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

7

8

9

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

15

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

19

20 X-ray detectors: IP

21

22

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

29

30 Debye geometry at ESRF: ID31

31 MYTHEN II detector SLS-MS powder diffraction station

32 X-ray detectors: translating IP

33

34

35 translating cylindrical image plate chamber MCX station Elettra

36 André Guinier [ ]

37 focusing geometry S D 2 2

38 parafocusing geometry

39

40

41

42 Remind: The Bragg-Brentano diffractometer only samples a small portion of the Debye cone!!!! Beware!!!

43 parafocusing geometry

44

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?

49

50

51 CuO tenorite monoclinic C2/c

52 CuO monoclinic C2/c

53 Framework Type MFI

54

55

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)

78

79 Energy dispersive diffraction imaging (TEDDI)

80

81 Pencil beam tomographic scan

82

83

84

85 Sample2_slice1_glass capillary ROI Sinogram Back projection

86

87 ettringite C-S-H portlandite

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