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Home  >  Journal list  >  Journal of the Ceramic Society of Japan ( 2003 - 2007 )  >  Vol.113  No.1322 (October) (2005)  >  pp.647-653

Journal of the Ceramic Society of Japan ( 2003 - 2007 )
<<Previous article Vol.113  No.1322 (October) (2005)   pp.647 - 653 Next article>>

Surface Structure of Commercial Si3N4 Powders Analyzed by X-Ray Photoelectron Spectroscopy (XPS)

Tran Thi Thu HIEN1), Chanel ISHIZAKI2) and Kozo ISHIZAKI1)
1) School of Mechanical Engineering, Nagaoka University of Technology (Nagaoka Gijutsu-Kagaku Daigaku)
2) Nano-TEM Co., Ltd.


  Surface structures of seven different commercial Si3N4 powders were investigated by X-ray photoelectron spectroscopy (XPS). The evaluated powders were produced by three different methods: diimide precipitation, carbothermal reduction and nitridation of silicon using different nitriding media with final treatments. The XPS spectra of all as received powders show Si2p, C1s, N1s and O1s signals after 0, 5 and 10 s etching priods. Tetrahedral structures Si-XYZW with different atoms (Si; H; N; O) or groups (NH; NH2; OH) in XYZ and W, from here after substituted by them, were observed for all as received commercial Si3N4 powders. For five out of the seven Si3N4 powders, the two main tetrahedra present on the most outer surface layer are Si-SiSiN(OH), and tetrahedra containing O; Si-O(NNN; SiSiH; SiNN; NNO). The two powders produced by nitridation of silicon with HF acid washing in the final treatment present Si-SiSiN(NH2) and tetrahedra containing OH; Si-SiN(Si; N) (OH). The powder produced by carbothermal reduction process using NH3 (g) presents the highest fraction of O containing tetrahedra. For all powders after 5 and 10 s etching periods, the main structure changed to NH2; Si-SiN(H; Si)(NH2) and NH groups containing configurations Si-SiN(Si; N)(NH), respectively. The surface of Si3N4 powders of any production method does not have structure close to SiO2, Si2N2O or an intermediate between them as commonly accepted.



Keyword:
Silicon nitride, Powder, Surface structure, X-ray photoelectron spectroscopy (XPS), Si tetrahedra

Received: May 17, 2005
Accepted: July 21, 2005 , Published online: October 01, 2005
Copyright (c) 2005 The Ceramic Society of Japan

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