1、Designation: D3222 05 (Reapproved 2010)Standard Specification forUnmodified Poly(Vinylidene Fluoride) (PVDF) MoldingExtrusion and Coating Materials1This standard is issued under the fixed designation D3222; the number immediately following the designation indicates the year oforiginal adoption or, i
2、n the case of revision, 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 T
3、his specification 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
4、This specification 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 unmodif
5、ied PVDF homopolymer 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 occu
6、r under certain conditions.)1.5 The values stated in SI units, as detailed in IEEE/ASTMS-10, are to be regarded as the standard. The values given inparentheses are for information only.NOTE 1PVDF exhibits polymorphism.2The type and extent ofcrystalline structure varies with the thermomechanical hist
7、ory of thesample. Specimens 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 t
8、his standard to establish 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
9、 technically equivalent to relatedinformation in ISO 12086-1 and ISO 12086-2.2. Referenced Documents2.1 ASTM Standards:3D149 Test Method for Dielectric Breakdown Voltage andDielectric Strength of Solid Electrical Insulating Materialsat Commercial Power FrequenciesD150 Test Methods for AC Loss Charac
10、teristics and Per-mittivity (Dielectric Constant) of Solid Electrical Insula-tionD256 Test Methods for Determining the Izod PendulumImpact Resistance of PlasticsD257 Test Methods for DC Resistance or Conductance ofInsulating MaterialsD542 Test Method for Index of Refraction of TransparentOrganic Pla
11、sticsD618 Practice for Conditioning Plastics for TestingD638 Test Method for Tensile Properties of PlasticsD790 Test Methods for Flexural Properties of Unreinforcedand Reinforced Plastics and Electrical Insulating MaterialsD792 Test Methods for Density and Specific Gravity (Rela-tive Density) of Pla
12、stics by DisplacementD883 Terminology Relating to PlasticsD1238 Test Method for Melt Flow Rates of Thermoplasticsby Extrusion PlastometerD2863 Test Method for Measuring the Minimum OxygenConcentration to Support Candle-Like Combustion ofPlastics (Oxygen Index)D3418 Test Method for Transition Tempera
13、tures and En-thalpies of Fusion and Crystallization of Polymers byDifferential Scanning CalorimetryD3835 Test Method for Determination of Properties ofPolymeric Materials by Means of a Capillary RheometerD3892 Practice for Packaging/Packing of Plastics1This specification is under the jurisdiction of
14、 ASTM Committee D20 onPlastics and is the direct responsibility of Subcommittee D20.15 on ThermoplasticMaterials.Current edition approved Nov. 1, 2010. Published March 2011. Originallyapproved in 1973. Last previous edition approved in 2005 as D3222 - 05. DOI:10.1520/D3222-05R10.2Lovinger, A. J., “P
15、oly(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 Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume informa
16、tion, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.IEEE/ASTM S-10 Use of the International System of Units(SI): The Modern Metric System2.2 IEC and ISO Standards:ISO
17、12086-1 PlasticsFluoropolymer Dispersion andMoulding 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
18、:3.1.1 For definitions of plastics terms used in this specifi-cation, see Terminology D883.3.1.2 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
19、moldingand extrusion, 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 isolate
20、d from theemulsion 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 thisdiffere
21、nce is the basis 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
22、 these resins rangefrom 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
23、 system uses predefined cells to refer to specificaspects of this specification, as illustrated below.SpecificationStandard Number Block Type Grade ClassSpecialNotesExample: SpecificationD3222 05 I 2 . .For this example (D3222 05, I2), the line callout describesa PVDF resin polymerized in emulsion,
24、having a specificgravity 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, su
25、ch as apreferred 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:4Available from American Nation
26、al Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.5Dohany, J. E., and Robb, L. E., “Poly(Vinylidene Fluoride)” Kirk-OthmerEncyclopedia of Chemical Technology, Vol 11, 3rd Edition, 1980, pp. 6474.6See the ASTM Form and Style for ASTM Standards, available
27、from ASTMHeadquarters.TABLE 1 Classification of PVDF ResinsPropertyTypical Values or RangesType I Type IIGrade 1 Grade 2Specific Gravity Gms/cc 1.75-1.79 1.75-1.79 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 Viscosit
28、y 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 2500-4000Medium Viscosity 2300-2800 1300-2800 1300-2500Low Viscosity . 350-1300 250-1300Note: For measuring MFR values of PVDF, the load must be selected
29、 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 232C (450F) using 0.027 radian (60) entrance angle die with L/D of 15 and in accordancewith procedures of Test Method D3835. Multiply the pa
30、scal second values by ten to obtain poise values.D3222 05 (2010)26.1.1 Peak Melting EndothermThe material covered bythis specification shall have a minimum peak melting endot-herm for the type and class as shown in Table 1 when tested inaccordance with Test Method D3418. For Type I resins, thisshall
31、 involve heating a solid specimen of 5 6 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
32、.1.1.1 TemperatureTest Type II resins likewise 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 wi
33、th Test MethodD792.NOTE 3Test attached to 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 refra
34、ctive index of 1.42 when measured atthe sodium D line at 25C (77F) in accordance with therefractometer procedure in Test Methods D542, 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
35、-mm (0.079-in.)thick that have been quenched 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 D2863.NOTE 4If a column with a restricted opening is used, posit
36、ion the topof the specimen 40 mm below the 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 D1238 using loads shown in parentheses in Table 1.6.2.2 Rheological PropertiesThe apparent me
37、lt viscosityof these materials shall be tested in accordance with TestMethod D3835 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
38、shall have a tensile yield strength exceeding 36MPa (5200 psi) at 23C (74F) and a minimum elongation atbreak of 10 % when tested in accordance with Test MethodD638 at 51 mm (2 in.)/min, using Type I specimens 3.2-mm(0.125-in.) thick as specified in Test Method D638. Preferably,compression-molded sam
39、ples are used (see Section 8), butinjection molded 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 elon
40、gation values compared tocompression-molded specimens. 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
41、 modulus of 1.38GPa (190 3 103psi) when tested in accordance with Method Iof Test Methods D790, 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 t
42、he 16-hconditioning period.6.3.3 Impact ResistanceType I material covered in thisspecification shall have a minimum impact strength of 80.0 J/m(1.50 ftlbf/in.) determined by Test Methods D256 using6.4-mm (0.25-in.) thick specimens prepared by injection mold-ing under conditions specified by the manu
43、facturer. Alterna-tively, specimens are compression-molded 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 gre
44、ater than 1.2Vm(1.2 3 1014Vcm) when tested as a 0.76-mm (0.030-in.)compression-molded specimen (see Section 8) in accordancewith Test Methods D257.6.4.2 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
45、 “short-time” method ofTest Methods D149 with 0.13-mm (0.05-in.) 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 grea
46、ter than 5.8 at 1 MHz when tested as a 3.2-mm(0.125-in.) thick compression-molded specimen (see Section 8)in accordance with Test Methods D150 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
47、 at 1 MHz when tested as 3.2-mm(0.125-in.) compression-molded specimens (see Section 8)inaccordance with Test Methods D150 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 ex
48、cept as required for a specific test method.However, no moisture shall 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 sat
49、isfy therequirements of 12.4.8. Preparation of Compression Molded Specimens8.1 Equipment:8.1.1 Press with approximately 180 kN (20 ton) capacityand heating capability for maintaining platens between 220 and240C (428 to 464F).D3222 05 (2010)38.1.2 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 mm(6 by 6 by 0.02 in.).8.1.3 Flat open-cavity steel molds, that is, frames, to pro-vide the shape
