Research advances in preparation technology and quality of silicon nitride powder

doi:10.11949/0438-1157.20210866

Abstract

Abstract:

Silicon nitride (Si₃N₄) has excellent physical and chemical properties and occupies an important position in key fields such as national defense and electronic information. High quality Si₃N₄ powders are the primary prerequisite for the preparation of high performance Si₃N₄ ceramics. The high-quality powder requisites the conditions of fine particle size with narrow distribution, high α phase, low impurity and so on. The research advances in preparation technology of silicon nitride powder are summarized from the point of the synthesis reaction system, with the emphasis on summarizing the progress of the improvement of powder quality by enhancing heat and mass transfer. In addition, the present situations of industrial manufacture are introduced, and the development trend and direction of the preparation technology of high quality Si₃N₄ powder are also prospected.

Key words: silicon nitride, powder technology, carbo-thermal nitriding method, silicon directly nitriding method, chemical vapor deposition method, silamine precursor conversion method, synthesis mechanism

摘要：

氮化硅(Si₃N₄)具有优异的物化性能，在国防、电子信息等关键领域都占据重要的地位。高质量粉体是制备高性能Si₃N₄陶瓷的首要前提。通常高质量Si₃N₄粉体需要满足粒径细、分布窄、α相含量高、杂质含量低等条件。基于合成反应体系综述了当前国内外制备Si₃N₄粉体的方法，着重从强化传热与传质角度介绍了改善粉体质量的研究进展，并介绍了当前工业生产现状，展望了高质量Si₃N₄粉体制备技术的发展趋势和方向。

关键词: 氮化硅, 粉体技术, 碳热氮化法, 硅粉直接氮化法, 化学气相沉积法, 硅胺前体转化法, 合成机理

CLC Number:

TQ 174

Maoqiao XIANG, Yuqi GENG, Qingshan ZHU. Research advances in preparation technology and quality of silicon nitride powder[J]. CIESC Journal, 2022, 73(1): 73-84.

向茂乔, 耿玉琦, 朱庆山. 氮化硅粉体制备技术及粉体质量研究进展[J]. 化工学报, 2022, 73(1): 73-84.

Figures/Tables 9

Fig.1 Predominance area diagram of the SiO2-C-N2 system under different temperature and partial pressure (calculated by HSC 6.0 thermodynamic analysis software)

Fig.2 Product of the SiO2-C-N2 system

Table 1 The quality of Si3N4 powders synthesized by carbothermal nitriding of SiO2 in the domestic and overseas

企业	α相/%(质量)	C/%(质量)	O/%(质量)	Fe/%(质量)	Al/%(质量)	Mg/%(质量)	Ca/%(质量)
日本东芝	约96	0.09~0.8	0.9~3.5	约0.0044	约0.0006	约0.0002	0.0018~0.0052
日本住友	约99	0.6~1.3	1.0~4.1	约0.003	约0.0022	约0.0009	约0.002
臻璟新材	约95.3	约0.9	约1.5	<0.01	<0.01	<0.01	<0.01
凯新特材	约90	0.2~3.8	约1.3	<0.01	<0.01	<0.01	<0.01

Fig.3 Schematic diagram of the process of nitridation reaction[24]

Table 2 Misfit strain between Si and α-Si3N4 with different orientation［35］

取向关系	失配应变/%
α-Si₃N₄ Si	失配应变/%
(2 $1 ˉ$ $1 ˉ$ 0) // (1 1 0)	1.8
(0 3 $3 ˉ$ 0) // (1 1 2)	1.8
(2 $1 ˉ$ $1 ˉ$ 1) // (1 1 1)	2.2
(3 $1 ˉ$ $2 ˉ$ 1) // (2 1 0)	-4.1
(0 0 0 2) // (1 1 1)	10.8

Table 2 Misfit strain between Si and α-Si3N4 with different orientation［35］

取向关系	失配应变/%
α-Si₃N₄ Si	失配应变/%
(2 $1 ˉ$ $1 ˉ$ 0) // (1 1 0)	1.8
(0 3 $3 ˉ$ 0) // (1 1 2)	1.8
(2 $1 ˉ$ $1 ˉ$ 1) // (1 1 1)	2.2
(3 $1 ˉ$ $2 ˉ$ 1) // (2 1 0)	-4.1
(0 0 0 2) // (1 1 1)	10.8

Fig.4 TEM image of product by the direct nitridation of Si powder

Fig.5 Schematic diagram and micrograph of Si3N4 production through self -propagating combustion method

Table 3 The quality of Si3N4 powders synthesized by self-propagating combustion technology in the domestic and overseas

企业	α相/%(质量)	Si/%(质量)	O/%(质量)	Fe/%(质量)	Al/%(质量)	Ca/%(质量)
H?gan?s(H.C.Starck)	90	≤0.9	1.3	0.0005	0.001	0.0005
ALZChem	93	≤0.2	≤1.0	0.0015	0.0001	0.0008
烟台同立高科	90	≤0.1	≤1.6	0.0002	0.0004	0.0003
埃克诺新材料	92	0.1	1.3	0.0005	0.0005	0.0005
河北高富	80	0.1	1.0	0.01	0.01	0.01
淄博恒世科技	90	0.1	≤0.6	0.0003	0.0003	0.0003
青岛瓷兴	>90	0.2	≤1.5	≤0.0005	≤0.0005	≤0.0005
中材高新	93	0.2	≤1.5	≤0.00002	<0.01	<0.01
德盛特种陶瓷	90	0.025	1.2	0.002	—	0.001
北京中联阳光	90	0.15	≤1.0	0.001	0.0005	0.0005
泰晟新材料	92	1.2	1.5	<0.01	0.003	0.001
安赛美精细陶瓷	93.5	0.5	1.5	0.06	0.01	0.008

Fig.6 Flow chart and microscopic image for preparing high quality Si3N4 powder by UBE industry

References 95

1	Iijima M, Hasegawa K, Tatami J. Nonaqueous gel casting using multicomponent concentrated slurries through Michael additive reaction for fabricating silicon nitride dense ceramics[J]. Advanced Powder Technology, 2021, 32(2): 472-479.
2	Frank L, Riley F L. Silicon nitride and related materials[J]. Journal of the American Ceramic Society, 2000, 83(2): 245-265.
3	Chen F, Shen Q, Zhang L M. Electromagnetic optimal design and preparation of broadband ceramic radome material with graded porous structure[J]. Progress In Electromagnetics Research, 2010, 105: 445-461.
4	Zhang X Y, Huo W L, Qi F, et al. Ultralight silicon nitride ceramic foams from foams stabilized by partially hydrophobic particles[J]. Journal of the American Ceramic Society, 2016, 99(9): 2920-2926.
5	李贵佳, 孙峰. 利用国外专利技术, 解决国内氮化硅陶瓷轴承球产业化问题[J]. 中国陶瓷, 2015, 51(10): 43-47.
	Li G J, Sun F. To solve the domestic industrialization problem of silicon nitride ceramic bearing ball by means of foreign patent technology[J]. China Ceramics, 2015, 51(10): 43-47.
6	吴承伟, 张伟, 李东炬. 超精密高性能氮化硅轴承研究现状与应用[J]. 精密制造与自动化, 2020, 221(1): 1-3.
	Wu C W, Zhang W, Li D J. Current situation and application of research on super-precision high-performance silicon nitride bearings[J]. Precise Manufacturing & Automation, 2020, 11(1): 1-3.
7	Hu F, Xie Z P, Zhang J, et al. Promising high-thermal-conductivity substrate material for high-power electronic device: silicon nitride ceramics[J]. Rare Metals, 2020, 39(5): 463-478.
8	郑彧, 童亚琦, 张伟儒. 高导热氮化硅陶瓷基板材料研究现状[J]. 真空电子技术, 2018, 335(4): 13-17.
	Zheng Y, Tong Y Q, Zhang W R. Research on high thermal conductivity silicon nitride ceramic substrate materials[J]. Vacuum Electronics, 2018, 335(4): 13-17.
9	李少鹏. 新一代IGBT模块用高可靠氮化硅陶瓷覆铜基板研究进展[J]. 电子工业专用设备, 2019, 48(1): 1-7.
	Li S P. Research and development of bonding copper to Si₃N₄ ceramic substrates used in IGBT module[J]. Equipment for Electronic Products Manufacturing, 2019, 48(1): 1-7.
10	吴庆文, 胡丰, 谢志鹏. 高性能氮化硅陶瓷的制备与应用新进展[J]. 陶瓷学报, 2018, 39(1): 13-19.
	Wu Q W, Hu F, Xie Z P. New progress in the preparation and application of high performance silicon nitride ceramics[J]. Journal of Ceramics, 2018, 39(1): 13-19.
11	Takeshi Y, Michio H, Shinsuke J. Silicon nitride powder, silicon nitride sintered body and cricut substrate, and production method for said silicon nitride powder: US10399854B2[P]. 2019-09-03.
12	Shibata K, Ohmaru T, Yamao T, et al. Silicon nitride powder production method, silicon nitride powder, silicon nitride sintered body and circuit substrate using same: US9085462B2[P], 2015-07-21.
13	万小涵, 张广清, Ostroviski Oleg. 碳热还原/氮化合成氮化硅工艺中碳化硅生成的分析[J]. 云南冶金, 2015, 44(3): 47-49, 73.
	Wan X H, Zhang G Q, Ostroviski O. Analysis on silicon carbide formation in the process of carbothermal reduction/nitration synthesis of silicon nitride[J]. Yunnan Metallurgy, 2015, 44(3): 47-49, 73.
14	Ortega A, Alcalá M D, Real C, Carbothermal synthesis of silicon nitride (Si3N₄): Kinetics and diffusion mechanism[J]. Journal of Materials Processing Technology, 2008, 195: 224-231.
15	Vlasova M V, Bartnitskaya T S, Sukhikh L L, et al. Mechanism of Si₃N₄ nucleation during carbothermal reduction of silica[J]. Journal of Materials Science, 1995, 30: 5263-5271.
16	Ma B, Huang Z H, Mei L F, et al. Preparation of Si₃N₄ form diatomite via a carbothermal reduction-nitridation process[J]. The Minerals, Metals & Materials Society, 2016, 68(5): 1456-1464.
17	Weimer A W, Eisman G A, Susnitzky D W, et al. Mechanism and kinetics of the carbothermal nitridation synthesis of α-silicon nitride[J]. Journal of the American Ceramic Society, 1997, 80(11): 2853-2863.
18	Chen K, Huang Z H, Liu Y, et al. Synthesis of β-Si₃N₄ powder from quartz via carbothermal reduction nitridation[J]. Powder Technology, 2013, 235: 728-734.
19	Ishii T, Imai I, Sano A, et al. Method for making silicon nitride powder: US4986972[P]. 1991-01-22.
20	Inoue H, Komeya K, Tsuge A, et al. Process for preparing silicon nitride powder: US4514370[P]. 1985-04-30.
21	Chung S L, Chang C W. Carbothermal reduction and nitridation synthesis of silicon nitride by using solution combustion synthesized precursors[J]. Journal of Materials Science, 2009, 44(14): 3784-3792.
22	Ghosh Chaudhuri M, Ahmadullah S, Dey R, et al. Novel technique for synthesis of silicon nitride nanowires[J]. Advances in Applied Ceramics, 2011, 110(4): 211-214.
23	Schonfelder L, Franz G. Process for the preparation of silicon nitride low in carbon content: US4798714[P]. 1989-01-17.
24	Jennings H M, On reactions between silicon and nitrogen[J]. Journal of Materials Science, 1983, 18(4): 951-967.
25	Atkinson A, Leatt P J, Moulson A J, et al. A mechanism for the nitridation of silicon powder compacts[J]. Journal of Materials Science, 1974, 9(6): 981-984.
26	Atkinson A, Moulson A J, Roberts E W, et al. Nitridation of high-purity silicon[J]. Journal of the American Ceramic Society, 1976, 59(7/8): 285-289.
27	Barsoum M, Kangutkar P, Koczak M J. Nitridation kinetics and thermodynamics of silicon powder compacts [J]. Journal of the American Ceramic Society, 1991, 74(6): 1248-1253.
28	Sheldon B W, Haggerty J S. The formation of reaction bonded Si₃N₄ at low temperatures and in short times[C]//A Collection of Papers Presented at the 13th Annual Conference on Composites and Advanced Ceramic Materials: Ceramic Engineering and Science Proceedings. Hoboken, NJ, USA: John Wiley & Sons, Inc., 1989, 10: 784-793.
29	Sheldon B W, Haggerty J S. The nitridation of high purity, laser-synthesized silicon powder to form reaction bonded silicon nitride[C]//Proceedings of the 12th Annual Conference on Composites and Advanced Ceramic Materials: Ceramic Engineering and Science Proceedings. Hoboken, NJ, USA: John Wiley & Sons, Inc.,1988: 1061-1071.
30	Moulson A J. Reaction-bonded silicon nitride: its formation and properties[J]. Journal of Materials Science, 1979, 14(5): 1017-1051.
31	Inomata Y, Uemura Y. Nitridation kinetics of silicon powder[J]. Journal of the Ceramic Association, Japan, 1975, 83(957): 244-248.
32	Jennings H M, Dalgleish B J, Pratt P L. Reactions between silicon and nitrogen [J]. Journal of Materials Science, 1988, 23(7): 2573-2583.
33	Maalmi M, Varma A. Intrinsic nitridation kinetics of high-purity silicon powder[J]. AIChE Journal, 1996, 42(12): 3477-3483.
34	Chang F W, Liou T H, Tsai F M. The nitridation kinetics of silicon powder compacts[J]. Thermochimica Acta, 2000, 354(1/2): 71-80.
35	Koike J, Kimura S. Mechanism of nitridation of silicon powder in a fluidized-bed reactor[J]. Journal of the American Ceramic Society, 1996, 79(2): 365-370.
36	Li W B, Lei B Q, Lindbäck T, et al. Stresses developed in reaction-bonded ceramics[J]. Journal of the European Ceramic Society, 1999, 19(3): 277-283
37	Wang H B, Han J C, Du S Y. Effect of nitrogen pressure and oxygen-containing impurities on self-propagating high temperature synthesis of Si₃N₄[J]. Journal of the European Ceramic Society, 2001, 21(3): 297-302.
38	杨福明, 王立, 尹少武, 等. 硅粉常压直接氮化过程的非催化气固反应模型[J]. 北京科技大学学报, 2013, 35(6): 785-792.
	Yang F M, Wang L, Yin S W, et al. Noncatalytic gas-solid reaction model for directly nitridizing silicon powder under atmospheric pressure[J]. Journal of University of Science and Technology Beijing, 2013, 35(6): 785-792.
39	Duan S C, Ma J J, Guo H J, et al. Thermodynamic analysis and kinetics mechanism for direct nitridation reaction[J]. Nonferrous Metals Science and Engineering, 2016, 7(4): 14-21.
40	杨春. 流化床直接氮化硅粉技术的研究现状及发展方向[J]. 能源工程, 2015, 2: 21-26.
	Yang C. Development and research status of preparation of silicon nitride powder by direction nitridation of silicon in fluidized bed[J]. Energy Engineering, 2015, 2: 21-26.
41	Li J T, Tian S Y, Chen K X. Investigation of the on-line industrial production of Si₃N₄ by combustion synthesis[J]. Journal of Ceramic Society of Japan, 2004, 112(5): S1-S5.
42	Ge Y, Wang Q, Cui W, et al. Crystal growth in the combustion synthesis of α-Si₃N₄ using Si with different particle sizes[J]. Journal of the American Ceramic Society, 2015, 98(10): 3398-3403.
43	Ge Y, Cui W, Wang Q, et al. Microstructure and thermo-kinetics analysis in combustion synthesis of Si₃N₄ with high α-phase content[J]. Journal of the American Ceramic Society, 2015, 98(1): 263-268.
44	Li J T, Mei L, Yang Y, et al. Combustion synthesis of Si₃N₄ by selective reaction of silicon with nitrogen in air[J]. Journal of the American Ceramic Society, 2009, 92(3): 636-640.
45	Kim M, Park J, Lee H W, et al. A cyclic process for the nitridation of Si powder[J]. Materials Science and Engineering A, 2005, 408(1/2): 85-91.
46	张宝林, 庄汉锐, 符锡仁. 硅粉在高压氮气中自蔓延燃烧合成氮化硅的反应机理[J]. 无机材料学报, 1993, 4(8): 433-440.
	Zhang B L, Zhuan H R, Fu X R. A Mechanism for self-propagating combustion synthesis of Si₃N₄ under pressurized nitrogen[J]. Journal of Inorganic Materials, 1993, 4(8): 433-440.
47	Hirao K, Miyamoto Y, Koizumi M. Synthesis of silicon nitride by a combustion reaction under high nitrogen pressure[J]. Journal of the American Ceramic Society, 1986, 69(4): C-60.
48	Hirao K, Miyamoto Y, Koizumi M. Combustion reaction characteristics in the nitridation of silicon[J]. Advanced Ceramic Materials, 1987, 2(4): 780-783.
49	Singh S, Godkhindi M M, Krishnarao R V, et al. Effect of mechanical activation on synthesis of ultrafine Si₃N₄-MoSi₂in situ composites[J]. Materials Science and Engineering: A, 2004, 382(1/2): 321-327.
50	Jin H B, Yang Y, Chen Y X, et al. Mechanochemical-activation-assisted combustion synthesis of α-Si₃N₄[J]. Journal of the American Ceramic Society, 2006, 89(3): 1099-1102.
51	Jin H B, Cao M S, Chen Y X, et al. The influence of mechanochemical activation on combustion synthesis of Si₃N₄[J]. Ceramics International, 2008, 34(5): 1267-1271.
52	曹永革, 葛昌纯, 周张健. 初始硅粉粒度对自蔓延高温合成氮化硅的影响[J]. 硅酸盐学报, 1998, 26(5): 4-10.
	Cao Y G, Ge C C, Zhou Z J. Effect of Si particle size on SHS Si₃N₄[J]. Journal of the Chinese Ceramic Society, 1998, 26(5): 4-10.
53	任克刚, 陈克新, 金海波. 活化燃烧合成氮化硅陶瓷粉体[J]. 稀有金属材料与工程, 2005, 34(z1): 208-210.
	Ren K G, Chen K X, Jin H B. Combustion synthesis Si₃N₄ powders by using activation process[J]. Rare Metal Materials and Engineering, 2005, 34(z1): 208-210.
54	尹少武, 王立, 刘传平, 等. 硅粉常压直接氮化制备氮化硅粉的研究[J].硅酸盐通报, 2008, 27(2): 230-235.
	Yin S W, Wang L, Liu C P, et al. The study on the preparation of silicon nitride powders by direct nitridation at normal pressure[J]. Bulletin of the Chinese Ceramics Society, 2008, 27(2): 230-235.
55	Yeh C L, Liu E W. Effects of Si₃N₄ addition on formation of aluminum nitride by self-propagating combustion synthesis[J]. Journal of Alloys and Compounds, 2007, 433: 147-153.
56	Yang Y, Chen Y X, Lin Z M, et al. Synthesis of alpha-Si₃N₄ using low-α-phase Si₃N₄ diluent by the seeding technique[J]. Scripta Materialia, 2007, 56(5): 401-404.
57	Cano I G, Borovinskaya I P, Rodriguez M A, et al. Effect of dilution and porosity on self-propagating high-temperature synthesis of silicon nitride[J]. Journal of the American Ceramic Society, 2002, 85(9): 2209-2211.
58	Cano I G, Pérez Baelo S, Rodrı́guez M A, et al. Self-propagating high temperature-synthesis of Si₃N₄: role of ammonium salt addition[J]. Journal of the European Ceramic Society, 2001, 21(3): 291-295.
59	Ge C C, Wang F, Shen W P. New progress on SHS of silicon nitride with high α-phase content[J]. Materials Science Forum, 2005, 475: 1599-1604.
60	Komeya K, Inoue Y H, Ohta T, et al. Method of making alpha type silicon nitride powder: US4117095[P]. 1978-09-26.
61	Jiang J X. A new synthesis method of α-silicon nitride powder-reductive combustion synthesis from silicon and silicon dioxide[J]. Journal of the American Ceramic Society, 2009, 92 (12): 3095-3097.
62	Fukuoka H, Shimizu M, Ochiai H, et al. Preparation of silicon nitride powder by partially nitriding in a fluidized bed and then completing nitridation in a moving bed: US5232677[P]. 1993-08-03.
63	Fukuoka H, Watanabe M, Konya Y, et al. Preparation of high alpha-type silicon nitride powder: US5456896[P]. 1995-08-10.
64	Fukuoka H, Konya Y, Fukuhira M. Continuous preparation of silicon nitride powder: US5817285[P]. 1998-10-06.
65	Liu Y D, Kimura S. Fluidized-bed nitridation of fine silicon powder[J]. Powder Technology, 1999, 106(3): 160-167.
66	Yang F M, Wang L, Yin S W, et al. Experimental study on the entrainment characteristics of ultrafine powder in a fluidized bed with vibrator and agitator[J]. Industrial & Engineering Chemistry Research, 2013, 52(3): 1359-1364.
67	尹少武, 王立, 童莉葛, 等. 基于流态化技术硅粉直接氮化制备氮化硅粉[J]. 北京化工大学学报(自然科学版), 2008, 35(1): 70-74.
	Yi S W, Wang L, Tong L G, et al. Preparation of silicon nitride powder by a direct nitridation process based on fluidization technology[J]. Journal of Beijing University of Chemical Technology (Natural Science Edition), 2008, 35(1): 70-74.
68	尹少武, 王立, 孙淑凤, 等. 悬浮床氮化硅合成热过程的实验研究与数值模拟[J]. 北京科技大学学报, 2008, 30(10): 1169-1173.
	Yin S W, Wang L, Sun S F, et al. Experiment research and numerical simulation of thermal process in a suspended bed for Si₃N₄ synthesis[J]. Journal of University Science and Technology Beijing, 2008, 30(10): 1169-1173.
69	陈俊, 叶旭初, 宋涛, 等. 流态化合成氮化硅的鼓泡床冷模试验与CFD模拟[J]. 南京工业大学学报(自然科学版), 2005, 27(1):57-61.
	Chen J, Ye X C, Song T, et al. The fluid-dynamic study and CFD simulation of bubbling fluidized bed for Si₃N₄ synthesis[J]. Journal of Nanjing University of Technology, 2005, 27(1): 57-61.
70	张林进, 叶旭初, 吕秀玮. 高温流态化合成氮化硅的实验研究[J]. 材料工程, 2009, 11: 1-3.
	Zhang L J, Ye X C, Lv X W. Experimental study on preparation of silicon nitride by high-temperature fluidization[J]. Journal of Materials Engineering, 2009, 11: 1-3.
71	雷超, 魏飞. 单晶α-Si₃N₄纳米线宏量制备研究[J]. 无机材料学报, 2019, 34(6): 667-672.
	Lei C, Wei F. Mass production of α-silicon nitride single-crystalline nanowires[J]. Journal of Inorganic Materials, 2019, 34(6): 667-672.
72	Lee W Y, Strife J R, Veltri R D. Low-pressure chemical vapor deposition of alpha-Si₃N₄ from SiF₄ and NH₃: kinetic characteristics[J]. Journal of the American Ceramic Society, 1992, 75(8): 2200-2206.
73	Kijima K, Setaka N, Tanaka H. Preparation of silicon nitride single crystals by chemical vapor deposition[J]. Journal of Crystal Growth, 1974, 24/25: 183-187.
74	Zhu H J, Li C Z, Chen H, et al. Preparation of ultrafine Si₃N₄ powder by chemical vapor deposition[J]. Journal of Inorganic Materials, 1995, 10(1): 43-48.
75	Prochazka S, Greskovich C D. Preparation of silicon nitride powder: US4122155[P]. 1978-08-24.
76	王勇, 沃银花, 姚奎鸿, 等. 流态床CVD法纳米氮化硅粉体的制备[J]. 无机材料学报, 2006, 21(1): 41-45.
	Wang Y, Wo Y H, Yao K H, et al. CVD synthesis of silicon nitride(SiN) nanopowders in a novel two-stage fluidized bed reactor[J]. Journal of Inorganic Materials, 2006, 21(1): 41-45.
77	王勇, 周俊, 汪新颜, 等. 流态床CVD法制氮化硅超微粉过程分析及实验验证[J]. 浙江理工大学学报, 2007, 24(1): 36-39.
	Wang Y, Zhou J, Wang X Y, et al. Analysis and verification of silicon nitride super-micro powder synthesis with FBR-CVD technique[J]. Journal of Zhejiang Sci-Tech University (Natural Sciences Edition), 2007, 24(1): 36-39.
78	Kostić Ž G, Stefanović P L, Pavlović P B. Thermodynamic consideration of Si-N and Si-H-N systems for silicon nitride powder production in thermal plasma[J]. Ceramics International, 1996, 22(3): 179-186.
79	王锐, 黄永攀, 罗丽明, 等. 双光束激励制备纳米氮化硅粉体[J]. 硅酸盐学报, 2004, 32(11): 1425-1429.
	Wang R, Huang Y P, Luo L M, et al. Silicon nitride nano-powder prepared by double beam optical stimulation[J]. Journal of the Chinese Silicate Society, 2004, 32(11): 1425-1429.
80	Zhou R C, Chen Y Z, Liang Y, et al. Dispersion behavior of laser-synthesized Si₃N₄ nanopowders in N-N-dimethylformamide[J]. Ceramics International, 2002, 28(7): 705-709.
81	Iwai T, Kawahito K, Yamada T. Process for producing silicon nitride powder: US4405589[P]. 1983-09-20.
82	Tetsuo Y, Takashi Y, Keiichiro W, et al. Silicon nitride powder: US5585084[P]. 1996-12-17.
83	Kasai K, Tsukuma K,Tsukidate T. Method of manufacturing high-purity silicon nitride powder: US4387079[P]. 1983-06-07.
84	Mazdiyasni K S, Cooke C M. Synthesis of the high purity, alpha phase silicon nitride powder: US3959446[P]. 1976-05-25.
85	Yamada T, Yamao T, Kondo Y, et al. Process for producing a crystalline silicon nitride powder: US5595718[P]. 1997-01-21.
86	Clarke D R. Densification of silicon nitride: effect of chlorine impurities[J]. Journal of the American Ceramic Society, 1982, 65(2): C-21.
87	Billy M, Brossard M, Desmaison J, et al. Synthesis of Si and Ge nitrides and Si oxynitride by ammonolysis of chlorides comment on “synthesis, characterization, and consolidation of Si₃N₄ obtained from ammonolysis of SiCl₄”[J]. Journal of the American Ceramic Society, 1975, 58(5/6): 254-255.
88	Mazdiyasni K S, Cooke C M. Synthesis, characterization, and consolidation of Si₃N₄ obtained from ammonolysis of SiCl₄[J]. Journal of the American Ceramic Society, 1973, 56(12): 628-633.
89	Itoh N, Sasamoto T, Sata T, et al. Impurities in silicon nitride raw materials and correlation with mechanical strength of the hot-pressed body[J]. Journal of the Ceramic Association, Japan, 1982, 90(1040): 209-213.
90	Pezzotti G, Ota K, Kleebe H J. Viscous slip along grain boundaries in chlorine-doped silicon nitride[J]. Journal of the American Ceramic Society, 1997, 80(9): 2341-2348.
91	Kusano D, Noda Y, Shibasaki H, et al. Effects of impurity iron content on characteristics of sintered reaction-bonded silicon nitride[J]. International Journal of Applied Ceramic Technology, 2013, 10(4): 690-700.
92	胡智源, 张克鋐, 蔡作乾. SiCl₄气相氮化法合成超细氮化硅粉[J]. 化学通报, 1989, 52(11): 35-38.
	Hu Z Y, Zhang K H, Cai Z Q. Synthesis of ultrafine silicon nitride powder by nitridation of SiCl₄ gas[J]. Chemistry, 1989, 52(11): 35-38.
93	张克鋐, 安健, 刘艳生, 等. L-G法合成微细氮化硅粉和晶须[J]. 硅酸盐通报, 1994, 13(4): 8-12.
	Zhang K H, An J, Liu Y S, et al. The formation of Si₃N₄ superfine powder and α-Si₃N₄ whisker by L-G method[J]. Bulletin of the Chinese Ceramic Society, 1994, 13(4): 8-12.
94	Ziegenbalg G, Focke T, Holldorf H, et al. Gas-phase synthesis of amorphous silicon nitride-reaction paths and powder characteristics[J]. Journal of Materials Science, 1999, 34(9): 2199-2206.
95	Lin S S. Mass spectrometric detection of intermediates in chemical vapor deposition of Si₃N₄ from SiCl₄ and NH₃[J]. Journal of the Electrochemical Society, 1978, 125(11): 1877-1879.

[1]	Simin YI, Yali MA, Weiqiang LIU, Jinshuai ZHANG, Yan YUE, Qiang ZHENG, Songyan JIA, Xue LI. Study on ammonia evaporation and hydration kinetics of microcrystalline magnesite [J]. CIESC Journal, 2023, 74(4): 1578-1586.
[2]	Shiyi GE, Yao YANG, Zhengliang HUANG, Jingyuan SUN, Jingdai WANG, Yongrong YANG. Analyzing particle growth and morphology evolution of polyethylene based on electrostatic separation [J]. CIESC Journal, 2022, 73(4): 1585-1596.
[3]	WEI Juan, WANG Yujun, LUO Guangsheng. Influence of pore volume and heating process on preparation of aluminum nitride powder by carbothermal reduction method [J]. CIESC Journal, 2021, 72(2): 1156-1168.
[4]	SUN Zhanpeng, SUN Guogang, DU Yan. Effects of feed position and inlet gas velocity on particle classification in cyclonic classifier [J]. CIESC Journal, 2018, 69(4): 1324-1331.
[5]	KANG Junpei, GE Ting, LIU Sa, YANG Junzhong, REN Li. Effect of different ball milling processes on purity and particle size of β-tricalcium phosphate powders by solid-state synthesis [J]. CIESC Journal, 2017, 68(1): 424-429.
[6]	LONG Wenyu, XU Jun, FAN Yiping, LU Chunxi. Phenomenon of pinning in trapezoidal moving beds with cross-flow [J]. CIESC Journal, 2014, 65(4): 1179-1185.
[7]	WANG Haisheng，ZHANG Xiaoxia，LU Yuan，RUAN Zhiyong，XING Xinhui，JIANG Ruibo. Recent research progress of bacterial violacein [J]. , 2008, 27(3): 315-.