Table 2, determined inaccordance with specified test methods.TABLE 2 - PropertiesParagraph Property Requirement Test Method3.3.1Epoxy Content (equivalentper 100 grams) 0.36 to 0.62ASTM D 16523.3.2 4,4 - Diaminodiphenyl Sulfone 23.0 to 27.0%

15、 4.5.23.3.3 Boron Trifluoride Amine Complex 0.8 to 1.6% 4.5.33.3.4 Epoxy Resin, Cycloaliphatic Liquid 8.0 to 10.0% 4.5.43.3.5 Thermal Analysis by DifferentialScanning Calorimeter (DSC)Tpeak 202 to 222 C(396 to 432 F)4.5.53.3.6 Resin Rheology Flow Number 5.0 to 10.0 minutes/poise 4.5.63.4 Quality:The

16、 resin, as received by purchaser, shall be uniform in quality andcondition, and free from foreign materials and from contaminants detrimentalto usage of the resin.4. QUALITY ASSURANCE PROVISIONS:4.1 Responsibility for Inspection:(R)The manufacturer of resin shall supply all samples for required test

17、s andshall be responsible for performing all required tests. Purchaser reservesthe right to sample and to perform any confirmatory testing deemed necessaryto ensure that the resin conforms to the requirements of this specification.4.2 Classification of Tests:4.2.1 Acceptance Tests: Tests for impurit

18、ies (3.2) and epoxy content (3.3.1) areacceptance tests and shall be performed on each lot.4.2.2 Preproduction Tests: Tests for all technical requirements arepreproduction tests and shall be performed prior to or on the initialshipment of resin to a purchaser, when a change in ingredients and/orproc

19、essing requires reapproval as in 4.4.2, and when purchaser deemsconfirmatory testing to be required.SAE INTERNATIONAL AMS3729A Page 3 of 9 4.3 Sampling and Testing:(R)Shall be as follows:4.3.1 For Acceptance Tests: Each lot of resin shall be sampled at random toprovide sufficient resin to perform al

20、l required tests. The number ofdeterminations for each requirement shall be as specified in the applicabletest procedure or, if not specified therein, not less than three.4.3.1.1 A lot shall be all resin produced in a continuous production run from thesame batches of raw materials under the same fix

21、ed conditions andpresented for manufacturers inspection at one time.4.3.1.2 A batch shall consist of the quantity of material run in a reactor ormixer at one time.4.3.1.3 When a statistical sampling plan has been agreed upon by purchaser and(R) supplier, sampling shall be in accordance with such pla

22、n in lieu ofsampling as in 4.3.1 and the report of 4.6 shall state that such plan wasused.4.3.2 For Preproduction Tests: As agreed upon by purchaser and supplier.4.4 Approval:4.4.1 Sample resin shall be approved by purchaser before resin for production useis supplied, unless such approval be waived

23、by purchaser. Results of testson production resin shall be essentially equivalent to those on theapproved sample.4.4.2 Manufacturer shall use ingredients, manufacturing procedures, processes,and methods of inspection on production resin which are essentially thesame as those used on the approved sam

24、ple. If necessary to make any changein ingredients, in type of equipment for processing, or in manufacturingprocedures, manufacturer shall submit for reapproval a statement of theproposed changes in ingredients and/or processing and, when requested,sample resin. Production resin made by the revised

25、procedure shall not beshipped prior to receipt of reapproval.4.5 Test Methods:Shall be as follows:4.5.1 Volatile Content: Shall be determined by accurately weighing (W,) to thenearest 0.1 mg, four samples weighing not less than 1.0 gram each. Usingporcelain crucibles (preferably covered) previously

26、brought to constantweight by igniting at 845 C 25 (1553 F 45), dry samples in acirculating-air oven at 175 C 5 (347 F 9) for 15 minutes 1. Coolin a desiccator and reweigh (W2). Calculate the individual results of thefour determinations using Equation 1.SAE INTERNATIONAL AMS3729A Page 4 of 9 (W1 W2)V

27、olatile Content, % =W1X 100 (Eq.1)4.5.1.1 Report both the individual results and the arithmetic mean.4.5.2 4,4 - Diaminodiphenyl Sulfone (DDS) Content: Shall be determined byinfrared absorption spectroscopy (IR) in accordance with ARP1610. Thepercent by weight DDS shall be reported.4.5.3 Boron Trifl

28、uoride Amine Complex Content: Shall be determined by atomicabsorption (AA) in accordance with ARP1610. The percent by weightaccelerator shall be reported.4.5.4 Epoxy Cycloaliphatic Liquid Resin (ECLR) Content:4.5.4.1 Weigh, to the nearest 0.1, 50, 100, 150, and 200 mg samples of the ECLR.Transfer th

29、e samples to 100 mL volumetric flasks and dilute to volumewith chloroform.4.5.4.2 Place two 2.0 mm potassium bromide (KBr) precision path length, matchedliquid cells filled with chloroform in both the sample and referencebeams of the infrared (IR) spectrophotometer. Scan the region from 1600to 1800

30、cm-1to ensure a clean baseline free of extraneous absorptions.For the Beckman IR-9 infrared spectrophotometer, instrumental parametersshown in Table 3 are suggested:TABLE 3 - Instrumental ParametersParameter ValueScan range 1600 to 1800 cm-1Scan Speed 40 cm-1/minuteSlit Routine (2 times standard)Gai

31、n 3%Period 2Scale 0 to 100% TReference Chloroform4.5.4.3 Replace the chloroform in the sample cell with a standard samplesolution. Flush the sample cell 2 to 3 times with the solution to beanalyzed. Record the spectrum from 1600 to 1800 cm-1 for each standardsolution.4.5.4.4 ECLR exhibits an absorpt

32、ion maximum at 1730 cm-1. Construct acalibration curve on linear graph paper for percent ECLR by plotting theabsorbance values for the standard solutions, minus the baselineabsorbance, versus their concentration in mg/mL of ECLR.SAE INTERNATIONAL AMS3729A Page 5 of 9 4.5.4.5 Weigh, to the nearest 0.

33、1 mg, a 2.5 gram sample of the epoxy resin matrixor adhesive. Transfer this sample to approximately 70 mL of chloroform.Thoroughly agitate the mixture in an ultrasonic bath for 15 minutes.Filter the mixture using a glass crucible, wash the crucible and contentswith two 10 mL portions of fresh chloro

34、form, and dilute the filtrate andwashings to volume with chloroform in a 100 mL volumetric flask. Shakethe solution to ensure adequate mixing.4.5.4.6 Analyze the chloroform solution in accordance with 4.5.4.2 and 4.5.4.3.4.5.4.7 Take the absorbance value of the sample from the IR spectra and determi

35、nethe amount of ECLR in the solution from the calibration curve.4.5.4.8 Record the ECLR value (mg/mL).4.5.4.9 Calculate weight percent ECLR in the resin matrix using Equation 2.ECLR concentration mg/mL%ECLR =Sample concentration mg1mLX 100 (Eq.2)4.5.5 Thermal Analysis by Differential Scanning Calori

36、metry (DSC): Shall be usedto measure the exotherm peak temperature for the self-curing reaction inaccordance with ARP1610. The temperature obtained for a heating rate of5 C degrees per minute (9 F degrees per minute) shall be reported.4.5.6 Resin Rheology, Flow Number:4.5.6.1 Remove epoxy resin matr

37、ix from the freezer and allow to warm to roomtemperature before opening the package. Hydraulically press resinsamples between teflon cloth to approximately 5 mil (0.13 mm) thicknessand place uncovered in a desiccator at room temperature for 24 hoursprior to testing.4.5.6.2 After desiccation, cut 24-

38、mm circular resin wafers for rheology tests.4.5.6.3 Determine the flow characteristics of the resin using a RheometricDynamic Spectrometer Model RDS-7700, or equivalent. With thespectrometer in the parallel plate mode, the instrumental parameters andtest conditions are shown in Table 4.TABLE 4 - Ins

39、trumental Parameters and Test ConditionsParameter ValueSample Plates 25 mm disposableGap Setting 0.5 mm 0.01 mm (0.02 inch 0.0004)Starting Temperature 50 C (122 F)Strain 50%Frequency 10 rads/secondHeating Rate 50 C (122 F) (start) to gel temperature at 1 C degree per minute(1.8 F degree per minute)P

40、rogram Plot Viscosity versus time. Plot data to 103poise.SAE INTERNATIONAL AMS3729A Page 6 of 9 4.5.6.4 Calculate flow number by integrating Equation 3.tgel dtFlow Number =to n (Eq.3)minutespoisewhere:t = time (minutes)n = time dependent viscosity (poise)tgel= t at n = 103poise4.5.6.5 Report the flo

41、w number as ( ).4.6 Reports:The supplier of resin shall furnish with each shipment a report showing theresults of tests for impurities and properties, including copies ofthermograms and chromatograms, and stating that the resin conforms to theother technical requirements. This report shall include t

42、he purchase ordernumber, lot number, AMS 3729A, manufacturers product designation, date ofmanufacture, and quantity.4.6.1 A material safety data sheet conforming to AMS 2825, or equivalent, shallbe supplied to each purchaser prior to, or concurrent with, the report ofpreproduction test results or, i

43、f preproduction testing be waived bypurchaser, concurrent with the first shipment of resin for production use.Each request for modification of resin formulation shall be accompanied bya revised data sheet for the proposed formulation.4.7 Resampling and Retesting:(R)If any specimen used in the above

44、tests fails to meet the specifiedrequirements, disposition of the resin may be based on the results of testingthree additional specimens for each original nonconforming specimen. Failureof any retest specimen to meet the specified requirements shall be cause forrejection of the resin represented. Re

45、sults of all tests shall be reported.5. PREPARATION FOR DELIVERY:5.1 Packaging and Identification:5.1.1 A lot of resin may be packaged in small quantities and delivered under thebasic lot approval provided lot identification is maintained.5.1.2 Resin shall be packaged in airtight containers and main

46、tained at atemperature not higher than -18 C (0 F). Type and size of containersshall be agreed upon by purchaser and supplier.minutespoiseSAE INTERNATIONAL AMS3729A Page 7 of 9 5.1.3 Each container of epoxy resin shall be legibly identified, with not lessthan the following information, by an attache

47、d label using characters whichwill not be obliterated by normal handling:EPOXY RESIN MATRIX, THERMOSETTINGAMS 3729AMANUFACTURERS IDENTIFICATIONPURCHASE ORDER NUMBER DATE OF MANUFACTURELOT NUMBER QUANTITY PERISHABLE - REFRIGERATE AT -18 C (0 F) OR LOWER5.1.4 Containers of resin shall be prepared for

48、shipment in accordance with(R) commercial practice and in compliance with applicable rules and regulationspertaining to the handling, packaging, and transportation of the resin toensure carrier acceptance and safe delivery.5.1.5 For direct U.S. Military procurement, packaging shall be in accordance

49、with(R) MIL-STD-2073-1, Commercial Level, unless Level A is specified in therequest for procurement.6. ACKNOWLEDGMENT:Supplier of resin shall mention this specification number and its revisionletter in all quotations and when acknowledging purchase orders.7. REJECTIONS:Resin not conforming to this specification, or to modifications authorized bypurchaser, will be subject to rejection.8. NOTES:8.1 Revision