ASTM D3222-2018 Standard Specification for Unmodified Poly(Vinylidene Fluoride) (PVDF) Molding Extrusion and Coating Materials.pdf

1、Designation: D3222 05 (Reapproved 2015)D3222 18Standard 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 adopti

2、on or, in 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 U.S. Department of Defense.

3、1. Scope Scope*1.1 This specification covers melt processable molding and extrusion materials, as well as coating materials of poly(vinylidenefluoride) fluoroplastic, commonly abbreviated PVDF (or PVF2 in scientific literature). This specification covers thermoplastic resinmaterials supplied in pell

4、et or powder form.1.2 This specification applies only to the virgin homopolymer prepared from vinylidene fluoride, not copolymers, reinforced,filled grades or special grades with additives or treatments for modification of attributes.1.3 The tests involved are intended to provide information for spe

5、cification of unmodified PVDF homopolymer resins. It is notthe purpose of this specification to provide engineering data for design purposes.1.4 PVDF fluoroplastics melt between 156 and 180C (312 and 356F) and are thermally stable up to about 370C (698F).(WarningEvolution of corrosive and toxic hydr

6、ogen fluoride can occur under certain conditions.)1.5 The values stated in SI units, as detailed in IEEE/ASTM S-10, are to be regarded as the standard. The values given inparentheses are for information only.NOTE 1PVDF exhibits polymorphism.2 The type and extent of crystalline structure varies with

7、the thermomechanical history of the sample.Specimens prepared by techniques different than prescribed in this specification can have properties that vary from the values specified.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the res

8、ponsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 10.NOTE 2There is no equivalent ISO standard for thi

9、s specification. Information in this specification is technically equivalent to related informationin ISO 12086-1 and ISO 12086-2.1.7 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the

10、 Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:3D149 Test Method for Dielectric Breakdown Voltage and Dielectric Strength of Solid Electrical Insulating Ma

11、terials atCommercial Power FrequenciesD150 Test Methods for AC Loss Characteristics and Permittivity (Dielectric Constant) of Solid Electrical InsulationD256 Test Methods for Determining the Izod Pendulum Impact Resistance of PlasticsD257 Test Methods for DC Resistance or Conductance of Insulating M

12、aterialsD542 Test Method for Index of Refraction of Transparent Organic PlasticsD618 Practice for Conditioning Plastics for TestingD638 Test Method for Tensile Properties of Plastics1 This specification is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of S

13、ubcommittee D20.15 on Thermoplastic Materials.Current edition approved May 1, 2015May 1, 2018. Published June 2015May 2018. Originally approved in 1973. Last previous edition approved in 20102015 asD3222 - 05(2010).(2015). DOI: 10.1520/D3222-05R15.10.1520/D3222-18.2 Lovinger, A. J., “Poly(Vinylidene

14、 Fluoride)” Developments in Crystalline Polymers, Vol 1, Chapter 5, D. C. Bassett, Ed., Applied Science, London, 1982.3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to

15、 the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes

16、 accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr H

17、arbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1D790 Test Methods for Flexural Properties of Unreinforced and Reinforced Plastics and Electrical Insulating MaterialsD792 Test Methods for Density and Specific Gravity (Relative Density) of Plastics by DisplacementD883 Termino

18、logy Relating to PlasticsD1238 Test Method for Melt Flow Rates of Thermoplastics by Extrusion PlastometerD2863 Test Method for Measuring the Minimum Oxygen Concentration to Support Candle-Like Combustion of Plastics(Oxygen Index)D3418 Test Method for Transition Temperatures and Enthalpies of Fusion

19、and Crystallization of Polymers by DifferentialScanning CalorimetryD3835 Test Method for Determination of Properties of Polymeric Materials by Means of a Capillary RheometerD3892 Practice for Packaging/Packing of PlasticsIEEE/ASTM S-10 Use of the International System of Units (SI): The Modern Metric

20、 System2.2 IEC and ISO Standards:ISO 12086-1 PlasticsFluoropolymer Dispersion and Moulding and Extrusion MaterialsPart 1: Designation and Basis forSpecification4ISO 12086-2 PlasticsFluoropolymer Dispersion and Molding and Extrusion MaterialsPart 2: Preparation of TestSpecimens and Determination of P

21、roperties43. Terminology3.1 Definitions:3.1.1 For definitions of plastics terms used in this specification, see Terminology D883.3.1.2 lot, none production run or a uniform blend of two or more production runs.4. Classification4.1 This specification covers two types5 of natural, unmodified PVDF fluo

22、roplastics supplied in pellet form for molding andextrusion, and in powder form for solutions, dispersions, or coatings.4.1.1 Type IPVDF fluoroplastics are polymerized in emulsion. Depending upon the polymerization conditions, the peakmelting point of the resin can be varied between 156 and 170C.172

23、C. The diameter of the primary particle isolated from theemulsion is typically less than 1 m; the dried powder has an average agglomerate diameter range of 3 to 15 m.4.1.1.1 Two distinctly different Type I emulsion PVDF resins are available commercially. These are differentiated by peakmelting endot

24、herm values, as shown in Table 1, and this difference is the basis for subdividing Type I resins into Grades 1 and2. Table 1 shows the melt viscosity ranges encompassing resin grades available from several sources and are provided forinformation purposes only.4 Available from American National Stand

25、ards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.5 Dohany, J. E., and Robb, L. E., “Poly(Vinylidene Fluoride)” Kirk-Othmer Encyclopedia of Chemical Technology, Vol 11, 3rd Edition, 1980, pp. 6474.TABLE 1 Classification of PVDF ResinsPropertyTypical Values or R

26、angesType I Type IIGrade 1 Grade 2Specific Gravity Gms/cc 1.75-1.79 1.75-1.79 1.76-1.79Peak Melting Endotherm C 156-162 162-170 164-180Peak Melting Endotherm C 156-162 162-172 164-180Melt Flow Rate g/10 min (wt in Kg)Ultra High Viscosity . . 0.5-10AHigh Viscosity 0.5-8A 5-8B 0.5-10CMedium Viscosity

27、4-18A 5-36B 0.5-30DLow Viscosity . 3.5-45E 0.5-60FApparent 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 based on the viscosity as follow

28、s:A= 21.6 KgB= 12.5 KgC= 10.0 KgD= 5 KgE= 3.8 KgF= 2.16 KgG Reported for a shear rate of 100 s1 determined 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 t

29、o obtain poise values.D3222 1824.1.2 Type IIPVDF fluoroplastics are polymerized in suspension. Peak melting temperatures of these resins range from 164to 180C. The particles isolated from suspension are spherical and range typically from 20 to 150 m in diameter.4.1.2.1 Type II resins are available c

30、ommercially, and the data of Table 1 reflect ranges encompassing values typical for theproperties of available grades.4.2 The system uses predefined cells to refer to specific aspects of this specification, as illustrated below.SpecificationStandard Number Block Type Grade Class SpecialNotesExample:

31、 SpecificationD3222 05 I 2 . .D3222 I 2 . .For this example (D3222 05D3222, I2), the line callout describes a PVDF resin polymerized in emulsion, having a specificgravity between 1.75 and 1.79, and a peak melting endotherm between 162 to 170C.172C. A comma is used as the separatorbetween the Standar

32、d Number and the Type. Separators are not needed between the Type, Grade, and Class.6 Provision for SpecialNotes is included so that other information, such as a preferred viscosity range, can be provided when required. When special notesare used, they shall be preceded by a comma.5. General Require

33、ments5.1 The material shall be of uniform composition and free of foreign matter.6. Detail Requirements6.1 General Attributes:6.1.1 Peak Melting EndothermThe material covered by this specification shall have a minimum peak melting endotherm forthe type and class as shown in Table 1 when tested in ac

34、cordance with Test Method D3418. For Type I resins, this shall involveheating a solid specimen of 5 6 1 mg from room temperature to 200C at 10C/min, maintaining the temperature at 200C for 5min, followed by cooling at a controlled rate of 10C/min to about 30C, then reheating at 10C/min to 200C. Reco

35、rd the peakmelting endotherm during the second melting cycle.6.1.1.1 TemperatureTest Type II resins likewise except that the maximum is 250C.6.1.2 Specific GravityA solid specimen of the material covered by this specification shall have the minimum specific gravityindicated in Table 1 (1.75 for Type

36、 I, Class 1 and 1.76 for all others) when tested in accordance with Test Method D792.NOTE 3Test attached to the specimen upon immersion. Dipping the specimens in a very dilute solution (less than 0.1 weight percent) of an ammoniumperfluorooctanoate surfactant minimizes this problem.6.1.3 Refractive

37、IndexThe material covered in this specification shall have a refractive index of 1.42 when measured at thesodium D line at 25C (77F) in accordance with the refractometer procedure in Test Methods D542, using specimens that havenot been subjected to any processes which induce orientation of the polym

38、er chains or crystal-lites. Compression-moldedspecimens 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 this specification shall have a minimum limiting oxygen index of 42when tested in accordance with Test Met

39、hod D2863.NOTE 4If a column with a restricted opening is used, position the top of the specimen 40 mm below the opening.6.2 Processing Related Attributes:6.2.1 Flow RateMaterials conforming to this specification shall be tested for melt flow rate in accordance with Test MethodD1238 using loads shown

40、 in parentheses in Table 1.6.2.2 Rheological PropertiesThe apparent melt viscosity of these materials shall be tested in accordance with Test MethodD3835 at 231 6 1C (450F) using a die with an entrance angle of 60 (cone angle of 120) and a minimum capillary L/D of 15.See Table 1.6.3 Mechanical Prope

41、rties:6.3.1 Tensile PropertiesThe material covered in this specification shall have a tensile yield strength exceeding 36 MPa (5200psi) at 23C (74F) and a minimum elongation at break of 10 % when tested in accordance with Test Method D638 at 51 mm (2in.)/min, using Type I specimens 3.2-mm (0.125-in.

42、) thick as specified in Test Method D638. Preferably, compression-moldedsamples are used (see Section 8), but injection molded specimens also are used, providing that the samples yield and rupture inthe gage region and not near the heel. Specimens shall be molded under conditions specified by the re

43、sin suppliers. Generally,injection molded specimens show low and variable elongation values compared to compression-molded specimens. Typically, themelt temperature is 30 to 60C higher than the upper peak melting endotherm value depending on the grade. Mold temperatureis 120 6 10F.6 See the ASTM For

44、m and Style for ASTM Standards, available from ASTM Headquarters.D3222 1836.3.2 Flexural PropertiesThe material covered in this specification shall have a minimum flexural modulus of 1.381.31 GPa(190 103 psi) when tested in accordance with Method I of Test Methods D790, using 6.4-mm (0.25-in.) thick

45、 specimens preparedby injection molding under conditions specified by the resin supplier. Alternatively, compression-molded samples are used (seeSection 8) and tested after the 16-h conditioning period.6.3.3 Impact ResistanceType I material covered in this specification shall have a minimum impact s

46、trength of 80.0 J/m (1.50ftlbf/in.) determined by Test Methods D256 using 6.4-mm (0.25-in.) thick specimens prepared by injection molding underconditions specified by the manufacturer.Alternatively, specimens are compression-molded and tested after the conditioning periodas specified above. For Type

47、 II material, impact testing is not required.6.4 Electrical Properties:6.4.1 D-C ResistanceThe material covered in this specification shall have a d-c volume resistivity greater than 1.2m(1.2 1014 cm) when tested as a 0.76-mm (0.030-in.) compression-molded specimen (see Section 8) in accordance with

48、 TestMethods D257.6.4.2 Dielectric StrengthThe material covered in this specification shall have a dielectric strength in air no less than 57 kV/mm(1280 V/0.001 in.) by the “short-time” method of Test Methods D149 with 0.13-mm (0.05-in.) thick compression-moldedspecimens (see Section 8) tested in ai

49、r using 25.4-mm (1-in.) Type 3 electrodes.6.4.3 Dielectric ConstantThe material covered in this specification shall have a dielectric constant less than 11.0 at 100 Hzand greater than 5.8 at 1 MHz when tested as a 3.2-mm (0.125-in.) thick compression-molded specimen (see Section 8) inaccordance with Test Methods D150 at 23C (73F).6.4.4 Dissipation FactorThe material covered in this specification shall have a dissipation factor of less than 0.045 at 100 Hzand less than 0.24 at 1 MHz when tested as 3.2-m