Ten-gram-scale preparation of PTMS-based monodisperse ORMOSIL nano- and microparticles and conversion to silica particles

Kim, Jung Soo; Jung, Gyu Il; Kim, Soo Jung; Koo, Sang Man

doi:10.1007/s11051-018-4186-6

Cited by 3 publications

(4 citation statements)

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“…The effect of sulfur on the morphology of hollow SiC composite particles obtained after magnesiothermic reduction will be discussed later in detail. Monodisperse, spherical ORMOSIL particles with sizes from 70 nm to 4 μm were prepared at the 10‐g scale 37,38 . Subsequently, these ORMOSIL particles were converted to monodisperse spherical SiC composite particles via magnesiothermic reduction as shown in Figure 1.…”

Section: Resultsmentioning

confidence: 99%

“…Monodisperse, spherical ORMOSIL particles with sizes from 70 nm to 4 μm were prepared at the 10-g scale. 37,38 Subsequently, these ORMOSIL particles were converted to monodisperse spherical SiC composite particles via magnesiothermic reduction as shown in Figure 1. No additional mixing of Si sources and carbonaceous precursors was necessary because ORMOSIL particles already contain well-dispersed pre-set amounts of Si and carbon.…”

Section: Resultsmentioning

confidence: 99%

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Self‐templated magnesiothermic reduction of ORMOSIL particles to monodisperse hollow spherical SiC composite particles

Jung,

Lim,

Lee

et al. 2024

J Am Ceram Soc.

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Hollow silicon carbide (SiC) particles have attracted attention due to their well‐defined morphology, low density, and large surface area that can be leveraged for a wide variety of applications. Here, we report the self‐templated synthesis of monodisperse hollow spherical SiC composite particles with controllable shell thicknesses using magnesiothermic reduction of organically modified silica (ORMOSIL) particles. Monodisperse ORMOSIL particles containing three organic groups of methyl, vinyl, and mercaptopropyl were produced by a simple one‐pot sol–gel process and then converted to hollow spherical SiC composite particles via a magnesiothermic reduction at 700°C under an inert atmosphere. The spherical morphologies of the original ORMOSIL particles were well maintained through this self‐templated conversion process, but the sizes of the hollow SiC particles were slightly reduced by the thermal treatment. Field emission transmission electron microscopy studies revealed that the shell of hollow particles mainly consists of primary β‐SiC particles with nanometer‐scale sizes. The physical and chemical properties of the hollow SiC composite particles were investigated by scanning electron microscopy, transmission electron microscopy, X‐ray photoelectron spectroscopy, Brunauer–Emmett–Teller, X‐ray diffraction, Fourier transform infrared spectroscopy, Raman, and solid‐state nuclear magnetic resonance analyses. The shell thickness of hollow spherical SiC composite particles can be controlled by simply changing the duration of the thermal conversion process. This study not only provides a simple and easy approach for the preparation of hollow spherical SiC particles but also opens the possibility of large‐scale manufacturing of such particles for commercial applications.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Self‐templated magnesiothermic reduction of ORMOSIL particles to monodisperse hollow spherical SiC composite particles

Jung,

Lim,

Lee

et al. 2024

J Am Ceram Soc.

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“…The natural graphite was purchased from Xiamen TOB New Energy Technology (China), while the Si@TiO 2 nanoparticles were synthesized in-house using a peptization technique. 49 The synthesis process comprised mixing silicon nanoparticles with titanium (IV) isopropoxide (precursor) in distilled water, followed by stirring, heating, and centrifugal separation. The separated Si@TiO 2 nanoparticles were then vacuum-dried at 70 °C overnight.…”

Section: Methodsmentioning

confidence: 99%

Graphite-Si@TiO₂ Core-Shell Nanoparticles as Composite Anode for Li-ion Batteries: Electrochemical Response

Vats,

Gupta,

Gupta

et al. 2024

J. Electrochem. Soc.

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This study focuses on optimizing composite anodes through varying Si@TiO2 core-shell nanoparticle percentages in graphite. Material characterization reveals the morphological transformation of graphite and silicon nanoparticles into composite anodes. Electrochemical tests, including cyclic voltammetry, galvanostatic charge-discharge, and electrochemical impedance spectroscopy (EIS), provide essential insights into the electrochemical behavior of these composites. In the cycling tests, Graphite with 5% core-shell (GrCS5), Graphite with 10% core-shell (GrCS10), and Graphite with 15% core-shell (GrCS15) show initial discharge capacities of 568, 675, and 716 mAh/g, retaining 76%, 75%, and 72% after 100 cycles, respectively. Conversely, the Gr/Si composite, commencing with 728 mAh/g, exhibits rapid degradation, retaining 54% after 100 cycles. Moreover, the EIS analysis reveals higher values of ohmic, solid electrolyte interphase, and charge transfer resistances in Graphite with 10% silicon (GrSi10) compared to other composite anodes after 100 cycles. The examination of the lithium diffusion coefficient indicates that GrCS5 demonstrates superior lithium diffusion kinetics, displaying the highest coefficient among all composite anodes. The research objective is to identify the optimal composite anode composition through quadrant analysis, considering specific capacity and lithium diffusivity after 100 cycles. In conclusion, integrating Si@TiO2 core-shell nanoparticles in graphite anodes improves their performance, with GrCS10 demonstrating notable effectiveness

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“…Titanium tetra-isopropoxide (TTIP) was purchased from Sigma Aldrich Chemicals Pvt Ltd (India). The preparation process of core-shell nanoparticles was referred from Kim et al [21]. Initially, 1 g of silicon nanoparticles were added to the 50 ml distilled water.…”

Section: Methodsmentioning

confidence: 99%

Investigation of Peptization Technique to Synthesize Si@TiO<sub>2</sub> for a Li-Ion Battery Anode Material

Vats,

Gupta,

Gupta

et al. 2023

MSF

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Electric vehicles (EVs) have a significant advantage in terms of energy efficiency and environmental friendliness. In lithium-ion batteries, silicon is seeking more attention than graphite-based anodes due to its high storage capacity. However, it faces severe structural degradation due to volume expansion which is responsible for fast capacity degradation. In the present study, the core shell is developed with the core as silicon and titania as shell (Si@TiO2) and utilized it as an anode in the 2016-coin cell. The material characterization (FE-SEM, TEM, EDS, XRD and XPS) of this developed core-shell material is recorded to confirm its elemental composition and structural validation. The electrochemical performance is measured using cyclic voltammetry (CV) and galvanostatic charge/discharge (GCD) test. Cyclic voltammetry profiles reveal the stable lithiation and delithiation process. Initial specific capacity of ≈3180 mAh/g is reported, capacity retention of 61% for the developed core-shell while 34% for the bare silicon is noted over 100 cycles. The proposed method (peptization technique) for the development of core-shell nanoparticles is also compared with the sol-gel approach. The result shows an increment of 5% in capacity retention after 100 cycles by following the peptization technique.

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Ten-gram-scale preparation of PTMS-based monodisperse ORMOSIL nano- and microparticles and conversion to silica particles

Cited by 3 publications

References 24 publications

Self‐templated magnesiothermic reduction of ORMOSIL particles to monodisperse hollow spherical SiC composite particles

Self‐templated magnesiothermic reduction of ORMOSIL particles to monodisperse hollow spherical SiC composite particles

Graphite-Si@TiO₂ Core-Shell Nanoparticles as Composite Anode for Li-ion Batteries: Electrochemical Response

Investigation of Peptization Technique to Synthesize Si@TiO<sub>2</sub> for a Li-Ion Battery Anode Material

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Ten-gram-scale preparation of PTMS-based monodisperse ORMOSIL nano- and microparticles and conversion to silica particles

Cited by 3 publications

References 24 publications

Self‐templated magnesiothermic reduction of ORMOSIL particles to monodisperse hollow spherical SiC composite particles

Self‐templated magnesiothermic reduction of ORMOSIL particles to monodisperse hollow spherical SiC composite particles

Graphite-Si@TiO2 Core-Shell Nanoparticles as Composite Anode for Li-ion Batteries: Electrochemical Response

Investigation of Peptization Technique to Synthesize Si@TiO<sub>2</sub> for a Li-Ion Battery Anode Material

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Product

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Graphite-Si@TiO₂ Core-Shell Nanoparticles as Composite Anode for Li-ion Batteries: Electrochemical Response