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1 XAFS 6.5GeV PF-AR 2.5 GeV PF XAFS QXAFS DXAFS XAFS XAFS 1
2 XAFS X 2.342keV K SCe L Nb * 2
3 XAFS XAFS * 3
4 Cu XAFS 5 days * M. Nomura, A. kazusaka, Y. Ukisu and N. Kakuta, J. Chem. Soc., Faraday Trans., 83, 2635 (1987). 4
5 a. b. c. d. e. 5
6 * a. t = fm /(I 0 n) t f 1 I 0 m: XAFS n: XAFSS/N I 0 (x) d =0.245 T X=2.55 S/N=1 A / T =10 4 f=310 8 f A / T =10 3 f=310 6 N S A Rev. Mod. Phys., 53 (1981) 769. T 6
7 x) 0 = X=2.55 S/N S/N = A / (I IN ) 1/2 A XAFS I IN I IN = ph x) 0 = 0.12 k 3 =1A -3 at k=16a -1 k=16a -1 S/N 16 3 =4096 =210 background 7
8 PFXAFS-BL 7C NW2A 9A 12C ph/s NW10A 9C 12C * 8
9 t = fm /(I 0 n) t f I 0 m: XAFS n: XAFSS/N (x) d =0.556 [I 0 ] T X=2.55 []S/N=1 A / T =10 4 f=310 8 A / T =10 3 f=310 6 Rev. Mod. Phys., 53 (1981) 769. N S T A f I 0 = ph/sf=310 8 n=1m=1 t=10ms m=1000 t=10s ** 9
10 S/NX (1/n) X 10
11 X 9ABLIC BL-9AMnO 4 * 11
12 b pulse/deg 8000 pulse/s 4.5s/deg * Si(111) 2021keV keV keV keV keV sin 1 ( hc ) 2dE Bragg 12
13 c. ms 100msrise time (Keithley 427) rise time) 10 8 V/A A (60s), A (1ms) V/A A(400s), A (100ms) V/A A(1.5ms), A (330ms) SSD ph/s
14 EXAFS (m=1000) XANES (m=100) 10s 1s 1s(E) 0.1s5s 50s(E) 1s 0.1s PF Quick XAFS * 14
15 [] on the fly XAFS QXAFS DMM/ ADC DMM/ ADC QXAFS * E t XAFS R. Frahm, Nucl. Instrum. Methods, A270 (1988)
16 QXAFS ( rise time VFC DMM(PF)ADC(SP8) Bragg (QXAFSBL VFC Voltage to Frequency Converter DMM: Digital Multi-Meter ADC: Analog to Digital Converter 16
17 QXAFS XAFS XANES 17
18 PF DXAFS (NW2A) QXAFS (NW10A, 12C, 9C) ms s min hr Time
19
20
21 XANES Ni 8s/spectrum
22 Fitting Results (Ni O) stageni-o stageni-o (5.8 4) XANES
23 QXAFS trade off channel-cut 23
24 channel-cut Bragg 2d sin = n n n E = hc = [ev A] detune * D const. h const. channel-cut mono. h 2Dcos 1keV Si(111)D=10mm 2021keV 1516keV 1011keV 56keV 34keV mm mm mm mm mm channel-cut 24
25 XAFS XAFS SPring-8 BL40XU X X X (2714 mm) PC T. Uruga et al., AIP Conf. Proc., 882, 914 (2007) Pt L III 25
26 XAFS SPring-8 X XAFS I0 X X Pt L 3 XANES Pt 26
27 QEXAFS (NH 4 ) 2 Cr 2 O 7 Cr 2 O 3 20ms H. Bornebusch et al. J. Synchrotron Rad., 6, 209 (1999) 27
28 Dispersive XAFS (DXAFS) []X ns T. Matsushita and P. Phizackerley, JJAP 20, 2223 (1981). A.M. Flank, A. Fontaine, A. Jucha, M. Lemonnier and C. Williams, J. Phys. (Paris), 43, L315 (1982). 28
29 PF DXAFS (NW2A) QXAFS (NW10A, 12C, 9C) ms s min hr Time
30 DXAFS l p p: q R Bragg 1 1 p q 2 Rsin w ** l E Ecot sin lecot 1 R p wlsin p=30m, l=0.1m, Si(111) Cu K Br K q=0.33m, E=1.3keV, w=2.2cm q=0.22m, E=2.9keV, w=1.5cm Multi-Pole Wiggler NW2A1cm 30
31 NW2A Tapered undulator u = 4cm, N = 90 periods high emittance S. Yamamoto et al., AIP Conf. Proc., 705, (2004). 31
32 beamline and DXAFS system: NW2A in situ reaction cell slit Water cooled Curved crystal (Bragg type) slit NW2 Sample Driver mirror Tapered undulator u 4cm *90 0.8T PF-AR ring 3 mirrors vertical focus, higher order red. Bremsstrahlung Stepping Motor Controller trigger Synchronize the gas inlet and data-taking Photodiode array or CCD detector ***** Detector Driver ADC PC 32
33 DXAFS equipment: NW2A sample cell polychromator PDA PDA In situ cell Curved crystal gas cells 33
34 DXAFS system Bragg Si(111), Si(311) etc. Laue E Si(311), Si(511) etc. E
35 Bragg case & Laue case Si(311) Rh 23.2keV a): DXAFS*, Laue, :PDA(S N,2.4 ev/ch) b): DXAFS*,Laue,:PDA(S F/CsI, 1.1 ev/ch) c): DXAFS*,Bragg, PDA(S F/CsI, 1.1 ev/ch) *:DXAFS,NW2, 2.0mrad, : 6x0.8 mm, Gap:25 : 30 m :Si(311), :260mm(Bragg), t Laue case Bragg case step scan 480mm(Laue) PDA 21500mm R:3000mm(Bragg), R:900(Laue) Rh-k edge (23.2 kev) E = 1844eV d): Conventional XAFS(BL-10B), Bragg, Rh k edge e): DXAFS(Spring-8),:CCD(1.6 ev/ch) :Si(422), : 48m :500mm PDA1140mm R:1000mm Pd-k edge (24.3 kev) E=1056 ev) f): Conventional XAFS (BL-10B), Bragg, Pd k edge t Energy / ev Energy / ev 2005/2/25 35
36 X X X PAD (XSTRIP / CCD (s) SPring-8ESRF Photo Diode Array 25/50m2.5mm1024/512ch) PDA PDA t=2ms 36
37 37
38 Energy resolution Pt LIIL II DXAFS Pt LIIIL III DXAFS Usual XAFS t Usual XAFS t Si(311) Si(111) E / ev E / ev DXAFS gives sufficient energy resolution 38
39 Dispersive and usual XAFS spectra A1: usual XAFS A2: DXAFS well prepared sample 60ms Pt/MCM min 2100 times k 3 (k) B1: usual XAFS B2: DXAFS 21 min Non-uniform sample 60ms k/10 nm -1 DXAFS requires highly uniform sample. X-rays of different energies pass different sample position. 39
40 thickness effect like phenomenon knife-edge test cf.) M. Hagelstein, et al., J. Synchrotron Rad., 5,, 753 (1998) 40
41 DXAFS A(d) B(Pt-H) t Ratio of species A B t / s Energy / ev t / s E/ ev 900 ms 41 8
42 DXAFS FT Pd(0)-O Pd(0)-Pd(0) Pd(II) Pd(II) Pd ln(i 0 /I) kpa 673 K E / kev t / s R / 10 2 pm PdO PdO Pd Pd(II)-O PdO10
43 43 probe probe pump probe probe pump pump SR SR SR SR SR SR XAFS (QXAFSDXAFS) SR mss XAFS NW2AXAFS SR SR pump( probe( SR pump( probe( SR pump( probe( SR pump( probe( SR 2ns 1.26s 1.26s
44 XSTRIP 44
45 DXAFSQXAFS DXAFS ns Quick XAFS XAFS XANES 20ms 45
46 DXAFSQXAFS DXAFS Quick XAFS E E k k E E QXAFS k 46
47 QXAFSDXAFS Fe(0)FeO1 DXAFS QXAFS 47
48 QXAFSDXAFSXAFS Quick XAFS step-scan DXAFS 48
49 15m/s 10m930m XAFS 15m250m S. Saigo et al., Biochim. Biophys. Acta, 1202 (1993) 99. D. J. Thiel et al., Nature, 362 (1993)
50 (flow, batch) 50
51 BL-12C11 Ge K GeBN k 3 /A k/a XAFS 51
52 hand press for powdery samples For solid-gas reactions, ex. catalytic reaction 1. keep enough gas diffusion into sample 2. high degree of sample homogeneity 3. high temperature, ex K 4. support pellet with tube OD 10ID 7 52
53 gas diffusion into pellet Chemisorption measurements in a glass cell. H 2 adsorption isotherm at 298 K Torr blank powder Hand-pressed sample no difference between powder and hand-pressed samples. t / s 53
54 He, N 2, Ar etc 200 ml/min 200 ml/min 2 L/min 54
![XAFSFlow Chromel-Almel thermocouple (C) heater catalyst [I] (E) Cu gasket ring ring cell](/docs-images/91/105473524/images/55-0.jpg "volume dead volume < 1mL <400W)1000 gas(d) kapton window reference [I0] (F) gas pin (H) *** 10")
55 XAFSFlow Chromel-Almel thermocouple (C) heater catalyst [I] (E) Cu gasket ring ring cell volume dead volume < 1mL <400W)1000 gas(d) kapton window reference [I0] (F) gas pin (H) *** 10 mm 55
56 Pt in-situ CZ support Normalized Peak Height Pt particle size: 7 nm 3% H 2 /He(60sec) 20% O 2 /He(60sec) 600ºC I I Time (sec) 30 sec 5 nm 1500 sec 3 nm ESRF ID-24 PF 56
57 Batch XAFS ( ) 200 ml 24 mm 60 mm V cut water Vcut Heater T = R.T.~800 * P= 10-5 ~ 900 Torr
58 XAFS ** 58
59 XAFS QXAFS QXAFS, DXAFS DXAFS, QXAFS ultrafast (t<ps) pump-probe 59
60 60
61 XAFS XAFS
62 a. (1) 62
63 Kr 20 kpakr K edge. 10 ms. t > 10 ms.
64 IR MSGC TR-XAFS 64
65 * 65
66 Sample temp./ Flow Power/w W T.C. reading/ T.C. reading/ 1000 : 0.3mA 660W(800) 300W (1000) * 66
67 DXAFS Pixel Array Detector XSTRIP Ge QXAFS 67
68 operand QXAFSDXAFS XAFS XAFS 68
69 PF KEK Proc., (2005). XAFSKEK Proc., (2008). 69
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6 2 T γ T B (6.4) (6.1) [( d nm + 3 ] 2 nt B )a 3 + nt B da 3 = 0 (6.9) na 3 = T B V 3/2 = T B V γ 1 = const. or T B a 2 = const. (6.10) H 2 = 8π kc2
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