1、Designation: D 3222 05Standard Specification forUnmodified Poly(Vinylidene Fluoride) (PVDF) MoldingExtrusion and Coating Materials1This standard is issued under the fixed designation D 3222; the number immediately following the designation indicates the year oforiginal adoption or, in the case of re
2、vision, 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. Scope*1.1 This specificat
3、ion covers melt processable molding andextrusion materials, as well as coating materials of poly(vi-nylidene fluoride) fluoroplastic, commonly abbreviated PVDF(or PVF2in scientific literature). This specification coversthermoplastic resin materials supplied in pellet or powderform.1.2 This specifica
4、tion applies only to the virgin homopoly-mer prepared from vinylidene fluoride, not copolymers, rein-forced, filled grades or special grades with additives ortreatments for modification of attributes.1.3 The tests involved are intended to provide informationfor specification of unmodified PVDF homop
5、olymer resins. Itis not the purpose of this specification to provide engineeringdata for design purposes.1.4 PVDF fluoroplastics melt between 156 and 180C 312and 356F and are thermally stable up to about 370C 698F.(WarningEvolution of corrosive and toxic hydrogen fluo-ride can occur under certain co
6、nditions.)1.5 The values stated in SI units, as detailed in IEEE/SI-10,are to be regarded as the standard. The values given in bracketsare for information only.NOTE 1PVDF exhibits polymorphism.2The type and extent ofcrystalline structure varies with the thermomechanical history of thesample. Specime
7、ns prepared by techniques different than prescribed inthis specification can have properties that vary from the values specified.1.6 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish
8、 appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific precau-tionary statements are given in Section 10.NOTE 2There is no equivalent ISO standard for this specification.Information in this specification is technically equivalent t
9、o relatedinformation in ISO 12086-1 and ISO 12086-2.2. Referenced Documents2.1 ASTM Standards:3D 149 Test Method for Dielectric Breakdown Voltage andDielectric Strength of Solid Electrical Insulating Materialsat Commercial Power FrequenciesD 150 Test Methods for A-C Loss Characteristics andPermittiv
10、ity (Dielectric Constant) of Solid Electrical Insu-lating MaterialsD 256 Test Methods for Impact Resistance of Plastics andElectrical Insulating MaterialsD 257 Test Methods for D-C Resistance or Conductance ofInsulating MaterialsD 542 Test Methods for Index of Refraction of TransparentOrganic Plasti
11、csD 618 Practice for Conditioning Plastics for TestingD 638 Test Method for Tensile Properties of PlasticsD 790 Test Methods for Flexural Properties of Unreinforcedand Reinforced Plastics and Electrical Insulating MaterialsD 792 Test Methods for Density and Specific Gravity (Rela-tive Density) of Pl
12、astics by DisplacementD 883 Terminology Relating to PlasticsD 1238 Test Method for Flow Rates of Thermoplastics byExtrusion PlastometerD 2863 Test Method for Measuring the Minimum OxygenConcentration to Support Candle-like Combustion of Plas-tics (Oxygen Index)D 3418 Test Method for Transition Tempe
13、ratures of Poly-mers by Thermal AnalysisD 3835 Test Method for Determination of Properties ofPolymeric Materials by Means of a Capillary RheometerD 3892 Practice for Packaging/Packing of PlasticsIEEE/ASTM S-10 Use of the International System of Units(SI): The Modern Metric System2.2 IEC and ISO Stan
14、dards:ISO 12086-1 PlasticsFluoropolymer Dispersion and1This specification is under the jurisdiction of ASTM Committee D20 onPlastics and is the direct responsibility of Subcommittee D20.15 on ThermoplasticMaterials.Current edition approved July 1, 2005. Published July 2005. Originally approvedin 197
15、3. Last previous edition approved in 1999 as D 3222 - 99.2Lovinger, A. J., “Poly(Vinylidene Fluoride)” Developments in CrystallinePolymers, Vol 1, Chapter 5, D. C. Bassett, Ed., Applied Science, London, 1982.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Custome
16、r Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, P
17、A 19428-2959, United States.Moulding and Extrusion MaterialsPart 1: Designationand Basis for Specification4ISO 12086-2 PlasticsFluoropolymer Dispersion andMolding and Extrusion MaterialsPart 2: Preparation ofTest Specimens and Determination of Properties43. Terminology3.1 Definitions:3.1.1 For defin
18、itions of plastics terms used in this specifi-cation, see Terminology D 883.3.1.2 lot, none production run or a uniform blend of twoor more production runs.4. Classification4.1 This specification covers two types5of natural, unmodi-fied PVDF fluoroplastics supplied in pellet form for moldingand extr
19、usion, and in powder form for solutions, dispersions, orcoatings.4.1.1 Type IPVDF fluoroplastics are polymerized inemulsion. Depending upon the polymerization conditions, thepeak melting point of the resin can be varied between 156 and170C. The diameter of the primary particle isolated from theemuls
20、ion is typically less than 1 m; the dried powder has anaverage agglomerate diameter range of 3 to 15 m.4.1.1.1 Two distinctly different Type I emulsion PVDFresins are available commercially. These are differentiated bypeak melting endotherm values, as shown in Table 1, and thisdifference is the basi
21、s for subdividing Type I resins into Grades1 and 2. Table 1 shows the melt viscosity ranges encompassingresin grades available from several sources and are providedfor information purposes only.4.1.2 Type IIPVDF fluoroplastics are polymerized insuspension. Peak melting temperatures of these resins r
22、angefrom 164 to 180C. The particles isolated from suspension arespherical and range typically from 20 to 150 m in diameter.4.1.2.1 Type II resins are available commercially, and thedata of Table 1 reflect ranges encompassing values typical forthe properties of available grades.4.2 The system uses pr
23、edefined cells to refer to specificaspects of this specification, as illustrated below.SpecificationStandard Number Block Type Grade ClassSpecialNotesExample: SpecificationD 3222 05 I 2 . .For this example (D 3222 05, I2), the line callout describesa PVDF resin polymerized in emulsion, having a spec
24、ificgravity between 1.75 and 1.79, and a peak melting endothermbetween 162 to 170C. A comma is used as the separatorbetween the Standard Number and the Type. Separators are notneeded between the Type, Grade, and Class.6Provision forSpecial Notes is included so that other information, such as aprefer
25、red viscosity range, can be provided when required.When special notes are used, they shall be preceded by acomma.5. General Requirements5.1 The material shall be of uniform composition and free offoreign matter.6. Detail Requirements6.1 General Attributes:6.1.1 Peak Melting EndothermThe material cov
26、ered bythis specification shall have a minimum peak melting endot-herm for the type and class as shown in Table 1 when tested in4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.5Dohany, J. E., and Robb, L. E., “Poly(Vinylidene Fluoride)” Kirk
27、-OthmerEncyclopedia of Chemical Technology, Vol 11, 3rd Edition, 1980, pp. 6474.6See the ASTM Form and Style for ASTM Standards, available from ASTMHeadquarters.TABLE 1 Classification of PVDF ResinsPropertyTypical Values or RangesType I Type IIGrade 1 Grade 2Specific Gravity Gms/cc 1.75-1.79 1.75-1.
28、79 1.76-1.79Peak Melting Endotherm C 156-162 162-170 164-180Melt Flow Rate g/10 min (wt in Kg)Ultra High Viscosity . . 0.5-10AHigh Viscosity 0.5-8A5-8B0.5-10CMedium Viscosity 4-18A5-36B0.5-30DLow Viscosity . 3.5-45E0.5-60FApparent Melt Viscosity Pas:GHigh Viscosity 2800-3800 2800-3700 2500-4000Mediu
29、m Viscosity 2300-2800 1300-2800 1300-2500Low Viscosity . 350-1300 250-1300Note: For measuring MFR values of PVDF, the load must be selected based on the viscosity as follows:A= 21.6 KgB= 12.5 KgC= 10.0 KgD=5KgE=3.8KgF= 2.16 KgGReported for a shear rate of 100 s1determined by capillary rheometry at 2
30、32C 450F using 0.027 radian (60) entrance angle die with L/D of 15 and in accordancewith procedures of Test Method D 3835. Multiply the pascal second values by ten to obtain poise values.D3222052accordance with Test Method D 3418. For Type I resins, thisshall involve heating a solid specimen of 5 6
31、1 mg from roomtemperature to 200C at 10C/min, maintaining the tempera-ture at 200C for 5 min, followed by cooling at a controlledrate of 10C/min to about 30C, then reheating at 10C/min to200C. Record the peak melting endotherm during the secondmelting cycle.6.1.1.1 TemperatureTest Type II resins lik
32、ewise exceptthat the maximum is 250C.6.1.2 Specific GravityA solid specimen of the materialcovered by this specification shall have the minimum specificgravity indicated in Table 1 (1.75 for Type I, Class 1 and 1.76for all others) when tested in accordance with Test MethodD 792.NOTE 3Test attached t
33、o the specimen upon immersion. Dipping thespecimens in a very dilute solution (less than 0.1 weight percent) of anammonium perfluorooctanoate surfactant minimizes this problem.6.1.3 Refractive IndexThe material covered in this speci-fication shall have a refractive index of 1.42 when measured atthe
34、sodium D line at 25C 77F in accordance with therefractometer procedure in Test Methods D 542, using speci-mens that have not been subjected to any processes whichinduce orientation of the polymer chains or crystal-lites.Compression-molded specimens at least 2-mm 0.079-in.thick that have been quenche
35、d rapidly in water are preferred.6.1.4 Limiting Oxygen IndexThe material covered in thisspecification shall have a minimum limiting oxygen index of42 when tested in accordance with Test Method D 2863.NOTE 4If a column with a restricted opening is used, position the topof the specimen 40 mm below the
36、 opening.6.2 Processing Related Attributes:6.2.1 Flow RateMaterials conforming to this specificationshall be tested for melt flow rate in accordance with TestMethod D 1238 using loads shown in parentheses in Table 1.6.2.2 Rheological PropertiesThe apparent melt viscosityof these materials shall be t
37、ested in accordance with TestMethod D 3835 at 231 6 1C 450F using a die with anentrance angle of 60 (cone angle of 120) and a minimumcapillary L/D of 15. See Table 1.6.3 Mechanical Properties:6.3.1 Tensile PropertiesThe material covered in thisspecification shall have a tensile yield strength exceed
38、ing 36MPa 5200 psi at 23C 74F and a minimum elongation atbreak of 10 % when tested in accordance with Test MethodD 638 at 51 mm 2 in./min, using Type I specimens 3.2-mm0.125-in. thick as specified in Test Method D 638. Preferably,compression-molded samples are used (see Section 8), butinjection mold
39、ed specimens also are used, providing that thesamples yield and rupture in the gage region and not near theheel. Specimens shall be molded under conditions specified bythe resin suppliers. Generally, injection molded specimensshow low and variable elongation values compared tocompression-molded spec
40、imens. Typically, the melt tempera-ture is 30 to 60C higher than the upper peak meltingendotherm value depending on the grade. Mold temperature is120 6 10F.6.3.2 Flexural PropertiesThe material covered in thisspecification shall have a minimum flexural modulus of 1.38GPa 190 3 103psi when tested in
41、accordance with Method Iof Test Methods D 790, using 6.4-mm 0.25-in. thick speci-mens prepared by injection molding under conditions specifiedby the resin supplier. Alternatively, compression-moldedsamples are used (see Section 8) and tested after the 16-hconditioning period.6.3.3 Impact ResistanceT
42、ype I material covered in thisspecification shall have a minimum impact strength of 80.0 J/m1.50 ftlbf/in. determined by Test Methods D 256 using6.4-mm 0.25-in. thick specimens prepared by injection mold-ing under conditions specified by the manufacturer. Alterna-tively, specimens are compression-mo
43、lded and tested after theconditioning period as specified above. For Type II material,impact testing is not required.6.4 Electrical Properties:6.4.1 D-C ResistanceThe material covered in this speci-fication shall have a d-c volume resistivity greater than 1.2Vm(1.2 3 1014Vcm) when tested as a 0.76-m
44、m 0.030-pression-molded specimen (see Section 8) in accordancewith Test Methods D 257.6.4.2 Dielectric StrengthThe material covered in thisspecification shall have a dielectric strength in air no less than57 kV/mm (1280 V/0.001 in.) by the “short-time” method ofTest Methods D 149 with 0.13-mm 0.05-i
45、n. thickcompression-molded specimens (see Section 8) tested in airusing 25.4-mm 1-in. Type 3 electrodes.6.4.3 Dielectric ConstantThe material covered in thisspecification shall have a dielectric constant less than 11.0 at100 Hz and greater than 5.8 at 1 MHz when tested as a 3.2-mm0.125-in. thick com
46、pression-molded specimen (see Section 8)in accordance with Test Methods D 150 at 23C 73F.6.4.4 Dissipation FactorThe material covered in thisspecification shall have a dissipation factor of less than 0.045at 100 Hz and less than 0.24 at 1 MHz when tested as 3.2-mm0.125-in. compression-molded specime
47、ns (see Section 8)inaccordance with Test Methods D 150 at 23C 73F.NOTE 5Since this material has very low water-absorption character-istics, maintenance of constant humidity during testing or specimenpreparation is not necessary except as required for a specific test method.However, no moisture shall
48、 be present in the resin when preparingspecimens for testing. Heat the resin sample at 110C 230F in anair-circulating oven until the adventitious moisture is removed.7. Sampling7.1 Sampling shall be statistically adequate to satisfy therequirements of 12.4.8. Preparation of Compression Molded Specim
49、ens8.1 Equipment:8.1.1 Press with approximately 180 kN 20 ton capacityand heating capability for maintaining platens between 220 and240C 428 to 464F.8.1.2 Two smooth chromium-finished plates with approxi-mate dimensions 150 by 250 by 5 mm 10 by 10 by 0.02 in.,or, if more appropriate to the press type, 150 by 150 by 5 mm6 by 6 by 0.02 in.D32220538.1.3 Flat open-cavity steel molds, that is, frames, to pro-vide the shape and thicknesses requisite for the
