HfC Precursor: Synthesis and Pyrolysis Behavior

doi:10.15541/jim20160692

Abstract

Abstract:

Hafnium carbide ceramic powders were prepared by pyrolysis of a novel precursor, which was synthesized via one pot method using hafnium tetrachloride, acetylacetone, methanol, and hydroquinone as raw materials. The composition, morphology and microstructure of the pyrolysis products were characterized by XRD, FTIR, SEM/EDS, TEM, and SAED. The pyrolysis behavior of the obtained HfC precursor was investigated by TG-DSC and TG-MS. The results show that the ceramization of the HfC precursor starts at about 600℃, and the formation of HfC ceramics is initiated at about 1300℃. At temperature above 1500℃, the precursor completely transforms into HfC ceramics and free carbon. The as-obtained HfC phase has a single crystal structure and the size of the HfC particles ranges from 50 to 100 nm. Formation of the HfC ceramics can be attributed to the carbothermal reduction reaction of the HfO₂, which is produced by pyrolysis of the precursor at a relative low temperature. The growth of the HfC crystals is retarded by free carbon formed during pyrolysis of the precursor.

Key words: Hafnium carbide, precursor, pyrolysis behavior, carbothermal reduction reaction

CLC Number:

TB332

ZHANG Cheng, GONG Jun-Jie, DONG Zhi-Jun, MENG Jian, ZHOU Si-Cheng, YUAN Guan-Ming, LI Xuan-Ke. HfC Precursor: Synthesis and Pyrolysis Behavior[J]. Journal of Inorganic Materials, 2017, 32(10): 1095-1101.

Figures/Tables 7

Fig. 1 Synthesis route of HfC precursor

Fig. 2 FTIR spectra of the HfC precursor and products pyrolyzed at different temperatures(a) 400-800℃; (b) 1000-1500℃

Fig. 3 XRD patterns of the products from HfC precursor pyrolyzed at different temperatures(a) 400-1000℃; (b) 1200-1600℃

Fig. 4 TG-DSC curves of the HfC precursor

Fig. 5 TG-MS analysis of the released gaseous products during the pyrolysis of HfC precursor

Fig. 6 SEM images, EDS patterns and EDS mapping of the pyrolysis products from HfC precursor at different temperatures for 1 h(a, e) 1200℃; (b, f) 1300℃; (c)1400℃; (d, g)1500℃; (h, i, j)1600℃

Fig.7 TEM (a-b) and HRTEM (c) images as well as SAED pattern (d) of the pyrolysis products from HfC precursor at 1600℃ for 1 h

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