1、Designation: D3222 18aStandard 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, in the case of rev
2、ision, 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 U.S. Department of Defense.1. Scope*1.1 This specifi
3、cation 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 specif
4、ication applies only to the virgin homopoly-mer prepared from vinylidene fluoride, not copolymers,reinforced, 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 homo
5、polymer 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 certa
6、in 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 history of thesam
7、ple. 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 this standard
8、to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.Specific precautionary statements are given in Section 10.NOTE 2There is no equivalent ISO standard for this specification.Information in this specification i
9、s technically equivalent to relatedinformation in ISO 12086-1 and ISO 12086-2.1.7 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides an
10、d Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:3D149 Test Method for Dielectric Breakdown Voltage andDielectric Strength of Solid Electrical Insulating Materialsat Commercial Power FrequenciesD150 Test Me
11、thods for AC Loss Characteristics and Permit-tivity (Dielectric Constant) of Solid Electrical InsulationD256 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
12、 TransparentOrganic PlasticsD618 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 Materi-alsD792 Test Methods for Density and Specific Gravity (R
13、ela-tive Density) of Plastics 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)1This specificat
14、ion is under the jurisdiction of ASTM Committee D20 onPlastics and is the direct responsibility of Subcommittee D20.15 on ThermoplasticMaterials.Current edition approved Aug. 1, 2018. Published August 2018. Originallyapproved in 1973. Last previous edition approved in 2018 as D3222 - 18. DOI:10.1520
15、/D3222-18A.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 Customer Service at serviceastm.org. For Annual Book
16、of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international st
17、andard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1D34
18、18 Test Method for Transition Temperatures 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 PlasticsIEEE/ASTM S
19、-10 Use of the International System of Units(SI): The Modern Metric System2.2 IEC and ISO Standards:ISO 12086-1 PlasticsFluoropolymer Dispersion andMoulding and Extrusion MaterialsPart 1: Designationand Basis for Specification4ISO 12086-2 PlasticsFluoropolymer Dispersion andMolding and Extrusion Mat
20、erialsPart 2: Preparation ofTest Specimens and Determination of Properties43. Terminology3.1 Definitions:3.1.1 For definitions of plastics terms used in thisspecification, see Terminology D883.3.1.2 lot, none production run or a uniform blend of twoor more production runs.4. Classification4.1 This s
21、pecification covers two types5of natural, unmodi-fied PVDF fluoroplastics supplied in pellet form for moldingand extrusion, and in powder form for solutions, dispersions, orcoatings.4.1.1 Type IPVDF fluoroplastics are polymerized in emul-sion. Depending upon the polymerization conditions, the peakme
22、lting point of the resin can be varied between 156 and172C. The diameter of the primary particle isolated 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 comm
23、ercially. These are differentiated bypeak melting endotherm values, as shown in Table 1, and thisdifference 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 p
24、urposes only.4.1.2 Type IIPVDF fluoroplastics are polymerized in sus-pension. Peak melting temperatures of these resins range from164 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 t
25、hedata of Table 1 reflect ranges encompassing values typical forthe properties of available grades.4.2 The system uses predefined cells to refer to specificaspects of this specification, as illustrated below.SpecificationStandard Number Block Type Grade ClassSpecialNotesExample: SpecificationD3222 I
26、 2 . .For this example (D3222, I2), the line callout describes aPVDF resin polymerized in emulsion, having a specific gravitybetween 1.75 and 1.79, and a peak melting endotherm between162 to 172C. A comma is used as the separator between theStandard Number and the Type. Separators are not neededbetw
27、een the Type, Grade, and Class.6Provision for SpecialNotes is included so that other information, such as a preferredviscosity range, can be provided when required. When specialnotes are used, they shall be preceded by a comma.4Available from American National Standards Institute (ANSI), 25 W. 43rd
28、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 from ASTMHeadquarters.TABLE 1 Classificati
29、on 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 156-162 162-172 164-180Melt Flow Rate g/10 min (wt in Kg)Ultra High Viscosity . . 0.5-10AHigh Viscosity 0.5-8A5-8B0.5-10CMedium Viscosity 4-18A5
30、-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 . 250-1300 250-1300Note: For measuring MFR values of PVDF, the load must be selected based on the viscosity as follows:A= 21.6
31、 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 pascal second values by ten to obtain poise
32、values.D3222 18a25. 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 covered bythis specification shall have a minimum peak melting endo-therm for the type and class as
33、 shown in Table 1 when testedin accordance with Test Method D3418. For Type I resins, thisshall 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
34、reheating at 10C/min to200C. Record the peak melting endotherm during the secondmelting cycle.6.1.1.1 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 specific gravityindicated in
35、 Table 1 when tested in accordance with TestMethod D792.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 t
36、his speci-fication shall have a refractive 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.Co
37、mpression-molded specimens at least 2-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 wit
38、h a restricted opening is used, position 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
39、Rheological PropertiesThe apparent melt 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 m
40、aterial covered in thisspecification 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 D6
41、38. Preferably,compression-molded samples 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 molde
42、d specimensshow low and variable elongation 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 thisspecif
43、ication shall have a minimum flexural modulus of 1.31GPa (190 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
44、 (see Section 8) and tested after the 16-hconditioning period.6.3.3 Impact ResistanceType I material of medium orhigh viscosity shall have a minimum impact strength of 80.0J/m (1.50 ftlbf/in.). Type I material of low viscosity shall havea minimum impact strength of 40.0 J/m (0.75 ft-lbf/in.). Theimp
45、act strength shall be determined by Test Methods D256using 6.4-mm (0.25-in.) thick specimens prepared by injectionmolding under conditions specified by the manufacturer.Alternatively, specimens are compression-molded and testedafter the conditioning period as specified above. For Type IImaterial, im
46、pact 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 1.2m(1.2 1014cm) when tested as a 0.76-mm (0.030-in.)compression-molded specimen (see Section 8) in accordancewith Test Methods D257
47、.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 D149 with 0.13-mm (0.05-in.) thickcompression-molded specimens (see Section 8) tested in airusing 25.4-mm (1-i
48、n.) 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-mm(0.125-in.) thick compression-molded specimen (see Section 8)in accordance with Test Methods D150 at
49、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-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-absorptioncharacteristics, maintenance of constant humidity during testing or speci-men preparation is not necessary except as required for a specific testmethod. However, no moist
