Method of Discrimination of Surface Fractality

Abstract A simple method for the discrimination of surface fractality is proposed. This method is based on the comparison of the nitrogen adsorption isotherm on a given sample with the "standard" isotherm on a smooth surface. The proposed comparative method makes it possible to determine the lower limit of the scale range of surface fractality. A thermodynamic method is recommended as a complement to fractal analysis in the scale range of about 10-1000 A. The results of the investigation of surface roughness are presented with examples of typical samples of silica gels, porous glasses, apatite, and coal.

A model for polybutadiene coatings on porous silica

Non-wetting viscous liquids such as oligobutadiene prefer “active” sites such as pores during the process of physisorption. Thus, polybutadiene (PBD) coatings on porous silica do not result in a homogeneous polymer film but in an inhomogeneous loading where the bulk polymer is mainly sited in the pores of the silica. An increasing polymer loading leads to increasingly filled pores instead of a thicker polymer film. We cannot exclude the possibility that most of the surface is covered at least with a thin polymer film since the chromatographic behaviour is relatively good for polypeptides, which are highly susceptible to the silanol groups of silica.

Capillary Hysteresis in Nanopores: Theoretical and Experimental Studies of Nitrogen Adsorption on MCM-41

Capillary hysteresis in cylindrical nanopores has been studied using MCM-41 as the prime example of a mesoporous material. These materials, due to their regular pore structure, can be considered to be candidates for reference adsorbents for standardizing adsorption measurements and methods for characterization of porous solids. They provide a unique opportunity for verification of theoretical models employed for predicting phase equilibrium in confined geometry. Three samples with monodisperse pore channels have been synthesized and examined using X-ray diffraction (XRD). Nitrogen adsorption isotherms were modeled using nonlocal density functional theory (NLDFT) in a wide range of pore size…

Critical Appraisal of the Pore Structure of MCM-41

Purely siliceous and aluminosilicate types of MCM-41 were synthesized and characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), nitrogen sorption (NS) and size exclusion chromatography (SEC).

SELF SIMILARITY IN SWELLING SYSTEMS: FRACTAL PROPERTIES OF PEAT

Sphagnum peat gives an example of a swelling system with a self-similar structure in sufficiently wide range of scales. The surface fractal dimension, dfs, has been calculated by means of thermodynamic method on the basis of water adsorption and capillary equilibrium measurements. This method makes possible the exploration of the self-similarity in the scale range over at least 4 decimal orders of magnitude from 1 nm to 10 μm. In a sample explored, two ranges of fractality have been observed: dfs ≈ 2.55 in the range 1.5–80 nm and dfs ≈ 2.42 in the range 0.25–9 µm.

Theoretical and Experimental Studies of Capillary Hysteresis in MCM-41

Mesoporous materials of MCM-41 type are considered to be reference model adsorbents due to their regular pore structure. Nitrogen adsorption isotherms on MCM-41 are modeled using the Non-Local Density Functional Theory (NLDFT). The thermal dependence of the thermodynamic hysteresis predicted by the NLDFT is confirmed by experimental measurements. The nitrogen hysteresis on MCM-41 at temperatures below 77.4 K or in pores greater than 4 nm is associated with the metastability of the adsorption branch of the isotherm. In the hysteresis regime, the desorption branch is likely to be thermodynamically stable and is recommended for calculating pore size distributions.

Characterization of MCM-48 Materials

Mesoporous molecular sieves of MCM-48 type were prepared by conventional hydrothermal and novel room temperature syntheses. Scanning electron microscopy (SEM) studies have shown that nonagglomerate...

Berechnung der Fraktaldimension einiger poröser Feststoffe aus der Stickstoff-Adsorptionsisotherme

Pore Size Analysis of MCM-41 Type Adsorbents by Means of Nitrogen and Argon Adsorption

Methods of nonlocal density functional theory (NLDFT), proposed recently for predictions of adsorption equilibrium and calculations of pore size distributions in micro- and mesoporous materials, were tested on reference MCM-41 materials. Five newly synthesized MCM-41 adsorbents with presumably uniform pore channels varying from 32 to 45 Å were characterized by X-ray diffraction (XRD), nitrogen adsorption at 77 K, and argon adsorption at 77 and 87 K. New sets of intermolecular interaction parameters of the NLDFT model for N2 and Ar adsorption on MCM-41 were determined. The parameters were specified to reproduce the bulk liquid-gas equilibrium densities and pressures, liquid-gas interfacial t…

Electrophysical properties of metal–solid-electrolyte composites

Liquid intrusion and alternative methods for the characterization of macroporous materials (IUPAC Technical Report)

This document deals with the characterization of porous materials having pore widths in the macropore range of 50 nm to 500 μm. In recent years, the development of advanced adsorbents and catalysts (e.g., monoliths having hierarchical pore networks) has brought about a renewed interest in macropore structures. Mercury intrusion–extrusion porosimetry is a well-established method, which is at present the most widely used for determining the macropore size distribution. However, because of the reservations raised by the use of mercury, it is now evident that the principles involved in the application of mercury porosimetry require reappraisal and that alternative methods are worth being listed…

Gravimetric characterisation of the surface properties of a porous drug carrier

The gas adsorption method is the most common means to characterise the topology of solid surfaces with regard to its use as an adsorbent. Adsorption isotherms are determined advanta-geously using a vacuum microbalance: Thermogravimetric techniques allow the observation of sample degassing and its optimization. The dry mass is determined in situ, the mass of gas adsorbed is measured directly and different gases can be used without calibration. From the isotherm the pore size distributions, specific surface area, fractal dimension and density can be derived. Commercially available gravimetric sorption apparata and vacuum balances as well as software for data evaluation are reviewed in tables.…