1、Designation: D 4018 99 (Reapproved 2004)Standard Test Methods forProperties of Continuous Filament Carbon and GraphiteFiber Tows1This standard is issued under the fixed designation D 4018; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revi
2、sion, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript 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. Scope1.1 These test methods
3、 cover the preparation and tensiletesting of resin-impregnated and consolidated test specimensmade from continuous filament carbon and graphite yarns,rovings, and tows to determine their tensile properties.1.2 These test methods also cover the determination of thedensity and mass per unit length of
4、the yarn, roving, or tow toprovide supplementary data for tensile property calculation.1.3 These test methods include a procedure for sizingremoval to provide the preferred desized fiber samples fordensity measurement. This procedure may also be used todetermine the weight percent sizing.1.4 These t
5、est methods include a procedure for determiningthe weight percent moisture adsorption of carbon or graphitefiber.1.5 The values stated in SI units are to be regarded as thestandard. The values in parentheses are for information only.1.6 This standard does not purport to address all of thesafety conc
6、erns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 70 Test Method for Specific Gravity a
7、nd Density ofSemi-Solid Bituminous Materials (Pycnometer Method)D 123 Terminology Relating to TextilesD 891 Test Methods for Specific Gravity, Apparent, ofLiquid Industrial ChemicalsD 1193 Specification for Reagent WaterD 3800 Test Method for Density of High-Modulus FibersD 3878 Terminology for Comp
8、osite MaterialsD 5550 Test Methods for Specific Gravity of Soil Solids byGas PycnometerE 4 Practices for Force Verification of Testing MachinesE 6 Terminology Relating to Methods of Mechanical Test-ingE 83 Practice for Verification and Classification of Exten-sometersE 100 Specification for ASTM Hyd
9、rometers2.2 Other Document:CRC Handbook of Chemistry and Physics33. Terminology3.1 Definition:3.1.1 sizing, na generic term for compounds which, whenapplied to yarn or fabric, form a more or less continuous solidfilm around the yarn and individual fibers.3.2 Definitions of Terms Specific to This Sta
10、ndard:3.2.1 desized fiber, nfiber which has had a sizing removedfrom it.3.2.2 fiber, ncontinuous filament carbon or graphite yarn,roving, or tow.3.2.3 sized fiber, na fiber with a sizing applied to it.3.2.4 unsized fiber, nfiber which has never had a sizingapplied to it.3.3 Symbols3.3.1 AUnit conver
11、sion factor for tensile strength3.3.2 BUnit conversion factor for tensile modulus3.3.3 Efiber chord modulus3.3.4 elLower strain limit3.3.5 euUpper strain limit3.3.6 kccorrection factor for density of size3.3.7 Lspecimen length3.3.8 MULthe mass per unit length of the sized fiber3.3.9 MULIthe mass per
12、 unit length of the impregnatedand consolidated fiber3.3.10 Pmaximum load3.3.11 Pltensile load at lower strain limit3.3.12 Putensile load at upper strain limit1These test methods are under the jurisdiction of ASTM Committee D30 onComposite Materials and are the direct responsibility of Subcommittee
13、D30.03 onConstitutuent/Precursor Properties.Current edition approved Oct. 1, 2004. Published October 2004. Originallyapproved in 1981. Last previous edition approved in 1999 as D 4018 99.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at servicea
14、stm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3CRC Press Inc., Boca Raton, Ann Arbor, London, Tokyo, 73rd Edition,19921993.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-29
15、59, United States.3.3.13 rfdensity of the fiber3.3.14 rsfdensity of the fiber with sizing3.3.15 RCweight percent of resin (resin content)3.3.16 W1specimen mass4. Summary of Test Methods4.1 These test methods include procedures for determiningthe tensile strength and modulus of a resin-impregnated an
16、dconsolidated carbon fiber tow. Also included are procedures tomeasure the mass per unit length and density of the carbonfiber and the resin content of the resin-impregnated andconsolidated specimens.4.2 MULThe MUL of the fiber is determined by dividingthe mass of a sample of sized fiber by its leng
17、th.4.3 DensityThe density of the fiber is determined usingArchimedes method or a pycnometer method. The recom-mended specimen is desized or unsized fiber. The idealimmersion fluid is one that completely wets the specimen andprovides minimum toxicity or environmental hazard.4.4 Resin ContentThe resin
18、 content (weight percent) ofthe resin-impregnated and consolidated fiber is determined bycomparing the mass per unit length of the impregnated andconsolidated specimen to the fiber mass per unit length.4.5 Tensile PropertiesThe tensile strength and tensilechord modulus of the fiber are determined by
19、 the tensileloading to failure of the resin-impregnated and consolidatedfiber. The chord modulus is determined between defined strainlimits. The purpose of the impregnating resin is to provide thefiber, when consolidated, with sufficient mechanical strength toproduce an easily handled test specimen
20、capable of sustaininguniform loading of the individual filaments in the specimen.The resin shall be compatible with the fiber and any sizeapplied to it. The strain capability of the consolidated resinshall be at least twice the strain capability of the fiber.5. Significance and Use5.1 The properties
21、 determined by these test methods are ofvalue in material specifications, qualifications, data base gen-eration, certification, research, and development.5.2 These test methods are intended for the testing of fibersthat have been specifically developed for use as reinforcingagents in advanced compos
22、ite structures. The test results of animpregnated and consolidated fiber should be representative ofthe strength and modulus that are available in the materialwhen used as intended. The performance of fibers in differentresin systems can vary significantly so that correlations be-tween results using
23、 these test methods and composite testingmay not always be obtained.5.3 The reproducibility of test results is dependent uponprecise control over all test conditions. Resin type, content anddistribution, curing process, filament alignment, gripping in thetesting machine, and alignment in the testing
24、 machine are ofspecial importance.5.4 The measured strengths of fibers are not unique quan-tities and test results are strongly dependent on the test methodsused. Therefore the test method described here will notnecessarily give the same mean strengths or standard devia-tions as those obtained from
25、single filaments, dry fibers,composite laminas, or composite laminates.6. Apparatus6.1 Three sets of apparatus are required. One set is for resinimpregnation of the fiber. A second set is for curing theresin-impregnated specimens. A third set is for tensile testingthe resin-impregnated and consolida
26、ted specimens. Optionalapparatus may be used for applying end tabs to the specimensand removing sizing.6.1.1 Resin ImpregnationThe goal of the resin-impregnation apparatus is to apply and uniformly impregnateresin into the fiber. This is normally achieved by dipping thefiber into the resin and then
27、working the wet fiber over rolls orthrough a die, or both. While automated apparatuses arepreferred for consistency, any apparatus which achieves uni-form impregnation of 35 to 60 % resin by weight and does notdamage the fiber is acceptable.6.1.2 ConsolidationAn apparatus to hold the impregnatedspec
28、imens under tension during consolidation is required.6.1.3 Optional End TabsAn apparatus to cast resin endtabs on specimens may be used. Apparatuses to apply and alignother forms of end tabs such as bonded on cardboard or metaltabs may also be used.6.1.4 TestingA tensile testing machine and recorder
29、 meet-ing the requirements of Practices E 4 at the maximum expectedtest load are required. The load recording device shall becoordinated with the extensometer and strain recorder to assurethat the corresponding load and elongation of the specimen arerecorded at essentially the same time. The testing
30、 machineshall also have the following features:6.1.4.1 GripsGrips suitable for loading the tabbed oruntabbed specimen without damaging it are required. For resintabbed specimens a custom grip is generally required. Foruntabbed or cardboard tabbed specimens pneumatic or hydrau-lically powered grips a
31、re typically used. Different grip pressuresettings may be required for different fibers.6.1.4.2 JawsJaws compatible with the grips and capableof holding a specimen without damaging it are required. Foruntabbed specimens, flat jaws with rubber or other compliantmaterials bonded to the face are genera
32、lly used. Sandpapermay also be placed on the grips to reduce slippage. Forcardboard tabbed specimens serrated jaws are generally used.Jaws should be inspected regularly and cleaned or repaired asrequired.6.1.4.3 Extensometer and RecorderAn extensometer andrecording device in accordance with the requ
33、irements ofPractice E 83 Class B-2 are required. The extensometer andrecorder shall be coordinated with the tensile testing machineso that the corresponding load and elongation of the specimenare recorded at essentially the same time.6.1.4.4 Balance, AnalyticalAccuracy of 60.0002 g formass per unit
34、length, density, and resin or size contentdeterminations.6.1.4.5 Balance, LaboratoryAccuracy of 60.1 g for mea-suring components of resin.6.1.4.6 Length Measuring DevicesDevices to measure thelength of impregnated and consolidated specimens and dryfiber to 62-mm accuracy are required.6.1.4.7 Density
35、 Measuring DeviceSee Test MethodsD 70, D 3800, or D 5550.D 4018 99 (2004)26.1.4.8 Forced Air OvenA forced air oven of sufficientsize and temperature capabilities to cure the impregnated fiberon the curing device. The temperature shall be controlled to610C.7. Reagents and Materials7.1 Reagent WaterUn
36、less otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Type III of Specification D 1193.7.2 Resin.7.3 Commercial Grade Solvent, (optional) for resin dilu-tion.7.4 Hardener or Catalyst.7.5 Surfactant (optional).8. Test Specimens8.1 Mass per Unit Length Spe
37、cimenThe specimen tomeasure mass per unit length is a 1-m minimum length of fiberin the form in which it is intended to be used. Test onespecimen per sample. Coil the specimen into a usable form fortesting. Care is required to not damage and lose filaments fromthe specimen.8.2 Density SpecimenDensit
38、y specimens may be sized,unsized, or desized material. Unsized or desized samples arepreferred. Test one specimen per sample. A 1-m minimumlength is required for Test Method D 3800. For methods in TestMethods D 70 and D 5550, a suitable volume to fill thecontainer is recommended. Coil the specimen i
39、nto a usableform for testing. Care is required to not damage and losefilaments from the specimen.8.3 Tensile Test SpecimenThe tensile specimen shall be atabbed or untabbed resin-impregnated and consolidated fiber.Tabbed specimens shall have a 150-mm gage length betweenthe tabs. Untabbed specimens sh
40、all be of sufficient length toallow a 150-mm gage length between the grips when they aretested. Samples with 3000 filaments or less may be tested usingspecimens of more than one fiber bundle to facilitate handling.Combine the bundles before resin impregnation and count thetest results as one specime
41、n. Test a minimum of four testspecimens per sample. Separate test specimens for modulusand strength determination are permitted; however, four speci-mens for each test are required. Specimens that are fuzzy,curved, not uniform in cross section, have broken filaments,resin lumps, or other observable
42、defects should be rejectedunless they are representative of the material being tested.9. Conditioning9.1 Fibers that adsorb less than 0.5 % moisture by weight at23 6 2C and 90 % or greater relative humidity require noconditioning before testing. Conduct mass per unit length,density, and tensile test
43、ing for these materials at 23 6 7C and50 6 20 % relative humidity unless other conditions are thevariables of interest.9.2 Condition fibers that adsorb more than 0.5 % moistureby weight (at 23 6 2C and 90 % or greater relative humidity)for a minimum of 24 h at 23 6 2C and 50 6 10 % relativehumidity.
44、 Conduct mass per unit length and density testing at23 6 2C and 50 6 10 % relative humidity unless otherconditions are the variables of interest. Conduct tensile testingat 23 6 7C and 50 6 20 % relative humidity unless otherconditions are the variables of interest.9.3 To determine moisture adsorptio
45、n, dry a minimum offive mass per unit-type specimens at 120 6 5C for 24 h in acirculating air oven. Cool samples in a desiccator. Removesamples from desiccator one at a time and immediately weighthem. Place samples in a humidity chamber and maintain at 236 2C and 90 % or greater relative humidity fo
46、r 24 h. Removesamples from the humidity chamber one at a time and weighimmediately.9.4 If all specimens are conditioned for 24 h and mass perunit length and density testing are performed at 23 6 2C and50 6 10 % relative humidity, then no testing for moistureadsorption is required.9.5 Moisture adsorp
47、tion testing is only required once annu-ally for a standard product.10. Specimen Preparation10.1 Mass per Unit LengthNo preparation is required.The sample is taken from a package of material as it is intendedto be used.10.2 DensityThe preferred density specimen is a desizedor unsized fiber. This eli
48、minates any need to correct for thedensity of the sizing. The sizing may be removed using solventextraction, pyrolysis, or other means. An example method isdescribed in Appendix X1. An unsized sample of a sized fiberwould have to be collected during the production of the fiberand is therefore not re
49、commended.10.3 Tensile TestThe tensile test specimen must be im-pregnated with resin and consolidated before testing.10.3.1 Resin PreparationAny resin that meets the re-quirements of 4.5 may be used. The resin when combined withthe fiber shall produce a composite (reinforcement/matrix)failure. A resin generally found satisfactory is a combination ofbisphenol A (or bisphenol F) epoxy and diethyltoluene diaminein the weight ratio of 3.9:1. A solvent that lowers the viscosityof a resin mixture or softens the sizing, or both, may b
