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1 Applied Chemistry and Biotechnology
2 Many elements can be a candidate for developing the active catalyst. However, there are some restrictions such as cost, abundance, etc. Platinum group metals show the higher activity toward many reactions. However, they are really precious and distributed unevenly. Base elements are relatively inexpensive and abundant. They also have the activity as catalyst. However, their activity is not high enough Surface atom ratio / % Particle size / nm M. Haruta, Catal. Today, 36 (1997) H. Tsunoyama, N. Ichikuni, H. Sakurai, T. Tsukuda, J. Am. Chem. Soc., 131 (2009)
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4 Ni metal nanocluster on alumina N. Ichikuni et al. Trans. Mater. Res. Soc. Jpn., 37 (2012) Ni colloid Al 2 O 3 catalyst preparation Ni(OAc) 2 Al 2O 3 (Aerosil, -C) reflux H K NaH+alcohol*/THF Ni colloid col Ni/Al 2O 3 N 2 atmosphere *alcohol Ni loading: 3 wt% P. Caubère et al. J. Organomet. Chem., 157 (1978) OH OH OH OH 2-propanol (2-Pr) 2-butanol (2-Bu) 2-pentanol (2-Pe) 2-octanol (2-Oc) 2-decanol (2-De) OH 2-dodecanol (2-Do) H. Kitagawa, N. Ichikuni, S. Xie, T. Tsukuda, T. Hara, S. Shimazu, e-j. Surf. Sci. Nanotech., 10 (2012) OH
5 Ni K-edge XANES <H2 treated at 673 K> Ni K-edge in situ XANES spectra during H2 treatment. Ni K-edge XANES spectra of Ni catalysts H2-treated at 673 K. Ni K-edge XANES <H2 treated at 673 K> catalysts ratio of Ni metal / % imp Ni/SiO2 95 col Ni/SiO2 90 imp Ni/Al2O3 25 col Ni/Al2O3 85 <H2 treated at 773 K> catalysts ratio of Ni metal / % imp Ni/SiO2 95 col Ni/SiO2 90 imp Ni/Al2O3 55 col Ni/Al2O3 85
6 catalyst preparation Ni(OAc) 2 Al 2O 3 (Aerosil, -C) reflux H K NaH+alcohol*/THF Ni colloid col Ni/Al 2O 3 N 2 atmosphere *alcohol Ni loading: 3 wt% P. Caubère et al. J. Organomet. Chem., 157 (1978) pentanol(2-Pe) 2-octanol (2-Oc) 2-decanol (2-De) NaH/Ni = 9, 15, 20 alcohol/ni = 1, 3, 6, 9 effect of alkyl chain length FT Ni foil col Ni/Al 2 O 3 2-De col Ni/Al 2 O 3 2-Oc Sample CN a r b / nm Ni foil col Ni/Al 2 O 3 2-De 10.3± col Ni/Al 2 O 3 2-Oc 8.4± col Ni/Al 2 O 3 2-Pe 8.9± a Coordination number of Ni-Ni1 b Coordination distance of Ni-Ni1 col Ni/Al 2 O 3 2-Pe r / 10-1 nm FT k-range: nm -1 2-Oc
7 SPring-8講習会 <産業利用に役立つXAFSによる先端材料の局所構造解析 2017> 2017/1/30 炭素鎖長の短いアルコキシド 還元剤となるNaHとの複合体形成が速い 還元速度が速い Reducing timea / min effect of alkyl chain length a溶液が黒色化するま での時間 炭素鎖長の長いアルコキシド 保護基としてのNiへの配位時の保護能が高い クラスターの微細保持 還元剤としての機能: 2-Pe > 2-Oc > 2-De 保護剤としての機能: 2-Pe < 2-Oc < 2-De 2-octanolが両機能を最適化 SPring-8講習会 <産業利用に役立つXAFSによる先端材料の局所構造解析 2017> 2017/1/30 TEM observation 12 Distribution / % Distribution / % Particle size / nm d = 3.2±0.8 nm CN = 10.3 col Ni/Al2O3 2-Oc NaH(15) 12 Distribution / % Particle size / nm d = 3.0±0.8 nm CN = 8.9 col Ni/Al2O3 2-Oc THF(10) col Ni/Al2O3 2-Pe 1 Distribution / % col Ni/Al2O3 2-De Particle size / nm d = 2.9±0.7 nm CN = Particle size / nm d = 2.7±0.7 nm CN = 6.7
8 water gas shift reaction 8.0 < CN CN < 8.0 CO: 5 Torr, H 2 O: 5 Torr, He: 40 Torr, T = 523 K reaction order CO + H 2 O CO 2 + H 2 r = k [CO] x [H 2 O] y H 2 O CO terrace site ratio order for CO CN terrace site ratio H 2 O CO CO CO
9 Ratio of distorted particles (rdp*) col Ni/Al 2 O 3 2-De rdp = 6.3 % d = 3.2±0.8 nm CN = 10.3 col Ni/Al 2 O 3 2-Pe col Ni/Al 2 O 3 2-Oc NaH(15) rdp = 9.6 % d = 3.0±0.8 nm CN = 8.9 rdp = 10.4 % d = 2.9±0.7 nm CN = 8.0 col Ni/Al 2 O 3 2-Oc THF(10) rdp = 10.6 % d = 2.7±0.7 nm CN = 6.7 rdp: Number of the distorted particles/number of all particles observed in HAADF STEM images. The reason of volcano-shape size dependence K.B.Kester, E.Zagli, J.L.Falconer, Appl.Catal. 22 (1986) col Ni/Al 2 O 3 2-Oc THF(10) col Ni/Al 2 O 3 2-Pe rdp = 9.6 % d = 3.0±0.8 nm Ea = 58 kj mol -1 rdp = 10.6 % d = 2.7±0.7 nm Ea = 82 kj mol -1
10 Size regulated Ni nanocluster was preparaed on alumina support. Ni nanocluster showed the volcano shape size dependence on WGSR H. Kitagawa, N. Ichikuni, H. Okuno, T. Hara, S. Shimazu., Appl. Catal. A, 478 (2014)
11 Ni foil normalized absorption NiO imp Ni(N)/SiO 2 imp Ni(Ac)/SiO 2 col Ni(A)/SiO 2 col Ni(C)/SiO 2 col Ni(N)/SiO 2 col Ni(Ac)/SiO 2 N. Ichikuni, O. Tsuchida, J. Naganuma, T. Hara, H. Tsunoyama, T. Tsukuda, S. Shimazu, Trans. Mater. Res. Soc. Jpn., 37 (2012) photon energy / ev 8400 normalized absorption Co(OH)2 Co3O4 oxidation 673 K oxidation 573 K oxidation 453 K w/o pretreatment FT photon energy / ev r / 0.1 nm 5 6 N. Ichikuni, T. Fujii, T. Hara, S. Shimazu, PF Activity Report 2013 #31(2014) B, 93.
12 Co(OAc) 2 SiO 2 NaH 2-Butanol/ THF Co colloid N 2 atmosphere col CoO x /SiO 2 Co: 3 wt%, 5wt% Na + O - Na + O - Na+ O - O - Na + n=alcoholate/co=3, 4, 9 col CoO x /SiO 2 (n) 10 5 col CoOx/SiO 2 (3) col CoOx/SiO 2 (4) col CoOx/SiO 2 (9) col CoOx/SiO 2 (3) col CoOx/SiO 2 (4) col CoOx/SiO 2 (9) k 3 χ(k) 0 FT k / 10 nm -1 r / nm Table Curve-fitting result of Co-Co (Oh) coordination for col CoOx/SiO2 catalyst CN r (nm) de (ev) DW (nm) col CoOx/SiO2 (3) 3.8± ± ± ± col CoOx/SiO2 (4) 3.4± ± ± ± col CoOx/SiO2 (9) 2.6± ± ± ± FT k-range: nm -1, Co-(O)-Co parameter: Co3O4 alcoholate/co
13 XPS spectra of 5 wt% col CoO x /SiO 2 Co 3+ /(Co 3+ +Co 2+ ) (%) pretreatment temp. (K) col CoO x /SiO 2 (3) col CoO x /SiO 2 (4) col CoO x /SiO 2 (9) Co 2p 3/2 Co 2p 1/2 Co 3+ Co 2+ Co 2p 1/2 Co 2p 3/2 Co 2+ Co 3+ Co 2p 1/2 Co 2p 3/2 Co 3+ Co 2+ Intensity / a.u. Intensity / a.u. Intensity / a.u. 573 K K Binding energy / ev Binding energy / ev Binding energy / ev K Co 3+ /(Co 3+ +Co 2+ ) (%) pretreatment temp. (K) col CoO x /SiO 2 (3) col CoO x /SiO 2 (4) col CoO x /SiO 2 (9) , evac at
14 Initial rate of CO oxidation on 5 wt% CoO x /SiO 2 catalyst catalyst r0 (10-5 mol min -1 gcat -1 ) col CoO x /SiO 2 (3) 13.7 col CoO x /SiO 2 (4) 13.6 *col CoO x /SiO 2 (4) *6.3 col CoO x /SiO 2 (9) 5.8 *col CoO x /SiO 2 (9) *1.1 imp CoO x /SiO bulk CoO n. r. P0(CO)=10 Torr, P0(O2)=5 Torr. 273 K. Cat.: g. Pretreatment: oxidation at 573 and 673 K, followed by evacuation at 273 K. *Pretreatment: oxidation at 573 and 673 K, followed by evacuation at 673 K. Co 3 O 4 (110)-type A Co 3 O 4 (110)-type B H.-F. Wang et al, J. Catal., 296 (2012) Small Co oxide nanocluster was preparaed on silica support. nanocluster catalyst: 4.8 nm, impregnation catalyst 17 nm. Lowering the desorption temperature prevented the surface reduction from Co 3+ to Co 2+ and showed the activity for CO oxidation reaction. Desorption temperature of surface oxygen became lowered as Co oxide nanocluster size diminished.
15 M. Haruta, Faraday Discuss, 152 (2011)
16 Catalyst Preparation NiO(precursor)/support-T precursor: amm: [Ni(NH 3 ) 6 ] 2+ in ammonia solution ace: Ni(acac) 2 in MeOH nit: Ni(NO 3 ) 2 aq support: SiO 2 A.C.: activated carbon calcination temperature: 573, 673 or 773 K loading amount: 5 wt% Catalytic reaction Catalyst CN a (Ni-Ni) Yield b (%) NiO(amm)/SiO 2 -RT 7.3± NiO(amm)/SiO ± NiO(amm)/SiO ± NiO(amm)/A.C ± NiO(ace)/SiO ± NiO(nit)/SiO ± a Coordination number (CN) of Ni-Ni, determined by curve fitting analysis of Ni K-edge EXAFS for NiO catalysts. b Determined by gas chromatography using an internal standard method.
17 Ni K-edge XANES Ni-Ni Catalyst CN a r b (nm) de c (ev) DW d (nm) R e NiO(amm)/A.C ± ± ± NiO(ace)/SiO ± ± ± NiO(nit)/SiO ± ± ± bulk NiO (model) a Coordination number of Ni-Ni, b bond distance, c difference between model compound and experimental threshold energies, d Debye-Waller factor, e R-factor. FT range: nm -1. NiO Ni-Ni
18 TEM NiO(ace)/SiO 2-673) : 1.0 nm : 0.24 nm Catalyst CN NiO(amm)/A.C ±0.8 NiO(ace)/SiO ± nm NiO NiO(nit)/SiO ±2.1 bulk NiO 12 Ni K-edge EXAFS NiO
19 NiO(amm)/SiO 2 -T Ni-O-Si T. Lehmann et al., Micro. Meso. Mater., 151 (2012) (a) SiO 2 (b) [Ni(NH 3 ) 6 ] 2+ NiO Ni-O-Si SiO 2 (c) Ni-O-Si Ni K-edge EXAFS Nickel silicate
20 Catalytic reaction Ni-O-Si Catalyst NiO ratio (%) Ni-O-Si ratio (%) Yield (%) NiO(amm)/SiO 2 -RT NiO(amm)/SiO NiO(amm)/SiO NiO(amm)/SiO 2 -RT NiO(amm)/SiO NiO(amm)/SiO SiO 2 SiO 2 SiO 2 NiO Ni-O-Si
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20 5 Absorption spectra of biomolecules over wide energy range are very important to study their radiation effects in terms of the optical approximation proposed by Platzman. Using synchrotron radiation
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213 74 AlGaN/GaN Influence of metal material on capacitance for Schottky-gated AlGaN/GaN 1, 2, 1, 2, 2, 2, 2, 2, 2, 2, 1, 1 1 AlGaN/GaN デバイス ① GaNの優れた物性値 ② AlGaN/GaN HEMT構造 ワイドバンドギャップ半導体 (3.4eV) 絶縁破壊電界が大きい
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High sensitive determination of oxysterols in human plasma using gas chromatography-mass spectrometry (GC-MS) Saori Nakagawa and Susumu Yamato Oxysterols, cholesterol oxidation products, have been important
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Isogai, T., Building a dynamic correlation network for fat-tailed financial asset returns, Applied Network Science (7):-24, 206,
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