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1.
G. W. Chądzyński P. Staszczuk D. Sternik M. Błachnio 《Journal of Thermal Analysis and Calorimetry》2008,94(3):623-626
Properties relating to porosity of solids (fractal dimensions, surface roughness parameters) were evaluated from atomic force
microscopy (AFM) and nitrogen adsorption-desorption isotherms measured at 77 K for selected high-temperature [(RE) Ba2Cu3O7−x, RE=Y, Sm] superconductors. Adsorption capacity, specific surface area, fractal dimensions were determined from adsorption-desorption
isotherms. The adsorption isotherms of all samples were S-shaped and belong to type II according to the IUPAC classification.
A linear relationship was demonstrated between the fractal coefficients calculated by using the two methods and values of
adsorption capacity of monolayer. 相似文献
2.
G. W. Ch?dzyński P. Staszczuk D. Sternik M. B?achnio 《Journal of Thermal Analysis and Calorimetry》2012,108(3):985-989
The porous structure of MgB2 has been investigated using atomic force microscopy (AFM) and sorption techniques. The fractal dimension and surface roughness parameters were evaluated from (AFM) and nitrogen adsorption?Cdesorption isotherms measured at ?196?°C for MgB2 sample. Adsorption capacity, specific surface area, and fractal dimensions were determined from adsorption?Cdesorption isotherms. The sorption isotherms of MgB2 samples were S-shaped and belong to type II according to the IUPAC classification. The results of fractal dimensions of MgB2 surface determined on the basis sorptometry and AFM data are compared. 相似文献
3.
Agnihotri S Mota JP Rostam-Abadi M Rood MJ 《The journal of physical chemistry. B》2006,110(15):7640-7647
Hexane adsorption on single-walled carbon nanotube (SWNT) bundles is studied by both simulation and experimentally using a previously developed computer-aided methodology, which employed a smaller physisorbed probe molecule, nitrogen, to explore the porosity of nanotube samples. Configurational-bias grand canonical Monte Carlo simulation of hexane adsorption on localized sites of the bundles is carried out to predict adsorption on their external surface and in their internal sites. These localized isotherms are then combined into a global isotherm for a given sample by using knowledge of its tube-diameter distribution and structural parameters, such as the fraction of open-ended nanotubes and the external surface area of bundles in samples, which have been independently determined from the standard nitrogen adsorption isotherm. The near-perfect replication of experimental isotherms demonstrates the validity of our method for structural characterization of SWNT samples. The effect of temperature on adsorption is also studied and the simulation results are extrapolated to predict the limiting hexane adsorption capacity of the samples. The similarity between the hexane adsorption isotherms and those of other organic molecules demonstrates that the adsorption mechanisms explored here are not specific to hexane, and that the proposed methodology can be potentially applicable to other sorbates with equal success. 相似文献
4.
Microporous silica gels were prepared in the pH range of 3–4 using sodium silicate as a silica source. Surface polarity of these gels was modified by grafting hydrophobic groups into the silica gel matrix with the help of hydrophilic solvents (acetone, acetonitrile, ethanol and methanol) and alkoxysilane compounds containing nonhydrolyzable alkyl groups. The porous framework and hydrophobicity of the silica gels were evaluated using nitrogen adsorption/desorption and water adsorption measurement techniques. All the measured isotherms were found to be type I which is indicative of microporosity. The surface area and microporosity of these samples were estimated by analyzing the measured nitrogen adsorption/desorption data using BET, Langmuir and Dubinin-Radushkevich (D-R) adsorption isotherms. The micropore size distribution was determined from their nitrogen adsorption isotherms using the slit-pore model of the Horvath-Kawazoe equation. Silica gels with high surface area (over 500 m2/g) as well as high microporosity (over 0.2 cc/g) were obtained at gelation pH of 3.50 from the water-solvent system. 相似文献
5.
活性炭纤维的微孔结构水吸附 总被引:3,自引:0,他引:3
测定了两种活性炭纤维(ACF)的氮气、水吸附等温线和XPS,研究了ACF的微孔结构和表面性质,用αs图分析氮吸附等温线获得了ACF的比表面积、微孔容量和微孔径。XPS表明在ACF表面存在多种不同结合状态的氧。水在ACF上的吸附等温线呈V型,具有很大的脱附滞后环。水通过与ACF表面的氧形成氢键发生吸附。ACF表面的初始吸附点多,则在低、中压时的水吸附量就大。 相似文献
6.
Imre Dékány József Németh Márta Szekeres Robert Schoonheydt 《Colloid and polymer science》2003,282(1):1-6
The surface of silica spheres with a diameter of 500 nm was modified with ethoxysilane. Hydrophilic and partially hydrophobic silica spheres were obtained, suitable for the preparation of two-dimensional monoparticle films at the liquid-air interface. The tendency of these particles to self-assemble is basically dependent on surface hydrophobicity. Liquid sorption excess isotherms were studied in ethanol-cyclohexane and ethanol-chloroform mixtures with the aim of characterizing the adsorption capacity of the particles. Specific surface area and porosity were measured by nitrogen adsorption. The specific surface area determined by liquid sorption was considerably larger than determined by gas adsorption. This is ascribed to penetration of ethanol into the pores and the swelling of the silica particles in ethanol. Surface modification of hydrophilic particles changed the film-forming properties of the particles. The compressibility and the lift-off area of the monolayer films of hydrophobic particles on water were higher than for the films of hydrophilic particles. 相似文献
7.
Hernane T. Barcelos Luclecia D. Nunes Guilherme W. Tavares Edesio F. C. Alcantara Alexandre G. S. Prado 《Journal of Thermal Analysis and Calorimetry》2011,106(2):421-425
Silica gel was modified by silanization reaction followed by functionalization of histamine in a heterogeneous route. These
materials were characterized by elementary nitrogen and chloride analyses, porosity, thermogravimetry, and infrared. The functionalized
surface adsorbed Cu(II), Co(II), Ni(II), and Zn(II) ions in an aqueous solution at 25 °C. The isotherms of adsorption are
in accordance with Langmuir model and the surface presented a great potential to form complexes metal-surface in the chemical
reason of 1:1. 相似文献
8.
P. Staszczuk M. Planda-Czyz D. Sternik M. Blachnio G. Grodzicka J. Pekalska S. Wasak K. Pilorz 《Journal of Thermal Analysis and Calorimetry》2006,85(2):339-349
The paper presents the complex studies of adsorption
and porosity of pure and modified–aluminium oxides samples. The presence
of Mn2+ and Ni2+ modifiers
on the aluminium oxide surface causes increase in water adsorption capacity
and its decrease in the case of benzene and n-octane.
This is due to decrease of specific surface area, volume and radius of pores
as a result of surface impregnation and microcrystals formation during modification
with manganese and nickel chlorides. Microcrystals formation on the surface
and porosity decrease where confirmed by the AFM and SEM studies.
From
the Q-TG and Q-DTG data, the energies of liquid desorption from the surface
of the samples and the functions of desorption, energy distribution were calculated.
High degree of nonlinearity of the run of the functions resulting from great
heterogeneity of the studied surface was found. Adsorption of cations creates
more homogeneous surface of aluminium oxide, and it is responsible for the
change in adsorbate molecule interaction energy and changes mechanism of adsorption
and desorption as well as thickness and structure of the adsorbed film. From
the experimental data some parameters characterizing adsorption properties
and porosity of the studied samples were determined using the measuring methods
(thermal analysis, sorptomate, porosimetry, AFM). 相似文献
9.
P. Staszczuk M. Majdan S. Pikus D. Sternik M. Błachnio 《Journal of Thermal Analysis and Calorimetry》2008,94(3):655-662
Complex studies of physicochemical properties of pure and modified of aluminia oxides samples are presented. The presence
of Mn2+ and Ni2+ modifiers on the aluminium oxide surface causes increase in water adsorption capacity and decrease in benzene and n-octane adsorption. This is due to decrease of specific surface area, volume and radius of pores as a result of surface impregnation
and microcrystal formation during modification with manganese and nickel chlorides. Microcrystal formation on the surface
and porosity decrease as confirmed by AFM, EDX and powder diffraction studies using automated diffractometer by step scanning.
From the Q-TG and Q-DTG data, the energies of liquid desorption from the surface of the samples and the functions of desorption,
energy distribution were calculated. High degree of nonlinearity of the functions resulting from great heterogeneity of the
studied surface was found. Adsorption of cations creates more homogeneous surface in aluminium oxide, and it is responsible
for the change in adsorbate molecule interaction energy and changes mechanism of adsorption and desorption as well as thickness
and structure of the adsorbed film. From the experimental data some parameters characterizing adsorption properties and porosity
of the studied samples were determined using the complex measuring methods (thermal analysis, sorptometry, porosimetry, AFM
and EDX). 相似文献
10.
Naono H Hakuman M Tanaka T Tamura N Nakai K 《Journal of colloid and interface science》2000,225(2):411-420
Four samples of MCM-41 mesoporous silicas whose average pore diameters are 2.4, 2.8, 3.2, and 3.6 nm were prepared using sodium orthosilicate and cationic surfactants of [CH(3)(CH(2))(n)N(CH(3))(3)]X (n=11, 13, 15, 17). These four samples were calcined at 1123 K in vacuo to obtain the dehydroxylated samples, which were further rehydroxylated at 298 K to obtain the rehydroxylated samples. The adsorption isotherms of nitrogen gas (77 K) for the 12 MCM-41 mesoporous silicas are of Type IVc, giving no adsorption hysteresis. On the other hand, the first adsorption isotherms of water vapor (298 K) for the dehydroxylated MCM-41 samples are quite different from those of nitrogen gas, giving the remarkable adsorption hysteresis. The second water isotherms for the rehydroxylated MCM-41 samples are of Type IV, showing slight hysteresis. Using the nitrogen isotherms, the relation between the pore size and carbon chain length of the surfactant has been determined, and the effect of dehydroxylation and rehydroxylation on the porous texture has been examined. Using the first and second water isotherms, the adsorption model of physisorbed waters adsorbed on the surface silanol groups has been proposed. From the pore size distribution curves of nitrogen and water, the presence of constrictions in the cylindrical pores has been predicted. Copyright 2000 Academic Press. 相似文献
11.
12.
Study of Water Adsorption on Activated Carbons with Different Degrees of Surface Oxidation 总被引:1,自引:0,他引:1
A carbon of wood origin was oxidized with different oxidizing agents (nitric acid, hydrogen peroxide, and ammonium persulfate). The microstructural properties of the starting material and the oxidized samples were characterized using sorption of nitrogen. The surface acidity was determined using Boehm titration and potentiometric titration. The changes in the surface chemistry were also studied by diffuse reflectance FTIR. Water adsorption isotherms were measured at three different temperatures close to ambient (relative pressure from 0.001 to 0.3). From the isotherms the heats of adsorption were calculated using a virial equation. The results indicated that the isosteric heats of water adsorption are affected by the surface heterogeneity only at low surface coverage. In all cases the limiting heat of adsorption was equal to the heat of water condensation (45 kJ/mol). 相似文献
13.
Prélot B Villiéras F Pelletier M Gérard G Gaboriaud F Ehrhardt JJ Perrone J Fedoroff M Jeanjean J Lefèvre G Mazerolles L Pastol JL Rouchaud JC Lindecker C 《Journal of colloid and interface science》2003,261(2):244-254
In the framework on a study of the acido-basic and sorption properties of iron oxides, a thorough characterization of two types of goethite powders was performed in several laboratories joined in a common project. Chemical analysis by ICPAES; high-resolution SEM, TEM, and AFM observations; XRD with line width analysis; and argon and nitrogen sorption isotherms were used for that purpose. The main crystallographic faces of goethite particles could be identified as {001}, {101}, and {121}, and their abundance correlated with the distribution of low-pressure argon adsorption local isotherms. These results will be very useful for further studies on the relationship between surface reactivity in aqueous solution and orientation of solid surfaces. 相似文献
14.
Investigation of hydrogen physisorption active sites on the surface of porous carbonaceous materials
Qu D 《Chemistry (Weinheim an der Bergstrasse, Germany)》2008,14(3):1040-1046
Hydrogen physisorption in different carbonaceous materials was investigated in liquid nitrogen (77 K). The total hydrogen adsorption was found to have a linear relationship with the surface area of pores <30 A. The surface area and porosity of the carbon materials were determined by dinitrogen adsorption at 77 K and density function theory (DFT). The active sites for hydrogen adsorption were investigated and found to be related to the edge orientation of defective graphene micro-sheet domains. 相似文献
15.
P. Staszczuk J. C. Bazan M. Błachnio D. Sternik N. J. Garcia 《Journal of Thermal Analysis and Calorimetry》2006,86(1):57-68
This paper presents possible applications of thermal analysis, sorptometry
and porosimetry to study physico-chemical properties of Na- and La-montmorillonite
samples, especially for determination of total surface heterogeneity. The
quasi-isothermal thermogravimetric (Q-TG) mass loss and its first derivative
(Q-DTG) curves with respect to temperature and time obtained during programmed
liquid thermodesorption under quasi-isothermal conditions have been used to
study adsorbed layers and heterogeneous properties of the Na- and La-montmorillonites.
Calculations of the desorption energy distribution functions by analytical
procedure using mass loss Q-TG and differential mass loss Q-DTG curves of
thermodesorption under quasi-isothermal conditions of polar and non-polar
liquid vapours preadsorbed on a material surface are presented. Parameters
relating to porosity of samples were determined by sorptometry, mercury porosimetry
and atomic force microscopy (AFM). From nitrogen sorption isotherms from sorptometry
and porosimetry methods, the fractal dimensions of montmorillonites have been
calculated. Moreover, a new approach is proposed to calculate fractal dimensions
of materials obtained from Q-TG curve; this is compared with values obtained
by the above methods. The total heterogeneous properties (energy distribution
function and pore-size distribution functions) of samples studied were estimated.
The radius and pore volume of the tested samples calculated on the basis of
thermogravimetry, sorptometry and porosimetry techniques were compared and
good correlations obtained. 相似文献
16.
Adsorption of nitrogen, argon, and methane in a polymer adsorbent MN-200 was studied in the pressure range of 0.1–40 MPa at temperatures of 303, 323, 343, and 363 K. The excess adsorption isotherms were measured, the adsorption volumes were determined, the adsorption isotherms of total content and the characteristic adsorption energies were calculated. Isosteric, integral, and average heats of adsorption were determined.
相似文献17.
Aoki Y Hashizume M Onoue S Kunitake T 《The journal of physical chemistry. B》2008,112(46):14578-14582
The Brunauer-Emmett-Teller (BET) surface area of 15 nm-thick films made of TiO2/polyelectrolyte bilayer was determined by quartz crystal microbalance (QCM) measurement of N2 and Ar adsorption isotherms at 77 K. The measurements were carried out using a home-built vacuum chamber that includes built-in 9 MHz QCM and cryostat units. As little as 1 ng of the adsorbed gas could be detected, and the BET surface area of a flat Au film (ca. 0.5 cm2) on an oscillator was determined within an experimental error of +/-5%. The titania/polymer composite film gives N2 and Ar adsorption isotherms consisting of a less-pronounced type-I curve and a break at around p/p0 = 0.7. This behavior is ascribed to the presence of irregular micropores and 6 nm phi-mesopores in the composite film. An analysis of the isotherms shows that the porosity of the composite film is about 12%, which is much smaller than that of bulk titania gel powder. The greater density appears to be related to the reported superior properties (robustness and resistance to electrical breakdown) of the organic/inorganic multilayer film. We conclude that the QCM-based, high-precision measurement of gas adsorption is a powerful tool for investigation of the detailed morphology of nanometer-thick films. 相似文献
18.
Y. S. Lipatov V. N. Bliznyuk T. T. Todosiychuk V. N. Chornaya R. K. Katumenu V. D. Konovalyuk 《Colloid and polymer science》2006,284(8):893-899
The thickness of nanolayers formed by adsorption from dilute and semi-dilute solutions on a solid SiO2 surface has been estimated from adsorption isotherms and atomic force microscopy (AFM) measurements for polystyrene, poly(butyl methacrylate), and their mixtures. The thickness of the adsorption layers depends strongly on the adsorption conditions and is controlled by several features of the adsorbing entities. In a low-concentration regime of adsorption, the length of polymer chains and the nature of their interaction with the substrate are the most important factors controlling the adsorption process. Above the critical concentration C*, macromolecular clusters (aggregates of several overlapping chains) are formed in a solution as a result of polymer chains self-assembly. Therefore, the final adsorption layer thickness is determined mainly by the size of the clusters in this concentrated regime of adsorption. We also demonstrate that in the case of polymer mixtures, the adsorption leads to formation of mosaic structures with alternation of the polymeric components in plane of the substrate and a characteristic domain size of approximately 200 nm for each of the components. AFM study reveals that the adsorbed layers are fractal structures whose fractal dimensions depend on the type of the polymer and the adsorption process. We demonstrate therefore that the structure of nanolayers of polymers and their mixtures on the solid surface can be regulated by variation of the adsorption conditions. 相似文献
19.
P. Staszczuk M. Błachnio E. Kowalska D. Sternik 《Journal of Thermal Analysis and Calorimetry》2006,86(1):51-56
Calculations based on the fractal geometry in the estimation of surface
heterogeneity are superior compared with conventional calculation methods
(e.g. from the data of gas adsorption or X-ray radiation scattering) as they
can be applied without limitation as far as the range of surface sizes of
the studied structures is concerned. This paper presents structural characteristics
of carbon and carbon- free nanomaterials based on the determined surface and
volumetric fractal coefficients. Fractal coefficients were determined from
the data obtained by means of two independent methods: sorptometry and atomic
force microscopy (AFM). Correlation between porosity parameters and fractal
coefficients is presented. 相似文献
20.
《Surface and interface analysis : SIA》2006,38(7):1117-1121
The surface energetic heterogeneity of pure and poly (acrylic acid) (PAA)‐adsorbed carbon nanotubes (CNTs) were studied by a nitrogen probe adsorption technique in a wide range of pressures. The adsorption energy distributions (AEDs) were calculated from the low‐pressure data of isotherms by deconvoluting the low‐pressure experimental nitrogen adsorption isotherms. The surface of pure CNTs is heterogeneous as its AED presents four peaks at 42, 52, 57 and 78 K. It is observed that the AED of CNTs can be evidently modified by PAA adsorption. While the PAA adsorption amount increases, the high‐energy peaks at 52, 57 and 78 K gradually weaken and diminish at last, whereas the low ones such as at 42 K strengthen and new peaks arise at 27 and 32 K. It is proposed that PAA molecules prefer interacting with and screening the higher energetic sites to the lower ones. It will facilitate the understanding of the polymer adsorption on energetic heterogeneity surfaces. Copyright © 2006 John Wiley & Sons, Ltd. 相似文献