羟基化结合硅烷偶联剂改性对光固化Si3N4膏料性能的影响

摘要/Abstract

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64 μm。烧结后Si₃N₄试样致密度为83%,断裂韧性为(4.38±0.45) MPa·m^1/2,抗弯强度达到(407.95±10.50) MPa。

关键词: 立体光固化, Si₃N₄陶瓷, 硅烷偶联剂, 羟基化, 表面改性, 流变特性, 固化深度

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·m^1/2, 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

中图分类号:

TQ174

吴佩遥, 鲍崇高, 李世佳, 董文彩, 马海强, 宋索成. 羟基化结合硅烷偶联剂改性对光固化Si₃N₄膏料性能的影响[J]. 硅酸盐通报, 2022, 41(6): 2134-2142.

WU Peiyao, BAO Chonggao, LI Shijia, DONG Wencai, MA Haiqiang, SONG Suocheng. Effects of Hydroxylation and Silane Coupling Agent Modification on Properties of Stereolithography Si₃N₄ Paste[J]. BULLETIN OF THE CHINESE CERAMIC SOCIETY, 2022, 41(6): 2134-2142.

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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

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