XRD

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An seminar on the XRD equipment and lab process.

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XRD

  1. 1. A SEMINAR ON XRD K. GANAPATHI RAO (13031D6603) Presented By Presence of Mr. D. RAKESH
  2. 2. Introduction Constructive and Destructive Basic components Operating Procedure Shut down procedure XRD pattern Significance of Peak Applications of XRD Most important uses of XRD References
  3. 3. The atomic planes of a crystal cause an incident beam of X-rays to interfere with one another as they leave the crystal. The phenomenon is called X-ray diffraction.
  4. 4. Bragg developed a relationship in 1913 to explain why the cleavage faces of crystals appear to reflect X-ray beams at certain angles of incidence. (Roentgenstrahlinterferenzen), commonly known as X-ray diffraction (XRD), and was direct evidence for the periodic atomic structure of crystals postulated for several centuries.
  5. 5. D8 machine PC + UPS Chiller
  6. 6. Switch on system Switch on D8 machine and press green button on D8 machine Switch on chiller Click on D8 icon on system Click on “Online status” Click on “Online refresh”
  7. 7. Go to “x-Ray generator” icon Then click “X-Ray software safety capture register” Go to “Utilities” Go to “X-Ray Hardware safety capture register” through X-Ray Go to “X-Ray ware safety capture register” through X-Ray Enter password as designed “*******”, ok Go to positioning Drives Then initialize the theta, 2 theta, spinner step by step, by clicking adjust symbol
  8. 8. Switch on X-Ray generator power supply, by rotating knob in clock wise direction (4 sec, upto x-rays on) Close D8 tools window Open x-ray commander symbol Then increase kV & mA gradually, up to 40kV, 30mA Click open door for insert sample Then insert sample And give 2 theta, scan speed, step size Start Save as .raw file
  9. 9. Gradually decrease kV and mA up to 20kV, 5mA Click on Init Drives for initializing drives on main menu Close window X-ray off by rotating anticlock wise direction Shut down system Swithoff D8 power and chiller
  10. 10. Peak position Peak width Peak intensity
  11. 11. XRD is a nondestructive technique To identify crystalline phases and orientation To determine structural properties: (Lattice parameters (10-4Å), strain, grain size, expitaxy, phase composition, preferred orientation , (Laue) order-disorder transformation, thermal Expansion To measure thickness of thin films and multi-layers* To determine atomic arrangement Tooth enamel & dentine have been examined.
  12. 12. Obtain XRD pattern Measure d-spacings Obtain integrated intensities Compare data with known standards in the JCPDS file, which are for random orientations (there are more than 50,000 JCPDS cards of inorganic materials) (Joint Committee on Powder Diffraction Standards)
  13. 13. http://pubs.rsc.org/en/Content/ArticleLanding/1991/J M/jm9910100511#!divAbstract http://www.iucr.org/publ/50yearsofxraydiffraction http://en.wikipedia.org/wiki/X-ray_crystallography http://webmineral.com/help/XRayDiffraction.shtml#.U 7VsJfmSydw http://serc.carleton.edu/research_education/geochem sheets/techniques/XRD.html http://web.pdx.edu/~pmoeck/phy381/Topic5a- XRD.pdf

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