Journal of Textile Research ›› 2022, Vol. 43 ›› Issue (08): 48-54.doi: 10.13475/j.fzxb.20210505807

• Fiber Materials • Previous Articles     Next Articles

Preparation and properties of silicon nitride fibers by oxygen thermal cross-linking of polysilazane

LI Hailong, CHEN Jianjun(), BAO Zhihao, XIONG Yilian, LIN Wenxin   

  1. School of Materials Science and Engineering, Zhejiang Sci-Tech University, Hangzhou, Zhejiang 310018, China
  • Received:2021-05-24 Revised:2022-05-06 Online:2022-08-15 Published:2022-08-24
  • Contact: CHEN Jianjun E-mail:chen@zstu.edu.cn

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Abstract:

To explore the optimum technology of oxygen thermal cross-linking for polysilazane (PSZ) fibers and the effect of oxygen thermal cross-linking on compositions and structures of PSZ fibers and silicon nitride (Si3N4) fibers, Si3N4 fibers were successfully prepared using methyldichlorosilane and dimethyldichlorosilane as raw materials by ammonolysis polycondensation, thermopolymerization, melt spinning, oxygen thermal cross-linking and pyrolysis. Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction and some other measures were utilized to analyze the structure and properties of the samples. After the PSZ fibers cured at 120 ℃ for 12 h, its ceramic yields were higher than that of uncured PSZ fibers by about 10.2％. The Si3N4 fibers with smooth flat surface and without groove cracks and other defects were obtained by pyrolysis of the cured PSZ fibers at 1 400 ℃ for 2 h. Furthermore, a layer of SiO2 crystalline phase was observed on the surface of the Si3N4 fibers after high-temperature oxidation in air at 1 500 ℃ for 2 h. The obtained fibers after oxidation was a typical type of skin-core structure fibers.

Key words: precursor derived method, polysilazane, silicon nitride fiber, oxygen thermal cross-linking

CLC Number: 

  • TB34

Fig.1

Infrared spectra of silazane oligomers, PSZ fiber precursors, cross-linked PSZ fibers and Si3N4 fibers"

Fig.2

XPS full spectra of polysilazane and Si3N4 fibers"

Tab.1

Elements content in PSZ and Si3N4 fibers ％"

纤维名称 O1s N1s C1s Si2s Si2p
PSZ纤维 2.79 16.02 38.97 21.01 21.22
Si3N4纤维 17.47 11.50 30.24 19.89 20.89

Fig.3

XPS narrow scan spectra of polysiloxane and Si3N4 fibers"

Fig.4

Apparent morphology of polysilazane fibers treated at different temperatures"

Fig.5

Apparent morphology of polysilazane fibers treated at 120 ℃ for different time"

Fig.6

TG curves of polysilazane fibers before and after thermal oxidation"

Fig.7

SEM images of silicon nitride fiber and high temperature oxidation treated fiber. (a) Si3N4fiber; (b) Si3N4 oxidized at high temperature"

Fig.8

XRD pattern of Si3N4 fibers and high temperature oxidation treated Si3N4 fibers"

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