Formation Mechanism of TaC by Tantalum-contained Resin Precursor
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1 » 22» 5 É Æ ½ Vol. 22, No Journal of Inorganic Materials Sep., 2007 : X(2007) Ų» À Ö TaC Þ Ð Ñ ( ÎÇ ÉÍ ÌÊË È ÆÏ ) û Ãʲµ± C/C-TaC ÉÆ²Ï Ø C/C ÉƱÎÔµ XRD SEM» Ã Đ ²Òµ± Õ ² Õ Ú Ã± DSC-TG º ÔßÄ TaC Ó±Í «Ú Ã Í ± ºÊ Í Ä ± º 100 C Đ º Ò Ã ± TaF 5 Ý TaO 2F. µ Ý Ø 800 C ÌÊ ±È TaO 2F Ý Ta 2O 5 TaF 5. ±² Ta 2O C Ò Ü ½½ßº Ø«< 1µm ± TaC «º² ± ² Ò Đ ( 100 C) ( C) ¾ «Ú TaC; Í µ TB332 ½Ð A Formation Mechanism of TaC by Tantalum-contained Resin Precursor LI Jiang-Hong, ZHANG Hong-Bo, XIONG Xiang, XIAO Peng, ZHAO Lei, HUANG Bai-Yun (The State Key Laboratory for Powder Metallurgy, Central South University, Changsha , China) Abstract: C/C-TaC composites prepared by liquid precursors are promising in improving the ablation properties of C/C composites. The formation mechanism of TaC by tantalum-contained resin precursor was investigated through the analysis of components and morphologies of tantalum-contained resin after different heat treatment by XRD and SEM together with the DSC-TG results of tantalum-contained solution. The results show that tantalum-contained solution promotes the solidification of resin. Treated at 100 C, TaF 5 will hydrolyze into TaO 2 F and the resin will solidify. Treated at 800 C in vacuum atmosphere, part of TaO 2 F in tantalum-contained resin will decompose into Ta 2 O 5 solid and TaF 5 gas. Then, Ta 2 O 5 will be reduced and compounded by carbon into TaC with fine sizes at 1000 C. The loss of tantalum can be controlled by prolonging treatment time at lower temperatures (room temperature 100 C) and introducing anhydrous ammonia into the solution. Key words: tantalum-contained resin; TaC; formation mechanism 1 C/C Ñ ËÈ Ð³ Ù ÏÕ ¹ à ²³ Í Ò ² à ¹ÝÁËÙ²Ù ËÈ Ê Ò È (SRM) [1]. ²ÁÍ Ù Ç Ë² Æ Ù Æ SRM ²Ý È C/C Ñ ËÈ ÏÕ , Û Đ ¾ 973 ¾ Ð Ç Ð (2006CB600908) Á «Æ (1975 ), «Ð LJH138@mail.csu.edu.cn ÝÅÛÙ² ¹ C/C Ñ ËȲÏÕ ÈÆÊÐ É ² TaC ÐÙ (3880 C) Ù Ù» Õ Ú Ä² Ù Þ TaC ËȲ ÆË ²Á Ð C Ï ÖÆ Ð ² ÏÕ [2]. Ñ Â Ë
2 974 É Æ ½ 22 Å Ý C/C Ñ ËȺ TaC ZrC SiC HfC»» Ó Ù C/C Ñ ËȲ» ¹ÏÕ ÕÅÛÙ² Û ²ÝÎÓ Û Ð Æ½½ C/C Ñ ËÈ Û ² ÏÕËÈ [3]. Choury Ý [4], ³ ÕÅ 3700 C Í Ë ² ËÈ ¹»»Ó C/C Ñ ËȺ C/C Ñ ËȺ TaC Ð ½ Ë Æ½ Í Æ Ðܳ ÅÔ³ Æ Ù» TaC, ½ Ë µè IJ TaC ÐÐÒ Å º [5]. Ìƽ Ë» Æ (CVD)» Æ Î (CVR) ³ TaC à [6 8], ½³ à ² Ë Ã ËȲӻ Æ Ý Ã Ä² л Æ TaC ²Ð¼ Ò Ù ¼ ½ Ë Í ÄË TaC C/C Ñ ËȺ Ò Ò»»» ²Ô C/C Ñ ËÈ²Ô Æ Ò Í À² Ó Ë Í Ð ÉÝ ËÈ Ü ß Áº Ð ÊÄ ËȲÏÕ [9,10] ² TaC ZrC»»Ó Ò ºÅÔ C/C Ë È Ø Ó Å Î ÏÕËȲ Î Æ [11,12] Í ÄË C/C Ñ ËȺ»» Ó (ZrC HfC TaC WC), ÙË È Ï Õ ² «Ü TaC ² ³ ÝÏ ÍÐ ÆÆ ¼ É ³Åƽ¾ÄÆ ÄË Ä Ä Ò ² Å Ä ³ ² C/C-TaC ËȺ TaC ²Ò Å [13,14] È ÆÔº È Ð TaC Ý º Ó» Ta 2 O 5. ÆÔº Ä ² ٠л Íû Ð Ta 2 O 5 Ë»¹ C ¾ Ð TaC ² ³ Ù ¼ Æ Ä ³ ²Ð Û Ä ² DSC-TG ² Ö Õ Å Ä ÆÔº ȲÆÙÉ» Î ÝÅÍ Ó Ð Æ ß Ù TaC ²» ² ² 2 Ø 2.1 Ò HF Ä ÅÛ»Ý ² Ö ÂÄ Ò 40%, GB Ta Á Å Ð ß ² Æ FTa-1, 100µm.»ÝÐ ß Æ Â ² Ta Ð HF Ä ² È ºÒÐ ²Ô 80 C Û ÆÔºÈ Ta Þ Ó³ Ý Î ËÐ³È È Ë«Ð Â ß Ë Ä Æ ³ ² Ä ÍÆ ½ ÆÐ Ò Õ º ³ C ² 1400 C Ó² CVI(» Æ ) 20 C/min. 100 C Ñ 1 Âñ Ý Ð Table 1 Properties of furan resin ÓÍ ³Ý ² ˾» ³ Ä Ý C ² ÊÄ Ô» ÐÐÄ 2.3 ÅÔ º Í SDTQ600 Æ ÖÇ C Ä ³ DSC-TG Ö 20 C/min, Í Ë¾³ È Ð Ä² Á Ð Â Ó 3014 X Å Ç (XRD) Î Ë ²  ßÍà «Ä ³ ² Ó Ã«1400 CDSC-TG Ö ³ ²ÏÎÓ ³ ÓÆ Ö JSM-5600L Ø Ë Ó ³ SEM Brand Furfuralcohol modified urea-formaldebyde Free formaldebyde/wt% Solid content/wt% Nitrogen content/wt% Viscosity(25 C) η/pa s
3 5» TaC ± Ó Ð¹ 3.1 Ä Ù Õß ß Â ± Ô Á 1, Á 2. Â É ÀÞ Â 500 C ± XRD Á Á 1(a), Á 1(a) ±Ë Û Ñ«TaO 2 F, ± à ŠÀÞ SEM (Á 2(a)) Ù ÅĐ < 1µm Ú È ± Ö ĐÓÅ Ú Ä Å Å± Ñ Ta Ñ HF TaF 5 ( Ì (1)) Á Æ Ü Ã ÃĐÓÅ Â TaO 2 F(Ì (2)). Á 1(a) TaO 2 F à ٠À Ü TaO 2 F ¹Ò SEM Á 2(b) 2(c) Ú Ù Đ ÖÃ Ú TaO 2 F ¹Ò Ñ ¼ Æ TaO 2 F Å Ã ĐÅ C ± XRD Á Á 1(b). 700 C ± Ñ««TaO 2 F È Á Ta 2 O 5. SEM (Á 2(a)) Đ Þ À Ñ Ð Ta 2 O [14] 5. Ù Ö C XRD ÔÙ ± «Ta 2 O 5 TaO 2 F ýŠ900 C ± TaO 2 F É ½Ç Ta 2 O 5. [15] Ð C TaO 2 F Ô ËÝ (3) ÝÝÌ Ñ Ã 700 C ËÉ TaO 2 F Ô ±ËÌ (4) ÝÝËÑ» ±Åº Ñ ÂÔ Á Ò µô Á Å Ë Ì (3) Ô (4) Æ 700 C ѱ Æ É TaO 2 F ÜÌ Æ Å Á 1(c) 1000 C ± XRD Á ÙÇ Ta 2 O 5 Ô C Æ ¼ Þ - ¹ Ì Ã TaC Ý (5), ¼ Ì Ì (5) Ý 1109 C [13], Ѻ Æ Ta 2 O 5 ¼ Ö «Ñ Ë Ì (5) Æ Ñ Â ËÎÓ Ç Ì ¹ Ta 2 O 5. Á 1(d)1400 C ± XRD Á Ù Ta 2 O 5 É½Ç Ã TaC. SEM (Á 2(e)) Ñ Ù Đ À«¼ Ô ¼¹ÑÏ Å (Á 2(f)) Æ TaC Ú Å <1µm.  1 Ã Đ ² ± XRD  Fig. 1 XRD patterns of tantalum-contained resin after heat-treated at various temperatures
4 976 É Æ ½ 22  2 Ã Đ ² ± SEM Fig. 2 SEM morphologies of tantalum-contained resin heat-treated at various temperatures (a) Without heat-treatment; (b) 300 C; (c) 500 C; (d) 700 C; (e),(f) 1400 C 2Ta+10HF 2TaF 5 +5H 2 (G) (1) TaF 5 +2H 2 O TaO 2 F+4HF(G) (2) 2TaO 2 F+H 2 O Ta 2 O 5 +HF(G) (3) 6TaO 2 F+H 2 O 3Ta 2 O 5 +6HF(G) (4) Ta 2 O 5 (s)+7c(s) 2TaC(s)+5CO(g) (5) Ô 1400 C CVI ¼ ±ÃÑ«ÔÔ Ù Á 3(a) 3(b). Á 3(a) Ù CVI ¼Ö TaC ÅÁ 3(b) SEM Æ TaC Ë À À Ä Ô TaC (Á 2(f)) Å«±Æ ± Å ÅÉ±Æ Ñ TaF 5 ż Ð TaF 5 Â Ì Ð¹É Ì Đ Ð¹ 100 C й й± Ta Ë TaO 2 F Ñ Å Ñ 500 C TaO 2 F Æ ¹Ô 500 C ËÉ Ü TaO 2 F Ü Ta 2 O 5, 700 C ËÉ ÜÌ» Æ ± λ Ta 2 O 5 Ô C ¼Þ¹ TaC. Ã Ò Æ ¼¹ Û H 2 H 2 O CO ³ ÂÅ 1400 C Ñ¼Æ Ç Æ Æ Ô ¼Ì à TaC. 3.2 Ä Ü DSC-TG ß Ó Þ É Ò ³  C Ï Ü ± DSC-TG Ô Â DSC-TG ±Ñ Ô ±Ã XRD ÔÔ SEM Å Á 4  DSC-TG ÔÙ Å Á 4 ±Ë  3 Õ 1400 C Đ CVI º± XRD Â Õ SEM Fig. 3 XRD pattern (a) and SEM morphology (b) of CVI carbon at the same furnace with tantalumcontained resin heat-treated at 1400 C
5 5» TaC ± Ó 977  4 ñ DSC-TG ÕÚÅ Fig. 4 DSC-TG results of tantalum-contained solution from 0 to 1400 C Û Â TG ¹ ± AB BC CD DE EF 5 Ú Å Â ¾ Æ Ú ÅºÅ AB ( 240 C), ¾Æ 44.33%; Æ BC ( C), ¾ 6 %; ʱ DE ( C), ¾Æ 6.54%. Ü Ö Ù Ø Â ± Ô Â TG ¹ ÉÂ Ì ± ÔÅ B ( 240 C): Ñ Ñ ß À Ó HF Æ ± TaF 5 Ü Ì Ò (3) Ý Ì Ë HF ݳ 25.64% Á ÖÀ H 2 O ÆÅ Ñ DSC ¹ É±Æ Ø M. BC ( C): Ñ» (20 C/s), (Á 5(b)) Ô 700 C (Á 2(d)) À Ñ Ð Ç Ö¼± ÙĐ Å TaF 5 Û±ÍÜ Ì É ÙÅ É Ì Æ ±ËÜ ÉØ Ô 1400 C CVI ¼ TaC Å CTaO 2 F Ü TaF 5 Æ Æ TaF 5 Ç Æ TaO 2 F ØÒ CVI ¼É Ñ»Æ ÜÌ (2) (3) (3), λ Ta 2 O 5 Ô C Æ ¼Þ¹ Ì (5) Ú TaC. ¹± Â Ñ Æ³ ± ¹± BC DE ¾½Ö ÅBC ½ÂÂ Ü TaF 5 Æ Ë ³ ± AB ÞÙÇ Ñ TaF 5 Ê ½ ÜÅ DE ³ ± ( C) Ñ Ú TaO 2 F Ü Ta 2 O 5 Ã Õ TaO 2 F ÜÅ Ã TaF 5 ½ Ñ (229 C), Ë Á TaF 5 ½ÂÂ Ü ¹ Æ 6% ¾Ä Ü TaF 5 ÁÅ ½Â CD ( C): Ù Đ ¹ ¼ Ì Æ TaO 2 F Å DE ( C): Æ Ã 6% ¾Å [17] 500 C Ë É Ü TaO 2 F ± Ë TaF 5 ݳ Ç Å Ñ - ¾Ö Ï ± BC Æ Û Ë±Æ 800 C Ë ± TaO 2 F Æ Ã Ü ÜÌ Å 5TaO 2 F TaF 5 (G)+2Ta 2 O 5 (6) EF ( C): ÙĐ¹¼Ì Æ Å Á 5  DSC-TG ± XRD Á Ô SEM XRD Á (Á 5(a)) ÖÀ  1400 C ± ÀÑ Ta 2 O 5, Ô Â 5 à DSC-TG( C) ²± XRD  (a) Õ SEM (b) Fig. 5 XRD pattern (a) and SEM morphology (b) of tantalum-contained solution after DSC-TG test from 0 to 1400 C Ö ÔÌ (6) Ý Ñ«Åñ Ta 2 O 5
6 978 É Æ ½ 22 4 ³ TaF 5 ÂÌ Ð¹É Ì Ð¹± Ta Ë TaO 2 F Ñ Å Ñ 500 C TaO 2 F Æ ¹ Ãй Æ Ü¼¹Ì Å Ü µ Ñ Ñ ¼¹ º Æ Á Á TaO 2 F Æ Ý (3) (4) Ü Ì Å Ñ µô TaO 2 F ʽ Ü Ta 2 O 5, 800 C Ë É Ü ½ÂÂ Ü TaO 2 F Ü Ç Ta Ë TaF 5 ÆÅ 1000 C, ÜÔ Ü Ta 2 O 5 Ô C ¼ Þ ¹ TaC. Ñ Ü TaF 5 ¼ ( ¼ ¼Ô ¼) Ø Ò Æ ÜÌ Ã Ta 2 O 5, Ta 2 O 5 Ô C Î»Æ ¼Þ¹ Ì Ã TaC. ³ ¹± Ta Ë TaF 5 Ý Æű ËÜż ÉÖ Æ 1. ¹± 100 C Ë TaF 5 ٠ʽ Ü TaF 5 ʽ Ü Þ BC ¾Å 2. [19] Ð C Ú F Ô NH + 4 Ù NH 4F, Ã Õ Ë TaF 5 ³ Ô TaO 2 F Ü Ì Ta ³ Å Ã Ø ( C) Ñ Ú TaO 2 F Ü Ta 2 O 5 ù± ³ ÉÂÈ Ì Å Ñ ¼¹ ¼ à ¼Ô Æ Ì (7) à ¼ ³ Å 5 C+H 2 O(g) CO(g)+H 2 (g) (7) 1. TaF 5 ÂÌ Ð¹ É Ì Ð¹± Ta Ë TaO 2 F Ñ Å 2. µô TaO 2 F Ç Ü Ta 2 O 5, Ç Ü TaF 5 Ta 2 O 5. Ñ ¼¹ Ta 2 O 5 Ô C ¼Þ¹ TaC. Æ TaF 5 ¼ØÒ Æ ÜÂÔ C ¼Þ¹ Ì Ú TaC. 3. ± Ñ ( 100 C) ( C) ½¹± Ñ ³ Å Ó ¼ [1] Paulmier T, Balat-Pichelin M, Quéau D. Le. Applied Surface Science, 2005, 243: [2] Kim C, Gottstein G, Grummon D S. Acta Metallurgica et Materialia, 1994, 42 (7): [3] Ï Đ Ç 2001, 24 (1): [4] Choury J J. AIAA paper, [5] Û Ç Ð ÊǾ± 2003, 20 (3): [6] Tsutsumoto T. Thin Solid Films, 1998, 317: [7] Rubinshtein A, Shneck R, Danon A, et al. Materials Science and Engineering, 2001, A302 (1): [8] Teghil R, D Alessio L, Maria G D, et al. Applied Surface Science, 1995, 86: [9] Û µ ³ÜÀ ¾¾± 2000, 18 (4): [10] Û µ Đ Ç 2001, 24 (3): [11] Í Å Ï Ø ÊÇÜÎ 2001, 3 (6): [12] Í Å Û µ ¾ÊÇ 2005, 20 (2): [13] µ (YAN Zhi-Qiao, et al). ÊǾ± (Journal of Inorganic Materials), 2005, 20 (5): [14] µ ¹ ÁĐ«¾± 2005, 15 (10): [15] Ì Ï Í µ ÁĐ«1998, (2): [16] T H A.B.E, kop yhob B. µ µ Ö Ã ¹ ÜÀ ¾Ü [17] º µ (XIANG Hua, et al). ÊǾ± (Journal of Inorganic Materials), 2006, 21 (4): [18] Frevel L K, Rinn H W. Acta Cryst., 1956, 9: [19] Gibson J, Gibson M G. Production of carbon fibertantalum carbide composites. US
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