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SEMATECH Technology Transfer 90120403B-STD SEMASPEC Test Method for XPS Analysis of Surface Composition and Chemistry of Electropolished Stainless Steel Tubing for Gas Distribution System Components

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Page 1: SEMASPEC Test Method for XPS Analysis of Surface ... · PDF filetest method is expected to yield comparable data among components tested for the ... 2.8 Seah, M.P. and W.A. Dench

SEMATECHTechnology Transfer 90120403B-STD

SEMASPEC Test Method for XPSAnalysis of Surface Composition and

Chemistry of ElectropolishedStainless Steel Tubing for Gas

Distribution System Components

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© 1996 SEMATECH, Inc.

SEMATECH and the SEMATECH logo are registered service marks of SEMATECH, Inc.

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SEMASPEC Test Method for XPS Analysis of Surface Compositionand Chemistry of Electropolished Stainless Steel Tubing for Gas

Distribution System ComponentsTechnology Transfer # 90120403B-STD

SEMATECHFebruary 22, 1993

Abstract: This SEMASPEC defines a method of testing the interior surface of chromium enhanced stainlesssteel tubing, fittings, and valves to determine the surface composition and chemistry as a measureof the effectiveness of electropolishing. Its purpose is to evaluate components considered for use inultra-high purity gas distribution systems. Application of this test method is expected to yieldcomparable data among components tested for the purposes of qualification for installation. Thisdocument is in development as an industry standard by Semiconductor Equipment and MaterialsInternational (SEMI). When available, adherence to the SEMI standard is recommended.

Keywords: Surface Composition, ESCA, Stainless Steel Tubing, Defect Sources, Facilities, Gas DistributionSystems, Specifications, Components, Component Testing

Authors: Jeff Riddle

Approvals: Jeff Riddle, Project ManagerVenu Menon, Program ManagerJackie Marsh, Director of Standards ProgramGene Feit, Director, Contamination Free ManufacturingJohn Pankratz, Director, Technology TransferJeanne Cranford, Technical Information Transfer Team Leader

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Technology Transfer # 90120403B-STD SEMATECH

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SEMASPEC #90120403B-STD

SEMASPEC Test Method for XPS Analysis of Surface Composition and Chemistryof Electropolished Stainless Steel Tubing for Gas Distribution System Components

1. Introduction

Semiconductor cleanrooms are serviced by high-purity gas distribution systems. Thisdocument presents a test method that may be applied for the evaluation of one or morecomponents considered for use in such systems.

1.1 Purpose

1.1.1 The purpose of this document is to define a method for testing components beingconsidered for installation into a high-purity gas distribution system. Application of thistest method is expected to yield comparable data among components tested for thepurposes of qualification for this installation.

1.1.2 This document defines a method of testing the interior surface of stainless steel tubing,fittings and valves, to determine the surface composition and chemistry, as a measure ofthe effectiveness of electropolishing.

1.1.3 The objective of this method is to describe a general set of instrument parameters andconditions that will achieve precise and reproducible measurements of important surfacechemistry within the chromium-enriched oxide layer.

1.2 Scope

1.2.1 This document describes a test method to characterize "as received" surface compositionand chemistry encompassing all chromium enhanced stainless steel surfaces in tubing,connectors, regulators and valves of all sizes.

1.2.2 This procedure describes measurement of Cr/Fe elemental ratios, chemical species ratiosfor Cr and Fe, and independent estimates of Cr, Fe, and Ni oxide thickness by X-rayphotoelectron spectroscopy (XPS), also referred to in the literature as electronspectroscopy for chemical analysis (ESCA). Measurement of elemental surfacecomposition and chemistry of phosphorus, sulfur, and residual organic material is alsodescribed.

1.3 Limitations

1.3.1 This methodology assumes an XPS analyst with a skill level typically achieved over atwelve-month period and familiarity with the XPS technique and instrumentation.

1.3.2 The methodology and instrumentation described in this procedure is not intended topreclude the use of any particular brand or model of surface analysis equipment. Whilemuch of the test methodology has been developed using specific instrumentation, themethod can be adapted to most state-of-the-art surface analytical instrumentation. Whenusing this method, it is essential to document the key instrument parameters that definethe sampling volume and sensitivity of the measurements.

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2. Reference Documents

2.1 ASTM1

ASTM E1078–85 Standard Guide for Specimen Handling in Auger ElectronSpectroscopy and X-Ray Photoelectron Spectroscopy, 1985.

ASTM E902–88 Standard Practice for Checking the Operating Characteristics of X-Ray Photoelectron Spectrometers, 1988.

ASTM E1015–84 Standard Practice for Reporting Spectra in X-Ray PhotoelectronSpectroscopy, 1984.

ASTM Standard Definitions, Guides, and Practices for Surface Analysis. AVSMonograph Series.

2.2 Briggs, D. and M.P. Seah, ed. Practical Surface Analysis by Auger and X-Ray Photo–electron Spectroscopy. John Wiley and Sons. 1983.

2.3 Dilkes, A. "X-Ray Photoelectron Spectroscopy for the Investigation of PolymericMaterials." Electron Spectroscopy: Theory, Techniques, and ApplicationsBrundle, C.R. and Baker, A.D., editors. Academic Press. 1981:277–359.

2.4 Linder, R.E. and P.B. Mee. "ESCA Determination of Fluorocarbon Lubricant FilmThickness on Magnetic Disc Media." IEEE Transactions. July 1982:1073–1076.(Calculation of oxide thin films from ESCA spectra)

2.5 Perkin–Elmer Corp. Handbook of X-Ray Photoelectron Spectroscopy: A Reference Bookof Standard Data for Use in XPS. Perkin Elmer Corporation, Physical ElectronicsDivision. 1979.

2.6 Tanuma, S., C.J. Powell, and D.R. Penn. Surface Science, 192, L849. 1987.

2.7 Tanuma, S., C.J. Powell, and D.R. Penn. Surface Interface Anal. 11:577. 1988.

2.8 Seah, M.P. and W.A. Dench. Surface Interface Anal. 1:2. 1979.

2.9 Wagner, C.D. et al. "Handbook of X-Ray Photoelectron Spectroscopy. G.E. Muhlenberg(ed.). Perkin-Elmer Corporation Physical Electronics Division, Eden Prairie, MN,pp. 38-39. 1979.

2.10 Walls, J.M. "Methods of Surface Analysis: Techniques and Applications. CambridgeUniversity Press, New York, NY. 1989.

1 American Society for Testing and Materials, 1916 Race St. Philadelphia, PA 19103.

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3. Terminology

3.1 ESCA—electron spectroscopy for chemical analysis

3.2 psia—pounds per square inch absolute

3.3 standard conditions—101.3 kPa, 0.0 °C (14.73 psia, 32.0 °F).

3.4 sampling volume—the volume from which the photoelectrons are ejected. Lateraldimensions are determined by the X-ray spot size. A length of three times the mean freepath is considered to be the maximum XPS depth sensitivity. The measurement volumefor a given instrument is dependent on the sample and the take-off-angle geometry.

3.5 take-off-angle (TOA)—the angle that the lens forms with the sample surface plane(See Figure 7).

3.6 XPS—X-ray photoelectron spectroscopy.

4. Test Protocol

4.1 Test conditions

4.1.1 Precautions

4.1.1.1 This test method may involve hazardous materials, operations, and equipment. This testmethod does not purport to address the safety considerations associated with its use. It isthe responsibility of the user to establish appropriate safety and health practices anddetermine the applicability of regulatory limitations before using this method.

4.1.1.2 All normal and acceptable precautions regarding use of high voltage, vacuum, and X-rayproducing equipment must be observed.

4.1.2 Sample preparation

4.1.2.1 The samples are to be prepared and mounted for analysis using standard practicesconsistent with high vacuum surface analytical procedures. Samples shall be cut downto roughly 1 cm square using a clean, dry hack saw or low speed band saw. Anymechanical cutting must not introduce organic or inorganic contamination onto thesample surface. In addition, sample preparation must be done in a manner that avoidsexcessive heating; i.e., the surface temperature should not exceed 50 °C, to avoid oxidegrowth or change in surface composition.

4.1.2.2 Cleaning of samples—Unless specifically requested, such as when only chromium andiron will be analyzed, the sample surface is not to be cleaned with any organic solvent orwater. Residual particles from the cutting process will be removed aerodynamically bychemically inert, particle-free gas flow such as dry nitrogen.

4.1.2.3 Mounting of the samples onto XPS compatible mounts (using nonmagnetic screws andfixtures) shall be done in a manner consistent with high vacuum practices to avoidcontamination of the surface to be analyzed. If applicable, the sample should belongitudinally oriented with the direction of the X-ray beam parallel to the axis of thetubing.

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4.2 Apparatus

4.2.1 Materials

4.2.1.1 Teflon® tape and high molecular weight (1,000,000 Daltons minimum) dimethyl silicone is to beused for composition calibration.2 From the Teflon and dimethyl silicone, calibration ofsensitivity factors is performed as described in Appendix A.1. These samples shall be analyzedusing X-ray power and beam size consistent with those used for the electropolished stainlesssteel analyses. Copper foil and sputtered gold film foil are to be used for binding energy scalecalibration as described in Appendix A.1.

4.2.2 Instrumentation

4.2.2.1 An X-ray photoelectron spectrometer with:

Defined area for analysis of variation along a surface or in narrow diameter tubes and fittings,ideally 1 mm square or smaller, so that narrow diameter tubing surface, or changes in surfacechemistry along a surface can be measured.

Good signal-to-noise ratio (S/N >3 for survey spectra, S/N >10 for high-resolution spectra) forquantitation of low level contamination to detect low abundance surface contaminants such asSi, P, and S at roughly one atomic percent. [This can be achieved with a count rate of about100,000 to 500,000 counts per minute as measured for Au (4f 7/2).]

Sufficient peak resolution (roughly 1 eV Full Width Half Maximum Au 4f 7/2) to ensurespectral resolution of the metal and oxide peaks for chromium, iron, and nickel.

4.2.2.2 It is essential that the XPS spectrometer be accurately calibrated for binding energydetermination so that the proper peak assignments for Cr, Fe, Ni, P, S, and Si can be made. It iscritical that the sensitivity factors for Cr, Fe and Ni be determined from Teflon and dimethylsilicone reference standards so that accurate and comparable data can be obtained for specimensthat may be analyzed at various analytical facilities. An accurate set of composition sensitivityfactors (for composition calibration) can be calculated from Scofield X-ray cross sections, againusing analytical standards such as Teflon tape and dimethyl silicone (see Annex A1).

4.2.2.3 If the instrument does not have a focused monochromatic source, the analyzer should beapertured to allow 1–mm spatial resolution. The irradiation by a non-monochromatized sourcemay result in lower observed carbon and reduction of transition metal species. This result can belimited by using an aluminum or berylium window and by adjusting X-ray anode power.Thermal damage may also occur, requiring characterization of composition as a function ofanalysis time. If the analyzer is of a variable take-off angle (TOA) design, the analyzer shouldbe set to an angle as close to a 35° TOA as possible. The orientation of geometry and angles ofincident X-ray irradiation and lens axis to the plane of the sample should be recorded.

2Teflon is a registered trademark of E.I. du Pont de Nemours and Company.

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4.2.2.4 A turbo-mechanical roughing pump is preferred to avoid hydrocarbon backstreaming that mightcontaminate the sample surface during initial pumpdown.

4.2.2.5 Binding energy calibration—The binding energy scale is calibrated using gold and copper (Au4f7/2 at 83.93 eV and Cu 2p3/2 at 932.47 eV), as described in Appendix A.1. A record ofinstrument calibration must be kept. Interpretation of the XPS spectra are based on bindingenergies from reference compounds. [For additional information, see reference 2.5.]

4.2.3 Setup and schematic - per manufacturer's instructions

4.3 Test Procedures—(Summary) This test procedure measures the elemental Cr/Fe ratio and Croxide/Fe oxide species ratio within the "as-received" detection volume and determines surfacecomposition of the "as-received" surface. Estimating individual oxide thicknesses for Cr, Fe, orNi (i.e., the depth to which that element is oxidized) using the high resolution data is optionaland is not an essential part of this method.

4.3.1 Introduce the sample into the XPS (introduction) vacuum chamber. Pump down and transfer tothe analytical chamber at the manufacturer's recommended base pressure.

4.3.2 Align the sample with respect to the X-ray beam and analyzer so that the optimum count ratefrom the desired analytical location is obtained. As a general convention, tubing samples shouldbe oriented parallel to the axis of incident X-ray irradiation. The use of a collimated highvoltage electron beam to align the sample surface with respect to lens optics should be avoided,as this will desorb surface carbon and potentially alter surface oxide chemistry. If an inelastic,electron-beam focusing procedure is used, the area for XPS analysis should be at least 1/2 cmaway.

The surface area to be analyzed should be free of visible particles, and large visible defectfeatures such as pits should be avoided.

4.3.3 Carry out the following analytical protocol for surface composition.

4.3.3.1 Survey data (0–1100 eV) are to be measured from the sample surface to determine the elementspresent and their approximate surface abundances. These measurements should be performedusing a high-throughput analyzer setting so that a signal–to–noise ratio sufficient to detect sulfurand phosphorus at better than one atom percent is obtained. (Typically, 15 to 30-minuteacquisition times at highest throughput conditions are sufficient to achieve a reasonable signal–to–noise ratio of ≥3.) A typical survey spectrum, with an energy resolution of roughly one eVper channel (one eV per data point), is shown in Figure 1.

4.3.3.2 Binding energies for phosphorus and sulfur shall be determined from peak maxima with anuncertainty of no more than one eV, requiring an energy resolution of no more than 1 eV perchannel. These binding energies should be referenced to the principal C(1s) carbon peak at285.0 eV.

4.3.3.3 A beam size not smaller than 600 by 1000 µm should be used to ensure measurement of arepresentative surface. The beam should not be so large as to overlap cut edges of narrow I.D.tubing. Quantification is to be done using sensitivity factors derived from polymeric materials,as described in Annex A1.

4.3.4 Analytical protocol for measuring surface chemical species—High resolution spectra fromelements other than C, Cr, Fe and Ni can be determined using an energy resolution of better than0.2 eV per channel (data point). This is accomplished by using data collection parametersequivalent to a full width half maximum (FWHM) on Au (4f7/2) peak of 1.0 eV or better, andspectral widths of roughly 20 eV. Standard peak-fit (deconvolution) routines can be used tomore precisely define peak position and deconvolute multiple species. Chemical assignments

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for all high resolution measurements should be consistent with accepted reference compounds(See Section 2.1, Reference Documents).

4.3.5 Analytical protocol for measuring Cr, Fe, and Ni chemical bonds—Measurement andquantification of Cr/Fe elemental ratio, and metal/oxide species ratios for Cr, Fe, and Ni aredetermined from high resolution measurements of the Cr(2p3/2), Fe(2p3/2) and Ni(2p3/2)spectral windows respectively, as detailed in Sections 4.3.5.1–4.3.5.3.

4.3.5.1 Using an analyzer, pass energy sufficient enough to provide an FWHM on Au 4f7/2 of betterthan 1.0 eV and an energy resolution of better than 0.2 eV per channel (data point). Highresolution spectra from Cr, Fe, and Ni are typically measured from 20 eV scan widths.

4.3.5.2 The energy windows for Cr, Fe, and Ni are as follows: Cr(2p3/2) from 570 to 590 eV, Fe(2p3/2)from 700 to 720 eV, and Ni2p3/2 from 845 to 865 eV.

4.3.5.3 Data acquisition times should be long enough to provide at least 50,000 integrated counts for theintegrated (curve fit) peak envelope. Signal to noise should be at least 10.

4.3.6 Calculation of key Cr and Fe ratios from high resolution data—The calculation of Cr and Feelemental ratios is performed using integrated peak areas as determined from curve fitting theindividual Cr(2p3/2) and Fe(2p3/2) peaks and using appropriate sensitivity factors (asdetermined from calibration in Appendix A.1) and background corrections.

4.3.7 Cr and Fe oxide species ratios:

4.3.7.1 Cr–O/Fe–O ratio—This determination is a straight-forward calculation using the relative oxidespecies abundances as determined from the Cr(2p3/2) and Fe(2p3/2) spectra. In the Cr(2p3/2)spectrum the peak at 574 eV is assigned as reduced chromium, and the peaks at 576 and 577 areassigned as oxidized chromium. In the Fe (2p3/2) spectrum, the two peaks at 707 and 708.5 eVare assigned as reduced species, and the three peaks at 710, 711.5 and 713 eV are assigned asoxidized species. The Cr–O/Fe–O species ratio is the atomic abundance of oxidized chromiumdivided by atomic abundance of oxidized iron. (See Figures 2 and 3.)

4.3.7.2 For Ni 2p3/2 measurements, the peak at 852.47 eV is defined as the metallic (reduced) speciesand the peak at roughly 854 to 855 eV is defined as the oxidized species. (See Figure 4.)

4.3.8 Estimate Cr, Fe, and Ni oxide thickness from high resolution data.

4.3.8.1 The oxide thicknesses for Cr, Fe, and Ni can be estimated from the high resolution 20 eVwindow XPS measurements using a thin film thickness algorithm.

4.3.8.2 The specific forms of these equations are as follows:

Cr oxide thickness ≈ 20 Å × ln [(Cr oxide area/Cr metal area) × "a1" + 1]

Fe oxide thickness ≈ 20 Å × ln [(Fe oxide area/Fe metal area) × "a2" + 1]

Ni oxide thickness ≈ 20 Å × ln [(Ni oxide area/Ni metal area) × "a3" + 1] ,

where "a1", "a2", and "a3" are the respective atomic densities (number of Cr, Fe, or Ni atomsper unit volume) in the elemental (reduced form) divided by the atomic densities in the oxideform for Cr, Fe, and Ni respectively. The values of "a1," "a2," and "a3" are 2.15, 2.01, and 1.70respectively.

4.3.9 Organic Material—Characterization of residual organic material on the electropolished surfacesis done using high resolution scans of the C(1s) spectral region (window) typically from 275 to295 eV, using data acquisition parameters sufficient to achieve a peak width for Au 4f7/2(FWHM) of 1.0 or better, and an energy resolution of better than 0.2 eV per channel (datapoint). Data acquisition times should be sufficient to achieve a total integrated signal in the peak

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envelope of 10,000 counts. Curve fitting routines (peak deconvolution) are used to estimate therelative peak areas associated with each of the chemical forms.

The chemical assignments for organic compounds can be determined from the analysis ofstandards. Moreover, accepted chemical peak shifts have been reported in the literature.Differential charge correction can be accomplished by setting the aliphatic peak in the carbon 1shigh-resolution spectrum to 285.0 eV (or 284.6 eV). With the aliphatic peak set to 285.0 eV, thecorresponding chemical shifts are:

Approximate Peak Position (eV) Chemical Assignment

285.0 C-C, C=C, C-H (aliphatic, unsaturated carbon)

286.4 C-O (ether, alcohol)

288.0 CONH2

288.2 C=O (carbonyl)

289.0 COO- (ester)

290.0 CO22- (carbonate)

A representative carbon C(1s) spectrum is shown in Figure 5.

4.3.9.1 Documentation of carbon species should include the atomic percent abundance of each of theabove functional groups as determined from curve fit spectra and the relative surface abundanceof carbon as determined from elemental composition data.

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4.4 Data Presentation—The key figure–of–merit measurements determined from this method are asfollows:

• The elemental Cr/Fe ratio and Cr oxide/Fe oxide species ratio in the "as-received"detection volume using high resolution measurements

• The elemental surface composition of the "as-received" surface using the 0 to 1100 eVsurvey scan

4.4.1 Hard copy reports must accompany the measurements and clearly:

• Show sample identification

• Outline experimental details

• Describe all spectral labelling

• Include all pertinent numerical results in tabular form:

• Surface elemental composition

• Cr/Fe elemental ratios

• Oxide/reduced species ratios for Cr, Fe, and Ni

Figures are to be mounted with captions. Worksheets or annexes explaining how values werecalculated are to be included. All reports must indicate:

• The name of the individual who performed the analyses

• The date of the analyses

• The serial number of the instrument used for verification of calibration

It is recommended that each report include a table that describes all experimental parameters,including:

• Settings

• X-ray source (Al or Mg)

• Monochromatized or nonmonochromatized

• Resolution settings

• Beam size

• Data acquisition time

• All pertinent sensitivity factors, calibrations, and calculations.

4.4.2 Thoroughly describe the data acquisition conditions. Use standard reference materials forcalibration. Document all calibration results in a log book.

4.4.3 Use of the AVS AES/XPS Contributors Form, reproduced in Appendix X1 (see Figure X1.1), isoptional.

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5. Illustrations

Figure 1 Illustration of Typical XPS Survey Spectrum

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Figure 2 Illustration of Typical Cr High Resolution Spectrum

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Figure 3 Illustration of Typical Fe High Resolution Spectrum

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Figure 4 Illustration of Typical Ni High Resolution Spectrum

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Figure 5 Illustration of Typical C High Resolution Spectrum

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Figure 6 Calibration of Sensitivity Factors Using Measurements from ReferenceStandards

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Figure 7 Schematic

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A1. Reference Standards for Calibration of XPS Spectrometers

A1.1 Purpose—To describe sample materials and procedures for ensuring that elementalcomposition measurements from XPS spectrometers, especially Cr, Fe, and Ni, are asaccurate and precise as possible.

A1.2 Clean copper and gold should be used to accurately calibrate the binding energy scale ofthe XPS instrument where the Au (4f7/2) and Cu(2p3/2) peaks are assigned as 83.93 and932.47 eV, respectively.

Two polymers, Teflon tape and high molecular weight dimethyl silicone, can be used asprimary standards to determine sensitivity factors for elements with spectral lines in thebinding energy range from 90 to 700 eV. This binding energy encompasses C, O, Cr,and Fe and is close enough to nickel (853 eV) to ensure reasonably accurate sensitivityfactors for elements typically observed on stainless steel surfaces.

A1.3 The following procedure is adapted for calibrating sensitivity factors for an XPSspectrometer which uses a truncated sphere hemispherical analyzer. While some of theprocedures described below are not directly applicable to all XPS spectrometers, thismethod is intended as a guide for determining sensitivity factors for elements commonlyobserved on electropolished stainless steel surfaces.

A1.3.1 Teflon tape, polytetrafluoroethylene (PTFE), with a stoichiometry of CF2 with minimaladsorbed hydrocarbon should be used. The C(1s) spectrum should be measured to verifythat the C–C/C–H peak at 285 eV represents less than five percent of the total C(1s)counts from 275 to 295 eV.

A1.3.2 High molecular weight dimethyl silicone (1,000,000 Daltons) evenly spread as a thinfilm on aluminum foil, with a stoichiometry of C2SiO and with essentially nocontamination from hydrocarbon should be used.

A1.3.3 XPS spectral measurements on Teflon should include F(2s) at 33 eV, C(1s) at 293 eV,and F(1s) at 689 eV. The C(1s) sensitivity factor is assigned as 1.00, and the F(1s) andF(2s) sensitivity factors are calculated to give CF2 stoichiometry.

A1.3.4 XPS spectral measurements of dimethyl silicone should include O(2s) at 25 eV, Si(2p) at102 eV, Si(2s) at 153 eV, C(1s) at 285 eV, and O(1s) at 533 eV. The C(1s) sensitivityfactor is assigned as 1.00, and the O(2s), Si(2p), Si(2s), and O(1s) sensitivity factors arecalculated to give the proper stoichiometry: (C2SiO).

[Note: When determining sensitivity factors for each of the spectral lines above, XPSmeasurements must be acquired at the instrument settings used for measuring data fromreal samples. Since the overall surface composition from survey data (e.g., high countrate low resolution mode) and calculation of the Cr/Fe elemental and metal/oxide speciesratios from high resolution data(e.g., low count rate high resolution mode) are run at twodifferent instrument settings, the Teflon and dimethyl silicone will also have to beanalyzed at these two settings. A separate set of sensitivity factors will exist for highcount rate/low resolution and low count rate/high resolution modes. Measure, record,and use the appropriate set of sensitivity factors for the overall composition and Cr/Feelemental and species ratio measurements.]

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A1.4 This section describes calibration of sensitivity factors for elements other than C, O, Si,and F from Teflon and dimethyl silicone polymer materials. It is intended to calibrateXPS spectrometers (using a monochromatic aluminum k alpha X-ray source) for cases inwhich transmission function changes exponentially with kinetic energy. For eitherinstrument acquisition mode, a calibration curve can be plotted from which all otherelemental sensitivity factors can be determined by interpolation or extrapolation.

This calibration curve is a plot of sensitivity factor (as determined from Teflon anddimethyl silicone) divided by the Scofield photoelectron cross section (the y–variable)vs. ln [peak kinetic energy/C(1s) kinetic energy] (the x–variable). If all spectral lines aremeasured for Teflon and dimethyl silicone, the plot will comprise seven measurementsfrom O(2s), ln (1461 eV/1201 ev), to F(1s), ln (803 eV/1201 eV). The sensitivity factorof an unknown line, such as nitrogen, chromium, or iron, is calculated by multiplying theScofield cross section for that line by the y–value at the ln of the particular photopeakkinetic energy/1201 eV (kinetic energy of C(1s).

A typical calibration plot showing results of silicone and Teflon measurements andinterpolation of Cr and Fe sensitivity factors is shown in Figure 6.

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X1. AVS AES/XPS Contributors Form for Reporting Test Results

X1.1 The AES/XPS Contributors Form (Abbreviated Version) prepared by the DatabaseCommittee of the American Vacuum Society (Editors: Charles E. Bryson III and GaryE. McGuire) may be used for reporting all test results. The original purpose of this formis to provide a standard form for submitting AES/XPS data records to Surface ScienceSpectra, an international journal electronically archiving surface science spectra oftechnological and scientific interest and distributing hard copies of selected surfacespectroscopy data files quarterly. The goal of the form is to adequately describe theconditions under which the reported spectra were collected so that others can repeat themfrom the information provided on the form alone. Because of its thoroughness and of thedesire to promote uniform reporting of results, the major sections of this form areadopted as the format for reporting the test results of this test method. (Sections A & Gof the AVS Contributors Form are not deemed necessary for reporting test results and areomitted.)

X1.2 The form lists five levels of entries keyed as follows:

Level 1: Mandatory entry - An entry must be made, even if the only valid entry isN/A (not applicable). The absence of an entry is not equivalent to entering zero,none, or N/A.

Level 2: Mandatory entry - An entry must be made unless there are specialconsiderations. Failure to make an entry would be acceptable only if the datarecord were of such unusual technical importance that it should be archived, evenin the absence of some data entries at this level. All entries in the form at thislevel are usually required to establish the utility or significance of a data record.

Level 3: Recommended entry - An entry, though not required, is important toreaders who wish to have a complete interpretation of the data record.

Level 4: Recommended entry - An entry allows the most critical uses of the datarecord.

Level 5: Optional entry - An entry should be made at the author’s discretion (e.g.,see Field 16, Section B).

All level 1 and 2 entries must be completed in reporting the test method results. Level 3-5 entries are optional.

X1.3 Figure X1.1 reproduces the sheets of the AVS AES/XPS Contributors Form(Abbreviated Version) appropriate for reporting the test results of this test method.

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Figure X1.1 AVS AES/XPS Contributors Form (Page 1 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 2 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 3 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 4 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 5 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 6 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 7 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 8 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 9 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 10 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 11 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 12 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 13 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 14 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 15 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 16 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 17 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 18 of 19)

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Figure X1.1 AVS AES/XPS Contributors Form (Page 19 of 19)

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NOTICE: SEMATECH DISCLAIMS ALL WARRANTIES, EXPRESS OR IMPLIED,INCLUDING THE IMPLIED WARRANTIES OF MERCHANTABILITY AND FITNESS FORA PARTICULAR PURPOSE. SEMATECH MAKES NO WARRANTIES AS TO THESUITABILITY OF THIS METHOD FOR ANY PARTICULAR APPLICATION. THEDETERMINATION OF THE SUITABILITY OF THIS METHOD IS SOLELY THERESPONSIBILITY OF THE USER.

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