Correlating pore size and shape to local disorder in microporous carbon: A combined small angle neutron and X-ray scattering study

Jafta, Charl J.; Petzold, Albrecht; Risse, Sebastian; Clemens, Daniel; Wallacher, Dirk; Goerigk, G.; Ballauff, Matthias

doi:10.1016/j.carbon.2017.07.046

Cited by 53 publications

(83 citation statements)

References 47 publications

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“…For instance, it was used to study pore volume fractions of micro- and mesopores of porous powders from CaCo 3 [ 19 ]. It was also used in combination with small-angle neutron scattering to investigate pores in disordered porous carbon, where special care was taken of the evaluation procedure related to the porous nature of the graphitic material [ 20 ]. The necessity of SAXS to access buried porosity was shown, e.g., with the characterization of disordered carbons [ 21 ].…”

Section: Introductionmentioning

confidence: 99%

Pore Development during the Carbonization Process of Lignin Microparticles Investigated by Small Angle X-ray Scattering

et al. 2021

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Application of low-cost carbon black from lignin highly depends on the materials properties, which might by determined by raw material and processing conditions. Four different technical lignins were subjected to thermostabilization followed by stepwise heat treatment up to a temperature of 2000 °C in order to obtain micro-sized carbon particles. The development of the pore structure, graphitization and inner surfaces were investigated by X-ray scattering complemented by scanning electron microscopy and FTIR spectroscopy. Lignosulfonate-based carbons exhibit a complex pore structure with nanopores and mesopores that evolve by heat treatment. Organosolv, kraft and soda lignin-based samples exhibit distinct pores growing steadily with heat treatment temperature. All carbons exhibit increasing pore size of about 0.5–2 nm and increasing inner surface, with a strong increase between 1200 °C and 1600 °C. The chemistry and bonding nature shifts from basic organic material towards pure graphite. The crystallite size was found to increase with the increasing degree of graphitization. Heat treatment of just 1600 °C might be sufficient for many applications, allowing to reduce production energy while maintaining materials properties.

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Section: Introductionmentioning

confidence: 99%

Pore Development during the Carbonization Process of Lignin Microparticles Investigated by Small Angle X-ray Scattering

et al. 2021

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“…For q > 0.1 Å À1 a scattering proportional to q À2 is observed, which is customary for this type of material. The exponent 2 results from the disordered structure of the carbon layers that make up the solid at nearly atomic scale (Perret & Ruland, 1968;Jafta et al, (a) Small-angle X-ray scattering (SAXS) patterns of the Vulcan XC72 porous solid and of the catalysts consisting of PtNi nanoparticles supported on Vulcan XC72; the dash-dotted blue lines are power laws of the type I ' q À2 and I ' q À4 . (b) Nitrogen adsorption-desorption isotherms of Vulcan XC72.…”

Section: Methodsmentioning

confidence: 99%

“…where I S is given by equation 6, the constant b accounts for the turbostratic structure of carbon (Perret & Ruland, 1968;Jafta et al, 2017) and A is a factor that accounts for the unknown amount of material crossed by the X-ray beam as well as for the scattering cross section of carbon. In addition to A and b, the only fitting parameter is the solid fraction S , which is constrained to remain in the interval ½0 0:48, as imposed by nitrogen adsorption.…”

Section: Saxs Analysis Of the Empty Supportmentioning

confidence: 99%

Small-angle scattering by supported nanoparticles: exact results and useful approximations

2019

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In functional materials, nanoparticles are often dispersed in a porous support for the purpose of stabilizing them. This makes their characterization by small‐angle scattering challenging because the signal comprises contributions from the nanoparticles of interest, from the inert support and from their cross‐correlation. Exact analytical expressions for all three contributions are derived in the case of a Gaussian‐field model of the porous support, with nanoparticles randomly distributed over the surface. For low nanoparticle loading, the expressions simplify to the addition of properly scaled support and particle scattering. For higher loadings, however, the cross‐correlation cannot be ignored. Two approximations are introduced, which capture correlation effects in cases where the pores of the support are much larger or only slightly larger than the nanoparticles. The methods of the paper are illustrated with the small‐angle X‐ray scattering analysis of hollow metallic nanoparticles supported on porous carbon.

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“…Although not used to date in monitoring of LSB systems, in situ SAXS may be utilized in the same types of transmission in situ XRD electrochemical cells to elucidate critical nano‐to‐microstructural information about LSB systems. SAXS can precisely probe the quantitative morphological and structural information on nanoporous systems, for example, pore size, surface area, and pore structure . This information can provide a critical guide when designing the porous carbon‐host sulfur cathode.…”

Section: Technique Reviewmentioning

confidence: 99%

In Situ Techniques for Developing Robust Li–S Batteries

Amirzadeh

Tan

et al. 2018

Small Methods

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Rechargeable lithium–sulfur batteries (LSBs) are of great interest in the field of energy storage due to their favorable operational characteristics, for example, high theoretical energy density and low cost. However, LSBs are limited by long‐term degradation, caused by the dissolution of intermediate lithium polysulfide phases. Further improvement of LSBs requires an in‐depth understanding of the underlying redox reactions and active‐material degradation mechanisms. Advanced characterization techniques, especially in situ/in operando characterization tools, are used and developed in the field of LSBs to probe the rate‐limiting performance and design characteristics of functional materials. Here, common in situ/in operando techniques are reviewed with regard to recent research significance and practical limitations, with the aim of providing a comprehensive treatise on in situ characterization technique selection for LSBs, thereby allowing their future development and improvement.

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Correlating pore size and shape to local disorder in microporous carbon: A combined small angle neutron and X-ray scattering study

Cited by 53 publications

References 47 publications

Pore Development during the Carbonization Process of Lignin Microparticles Investigated by Small Angle X-ray Scattering

Pore Development during the Carbonization Process of Lignin Microparticles Investigated by Small Angle X-ray Scattering

Small-angle scattering by supported nanoparticles: exact results and useful approximations

In Situ Techniques for Developing Robust Li–S Batteries

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