Electron Microprobe Analysis X-ray spectrometry:
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1 Electron Microprobe Analysis X-ray spectrometry: 1. X-ray generation and emission 2. X-ray detection and measurement
2 X-ray energy and wavelength E=hν h : Planck's constant (6.626x10-34 Joule.sec or, 6.626x10-34 /1.6021x10-16 kev.sec) ν : frequency (= c/λ) (c : speed of light in vacuum = x10 17 nm/sec λ : wavelength) λ (nm) = c/ν = hc/e = /E (kev)
3 The electromagnetic spectrum UMα 3.17 kev 0.39 nm SiKα 1.74 kev 0.71 nm λ (nm) = /E (kev)
4 Characteristic X-ray X generation Inner-shell ionization X-ray and electron transition Kα: L to K-shellK Lα: M to L-shellL Mα: N to M-shellM Kβ: M to K-shellK Lβ: N to L-shellL K-shell L-shell Ti KαK Fe KαK Flowchart for X-ray generation Ti KβK Fe KβK
5 Overvoltage U = E/E c where, E is the beam energy (usually kev) E c : critical excitation energy or absorption edge of the shell Condition for inner shell ionization : U > 1
6 Kα Lα Mα kev
7 Inner-shell ionization cross-section section Q = 6.51x10-20 [(n s b s )/(UE 2 c )] ln(c s U ) Q : Cross section n s : # electrons in the shell b s,c s : constants
8 Inner-shell ionization cross-section section Al K-shell Best analytical condition, U 5 E c = 1.84 kev
9 X-ray production range An analogous expression to the electron range ( R = KE n 0 /ρ ) X-ray Range: R = K(E 0n - E n c )/ρ where, K = 0.064, n = 1.68 Always smaller than electron range
10 X-ray depth-distribution: distribution: φ(ρz) ρ = density z = depth φ(δρz) = X-ray intensity generated in a freestanding layer φ(ρz) at depth z = Intensity from depth z divided by φ(δρz)
11 Wavelength Dispersive Spectrometer (WDS) WDS WDS detector crystal
12 Bragg s s Law d = lattice spacing θ = angle of diffraction n = order of diffraction (any integer) nλ = 2 2d sin θ = path length ABC
13 WDS: Focusing geometry angle of diffraction take-off angle L = nλ.r/d
14 WDS: Analyzing crystals Name 2d (Å) Type Elements usually analyzed LDEC 98 Ni/C Multi-layer B-O (Kα), optimized for C analysis STE Pb stearate B-O (Kα), optimized for C analysis LDE W/Si Multi-layer C-F (Kα), optimized for O analysis TAP 25.8 Thallium acid phthalate Na-P (Kα); Cu-Zr (Lα); Sm-Au (Mα) PET Pentaerythritol S-Mn (Kα); Nb-Pm (Lα); Hg-U (Mα) LIF Lithium fluoride Ti-Rb (Kα); Ba-U (Lα)
15 Curved diffracting crystals Johansson type bending curvature: 2R polished and ground to R R Johan type only bent to 2R, not ground FWHM of fully focusing Johansson-type crystal ~10 ev Some defocusing in Johan-type, but resolution is not compromised
16 WDS: Analyzing crystals Vertical, horizontal and tilted spectrometers
17 WDS: X-ray X detector (proportional counter) Flow proportional counter
18 WDS detector: Proportional counter Tungsten collection wire set at kv bias Flow counter: 90% Ar +10% CH 4 (P-10); poly-propylene propylene window Sealed counter: Xe or Kr; Be window
19 Amplification in proportional counter Collection wire bias range (applied potential): kv (Bias) Bias is set so that amplification is in the proportional region
20 Counting efficiency of gas in proportional counter Heavy elements Light elements Gas used for long wavelengths: 90% Ar +10% CH 4 (P-10) Gas used for short wavelengths: Xe or Kr
21 WDS: changing the angle of diffraction
22 Theoretical and actual limits of spectrometer movement
23 WDS signal processing Single channel analyzer (SCA) and pulse height analysis (PHA) window baseline Only pulses in this voltage interval are counted
24 WDS: PHA setup Single Channel Analyzer (SCA) scan
25 Imaging with X-rays: X compositional mapping Mg Na Ca Ti Beam-rastered image: electron beam rasters over the area to be imaged Stage-rastered image: electron beam is stationary, stage moves
26 X-ray image artifact: background Zn-Sn composite
27 Continuum X-rays X (background) Characteristic X-raysX Continuum X-rays Generated by deceleration of beam electrons in the Coulombic field of outer shells of target atoms. X-ray background (maximum energy = electron beam energy, E0) E
28 Continuum X-rays: X background artifact A composite made of 2 materials is being mapped: 1 2 Neither material contains Cr But background counts for Cr : in 1 in 2 Therefore, if a Cr X-ray X map is acquired, material 2 will show higher Cr than material 1
29 Defocusing in beam-rastered WDS X-ray X maps
30 Stage-rastered X-ray mapping parameters Resolution : # pixels (step size) Signal: beam current and dwell time/point Acquisition time increases as resolution increases as dwell time/point increases
31 Large area stage-rastered images BSE O Mg Ca Resolution: 20 μm/step Image size: 30mm x 15mm #steps (pixels): 1500x750 Dwell time: 30 msec/point Beam current: 30 na Voltage: 15 kv Avg stage speed: 0.71 mm/sec Acquisition time: 14 hrs Scale bar: 4 mm
32 MIT OpenCourseWare Electron Microprobe Analysis by Wavelength Dispersive X-ray Spectrometry January (IAP) 2010 For information about citing these materials or our Terms of Use, visit:
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