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首页> 外文会议>International Symposium on Metastable and Nano-Materials(ISMANAM-2005); 20050703-07; Paris(FR) >Raman spectroscopy sheds new light on TiC formation during the controlled milling of titanium and carbon
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Raman spectroscopy sheds new light on TiC formation during the controlled milling of titanium and carbon

机译：拉曼光谱学为钛和碳的受控研磨过程中的TiC形成提供了新的思路

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摘要

A magneto ball mill was used to mill titanium and carbon elemental powder mixtures with compositions of To_(50)C_(50) and Ti_(60)C_(40) under a helium atmosphere. Previous studies on the milling of titanium and carbon powder mixtures have reported a sudden increase in the temperature of the milling vial, which occurs after a specific milling interval, referred to as t_(ig) [Z.G. Liu, J.T. Guo, L.L. Ye, G.S. Li, Z.Q. Hu, Appl. Phys. Lett. 65 (1994) 2666-2668; G.B. Schaffer, J.S. Forrester, J. Mater. Sci. 32 (1997) 3157-3162; N.Q. Wu, S. Lin, J.M. Wu, Z.Z. Li, Mater. Sci. Technol. 14 (1998) 287-291; Z. Xinkun, Z. Kunyu, C. Baochang, L. Qiushi, Z. Xiuqin, C. Tieli, S. Yunsheng, Mater. Sci. Eng. C 16 (2001) 103-105; C. Deidda, S. Doppiu, M. Monagheddu, G. Cocco, J. Metastable Nanocryst. Mater. 15/16 (2003) 215-220]. This sudden temperature increase has been found to correspond to the formation of TiC via a rapid, highly exothermic reaction. In these cases, XRD analysis did not detect TiC in powder sampled before t_(ig). These results, combined with those from studies suggested that the milling period prior to t_(ig) represents an incubation period during which the powders become mechanically activated and that no reaction between the starting powders occurs during this time [L. Takacs, J. Solid State Chem. 125 (1996) 75-84; B.K. Yen, T. Aizawa, J. Kihara, J. Am. Ceram. Soc. 81 (1998) 1953-1956; M. Puttaswamy, Y. Chen, B. Jar, J.S. Williams, Mater. Sci. Forum 312-314 (1999) 79-84; G.B. Schaffer, P.G. McCormick, Metall. Transact. A 23A (1992) 1285-1290; M. Mingliang, L. Xinkuan, X. Shenqui, C. Donglang, Z. Jingen, J. Mater. Process. Technol. 116 (2001) 124-127].In the current investigation a sudden increase in the temperature of the milling vial was also observed after a specific milling duration of t_(ig). XRD analysis of powder sampled before t_(ig) did not detect TiC, whilst for powder sampled after t_(ig), XRD analysis indicated that the powder had almost completely transformed into TiC. However, Raman spectroscopy showed the formation of non-stoichiometric TiC in Ti_(50)C_(50) and Ti_(60)C_(40) powders sampled before t_(ig). It is believed that the current, and many previous XRD analyses did not detect the formation of TiC prior to t_(ig) either because the TiC grain size was too small and/or the phase represented too small a volume fraction of the powder samples to be detected by the XRD method employed. These Raman spectroscopy results suggest that a significant component of the heat generated at t_(ig) may be due to a combination of growth of TiC accompanied by consumption of unreacted Ti and carbon, and/or recrystallisation of the TiC formed prior to t_(ig), rather than the direct formation of TiC.
机译：使用电磁球磨机在氦气气氛下研磨具有To_（50）C_（50）和Ti_（60）C_（40）组成的钛和碳元素粉末混合物。以前关于研磨钛和碳粉混合物的研究已经报告了研磨瓶温度的突然升高，这是在特定的研磨间隔后发生的，称为t_（ig）[Z.G.刘建堂郭L.L.叶G.S.李ZQ胡，应用物理来吧65（1994）2666-2668; G.B. Schaffer，J.S. Forrester，J。Mater。科学32（1997）3157-3162; N.Q. Wu，S. Lin，J.M. Wu，Z.Z.李母科学技术。 14（1998）287-291; Z. Xinkun，Z. Kunyu，C.Baochang，L.Quushi，Z.Xiuqin，C.Tieli，S.Yunsheng，Mater。科学。 C 16（2001）103-105; C.Deidda，S.Doppiu，M.Monagheddu，G.Cocco，J。亚稳纳米晶体。母校15/16（2003）215-220]。已经发现这种突然的温度升高对应于通过快速，高度放热反应形成的TiC。在这些情况下，XRD分析未检测到t_（ig）之前采样的粉末中的TiC。这些结果与研究结果相结合，表明t_（ig）之前的研磨时间代表了一个粉末被机械活化的孵育期，并且在此期间起始粉末之间没有任何反应发生[L.]。 Takacs，J。固态化学。 125（1996）75-84; B.K.日元，T。Aizawa，J。Kihara，J。Am。陶瓷Soc。 81（1998）1953-1956; M.Puttaswamy，Y.Chen，B.Jar，J.S。威廉姆斯，马特。科学论坛312-314（1999）79-84; G.B.沙弗尔P.G. Metall的McCormick。办理。 A 23A（1992）1285-1290； M. Mingliang，L。Xinkuan，X。Shenqui，C。Donglang，Z。Jingen，J。Mater。处理。技术。 116（2001）124-127]。在目前的研究中，在特定的研磨时间t_（ig）之后，还观察到研磨瓶的温度突然升高。 t_（ig）之前采样的粉末的XRD分析未检测到TiC，而t_（ig）之后采样的粉末的XRD分析表明，粉末几乎完全转化为TiC。然而，拉曼光谱显示在t_（ig）之前取样的Ti_（50）C_（50）和Ti_（60）C_（40）粉末中形成了非化学计量的TiC。可以认为，当前和许多以前的XRD分析都未检测到t_（ig）之前形成TiC，或者是因为TiC晶粒尺寸太小和/或相代表粉末样品的体积分数太小而无法通过采用的XRD方法进行检测。这些拉曼光谱结果表明，t_（ig）处产生的热量的很大一部分可能是由于TiC的生长伴随着未反应的Ti和碳的消耗和/或t_（ig）之前形成的TiC的重结晶的综合作用。 ），而不是直接形成TiC。

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