X-ray powder diffraction a practical guide. Dinnebier 0; InternationalTables 0; Will 0; Young 0; Pecharsky 0
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1 X-ray powder diffraction a practical guide Dinnebier 0; InternationalTables 0; Will 0; Young 0; Pecharsky 0
2 X-ray hitting condensed matter Cullity 114
3 X-ray hitting condensed matter Dinnebier Pre6
4 Debye-Scherrer cones from a polycrystalline sample Cullity 98
5 Bragg-Brentano and Guinier diffractometer Dinnebier 34, 35_1, 35_2, 37
6 Bragg-Brentano diffractometer with monochromator Dinnebier 36
7 Generation of x-ray Dinnebier 22
8 Generation of x-ray Optimum voltage ~4 times characteristic energy (~30 kv for Cu anodes) Dinnebier 23, 24
9 Generation of x-ray Suppression of Kβ radiation by filter with lighter neighbor element in periodic table Cullity 20, 21
10 Samples for x-ray powder diffraction Well prepared samples at the right sample holder is the key for success!!! Dinnebier 42_1, 42_2
11 Samples for x-ray powder diffraction Hygiene in preparing the powder is the second key for success!!! Dinnebier 42_1, 42_2
12 Samples for x-ray powder diffraction Cullity 283
13 Samples for x-ray powder diffraction Cullity 289
14 Bragg-Brentano diffractometer for the desk Dinnebier 36
15 Example: growth of PrAuSi out of Sn flux Which phases are present? E. D. Mun: PM721-Ex1a
16 Phase analysis with the PDF database PDF_DataBase 1; 2; 3; 4
17 Phase analysis with the PDF database PDF_DataBase 5; 6
18 Phase analysis with the PDF database PDF_Hanawalt 1; 2; PDF_Fink 1; 2
19 Example: growth of PrAuSi out of Sn flux If your phase is not in the database search for isostructural compounds... E. D. Mun: PM721-Ex1g
20 Powdercell The best tool to calculate diffraction pattern, to verify structure data and more... Powdercell 1
21 Powdercell The best tool to calculate diffraction pattern, to verify structure data and more... Powdercell 2
22 Powdercell The best tool to calculate diffraction pattern, to verify structure data and more... Powdercell 3
23 International Tables for Crystallography InternationalTables E1
24 International Tables for Crystallography InternationalTables E2
25 International Tables for Crystallography InternationalTables 7_1
26 International Tables for Crystallography InternationalTables 7_2
27 International Tables for Crystallography InternationalTables 8
28 International Tables for Crystallography InternationalTables 9
29 International Tables for Crystallography Cullity 35, 36
30 International Tables for Crystallography InternationalTables E4
31 International Tables for Crystallography InternationalTables E3
32 Problems describing a structure Rhombohedral unit cell InternationalTables 84
33 Problems describing a structure Rhombohedral unit cell InternationalTables 146_11; 12a; 21; 22
34 Problems describing a structure Origin of cell InternationalTables 129_11; 21
35 Problems describing a structure Origin of cell InternationalTables 129_11; 12; 21; 22
36 Powdercell Extract the reflection list: (hkl) position - intensity Powdercell 5
37 Preparation of a reflection list for further use Dinnebier 307
38 Example: growth of YbPtBi with partial element substitution YbPtBi 0.9 Sb 0.1 Yb 0.9 Lu 0.1 PtBi YbPt 0.9 Au 0.1 Bi YbPtBi Which phases were grown successfully? E. D. Mun: PM935-Ex2b
39 Example: growth of YbPtBi with partial element substitution YbPtBi 0.9 Sb 0.1 Yb 0.9 Lu 0.1 PtBi YbPt 0.9 Au 0.1 Bi YbPtBi Only YbPt 0.9 Au 0.1 Bi was grown successfully. E. D. Mun: PM935-Ex2c
40 Example: growth of Ba(Fe 1-x Co x ) 2 As 2 x = 0.10 PM915 PM892 PM871 Preparation of samples with same stoichiometry is reproducible. N. Ni: PM871-Ex3a
41 Example: growth of Ba(Fe 1-x Co x ) 2 As 2 x = 0.15 x = x = 0.10 x = x = 0.05 x = x = 0 Preparation of samples with varying stoichiometry seems also successful. N. Ni: PM871-Ex3b
42 Example: growth of Ba(Fe 1-x Co x ) 2 As 2 x = 0.15 x = x = 0.10 x = x = 0.05 x = x = 0 Use of inner standard a MUST. N. Ni: PM871-Ex3e
43 Position of Bragg reflections in powder pattern Pecharsky-MSE ; 13
44 Example: growth of Ba(Fe 1-x Co x ) 2 As 2 x = 0.15 x = x = 0.10 x = x = 0.05 x = x = 0 Combined analysis of series of Bragg reflections (main phase + standard) necessary. N. Ni: PM871-Ex3c
45 Combined fitting of Bragg reflections Pecharsky-MSE ;
46 Profile of Bragg reflections in powder pattern Dinnebier 169
47 Profile of Bragg reflections in powder pattern Will 23; 80_1,2; 81_1,2,3
48 R-values (residuals) reliability criteria for refinements Will 115; 120_1,2,3; 121
49 Example: growth of Ba(Fe 1-x Co x ) 2 As 2 Realized stoichiometry by WDS study; Vegard s law for lattice parameter NNi_PhysRevB_78_ ; 3
50 Example: preparation of RFeAs(O/F) High-temperature x-ray diffraction with 2-dimensional detector Rimg3307; 3318
51 Example: preparation of RFeAs(O/F) undoped F doped High-temperature x-ray diffraction with 2-dimensional detector McCallum 1; 2
52 Rietveld refinement of powder pattern Pecharsky-MSE ;
53 Intensity of Bragg reflections in powder pattern Pecharsky-MSE
54 Lorentz and Polarization factor Pecharsky-MSE
55 Absorption factor Pecharsky-MSE
56 Preferred orientation factor Pecharsky-MSE
57 Extinction factor Pecharsky-MSE
58 Temperature factor Pecharsky-MSE
59 Atomic scattering factor Pecharsky-MSE
60 Example: preparation of RFeAs(O/F) F doped undoped Temperature Temperature-dependent x-ray diffraction (20 sec. pattern) SDas 1
61 Example: preparation of RFeAs(O/F) F doped undoped Temperature Temperature-dependent x-ray diffraction (20 sec. pattern) SDas 2
62 Example: preparation of RFeAs(O/F) Multi-phase Rietveld refinement SDas 5
63 Example: preparation of RFeAs(O/F) F doped undoped Crystalline phase fraction determined by Rietveld analysis SDas 3
64 Example: preparation of RFeAs(O/F) undoped F doped Unit-cell volume of RFeAs(O/F) phase determined by Rietveld analysis SDas 4
65 Why and when powder for structure determination? Dinnebier Pre9
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