Quantitative atomic-scale structure characterization of ordered mesoporous carbon materials by solid state NMR

Wang, Zhuoran; Opembe, Naftali N.; Kobayashi, Takeshi; Nelson, Nicholas C.; Slowing, Igor I.; Pruski, Marek

doi:10.1016/j.carbon.2018.01.087

Cited by 14 publications

(8 citation statements)

References 41 publications

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“…The chemical structure of CNR-2.6 was further investigated by solid state nuclear magnetic resonance (NMR) with 1 H- 13 C cross polarization (CP) magic angle spinning (MAS) measurement (Figure 3a). The intense peak at around 122 ppm represented aromatic carbons [22] , while the broad asymmetric signal around 22 ppm is assigned to sp 3 carbon moieties. The ratio of sp 2 carbon to sp 3 carbon was estimated to be 95:5.…”

Section: Resultsmentioning

confidence: 99%

High Pressure Induced Formation of Carbon Nanorods from Tetracosane

Liang

Ender

Rohrbeck

et al. 2022

Preprint

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Morphology control of carbon nanostructures is essential for improving their performance in many applications. Direct pyrolysis of organic precursors, however, usually yields bulk amorphous carbon. Therefore, traditional methods for controlling the morphology of carbon nanostructures involve multistep processes and complex precursor molecules. While various methods have been developed under ambient pressure, the impact of pressure on the morphology of the resulting carbon nanostructures remains unexplored. Herein, we present the synthesis of carbon nanorods by direct pyrolysis of the low-cost aliphatic hydrocarbon tetracosane under high pressure conditions. The diameters of the carbon nanorods are adjusted by simply varying the synthetic pressures. High pressure allows controlling both the nanorod morphology as well as the degree of order, and local conductivity of the thus prepared nanorods has been confirmed by conductive AFM measurements. Our method promises a convenient strategy to synthesize carbon nanostructures with controlled morphology and high ordered chemical structure, which opens opportunities for potential electronic and electrochemical applications.

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Section: Resultsmentioning

confidence: 99%

High Pressure Induced Formation of Carbon Nanorods from Tetracosane

Liang

Ender

Rohrbeck

et al. 2022

Preprint

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“…Likewise, the 13 C NMR spectrum was recorded on carbonized material, KPS-1. In this case, we employed the 13 C DPMAS NMR technique, since the low proton content and the influence of paramagnetic interactions in KPS-1 are problematic for recording a 13 C NMR spectrum using the CPMAS technique [50].…”

Section: Resultsmentioning

confidence: 99%

“…Indeed, a combination of several technical challenges, such as the highly electrically conductive nature of carbonized material, the magnetic susceptibility effects observed in graphitic material, the very low isotopic abundance of 13 C, very long carbon recycle delay, and the low sample volume (less than 10 mg in a 2.5 mm rotor) made the acquisition of a good 13 C spectrum quite problematic [50].…”

Section: Resultsmentioning

confidence: 99%

A Porous Carbon with Excellent Gas Storage Properties from Waste Polystyrene

et al. 2019

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In this paper, we describe the synthesis and gas adsorption properties of a porous carbonaceous material, obtained from commercial expanded polystyrene. The first step consists of the Friedel-Craft reaction of the dissolved polystyrene chains with a bridging agent to form a highly-crosslinked polymer, with permanent porosity of 0.7 cm3/g; then, this polymer is treated with potassium hydroxide at a high temperature to produce a carbon material with a porous volume larger than 1.4 cm3/g and a distribution of ultramicro-, micro-, and mesopores. After characterization of the porous carbon and determination of the bulk density, the methane uptake was measured using a volumetric apparatus to pressures up to 30 bar. The equilibrium adsorption isotherm obtained is among the highest ever reported for this kind of material. The interest of this product lies both in its excellent performance and in the virtually costless starting material.

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“…The average pore size was limited to ~4 nm even in the presence of a swelling agent (Entry 13). [25] and [26], respectively.…”

Section: Hydrothermal Carbonization (Htc)mentioning

confidence: 99%

“…A relatively large Pd particle size was obtained on MC400 (Supplementary Materials, Figure S5), while the particles were significantly smaller and well-dispersed in the case of MC-ox samples (Figure 8a-d). Such a phenomenon can be due to the lack of proper adsorption sites on the MC sample prior to oxidation, as oxygen is primarily embedded in the carbon structure in the form of ether (C-O-C) bonds in carbonized RF resin (Figure 2b) [26] inducing a weak interaction with the metal precursor and nanoparticles. In contrast, the oxidation process introduced oxygenfunctional groups and defects in the carbon structure that can serve as proper anchors for metal nanoparticles/clusters to the carbon support.…”

Section: Catalystmentioning

confidence: 99%

Bottom-Up Synthesis Strategies Enabling the Investigation of Metal Catalyst-Carbon Support Interactions

Bateni

Prabhu

Gebur

et al. 2022

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The structural versatility and vibrant surface chemistry of carbon materials offer tremendous opportunities for tailoring the catalytic performance of supported metal nanoparticles through the modulation of interfacial metal-support interactions (MSI). MSI’s geometric and structural effects are well documented for these materials. However, other potential support effects such as electronic metal-carbon interactions remain poorly understood. Such limitations are tied to constraints intrinsic to commonly available carbon materials such as activated carbon (e.g., microporosity) and the top-down approach that is often used for their synthesis. Nonetheless, it is crucial to understand the interplay between the structure, properties, and performance of carbon-supported metal catalysts to take steps toward rationalizing their design. The present study investigates promising and scalable bottom-up synthesis approaches, namely hydrothermal carbonization (HTC) and evaporation-induced self-assembly (EISA), that offer great flexibility for controlling the carbon structure. The opportunities and limitations of the methods are discussed with a particular focus on harnessing the power of oxygen functionalities. A remarkable production yield of 32.8% was achieved for mesoporous carbons synthesized via EISA. Moreover, these carbon materials present similar external surface areas of 316 ± 19 m2/g and average pore sizes of 10.0 ± 0.1 nm while offering flexibility to control the oxygen concentration in the range of 5–26 wt%. This study provides the cornerstone for future investigations of metal-carbon support interactions and the rational design of these catalysts.

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Quantitative atomic-scale structure characterization of ordered mesoporous carbon materials by solid state NMR

Cited by 14 publications

References 41 publications

High Pressure Induced Formation of Carbon Nanorods from Tetracosane

High Pressure Induced Formation of Carbon Nanorods from Tetracosane

A Porous Carbon with Excellent Gas Storage Properties from Waste Polystyrene

Bottom-Up Synthesis Strategies Enabling the Investigation of Metal Catalyst-Carbon Support Interactions

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