Coherent analysis of disordered mesoporous adsorbents using small angle X-ray scattering and physisorption experiments

Stoeckel, Daniela; Wallacher, Dirk; Zickler, Gerald A.; Perlich, Jan; Tallarek, Ulrich; Smarsly, Bernd M.

doi:10.1039/c3cp55072a

Cited by 25 publications

(39 citation statements)

References 64 publications

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“…The classic Porod’s scattering law has been widely applied for extracting the surface-to-volume ratio in two-phase systems such as porous materials 20 and colloids 22 . The GPSLM developed in this work significantly extends the applications of original Porod’s law from simple homogeneous systems to heterogeneous multiple-phase systems.…”

Section: Discussionmentioning

confidence: 99%

“…In 1951, Porod established the well-known Porod’s scattering law for scattering data of materials measured either by X-rays or neutrons 18 , 19 , which is now widely used for extracting the surface area and the average scattering length density (SLD) of materials in various relatively homogeneous two-phase systems such as porous materials 20 , biological macromolecules 21 , and colloids 22 . SLD is only a function of molecular formula and material density and therefore is an intrinsic property of a material.…”

Section: Introductionmentioning

confidence: 99%

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A non-invasive method to directly quantify surface heterogeneity of porous materials

et al. 2018

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It is extremely challenging to measure the variation of pore surface properties in complex porous systems even though many porous materials have widely differing pore surface properties at microscopic levels. The surface heterogeneity results in different adsorption/desorption behaviors and storage capacity of guest molecules in pores. Built upon the conventional Porod’s law scattering theory applicable mainly to porous materials with relatively homogeneous matrices, here we develop a generalized Porod’s scattering law method (GPSLM) to study heterogeneous porous materials and directly obtain the variation of scattering length density (SLD) of pore surfaces. As SLD is a function of the chemical formula and density of the matrix, the non-invasive GPSLM provides a way to probe surface compositional heterogeneity, and can be applied to a wide range of heterogeneous materials especially, but not limited to, porous media and colloids, using either neutron or X-ray scattering techniques.

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Section: Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

A non-invasive method to directly quantify surface heterogeneity of porous materials

et al. 2018

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“…Reproduced with permission from [75] In the case of higher-ordered porous materials, chords may go through the pores or the solid twice, which leads to side maxima and zeros in ( ) (Figure 7). The interpretation of ( ) measured for such materials is then a difficult task [92]. However, for the disordered carbon materials under consideration here, these higher order terms cancel out each other, and ( ) can be , porosity φ, number-average chord length l P , mean chord length of the pore l pore and the carbon matrix l solid , weight-averaged chord length l c , ansiometric ratio l c /l SAXS p , lateral correlation length l R , degree of angularity g(0), and the degree of disorder In the case of higher-ordered porous materials, chords may go through the pores or the solid twice, which leads to side maxima and zeros in g(r) (Figure 7).…”

Section: Analysis Of Carbons By Small-angle Scattering: Evaluation Of the Datamentioning

confidence: 99%

“…Perret and Ruland used this idea to develop a correct evaluation of the SAXS intensities obtained for non-graphitizable and glassy carbons by SAXS [46,50,82,91]. Later, Smarsly et al improved this analysis of SAXS-data [52,92] by the evaluation of the data in terms of the chord length distribution (CLD) [93].…”

Section: Introductionmentioning

confidence: 99%

Carbonaceous Materials Investigated by Small-Angle X-ray and Neutron Scattering

Härk

Ballauff

2020

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Carbonaceous nanomaterials have become important materials with widespread applications in battery systems and supercapacitors. The application of these materials requires precise knowledge of their nanostructure. In particular, the porosity of the materials together with the shape of the pores and the total internal surface must be known accurately. Small-angle X-ray scattering (SAXS) and small-angle neutron scattering (SANS) present the methods of choice for this purpose. Here we review our recent investigations using SAXS and SANS. We first describe the theoretical basis of the analysis of carbonaceous material by small-angle scattering. The evaluation of the small-angle data relies on the powerful concept of the chord length distribution (CLD) which we explain in detail. As an example of such an evaluation, we use recent analysis by SAXS of carbide-derived carbons. Moreover, we present our SAXS analysis on commercially produced activated carbons (ACN, RP-20) and provide a comparison with small-angle neutron scattering data. This comparison demonstrates the wealth of additional information that would not be obtained by the application of either method alone. SANS allows us to change the contrast, and we summarize the main results using different contrast matching agents. The pores of the carbon nanomaterials can be filled gradually by deuterated p-xylene, which leads to a precise analysis of the pore size distribution. The X-ray scattering length density of carbon can be matched by the scattering length density of sulfur, which allows us to see the gradual filling of the nanopores by sulfur in a melt-impregnation procedure. This process is important for the application of carbonaceous materials as cathodes in lithium/sulfur batteries. All studies summarized in this review underscore the great power and precision with which carbon nanomaterials can be analyzed by SAXS and SANS.

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“…The photocatalysts were further analyzed by SAXS, which provides structural information, that is, a broader and clearer view of catalysts formation and aggregation (57). The multihierarchical organization of these materials, their gyration radius (Rg), and fractal structure (P) were investigated through the Unified approach (41)(42)(43) in the Guinier and Power-law regions.…”

Section: Multi-scale Organization Of the Photocatalysts Analyzed By Saxsmentioning

confidence: 99%

Alternative Approaches in Development of Heterogeneous Titania-Based Photocatalyst

Ruiz¹,

Escobar²,

Silva³

et al. 2016

Semiconductor Photocatalysis - Materials, Mechanisms and Applications

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Three alternative approaches for the development of heterogeneous photocatalysts are comparatively evaluated, namely (i) the use of molecular imprinting concept for the development of heterogeneous catalysts employing rhodamine B as template and solgel as synthesis route; (ii) the impregnation of TiCl 4 on mixed nano-and micro-metric silicas, followed by calcination; (iii) the use of industrial and academic chemical residues as source of potential photocatalyst species impregnated on supports. All tests were carried on with rhodamine B as target molecule. For comparative reasons, photocatalytic tests were carried out with commercial titania (P25). The solids were characterized by nitrogen porosimetry, small-angle X-ray scattering (SAXS), zeta potential (ZP), diffuse reflectance spectroscopy in the ultraviolet region (DRS-UV), diffuse reflectance infrared Fourier transmission spectroscopy (DRIFTS), and Rutherford backscattering spectrometry (RBS). The supported catalysts resulting from silica nanoparticles and residue of the petrochemical industry achieved higher percentage of the dye degradation under ultraviolet (68.0 and 66.8%, respectively) radiation. The industrial waste reached the highest photocatalytic activity under visible (61%) radiation, while the commercial P25 achieved 82.0and 12.3% for ultraviolet and visible radiation, respectively. The textural and structural characteristics of the supported catalyst prepared with fumed silica and petrochemical waste (SiPe), namely the low-energy bandgap (1.8 eV), large surface area (280 m 2 g −1), high pore volume (1.9 cm 3 g −1), and high zeta potential value (−36.4 mV), may have been responsible for their high activity.

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Coherent analysis of disordered mesoporous adsorbents using small angle X-ray scattering and physisorption experiments

Cited by 25 publications

References 64 publications

A non-invasive method to directly quantify surface heterogeneity of porous materials

A non-invasive method to directly quantify surface heterogeneity of porous materials

Carbonaceous Materials Investigated by Small-Angle X-ray and Neutron Scattering

Alternative Approaches in Development of Heterogeneous Titania-Based Photocatalyst

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