Effects of Carbon Sources on Structure and Properties of TaC Ceramic Powder Prepared by Polymer Derived Ceramics

doi:10.15541/jim20220553

Abstract

Abstract:

Polymer derived ceramic is one of the effective methods for producing ultra-high temperature ceramics and powders, but effect of source material type on precursor cross-linking degree and ceramic yield has rarely been reported. Here, TaC precursors were synthesized using two carbon sources and poly-tantalumoxane (PTO). Phase composition and microstructure of TaC ceramic powders from different carbon sources, tantalum/carbon mass ratios, and pyrolysis temperatures were characterized. It was found that PF-3 resin with C=C was effective in promoting the cross-linking of PTO and increasing the ceramic yield. When the mass ratio of PTO to PF-3 Resin was 1 : 0.25 and PTO to 2402 Resin was 1 : 0.4, TaC ceramic powders could be obtained at 1400 ℃ without residue Ta₂O₅. Ceramic yields of ceramic powders were 54.02% and 49.64%, and the crystal sizes were 47.2 and 60.9 nm, respectively. Therefore, PF-3 resin is able to reduce crystal size while increasing ceramic yield, but has less impact on the powder purity and particle size. The purity of TaC ceramic powders derived from different carbon sources are 96.50% and 97.36%, respectively, meanwhile the median diameters are 131 and 129 nm, respectively.

Key words: poly-tantalumoxane (PTO), polymer derived ceramics, TaC, cross-linking, curing, ceramic yield

CLC Number:

TH145

SUN Jingwei, WANG Honglei, SUN Chuhan, ZHOU Xingui, JI Xiaoyu. Effects of Carbon Sources on Structure and Properties of TaC Ceramic Powder Prepared by Polymer Derived Ceramics[J]. Journal of Inorganic Materials, 2023, 38(2): 184-192.

Figures/Tables 12

Fig. 1 Preparation process of TaC ceramic powder

Fig. 2 FT-IR of different carbon sources and crosslinked products (a) PTO, PF-3, PTC1 pioneer; (b) PTO, 2402 Resin, PTC2 pioneer

Fig. 3 TG curves of different tantalum carbon sources and crosslinked products (a) PTO, PF-3, 2402 Resin, PTC1-25 (220 ℃), PTC2-40(220 ℃); (b) PTC1-25 (1000 ℃); (c) PTC2-40(1000 ℃) Colorful figures are available on website

Fig. 4 XRD patterns of ceramic products obtained at different pyrolysis temperatures and tantalum/carbon ratios (a) PTC1-25, 800~1500 ℃; (b) PTC1-(10~40), 1400 ℃, 2 h; (c) PTC2-(20~45), 1400 ℃ 2 h

Table 1 Average grain size of TaC powder with different carbon source ratios

Sample	L/nm	Sample	L/nm
PTC1-10	62.5	PTC2-20	71.3
PTC1-15	73.9	PTC2-30	67.9
PTC1-20	67.2	PTC2-35	66.0
PTC1-25	47.2	PTC2-40	60.9
PTC1-30	45.5	PTC2-45	54.8
PTC1-35	39.7
PTC1-40	37.5

Fig. 5 Raman spectra of TaC powders obtained at different tantalum/carbon ratios (a) PTC1-(10-40); (b) PTC2-(25-45)

Table 2 Center positions of D and G peaks of PTC1-25 products obtained at different pyrolysis temperatures and ratios of ${{I}_{\mathbf{D}}}/{{I}_{\mathbf{G}}}$

Temperature/℃	ω_D/cm^-1	ω_G/cm^-1	${{I}_{\text{D}}}/{{I}_{\text{G}}}$
1200	1313	1576	2.045
1300	1315	1579	1.641
1400	1313	1580	1.605

Table 3 Elements mass contents of TaC powders obtained at optimal tantalum/carbon ratio

Sample	Ta/%	C/%	O/%	C_free/%
PTC1-25	91.72	5.02	1.31	2.19
PTC2-40	92.14	6.42	0.89	1.75

Fig. 6 Histograms of the granularity distributions of TaC powders obtained at optimal tantalum/carbon mass ratios (a) PTC1-25; (b) PTC2-40

Fig. 7 SEM images of TaC powders obtained at different tantalum/carbon mass ratios (a) PTO; (b) PTC1-25; (c) PTC1-40; (d) PTC2-40; (e) PTC2-45

Fig. 8 Elemental distributions of TaC powders obtained at optimal tantalum/carbon mass ratios (a) PTC1-25; (b) PTC2-40

Fig. 9 TEM and HRTEM images of TaC powders obtained at optimal tantalum/carbon ratios (a, b) PTC1-25; (c, d) PTC2-40

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