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QuantitativeQuantitativeElectron Microprobe AnalysisElectron Microprobe AnalysisGoal: Goal: Measurement of concentration Measurement of concentration
of elements in a microscopic volumeof elements in a microscopic volume
Wavelength Dispersive XWavelength Dispersive X--ray ray Spectrometry (WDS)Spectrometry (WDS)
EPMA: Analytical procedureEPMA: Analytical procedure
Sample preparationQualitative analysis with EDSStandard intensity measurement (calibration)Measurement of X-ray intensities in the specimenData reduction through matrix corrections
Sample preparationSample preparationSample cut and mounted in epoxyPolished first with coarse SiC paper, then with alumina grit slurry (final size: ≤0.25 μm) 1
Washed with water in ultrasonic cleaner 2
Dried with blow duster and airCarbon coated 3
1: diamond paste or colloidal silica for some samples; dry polishing paper for water-soluble samples
2: ethanol may be used sparingly; cleaned with blow duster and cloth for samples that dissolve in water
3: for insulators; if standards are coated, however, all samples must be coated
Carbon coaterCarbon coater
Samplechamber(bell jar)
Carbon coatingCarbon coatingTo monitor coat-thickness, a
polished brass block is coated with the samples
Carbon coatingCarbon coating
Color of the brass surface changes with carbon-coat thickness
Recommended: 225-250 Å
WDS: XWDS: X--ray intensity measurementray intensity measurement
peak minus background intensitypeak minus background intensity
A polynomial fit to the background A polynomial fit to the background may be more accuratemay be more accurate
Background modeling in XBackground modeling in X--ray spectraray spectra
Peak overlap in XPeak overlap in X--ray spectraray spectra
WDS detector optimization withWDS detector optimization withpulse height analysis (PHA)pulse height analysis (PHA)
SCA scan: baseline and window optimized throughPHA
WDS spectraWDS spectra
Peak overlap: KPeak overlap: Kαα and Kand Kββ energies (energies (keVkeV))of Ti, V and Crof Ti, V and Cr
Kα Kβ
IIIII std-Ti
std-Ti
measmeascorr
VK
TiK
TiKVKVK α
α
ααα−=
CrK CrKVK
VK
CrKcorr meas
corr
V - stdV - std
α αα
α
αI I II
I= −
Peak overlap correctionsPeak overlap corrections
MIT OpenCourseWarehttp://ocw.mit.edu
12.141 Electron Microprobe Analysis by Wavelength Dispersive X-ray SpectrometryJanuary (IAP) 2010
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