X-ray Diffraction. X-ray Generation X-ray tube (sealed) Pure metal target (Cu) Electrons remover inner-shell electrons from target. Other electrons “fall”

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Presentation transcript:

X-ray Diffraction

X-ray Generation X-ray tube (sealed) Pure metal target (Cu) Electrons remover inner-shell electrons from target. Other electrons “fall” into hole.

X-ray Generation The incoming electron must have enough energy to remove inner 1s electrons from the copper atoms. This energy corresponds to the Cu absorption edge The 2s and 2p electrons fall back into the 1s shell and emit the K  1 K  2 lines.

X-ray Spectrum from Tube

Energy Calculations Planck’s constant (h) = 6.6 * joule-sec 1 electron-volt = * joule Speed of light (c) = 3.0 * 10 8 m/s Photon frequency = c/ Photon Energy E = h = hc/

Energy Calculations What is the minimum potential in KV that is required to excite Cu K-series radiation from a Cu-target X-ray tube? Absorption edge of Cu = 1.380Å E = hc/ = ( )(3*10 8 )/(1.380* ) E = 1.435* joule E = 1.435* /1.6016* = 8958 ev The potential on the tube must exceed KV

Diffraction Diffraction is the coherent scattering of waves from a periodic array of scatterers. The wavelength of light is about half a micron Light is diffracted by the tracks in a CD. The wavelengths of X-rays is about the same as the interatomic distances in crystals. Crystals diffract X-rays.

X-Ray Diffraction Atoms separated by distance d will scatter in phase when the path length difference is an integral number of wavelengths. Path length difference B-C-D = n n = 2d sin 

X-ray Diffraction Experiment We use the ‘monochromatic’ K  1-2 lines for our diffraction experiment. The wavelength is Å We use a diffracted beam monochro- mator to clean up the X-rays entering the detector. We use a powdered sample so that all orientations are present in the sample. We move the detector through angle 2 .

Miller Indices The real use of Miller indices is to describe diffraction planes. For a lattice plane with Miller indices h k l in an orthorhombic lattice a b c, d = 1 / [(h/a) 2 +(k/b) 2 +(l/c) 2 ] 1/2 For cubic: d = a/[h 2 +k 2 +l 2 ] 1/2

Diffraction Calculations For forsterite a = 4.75; b = 10.20; c = 5.98Å Calculate 2  for the (201) lattice spacing for Cuk  ( = Å) d = 1 / [(h/a) 2 +(k/b) 2 +(l/c) 2 ] 1/2 d = 1/ [(2/4.75) 2 +(1/5.98) 2 ] 1/2 d = 1/ = 2.207Å 2  = 2 sin -1 /2d = 2* sin -1 (1.5405/4.414) 2  = 2 * = 40.86º

XPOW XPOW uses the unit cell and atom position data to calculate the diffraction pattern. Intensities can be calculated knowing the position and scattering characteristics of each atom. F hkl = square root of integrated intensity. f j = scattering of atom j at angle 2  Atom j located at fractional coordinates x j, y j, z j.

Uses of X-ray Powder Diffraction Mineral identification Determination of Unit Cell Parameters Modal (phase percentage) Analysis Crystal Structure Determination

X-ray Fluorescence

Chemical analysis Major and minor element Uses Ag k  to excite secondary X-rays from sample. Powdered or flux-fused glass sample.

Electron Microprobe

Chemical analysis Major and minor element Uses electrons to excite secondary X- rays from sample. Electrons can be focussed onto a 10  m spot Sample is polished thin section