1、Designation:F277809(Reapproved 2015)Standard Test Method forMeasurement of Percent Crystallinity ofPolyetheretherketone(PEEK)Polymers by Means ofSpecular Reflectance Fourier Transform InfraredSpectroscopy(R-FTIR)1This standard is issued under the fixed designation F2778;the number immediately follow
2、ing the designation indicates the year oforiginal adoption 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.1.Scope1.1 This test method describe
3、s the collection of absorptionspectra of polyetheretherketone(PEEK)polymer in filled andunfilled grades,as supplied by a vendor,and the subsequentcalculation of the percent crystallinity.The material is evalu-ated by infrared spectroscopy.The intensity(height)of theabsorbance peaks is related to the
4、 amount of crystalline regionspresent in the material.1.2 This test method can be used for PEEK consolidatedforms,such as injection molded parts,as long as the samplesare optically flat and smooth.1.3 The applicability of the infrared method to industrialand medical grade PEEK materials has been dem
5、onstrated byscientific studies.2,3Percentage of crystallinity is related toR-FTIR measurement by calibration through wide-angle x-rayscattering(WAXS)crystallinity measurements.2,3It is antici-pated that this test method,involving the peak heights near1305 cm-1and 1280 cm-1,will be evaluated in an In
6、terlabora-tory Study(ILS)conducted according to Test Method E691.1.4 This test method does not suggest a desired range ofcrystallinity for specific applications.1.5 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.6 This standar
7、d may involve hazardous materials,operations,and equipment.This standard does not purport toaddress all of the safety concerns,if any,associated with itsuse.It is the responsibility of the user of this standard toestablish appropriate safety and health practices and deter-mine the applicability of r
8、egulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:4E691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3.Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 crystallinity index(CI),nthe ratio of the heightbetween t
9、he absorption peaks 1305 cm-1and 1280 cm-1.4.Significance and Use4.1 Mechanical properties of PEEK,such as stiffness oryield strength,are influenced by the level of crystallinity.5Thereported crystallinity index determined by this test method hasbeen correlated with percent crystallinity in PEEK by
10、wide-angle X-ray scattering(WAXS)experiments.2,34.2 This test method may be useful for both processdevelopment,process control,product development,and re-search.5.Interferences5.1 Samples must be smooth and optically flat over the areaof investigation,typical of injection-molded specimens.Theymust b
11、e sufficiently thick(for example,1 to 2 mm)such thatthere is no detectable back surface reflected radiation.1This test method is under the jurisdiction ofASTM Committee F04 on Medicaland Surgical Materials and Devices and is the direct responsibility of SubcommitteeF04.15 on Material Test Methods.Cu
12、rrent edition approved May 1,2015.Published May 2015.Originallyapproved in 2009.Last previous edition approved in 2009 as F2778 09.DOI:10.1520/F277809R15.2Chalmers J.M.,Everall,N.J.,Hewitson,K.,Chesters,M.A.,Pearson,M.,Grady,A.,Kuzicka,B.,“Fourier Transform Infrared Microscopy:SomeAdvances inTechniq
13、ues for Characterisation and Structure-Property Elucidations of IndustrialMaterial,”The Analyst,Vol 23,1998,pp.579586.3Jaekel,D.J.,Medel,F.J.,Kurtz,S.M.,“Validation of Crystallinity Measure-ments of Medical Grade PEEK Using Specular Reflectance FTIR-microscopy,”Society of Plastics Engineers Annual T
14、echnical Conference 2009,Chicago 2009,Manuscript ID ANTEC-0248-2009.4For 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 websit
15、e.5Kurtz,S.M.,Devine,J.N.,“PEEK biomaterials in trauma,orthopedic,andspinal implants,”Biomaterials,Vol 28,No.32,2007,pp.48454869.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.2 Samples must be sized appropriately to be accommo-dated i
16、n the FTIR apparatus.6.Apparatus6.1 Infrared Spectrometer:6.1.1 An infrared spectrometer capable of recording a re-flection absorption spectrum over the range of 500 cm-1to1500 cm-1is necessary.6.1.1.1 A minimum scan resolution of 4 cm-1shall be used.6.1.1.2 A minimum aperture of 360 360 m shall be used.6.1.1.3 A minimum of 100 scans shall be collected perspectrum.6.1.2 Software capable of using the Kramers-Kronig trans-form algorithm to derive the absorbance spectra.6.2 Specimen HolderEquipment
