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1、231Vol.23No.1 20092CHINESE JOURNAL OF MATERIALS RESEARCH February2009(710072/,.X ,/,.:;, 1:0.5;Si3N4.,/,TB3211005-3093(200901-0039-04 Preparation of silicon nitride ceramic derived by UV curepolymer ceramic precursor:The eect of polyceramicstructure on pyrolyzate propertiesCHEN LixinWANG Yazhou SONG

2、 Jiale(School of Science,Key Laboratory of Applied Physics and Chemistry of Ministry of Education,Northwestern Polytechnical University,Xi an710072*Supported by National Natural Science Foundation of China No.20574056,Military Equipment Foundation of Defence No.9140A12070106HK0338and Doctorate Innov

3、ation Foundation of Northwestern Polytechnical University No.CX200614.Manuscript received February21,2008;in revised form April29,2008.*To whom correspondence should be addressed,Tel:(02988431683,Email:lixin ABSTRACT The polymer ceramic precursors with varied structures were made from UV cure thiol/

4、vinyl silizane copolymer.Silicon nitride ceramic was obtained by pyrolyzing at high temperature.The eects of functionality of thiol,size of thiol molecular,thiol to vinyl ratio and the amount of inertller on crystallinity and grain size were investigated and characterized by XRD,FESEM and energy spe

5、ctrometer and investigated.It is found that the increase of functionality of thiol enhances the crystallinity of the ceramic,but makes the grain size decrease.Increasing the size of thiol molecular has the same eect.Increasing the ratio of thiol to vinyl can enhances the crystallinity of the ceramic

6、,and there is a peak of the grain size when the ratio is0.5:1.The incorporation of inertller(Si3N4can obviously depress the shrinkage of the size of ceramic.KEY WORDS inorganic non-metallic materials,system of thiol/vinyl,UV cure,precursor,crystallinity,.,:(1,;(2*2008221;2008429.:,;(3;(4.,1.:.,:2,3(

7、456.7.4023,.1:( (Tetrathiol(3(Trithiol(1,3(Dithiol1,6(HDT(DMPA,(VL20,560, 1.7.VL200.01%DMPA (,.,.1400,13/min, 24h.X(PANalytical,X Pert,Nether-lands,.22.11,Si3N4,SiN,.2.2234,.2,.,.,.,;,.,.,.,;, .1XFig.1XRD spectrum of pyrolyzate2Fig.2Eect of thiol functionality in preceramic on crystallinity and grai

8、n size of pyrolyzate2.3VL20(1,3-(A1,6(B,.X,Si3N4.3,AB,.,. B,A,VL20,.,B,.2.4/,.4,1:41,1:0.5./,., 3Fig.3Eect of thiol chemical structure on crys-tallinity and grain size of pyrolyzate4/Fig.4Eect of thiol to ene ratio on crystallinity and grain size of pyrolyzate,.,.,.VL20,.,1:0.5.2.5(5,(30%,.,/Si3N4.1

9、 ,., .5Fig.5Comparison of preceramic with pyrolyzate.Top:pyrolyzate;bottom:preceramic1Table1Eect of inertller amount on pyrolyzate propertiesSi3N4ller/%Crystallinity/%Average grain size/nm Retained quality ratio/%Retained size ratio/% 060.8421.5051.9968.031067.6024.4052.7773.232079.2236.2056.0578.66

10、4087.5034.0059.5883.3342233/,.,;,1:0.5;Si3N4.1ZHANG Junbao,LEI Tingquan,WEN Guangwu,ZHOU Yu,Research progress in synthesis of silicon oxynitrid,Ma-terials Science&Technology,9(4,434(2001(,9(4,434(20012O.Delverdier,M.Monthioux,Thermal behavior of (organosiliconpolymer-derived ceramics V:Main fact

11、s and trends,J.of the Eur.Ceram.Soc.,16,721(19963K.Kakimoto, F.Wakai,J.Bill, A.Fritz,Fabrication of polycarbosilane-derived SiC bulk ceramics by carbother-mic reduction:Eect of green density on crystallinity of pyrolyzed compacts,J.Am.Ceram.Soc.Sep.,82(9, 23(19994G.Ziegler,H.J.Kleebe,G.Motz,H.Muller

12、,S.Traszl, W.Weibelzahl,Synthesis,microstructure and properties of SiCN ceramics prepared from tailored polymers,Materials Chemistry and Physics,61(1,55(19995Linan An,Wenge Zhang,V.M.Bright,M.L.Dunn,R.Raj, The13th IEEE Annual International Conference on Mi-croelectromechanical Systems(MEMS-2000,Miyazaki, Japan,January,23-27,619(20006Sirish K.Reddy,Neil B.Cramer,Tsali Cross,Rishi Raj, Christopher N.Bowman,Polymer-derived

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