One step convenient synthesis of crystalline β-Si3N4

Well-crystallized β-Si3N4 was directly prepared at an initial reaction temperature of 150 °C through the reaction of SiCl4 and NaN3 in the presence of a small amount of CCl4. Characterization by X-ray diffraction, high-resolution electron microscopy, X-ray photoelectron spectroscopy and energy dispersive X-ray spectroscopy indicates that the product synthesized is crystalline β-Si3N4. The yield of β-Si3N4 is about 86% based on the amount of precursor SiCl4 used at the initial reaction temperature of 150 °C, and is more than 90% at the reaction temperature of 200 °C with the product β-Si3N4 in high crystallinity. The dominant morphology of the product is short rods with the growth axis along the [001] direction. The formation mechanism of crystalline β-Si3N4 was discussed briefly, and the role of CCl4 in the formation process of β-Si3N4 was analyzed.

[1]  P. Yin,et al.  Synthesis of nitrogen-doped carbon nanostructures by the reactions of small molecule carbon halides with sodium azide. , 2005, The journal of physical chemistry. B.

[2]  E. Kroke,et al.  Novel group 14 nitrides , 2004 .

[3]  M. A. Rodríguez,et al.  Synthesis of β-Silicon nitride by SHS: fiber growth ☆ , 2004 .

[4]  Junqing Hu,et al.  Uniform Micro‐Sized α‐ and β‐Si3N4 Thin Ribbons Grown by a High‐Temperature Thermal‐Decomposition/Nitridation Route , 2004 .

[5]  Y. Bando,et al.  Synthesis, structure, and photoluminescence of very thin and wide alpha silicon nitride (α-Si3N4) single-crystalline nanobelts , 2003 .

[6]  J. Dai,et al.  Effects of rare‐earth oxide additions and heat‐treatment temperature on the transformation and microstructure of silicon nitride , 2003 .

[7]  Yi Xie,et al.  Growth of pure β-Si3N4 nanorods from the synergic nitrogen sources , 2003 .

[8]  Z. Wang.  Nanobelts, Nanowires, and Nanodiskettes of Semiconducting Oxides—From Materials to Nanodevices , 2003 .

[9]  I. Parkin.  Solvent free reactions in the solid state: solid state metathesis , 2002 .

[10]  Zhang Baolin,et al.  Synthesis of β-Si3N4 whiskers by SHS , 2002 .

[11]  Huanchu Chen,et al.  Formation of α-Si3N4 whiskers with addition of NaN3 as catalyst , 2002 .

[12]  R. Brink,et al.  Synthesis of α-silicon nitride powder by gas-phase ammonolysis of CH3SiCl3 , 2001 .

[13]  Junichi Tatami,et al.  Effect of HfO2 Addition on Sintering of Si3N4 , 2001 .

[14]  Junqing Hu,et al.  A Novel Low‐Temperature Synthetic Route to Crystalline Si3N4 , 1999 .

[15]  M. Mackenzie,et al.  Solid state metathesis routes to transition metal carbides , 1999 .

[16]  Q. Pankhurst,et al.  Self propagating high temperature synthesis of BaFe12–xCrxO19 and Li0.5Fe2.5–xCrxO4 , 1999 .

[17]  I. Parkin,et al.  Solid state metathesis routes to Group IIIa nitrides : comparison of Li3N, NaN3, Ca3N2 and Mg3N2 as nitriding agents , 1998 .

[18]  W. Lee,et al.  Combustion synthesis of Si_3N_4 powder , 1997 .

[19]  I. Parkin.  Solid state metathesis reaction for metal borides, silicides, pnictides and chalcogenides: ionic or elemental pathways , 1997 .

[20]  S. Schwab,et al.  Nanostructure of polymer-derived silicon nitride , 1995 .

[21]  M. A. Rodríguez,et al.  Single crystal ß‐Si3N4 fibers obtained by self‐propagating high temperature synthesis** , 1995 .

[22]  I. Parkin,et al.  Sodium azide as a reagent for solid state metathesis preparations of refractory metal nitrides , 1995 .

[23]  M. Edirisinghe,et al.  Synthesis of α-silicon nitride powder from a polymeric precursor , 1995 .

[24]  W. R. Schmidt,et al.  Ammonia-induced pyrolytic conversion of a vinylic polysilane to silicon nitride , 1992 .

[25]  B. Forslund,et al.  Carbothermal Preparation of Silicon Nitride: Influence of Starting Material and Synthesis Parameters , 1992 .

[26]  R. Kaner,et al.  Rapid Solid-State Precursor Synthesis of Materials , 1992, Science.

[27]  A. Varma,et al.  Quantitative phase analysis of Si3N4 by X-ray diffraction , 1992 .

[28]  R. Kaner,et al.  Rapid solid-state synthesis of materials from molybdenum disulphide to refractories , 1991, Nature.

[29]  J. Heinrich,et al.  Relationships between processing, microstructure and properties of dense and reaction-bonded silicon nitride , 1987 .

[30]  Hughes,et al.  C 1s excitation studies of diamond (111). I. Surface core levels. , 1986, Physical review. B, Condensed matter.

[31]  R. Govila.  Strength characterization of yttria-doped sintered silicon nitride , 1985 .

[32]  K. Komeya,et al.  Synthesis of the α form of silicon nitride from silica , 1975 .