Nylon 6 (N6) Reference XPS Reference Core Level and Energy Loss Spectra

Nylon 6 „N6… Reference XPS ReferenceCore Level and Energy Loss Spectra

Pierre Louette,a� Frederic Bodino, and Jean-Jacques PireauxUniversity of Namur - LISE, 61, Rue de Bruxelles, B-5000 Namur, Belgium

�Received 23 September 2005; accepted 24 January 2006; published 13 October 2006�

XPS measurements of nylon 6 recorded with a SSX-100 spectrometer in standardized experimentalconditions are presented: survey scan, high resolution core level spectra as well as the energy lossregions of carbon, oxygen, and nitrogen peaks are analyzed. This is part of a contract work aimingto record spectra in the very same conditions of some forty different polymers. © 2006 AmericanVacuum Society. �DOI: 10.1116/11.20050903�

Keywords: x-ray photoelectron spectroscopy; XPS; surface; polymer; nylon; nylon 6; N6; poly-(caprolactam)

PACS: 79.60.Fr, 79.20.Uv, 73.20.At, 01.30.Kj

Accession # 00794

Technique: XPS

Host Material: Nylon 6

Instrument: Surface ScienceInstruments SSX-100

Major Elements in Spectrum: C, N,O

Minor Elements in Spectrum: none

Printed Spectra: 7

Spectra in Electronic Record: 7

Spectral Category: comparison

SPECIMEN DESCRIPTION

Host Material: nylon 6

CAS Registry #: 25038-54-4

Host Material Characteristics: homogeneous; solid; amorphous;dielectric; polymer

Chemical Name: poly�caprolactam�

Source: Scientific Polymer Products, Inc.

Host Composition: �NH�CH2�5CO�n

Form: pellets

Structure:

History & 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: spin-coated film

Analyzed Region: same as host material

Ex Situ PreparationÕMounting: none

In Situ Preparation: none

Pre-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 �0.5 eV�

Temp. During Analysis: 300 K

Pressure During Analysis: �6.6�10�8 Pa

INSTRUMENT DESCRIPTION

Manufacturer and Model: Surface Science Instruments SSX-100

Analyzer Type: spherical sector

Detector: position sensitive detector with microchannel plate

Number of Detector Elements: 128

a)Author to whom correspondence should be addressed.

12 Surface Science Spectra, Vol. 12, 2005 1055-5269/2005

INSTRUMENT PARAMETERS COMMON TO ALL SPECTRA

� SpectrometerAnalyzer Mode: constant pass energy

Throughput „TÄEN…: N�see comment below

Throughput Comment: T � EN , N � 0.7

Excitation Source Window: 1.5 �m Al foil

Excitation Source: Al K� monochromatic

Source Energy: 1486.6 eV

Source Strength: 130 W

Source Beam Size: 0.6 mm � 0.6 mm

Signal 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°

DATA ANALYSIS METHOD

Energy Scale Correction: To compensate for charging effects,we adjusted the largest C 1s component to 285.00 eV �Ref. 1�.

Recommended Energy-Scale Shift: �3.29 eV

Peak 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.

ACKNOWLEDGMENTS

This 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.

/12/12/6/$23.00 © 2006 American Vacuum Society

REFERENCES

1. G. Beamson and D. Briggs, in The Scienta ESCA 300 Database�Wiley, Chichester, 1992�.

Surface Science Spectra, Vol. 12, 2005

2. C. J. Powell, J. Electron. Spectrosc. Relat. Phenom. 47, 197�1988�.

SPECTRAL FEATURES TABLE

SpectrumID #

ElementÕTransition

PeakEnergy„eV…

Peak WidthFWHM„eV…

Peak Area„eV-ctsÕs…

SensitivityFactor

Concen-tration„at. %…

PeakAssignment

00794-02 C 1s 285.00 1.72 5739 1.00 44.0 1 in Diagram below




00794-03 N 1s 399.87 1.77 2615 1.68 11.9 5 in Diagram below

00794-04 O 1s 531.54 1.91 4283 2.49 13.2 6 in Diagram below

Comment to Spectral Features Table:

ANALYZER CALIBRATION TABLE

SpectrumID #

ElementÕTransition

PeakEnergy„eV…

Peak WidthFWHM„eV…

Peak Area„eV-ctsÕs…

SensitivityFactor

Concen-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 FIGURES

Spectrum„Accession… #

SpectralRegion

VoltageShift*

Multiplier Baseline Comment #

794-1 Survey �3.29 1 0

794-2 C 1s �3.29 1 0

794-3 N 1s �3.29 1 0

794-4 O 1s �3.29 1 0

794-5 C 1s�losses �3.29 1 0

794-6 N 1s�losses �3.29 1 0

794-7 O 1s�losses �3.29 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.

Nylon 6 by XPS 13

Accession # 00794-01

Host Material nylon 6

Technique XPS

Spectral Region survey

Instrument Surface Science Instruments SSX-100

Excitation Source Al K� monochromatic

Source Energy 1486.6 eV

Source Strength 130 W

Source Size 0.6 mm � 0.6 mm

Analyzer Type spherical sector

Incident Angle 57.6°

Emission Angle 14.7°

Analyzer Pass Energy 106.8 eV

Analyzer Resolution 1.17 eV

Total Signal Accumulation Time 960 s

Total Elapsed Time not specified

Number of Scans 2

Effective Detector Width 12.96 eV

14 Surface Science Spectra, Vol. 12, 2005 Nylon 6 by XPS

http://surfscispectra.org/cgi-bin/sssonlinedata.cgi?submissionno=20050903&datafile=N0079401.asc

� Accession #: 00794-03

� Host Material: nylon 6

� Technique: XPS

� Spectral Region: N 1s


Excitation Source: Al K�monochromatic



Source Size: 0.6 mm � 0.6 mm

Incident Angle: 57.6°


Analyzer Pass Energy: 29.97 eV

Analyzer Resolution: 0.76 eV


Total Signal Accumulation Time:1200 s

Total Elapsed Time: not specified

Number of Scans: 10

Effective Detector Width: 3.341 eV

� Accession #: 00794-02


� Technique: XPS

� Spectral Region: C 1s













Number of Scans: 10


Surface Science Spectra, Vol. 12, 2005 Nylon 6 by XPS 15



� Accession #: 00794-05


� Technique: XPS

� Spectral Region: C 1senergy losses













Number of Scans: 5


� Accession #: 00794-04


� Technique: XPS

� Spectral Region: O 1s













Number of Scans: 10


16 Surface Science Spectra, Vol. 12, 2005 Nylon 6 by XPS



� Accession #: 00794-07


� Technique: XPS

� Spectral Region: O 1senergy losses













Number of Scans: 5


� Accession #: 00794-06


� Technique: XPS

� Spectral Region: N 1senergy losses













Number of Scans: 5


Surface Science Spectra, Vol. 12, 2005 Nylon 6 by XPS 17



Nylon 6 (N6) Reference XPS Reference Core Level and Energy Loss Spectra

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