Study on preparation of Ti3AlC2 powder using sponge titanium as raw material
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摘要: 以海绵钛为钛源，海绵钛∶铝∶碳=3∶1.2∶1.8的比例混合，采用无压烧结的方法合成Ti3AlC2粉体。探讨保温温度在1000 ℃和1100 ℃下烧结产物结果，以及不同保温时间对试验结果的影响，同时在工艺上还采用了熔盐法探究掺杂NaCl或KCl对无压烧结制备Ti3AlC2的纯度的影响。试验结果表明，在氩气保护条件下，1100 ℃烧结出的产物纯度最好，采用熔盐法工艺中，掺杂盐所得产物中仍以1100 ℃的产物纯度最好，并且掺杂
$ \text{NaCl} $ 的产物纯度高于掺杂$ \text{KCl} $ 。同时保温时间不足会导致杂质Ti2AlC相与TiC相过多，保温时间过长也会导致产物分解。最终试验确定以海绵钛:铝:碳:盐的摩尔比例3∶1.2∶1.8∶2.5置于通氩气的管式炉中升温至1100 ℃，保温0.5 h的产物纯度最高，可达到90%。Abstract: Ti3AlC2 powder was synthesized by the pressureless sintering method with a mixture of the low-value titanium sponge, aluminum and carbon at a mixing ratio of 3∶1.2∶1.8. The sintered products at the holding temperature of 1000 ℃ and 1100 ℃ and the influence of different holding times on the experimental results were discussed. At the same time, the molten salt method was used to explore the influence of doping of NaCl or KCl on the purity of Ti3AlC2 prepared by pressureless sintering method. The experimental results show that the products sintered under the condition with argon gas protection show the best purity at 1100 ℃. In the molten salt process, the products sintered under the condition with salt doped still have the best purity at 1100 ℃, and the purity of the products doped with "NaCl" is higher than that of "KCl". Meanwhile, insufficient holding time would lead to excessive impurities of Ti2AlC phase and TiC phase, while too long holding time would also lead to product decomposition. The final experiment determined that the purity of the product with sponge titanium: aluminum∶carbon∶salt in the molar ratio of 3∶1.2∶1.8∶2.5 was the highest when it was heated to 1100 ℃ and kept for 0.5 h in a tubular furnace with argon protection, which could reaching 90%.-
Key words:
- Ti3AlC2 powder /
- sponge titanium /
- pressureless sintering /
- molten salt method /
- purity
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图 1 海绵钛为原料不同保温时间的粉体XRD谱
Figure 1. XRD patterns of powders using sponge titanium as raw material for different holding time
图 2 海绵钛为原料不同保温时间的粉体XRD谱
Figure 2. XRD patterns of powders using sponge titanium as raw material for different holding time
图 3 纯钛为原料在不同温度下粉体XRD谱
Figure 3. XRD patterns of powders using pure titanium as raw material at different temperatures
图 4 海绵钛为原料在不同温度下粉体XRD谱
Figure 4. XRD patterns of powders using sponge titanium as raw material at different temperatures
图 6 海绵钛为原料1000 ℃下掺杂不同盐的粉体XRD谱
Figure 6. XRD patterns of powders doped with different salts using sponge titanium as raw material at 1000 ℃
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