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Electrical and Thermal Properties of Nitrogen-Doped Sic Sintered Body

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Electrical and Thermal Properties of Nitrogen-Doped Sic Sintered Body 508 J. Jpn. Soc. Powder Powder Metallurgy Vol. 65, No. 8 ©2018 Japan Society of Powder and Powder Metallurgy Paper Electrical and Thermal Properties of Nitrogen-Doped SiC Sintered Body Yukina TAKI, Mettaya KITIWAN, Hirokazu KATSUI and Takashi GOTO* Institute for Materials Research, Tohoku University, 2-1-1 Katahira, Aoba-Ku, Sendai 980-8577, Japan. Received December 9, 2017; Revised January 24, 2018; Accepted February 6, 2018 ABSTRACT In this study, the effect of nitrogen (N) doping and microstructural changes on the electrical and thermal properties of silicon carbide (SiC) were investigated. SiC powder was treated in a N2 atmosphere at 1673, 1973 and 2273 K for 3 h and subsequently sintered by spark plasma sintering (SPS) at 2373 K for 300 s in a vacuum or in a N2 atmosphere. The a-axis of the N2-treated SiC powders was almost constant, while the c-axis slightly decreased with an increase in the temperature of N2 treatment. The relative density of the SiC powder sintered body decreased from 72% to 60% with an increase in the temperature of N2 treatment. The increase in temperature of N2 treatment caused a decrease in the thermal and electrical conductivities of the SiC. Upon N2 treatment at 3 −1 1673 K and sintering in a N2 atmosphere, SiC exhibited a high electrical conductivity of 1.5 × 10 S m at 1123 K. SiC exhibited n-type conduction, and the highest Seebeck coefficient was −310 μV K−1 at 1073 K. KEY WORDS silicon carbide, nitrogen doping, electrical conductivity, thermal conductivity 1 Introduction doping of N onto a SiC sintered body has not been investigated. Silicon carbide (SiC) has been widely used as a heating element Spark plasma sintering (SPS) would enable the densification of the owing to its high electrical conductivity, high thermal conductivity SiC in a N2 atmosphere without sintering aids. and excellent refractory properties1,2). The electrical and thermal SiC powder manufactured via the Acheson method is n-type conductivities of SiC can be controlled by doping it with various owing to unintentional doping of N from the ambient atmosphere elements2-4). Nitrogen (N) is a common dopant for producing n-type during the production process25,26). Intentional N-doping onto the SiC semiconductors. To produce a highly conductive electronic heater, SiC source powder would be more uniform and effective than 3) high N-doping is required . Many researchers have investigated doping while sintering. The treatment of SiC powder in a N2 the growth of SiC crystals by chemical vapor deposition with the atmosphere before consolidation has not been reported. In this 5-8) addition of N source gas . The carrier concentration (N content) paper, SiC powder was treated in a N2 atmosphere and consolidated 16 19 −3 of 10 –10 cm can be controlled by changing the Si/C ratio, by SPS. Then, the optimized condition of N2 treatment temperature nitrogen flow rate, nitrogen pressure and temperature5-8). to obtained high electrical and thermal properties of the N-doped Nitrogen has been doped in bulk SiC sintered bodies by adding SiC bodies was elucidated. 9-21) nitrides, such as YN, Si3N4, BN, TiN and AlN . High electrical conductivities of ~105 S m−1 at room temperature have been reported13). 2 Experimental procedure The liquid-phase sintering of SiC with rare earth oxides encourages Commercial SiC powder (α-type, 6H, OY-15, Yakushima Denko the incorporation of N into the SiC lattice19-21). However, a SiC Co., Ltd, Tokyo, Japan) with an average particle size of 0.84 μm body containing a liquid phase and/or second phases may degrade was used as the source material. SiC powder was treated in N2 at its mechanical properties at high temperature. Although the sintering 1673, 1973 and 2273 K for 3 h at 0.1 MPa. The SiC powder was of SiC in N2 enhances the electrical conductivity, the densification poured into a graphite die (inner diameter of 10 mm) and sintered using of SiC in a N2 atmosphere without sintering aids is difficult. N SPS equipment (SPS-210LX, Fuji Electronic Industrial, Kawasaki, atoms would dissolve in a SiC lattice and suppress the diffusion of Japan) at 2373 K for 300 s. The heating rate was 100 K min−1 with Si and C22-24). B and AlN are often added as sintering aids for SiC, a pressure of 50 MPa. The sintering was performed in a vacuum 3) while B and Al are p-type dopants . Therefore, the effect of solely or N2 atmosphere. The density of the SiC bodies was measured via the Archimedes method. The relative density was calculated using * Corresponding author, E-mail: [email protected] −3 ** The content of this article had been presented at JSPMIC2017. the theoretical density of SiC (3.21 Mg m ). The crystal phases 「粉体および粉末冶金」第 65 巻第 8 号 Electrical and Thermal Properties of Nitrogen-Doped SiC Sintered Body 509 and lattice parameters were examined by X-ray diffraction (CuKα, 0.077 and 0.111 nm, respectively23). The substitution of the N atom Ultima IV, Rigaku Corp., Tokyo, Japan) using a high-purity mostly occurs at the C site in the SiC lattice29). The small size of silicon powder as the internal standard. The microstructure was the N atom substitution causes a decrease in the lattice parameter observed using a scanning electron microscope (SEM; S-3400N, of SiC. The effect of N incorporation on the lattice parameter of Hitachi High-Technologies Corp., Tokyo, Japan). The electrical 3C (cubic)-SiC has been reported23,29). An increase in the N content conductivity (σ) was measured using the DC four probe method in resulted in a decrease in the lattice constant of 3C-SiC29). The vacuum at 298–1123 K. The Seebeck coefficient (S) was measured annealing of 3C-SiC in a N2 atmosphere at 1873–2073 K caused in a He atmosphere at 298–973 K by changing the temperature a decrease in the lattice parameter, while it was almost constant at gradient (ZEM-3, ULVACRIKO, Kanagawa, Japan). The thermal 2073–2173 K23). This suggests that the N content in SiC may be conductivity (κ) was measured via the laser flash method (TC-7000, close to the solubility limit. The N-doping in 6H (hexagonal)-SiC ULVAC-RIKO, Kanagawa, Japan) in a vacuum at 298–973 K. led to a decrease in the a-axis, while it caused an increase in the c-axis30). The N atom has been assumed to interstitially dissolve in 3 Results and discussion the hexagonal layer of 6H-SiC, thus elongating the c-axis30). Fig. 1 shows the images of the untreated SiC powder and N2- Fig. 3 shows the effect of an increase in the temperature of treated SiC powder at different temperatures. The untreated SiC N2 treatment of SiC powder on the relative density of the SiC body powder had a yellow-green color. After N2 treatment, the color of sintered at 2373 K for 300 s. The relative densities of the untreated the SiC powder changed from grey to dark green with an increase SiC sintered in a vacuum and N2 atmosphere were 81.6% and 72.6%, 27,28) in temperature, thus suggesting that N-doping in SiC occurred . respectively. This result implies that sintering in a N2 atmosphere Pochaczka et al.22) reported that the N content adsorbed in SiC tends retarded the densification of the SiC body. The relative density of to increase with an increase in N2 partial pressure and temperature. the N2-treated SiC specimens sintered in a vacuum also exhibited Fig. 2 shows the SEM images of the untreated SiC powder and higher values than those sintered in a N2 atmosphere. However, N2-treated SiC powder at different temperatures. The untreated relative densities of N2-treated SiC specimens sintered in a vacuum SiC had an average particle size of 0.84 μm. The N2-treated SiC and in a N2 atmosphere decreased from 71.5% to 59.9% and powder at 1673 K exhibited a slightly larger particle size that of from 69.7% to 59.6%, respectively, with an increase in the the untreated SiC powder. The particle size of the SiC powder increased with an increase in temperature. The average particle sizes of the SiC powders were 0.96 and 2.24 μm at 1973 and 2273 K, respectively. The crystal phase of the N2-treated powders was identified as 6H-SiC (ICSD #01-072-0018). The a-axis of the N2-treated powder was constant for all powders (a = 0.3090 nm), while the c-axis of the N2-treated SiC powder at 1973 and 2273 K (c = 1.5118– 1.5119) was slightly lower than that of the untreated powder (c = 1.5121 nm). The covalent atomic radii of N, C and Si are 0.075, Fig. 1 Pictures of (a) the untreated SiC powder, and N2-treated SiC powders Fig. 3 Effect of the temperature of the N2-treated SiC powder on the at (b) 1673 K, (c) 1973 K and (d) 2273 K. relative density of SiC bodies sintered at 2373 K for 300 s. Fig. 2 SEM images of (a) untreated SiC powder and N2-treated SiC powders at (b) 1673 K, (c) 1973 K and (d) 2273 K. 2018 年 8 月 510 Yukina TAKI, Mettaya KITIWAN, Hirokazu KATSUI and Takashi GOTO temperature of N2 treatment. The microstructures of the surface of those of specimens sintered in a vacuum. the SiC bodies are shown in Fig. 4. The SiC bodies had a porous Fig. 6 shows the temperature dependence of the electrical microstructure corresponding to the relative density.
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