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<p>This study presents a catalyst-free methodology for synthesizing silicon nitride (Si<sub>3</sub>N<sub>4</sub>) powders through the direct nitridation of Si. The influence of key parameters, including Si particle sizes (1&#xa0;μm, 5&#xa0;μm, 20&#xa0;μm, and 100&#xa0;μm), nitridation temperatures (1390−1450&#xa0;℃), holding times (0−6&#xa0;h), and gas composition (N<sub>2</sub> with or without H<sub>2</sub>), on the degree of nitridation and α-phase fraction of Si<sub>3</sub>N<sub>4</sub> was investigated. The experimental phase contents and microstructural properties were evaluated using X-ray diffraction and scanning electron microscopy. The α-phase fraction of Si<sub>3</sub>N<sub>4</sub> was quantitively assessed via Rietveld refinement of the XRD data, ensuring precise phase composition analysis. The results demonstrated that the optimal conditions for achieving phase-pure Si<sub>3</sub>N<sub>4</sub> with a predominant α-phase of 95.1% were a Si particle size of 5&#xa0;μm, a temperature of 1450&#xa0;℃, no additional holding time, and a gas composition of 96% N<sub>2</sub> and 4% H<sub>2</sub>. These findings highlight the critical role of particle size and process parameters in tailoring the phase composition of Si<sub>3</sub>N<sub>4</sub> powders. The promising results from this study could pave the way for large-scale production of high-purity Si<sub>3</sub>N<sub>4</sub> powders with a high α-phase content.</p>

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Catalyst-free synthesis of Si3N4 powders via direct nitridation of Si: influence of particle size and nitridation parameters on the α-phase fraction

  • 期刊论文

  • 发表日期：

    2025年3月24日

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  • Kati Raju,
  • Seunghwan Moon,
  • Minwook Kim,
  • Jaehun Cho,
  • Hyun-Kwuon Lee

摘要

This study presents a catalyst-free methodology for synthesizing silicon nitride (Si3N4) powders through the direct nitridation of Si. The influence of key parameters, including Si particle sizes (1 μm, 5 μm, 20 μm, and 100 μm), nitridation temperatures (1390−1450 ℃), holding times (0−6 h), and gas composition (N2 with or without H2), on the degree of nitridation and α-phase fraction of Si3N4 was investigated. The experimental phase contents and microstructural properties were evaluated using X-ray diffraction and scanning electron microscopy. The α-phase fraction of Si3N4 was quantitively assessed via Rietveld refinement of the XRD data, ensuring precise phase composition analysis. The results demonstrated that the optimal conditions for achieving phase-pure Si3N4 with a predominant α-phase of 95.1% were a Si particle size of 5 μm, a temperature of 1450 ℃, no additional holding time, and a gas composition of 96% N2 and 4% H2. These findings highlight the critical role of particle size and process parameters in tailoring the phase composition of Si3N4 powders. The promising results from this study could pave the way for large-scale production of high-purity Si3N4 powders with a high α-phase content.