Practical XRay Diffraction uocgr实际的X射线衍射uocgr.pptVIP

Practical X-Ray Diffraction Prof. Thomas Key School of Materials Engineering Instrument Settings Source Cu Kα Slits Less than 3.0 Type of measurement Coupled 2θ Detector scan Etc. Angle Range Increment Rate (deg/min) Detector LynxEye (1D) Coupled 2θ Measurements In “Coupled 2θ” Measurements: The incident angle w is always ? of the detector angle 2q . The x-ray source is fixed, the sample rotates at q °/min and the detector rotates at 2q °/min. Angles The incident angle (ω) is between the X-ray source and the sample. The diffracted angle (2q) is between the incident beam and the detector. In plane rotation angle (Φ) Bragg’s law and Peak Positions. For parallel planes of atoms, with a space dhkl between the planes, constructive interference only occurs when Bragg’s law is satisfied. First, the plane normal must be parallel to the diffraction vector Plane normal: the direction perpendicular to a plane of atoms Diffraction vector: the vector that bisects the angle between the incident and diffracted beam X-ray wavelengths l are: Cu Kα1=1.540598 ? and Cu Kα2=1.544426 ? Or Cu Kα(avg)=1.54278 ? dhkl is dependent on the lattice parameter (atomic/ionic radii) and the crystal structure Ihkl=IopCLP[Fhkl]2 determines the intensity of the peak Sample Preparation(Common Mistakes and Their Problems) Z-Displacements Sample height matters Causes peaks to shift Sample orientation of single crystals Affects which peaks are observed Inducing texture in powder samples Causes peak integrated intensities to vary Sample Preparation Crystal Orientation Matters Sample Preparation Inducing Texture In A Powder Sample Preparing a powder specimen An ideal powder sample should have many crystallites in random orientations the distribution of orientations should be smooth and equally distributed amongst all orientations If the crystallites in a sample are very large, there will not be a smooth distribution of crystal orientations. You will not get a powder average diffraction pattern.