Online ISSN : 1884-6440
Print ISSN : 0385-1036
ISSN-L : 0385-1036
41 巻, 1 号
選択された号の論文の7件中1~7を表示しています
特集:サブナノポア測定技術の最新動向:多孔質吸着剤および分離膜の開発に向けて
総説
  • 萩原 英昭, Brian O’Rourke, 伊藤 賢志
    2016 年 41 巻 1 号 p. 2-8
    発行日: 2016年
    公開日: 2016/10/05
    ジャーナル オープンアクセス
    Positron annihilation (PA) has been documented as a powerful tool for evaluating molecular-level open spaces in various materials such as semiconductors, gas sensors and separation membranes. There are several advantages of PA over other methods; it is nondestructive, sensitive to holes/pores (of 0.3 nm~50 nm in size) irrespective of either open or buried, while adsorption porosimetry can only detect open porosity. Furthermore, PA with a variableenergy beam is widely utilized in the investigation of thin films with thicknesses from tens nm up to several µ m. This paper demonstrates several examples of PA applications to the hole/pore characterization for functional polymer materials including separation membranes, followed by the short review of the principle and instrumentation for the PA techniques.
  • 吉本 茂, 伊藤 賢志
    2016 年 41 巻 1 号 p. 9-15
    発行日: 2016年
    公開日: 2016/10/05
    ジャーナル オープンアクセス
    Ellipsometric porosimetry (EP) can elucidate physisorption isotherms with sampling weights of several µ g, while conventional porosimetries based on both volumetric and gravimetric adsorption techniques require sampling weights in the mg-order range. This enables EP to be a powerful tool for evaluating the size distribution of subnano/nano-scaled pores for functional thin materials. This paper describes the principle and method for EP, and also demonstrates examples of its application to the characterization of the porosity of thin films achieved using the flowtype EP at AIST.
  • 佐藤 純
    2016 年 41 巻 1 号 p. 16-21
    発行日: 2016年
    公開日: 2016/10/05
    ジャーナル オープンアクセス
    Density Functional Theory (DFT) is powerful method for the description of the adsorption and phase behavior of confined fluid in small pores, in particular, sub nanometer–size pores in which the thermophysical properties of strongly confined fluid differ from the properties of corresponding bulk liquid. Equilibrium density profiles of fluid in pores calculated by DFT lead the adsorption/desorption isotherm and pore size distribution. This modern, statistical and microscopic method gives advantages on reliable pore size distribution of microporous and mesoporous materials. Besides, accurate pore size analysis covers from micropores to mesopores can be performed by single method.
  • 吉岡 朋久, 高橋 麻里子
    2016 年 41 巻 1 号 p. 22-29
    発行日: 2016年
    公開日: 2016/10/05
    ジャーナル オープンアクセス
    A simple new characterization method of ultra–microporous structures was developed by measuring pressure change through gas diffusion in constant volume around room temperature. Several gas species such as He, Ne, Ar, N2, and CH4, which had different molecular size each other, were utilized as molecular probes for detecting effective micropore volume for gas diffusion under a room temperature in gas phase. The feature of this characterization method was that observed micropore volume for gas diffusion depended on the probing gas molecular size, and it enabled the quantitative estimation of effective micropore volume for each probing molecule. Zeolite Y (FAU) and ZSM–5 (MFI), which were known to have regular micoporous structures, were adopted as a standard sample for verifying the mulita–gas diffusion method. The conventional N2 adsorption at 77 K was also employed to characterize microstructures of those zeolites and both the validity and superiority of the proposed multi-gas diffusion method were examined. The volume of major pores of FAU, which is calledα–cage whose size is about 1.3 nm, was also detected by diffusion of larger molecules such as Ar and N2. Ordinal N2 adsorption method can give the pore size and volume of onlyα–cage, however, a bi–modal porous structure of FAU comprised ofα–cage and SOD (β– cage) was successfully detected by diffusion of smallest He molecule. For the case of ZSM–5, all probing gas molecules showed similar but slightly different micropore volumes due to the different diffusing molecular size. Adsorption enthalpy was also reasonably estimated by the technique.
  • 瀬下 雅博, 酒井 求, 松方 正彦
    2016 年 41 巻 1 号 p. 30-35
    発行日: 2016年
    公開日: 2016/10/05
    ジャーナル オープンアクセス
    We have successfully investigated nitrogen adsorption measurement using ZSM–5 type zeolite membrane prepared by seed assisted hydrothermal synthesis with various crystallization periods under non–destructive condition. Micro– and meso–pores derived from zeolitic and non–zeolitic structures were analyzed using nitrogen adsorption isotherm with the Saito–Foley model and the Kelvin equation. ZSM–5 membranes synthesized for various crystallization periods were characterized and evaluated by SEM, XRD, nanopermporometry and permeation tests. In this study, it could be considered that ZSM–5 membrane formation process had two–step as follows. First, ZSM–5 seed crystal was grown up in/onα–alumina support, and ZSM–5 micro–crystals generated in pore ofα–alumina support until 6 hours synthesis. After that, ZSM–5 crystals on theα–alumina support surface were predominantly grown up, and these crystals covered the support surface. After synthesis of 12 hours, the membrane had hardly defects.
  • 金指 正言
    2016 年 41 巻 1 号 p. 36-43
    発行日: 2016年
    公開日: 2016/10/05
    ジャーナル オープンアクセス
    Subnano pore size evaluation method based on modified gas translation (GT) model and derived Normalized Knudsen–based Permeance (NKP) for zeolite and amorphous silica membranes was reviewed. The estimated pore size based on NKP plot for organosilica membranes suggested the network size increased with an increase of carbon number between 2 Si atoms, which was very consistent with the order of pore size, as determined by the He and/or H2 selectivity. Pore size determination with the temperature dependence of gas permeances was also introduced, and quantitatively discussed the effect of fabrication temperatures on silica network size and small gas (He, H2, Ne, NH3, CO2, N2, CH4)permeation properties.
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