X-ray diffraction. Talián Csaba Gábor University of Pécs, Medical School Department of Biophysics
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1 X-ray diffraction Talián Csaba Gábor University of Pécs, Medical School Department of Biophysics
2 Outline of the lecture X-ray radiation Interference, diffraction Crystal structure X-ray diffraction on crystals Diffractometer Applications
3 X-ray radiation 1895: discovery of X-ray radiation (1901: Nobel-prize) Wavelength of X-ray: 0,01-10 nm ( m) Energy of radiation: 0,1-100 kev High ionization effect Wilhelm Röntgen ( , GER)
4 Spectrum of X-ray Continuous spectrum (Bremsstahlung) Discrete spectrum (Characteristic)
5 Interference Superposition of coherent waves that results in a new wave pattern Constructive Destructive
6 Diffraction (bending of the light) double slit experiment Wave nature of the light! Thomas Young ( , ENG)
7 How is the diffraction pattern produced? d sin Θ = n λ Condition for constructive interference: diffracted rays are in the same phase! If we increase the distance (d) between the slits, then the intensity maximums are getting closer to each other! d sin Θ = d n λ ~ 1 sin Θ
8 Optical grating 0,1 mm height 3000 slits/mm Diffraction pattern of square shape slits Diffraction pattern of cross shape slits
9 Why can the crystal be used as a grating? A crystal is built up of a periodic three-dimensional arrangement of atoms, ions, or groups of atoms. c b a Unit cell: smallest repeating geometrical unit Lattice point: atom, ion, molecule
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12 Theoretical foundations of X-ray crystallography in 1912 he recognized, that spacing between planes of atoms in crystal is comparable to the wavelength of x-rays. Crystal as 3D diffraction (optical) grating! Max von Laue ( , GER) 1914: Nobel-prize in physics CuSO 4
13 Diffraction pattern is the result of elastic scattering X-ray beams elastically scatter on the electron cloud of the atoms (Thomson scattering). X-ray scattering is determined by the density of electrons around the atoms!
14 Laue equations Incident X-ray Path difference: s = AB CD AB α = a cos CD = a cosα n 0 Space between atoms 3 dimension: s s Diffracted X-ray sa = a (cosαn cosα0) = b (cos βn cos β0 = l λ = c (cosγ n cosγ 0 = m λ b ) c ) = Condition for constructive interference: sa = a (cosαn cosα0) k λ k=0,1,2,3.. = Only one dimension! k λ All equations have to be satisfied at the same time!
15 Bragg s equation William.H Bragg ( ) W. L.Bragg ( ) 1915 Nobel prize in phisycs! Criteria for constructive interference! 2 d sinθ = n λ Bragg s equation The distance between the atomic planes (d) can be calculated from the diffracted angle(θ) of the x-ray beam! Planes of the crystal behave as a mirror!
16 X-ray diffraction methods Single crystal method - Single crystal (100 μm) - Changing wavelength ( white x-ray ) - Inorganic solids and macromolecules (e.g. proteins, DNA) atomic structure - Goniometer (rotation of the sample) Powder diffraction - Monochromatic X-ray - every possible crystalline orientation is represented in a powdered sample - Identify unknown crystal samples International Centre for Diffraction Data (ICDD) 2Θ Diffractogramm of Zinc-sulphate
17 Arrangement of X-ray diffraction experiment Source: X-ray tube Goniometer Detector: - photographic plate -CCD (couple-charged device)
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20 Goniométer
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24 Study of protein structure by X-ray diffraction 1958 the first atomic structure of a protein Max Perutz and Sir John Cowdery Kendrew 1962 Nobel Prize in chemistry Sperm whale myoglobin So far ten thousends protein structure were solved by X-ray diffraction. The atomic coordinates of the proteins are freely accesible: Designing new drugs
25 DNA X-ray diffraction pattern 1953: DNA model of James D. Watson (1928-, USA) and Francis Crick ( , ENG)
26 Thank you for your attention!
27 Investigation of inorganic materials by X-ray diffraction The earliest structures were simple inorganic crystals (NaCl, ZnSO 4,diamond,graphite) Fundamental laws of physics and chemistry (nature of chemical bonds, radii of atoms). Diamond-tetrahedral arrangement with covalent bonds Graphite: hexagonal arrangement with delocalised electrons Crystal structure of diamond and graphite.
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