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Spectroscopy XRD

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Lesson 3 of 4 in the series of spectroscopic methods in Inorganic Chemistry

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  • very helpful, thank you! But I have a question, is the XRD characteristic peaks of graphene or graphene oxide very easily to be shielded by metal materials in composites? Because when I'm reading papers about XRD characterization of composites, the XRD pattern of metal oxide/graphene or metal oxide/graphene oxide composites didn't show peaks belonging to graphene or graphene oxide.
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Spectroscopy XRD

  1. 1. Spectroscopy XRD (X-Ray Diffraction on powders) Dr. Chris UP, Feb. 2016
  2. 2. Energy regions of electromagnetic waves
  3. 3. Different principles (1) Energy absorption E1 and E2 are different states of a molecule:  Vibrational states -> IR spectroscopy  Nuclear spin states -> NMR spectroscopy  electronic states -> UV/VIS spectroscopy
  4. 4. (2) Energy emission Raman (infrared) Fluorescence (uv)
  5. 5. (3) XRD “spectroscopy” Different principle: reflection of X-Rays on a sample
  6. 6. Generation of X-Rays The target metal defines the energy of the x-rays
  7. 7. Excitation of INNER electrons, falling back emits X-Rays Typical metals are Mo (λ = 0.07 nm) and Cu (λ = 0.154 nm)
  8. 8. XRD Principle Different planes in a crystal give different signals = positive interference of waves
  9. 9. Why 2 ϴ ? The Bragg diffraction condition contains only one factor of θ: 2dsinθ=nλ It should be noted that θ refers to the incidence angle of the x-ray beam, and the beam is actually deflected by an angle of 2θ, as illustrated in the image below:
  10. 10. Bragg’s Law
  11. 11. PLANES IN CRYSTALS MILLER INDICES
  12. 12. Crystal lattices – 3 cubic structures NaCl type
  13. 13. Movie clip: youtube.com/watch?v=pMTA_wiY784
  14. 14. Indices h k l http://slideplayer.org/slide/792387/#
  15. 15. Identify crystal layers Miller indices h k l http://www.iue.tuwien.ac.at/phd/dhar/node17.html
  16. 16. Practice Miller layers ½  2
  17. 17. Negative indices
  18. 18. Examples
  19. 19. Miller Indices Example http://www.wolframalpha.com/widget/widgetPopup.jsp?p =v&id=cc011df99e5873930ccb659743a221b&title=Calculat e%20Miller%20Indices%20for%20Planes&theme=purple&i 0=1&i1=2&i2=0&podSelect=&showAssumptions=1&show Warnings=1
  20. 20. Cubic structure – interplanar distances
  21. 21. Calculate plane distances
  22. 22. Examples
  23. 23. Examples http://www.slideshare.net/meonly21Icandependonh imallmylifeAA/xrd-lecture-1
  24. 24. What is the unit cell dimension a of NaCl ? Use plane 111 with 2x theta = 27 deg and λ = 1.54 nm (Cu-Kα)
  25. 25. Which plane will give a signal at 2x theta = 46 deg when the cubic constant a = 0.5 nm and λ = 1.54 nm ?
  26. 26. X-rays with wavelength 1.54 Å are “reflected” from the (1 1 0) planes of a cubic crystal with unit cell a = 6 Å. Calculate the Bragg angle, ϴ, for orders of reflection, n = 1-5.
  27. 27. Use Braggs Law to calculate possible values for ϴ : Solution:
  28. 28. Indexing Example
  29. 29. constant Find out which hkl combinations using in this formula will give a constant value.
  30. 30. ESTIMATED PARTICLE SIZES
  31. 31. http://mahendrakoppolu.blogspot.com/2013/07 /online-crystallite-size-calculator.html
  32. 32. AG NANOPARTICLES
  33. 33. From jcpds database http://comptech.compres.us/tools/jcpds/ In Angstrom = 10 x nm VERSION: 4 COMMENT: Silver (04-0783, shock wave) K0: 120.800 K0P: 4.84000 SYMMETRY: CUBIC A: 4.08620 ALPHAT: 0.000000 DIHKL: 2.3590 100. 1.00 1.00 1.00 DIHKL: 2.0440 52. 2.00 0.00 0.00 DIHKL: 1.4450 32. 2.00 2.00 0.00 DIHKL: 1.2310 36. 3.00 1.00 1.00 DIHKL: 1.1760 12. 2.00 2.00 2.00 DIHKL: 1.0215 6. 4.00 0.00 0.00 DIHKL: 0.9375 23. 3.00 3.00 1.00 DIHKL: 0.9137 22. 4.00 2.00 0.00 DIHKL: 0.8341 23. 4.00 2.00 2.00
  34. 34. Ag Nanoparticles XRD http://www.azonano.com/article.aspx?ArticleID=2318#5
  35. 35. Particle size estimation Debye-Scherrer Formula: λ = 0.154 nm , W = width at half maximum = 0.011 rad, Theta = 45 deg
  36. 36. Plane distance http://pubs.rsc.org/en/content/articlehtml/2013/ce/c3ce40497h
  37. 37. a = b = c = 0.4081 nm  Distance between 111 planes  between 100 planes
  38. 38. GRAPHITE AND GRAPHENE OXIDE (GO)
  39. 39. JCPDS DatabaseVERSION: 4 COMMENT: Graphite K0: 100.000 K0P: 4.00000 SYMMETRY: HEXAGONAL A: 2.456 C: 6.696 VOLUME: 34.9786 ALPHAT: 00.00E0 DIHKL: 3.3480 100. 0 0 2 DIHKL: 2.1270 3. 1 0 0 DIHKL: 2.0271 17. 1 0 1 DIHKL: 1.7953 3. 1 0 2 DIHKL: 1.6740 7. 0 0 4 DIHKL: 1.5398 5. 1 0 3 DIHKL: 1.2280 2. 1 1 0 DIHKL: 1.1529 3. 1 1 2 DIHKL: 1.1333 2. 1 0 5 DIHKL: 1.1160 2. 0 0 6 It needs 4 indices to describe the planes in hexagonal structure
  40. 40. Indices for HCP structures http://www.materials.ac.uk/elearning/matter /crystallography/indexingdirectionsandplanes /indexing-of-hexagonal-systems.html
  41. 41. https://www.youtube.com/watch?v=vK913oWl_XI
  42. 42. Graphite and Graphene Oxide http://www.rsc.org/suppdata/cc/c 0/c0cc01259a/c0cc01259a.pdf
  43. 43. Graphite structure
  44. 44. http://bgcryst.com/symp14/papers/291_Shalaby_ BCC_47-1_2015.pdf
  45. 45. Reduced GO: 2θ = 26.29 degree With λ = 0.154 nm the distance between the planes: The close d-spacing of RGO to pristine graphite and disappearance of peak at 2θ = 12.43 degree indicate that the oxygen containing group of graphite oxide have been efficiently removed
  46. 46. From: Nanomaterials 2015, 5, 826-834 Graphene Oxide Synthesis from Agro Waste The peak at 2θ = 11.6° indicates an interlayer distance of 0.79 nm  fully oxidized graphite sheets
  47. 47. FT-IR spectrum of GO
  48. 48. In the IR spectrum typical peaks of functional groups can be identified: Around 3500 cm-1: O-H stretching 1700 cm-1: typical for C=O stretching 1600 cm-1: C-C vibrations of graphite 1210 cm-1: C-OH stretching
  49. 49. From: Chem. Commun., 2011,47, 12370-12372 One-pot reduction of graphene oxide at subzero temperatures
  50. 50. From: J. Chil. Chem. Soc. vol.58 no.4 Concepción dic. 2013 http://dx.doi.org/10.4067/S0717-97072013000400067 GREEN SYNTHESIS AND CHARACTERIZATION OF GRAPHITE OXIDE BY ORTHOGONAL EXPERIMENT Different oxidation parameters for graphite
  51. 51. From: SENSORS AND ACTUATORS B CHEMICAL 199:190–200 · AUGUST 2014
  52. 52. ZINC OXIDE NANOPARTICLES
  53. 53. Hexagonal Closest Packing
  54. 54. Zinc oxide XRD – Wurzite Structure http://www.hindawi.com/journals/isrn/2012/372505/
  55. 55. Estimate particle sizes
  56. 56. Nanoscience and Nanotechnology 2015, 5(1): 1-6 Synthesis of Zinc Oxide Nanoparticles via Sol – Gel Route and Their Characterization
  57. 57. Hope this was helpful ! Please follow Ajarn Chris on Facebook

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