反应烧结制备Si_3N_4基复合材料
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摘要
本文用气态耗定升温法反应烧结制备了Si_3N_4结合SiC材料和Si_3N_4结合AlN材料，研究了材料的制备工艺，微观组织、气孔率、增重、表面硬度和抗弯强度和反应机理。结果表明，冷等静压成型的材料烧结后性能优于干压成型的材料，SiC颗粒在Si_3N_4基体中分布均匀，试样的气孔率随着SiC含量的增加而增加，材料抗弯强度随着SiC含量的增加有所降低，在SiC含量8％时可以达到最大值141MPa；反应烧结制备AlN结合Si_3N_4时由于烧结的过程中出现液相，容易生成β—Si_3N_4，容易使材料发生熔硅现象，在Al熔点附近延长保温时间，可以形成强度在200MPa的β相Si_3N_4—AlN复合陶瓷。
Reaction-sintered SiC/Si3N4 and reaction -sintered A1N /Si3N4 composite material were manufactured by quasi-static temperature-rising craft. The preparation craft, microstructure, pore ratio, surface hardness, bend strength and reaction theorem has been studied and analysed . The result showed the physical property of material molded by hydrostatic pressing is prior to that of material molded by uni-axial pressing. In the SiC/Si3N4 composite material, SiC partical dispersed uniformly in Si3N4 matrix, the pore ratio increased and the bend strength decreased with the increasing mass of SiC, the bend strength of material with 8% SiC is up to 141MPa. The melted silicon and β -Si3N4 could be seen in the A1N/SJ3N4 material because of the liquid phase appearing. Si3N4/AlN material which bend strength was 200Mpa could be prepared if prolong the heat preservation time near Al melting point.
Reaction-sintered SiC/Si3N4 and reaction -sintered A1N /Si3N4 composite material were manufactured by quasi-static temperature-rising craft. The preparation craft, microstructure, pore ratio, surface hardness, bend strength and reaction theorem has been studied and analysed . The result showed the physical property of material molded by hydrostatic pressing is prior to that of material molded by uni-axial pressing. In the SiC/Si3N4 composite material, SiC partical dispersed uniformly in Si3N4 matrix, the pore ratio increased and the bend strength decreased with the increasing mass of SiC, the bend strength of material with 8% SiC is up to 141MPa. The melted silicon and β -Si3N4 could be seen in the A1N/SJ3N4 material because of the liquid phase appearing. Si3N4/AlN material which bend strength was 200Mpa could be prepared if prolong the heat preservation time near Al melting point.
引文
1．董文麟．氮化硅陶瓷．中国建筑工业出版社．1987
2. Navuril Rishan Reddy et al.J.Am.Ceram Soc. 1991.74:1139
3．江东亮．精细陶瓷材料．中国物资出版社．2000
4．李世普．特种陶瓷工艺学．武汉工业大学出版社．1990
5．铃木弘茂．工程陶瓷．科学出版社．1989
6．陈华辉．现代复合材料．中国物质出版社．1997
7．孙兴伟等．(TiB_2，TiN)—Si_3N_4基复合材料的性能及显微结喉．硅酸盐学报．2000(1)65～67
8．沈建新．MoSi_2增韧Si_3N_4的研究．现代技术陶瓷．2000(1)15～18
9．吴锵著．材料科学基础．东南大学出版社．2001
10. claussen.Stability of Tetragonal ZrO_2 Particles. American Ceramic Society Bulletin. 1982 (12) 642～650
11．张宝清等．无压烧结Si_3N_4—3YZrO_2复相陶材料得力学性能和增韧机理研究．硅酸盐学报．1997．(2)176～182
12. Lange.F.F. Phase retention and fracture toughness of materials containing tetragonal ZrO_2. Proceedings-Computer Networking Symposium. 1980 (3) 45～56
13. woetting.G. et al. Influence of powder properties and processing conditions on microstructure and mechanical properties of sintered Si_3N_4. Ceramics International, 19-84(1～3) 18-22
14．倪国年．自韧化氮化硅陶瓷研究．北京理工大学学报．1996(4)380
15．赵振波等．自韧化氮化硅陶瓷的研究进展．无机材料学报．1997(1)1～9
16．罗学涛．β品种增韧Si_3N_4复合材料的制备与力学性能．硅酸盐学报．1999(4)461～465
17．许钫钫．Si_3N_4／BN(c)复合材料的相界面．无机材料学报．1998(1)109～112
18．汪长安．定向排布的SiC晶须补强Si_3N_4复合材料的制备．硅酸盐学报．1997(1)54～59
19. Coble,R.L. Sintering Crystalline Solids. Journal of Application Physics.32,787
20. Burke,J.E.,Lay, K,W.,Prochazka, S.(1980).Sintering Progresses:Kuczynski,G.C.,(ED.).
21．[英]理查德J．布鲁克主编．陶瓷工艺(第Ⅱ部分)．科学出版社．1999
22. Kingery, W.D.Densification During Sintering in the Presence of a Liquid Phase: Ⅰ, Theory. Journal of Application Physics.1950(3) 301～306
23. Kingery, W.D.,Narasimhan,M.D. Densification During Sintering in the Presence of a Liquid Phase: Ⅱ, Experimental, Journal of Application Physics. 1950 307～310
24．祝昌军．氮化硅陶瓷的制备及进展．江苏陶瓷．2001(3) 10～13
25．陈波．氮化硅陶瓷的生产工艺与应用前景．现代技术陶瓷．2002(2)28～30
26．初小葵．反应烧结氮化硅的研制．辽宁建材．2002(3)32～33
27．H.A.库恩．粉末冶金工艺新技术及其分析．冶金工业出版社．1982
28．张光明．Si_3N_4、SiC复合陶瓷的性质和应用．工业陶瓷1991(4)43～45
29．张林．Si_3N_4—SiC材料的生产与应用．陶瓷工程．1999(2)5～9
30．谭国强．高档优质反应结合氮化硅结合碳化硅窑具的制备．中国陶瓷．1996(5)16～18
31．张国军等．颗粒增韧陶瓷的增韧机理．硅酸盐学报．1994(1)：259
32．司文捷等．SiC颗粒弥散对相变增韧陶瓷高温蠕变性能的影响．硅酸盐学报．1997(3)：208
33．穆柏春．Si_3N_4／SiC_p复合材料的低温冷处理与强韧化．硅酸盐学报．25(4)．1997：413～419
34．刘铭等．提高氮化硅结合碳化硅制品抗热震性的研究．耐火材料．30(2)．1996：74—76
35．黄朝晖等．Si加入量对反应烧结Si_3N_4结合SiC性能的影响．耐火材料．1990(5)10～14
36．王资江．水蒸汽对氮化烧成品的影响．耐火材料．1998(1) 29～31
37．凌志达．Si—C—O—N系统相稳定性和相稳定性图．南京化工学院学报．1994．(1)33～40
38．池跃章．影响氮化硅制品显微结构及性能的因素．陶瓷工程．1997(4)12～13
39．黄朝晖等．Al2O3对Si3N4结合SiC材料抗氧化性和抗碱侵蚀的影响．耐火材料．2000．34(6)：13
40. Moulson. A.J .Review of reaction-bonded silicon nitride: its formation and properties. Journal of Material Science 1979 (5) 1017～1051
41. Mitomo. M. Effect of Fe and Al additions on Nitridation of Silicon. Journal of Material Science. 1977 (2) 273～276
42．池跃章、张湛等．添加剂的粒度及加入方式对RBSN显微结构及性能影响．陶瓷工程．30(4)：18
43．何钢．石磊．纳米Si_3N_4颗粒对反应烧结Si_3N_4结合SiC材料的影响．合肥工业大学学报．24(1)．2000：90～95
44. Heinyich.J. Compact ceramic heat-exchangers: design, fabrication and testing. British Ceramic
Transactions and Journal. 1987 (6) 178～182
45 Atkinson A,Leatt P.J.et al. Mechanism for the nitridation of silicon powder compacts.Journal of Material Science. 1974 (5) 981-984
46．王立军等．氮化硅结合碳化硅窑具材料的研制。硅酸盐通报．1994．3：4～6
47. Rice R.W.et al. Fracture energy of Si_3N_4 Journal of Material Science.1985 (5):1392-1406
48．李欣等．氮化硅结合碳化硅材料掺入稀土烧结机理研究．哈尔滨师范大学自然科学学报．2001(2)85～88
49．张建艺．陶瓷基复合材料在喷管上的应用．宇航材料工艺．2000(4) 14～16
50．G．P萨登著．火箭发动机．国防工业出版社．1966
51．郭景坤．陶瓷材料的强化与增韧新途径的探索．无机材料学报．13(1)．1998．：23～24
52．李风生．粉体工程．国防工业出版社．2001
53．费多尔钦科等．粉末冶金原理．冶金工业出版社．1974．
54．黄培云著．粉末冶金原理．冶金工业出版社．1997
55．马富康主编．等静压技术．机械工业出版社．1992
56．张长瑞．硅氮合成氮化硅的机理和动力学．华南理工大学所示论文．1984
57．徐永东．大型薄壁复杂氮化硅结合碳化硅陶瓷构件的制造与应用．材料导报．2000(10) 92～93
58．姚德超．粉末冶金试验技术．冶金工业出版社．1990
59．束德林．金属的力学性能．机械工业出版社．1987
60. Atkinson,A.,Moulson,A.M.Nitridation of High Purity Sicicon.Joumal of American Ceramic Society. 1976 (7～8)286～289
61. Jennings,H.M, Richman,M.H. Microstructural analysis of Reaction-Bonded Silicon Nitride.Metallography. 1976 (10) 427～446
62. boyer.moulson.
63. Lange,.F.F.Singhal,S.C. Phase relations and Stability Studies in the Si_3N_4-SiO_2-Y_2O_3 Pseudoternary System .Journal of the American Ceramics Society.1977 (5～7) 249～252,
64．蔡克峰，南策文．反应烧结制备AlN—Al_2O_3复合陶瓷的机理研究．硅酸盐学报．1996．2．216～221．
65．L．F．蒙多尔福著．王祝堂，张振录，郑璇等译．铝合金的组织与性能．冶金工业出版社．1988
2. Navuril Rishan Reddy et al.J.Am.Ceram Soc. 1991.74:1139
3．江东亮．精细陶瓷材料．中国物资出版社．2000
4．李世普．特种陶瓷工艺学．武汉工业大学出版社．1990
5．铃木弘茂．工程陶瓷．科学出版社．1989
6．陈华辉．现代复合材料．中国物质出版社．1997
7．孙兴伟等．(TiB_2，TiN)—Si_3N_4基复合材料的性能及显微结喉．硅酸盐学报．2000(1)65～67
8．沈建新．MoSi_2增韧Si_3N_4的研究．现代技术陶瓷．2000(1)15～18
9．吴锵著．材料科学基础．东南大学出版社．2001
10. claussen.Stability of Tetragonal ZrO_2 Particles. American Ceramic Society Bulletin. 1982 (12) 642～650
11．张宝清等．无压烧结Si_3N_4—3YZrO_2复相陶材料得力学性能和增韧机理研究．硅酸盐学报．1997．(2)176～182
12. Lange.F.F. Phase retention and fracture toughness of materials containing tetragonal ZrO_2. Proceedings-Computer Networking Symposium. 1980 (3) 45～56
13. woetting.G. et al. Influence of powder properties and processing conditions on microstructure and mechanical properties of sintered Si_3N_4. Ceramics International, 19-84(1～3) 18-22
14．倪国年．自韧化氮化硅陶瓷研究．北京理工大学学报．1996(4)380
15．赵振波等．自韧化氮化硅陶瓷的研究进展．无机材料学报．1997(1)1～9
16．罗学涛．β品种增韧Si_3N_4复合材料的制备与力学性能．硅酸盐学报．1999(4)461～465
17．许钫钫．Si_3N_4／BN(c)复合材料的相界面．无机材料学报．1998(1)109～112
18．汪长安．定向排布的SiC晶须补强Si_3N_4复合材料的制备．硅酸盐学报．1997(1)54～59
19. Coble,R.L. Sintering Crystalline Solids. Journal of Application Physics.32,787
20. Burke,J.E.,Lay, K,W.,Prochazka, S.(1980).Sintering Progresses:Kuczynski,G.C.,(ED.).
21．[英]理查德J．布鲁克主编．陶瓷工艺(第Ⅱ部分)．科学出版社．1999
22. Kingery, W.D.Densification During Sintering in the Presence of a Liquid Phase: Ⅰ, Theory. Journal of Application Physics.1950(3) 301～306
23. Kingery, W.D.,Narasimhan,M.D. Densification During Sintering in the Presence of a Liquid Phase: Ⅱ, Experimental, Journal of Application Physics. 1950 307～310
24．祝昌军．氮化硅陶瓷的制备及进展．江苏陶瓷．2001(3) 10～13
25．陈波．氮化硅陶瓷的生产工艺与应用前景．现代技术陶瓷．2002(2)28～30
26．初小葵．反应烧结氮化硅的研制．辽宁建材．2002(3)32～33
27．H.A.库恩．粉末冶金工艺新技术及其分析．冶金工业出版社．1982
28．张光明．Si_3N_4、SiC复合陶瓷的性质和应用．工业陶瓷1991(4)43～45
29．张林．Si_3N_4—SiC材料的生产与应用．陶瓷工程．1999(2)5～9
30．谭国强．高档优质反应结合氮化硅结合碳化硅窑具的制备．中国陶瓷．1996(5)16～18
31．张国军等．颗粒增韧陶瓷的增韧机理．硅酸盐学报．1994(1)：259
32．司文捷等．SiC颗粒弥散对相变增韧陶瓷高温蠕变性能的影响．硅酸盐学报．1997(3)：208
33．穆柏春．Si_3N_4／SiC_p复合材料的低温冷处理与强韧化．硅酸盐学报．25(4)．1997：413～419
34．刘铭等．提高氮化硅结合碳化硅制品抗热震性的研究．耐火材料．30(2)．1996：74—76
35．黄朝晖等．Si加入量对反应烧结Si_3N_4结合SiC性能的影响．耐火材料．1990(5)10～14
36．王资江．水蒸汽对氮化烧成品的影响．耐火材料．1998(1) 29～31
37．凌志达．Si—C—O—N系统相稳定性和相稳定性图．南京化工学院学报．1994．(1)33～40
38．池跃章．影响氮化硅制品显微结构及性能的因素．陶瓷工程．1997(4)12～13
39．黄朝晖等．Al2O3对Si3N4结合SiC材料抗氧化性和抗碱侵蚀的影响．耐火材料．2000．34(6)：13
40. Moulson. A.J .Review of reaction-bonded silicon nitride: its formation and properties. Journal of Material Science 1979 (5) 1017～1051
41. Mitomo. M. Effect of Fe and Al additions on Nitridation of Silicon. Journal of Material Science. 1977 (2) 273～276
42．池跃章、张湛等．添加剂的粒度及加入方式对RBSN显微结构及性能影响．陶瓷工程．30(4)：18
43．何钢．石磊．纳米Si_3N_4颗粒对反应烧结Si_3N_4结合SiC材料的影响．合肥工业大学学报．24(1)．2000：90～95
44. Heinyich.J. Compact ceramic heat-exchangers: design, fabrication and testing. British Ceramic
Transactions and Journal. 1987 (6) 178～182
45 Atkinson A,Leatt P.J.et al. Mechanism for the nitridation of silicon powder compacts.Journal of Material Science. 1974 (5) 981-984
46．王立军等．氮化硅结合碳化硅窑具材料的研制。硅酸盐通报．1994．3：4～6
47. Rice R.W.et al. Fracture energy of Si_3N_4 Journal of Material Science.1985 (5):1392-1406
48．李欣等．氮化硅结合碳化硅材料掺入稀土烧结机理研究．哈尔滨师范大学自然科学学报．2001(2)85～88
49．张建艺．陶瓷基复合材料在喷管上的应用．宇航材料工艺．2000(4) 14～16
50．G．P萨登著．火箭发动机．国防工业出版社．1966
51．郭景坤．陶瓷材料的强化与增韧新途径的探索．无机材料学报．13(1)．1998．：23～24
52．李风生．粉体工程．国防工业出版社．2001
53．费多尔钦科等．粉末冶金原理．冶金工业出版社．1974．
54．黄培云著．粉末冶金原理．冶金工业出版社．1997
55．马富康主编．等静压技术．机械工业出版社．1992
56．张长瑞．硅氮合成氮化硅的机理和动力学．华南理工大学所示论文．1984
57．徐永东．大型薄壁复杂氮化硅结合碳化硅陶瓷构件的制造与应用．材料导报．2000(10) 92～93
58．姚德超．粉末冶金试验技术．冶金工业出版社．1990
59．束德林．金属的力学性能．机械工业出版社．1987
60. Atkinson,A.,Moulson,A.M.Nitridation of High Purity Sicicon.Joumal of American Ceramic Society. 1976 (7～8)286～289
61. Jennings,H.M, Richman,M.H. Microstructural analysis of Reaction-Bonded Silicon Nitride.Metallography. 1976 (10) 427～446
62. boyer.moulson.
63. Lange,.F.F.Singhal,S.C. Phase relations and Stability Studies in the Si_3N_4-SiO_2-Y_2O_3 Pseudoternary System .Journal of the American Ceramics Society.1977 (5～7) 249～252,
64．蔡克峰，南策文．反应烧结制备AlN—Al_2O_3复合陶瓷的机理研究．硅酸盐学报．1996．2．216～221．
65．L．F．蒙多尔福著．王祝堂，张振录，郑璇等译．铝合金的组织与性能．冶金工业出版社．1988