Bodino, Frédéric

Louette, Pierre

Pireaux, Jean-Jacques

English

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RESEARCH OUTPUTS / RÉSULTATS DE RECHERCHEAuthor(s) - Auteur(s) :Publication date - Date de publication :Permanent link - Permalien :Rights / License - Licence de droit d’auteur :Bibliothèque Universitaire Moretus PlantinInstitutional Repository - Research PortalDépôt Institutionnel - Portail de la Rechercheresearchportal.unamur.bePoly(ether ether ketone) (PEEK) XPS reference core level and energy loss spectraLouette, Pierre; Bodino, Frédéric; Pireaux, Jean-JacquesPublished in:Surface science spectraPublication date:2005Document VersionEarly version, also known as pre-printLink to publicationCitation for pulished version (HARVARD):Louette, P, Bodino, F & Pireaux, J-J 2005, 'Poly(ether ether ketone) (PEEK) XPS reference core level andenergy loss spectra', Surface science spectra, vol. 12, pp. 149-153.General rightsCopyright and moral rights for the publications made accessible in the public portal are retained by the authors and/or other copyright ownersand it is a condition of accessing publications that users recognise and abide by the legal requirements associated with these rights.            • Users may download and print one copy of any publication from the public portal for the purpose of private study or research.            • You may not further distribute the material or use it for any profit-making activity or commercial gain            • You may freely distribute the URL identifying the publication in the public portal ?Take down policyIf you believe that this document breaches copyright please contact us providing details, and we will remove access to the work immediatelyand investigate your claim.Download date: 23. Jun. 2020Poly„ether ether ketone… „PEEK… XPSReference Core Level and Energy LossSpectraPierre Louette,a Frederic Bodino, and Jean-Jacques PireauxUniversity of Namur - LISE, 61, Rue de Bruxelles, B-5000 Namur, BelgiumReceived 21 October 2005; accepted 6 June 2006; published 16 February 2007XPS measurements of polyether ether ketone recorded with a SSX-100 spectrometer instandardized experimental conditions are presented: survey scan, high resolution core level spectraas well as the energy loss regions of carbon and oxygen peaks are analyzed. This is part of a contractwork aiming to record spectra in the very same conditions of some 40 different polymers. © 2006American Vacuum Society. DOI: 10.1116/11.20051106Keywords: x-ray photoelectron spectroscopy; XPS; surface; polymer; poly(ether ether ketone);PEEKPACS: 79.60.Fr, 82.80.Pv, 79.20.Uv, 61.41.e, 01.30.KjAccession # 00891Technique: XPSHost Material: poly(ether etherketone)Instrument: Surface ScienceInstruments SSX-100Major Elements in Spectrum: C, OMinor Elements in Spectrum: nonePrinted Spectra: 5Spectra in Electronic Record: 5Spectral Category: comparisonSPECIMEN DESCRIPTIONHost Material: polyether ether ketoneCAS Registry #: 31694-16-3Host Material Characteristics: homogeneous; solid; amorphous;dielectric; polymerChemical Name: polyether ether ketoneSource: ICIHost Composition: not specifiedForm: pelletStructure:O O CO nHistory & Significance: This study is a part of a reference spectradatabase of polymers, including survey and core level spectra,but also energy loss spectra of the main elements.As Received Condition: not specifiedAnalyzed Region: same as host materialEx Situ PreparationÕMounting: pressed powderIn Situ Preparation: nonePre-Analysis Beam Exposure: The analyzed region was exposedto x-rays for a very short time, around 2 min for sample posi-tion adjustment prior to measurements.Charge Control: use of a metal screen and a flood gun 2 eVTemp. During Analysis: 300 KPressure During Analysis: 6.6108 PaINSTRUMENT DESCRIPTIONManufacturer and Model: Surface Science Instruments SSX-100Analyzer Type: spherical sectorDetector: position sensitive detector with microchannel platea)Author to whom correspondence should be addressed.Surface Science Spectra, Vol. 12, 2005 1055-5269/2005/1Number of Detector Elements: 128INSTRUMENT PARAMETERS COMMON TO ALL SPECTRA SpectrometerAnalyzer Mode: constant pass energyThroughput „TÄEN…: NSee comment belowThroughput Comment: T  EN, N  0.7Excitation Source Window: 1.5 m Al foilExcitation Source: Al K monochromaticSource Energy: 1486.6 eVSource Strength: 130 WSource Beam Size: 0.6 mm  0.6 mmSignal Mode: not specified GeometryIncident Angle: 57.6°Source to Analyzer Angle: 70.8°Emission Angle: 14.7°Specimen Azimuthal Angle: 75.5°Acceptance Angle from Analyzer Axis: 0°Analyzer Angular Acceptance Width: 30°  30°DATA ANALYSIS METHODEnergy Scale Correction: To compensate for charging effects,we adjusted the largest C 1s component to 284.70 eV Ref. 1.Recommended Energy-Scale Shift: 6.03 eVPeak Shape and Background Method: A least square fitting rou-tine with mixed Gaussian/Lorentzian for the components and alinear background was used.Quantitation Method: Scofield factors corrected for energy de-pendence were used.ACKNOWLEDGMENTSThis study is a part of the EU-BCR contract ‘‘XPS Spectral In-tensity Data Bank.’’ We thank the NPL for authorizing us to pub-lish these spectra.© 2006 American Vacuum Society 1492/149/5/$23.00REFERENCES1. G. Beamson and D. Briggs, in The Scienta ESCA 300 DatabaseWiley, Chichester, 1992.150 Surface Science Spectra, Vol. 12, 20052. C. J. Powell, J. Electron. Spectrosc. Relat. Phenom. 47, 1971988.SPECTRAL FEATURES TABLESpectrumID #ElementÕTransitionPeakEnergy„eV…Peak WidthFWHM„eV…Peak Area„eV-ctsÕs…SensitivityFactorConcen-tration„at. %…PeakAssignment00891-02 C 1s 284.70 1.11 7815 1.00 64.5 1 in Diagram below00891-02 C 1s 286.31 1.09 1915 1.00 16.0 2 in Diagram below00891-02 C 1s 287.10 0.94 213 1.00 1.8 3 in Diagram below00891-02 C 1s 291.59 1.81 405 1.00 ¯ ¯00891-03 O 1s 531.31 1.42 1445 2.49 4.9 4 in Diagram below00891-03 O 1s 533.40 1.30 3542 2.49 11.9 5 in Diagram below00891-03 O 1s 540.91 3.29 154 2.49 ¯¯Comment to Spectral Features Table:O O CO n12 5 34ANALYZER CALIBRATION TABLESpectrumID #ElementÕTransitionPeakEnergy„eV…Peak WidthFWHM„eV…Peak Area„eV-ctsÕs…SensitivityFactorConcen-tration„at. %…PeakAssignment¯ Cu 2p3/2 932.34 1.19 202906 9.748 ¯ ¯¯ Cu 3p3/2 74.78 2.36 289045 2.774 ¯ ¯GUIDE TO FIGURESSpectrum„Accession… #SpectralRegionVoltageShift* Multiplier Baseline Comment #891-1 Survey 6.03 1 0891-2 C 1s 6.03 1 0891-3 O 1s 6.03 1 0891-4 C 1s  losses 6.03 1 0891-5 O 1s  losses 6.03 1 0* Voltage shift of the archived (as-measured) spectrum relative to the printed figure. The figure reflects the recommended energy scale correctiondue to a calibration correction, sample charging, flood gun, or other phenomenon.Poly(ether ether ketone) by XPS0   100 200 300 400 500 600 700 800 900 020004000600080001000012000Corrected binding energy (eV)CountsC 1sO 1s891−1(X10)Accession # 00891-01Host Material polyether ether ketoneTechnique XPSSpectral Region surveyInstrument Surface Science Instruments SSX-100Excitation Source Al K monochromaticSource Energy 1486.6 eVSource Strength 130 WSource Size 0.6 mm  0.6 mmAnalyzer Type spherical sectorIncident Angle 57.6°Emission Angle 14.7°Analyzer Pass Energy 106.8 eVAnalyzer Resolution 1.17 eVTotal Signal Accumulation Time 960 sTotal Elapsed Time not specifiedNumber of Scans 2Effective Detector Width 12.96 eVSurface Science Spectra, Vol. 12, 2005 Poly(ether ether ketone) by XPS 151520525530535540050010001500200025003000891−3Corrected binding energy (eV)CountsO 1s4 5  Accession #: 00891-03 Host Material: poly(ether etherketone) Technique: XPS Spectral Region: O 1sInstrument: Surface ScienceInstruments SSX-100Excitation Source: Al KmonochromaticSource Energy: 1486.6 eVSource Strength: 130 WSource Size: 0.6 mm  0.6 mmIncident Angle: 57.6°Analyzer Type: spherical sectorAnalyzer Pass Energy: 29.97 eVAnalyzer Resolution: 0.76 eVEmission Angle: 14.7°Total Signal Accumulation Time:1200 sTotal Elapsed Time: not specifiedNumber of Scans: 10Effective Detector Width: 3.341 eV27528028529029501000200030004000500060007000Corrected binding energy (eV)CountsC 1s 891−21 2 3  Accession #: 00891-02 Host Material: poly(ether etherketone) Technique: XPS Spectral Region: C 1sInstrument: Surface ScienceInstruments SSX-100Excitation Source: Al KmonochromaticSource Energy: 1486.6 eVSource Strength: 130 WSource Size: 0.6 mm  0.6 mmIncident Angle: 57.6°Analyzer Type: spherical sectorAnalyzer Pass Energy: 29.97 eVAnalyzer Resolution: 0.76 eVEmission Angle: 14.7°Total Signal Accumulation Time:1200 sTotal Elapsed Time: not specifiedNumber of Scans: 10Effective Detector Width: 3.341 eV152 Surface Science Spectra, Vol. 12, 2005 Poly(ether ether ketone) by XPS520530540550560570580200040006000800010000120001400016000Corrected binding energy (eV)CountsO 1s891−5  Accession #: 00891-05 Host Material: poly(ether etherketone) Technique: XPS Spectral Region: O 1senergy lossesInstrument: Surface ScienceInstruments SSX-100Excitation Source: Al KmonochromaticSource Energy: 1486.6 eVSource Strength: 130 WSource Size: 0.6 mm  0.6 mmIncident Angle: 57.6°Analyzer Type: spherical sectorAnalyzer Pass Energy: 106.8 eVAnalyzer Resolution: 1.17 eVEmission Angle: 14.7°Total Signal Accumulation Time:900 sTotal Elapsed Time: not specifiedNumber of Scans: 5Effective Detector Width: 12.956 eV28029030031032033034000.511.522.533.5x 104Corrected binding energy (eV)CountsC 1s891−4 Accession #: 00891-04 Host Material: poly(ether etherketone) Technique: XPS Spectral Region: C 1senergy lossesInstrument: Surface ScienceInstruments SSX-100Excitation Source: Al KmonochromaticSource Energy: 1486.6 eVSource Strength: 130 WSource Size: 0.6 mm  0.6 mmIncident Angle: 57.6°Analyzer Type: spherical sectorAnalyzer Pass Energy: 106.8 eVAnalyzer Resolution: 1.17 eVEmission Angle: 14.7°Total Signal Accumulation Time:900 sTotal Elapsed Time: not specifiedNumber of Scans: 5Effective Detector Width: 12.956 eVSurface Science Spectra, Vol. 12, 2005 Poly(ether ether ketone) by XPS 153

Poly(ether ether ketone) (PEEK) XPS reference core level and energy loss spectra

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Poly(ether ether ketone) (PEEK) XPS reference core level and energy loss spectra

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