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The mechanical alloying (MA) as an effective method as a process for preparing new material has gained a wide range of applications, the use of this method can be obtained under normal conditions very difficult to synthesize some of the new materials with unique properties. Mechanical RCAs induced recombination reaction people have successfully prepared many new materials including refractory carbide. However, has been the focus of researchers focused on materials synthesis and performance improvement, and analysis of mechanical alloying process is not enough. This paper focuses on metal elements (graphite, Te) structural changes in the mechanical alloying process. Experiment with the raw materials such as Al, graphite, diamond, Te powder milling with a planetary mill, using X-ray diffraction, Raman spectroscopy, differential thermal analysis, scanning electron microscopy and other means to study different milling time, annealing and other factors of these materials in the milling process changes in the structure, synthesis phase structure and stability. Obtained through the analysis of the milled product, about a metal element graphite and diamond, and graphite, Te, respectively, and the metal elements Al, structural changes in the mechanical milling process innovations: (1) graphite - Diamond ball milling, to give the turbostratic structure of graphite. Milling process, with the milling time increased, the XRD diffraction peak of graphite gradually broadening to small diffraction angular movement. XRD patterns of discovery through the simulation of graphite diffraction peak is not moving to the small diffraction angle due to the increase of the lattice parameter, but due to the grain size effect. When graphite grain size of less than 6nm, the broadening of the diffraction peaks, moving more and more obvious to the small diffraction angle. Contrast milled sample was found in the XRD pattern after annealing at 1700 ℃ with turbostratic structure of graphite analog XRD pattern, the graphite to turbostratic structure appears in the milling process, and that this structure is very stable, even at a high temperature of 1700 ℃ annealing did not recover the original graphite crystal structure. Graphite milling process, a small amount of amorphization. (2) Graphite - diamond milling process, the diamond of the XRD peaks and not significantly stretch or peak position movement, the calculation that the diamond grain size is always in the range of 57-50nm. Diamond diffraction peak intensity indicates that diamond gradually weakened as the milling time increases, there exists a critical size effect, and when the grain size less than 50nm, the role of the milled grain is very easy amorphous. Diamond because of its high hardness, the milling process more act as a grinding agent to speed up the process of milling of graphite. (3) Graphite in after milling, although less than a graphite diffraction peak is observed in the XRD pattern, Raman spectrum, annealing experiments showed that graphite even in to diamond grinding agent, milled after 500 hours, still exists portion
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