General introduction to XAS
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1 General introduction to XAS Júlio Criginski Cezar LNLS - Laboratório Nacional de Luz Síncrotron CNPEM - Centro Nacional de Pesquisa em Energia e Materiais julio.cezar@lnls.br 5 th School on X-ray Spectroscopy Methods /Aug/2016 Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
2 Spectroscopy?? It seems that was Sir Isaac Newton (him again...) that called spectra the dispersion of white light by a prism. Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
3 Yes! Spectroscopy!! Distorted denition: spectroscopy is how a physical property depends on the energy (wave length or number, frequency) of a test probe (radiation, electrons, neutrons, ions, etc); Normally the variations (spectra) can be indirectly correlated with useful information by means of models; Do you like acronyms? Pick yours...: XAS, XANES, EXAFS, XMCD, XMLD, RIXS, XES, XRF, XPS, UPS, ARPES, ARUPS, EELS, FTIR, AES, UVS, PDMS, TOFMS, NMR, EPR, FMR, ESCA, µsr, INS, LIBS, CRIMS, IRMS, MIMS, ZECSY, ESR, TOCSY, SEFT, QMS,... Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
4 X-ray absorption physical property absorption of electromagnetic radiation by matter energy/frequency check the electromagnetic spectrum... www2.lbl.gov/microworlds/alstool/emspec/emspec2.html Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
5 Outline 1 Very quickly: our radiation source 2 The classic XAS experiment 3 Soft, tender and hard X-rays: experimental aspects 4 Variants of X-ray absorption Natural linear dichroism Magnetic Linear Dichroism Magnetic Circular Dichroism 5 Concluding... Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
6 Very quickly: our radiation source Outline 1 Very quickly: our radiation source 2 The classic XAS experiment 3 Soft, tender and hard X-rays: experimental aspects 4 Variants of X-ray absorption Natural linear dichroism Magnetic Linear Dichroism Magnetic Circular Dichroism 5 Concluding... Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
7 Very quickly: our radiation source Synchrotrons particle accelerator: e continuous radiation energy spectra: µwaves to γ-rays 1 st, 2 nd or 3 rd generation en.wikipedia.org/wiki/synchrotron_light_source Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
8 Very quickly: our radiation source Synchrotron radiation bend magnets insertion devices Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
9 The classic XAS experiment Outline 1 Very quickly: our radiation source 2 The classic XAS experiment 3 Soft, tender and hard X-rays: experimental aspects 4 Variants of X-ray absorption Natural linear dichroism Magnetic Linear Dichroism Magnetic Circular Dichroism 5 Concluding... Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
10 The classic XAS experiment The classic X-ray absorption experiment I T = I 0 e µt µ:linear absorption coecient Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
11 The classic XAS experiment How radiation interacts with matter Radiation-matter interaction has several components: photoelectric eect Compton scattering pair creation Fig 2-17 Eisberg & Resnick Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
12 The classic XAS experiment XAS: absorption edges from Neutron and X-ray Spectroscopy, E. Lelièvre et al, Springer Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
13 The classic XAS experiment XAS: absorption edges Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
14 The classic XAS experiment XAS: electron transition from J. Stohr presentation found at Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
15 The classic XAS experiment XAS in atoms: Argon Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
16 The classic XAS experiment XAS in solids: Cobalt oxide Lamirand et al., PRB 88 (2013) Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
17 Soft, tender and hard X-rays: experimental aspects Outline 1 Very quickly: our radiation source 2 The classic XAS experiment 3 Soft, tender and hard X-rays: experimental aspects 4 Variants of X-ray absorption Natural linear dichroism Magnetic Linear Dichroism Magnetic Circular Dichroism 5 Concluding... Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
18 Soft, tender and hard X-rays: experimental aspects Tender, hard, soft: X-rays for all tastes... www2.lbl.gov/microworlds/alstool/emspec/emspec2.html Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
19 Soft, tender and hard X-rays: experimental aspects Attenuation length Attenuation length is the reciprocal of linear absorption coecient. It is tabulated. Optimun signal/noise thickness is when edge jump is equal to 1. Cu K edge: 6 µm Cu L edge: 120 nm Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
20 Soft, tender and hard X-rays: experimental aspects XAS: detection modes from Reiko Nakajima, PhD thesis (1998) Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
21 Soft, tender and hard X-rays: experimental aspects XAS: detection modes from J. Stohr presentation found at Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
22 Soft, tender and hard X-rays: experimental aspects The electron mean free path attwood/srms/2007/lec02.pdf Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
23 Soft, tender and hard X-rays: experimental aspects Fluorescence vs electron yield attwood/srms/2007/lec02.pdf Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
24 Soft, tender and hard X-rays: experimental aspects Take in consideration Hard X-rays 1 Are bulk sensitive 2 Can be used in transmission 3 Fluorescence: very eective 4 Don't need ultra high vacuum Soft X-rays 1 Are very, very surface sensitive 2 Normally use electron yield 3 Fluorescence: weak 4 Need ultra high vacuum Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
25 Variants of X-ray absorption Outline 1 Very quickly: our radiation source 2 The classic XAS experiment 3 Soft, tender and hard X-rays: experimental aspects 4 Variants of X-ray absorption Natural linear dichroism Magnetic Linear Dichroism Magnetic Circular Dichroism 5 Concluding... Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
26 Variants of X-ray absorption Let's start: X-ray absorption spectroscopy Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
27 Variants of X-ray absorption We should, but we're not going to discuss about... EXAFS Extended X-ray absorption ne structure XRF X-ray uorescence RIXS Resonant inelastic X-ray scattering XES X-ray emission spectroscopy XEOL X-ray excited optical luminescence DAFS Diraction anomalous ne structure PEEM Photoelectron emission microscopy STIF Some technique that I forgot... Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
28 Variants of X-ray absorption Soft X-rays absorption spectroscopy from J. Stohr presentation found at X-ray Absorption Spectroscopy (XAS) X-ray Absorption Near Edge Spectroscopy (XANES) Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
29 Variants of X-ray absorption Natural linear dichroism Breaking the symmetry 1: structural anisotropy Radiation interacts strongly with electrons; The strongest term in the interaction is between the photon electric eld and electrons; Near edge features require empty states in the atom; Fermi Golden Rule in the dipolar approximation: T if f ê ˆr i δ(e i E f )ρ(e f ) (1) Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
30 Variants of X-ray absorption Natural linear dichroism Exploring structural anisotropies: perovskites Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
31 Variants of X-ray absorption Natural linear dichroism Natural linear dichroism in LaMnO 3 /SrTiO 3 X-ray Linear Natural Dichroism (XLD ou XLND) Grazing incidence to probe in and out of plane directions; Garcia-Barriocanal et al., Nature Communications 1 (2010) doi: /ncomms1080 Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
32 Variants of X-ray absorption Magnetic Linear Dichroism Magnetic Linear Dichroism X-ray Linear Magnetic Dichroism (XMLD) Anisotropy induced by magnetization; Adds up to natural dichroism!! Attention to the geometry: magnetic eld perpendicular the X-ray beam propagation. Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
33 Variants of X-ray absorption Magnetic Linear Dichroism YbInNi 4 cubice crystal lattice; Yb and In oset FFC lattices by 1/4, 1/4, 1/4; Ni tetrahedra around Yb e In; magnetic order below 3 K; Yb valence xed 3+. Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
34 Variants of X-ray absorption Magnetic Linear Dichroism YbInNi 4 : debatable ground state Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
35 Variants of X-ray absorption Magnetic Linear Dichroism XMLD: YbInNi 4 Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
36 Variants of X-ray absorption Magnetic Linear Dichroism XMLD at the Yb M 5 edge Willers et al., PRL 107, (2011) Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
37 Variants of X-ray absorption Magnetic Circular Dichroism Magnetic circular dichroism X-ray Circular Magnetic Dichroism (XMCD) Anisotropy once more induced by magnetization; Eect does not add up with linear dichroism (natural or magnetic) Attention to the geometry: magnetic eld parallel to the X-ray beam propagation direction Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
38 Variants of X-ray absorption Magnetic Circular Dichroism Fe XMCD on Ca 2 FeReO 6 Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
39 Variants of X-ray absorption Magnetic Circular Dichroism XMCD: sum rules integrals m orb = L Z = n h 4q 3r m spin = 2 S Z + 7 T Z = n h 6p 4q r Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
40 Variants of X-ray absorption Magnetic Circular Dichroism XMCD is really cool!! XMCD is one of the most powerful tools to study magnetic materials : magnetic information for each element in the sample; for the same element, magnetic information for dierent orbitals; element sensitive hysteresis curves; element sensitive magnetic anisotropy; very sensitive: soft X-rays can detect hundreths of monolayer ;... but requires very good experimental data;... sum rules are not universal. To avoid troubles: spectra simulation (ab initio, multiplets,...)!... requires a good week of night shifts in the beam line. Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
41 Concluding... Outline 1 Very quickly: our radiation source 2 The classic XAS experiment 3 Soft, tender and hard X-rays: experimental aspects 4 Variants of X-ray absorption Natural linear dichroism Magnetic Linear Dichroism Magnetic Circular Dichroism 5 Concluding... Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
42 Concluding... XAS: take away messages XAS: intrisically element sensitive; XAS: needs a synchrotron; Can use hard or soft X-rays; Dierent detection modes: transmission: well suited for hard X-rays; bulk sensitive; uorescence: works better with hard X-rays; bulk sensitive; total electron yield: soft X-rays; surface sensitive; Absorption spectroscopy requires empty levels at the absorbing atom. Julio C. Cezar (LNLS/CNPEM) 5 th XAFS School Campinas, 22/Aug/ / 42
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