In-situ synthesis of nanocrystalline TiC powders, nanorods, and nanosheets in molten salt by disproportionation reaction of Ti(II) species

doi:10.1016/j.jmst.2019.08.017

Abstract

Abstract:

A high-efficiency method is developed to in-situ synthesize nanocrystalline TiC powders, nanorods, and nanosheets by using equimolar ratio of Ti powder and acetylene black, multiwalled carbon nanotubes (MWCNTs), and graphene, respectively, as precursor in eutectic NaCl-KCl molten salt at 800-900 °C for 2-3 h. Higher temperature and longer duration are more beneficial for TiC preparation. In addition, mechanism of TiC formation was investigated by linear scan voltammetry. Results indicate that nanocrystalline TiC is in-situ synthesized by reaction between Ti atoms, which come from disproportionation reaction of Ti(II) species in the molten salt, and C atoms on the surface of carbon sources.

Key words: Titanium carbide, Nanocrystalline, Nanorod, Nanosheet, Disproportionation, Molten salt

Lingxu Yang, Ying Wang, Ruijia Liu, Huijun Liu, Xue Zhang, Chaoliu Zeng, Chao Fu. In-situ synthesis of nanocrystalline TiC powders, nanorods, and nanosheets in molten salt by disproportionation reaction of Ti(II) species[J]. J. Mater. Sci. Technol., 2020, 37: 173-180.

Figures/Tables 9

Fig. 1. XRD patterns of samples obtained by using equimolar ratio of Ti powder and acetylene black as precursors in NaCl-KCl molten salt at different temperatures for 2?h.

Fig. 2. XRD patterns of samples obtained by using equimolar ratio of Ti powder and acetylene black as precursors in NaCl-KCl molten salt at 800?°C for different times.

Fig. 3. (a, b) FE-SEM images of the sample obtained by using equimolar ratio of Ti powder and acetylene black as precursors in NaCl-KCl molten salt at 850?°C for 2?h; the inset shows a statistical particle size distribution in Fig. 3(b); (c, d) the corresponding elemental mappings of titanium and carbon of area A in Fig. 3(a).

Fig. 4. (a) TEM image and (b) the corresponding SAED pattern of TiC powder obtained by using equimolar ratio of Ti and acetylene black in NaCl-KCl molten salt at 850?°C for 2?h; (c) TEM image of a single TiC nanocrystalline and (d) HRTEM image of area A in Fig. 4(c).

Fig. 5. LSV curves of a molybdenum electrode (S?=?0.163 cm2) in NaCl-KCl molten salt without and with 0.1?mol L-1 Ti powder at 800?°C for different times at scan rate of 300?mV s-1.

Fig. 6. LSV curves (a) of a molybdenum electrode (S?=?0.163 cm2) in NaCl-KCl molten salt containing 0.1?mol L-1 Ti powder at different scan rates after Ti powder was added for 1?h at 800?°C; (b) the relationship between cathodic peak potential and logarithm of scan rate.

Fig. 7. Schematic diagram of TiC formation in NaCl-KCl molten salt by using equimolar ratio of Ti powder and acetylene black as precursors.

Fig. 8. (a) XRD diffractogram and (b, c, d) TEM images of TiC nanorods prepared by using equimolar ratio of Ti powder and MWCNTs as precursors in NaCl-KCl molten salt at 850?°C for 2?h; (e, f) HRTEM images of TiC nanoparticle; the inset shows the corresponding SAED pattern of area A in Fig. 8(e).

Fig. 9. (a) XRD diffractogram and (b) SEM image of TiC nanosheets prepared by using equimolar ratio of Ti powder and graphene as precursors in NaCl-KCl molten salt at 850?°C for 2?h; (c) TEM image of an individual TiC nanosheet; (d) high magnification TEM image of area A in Fig. 9(c); the inset shows the corresponding SAED pattern; (e) and (f) HRTEM images of a TiC nanocrystalline; the inset shows the corresponding SAED pattern of area B in Fig. 9(e).

References

[1]	D.J. Ham, J.S. Lee, Energies 2 (2009) 873-899.
[2]	Y. Liu, T.G. Kelly, J.G. Chen, W.E. Mustain, ACS Catal. 3(2013) 1184-1194.
[3]	Z. Fu, R. Koc, Ceram. Int. 43(2017) 17233-17237.
[4]	P. Ettmayer, H. Kolaska, W. Lengauer, K. Dreyer, Int. J. Refract. Met. Hard Mater. 13(1995) 343-351.
[5]	J. Fan, Y. Yang, D. Tang, W. Xiao, X. Mao, D. Wang, J. Electrochem. Soc. 164(2017) E144-E150.
[6]	D.E. Grove, U. Gupta, A.W. Castleman, ACS Nano 4 (2010) 49-54.
[7]	L. Zhang, J. Hu, A.A. Voevodin, H. Fong, Nanoscale 2 (2010) 1670-1673.
[8]	Q. Dong, M. Huang, C. Guo, G. Yu, M. Wu, Int. J. Hydrogen Energy 42 (2017) 3206-3214.
[9]	Y. Ou, X. Cui, X. Zhang, Z. Jiang, J. Power Sources 195 (2010) 1365-1369.
[10]	Y. Zhao, Y. Wang, X. Cheng, L. Dong, Y. Zhang, J. Zang, Carbon 67 (2014) 409-416.
[11]	B.L. Yan, W.W. Meng, Y.J. Xu, J. Alloys Comp. 763(2018) 867-874.
[12]	S.J. Stott, R.J. Mortimer, S.E. Dann, M. Oyama, F. Marken, Phys. Chem. Chem. Phys. 8(2006) 5437-5443.
[13]	M. Krasnowski, T. Kulik, Intermetallics 15 (2007) 1377-1383.
[14]	H. Yang, T. Gao, H. Zhang, J. Nie, X. Liu, J. Mater. Sci. Technol. 35(2019) 374-382.
[15]	D. Zhou, F. Qiu, Q. Jiang, Mater. Sci. Eng. A 622 (2015) 189-193.
[16]	X. Yuan, L. Cheng, L. Kong, X. Yin, L. Zhang, J. Alloys. Compd. 596(2014) 132-139.
[17]	T. Yu, Y. Deng, L. Wang, R. Liu, L. Zhang, B. Tu, D. Zhao, Adv. Mater. 19(2007) 2301-2306.
[18]	X. Tao, J. Du, Y. Yang, Y. Li, Y. Xia, Y. Gan, H. Huang, W. Zhang, X. Li, Cryst. Growth Des. 11(2011) 4422-4426.
[19]	C.H. Liang, G.W. Meng, W. Chen, Y.W. Wang, L.D. Zhang, J. Cryst. Growth 220 (2000) 296-300.
[20]	D.W. Kim, U.S. Heo, K.S. Kim, D.W. Park, Curr. Appl. Phys. 18(2018) 551-558.
[21]	X. Wang, M. Lu, L. Qiu, H. Huang, D. Li, H. Wang, Y.B. Cheng, Ceram. Int. 42(2016) 122-131.
[22]	R. Cao, C. Liu, Z. Wu, J. Pan, J. Mater. Sci. Technol. 27(2011) 1006-1010.
[23]	Y.C. Woo, H.J. Kang, D.J. Kim, J. Eur. Ceram. Soc. 27(2007) 719-722.
[24]	W. Sen, B. Xu, B. Yang, H. Sun, J. Song, H. Wan, Y. Dai, Trans. Nonferrous Met. Soc. China 21 (2011) 185-190.
[25]	B. Ghosh, S.K. Pradhan, Mater. Chem. Phys. 120(2010) 537-545.
[26]	H. Jia, Z. Zhang, Z. Qi, G. Liu, X. Bian, J. Alloys. Compd. 472(2009) 97-103.
[27]	J.E. Oghenevweta, D. Wexler, A. Calka, Scr. Mater. 122(2016) 93-97.
[28]	B.H. Lohse, A. Calka, D. Wexler, J. Alloys. Compd. 394(2005) 148-151.
[29]	S.K. Mishra, S. Das, R.P. Goel, P. Ramachandrarao, J. Mater. Sci. Lett. 16(1997) 965-967.
[30]	D.W. Lee, S.V. Alexandrovskii, B.K. Kim, Mater. Lett. 58(2004) 1471-1474.
[31]	J. Ma, M. Wu, Y. Du, S. Chen, G. Li, J. Hu, Mater. Sci. Eng. B 153 (2008) 96-99.
[32]	J. Pan, R. Cao, Y. Yuan, Mater. Lett. 60(2006) 626-629.
[33]	A.K. Khanra, L.C. Pathak, M.M. Godkhindi, J. Mater. Process. Technol. 202(2008) 386-390.
[34]	S. Sivasankaran, M.J. Kishor Kumar, Ceram. Int. 41(2015) 11301-11305.
[35]	M.B. Rahaei, R.Y. Rad, A. Kazemzadeh, T. Ebadzadeh, Powder Technol. 217(2012) 369-376.
[36]	H. Wang, W. Zhu, Y. Liu, L. Zeng, L. Sun, Materials 9 (2016) 1-7.
[37]	L. Tong, R.G. Reddy, Scr. Mater. 52(2005) 1253-1258.
[38]	A. Kikuchihara, F. Sakurai, T. Kimura, J. Am. Ceram. Soc. 95(2012) 1556-1562.
[39]	Q. Song, Q. Xu, L. Xu, Z. Ning, T. Lou, H. Xie, Y. Qi, K. Yu, J. Alloys. Compd. 690(2017) 116-122.
[40]	P. Xue, H. Wu, Y. Lu, X. Zhu, J. Mater. Sci. Technol. 34(2018) 914-930.
[41]	Y. Wang, J. Ma, J. Tao, X. Zhu, J. Zhou, Z. Zhao, L. Xie, H. Tian, Mater. Lett. 60(2006) 291-293.
[42]	A.M. Abdelkader, J. Eur. Ceram. Soc. 36(2016) 33-42.
[43]	X. Li, Z. Dong, A. Westwood, A. Brown, R. Brydson, A. Walton, G. Yuan, Z. Cui, Y. Cong, Cryst. Growth Des. 11(2011) 3122-3129.
[44]	X. Li, Z. Dong, A. Westwood, A. Brown, S. Zhang, R. Brydson, N. Li, B. Rand, Carbon 46 (2008) 305-309.
[45]	J. Song, X. Huang, J. Wu, X. Zhang, Electrochim. Acta 256 (2017) 252-258.
[46]	B.L. Yan, Y.D. Yan, M.L. Zhang, W.W. Meng, J. Electrochem. Soc. 163(2016) E104-E109.
[47]	J. Song, Q. Wang, G. Hu, X. Zhu, S. Jiao, H. Zhu, Int. J. Miner. Metall. Mater. 21(2014) 660-665.
[48]	W.C. Kreye, H.H. Kellogg, J. Electrochem. Soc. 104(1957) 504-508.
[49]	M.E. Straumanis, S.T. Shih, A.W. Schlechten, J. Electrochem. Soc. 104(1957) 17-20.
[50]	J. Li, W. Pan, Z. Yuan, Y. Chen, Appl. Surf. Sci. 254(2008) 4584-4590.