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. 2020 May 6;13(9):2142.
doi: 10.3390/ma13092142.

Microstructures of a SiC-ZrC Ceramic Fiber Derived from a Polymeric Precursor

Min Ge  1 , Xiaoxu Lv  2 , Hao Zhang  1   3 , Shouquan Yu  1 , Zhenxi Lu  1 , Weigang Zhang  1   3
Affiliations

Microstructures of a SiC-ZrC Ceramic Fiber Derived from a Polymeric Precursor

Min Ge et al. Materials (Basel). .

Abstract

Continuous ceramic fiber comprising silicon carbide-zirconium carbide (SiC-ZrC) binary phases was obtained through melt spinning, electron-beam curing and pyrolysis of a pre-ceramic precursor of polyzirconocenecarbosilanes (PZCS). After pyrolysis and heat treatment, ZrC particles with mean diameters of 15-20 nm were formed and homogeneously dispersed in a matrix of fine crystalline β-SiC with an average grain size of 6-10 nm. Concentration of Zr in the fiber varies from 14.88% to 17.45% by mass. Fibers consisting of near-stoichiometric ZrC and SiC with little free carbon can be obtained through pyrolysis decarbonization of the as-cured fiber in hydrogen from room temperature to 1000 °C, and subsequently heat treatment in argon up to 1600 °C for 1 h. High-temperature treatment of these amorphous inorganic fibers leads to crystallization of the binary phases of β-SiC and ZrC. The removal of free carbon under hydrogen results in more rapid growth of β-SiC and ZrC crystals, in which obvious aggregation of the dispersed ZrC particles among the continuous β-SiC matrix can be ascribed to a fast migration of Zr cation.

Keywords: ceramic fiber; silicon carbide; zirconium carbide.

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Conflict of interest statement

The authors declare no conflict of interest.

Figures

Figure 1
Figure 1
Scanning electron microscopy (SEM) images of the surface (a) and cross-section (b) of the electron-beams (EB)-cured polyzirconocenecarbosilanes (PZCS) fiber and X-ray energy dispersive spectrometer (EDS) images (c) and (d) from surface to core of the fiber.
Figure 1
Figure 1
Scanning electron microscopy (SEM) images of the surface (a) and cross-section (b) of the electron-beams (EB)-cured polyzirconocenecarbosilanes (PZCS) fiber and X-ray energy dispersive spectrometer (EDS) images (c) and (d) from surface to core of the fiber.
Figure 2
Figure 2
Surface and cross-sectional SEM images of the as-cured PZCS fibers after H2–Ar process up to various temperatures of (a,b): 1200 °C; (c,d): 1400 °C; (e,f): 1600 °C, wherein (b,d,f) are the backscattered electron images.
Figure 3
Figure 3
XRD patterns of SiC–ZrC ceramic fibers through (a) H2–Ar process and (b) Ar–Ar process up to various temperatures of 1200, 1400 or 1600 °C.
Figure 4
Figure 4
Raman spectra of the SiC–ZrC fibers obtained at 1600 °C via the Ar–Ar process (a) and the H2–Ar process (b).
Figure 5
Figure 5
HR-TEM images of the as-cured fibers obtained via the Ar–Ar process up to (a) 1400 and (b) 1600 °C.
Figure 6
Figure 6
HR-TEM images of the as-cured fibers obtained via the H2–Ar process up to (a) 1400 and (b) 1600 °C.
Figure 7
Figure 7
Crystalline grain sizes of ZrC (a,b) and SiC (c,d) in the composite fibers after pyrolysis at 1000 °C and annealing at various temperatures from 1200 to 1600 °C (a,c: H2–Ar process; b,d: Ar–Ar process).
See this image and copyright information in PMC

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