Lecture 5: Characterization methods

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1 Lecture 5: Characterization methods X-Ray techniques Single crystal X-Ray Diffration (XRD) Powder XRD Thin film X-Ray Reflection (XRR) Microscopic methods Optical microscopy Electron microscopies (SEM, TEM) Spectroscopic methods X-Ray spectroscopies (XRF, XANES, etc.) Solid-state NMR spectroscopy Infrared and Raman spectroscopy Figures: AJK 1

2 Structure of non-molecular crystalline solids Lecture 5 Lecture 1 Lecture 5 Lecture 5 Ref: West p

3 Structure determination from single-crystal and powder XRD X-ray diffraction has been used for over a century in two main areas For the structure determination of crystalline materials (both single crystal and powder XRD) For the fingerprint identification of crystalline materials (powder XRD) Here the focus is on the fingerprint identification of materials via powder XRD Structure determination is discussed in detail on the course Crystallography Basics and Structural Characterization (CHEM-E4205) Lectured first time in Fall 2016 (Period I) X-ray diffraction pattern of aluminum single crystal (left) and powder (right) Figure: Susan Lehman / wooster.edu 3

4 Phase identification with XRD Powder XRD is a very powerful technique for the identification of solid phases Each crystalline phase has a characteristic powder XRD pattern which can be used as a fingerprint for identification purposes The two variables in a powder pattern are Peak position, i.e. d-spacing, which can be measured very accurately Intensity, which can be measured either qualitatively or quantitatively It is very rare that different crystalline phases have identical XRD patterns The normal practice in using XRD patterns for identification purposes is to pay most attention to the d-spacings and check that the intensities are roughly correct 4

5 Powder pattern matching Powder Diffraction File (PDF) powder patterns Expensive licences, normally fixed to to a single computer Pattern matching software bundled with diffractometers ICSD has simple powder diagrams available for all the structures (Assignment!) 5

6 Phase transitions with XRD BaTiO 3 perovskite 6

7 Grazing incidence X-Ray diffraction 7

8 X-Ray Reflectivity (XRR) analysis for thin-film samples Detector 8

9 Microscopic characterization methods With optical microscopes, particles down to a few micrometres or microns in diameter may be seen under high magnification The lower limit is reached when the particle size approaches the wavelength of visible light, μm For submicron-sized particles, it is essential to use electron microscopy Features as small as a few Å across can be imaged readily Ref: West p

10 Scanning Electron Microscopy In SEM, electrons from the electron gun, accelerated through 5 50 kev, are focused to a small spot, Å in diameter, on the sample surface Usually detection of secondary electrons The main application of SEM is for surveying materials under high magnification and providing information on sizes, shapes and compositions as seen from solid surfaces Ref: West p. 204,

11 Transmission Electron Microscopy TEM detects transmitted electrons and radiation, in contrast to SEM, which is a reflection-based technique Nowadays enables even atomic resolution ( 2 Å) With TEM, both diffraction patterns and magnified images can be obtained from the same sample area Diffraction patterns give unit cell and space group information In imaging mode, TEM gives morphological information on the sample The first TEM was in fact built by Max Knoll and Ernst Ruska in 1931 (Nobel 1986) Actual measurement requires lots of expertise (e.g. sample preparation!) Ref: West p

12 Structural challenge: m-allo-ge Chemistry of Materials, 2011, 23,

13 From Li 7 Ge 12 to m-allo-ge (1) H 2 O / EtOH Removal (deintercalation) of Li Li 7 Ge 12 precursor (P2/n) Ge atoms with two, three or four bonds m-allo-ge Oxidative coupling of the layers 13

14 HRTEM for m-allo-ge: Stacking faults along c-axis Li 7 Ge 12 precursor (P2/n) 14

15 Statistical model for the stacking faults The model derived from quantum chemical calculations was refined with FAULTS program package to match the experimental powder pattern (~Rietveld refinement) Total probabilities of interlayer bonding types: A: 60%, B: 40% 15

16 Powder XRD for the structural model 16

17 Electron Diffraction for m-allo-ge 17

18 Spectroscopies Spectroscopy gives information on local structure whereas XRD is concerned primarily with long-range order Structural characterization when structure cannot be (fully) solved by XRD (solid solutions, amorphous materials, thin films, complex hybrid materials) Helps to understand bonding and defects / impurities Fingerprinting (not so commonly used due to the dominance of powder XRD) Ref: West p

19 X-Ray and electron spectroscopies Ref: West p

20 X-Ray spectroscopies (1) The X-ray region of the electromagnetic spectrum is extremely useful for structural studies, analysis and characterisation of solids Emission: Utilise the characteristic X-ray emission spectra of elements generated by, for instance, bombardment with high-energy electrons. The spectra are used for chemical analysis of both bulk samples (X-ray fluorescence, XRF) and micron- or submicron-sized particles (analytical electron microscopy, AEM, electron probe microanalysis, EPMA, etc.). They also have some uses in determination of local structure and coordination Absorption: measure the absorption of X-rays by samples, especially at energies in the region of absorption edges. Powerful techniques for studying local structure but usually require a highenergy X-ray source such as a synchrotron 20

21 X-Ray spectroscopies (2) Ref: West p

22 X-Ray emission spectroscopies X-ray fluorescence (XRF): a solid sample is bombarded with high-energy electrons The resulting emission spectrum is recorded From the spectral peak positions, the elements present can be identified From their intensities, a quantitative analysis can be made Peak positions vary slightly with local environment Determination of local structure such as coordination numbers and bond distances 12 6 KAlSi 3 O 8 4 Ref: West p

23 X-Ray absorption spectroscopies Atoms give characteristic X-ray absorption spectra in addition to characteristic emission spectra X-ray Absorption Near Edge Structure (XANES) (Absorption edge fine structure, AEFS) The exact peak positions depend on details of oxidation state, site symmetry, surrounding ligands and the nature of the bonding Cu Ref: West p

24 X-Ray absorption spectroscopies Whereas XANES examines at high resolution the fine structure in the region of an absorption edge, Extended X-ray Absorption Fine Structure (EXAFS) examines the variation of absorption with energy (or wavelength) over a much wider range, extending out from the absorption edge to higher energies by up to 1 kev The absorption usually shows a ripple, known also as the Kronig fine structure, Fig. 6.32, from which information on local structure and, especially, bond distances may be obtained Often used to determine interatomic distances in amorphous materials 24

25 Electron spectroscopies Electron spectroscopy techniques measure the kinetic energy of electrons that are emitted from matter as a consequence of bombarding it with ionizing radiation or high-energy particles Electron spectroscopy for chemical analysis (ESCA) XPS (X-ray photoelectron spectroscopy) UPS (ultraviolet photoelectron spectroscopy) Auger electron spectroscopy (AES) Electron energy loss spectroscopy (EELS 25

26 Solid-state NMR spectroscopy Nuclear Magnetic Resonance (NMR) is extremely important specroscopy for the determination of molecular structure Which atoms are bonded together, coordination numbers, next nearest neighbors, etc. Not as widely applied for solids, but still very useful Utilizes the magnetic spin energy of atomic nuclei The magnetic energy levels split into two groups, depending on whether the nuclear spins are aligned parallel or antiparallel to applied magnetic field The energy difference between the parallel and antiparallel spin states is in the radiofrequency region of the electromagnetic spectrum The magnitude of the energy change and the associated frequency of absorption depends on the element and its chemical environment Solid-state NMR enabled by Magic Angle Spinning (MAS) The sample is rotated at a high velocity at a critical angle of to the applied magnetic field Solid-state NMR is not a routine technique like liquid-state NMR! First applications were on silicates ( 29 Si, J. Am. Chem. Soc., 1980, 102, 4889) Ref: West p

27 Solid-state NMR for A 8 Al 8 Si 38 (A=K, Rb, Cs) Chem. Eur. J. 2014, 20, M 20 cage M 24 cage (M = Si, Ge, Sn) Clathrate I (Pm-3n) 27

28 27 Al MAS NMR spectra Si and Al cannot be distinguished by XRD due to similar X-Ray scattering (neighboring elements) Combination of neutron diffraction, MAS NMR, and computational solid-state NMR enables the complete structural characterization of the Si/Al occupancy K 8 Al 8 Si 38 Rb 8 Al 8 Si 38 16i 24k 6c Cs 8 Al 8 Si 38 Peak area ratio -> Al occupancy of sites 28

29 Electron spin resonance spectroscopy (ESR) The ESR technique, also known as electron paramagnetic resonance (EPR), is closely related to NMR Detects changes in electron spin configuration ESR depends on the presence of permanent magnetic dipoles, that is, unpaired electrons, such as those which occur in many transition metal ions The reversal of spin of the unpaired electrons in a magnetic field is recorded From ESR spectra, one can obtain information on the paramagnetic ion and its immediate environment in the host structure The oxidation state, electronic configuration and coordination number of the paramagnetic ion Structural distortions arising from, for example, a Jahn Teller effect The extent of any covalency in bonds between the paramagnetic ion and its surrounding anions or ligands Ref: West p. 301 The ESR spectrum of CrO 4 3 in Ca 2 PO 4 Cl at 77 K 29

30 Vibrational spectroscopy Infrared spectroscopy Materials absorb specific frequencies that are characteristic of their structure Simply measure absorbance or transmittance Raman spectroscopy Material is excited by laser Most of the emitted photons have the same energy as the original (elastic scattering) Some of the emitted photons are shifted w.r.t to the laser wavelength due to coupling with vibrational levels -> Raman scattering Elastic scattering of photons Inelastic scattering of photons Figure: Wikipedia 30

31 Interpretation of Raman and IR spectra: Ba(BrF 4 ) 2 BrF 4 31

32 Ba(BrF 4 ) 2 Raman Experiment Theory (DFT-PBE0/SVP) 32

33 Ba(BrF 4 ) 2 Raman and IR: Assignment Complete assignment of the spectrum enabled by quantum chemistry! 33

34 Raman and IR spectra in structure determination: RbBrF 4 34

35 Raman and IR spectra in structure determination (2) RbCl impurity IR not as helpful as Raman in this case No RbCl (calculation on pure phase) 35

36 Raman and IR spectra in structure determination (3) 36

37 IR and Raman spectra of ZnO:organic hybrids Oxide:organic superlattice fabricated with ALD/MLD Structure cannot be determined from the thin film samples c b a c a b Combine theory and experiment to derive reasonable structural models 1.2 nm ZnO HQ = Schematic model Structural model from quantum chemical studies 37

38 IR and Raman for ZnO:HQ superlattice The predicted IR spectrum is in agreement with the experimental one Supporting evidence for the proposed structural model Experimental Raman spectrum not yet available 38

39 Strategy to Identify, Analyze and Characterize Unknown Solids The next two slides summarize how various characteriation methods can be applied to find out the composition and structure of an unknown solid The table does not include any property measurement techniques and their uses for the characterization of solids, for example: Magnetic properties such as magnetic moment give information on the unpaired spins (-> electronic structure) Electrical properties such as conductivity give information on the electronic structure, oxidation states, and the effect of dopants or defects Optical property measurements can also give information on oxidation states and d / f electron configurations Numerous physical property measurement techniques are not discussed here. Just to list a few examples: Mechanical/elastic properties (elastic moduli, hardness, ) Permittivities, refractive indices Thermo-, piezo-, pyro-, and ferroelectric properties Thermal conductivity, thermal expansion, heat capacity Ref: West p

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