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Deepa DEY, Valery PETRYKIN, Satoshi SASAKI, Masato KAKIHANA
2007 年 115 巻 1348 号 p.
808-812
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
A water-soluble tetraperoxo niobate [Nb(O
2)
4]
3- was prepared by reaction of niobic acid with H
2O
2 at pH=11 in aqueous ammonia solution. The corresponding ammonium salt, (NH
4)
3[Nb(O
2)
4], was grown as a single crystal, and its crystal structure was solved. A white precipitate has been obtained from the solution containing (NH
4)
3[Nb(O
2)
4] and Na
2CO
3. Based on the elemental, TG, redox titration and Raman spectroscopic analyses, we have concluded that the obtained compound was Na[Nb(O
2)
3]•2H
2O. This compound has been demonstrated to be a convenient precursor for synthesis of NaNbO
3 by simple calcinations in air at the reduced temperature of 400-500°C.
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Yoshitake MASUDA, Kazumi KATO
2007 年 115 巻 1348 号 p.
813-817
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
We produced a nano TiO
2 coating on SnO
2: F (FTO) electrodes in an aqueous solution. Anatase TiO
2 crystallized in the transparent solution at 50°C for 10 min. The FTO electrodes with markedly uneven surface were successfully covered by nano TiO
2 without annealing. The TiO
2 was deposited on the electrodes with no clearance, thus attaining high adhesion strength. The coating showed high transparency, over 75%, in visible-light regions of 400 to 800 nm, which is similar to bare FTO electrodes. The electrodes had a unique surface structure resulting from the combination of uneven FTO surface and microasperity due to the nano TiO
2 coating.
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Tetsuo UCHIKOSHI, Hidekazu TAKAHASHI, Naoto SHIRAHATA, Yoshio SAKKA
2007 年 115 巻 1348 号 p.
818-820
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
The cathodic electrodeposition of titania thin films from solutions containing a titanium salt was studied. Titanium tetrachloride was dissolved in an ethanol-water solution with hydrogen peroxide to prepare titanium peroxocomplex solutions. The deposition of the titania precursor on platinum-coated silicon wafer substrates was carried out by electrolysis of the solutions under constant current conditions. The deposits were thermally treated at fixed temperatures in air and then characterized by X-ray diffraction and scanning electron microscopy.
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Munehiro SAKANOUE, Yasuhiro KINOSHITA, Yuichi OTSUKA, Hiroaki IMAI
2007 年 115 巻 1348 号 p.
821-825
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
Nanoscale particles of rutile- and anatase-type titanium dioxides were selectively grown in acidic solutions of titanyl sulfate. The variation of photocatalytic activity as a function of UV light intensity was investigated using rutile and anatase powders having almost the same size (20-30 nm) and shape for a clear comparison of the performance depending on the crystal structure. Whereas the performance of anatase evaluated with the decomposition of methylene blue and the reduction of Cr(VI) under UV light was proportional to the square root of the UV light intensity, rutile showed a saturation of the activity in the high-intensity region regardless of the light sources and photochemical reactions. The saturating tendency of rutile weakened with an electron-withdrawing reaction or a decrease in the grain size. Then, the performance of rutile could be superior to that of anatase under illumination at a low-light-intensity. The difference in the photocatalytic performance between rutile and anatase is tentatively ascribed to a high recombination rate of generated electrons and holes associated with a low mobility of carriers in rutile.
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Yusuke MORISHIMA, Makoto KOBAYASHI, Valery PETRYKIN, Masato KAKIHANA, ...
2007 年 115 巻 1348 号 p.
826-830
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
Nanoparticles of brookite titanium oxide were prepared by microwave-assisted hydrothermal (MH) method at 200°C (heating time 5 min) for 0-60 minutes starting from the titanium peroxo glycolate complex in basic solution. The effect of microwave heating on the morphology of the brookite particles was examined. The samples were characterized by X-ray diffraction (XRD), Raman spectroscopy and transmission electron microscopy (TEM). It was found that all powders were composed of single phase brookite and contained two different types of particles. The activity in photodecomposition of oxalic acid by the samples prepared using MH method was higher than activities of brookite nanoparticles synthesized by the conventional hydrothermal method.
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Kiyofumi KATAGIRI, Kazutaka OHNO, Yoshitake MASUDA, Kunihito KOUMOTO
2007 年 115 巻 1348 号 p.
831-834
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
TiO
2 particles were obtained from aqueous solutions by the liquid phase deposition (LPD) method. The crystalline anatase TiO
2 particles could be prepared below 100°C directly from aqueous solutions. The growth behavior of TiO
2 particles via the LPD process was investigated by dynamic light scattering (DLS) measurement and transmission electron microscopy (TEM). From DLS measurement, the particle growth process shows a sigmoidal curve and can be divided into three stages, i.e., the initial stage, the acceleration stage, and the completion stage. TEM measurements revealed that the primary particles with a diameter of ca. 50 nm were deposited at the initial stage. At the acceleration stage, these primary particles were assembled to form raspberry-like particles with a diameter of ca. 300 nm. Finally, the particles were precipitated by further aggregation with the micro-meter size at the completion stage.
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Makoto KOBAYASHI, Valery PETRYKIN, Masato KAKIHANA, Koji TOMITA
2007 年 115 巻 1348 号 p.
835-839
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
Single phase rutile was synthesized by a simple hydrothermal treatment of an aqueous titanium glycolate complex solution at 200°C for 24 h. The obtained sample was composed of 50×150 nm rod-like nanoparticles. The aspect ratio of the prepared particles could be controlled by adding glycolic acid or lactic acid to reaction solution. Up to 30×2000 nm whisker-like particles could be obtained. The hydroxycarboxylic acids favor development of specific crystal facets and allow to control the aspect ratio of the rutile nanoparticles. We also proposed a model, which explains formation of anatase and rutile, and disappearance of anatase particles during rutile crystals development.
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Min ZENG, Naofumi UEKAWA, Takashi KOJIMA, Kazuyuki KAKEGAWA
2007 年 115 巻 1348 号 p.
840-845
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
The titania particles were prepared by aging the mixture of titanium isopropoxide (TIP) and H
2O at 318 K. The anatase titania particles were obtained by the aging procedure at 318 K for more than 16 h. The aging temperature was quite low to obtain anatase-type titania particles. According to the DTA measurement, the amount of amorphous phase included in the titania particles decreased with increases in the aging time. Furthermore, the titania particles obtained by aging the mixture of TIP and H
2O at 318 K for 24 h contained no amorphous phase. The obtained titania particles had a high BET specific surface area of more than 250 m
2/g. To characterize the titania surface, the adsorption isotherms of the organic dye molecules in an aqueous solution were measured. The negatively charged Evans blue molecules strongly adsorbed on the titania surface obtained by the low-temperature hydrolysis reaction as compared with the results of the methylene blue molecules. Furthermore, the decomposition kinetics of the dye molecules by the photocatalytic activity also deepened with the charge of the dye molecules. The relation between the UV irradiation time and the molar ratio of the decomposed dye molecules followed the Avrami equation. According to the results of the analysis using the Avrami equation, the Evans blue molecules were decomposed on the titania particle surface. In contrast, the methylene blue molecules were decomposed in the aqueous solution. The difference in kinetics was related to the interaction of the dye molecules and the titania surface. The high surface area of the titania particles obtained the low-temperature hydrolysis reaction of titanium alkoxides enhanced the effect of the surface interaction on kinetics of the photocatalytic activity.
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Osamu SAKURADA, Masaaki SAITO, Tomokazu OHYA, Minoru HASHIBA, Yasutaka ...
2007 年 115 巻 1348 号 p.
846-849
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
Titanate aqueous solution (TIP-Lac) prepared by direct reaction of titanium tetraisopropoxide (TIP) with lactic acid (Lac) in water shows characteristics of a polyanion and acts as a dispersant for preparing aluminum oxide suspension. When small amounts of TIP-Lac were added to aqueous dispersions of alumina, which had a positive surface charge at pH 4, agglomeration of alumina occurred, and alumina was redispersed by further addition of TIP-Lac. The fluidity and dispersion of alumina were studied from the zeta potential, sedimentation velocity, and rheological measurements.
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Noriko SAITO, Hajime HANEDA, Kunihito KOUMOTO
2007 年 115 巻 1348 号 p.
850-855
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
ZnO films were electrolessly deposited in the aqueous solution of zinc nitrate and dimethylamine-borane (DMAB). ZnO was deposited on the Pd catalyst layer grown by sputtering on the quartz substrate. The influences of the growth conditions to the morphology of the ZnO films have been examined. Amorphous gel-like deposits were observed at 30°C. Both amorphous gel and ZnO crystals were deposited at 40°C. Above 55°C, ZnO mono-particulate films with few particles being observed on them were obtained. The morphology of the ZnO depended on the concentration of Zn (0.01-0.5 mol•dm
-3). In a low Zn concentration, spindle-shaped particles composed of fibers were deposited. In a high Zn concentration, platelet deposits of a few micrometers were observed. For deposition of hexagonal shape ZnO, the Zn concentration of 0.05 mol•dm
-3 was suited. The concentrations of DMAB (0.001-0.05 mol•dm
-3) did not influence the morphology of the deposits. At 55°C, the deposition began just after soaking in the solution. Initially, the agglomerated particles of about 200 nm composed of small particles (10-30 nm) were deposited. According to the particle growth, the particles became hexagonal in shape. The hexagonal ZnO particles grew to micron sizes by the reaction for 4 h. At high reaction temperatures, the initial nucleation density was higher, and ZnO films of finer particles were obtained in a short period. After the catalyst layer was covered by ZnO, the growth rate became slow, but the growth continued due to the thermal decomposition of DMAB.
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Yasuhiro SAITO, Yukinari SEKIGUCHI, Minoru MIZUHATA, Shigehito DEKI
2007 年 115 巻 1348 号 p.
856-860
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
SnO
2 thin film was prepared from a SnF
2-HF aqueous solution with the addition of H
3BO
3 aqueous solution by the Liquid Phase Deposition (LPD) method. We focused on the construction of the continuous deposition system and the control of the deposition rate. Parent solution containing SnF
2-HF was intermittently added to the treatment solution, which consists of the excess amount of H
3BO
3. As a result, the deposition rate can be maintained almost constant, at least for 24 h, and uniform SnO
2 film with the thickness of more than 600 nm was obtained.
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Toshiyuki TAKAMUKU, Yasukuni NOGUCHI, Miki NAKANO, Masaru MATSUGAMI, H ...
2007 年 115 巻 1348 号 p.
861-866
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
Mixing states for aqueous solutions of water-miscible organic solvents, acetonitrile and 1,4-dioxane, have been investigated at the molecular level by means of small-angle neutron scattering (SANS) and NMR relaxation. It has been shown that the organic solvent and water molecules are inhomogeneously mixed each other at the molecular level, although their mixtures are homogeneous at the macroscopic scale. Thus, both organic solvent clusters and water clusters coexist in the mixtures. The present investigation has also revealed that the microinhomogeneity of acetonitrile-water and 1,4-dioxane-water mixtures is gradually enhanced by cooling or adding salts toward phase separation. Based on the results, the effect of microinhomogeneity for solvent mixtures on chemical reactions was considered.
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Feng DANG, Kai KAMADA, Naoya ENOMOTO, Junichi HOJO, Keiji ENPUKU
2007 年 115 巻 1348 号 p.
867-872
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
The magnetite nanoparticles were synthesized through a process including dissolution of Fe(OH)
2 and precipitation of an oxidized phase under ultrasonic irradiation in an aqueous solution. It was found that the ultrasonic irradiation accelerated the formation of magnetite. The crystallinity and magnetic properties of the magnetite particles synthesized under ultrasonic irradiation were better than those synthesized under mechanical stirring. The effects of dissolved gas and pH value were also studied. The dissolved gas was important to the effect of ultrasound on the formation of magnetite and the properties of particles were different when different gases were used as dissolved gas in the sonochemical synthesis of magnetite. The magnetite particles were successfully synthesized even at a neutral solution under ultrasonic irradiation. The low pH value delayed the formation of magnetite and affected the morphology of magnetite particles.
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Kongjun ZHU, Kazumichi YANAGISAWA, Rie SHIMANOUCHI, Ayumu ONDA, Koji K ...
2007 年 115 巻 1348 号 p.
873-876
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
A continuous series of solid solutions in the system of strontium and lead hydroxyapatite, Pb
xSr
1-xHAP (
x=0-1), was successfully synthesized by low-temperature mixing method (LTMM) at 160°C for 12 h under hydrothermal conditions. The samples were characterized by chemical analysis, electron microscopic observation and X-ray powder-pattern fitting. The site of the metal ions in the solid solutions was analyzed by the Rietveld method. The lattice constants of the prepared solid solutions varied linearly with Pb contents. It was found that Pb
2+ ions in the solid solutions preferentially occupied the M(2) site in the apatite structure.
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Bing LIU, Deping WANG, Wenhai HUANG, Aihua YAO, Masanobu KAMITAKAHARA, ...
2007 年 115 巻 1348 号 p.
877-881
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
Silica-coated magnetite nanoparticles were synthesized via sol-gel process, which comprises the hydrolysis and condensation of TEOS in ethanol/water solution with NH
3 aq. as catalyst. Transmission electron microscope and vibrating sample magnetometer was applied to characterize the nanocomposite particles. Results reveal that the reaction parameters including volume ratio of alcohol/water, the concentrations of NH
3 aq and TEOS play important roles of the formation of silica shell. The thickness of silica shell increased with TEOS concentration. The nanocomposite particles remained favorable superparamagnetism. The formation of silica shell mainly came from the aggregative growth of silica primary particles on the surface of magnetite nanoparticles.
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Ryoji TAKAHASHI, Satoshi SATO, Toshiaki SODESAWA, Yasuhide KOJIMA, Nao ...
2007 年 115 巻 1348 号 p.
882-887
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
Bimodal porous silica gel with both macropores and mesopores was prepared from water glass (WG) in the presence of low-molecular-weight surfactant, sodium dodecyl sulfate (SDS), by inducing phase separation during sol-gel reaction. The macroporous morphology was controlled by changing starting composition and gelation temperature: the change in the concentration of SDS was effective to control connectivity of macropores and silica gel skeleton in micrometer size, and the gelation temperature significantly affected macropore size. From the change in morphology with the concentration of SDS, it is considered that a homogeneous reacting solution separated into a phase of SDS and that of polymerized silica in contrast to other silica-surfactant systems, where phase separation proceeds between solvent and surfactant associated with silica gel surface. It is also suggested that SDS forms associated complex or micelle in aqueous acidic solution, and the formation of such structure plays an important role in the phase stability. We also controlled mesopore structures in the macroporous silica gel by aging as-geled samples under basic conditions.
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Isao KIMURA, Tatsuro HONMA, Richard E. RIMAN
2007 年 115 巻 1348 号 p.
888-893
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
Interfacial reaction in a multiple emulsion, was carried out with the aim of preparing hollow hydroxyapatite (HAp) microspheres. The multiple emulsion was a W/O/W emulsion, made of dipotassium hydrogen phosphate solution as an inner aqueous phase, cyclohexane as an oil phase, and calcium nitrate solution as an outer aqueous phase. The phase diagrams of Ca(NO
3)
2-K
2HPO
4-H
2O system were drawn by thermodynamic computations and used to simulate the chemical process in a multiple emulsion for determining the experimental conditions. Single phase HAp was synthesized at an initial pH of 12.0. HAp with a Ca/P ratio was measured by inductively coupled plasma spectroscopy to correspond to 1.49. The product was composed of microspheres of 0.5 to 2 μm in diameter. Each microsphere was composed of acicular particles with an aspect ratio of 2.5-10 with a short axis length of about 20 nm.
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Kazumichi YANAGISAWA, Daisuke GUSHI, Ayumu ONDA, Koji KAJIYOSHI
2007 年 115 巻 1348 号 p.
894-897
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
Large plate crystals of boehmite up to 4 μm were prepared from Al(NO
3)
3 solutions with the addition of NaOH under hydrothermal conditions at 250°C for 6 h. The conditions to obtain monodispersed boehmite large plate crystals were determined to be in the range of OH/Al molar ratio from 3.5 to 3.8 and Al concentration from 1.3 to 2.0 mol/kg. Bayerite formed by mixing the starting materials changed to gibbsite at 200°C, and at the same time boehmite started to crystallize from gibbsite. Even after complete phase change from gibbsite, small boehmite crystals grew larger by dissolution and precipitation mechanism. The key to obtain boemite large plate crystals is the preparation of homogenous fine boehmite crystals by quickly heating fine gibbsite crystals to the boehmite stable region, as well as the selection of OH/Al molar ratio and Al concentration.
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Peilin ZHANG, Shu YIN, Ruixing LI, Tsugio SATO
2007 年 115 巻 1348 号 p.
898-900
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
The layered structure of H
4Nb
6O
17 prepared by the proton exchange of K
4Nb
6O
17 was modified by using various n-alkylamines as swelling agents to enlarge the interlayer space. The incorporation of TiO
2 into the interlayer space was also attempted. XRD, EDX, and TG-DTA measurements were employed to characterize the products. The photocatalytic activities were evaluated by NO
x destruction under photo-irradiation with different light wavelengths. The results showed that the photocatalytic activity of a layered compound could be significantly promoted just by enlarging the interlayer space of it. And the incorporation of TiO
2 could further enhance the activity.
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Haruo SUDO, Bunpei HATANO, Jun-ichi KADOKAWA, Hideyuki TAGAYA
2007 年 115 巻 1348 号 p.
901-904
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
Layered double hydroxide (LDH) has positive charge between the layers and is known as anion exchangeable clay being able to intercalate various organic and inorganica nions. In this study, organic-inorganic layered nanohybrids were prepared by intercalation of organic carboxylate anions into Zn/Al LDH in an aqueous solution. Four intercalation compounds were prepared by the reactions of succinate, terephthalate, 4-pyridinecarboxylate, and
p-hydroxybenzoate anions with Zn/Al LDH in aqueous solution. Interlayer spacing of these four intercalation compounds decreased by the thermal treatment at 363 K, and recovered by the treatment in water, reversibly.
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Astushi NAKAHIRA, Kouji YOKOTA, Seiichi KATO, Noriyuki HIROTA, Hidehik ...
2007 年 115 巻 1348 号 p.
905-908
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
Alumina with nanoholes was prepared by anodic oxidation of aluminium and subsequently the synthesis of Fe nanofibers was attempted using nanoholes in alumina as a template. Various Fe nanofibers were synthesized by electroplating into alumina templates and subsequent chemical treatments in mixed-acid solutions to remove the templates. Obtained Fe nanofibers had the dimension with 20 nm-30 nm in diameters and typically 500 nm-2 μm in length. Effect of anodic oxidation treatments for a template on the microstructure of Fe nanofibers was examined. The length of Fe nanofibers could be changed by modifying the synthetic conditions, such as anodic oxidation times and electroplating times.
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Chiori SATO, Naoki ESUMI, Keita KUBO, Katsuyuki SUZUKI, Takahiko BAN, ...
2007 年 115 巻 1348 号 p.
909-915
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
The growth of inorganic particles with chemical zoning is studied with the reaction-diffusion in gel. The two kinds of cations Ca
2+ and Mg
2+ diffuse into a gel, and a reactive anion CO
3 2- diffuses from the opposite side. The distinct chemical zoning was generated in the particles formed in the agar and in the restricted concentration range of the electrolytes in the reservoir. No chemical zoning is observed in gelatin. The particle structure is significantly affected by the gel type especially in the early stage of the growth. These characteristics can be understood taking into account the difference in the diffusion rates of the two kinds of cations. When several kinds of cation pairs are used, there is a pair that forms a novel stripe pattern of the precipitates. The pattern is also controlled by the difference in the diffusion rates of two kinds of cations.
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Yasuha HIGASHINE, Shinobu FUJIHARA
2007 年 115 巻 1348 号 p.
916-919
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
Fluorite-type CeO
2 nanorods were synthesized from aqueous CeCl
3 solutions containing polyethylene glycol, NaOH, and NaCl. The solutions were hydrothermally treated at 140°C, resulting in the formation of nanorod-like precipitates. Further annealing of the precipitates led to the growth into well-defined nanorods 5-10 nm in diameter and 50-200 nm in length. It was found that the addition of NaCl to the solution could enhance the one-dimensional growth of CeO
2 and reduce the degree of aggregation. A high-resolution transmission electron microscopic observation revealed that the nanorod was single-crystalline and its growth direction was along the [110] axis of the cubic CeO
2 structure. Our results then demonstrated that the unusually [110]-oriented CeO
2 nanorods could be grown by a facile synthesis method.
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Masayuki IWAMURA, Valery PETRYKIN, Masato KAKIHANA
2007 年 115 巻 1348 号 p.
920-924
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
In this work we applied a “micro-gel spray freeze-drying method” for synthesis of YVO
4:Eu
3+ phosphor materials. The proposed approach combined usual freeze-drying technique with water soluble polymers: agarose, gelatin and PVA to reinforce the frozen particles due to gel formation. The nature and concentration of these water soluble compounds determine the structure of the gels, and thus it allows controlling microstructure of the ice particles. It was found that a polymer and its concentration affects the morphology of the primary particles and prevents aggregation of secondary particles during freeze-drying as well as during thermal treatment of the precursors in synthesis of YVO
4:Eu
3+ phosphor.
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Yasuaki TOKUDOME, Koji FUJITA, Kazuki NAKANISHI, Kazuyoshi KANAMORI, K ...
2007 年 115 巻 1348 号 p.
925-928
発行日: 2007年
公開日: 2007/12/01
ジャーナル
フリー
Yttrium aluminum garnet, Y
3Al
5O
12, (YAG) monoliths with well-defined macropores have been prepared from ionic precursors using the sol-gel method accompanied by phase separation. The addition of propylene oxide to the starting solution controls the gelation, while the addition of poly(ethylene oxide) induces the phase separation. Polymerization-induced phase separation and gelation concur by an appropriate selection of the starting composition, which allows the production of bicontinuous macroporous nanocomposite gels in large dimensions (~10×10×10 mm
3). During heat treatment at 800°C, the monolithic nanocomposite gels crystallize into YAG without the formation of any intermediate phases or the precipitation of impurity phases, indicating higher homogeneity of cation distribution in the dried gels. The macroporous YAG network was maintained even after heat treatment at 1000°C for 10 h.
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