Titanium Di-Boride Lab Report

Abstract Titanium Di-boride (TiB2) nano particle was prepared using sol-gel and carbothermal reduction method. The effect of temperature, solvent and precursor ratio on the synthesis of TiB2 was studied after the synthesis of TiB2. Earlier work which was done on to synthesize TiB2 via this process has given the optimum result at 15000C carbothermal reduction temp. and Titanium : boron : carbon precursor ratio should be 1 : 2 : 5 ; aim was/is to reduce the temp. of carbothermal reduction reaction and using low cost precursor for the source of boron(B) and carbon(C) and also to get nano size particle but previously via this process only 3-5µm particle range has been obtained. Here in this process firstly using precursor sol is prepared

The completion of the reaction can be judge by when a milky white colour solution is obtained or a thixotropic solution is obtained. Then the thixotropic solution is dried at an optimum temperature of 800C to 1200C at a drier for 2-3 hours. Then the dried product which is called “gel” is fired at 15000C by varying the rapid heating and cooling temperature of the reaction in a furnace in Ar or He atmosphere . Muffel furnace is used for this reaction with MoSi2 as heating element and graphite crucible is used for graphite high melting point (55300C at inert atmosphere). The samples which was obtained after firing was studied under XRD, ESEM, TEM and XPS to measure the phases present, crystal formation, crystalline phase and surface morphology of TiB2 and amount of TiB2 in the final product respectively. By the particle size distribution analyzer the particle size of the TiB2 was also

2 shows the XRD patterns of the product particles reacted from the mixture by carbothermal reduction with rapid heating and cooling at 15000C for various time under flowing argon atmosphere. In the figure, Ti3O5 peaks were observed with subsequent disappearance of TiO2 peaks, after firing for 3 min. And thereafter, Ti3O5 peaks rapidly disappeared and those due to TiC peaks emerged until 10 min, after the beginning of the firing. The TiB2 peaks were gradually appeared at temperature of 15000C for 15 min. The phases in the powder produced at 15000C for 15 min were TiB2 and TiC as determined by XRD technique. Finally, the formation of TiB2 was complete at 15000C for 20 min under flowing argon atmosphere. The present result shows that the carbothermal reduction of TiO2 to TiB2 proceeded through TiC as stated in Eqs. (2) and (3). Fig. 3 shows the morphology of the synthesized TiB2 particles formed by carbothermal