XAFS Spectroscopy Katarina Norén 23/11/2018.

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Presentation transcript:

XAFS Spectroscopy Katarina Norén 23/11/2018

X-ray Absorption Theory The absorpion coefficient -  Transmission of intensity through a material Lambert Beers’s Law: 23/11/2018

X-ray Absorption Theory XANES = X-ray Absorption Near-Edge Structure EXAFS = Extended X-ray Absorption Fine Structure Variation in X-ray absorption coefficient as function of energy related to structural or electronic properties of sample 23/11/2018

Early Developments of XAFS First noted in literature by students of Manne Siegbahn in Lund: Wilhelm Stenstöm and Hugo Fricke 1918-1920 Lots of early experimental and theoretical work in first 60 years of the 20th century 23/11/2018

23/11/2018

Modern History 1960s and later: XAFS is a routine X-ray technique Applications in catalysis, materials research, biology/life science, environmental and geosciences and others SciFinder Search: 2001-2012: EXAFS/XAFS ~9900/3400 Publications 1960-1975: EXAFS/XAFS = 18/0 Publications 2011: EXAFS/XAFS ~800/350 Publications 23/11/2018

Thin-film Catalysis Coordination chemistry Nano-structures An Element Specific Technique Chemistry and physics Biochemistry Thin-film Catalysis Coordination chemistry Nano-structures Metalloproteins Enzymes Environmental science Low concentrations of metals (Hg, Pb, Cr3+/Cr6+) XAFS is applicable to systems in liquid, solid, solution and gaseous phase 23/11/2018

Thin-film Catalysis Coordination chemistry Nano-structures An Element Specific Technique Chemistry and physics Biochemistry Thin-film Catalysis Coordination chemistry Nano-structures Metalloproteins Enzymes Environmental science Low concentrations of metals (Hg, Pb, Cr3+/Cr6+) XAFS is applicable to systems in liquid, solid, solution and gaseous phase 23/11/2018

Properties of Synchrotron Light High brightness: synchrotron light is extremely intense and highly collimated Wide energy spectrum: synchrotron light is emitted with energies ranging from infrared light to hard x-rays Tunable: it is possible to obtain an intense beam of any selected wavelength Polarised: the synchrotron emitts highly polarised radiation 23/11/2018

MAX IV – A Synchrotron Light Facility Insertion device Electron injector Linear accelerator Storage ring Beamlines

Why Beamlines? The storage ring and the insertion devices, also called light sources (bending magnets, undulators and wigglers) form the heart of the synchrotron radiation facility. However, the light sources as themselves are pretty useless for experiments. The properties of the source are practically always manipulated: most importantly, the optical properties Wavelength Portion of high-order light Coherence but also geometrical properties like the size of the light spot used for experiments. All this manipulation is done using the so-called beam lines. 23/11/2018

Main Functions of a Beamline The beam line's main tasks are: Monochromatize the radiation, this means that we need an energy dispersive element before the experiment Transport the source to the experiment’s sample region as effectively as possible using (mostly) mirrors Transport Focus Take out the heat load (as early as possible) Connects the experiment to the UHV environment of the storage ring 23/11/2018

Location of a Beamline The location of a beamline is dictated weather the experimental techniques requires high energies (Wiggler beamline), high brightness (undulator beamlines) or very low energies and modest flux (bending magnets) 23/11/2018

Insertion Devices 23/11/2018

XAFS at Beamline I811 Optical design 23/11/2018

XAFS at Beamline I811 Experiment station K L Si (111) crystals: K-edge: S K-edge to As K-edge L-edge: Zr L-edge to Au L-edge Si (311) crystals: K-edge: Fe K-edge to Mo K-edge L-edge: Lu L-edge to Am L-edge 23/11/2018

X-ray Absorption Theory The absorption of an x-ray photon Absorption Fluorescence Auger effect 23/11/2018

X-ray Absorption Theory The absorption of an x-ray photon Typical experiment: Transmission of intensity through a material: Absorption: (E) = log(I0/I) Fluorescence: (E)  If/I0 23/11/2018

X-ray Absorption Theory The absorption of an x-ray photon 23/11/2018

Scientific Results - XANES data 23/11/2018

The Vasa 1628 - 1961 23/11/2018

S-XANES 23/11/2018

Scientific Results- EXAFS data A little bit of data analysis Fe3+(aq) 23/11/2018

A little bit more data analysis Scientific Results A little bit more data analysis Fe3+(aq) F.T. 23/11/2018

Result: Fe – O distance Fe – O distance Model: 1.949 Å XAFS: 1.977 Å 23/11/2018

Conclusions Coordination chemistry Oxidaton state Coordination chemistry Structural information (distances, angles, types of atoms) Low detection limits (ppm) Simple and fast technique 23/11/2018