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羟基化结合硅烷偶联剂改性对光固化Si3N4膏料性能的影响
Effects of Hydroxylation and Silane Coupling Agent Modification on Properties of Stereolithography Si3N4 Paste
【摘要】 采用羟基化结合硅烷偶联剂(KH560)对氮化硅(Si3N4)粉体进行表面功能化改性,配制出高固含量、高固化深度的Si3N4膏料,并基于立体光固化(SL)工艺制备了高强度的Si3N4复杂结构件。结果表明:Si3N4表面的KH560改善了粉体与树脂的相容性,降低了Si3N4膏料的粘度;同时,KH560的环氧基团(—CH(O)CH2)与环氧树脂(EA)通过化学键等方式相结合,形成了EA核壳结构,降低了树脂与陶瓷颗粒之间的折射率差,从而提高了Si3N4膏料的固化深度。表面羟基化处理后Si3N4表面吸附了更多的KH560,从而进一步降低了Si3N4膏料的粘度,提高了Si3N4膏料的固化深度。最终,用羟基化和KH560改性后的Si3N4粉体配制出的Si3N4膏料固含量达到50%(体积分数),固化深度达到64μm。烧结后Si3N4试样致密度为83%,断裂韧性为(4.38±0.45) MPa·m1/2,抗弯强度达到(407.95±10.50) MPa。
【Abstract】 The surface of silicon nitride(Si3N4) powder was functionally modified by hydroxylation combined with silane coupling agent(KH560) to prepare Si3N4 paste with high solid content and high curing depth. High strength Si3N4 complex structures based on stereolithography(SL) process were fabricated. The results show that KH560 on the surface of Si3N4 improves the compatibility of powder and resin, and reduces the viscosity of Si3N4 paste. At the same time, the epoxy group(—CH(O)CH2) of KH560 is combined with epoxy resin(EA) through chemical bonds or other ways to form an EA core-shell structure, which reduces the refractive index difference between the resin and ceramic particles. Thus, the curing depth of Si3N4 paste is improved. After the surface hydroxylation treatment, more KH560 is adsorbed on the surface of Si3N4, which further reduces the viscosity of Si3N4 paste and increases the curing depth of Si3N4 paste. Finally, the Si3N4 paste prepared with hydroxylated and KH560 modified Si3N4 powder has a solid phase content of 50%(volume fraction) and a curing depth of 64 μm. After sintering, the density of Si3N4 sample is 83%, the fracture toughness is(4.38±0.45) MPa·m1/2, and the flexural strength reaches(407.95±10.50) MPa.
【Key words】 stereolithography; Si3N4 ceramics; silane coupling agent; hydroxylation; surface modification; rheological property; curing depth;
- 【文献出处】 硅酸盐通报 ,Bulletin of the Chinese Ceramic Society , 编辑部邮箱 ,2022年06期
- 【分类号】TQ174.758.12;V243.4;V443.4
- 【下载频次】188