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Comparing SDD vs Si(Li) @ Eo = 300 keV

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Nanochemistry of Phases in Obsidian (MMF is Important here)

200 nm

Log

Scale

O

Na

Al

Cl

Si

KCa

Fe

Ti

MnYb Hf

Ce

Y, S, Bi

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Element Z 10nm 50nm 100nm 500nm50nm 100nm 500nmElementElementCarbon

ZZ6

10nm10nm0.16

50nm50nm1.8

100nm100nm5.13

500nm500nm57.4Carbon

Aluminium 613

0.160.26

1.81.9

5.138.12

57.490.9Aluminium Aluminium

Copper 131329

0.260.260.68

1.91.97.6

8.128.1221.4

90.990.9*Copper Copper

Gold 2979

0.6815.5

7.617.3

21.4* *

*model invalid at higher kV and/or high scattering angles

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100 kV

Spatial Resolution /Beam Spreading Monte Carlo Calculations

DC Joy's MC Program

Al

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Monte Carlo Calculations of Monte Carlo Calculations of BB (Newbury & Myklebust (Newbury & Myklebust -(Newbury & Myklebust -1979)Monte Carlo Calculations of Monte Carlo Calculations of B (Newbury & Myklebust (Newbury & Myklebust (Newbury & Myklebust (Newbury & Myklebust (Newbury & Myklebust 1979)1979)1979)

ThicknessElement Z 10nm

Thickness50nmThickness

100nm 500nmElement Z 10nm 50nm 100nm100nm 500nm

Carbon 6 0.22 1.9 4.1 33.0Carbon Aluminium

613

0.220.41

1.93.0

4.17.6

33.066.4Aluminium Aluminium

Copper 1329

0.410.78

3.05.8

7.617.5

66.4244.0Copper Copper

Gold 292979

0.780.781.71

5.85.815.0

17.517.552.2

244.0244.01725.0

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Spectral ProcessingThin Film Quantification MethodsSpecimen Thickness Effects:

AbsorptionFluorescence

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Spectrum = Characteristic Peaks + Background

Data Reduction

Simple: Linear Background Fit & Integration

Curve Fitting: Non-Linear Background & Profile Matching

Frequency (Digital) Filtering: Background Suppression& Reference Spectra Fitting

Deconvolution: Fourier Method for Resolution Enhancement

Background Modeling

Simple - Linear and/or Polynominal Interpolation

Modeling - Parametric Fits of Analytic ExpressionsPhenomenological ExpressionsModified Bethe Heitler ModelDigital Filtering - Mathematical Supression

a*

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Recall that for a Gaussian Peak

Hence for the ratio of Intensities

Spectral Processing : XEDSSimple Data Reduction

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bK92(K)1(89< /UC8(01K(KT<4J8)/J0<68[


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Quantitative Analysis Equations

For a thin specimen

IIA = Measured xMeasured x-Measured x-ray intensity Measured xMeasured xMeasured x-ray intensity ray intensity ray intensity per unit area

- = KKthKthKthK -per unit areaper unit areaper unit areaper unit areaper unit areaper unit area

th-shell ionization crossshell ionization cross-shell ionization crossshell ionization cross-section-.

==

KKKKKthKKKththKthK -

shell ionization crossshell ionization crossshell ionization crossshell ionization crossshell ionization crossshell ionization cross-sectionsectionsectionshell ionization crossshell ionization cross-shell ionization crossshell ionization crossshell ionization crossthth shell fluorescence yield..

/===

KKKKKKKthKthKthKKKKththKthK -

shell fluorescence yieldshell fluorescence yieldshell fluorescence yieldshell fluorescence yieldshell fluorescence yieldshell fluorescence yieldshell fluorescence yieldshell fluorescence yieldth-shell fluorescence yieldshell fluorescence yieldshell fluorescence yield-shell fluorescence yieldshell fluorescence yieldthth-shell radiative partition function//

W==

KKKKKK -shell radiative partition functionshell radiative partition functionshell radiative partition functionshell radiative partition functionshell radiative partition functionshell radiative partition functionshell radiative partition functionshell radiative partition functionAtomic WeightWW

NNo

===

Atomic WeightAtomic WeightAtomic WeightAtomic WeightAtomic WeightAtomic WeightAvagodro's numberNNNNooNoNNoN

(===

Avagodro's numberAvagodro's numberDensity((

C==

DensityDensityComposition (At %)CC

%%o

===

Composition (At %)Composition (At %)Incident electron flux%%%oo

t===

Incident electron fluxIncident electron fluxSpecimen thicknesstt

'= = =

Specimen thicknessSpecimen thicknessDetector efficiency''

0===

Detector efficiencyDetector efficiencyDetector solid angle

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a;83 38</#& &k$"0827 3 0"0&3 0;"0 0;& 1&#"08P& 870&73804 1"08 2 2@ "74 0Y2';"1"'0&18308' \)1"4 #87&3 83 I81&'0#4 /12/210827"# 02 0;& 1&#"08P& '2</23808 271"082 2@ 0;&81 &#&<&70"# '2</27&703 <$#08/#8&I :4 32<& l'273 0"703l "7I 8387I&/&7I&70 2@ 0;8'T7&33K

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K-Factor Calculation Experiment

vsTheory

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Variation in Measured Composition on 308 SS for Different Labs

Example in which KExample in which K-Example in which K-Example in which K-Example in which K factor is stable Example in which KExample in which KExample in which K-Example in which K-Example in which K factor is stable factor is stable factor is stable Cr, Fe, Ni Cr, Fe, Ni Cr, Fe, Ni Cr, Fe, Ni Cr, Fe, Ni

Note: Detector efficiency ~ 100% in this energy range

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Variation in K-factor with AEM/Detector SystemSpecimen: Uniform NiO film on Be Grid

From: Comparison of UTW/WL XFrom: Comparison of UTW/WL X-From: Comparison of UTW/WL X-ray Detectors on TEM/STEMs and STEMs

Thomas, Charlot, Franti, GarrattThomas, Charlot, Franti, Garratt-Thomas, Charlot, Franti, Garratt-Reed, Goodhew, Joy, Lee, Ng, Plicta, Zaluzec.Thomas, Charlot, Franti, GarrattThomas, Charlot, Franti, GarrattThomas, Charlot, Franti, Garratt-Reed, Goodhew, Joy, Lee, Ng, Plicta, Zaluzec.Reed, Goodhew, Joy, Lee, Ng, Plicta, Zaluzec.Reed, Goodhew, Joy, Lee, Ng, Plicta, Zaluzec.Analytical Electron Microscopy

Reed, Goodhew, Joy, Lee, Ng, Plicta, Zaluzec.Analytical Electron MicroscopyAnalytical Electron Microscopy-

Reed, Goodhew, Joy, Lee, Ng, Plicta, Zaluzec.Reed, Goodhew, Joy, Lee, Ng, Plicta, Zaluzec.Reed, Goodhew, Joy, Lee, Ng, Plicta, Zaluzec.Analytical Electron MicroscopyAnalytical Electron Microscopy-1984 1 09876543210

0.0

0.2

0.4

0.6

0.8

1.0

X-ray Photon Energy (keV)

Calc

ulat

ed

Det

ecto

r Ef

fici

ency

S i ( L i )

HP GeDetector Parameters

Be Window: 0 nmGold Contact: 20 nmSi Dead Layer: 100 nmSi Active Layer: 3 mmGe Dead Layer: 200 nmGe Active Layer: 3 mm

20

30

40

50

60

70

80

0 1 2 3 4 5 6 7 8

NiO

Co

mp

osi

tio

n (

At

%)

Lab

513

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AR10<10<.R/<wY/0.w<)/.RKLW<YH.M 0C/D1)/(<DK)CK01.1K(<)H0.<Y/<Z/J1T1/L<1(L/C/(L/(.92M )H0.<R8Z/<8<0.8(L8JL<TKJ</Z/J2</9/)/(.<.K<Y/<0.HL1/L

H.1%/1(20)8"$)80=8)(2%&'

P../)C.<T1J0.<CJ1(D1C9/0<D89DH98.1K(<:(K[1(S0K)/<TH(L8)/(.89<C8J8)/./J0<KT<.R/?<020./)

=.8J.<[1.R<8<91)1./L<(H)Y/J<KT<<:PG<T8D.KJ<)/80HJ/)/(.0W<.R/(<T1.<.R/?<C8J8)/./J0<.K<Y/0.<)8.DR<.R/<L8.8I<>U.J8CK98./<.K<020./)0<[R/J/<)/80HJ/)/(.0<8(L"KJ<0.8(L8JL0<LK<(K.</U10.I

M G1(.%>"CI<VfK9L0./1(</.89X<<P00H)/<Z89H/0<TKJ</,.,' 8(L<L/./J)1(/<.R/<Y/0.<- .K<T1.<:PGI<AR10<CJKD/LHJ/< /00/(.18992<1./J8./0<.R/<T1.<KT<0<.K<.R/<L8.8I

G1(.%>"+I VQ89Hh/DX<P00H)/<Z89H/0<TKJ</,.,- L/./J)1(/<.R/<Y/0.<' .K<T1.<:PGI<AR10<CJKD/LHJ/< /00/(.18992<1./J8./0<.R/<T1.<KT</<VL/./D.KJ<[1(LK[<C8J8)/./J0X<<.K<.R/<L8.8I

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Sources of values for kSources of values for kAB AB AB CalculationsSources of values for kSources of values for kAB Sources of values for kAB CalculationsCalculationsAB Calculations

W -- International Tables of Atomic Weights

//(K) -- Schreiber and Wims , XSchreiber and Wims , X-Schreiber and Wims , X-ray Spectroscopy (1982)Schreiber and Wims , XSchreiber and Wims , XSchreiber and Wims , X ray Spectroscopy (1982)ray Spectroscopy (1982)ray Spectroscopy (1982)Vol 11, p. 42

//(L) -- Scofield, Atomic and Nuclear Data Tables (1974)Scofield, Atomic and Nuclear Data Tables (1974)Vol 14, #2, p. 121

.. (K) (K) -- Bambynek etal, Rev. Mod. Physics, Vol 44, p. 716Bambynek etal, Rev. Mod. Physics, Vol 44, p. 716Freund, X

Bambynek etal, Rev. Mod. Physics, Vol 44, p. 716Freund, XFreund, X-

Bambynek etal, Rev. Mod. Physics, Vol 44, p. 716Bambynek etal, Rev. Mod. Physics, Vol 44, p. 716Bambynek etal, Rev. Mod. Physics, Vol 44, p. 716Freund, XFreund, X-ray Spectrometry, (1975) Vol 4, p.90

..(L) -- Krause, J. Phys. Chem. Ref. Data (1974) Vol 8, Krause, J. Phys. Chem. Ref. Data (1974) Vol 8, p.307

--(Eo) -- Inokuti, Rev. Mod. Physics, Inokuti, Rev. Mod. Physics, 4343, 4343 No. 3, 297 (1971)Inokuti, Rev. Mod. Physics, -

Inokuti, Rev. Mod. Physics, Inokuti, Rev. Mod. Physics, 4343Inokuti, Rev. Mod. Physics, 4343Inokuti, Rev. Mod. Physics, - Goldstein etal, SEM

43434343Goldstein etal, SEM Goldstein etal, SEM Goldstein etal, SEM Goldstein etal, SEM 1

No. 3, 297 (1971)No. 3, 297 (1971)No. 3, 297 (1971)43, No. 3, 297 (1971)No. 3, 297 (1971)43, 11, 315, (1977)

-Goldstein etal, SEM Goldstein etal, SEM Goldstein etal, SEM Goldstein etal, SEM

- Chapman etal, XGoldstein etal, SEM Goldstein etal, SEM Chapman etal, X-Goldstein etal, SEM Goldstein etal, SEM , 315, (1977) , 315, (1977) , 315, (1977) , 315, (1977) , 315, (1977) 1, 315, (1977) , 315, (1977) , 315, (1977) Goldstein etal, SEM Goldstein etal, SEM Goldstein etal, SEM Goldstein etal, SEM Goldstein etal, SEM Goldstein etal, SEM Goldstein etal, SEM Goldstein etal, SEM Chapman etal, X-ray Spectrometry, ray Spectrometry, 121212,153,(1983)

-Chapman etal, XChapman etal, XChapman etal, XChapman etal, X

- Rez, XChapman etal, XChapman etal, XRez, X-Chapman etal, XChapman etal, XChapman etal, XChapman etal, XChapman etal, XChapman etal, X ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, Chapman etal, XChapman etal, XChapman etal, XChapman etal, XRez, X-ray Spectrometry,

ray Spectrometry, ray Spectrometry, ray Spectrometry, 13

ray Spectrometry, ray Spectrometry, 13,

ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, 12121212,153,(1983),153,(1983)121212,153,(1983)ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, 13, 55, (1984)

-Rez, XRez, XRez, XRez, XRez, XRez, X ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, ray Spectrometry, Rez, XRez, X

- Egerton, Ultramicroscopy, 1313

Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, 455, (1984)55, (1984)55, (1984)55, (1984)55, (1984)55, (1984)55, (1984)55, (1984)55, (1984)55, (1984)55, (1984)1313, ,

4444, 169, (1969)-

Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, - Zaluzec, AEM

Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, Zaluzec, AEMZaluzec, AEM-Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, 44, 169, (1969), 169, (1969), 169, (1969), 169, (1969), 169, (1969), 169, (1969), 169, (1969)4, 169, (1969)Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, Egerton, Ultramicroscopy, Zaluzec, AEMZaluzec, AEM-1984, San Fran. Press. 279, (1984)

'' (E) -- Use mass absorption coefficients from:Use mass absorption coefficients from:-

Use mass absorption coefficients from:Use mass absorption coefficients from:-Thinh and Leroux; X

Use mass absorption coefficients from:Thinh and Leroux; X-

Use mass absorption coefficients from:Use mass absorption coefficients from:Use mass absorption coefficients from:Thinh and Leroux; X-ray Spect. (1979), ray Spect. (1979), 8,8, p. 963

-Thinh and Leroux; XThinh and Leroux; XThinh and Leroux; XThinh and Leroux; XThinh and Leroux; XThinh and Leroux; X ray Spect. (1979), ray Spect. (1979), ray Spect. (1979), ray Spect. (1979), ray Spect. (1979), ray Spect. (1979), Thinh and Leroux; XThinh and Leroux; X

-Henke and Ebsiu, Adv. in Xray Spect. (1979), ray Spect. (1979),

Henke and Ebsiu, Adv. in X-ray Spect. (1979), ray Spect. (1979), ray Spect. (1979), ray Spect. (1979), ray Spect. (1979), ray Spect. (1979),

Henke and Ebsiu, Adv. in X-ray Analysis,ray Spect. (1979), 8,8, p. 963

ray Analysis,ray Analysis,ray Analysis,ray Analysis,17,p. 963p. 963p. 963p. 963

17,17, (1974)-Henke and Ebsiu, Adv. in XHenke and Ebsiu, Adv. in XHenke and Ebsiu, Adv. in XHenke and Ebsiu, Adv. in XHenke and Ebsiu, Adv. in XHenke and Ebsiu, Adv. in XHenke and Ebsiu, Adv. in XHenke and Ebsiu, Adv. in X

-Holton and Zaluzec, AEMHenke and Ebsiu, Adv. in XHenke and Ebsiu, Adv. in XHolton and Zaluzec, AEMHolton and Zaluzec, AEM-

ray Analysis,ray Analysis,ray Analysis,ray Analysis,ray Analysis,ray Analysis,ray Analysis,ray Analysis,ray Analysis,ray Analysis,17,17,17,17, (1974)(1974)(1974)(1974)ray Analysis,ray Analysis,17,17,17, (1974)ray Analysis,ray Analysis,Henke and Ebsiu, Adv. in XHenke and Ebsiu, Adv. in XHenke and Ebsiu, Adv. in XHenke and Ebsiu, Adv. in XHenke and Ebsiu, Adv. in XHenke and Ebsiu, Adv. in XHolton and Zaluzec, AEMHolton and Zaluzec, AEM--1984, San Fran Press,353,(1984)

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Quantitative Analysis using XEDSStandards based Method

Invoke the Intensity Ratio Method, that is consider the ratio of x-ray lines from the same element in both the Unknown and a Standard

This simple equation states that the relative intensity ratio of the samecharacteristic x-ray lines is directly proportional to the relativecomposition ratio of the elemental components mult iplied by aproportionality factor which, in the thin film approximation, isdependent upon , (, t and %

NOTE: The factor also is not a universal constant, and requires an accurate measurement/determination of density, thickness and beam current.

IAUnknown

IAS tandard =

CAU!U"UtU

"

CAS!S" StS

"

=#SU CA

U

CAS

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Quantitative Analysis using XEDS2 =factor Method

! t =IA

K!WA

! A (E, Z )!A!A( ) CANo( ) not( ) !A"( )=!A

IAK!

CAno( )

Rearrange the Intensity Equation

?I<O8.8(8Y/<j<@IGI<O19918)0W<iI<?1DJK0DI<&&#<V&''!X<B%M#'%I

Recognize

!A =WA

! A (E, Z )!A!A( ) No( ) !A"( )

With

A

CA )Ano )

)( )!A"( )

1 098765432100.0

0.2

0.4

0.6

0.8

1.0

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