1、Designation: D 4018 99 (Reapproved 2008)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 () 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 t
4、he 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 te
5、st 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 conce
6、rns, 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:2D70 Test Method for Density of Semi-Soli
7、d BituminousMaterials (Pycnometer Method)D 1193 Specification for Reagent WaterD 3800 Test Method for Density of High-Modulus FibersD 5550 Test Method for Specific Gravity of Soil Solids byGas PycnometerE4 Practices for Force Verification of Testing MachinesE83 Practice for Verification and Classifi
8、cation of Exten-someter Systems2.2 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 Ter
9、ms Specific to This Standard: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 Sy
10、mbols3.3.1 AUnit conversion factor for tensile strength3.3.2 BUnit conversion factor for tensile modulus3.3.3 Efiber chord modulus3.3.4 lLower strain limit3.3.5 uUpper 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
11、.3.9 MULIthe mass per 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 limit3.3.13 rfdensity of the fiber3.3.14 rsfdensity of the fiber with sizing3.3.15 RCweight percent of resin (resin content)1
12、These test methods are under the jurisdiction of ASTM Committee D30 onComposite Materials and are the direct responsibility of Subcommittee D30.03 onConstituent/Precursor Properties.Current edition approved Nov. 1, 2008. Published December 2008. Originallyapproved in 1981. Last previous edition appr
13、oved in 2004 as D 4018 99(2004).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3CRC Press Inc., Boca Raton,
14、Ann Arbor, London, Tokyo, 73rd Edition,19921993.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.3.16 W1specimen mass4. Summary of Test Methods4.1 These test methods include procedures for determiningthe tensile strength and modulus
15、 of a resin-impregnated andconsolidated 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
16、of sized fiber by its length.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.
17、4.4 Resin ContentThe resin 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 t
18、he fiber are determined by 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 eas
19、ily handled test specimen 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
20、 and Use5.1 The properties 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 reinforcin
21、gagents in advanced composite 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 correlati
22、ons be-tween results using 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, an
23、d alignment in the testing 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-tio
24、ns as those obtained from 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
25、-impregnated and consolidated 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 thefibe
26、r into the resin and then 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 t
27、o hold the impregnatedspecimens 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 TestingAtensile test
28、ing machine and recorder meet-ing the requirements of Practices E4at 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
29、same time. The testing 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-l
30、ically powered grips are 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
31、to the face are generally 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 ac
32、cordance with the requirements ofPractice E83Class 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
33、 g formass per unit 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 requ
34、ired.6.1.4.7 Density Measuring DeviceSee Test MethodsD 70, D 3800,orD 5550.D 4018 99 (2008)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
35、.1 Reagent WaterUnless 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 p
36、er Unit Length SpecimenThe 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 Dens
37、ity SpecimenDensity 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 D70 and D 5550, a suitable volume to fill thecontainer is recommended. Co
38、il the specimen into 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. Unta
39、bbed specimens shall 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 resul
40、ts as one specimen. 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
41、other observable 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,
42、 and tensile testing 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 %
43、relativehumidity. 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 m
44、oisture adsorption, 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 rel
45、ative humidity for 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.
46、5 Moisture adsorption 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 unsize
47、d fiber. This eliminates 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
48、 therefore not recommended.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/matr
49、ix)failure.Aresin generally found satisfactory is a combination ofbisphenolA(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 beselected for use with the resin. The amount and type of solventused will vary with the product and apparatus used forimpregnation. Prepare and store the resin in accordance withthe manufacturers instructions.10.3.2 Fiber ImpregnationThe resin shall be maintainedwithin a suitable v
