結晶性多孔体細孔を利用した物質合成
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- さわ ぜんじゅう
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1 Material Design in Cages of Micro-porous Materials Akihiko Koiwai, Noriaki Sugimoto 10nm ( 10nm ) ( 10nm ) ( Well-defined ) ( ) nm ( ) ( ) ( ALPO ) ALPOSAPOFSMMCM-41 R&D Vol. 31 No. 3 ( )
2 ( SAPO ) MCM-41 FSM ( Folded Sheets Mesoporous Material ) ALPOSAPO ( (a) ) SiO 4 AlO SiAl ( Si/Al ) SiAl ( Fig. 1(b) ) M 1-x ( Si x Al 1-x ) O 2 H 2 O ( M ) Si-O ( ) (a) Framework of zeolite X and zeolite Y, (b) structure of ion exchange sites in zeolite cages. Schematic diagram of channel structure of micro porous materials. (a) one dimensional channels, (b) two dimensional channels and (c) three dimensional channels. R&D Vol. 31 No. 3 ( )
3 ALPO ( (a) ) AlO 4 PO 4 ALPO ( Fig. 2 ) ALPO PSi SAPO ( Fig. 3(b) ) SAPO ALPOSAPO0.5-2nm nm ( ) Kresge MCM-41 ( Fig. 15 ) Inagaki FSM MCM-41FSM nm ( ) nm (1) ( )(2) (3) Channel structures of famous crystalline micro porous crystals. Channel dimension Micro porous material Maximum pore size / nm Crystal structure 1 zeolite L 0.71 hexagonal zeolite Ω 0.75 hexagonal VPI hexagonal ALPO hexagonal FSM hexagonal MCM hexagonal 2 mordenite orthorhombic ferierrite orthorhombic stilbite monoclinic 3 sodalite 0.22 cubic zeolite A 0.41 cubic zeolite X, zeolite Y 0.74 cubic erionite hexagonal ZSM orthorhombic R&D Vol. 31 No. 3 ( )
4 (1)(2) TO 4 ( T = Si, Al, P ) (3) ( ) sodalitezeolite A zeolite Xzeolite Y (a) sodalitesi zeolite A zeolite Xzeolite Y ( Fig. 5(b) ) CdS K Ag Structures of (a) aluminophosphate (ALPO) and (b) silicoaluminophosphate (SAPO). (a) Frameworks of sodalite, zeolite A, zeolite X and zeolite Y which are composed from sodalite cages. Schematic diagrams of clusters synthesized in cages of micro porous materials. (a) (CdS) 4 cluster encapsulated in a sodalite cage, (b) Se chain in a one dimensional channel. (b) Idealized structures of clusters encapsulated in sodalite cages of (i) sodalite, (ii) zeolite A, and (iii) zeolite X and zeolite Y. R&D Vol. 31 No. 3 ( )
5 SAPO ( ) Ag Pt Rh CdSe CdS PbS PbI 2 Clusters synthesized in micro-porous materials. Cluster Micro-porous material Synthetic method Properties Reference Na, K, Rb Zeolite A Ion exchange + vapor transfer Optical, magnetic 23, 4345) Ni, Fe Zeolite A, Ion exchange + H 2 reduction Magnetic 46, 47) Zeolite X Ag Sodalite Ion exchange Optical 24) Pt Zeolite A Ion exchange Catalytic, optical 25, 29) Rh Zeolite A Ion exchange Catalytic, optical 26, 29) CdS Zeolite A, Ion exchange + gas reaction Optical, structural 21, 41, 53, 54) Zeolite X, Zeolite Y PbS Zeolite A Ion exchange + gas reaction Optical 21) CdSe Zeolite Y Ion exchange + gas reaction Optical 27) ZnS, GaP Zeolite Y MOCVD Optical, magnetic 27) WO 3 Zeolite Y W(CO) 6 decomposition Optical 27) PbI 2 Zeolite A Ion exchange + gas reaction Optical 28) Se Zeolite A, Vapor transfer Optical, magnetic 3335) Zeolite X, ALPO AgBr, AgI, AgCl Sodalite Ion exchange Optical, magnetic 11) Ge MCM-41 GeH 4 gas decomposition HREM 55) Te, S, Br, I Zeolite A Gas transfer Optical 3538) p-nitroaniline ALPO-5 Gas transfer Optical 39, 66) (Dimethylamino)benzonitrile ALPO-5 Gas transfer Optical 56) Poly-aniline Mordenite Monomer transfer + polymerization Structural 58) Polypyrrole Mordenite Monomer transfer + polymerization Structural 57) Poly(acrylonitrile) Zeolite Y Monomer transfer + polymerization Structural 40) Polymethylacetylene Mordenite Monomer transfer + polymerization Structural 60) R&D Vol. 31 No. 3 ( )
6 (a)zeolite A zeolite Xzeolite Y ( Fig. 5(a) ) CdS NaCd Cd CdS CO Se S Te Br I p-nitroaniline polyaniline zeolite Ypolyacrylonitrile Fig. 6(b) ALPO Ga Te Hg Methods to synthesize materials in cages of micro porous materials. (a) CdS clusters synthesized by an ion exchange and gas reaction method, and (b) poly(aniline) polymerized in a channel after gas absorption ( Reprinted with permission from Chem. Mater. Copyright 1996 Am. Chem. Soc. ). R&D Vol. 31 No. 3 ( )
![polyacrylonitrile X CdS ( IR ) X ( EXAFS ) ( NMR ) ( HREM ) PbI 2 HREM An HREM image of PbI 2 confined in the cavities of zeolite A, at [001] incidence and taken on a 200kV electron microscope.](/docs-images/94/119986039/images/7-0.jpg "Table 2 Na K Ni Fe Ag Pt Rh K zeolite Aα ( Fig. 5(a) ) K4K zeolite A KK zeolite A K zeolite A αk ( K/zeolite A )K/zeolite A Fig. 89aj zeolite AαFig. 5(a) Si0.5nm K R&D Vol. 31 No. 3 ( 1996. 9 )")
7 polyacrylonitrile X CdS ( IR ) X ( EXAFS ) ( NMR ) ( HREM ) PbI 2 HREM An HREM image of PbI 2 confined in the cavities of zeolite A, at [001] incidence and taken on a 200kV electron microscope. Table 2 Na K Ni Fe Ag Pt Rh K zeolite Aα ( Fig. 5(a) ) K4K zeolite A KK zeolite A K zeolite A αk ( K/zeolite A )K/zeolite A Fig. 89aj zeolite AαFig. 5(a) Si0.5nm K R&D Vol. 31 No. 3 ( )
8 K Fig. 9 K K K Ozin Ag Pt Rh Ship-in-a-bottlePt RhIrPdRhIrRhFe 10nm Table 2CdSPbS CdSe Temperature dependence of ac magnetic susceptibility in K-loaded K/zeolite A for higher K densities. The dotted curve indicates the calculated susceptibility of spin h / 2 paramagnetic clusters assumed in each α cage. Magnetization at 1.7K and 100 Oe in K-loaded K/zeolite A as a function of the electron concentration per cluster. R&D Vol. 31 No. 3 ( )
9 RhCl Na + 3 aq. CO, H / zeolite A Rh 3+ 2 O / zeolite A (Rh) 6 (CO) 16 / zeolite A Rh 6 / zeolite A 90 C, 12hr 70 C 200 C C O 2 H 2 Synthetic scheme of Rh clusters in cages of zeolite A by a ship-in-a-bottle method. ZnSWO 3 PbI 2 Se AgBrAgI AgCl zeolite Azeolite Xzeolite YCdS Wang zeolite Azeolite X 0.5nm (CdS) 4 ( Fig. 4(a) ) (CdS) 4 /zeolite A (CdS) 4 /zeolite X ( CdS/ACdS/X ) (CdS) 4 CdS (CdS) 4 CdS (CdS) 4 CdS/ACdS/X ( (CdS) 4 10% ) (CdS) 4 ( 510nm ) Wang ( (CdS) 4 80% ) 350nm zeolite Azeolite XFig. 5(a) Absorption spectra of high- and low-loading CdS/A and CdS/X. Arrows show exciton peaks of high-loading CdS/A and CdS/X. Si (CdS) 4 ( CdS/ACdS/X )350nm CdS/ACdS/X Fig. 12 1µm ( ) R&D Vol. 31 No. 3 ( )
10 CdS/ACdS/X ( 1900nm ) χ (3) CdS χ (3) χ (3) χ (3) CdS/X Fig. 11χ (3) (CdS) 4 CdS/A χ (3) CdS/A CdS/X χ (3) ( ) ( ) Leon MCM-41 Ge GeMCM-41 Ge Ge GeMCM-41 MCM-41 Ge Ge Structure of super-cluster in CdS/A and CdS/X. Third-order nonlinear susceptibility (χ (3) ) and hyperpolarizability (γ) of CdS clusters at the fundamental wavelength of 1900nm. Sample χ (3) / esu γ / esu CdS/A CdS/X Surface-capped clusters a) CdS ( 1.5nm ) CdS ( 3.0nm ) a) Reference 52 Third-order nonlinear susceptibility (χ (3) ) spectra of high- and low-loading CdS/A and CdS/X. R&D Vol. 31 No. 3 ( )
11 MCM-41 µm MCM-41 ( SHG ) p-nitroaniline SHG SHG Cox p-nitroaniline SHG Mordenite SHG ALPO-5 SHG ALPO-5 ( Dimethylamino)benzonitrile SHG polyaniline ( Fig. 6(b) ) polypyrrole polyaniline polythiophene poly(acrylonitrile ) polymethylacetylene ( ) Phase contrast TEM micrograph obtained in axial bright-field imaging conditions shows the hexagonal framework of MCM-41. The Ge can be seen in some of the pores showing darker contrast due to stronger diffraction of the Ge crystals. Diagram of an MCM-41 crystallite showing the different possible orientations that produce the lattice images in Fig. 14. R&D Vol. 31 No. 3 ( )
12 1µm ( ) Bogomolov 100µm 39 Ozin mm µm Werner p-nitroaniline MCM-41FSM Ozin CdS K 100 R&D Vol. 31 No. 3 ( )
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陽電子科学 第4号 (2015) 3-8
4 (2015) 3 8 Japanese Positron Science Society Positron annihilation age momentum correlation (AMOC) measurement Abstract: Positron annihilation Age-MOmentum Correlation (AMOC) measurement is the coincidence