Powder diffraction and synchrotron radiation
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1 Powder diffraction and synchrotron radiation Gilberto Artioli Dip. Geoscienze UNIPD CIRCe Center for Cement Materials
2
3 single xl diffraction powder diffraction
4 Ideal powder Powder averaging Textured sample Preferred orientation
5 how do we describe texture? ODF = f(g) = orientation distribution function f (g) g V(g) V Graphical representation: Polar figures P k (, ) f (g, )d
6 We collect the whole powder spectra using different sample orientation, and then we fit directly a functional form of the ODF P k (, ) f (g, )d
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8
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10 Crystal structure analysis Unit cell parameters Space group symmetry Atomic coordinates Atomic displacement parameters
11 XRPD measurements we want to measure the intensity profile in reciprocal space position of diffraction peaks (2, E, ToF d hkl ) intensity ( I hkl F hkl 2 ) peak profile shape ( H(2 ) = f(2 ) g(2 ) ) a correct measurement assumes: the homogeneous spatial distribution of the crystallites in the sample the homogeneous probing of the material by the beam the statistically correct measurement of intensity
12 radiation source sample (goniometer) (chamber) detector optics optics
13 Available X-ray sources Synchrotron Insertion devices Synchrotron bending magnets X-ray tubes Rotating anodes / microsources
14 X-ray detectors Point detectors Linear detectors Area detectors
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16 X-ray detectors gas phosphors semi- other ionization conductors spot proportional scintillators solid state 0-D counters Si(Li), Ge(Li) linear 1-D gas linear PSD photo-diode arrays area multiwires phosphors CCD films 2-D IP
17 True 2D detector (with some energy discrimination) Empyrean: PIXcel ESRF: FRELON camera
18 CMOS hybrid-pixel technology Pilatus 2M detectors
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20 X-ray detectors: IP
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23 Experimental geometries Angle dispersive monochromatic 2 measured - X-ray tubes - thermal neutrons - synchrotron radiation Energy dispersive polychromatic 2 fixed - synchrotron radiation - pulsed neutrons
24 angle dispersive configuration n 2d = sin polychromatic beam monochromatic beam sample 2θ 2θ detector detector energy dispersive configuration n 2d = sin polychromatic beam polychromatic beam sample sample 2θ analyzer 2θ 2θ detector
25 Experimental geometries probed sample volume geometry commonly implemented instruments laboratory Debye cameras cylindrical Debye-Scherrer or cylindrical geometry parallel- or focusing-beam laboratory goniometers with capillary sample high resolution parallel-beam configurations at synchrotron sources flat-plate curved Bragg-Brentano or parafocusing geometry Guinier or focusing geometry diverging-beam Bragg-Brentano diffractometers Guinier cameras Seeman-Bohlin cameras thin-film focusing-beam goniometers
26 In terms of practical instrumental performance, the parameters to be optimized for specific applications are: Δd/d resolution, that is the ability to separate two contiguous Bragg peaks in reciprocal space. The resolution is generally measured by the Bragg-peak broadening in terms of angular full-width at half maximum (FWHM) as a function of q. Signal/noise ratio, that is the statistical significance of the Bragg-peak intensity over the instrumental background. The signal to noise ratio is commonly greatly enhanced in synchrotron experiments because of the intrinsic collimation of the source beam. Measurement time. The total time of the measurement depends on a number of factors including: the scattering power of the sample, the probed volume of sample, the incident flux, the type and efficiency of the detectors,.
27 Peter Debye [Petrus Josephus Wilhelmus Debije] Nobel Prize for Chemistry 1936
28 Debye- Scherrer geometry
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30 Debye geometry at ESRF: ID31
31 MYTHEN II detector SLS-MS powder diffraction station
32 X-ray detectors: translating IP
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35 translating cylindrical image plate chamber MCX station Elettra
36 André Guinier [ ]
37 focusing geometry S D 2 2
38 parafocusing geometry
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42 Remind: The Bragg-Brentano diffractometer only samples a small portion of the Debye cone!!!! Beware!!!
43 parafocusing geometry
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45 the exp peak profile shape the measured peak profile is the convolution of all instrumental and sample parameters common exp aberrations: axial divergence sample shift asymmetry absorption/transparency
46 Smaller Crystals Produce Broader XRD Peaks
47
48 ideal peak profile shape ID31-ESRF is the closest we get to ideal: incident flux from undulator monochromator band pass: 10-4 collection time: minutes optimal signal/noise ratio instrumental peak broadening: FWHM<0.001 how does it compare to laboratory data?
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51 CuO tenorite monoclinic C2/c
52 CuO monoclinic C2/c
53 Framework Type MFI
54
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56 Monoclinic phase Orthorhombic phase
57 fast measurements high resolution instruments 2D detectors
58 Non Ambient Studies - Time resolved studies
59 time scale of experiments equilibrium time-resolved
60 Non ambient XRD has been performed in the last years in several operating modes: kinetic studies (i.e. qualitative and quantitative phase info) slow (tr > 1 sec) routine in the lab fast (tr < 1 sec) state of the art in the lab SR and neutron facilities equilibrium studies (i.e. direct refinement of structure details) state of the art in the lab SR and neutron facilities state of the SR and neutron facilities
61 HT apparatuses
62 LT apparatuses
63 HP apparatuses
64 HP apparatuses
65 HP apparatuses
66 combined experiments = the sample is measured at different times using different techniques and experimental settings in sequence. simultaneous measurements = the sample is excited and different signals produced by the sample are measured at the same time
67 simultaneous SAXS-WAXS exp.
68 simultaneous SAXS-WAXS-FTIR exp. W. Bras archive, ESRF
69 simultaneous SAXS-WAXS-Raman exp. W. Bras archive, ESRF
70 simultaneous XRD-XAS exp.
71 simultaneous XAS-UV Vis exp.
72 simultaneous XRD-DLS exp. GILDA ESRF
73 simultaneous XRD-XRF exp. 2D XRD mapping
74 GRC West Dover
75 high energy X-ray scanning ID15B ESRF
76 Diffraction-contrast tomographic techniques for 3D crystal phase mapping: Box beam setup (DCT) Pencil beam tomographic scan (XRD-CT) Energy dispersive diffraction imaging (TEDDI)
77 X-ray diffraction contrast tomography (DCT) (grain mapping)
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79 Energy dispersive diffraction imaging (TEDDI)
80
81 Pencil beam tomographic scan
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85 Sample2_slice1_glass capillary ROI Sinogram Back projection
86
87 ettringite C-S-H portlandite
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