Formula 2 after 1200 ℃ heat for 10 minutes and 1300 ℃ heat for 10 minutes and formula 1 through 1200 ℃ respectively, 1300 ℃ and 1400 ℃ were heat preservation after 10 minutes of microwave heating synthesis, using X-ray diffraction (XRD) for phase analysis test, the XRD curve as shown in figure 1.
It is seen from Figure 1 (a) chart, formula 2 # after 1200 ℃ 10 minutes of microwave synthesis, the reaction proceeds more completely, basically been Ti (Cx, N1-x) single-phase solid solution.From this point the two peaks (111) and two networks (200) plane of view from the d values were 2.475 and 2.144, just in the PDF card single-phase TiN surface corresponding to the surface mesh network from the d value 2.44 and 2.12, and single-phase TiC corresponding surface mesh face net from close to the median value d 2.475 and 2.1495 between 2.51 and 2.179. It is estimated to be as Ti (C0.5, N0.5) close to form a solid solution when the temperature is raised to 1300 ℃ synthesis time, which can be seen the two characteristic peaks d values Ti (Cx, N1-x) Synthesis of solid solution becomes Small and respectively: 2.468 and 2.136, that is, to this end of TiN moved, indicating that other conditions remain unchanged and after the synthesis temperature increase, generating more TiN or partially converted to TiN and TiC solid solution.
Formulation 1 ” 1 (b), the 1200 ℃ x lOmin after microwave heating synthesis, there is generated Ti (Cx, N1-x) solid solution and the intermediate and transitional Ti3O5, &gamma -Ti3O5 curves at different temperatures XRD after synthesis is shown in ., the synthesis reaction is far from complete in which two characteristic peaks d value Ti (Cx, N1-x) solid solution, respectively: 2.463 and 2.131, apparently in a relatively close to the TiN end position improve after synthesis temperature to 1300 ℃, the middle of a transition phase and wherein the amount of reducing &gamma -Ti3O5 disappears, and a small amount of Ti3O5 becomes rutile TiO2 coexist, and the amount of Ti (Cx, N1-x) are significantly increased, d values corresponding characteristic peaks substantially no change, i.e., to maintain TiN and TiC the proportion of the previous solution synthesis temperature, indicating that the heating stage TiN and TiC generation amount or the amount of conversion of basic maintain balance. When again after the synthesis temperature to 1400 ℃, the intermediate phase disappears, got single phase Ti ( Cx, N1-x) of a solid solution. d values corresponding also come increased to 2.467 and 2.136 respectively, and to the direction of TiC end has been moved, the result becomes Formula 2 # after 1300 ℃ x lOmin synthesis of Ti ( Cx, N1-x) at substantially the same location solution that this heating process, generate more TiC or have turned into TiN TiC.
The results showed that: microwave carbothermal reduction can be synthesized Ti (Cx, N1-x) single-phase solid solution, synthesis conditions controlled, it can also be a solution in line with the proportion of solid solution requirements. However, after the synthesis temperature, recipe for reactivity large 2 ” solid solution TiN ratio increased, while the reactivity of small recipe 1″ on the contrary, that the amount of TiC improved.
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