Acta Chimica Sinica ›› 2012, Vol. 70 ›› Issue (08): 1035-1042.DOI: 10.6023/A1109254 Previous Articles     Next Articles

Special Topic


张建柯, 陈立新, 张红祥, 何玮奇   

  1. 西北工业大学理学院应用化学系 西安 710129
  • 投稿日期:2011-09-25 修回日期:2011-12-06 发布日期:2011-12-22
  • 通讯作者: 陈立新
  • 基金资助:

    西北工业大学研究生创业种子基金资助项目(No. Z2011014).

Synthesis, Characterization and Performance Study of Borosilazane as UV-Curable Borazine-Type Single Source Precursors for SiBNC Ceramic

Zhang Jianke, Chen Lixin, Zhang Hongxiang, He Weiqi   

  1. Department of Applied Chemistry, School of Science, Northwestern Polytechnical University, Xi'an 710129
  • Received:2011-09-25 Revised:2011-12-06 Published:2011-12-22
  • Supported by:

    Supported by Graduate Starting Seed Fund of Northwestern Polytechnical University (No. Z2011014).

A novel borosilazane monomer terminated with Si-Cl groups: B,B',B"-tris[(trichlorosilyl)- methyl] borazine (TSMB) was synthesized through one-step route by reacting boron trichloride (BCl3), chloromethyl trichlorosilane (CH2ClSiCl3) with hexamethyldisilazane (HMDZ) as the starting materials. From functionalizing TSMB by 2-hydroxethyl acrylate and 2-hydroxyethyl vinyl ether, two UV-curable single source precursors a-TSMB and e-TSMB were obtained, respectively. Then ceramic materials C1 and C2 can be prepared with a-TSMB and e-TSMB through UV-curing and cracking under 1400 ℃ for 2 h. The chemical composition, structure, photo-curing performance and ceramic yield of the TSMB, a-TSMB and e-TSMB were investigated using infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy (NMR), differential photocalorimetry (DPC), real time infrared spectroscopy (RT-IR) and thermo gravimetric analyzer (TGA). The content and high temperature performance of the ceramic C1 and C2 were studied by element analysis, X-ray photoelectron spectroscopy analysis (XPS) and X-ray diffraction (XRD). Results show that both the two ceramic precursors molecules, a-TSMB and e-TSMB, contain the B-N six-member ring structure, and are terminated with acrylate or vinyl ether functional groups, which matches well with the theoretical design. The photo polymerization of the a-TSMB and e-TSMB can finish 82% and 67% in 25 s, the final conversion of the double bond can reach 90.0% and 74.0%, and the corresponding ceramic yield at 1300 ℃ is 57.9% and 48.5%, respectively. There are five elements, Si, B, C, N, and O in the C1 and C2 ceramic materials, and the contents of B are 4.4% and 4.9%, respectively, which can achieve the requirement for the high temperature ceramic material on the B element. Both the ceramic materials C1 and C2 can preserve amorphous states at 1400 ℃ and have excellent high-temperature resistance properties.

Key words: SiBNC ceramic, borosilazane, single source precursor, UV curing, structure characterization