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Aluminum Foil by XPSJohn A. Rotole and Peter M. A. Sherwood Citation: Surface Science Spectra 5, 4 (1998); doi: 10.1116/1.1247850 View online: http://dx.doi.org/10.1116/1.1247850 View Table of Contents: http://scitation.aip.org/content/avs/journal/sss/5/1?ver=pdfcov Published by the AVS: Science & Technology of Materials, Interfaces, and Processing Articles you may be interested in Photoelectron spectroscopy study of the electronic structures of Al/MgF 2 /tris -(8-hydroxyquinoline) aluminuminterfaces Appl. Phys. Lett. 79, 105 (2001); 10.1063/1.1383798 Valence band x-ray photoelectron spectroscopic investigation of surface cleanliness of aluminum metal and itsalloys J. Vac. Sci. Technol. A 16, 1112 (1998); 10.1116/1.581242 Surface cleaning aluminum foil with ozone gas J. Vac. Sci. Technol. A 16, 961 (1998); 10.1116/1.581220 Core Level and Valence Band Spectra of Lead by XPS Surf. Sci. Spectra 5, 83 (1998); 10.1116/1.1247864 Aluminum Phosphate by XPS Surf. Sci. Spectra 5, 60 (1998); 10.1116/1.1247858

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Aluminum Foil by XPS

John A. Rotole and Peter M. A. SherwoodDepartment of Chemistry, 111 Willard Hall, Kansas State University, Manhattan, KS 66506-3702

The XPS spectra of argon ion etched aluminum metal were collected with a VSW HA150. Thisspectrometer is equipped with monochromatic AlKa x-radiation, a 16 channel multichanneldetector, and an electrostatic hemispherical analyzer with a radius of 150 mm providing aninstrument with exceptional capabilities. We report the Al 2p core level with resolved 2p1/2 and2p3/2 spin-orbit split components. The peak to valley separation on the high binding energy sidebetween the spin orbit components was determined to be 0.18 eV and the separation between thesecomponents was 0.44 eV. The valence band, survey, and the Al 2s, O 1s, and C 1s core levels arealso reported. ©1998 American Vacuum Society.@S1055-5269~97!00201-6#

Keywords: ESCA; XPS; valence band; aluminum; spin-orbit splitting

PACS: 79.60.Bm, 81.05.Bx, 82.80.Pv, 81.65.Ct

Accession # 00348

Technique: XPS

Host Material: aluminum foil

Instrument: VSW HA 150

Major Elements in Spectrum: Al

Minor Elements in Spectrum: O, C,Ar

Printed Spectra: 6

Spectra in Electronic Record: 6

Spectral Category: comparison

Original Submission: 10/20/97

Accepted for Publication: 1/13/98

SPECIMEN DESCRIPTION

Host Material: aluminum foil

CAS Registry #: 7429-90-5

Host Material Characteristics: homogeneous; solid; polycrystal-line; conductor; metal

Chemical Name: aluminum metal

Source: Alcan International

Host Composition: Al

Form: foil

Structure: fcc ~face centered cubic!

History & Significance: Ultrahigh purity aluminum foil was de-greased with acetone and placed in a special anaerobic pre-chamber~Ref. 1! used for sample preparation and electro-chemical studies. The argon gas to the saddle field etcher wasdelivered through a pre-baked quarter inch stainless steel lineto eliminate any oxidation problems associated with oxygencontamination. The sample was argon ion etched for 2.5 h tocompletely remove the native oxide. Analysis chamber pres-sure was maintained in the 1029 Torr range. The peak to valleyseparation of the Al 2p1/2 and 2p3/2 components was deter-mined to be 0.18 eV making this experiment an excellent testof spectrometer capabilities. The separation between the spinorbit split components was 0.44 eV, in excellent agreementwith studies using synchrotron radiation near the threshold forphotoexcitation~Ref. 2!.

As Received Condition: 99.9999% high purity aluminum

Analyzed Region: surface of host material

Ex Situ Preparation/Mounting: the sample was degreased withacetone

In Situ Preparation: the metal is argon ion etched to remove thenative oxide

Charge Control: not specified

Temp. During Analysis: 289 K

Pressure During Analysis: ,1.3331026 Pa

INSTRUMENT DESCRIPTION

Manufacturer and Model: VSW HA 150

Analyzer Type: spherical sector

Detector: multichannel

Number of Detector Elements: 16

INSTRUMENT PARAMETERS COMMON TO ALLSPECTRA

j SpectrometerAnalyzer Mode: constant pass energy

Throughput „T5EN…: N520.5

Excitation Source Window: N/A

Excitation Source: Al Ka monochromatic

Source Energy: 1486.6 eV

Source Strength: 240 W

Source Beam Size: 0.2 mm3 0.3 mm

Analyzer Width: 600 mm 3 1200mm

Signal Mode: multichannel direct

Effective Detector Width: 4.4 eV

j GeometryIncident Angle: 80°

Source to Analyzer Angle: 60°

Emission Angle: 10°

Specimen Azimuthal Angle: 180°

Acceptance Angle from Analyzer Axis: 0°

Analyzer Angular Acceptance Width: 0° 3 0°

j Ion GunManufacturer and Model: Ion Tech Ltd. B50

Energy: 5000 eV

Current: 2 mA

Current Measurement Method: biased stage

Sputtering Species: Ar

Comment: Ar ion etching was performed in a special UHV

chamber coupled to the x-ray photoelectron spectrometer

DATA ANALYSIS METHOD

Energy Scale Correction: All spectra were referenced to theC 1s peak of adventitious hydrocarbon at 284.60 eV.

Recommended Energy-Scale Shift: Accession #00348-3, 5.12eV; Accession #00348-6, 5.81 eV; all others, 5.98 eV

4 Surface Science Spectra, Vol. 5, 1998 © 1998 American Vacuum Society1055-5269/98/5(1)/4/7/$15.00


Peak Shape and Background Method: A horizontal linear back-ground was removed from the core levels and the valence bandspectrum. The survey scan was channel added for appearance.No curve fitting was conducted on these spectra.

Quantitation Method: Only peak area measurements are pro-vided.

ACKNOWLEDGMENTS

This material was based upon work supported by the NationalScience Foundation under Grant No. CHE-9421068. The U. S.Government has certain rights in this material.

REFERENCES

1. Y. Liang, D. K. Paul, Y. Xie, and P. M. A. Sherwood, Anal.Chem.65, 2276~1993!.

2. W. Eberhardt, G. Kaloffen, and C. Kunx, DESY Rt. SR 78/15~1978!.

3. ASTM, E90-93,1994 Annual Book of ASTM Standards~Ameri-can Society for Testing and Materials, Philadelphia, 1994!,Vol. 03.06.

4. M. P. Seah and G. C. Smith, inPractical Analysis by Auger andX-ray Photoelectron Spectroscopy, 2nd ed., edited by D.Briggs and M. P. Seah~Wiley, New York, 1990!, Vol. 1, p.535.

SPECTRAL FEATURES TABLE

SpectrumID #

Element/Transition

PeakEnergy„eV…

Peak WidthFWHM„eV…

Peak Area„eV counts …

SensitivityFactor

Concen-tration„at. %…

PeakAssignment

00348-02 Al 2s 117.33 1.27 3515 ¯ ¯ Al metal

00348-03 Al 2p1/2 73.00 ¯ ¯ ¯ ¯ Al metal

00348-03 Al 2p3/2 72.56 ¯ ¯ ¯ ¯ Al metal

00348-04 O 1s 531.47 2.62 1184 ¯ ¯ ¯

00348-05 C 1s 284.60 1.51 488 ¯ ¯ adventitious hydrocarbon

Footnote to Spectrum 00348-06: The sharp features of the Ar 3s at 22.38 eV and the Ar 3p at 8.37 eV arise from argon ion implantationinto the aluminum lattice during etching.

ANALYZER CALIBRATION TABLE

SpectrumID #

Element/Transition

PeakEnergy„eV…

Peak WidthFWHM„eV…

Peak Area„eV counts …

SensitivityFactor

Concen-tration„at. %…

PeakAssignment

00351-02 Ag 3d5/2 368.3 0.76 ¯ ¯ ¯ ¯

00351-03 AgMNN 1129.3 ¯ ¯ ¯ ¯ ¯

00352-02 Cu 2p3/2 932.7 1.01 ¯ ¯ ¯ ¯

00352-03 Cu 3p3/2 75.1 ¯ ¯ ¯ ¯ ¯

00352-04 CuLMM 568.2 ¯ ¯ ¯ ¯ ¯

Comment to Analyzer Calibration Table: The calibration was carried out according to the standard procedure reported in Ref. 3. Highpurity copper and silver foils were cut to the size of 1 cm 3 1 cm, polished and degreased with acetone. Each foil was then mounted on a samplecarrier and placed in an UHV prechamber for sputtering prior to data collection. The foils were argon ion etched for 40 min, using ultrahigh purityargon as the source gas. The etcher was operated at an ion acceleration potential of 5 kV and ion current of 2 mA. The binding energies of theCu and Ag photoemission and Auger lines were similar to the values that have been recommended in the literature for instrument calibration (Ref.4).

Surface Science Spectra, Vol. 5, 1998 Aluminum Foil by XPS 5


GUIDE TO FIGURES

Spectrum„Accession … #

SpectralRegion

SampleVoltage*

Multiplier Baseline Comment #

348-1 survey 25.98 1 0 1,2,3348-2 Al 2s 25.98 1 0 1,2348-3 Al 2 p 25.12 1 0 1,2348-4 O 1s 25.98 1 0 1,2348-5 C 1s 25.98 1 0 1,2348-6 Valence band 25.81 1 0 1,2

* Inferred sample potential relative to spectrometer ground due to charging, flood gun, or other phenomena.1. Author assigned correction to align C 1s line to 284.6 eV.2. Includes work function correction of 5.2 eV.3. Data have been compressed by summing every four channels.

6 Surface Science Spectra, Vol. 5, 1998 Aluminum Foil by XPS


Accession # 00348-01

Host Material aluminum foilTechnique XPS

Spectral Region surveyInstrument VSW HA 150

Excitation Source Al Ka monochromaticSource Energy 1486.6 eV

Source Strength 240 WSource Size 0.3 mm3 0.2 mm

Analyzer Type spherical sectorIncident Angle 80°

Emission Angle 10°Analyzer Pass Energy 44 eV

Analyzer Resolution 0.88 eVTotal Signal Accumulation Time 1009 s

Total Elapsed Time not specifiedNumber of Scans 1



j Accession #: 00348-03

j Host Material: aluminum foil

j Technique: XPS

j Spectral Region: Al 2p


Excitation Source: Al Ka

monochromatic



Source Size: 0.3 mm 3 0.2 mm

Incident Angle: 80°


Analyzer Pass Energy: 5 eV

Analyzer Resolution: 0.1 eV


Total Signal Accumulation Time:8500 s

Total Elapsed Time: not specified

Number of Scans: 17



j Technique: XPS

j Spectral Region: Al 2s



monochromatic











Number of Scans: 15





j Technique: XPS

j Spectral Region: C 1s



monochromatic











Number of Scans: 15



j Technique: XPS

j Spectral Region: O 1s



monochromatic











Number of Scans: 15





j Technique: XPS

j Spectral Region: O 2s; Ar 3s;Al edge; Ar 3p; valence band



monochromatic











Number of Scans: 50

Comment: See footnote below theSpectral Features Table.

