Scanning Electron Microscopy and X-Ray Microanalysis

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a24 000
22 000
20 000
18 000
16 000
14 000
12 000
10 000
8 000
6 000
4 000
2 000
0
3.0 3.5 4.0 4.5 5.0
Photon energy (keV)

Counts

5.56.0 6. 57 .0

K2496
O
Si
Ti
Ba
Ba/Ti =

0.323
0.229
0.018
0.430
23.9

K2496 glass
E 0 = 10 kev
1000 nA-s
0.1-10keV integral = 12,175,000 counts
SiO 2
BaSi 2 O 5 (Sanbornite) for Ba
Ti

b

0

1 000

2 000

3 000

4 000

5 000

6 000

Counts

3.0 3.2 3.4 3.6 3.8 4.0 4.2 4.4 4.6 4.8 5.0 5.2 5.4 5.6 5.8 6.0 6.2 6.4 6.6 6.8 7.0
Photon energy (keV)

K2496 glass
SiO 2
BaSi 2 O 5 (Sanbornite) for Ba
No peak fitting for Ti

K2496_1_10kV20nAMED73kHz8DT_100s
Residual_K2496_1_10kV20nAMED73kHz8DT_100s]

K2496_10kV20nA8%DT
Residual_K2496_10kV20nA8%DT

. Fig. 20.8 a SDD-EDS spectrum of NIST microanalysis glass K2496
(red) at E 0 = 10 keV (12,175,000 counts) and residual (blue) after DTSA II
analysis using BaSi2O 5 (sanbornite) and Ti as fitting references and stan-


dards. b Same analysis protocol, but not including Ti in the peak-fitting.
Note low level peaks for Ti K-L2,3 and Ti K-M 3 (Ba L-family peaks marked
as green lines)

. Table 20.8 Analysis of NIST microanalysis glass K2496 at E 0 = 10 keV with Ti and sanbornite (BaSi 2 O 5 ) as fitting references and
standards; integrated spectrum count = 12,175,000. Analysis performed with O K- L2,3, Si K-L2,3, Ti K-L2,3 and Ba L 3 -M4,5


O Si Ti Ba

Cav (atom frac) 0.6228 0.2585 0.01171 0.1069
Z-correction 0.984 0.983 0.983 0.98
A-correction 0.966 1.017 0.986 1.001
F-correction 1 1 1.01 1
σ (7 replicates) 0.000158 0.000277 0.000217 0.000226
σRel (%) 0.03 % 0.11 % 1.80 % 0.21 %
RDEV (%) −1.70 % 0.99 % −0.64 % 8.70 %
C (mass frac) 0.3066 0.223 0.0177 0.4527
Counting error, std 0.0002 0.0002 1.10×10–5 0.0008
Counting error, unk 0.0002 0.0001 0.0004 0.0007
A-factor error 0.0021 8.80×10–5 3.90×10–6 1.20×10–5
Z-factor error 0.0003 2.70×10–5 1.80×10–7 4.00×10–6
Combined errors 0.0021 0.0002 0.0004 0.0011

Chapter 20 · Quantitative Analysis: The SEM/EDS Elemental Microanalysis k-ratio Procedure for Bulk Specimens, Step-by-Step
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