XAS: X-ray Absorption Spectroscopy
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1 XAS: X-ray Absorption Spectroscopy Hwo-Shuenn Sheu NSRRC, Taiwan Malaya University, 2011/12/ outline Basic principles for XAS Experimental setup for XAS Applications 2 1
2 The X-ray Absorption Coefficient: μ I = I 0 e μt Absorption Photon energy (ev) 3 X-ray Absorption 4 2
3 Why need SR X-ray sources? 5 XAS accessible elements 26 H Li Na Be Mg XANES only; EXAFS hardish; K-edge EXAFS; L3-edge EXAFS; L3/K-edge EXAFS B Al C Si N P O S F Cl He Ne Ar K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe Cs Ba * Lu Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn Fr Ra * * Lr Rf Db Sg Bh Hs Mt Ds Rg * La Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb ** Ac Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No 6 3
4 X-ray Absorption Basic Principles: x XANES eV EXAFS eV NEXAFS: near edge x-ray absorption fine stuture XANES: x-ray absorption near edge spectroscopy EXAFS: extended x-ray absorption fine structure 0.0 -Ge Pre-edge X-ray photon energy (kev) 7 X-ray absorption spectroscopy 8 4
5 The interference of the outgoing and backscattered photoelectron wave From Matthew Newville 5
6 11 From Matthew Newville 12 From Matthew Newville 6
7 Excursion: Wave-particle dualism 13 The EXAFS formula: quantitative information 14 7
8 15 From Matthew Newville Structure parameters extracted from EXAFS R N Z 16 8
9 Experimental setup for XAS Transmission mode I0 x ln I t Fluorescence mode x = I f / I 0 17 XAS Beamline (BL17C1) at NSRRC I 0 I t sample I ref Dr. Jyh Fu Lee 18 9
10 Fluorescent (Lytle & 13 element array) detector 19 Transmission mode (a) and fluorescent mode (b) 20 10
11 Applications
12 K-shell photoabsorption of N 2 molecule C.T. Chen and F. Sette, Phys. Rev. A 40 (1989) (a) * (c) N 1s 1 g K-shell photoabsorption of gas-phase N 2 Absorption Intensity (arb.units) * N 1s 1 g N 1s Rydberg series x10 Double excitations Shape resonance Photon energy (ev) Absorption Intensity (arb. Units) (b) Double excitations N 1s Rydberg series Photon Energy (ev) (a) 8 vibrational levels observed in the absorpttion spectrum: N 1s 1 * g (b) N 1s Rydberg series (c) Double excitations in the N 2 spectrum Rydberg associated to the N 1s 1 * g transition. 23 XANES Chemical information: oxidation state Cu 2 O Cu CuO KCuO 2 Y-Ba-Cu-O Oxidation Numbers (formal valences) I Cu 2 O II CuO III KCuO 2 Higher transitions energy are expected for higher valence states E (ev) (J.B. Boyce et al. Phys. Rev. B 1987) 24 12
13 Pt L 3 and L 2 edge XANES 25 White line reflects the d-orbital occupancy 26 13
14 White line reflects oxidation state Higher oxidation state More empty d-orbitals More intense white line 27 Pre edge reflect local coordination symmetry Co K-edge Td (tetrahedral) (tetrahedral) (spinel) (octahedral) (octahedral) Oh 28 14
15 EXAFS of LiCoO 2 powder 29 EXAFS of LiCoO 2 powder 30 15
16 EXAFS of LiCoO 2 powder 31 EXAFS of LiCoO 2 during charging cycled Static ordering Thermal vibration 32 16
17 Use EXAFS to probe coordination environment: Na(Co 0.99 Mn 0.01 )O 2 Similar EXAFS spectrum indicate Mn and Co are in similar chemical environment. 33 Ru/Cu core shell structure characterization Ru/SiO 2 Ru-Cu/SiO
18 Ru/Cu core shell structure characterization Cu/SiO 2 Cu-Ru/SiO 2 35 Ru/Cu core shell structure characterization Ru Cu Fresh Oxidized Fresh Oxidized 36 18
19 High pressure x-ray absorption spectroscopy 37 Pressure-induced structural distortion of TbMnO3: A combined XRD and XAS study XRD data and the enhanced intensity of the white line and the shifted absorption threshold of Mn K- edge spectra enabled observation of a reduced local Jahn-Teller distortion of Mn sites within MnO 6 octahedra in TbMnO 3 with increasing pressure. These provide spectral evidence for pressureinduced bandwidth broadening for mangnites. Physical Review B 79, º Mn(1) b Mn(2) 1.889Å a Mn(2) J` 2.243Å 38 J Mn(1) 19
20 Horse tail hair has been measured to grow between 390 and 1260 micrometers per day (compared to ca. 330 micrometers for human head hair).[7] The growth of mane hair may be within this range, in which case a 500 micrometer segment would correspond to between approximately hours of growth. 39 Determination of Arsenic Poisoning and Metabolism in Hair by Synchrotron Radiation: The Case of Phar Lap** Ivan M. Kempson* and Dermot A. Henry Angew. Chem. Int. Ed. 2010, 49,
21 Photo-Induced Magnetization in Co-Fe Prussian Blue Magnets K x Co y [Fe(CN) 6 ] zh 2 O Fe Co C N K + is interstitial Defect (missing Fe) Structural disorder dictated by composition/processing PIM initially observed in K 0.2 Co 1.4 [Fe(CN) 6 ] 6.9H 2 O O.Sato et al., Science 272, 704 (1996) - Ferrimagnetic ordering below ~16 K - Magnetization increase obtained by red light - Photoinduced state has lifetime >10 5 s at low T - Effect reversed by blue light, heating 41 Magnetization Change (x 10 5 emu-g) Rb j Co k [Fe(CN) 6 ] l.nh 2 O Light Off Magnetic field parallel Magnetic field perpendicular x5 Light On Time (min) The magnetism of a nanoscale film of a molecule-based magnet is controlled by both light and orientation. h Diamagnetic Fe II -CN-Co III Electron transfer and spin crossover Ferrimagnetic Fe III -CN-Co II Photoinduced magnetism in Rb j Co k [Fe(CN) 6 ] l.nh 2 O 42 21
22 XRD and XANES of K x Co y [Fe(CN) 6 ] Synthesized in Various Concentration of KCl (2 0 0) reflection XANES of Co K-edge 4 2.0x M KCl 3 Counts (a. u.) 1.5x x x M KCl 0.1 M KCl 0 M KCl Absorption (a.u.) 2 1 0M KCl 0.1M KCl 0.5M KCl 1M KCl (degree) Energy (ev) 43 X-ray Powder Diffraction of K x Co y [Fe(CN) 6 ] Synthesized in 0.1 M KCl Solution counts (a. u.) Space group: F m 3 m PI : a= (1) PII : a= (6) wrp=0.050 Rp=0.033 X= /13/00 Co N C Fe PI : 1.987(5) (5) PII: 1.86(3) (3) (degree) 44 22
23 Water- desorption of K x Co y [Fe(CN) 6 ].nh 2 O XANES of Co K-edge Heating vacuum Absorption C 45 C 55 C 65 C 75 C 85 C 95 C 105 C 125 C Co K-edge torr (30min) Absorption (a. u.) Pre-edge RT in air 14K to RT in Vacuum 14K to RT then in air Absorption % 11% 18% 19% 32% 42% Energy (ev) Energy (ev) Energy (ev) Humidity 45 Light irradiation of Co, Fe Prussian Blue magnets Lytle Detector APD Cryostat Xe Lamp 46 23
24 XANES of Co K-edge: In-situ Xe-lamp Red light (650±40nm) illuminated at 15K Absorption Co-Kedge 30 min 27 min 20 min 11 min 4.5 min 1 min 0 min The Co 3+ become Co 2+ during red light illumination at 15K and saturation in 20 min. The K-edge of Fe also show significant change during the irradiation Fe K-edge Energy (ev) min 38 min 42 min min X-ray Absorption Spectroscopic Studies on Light-Induced Excited Spin State Trapping of an Fe(II) Complex Yu Wang, et al J. Am. Chem. Soc. 2000, 122(24),
25 X-ray Absorption Spectroscopic Studies on Light-Induced Excited Spin State Trapping of an Fe(II) Complex K-edge L-edge 49 X-ray Absorption Spectroscopic Studies on Light-Induced Excited Spin State Trapping of an Fe(II) Complex 50 25
26 X-ray Absorption Spectroscopic Studies on Light-Induced Excited Spin State Trapping of an Fe(II) Complex 51 Acknowledgement Prof. Yu Wang ( NTU) Prof. Bing-Joe Hwang (NTUST) Dr. Jyh-Fu Lee (NSRRC) Dr. Ting-Shan Chan (NSRRC) Dr. Jin-Ming Chen (NSRRC) Thank you for your attention! 52 26
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