采用燃烧合成技术,通过改变Ti、Al和C 3种粉末的比例制备出高纯度的Ti_3AlC_2块体材料,并对其在氩气中的高温热稳定性进行了研究.X射线衍射(XRD)表明合成产物除了含有Ti_3AlC_2外,还含有少量TiC和Ti-Al金属间化合物,经k值法计算得Ti_3AlC_2最高含量为96.7%.耦合等离子-原子发射光谱(ICP-AES)结果表明最高纯度的合成产物中Ti、Al质量分数分别为74.2%和13.7%,与Ti_3AlC_2中Ti和Al含量十分接近.利用SEM对燃烧产物断口进行了观察,发现明显的层片状结构.热重-差热(TG-DTA)结果表明燃烧合成的高纯Ti_3AlC_2在加热过程中没有明显的热效应,说明合成的产物处于近似平衡状态.Ti_3AlC_2的分解温度在1370 ℃左右,同时由于氧化作用而导致试样质量略有增加.
Highly pure Ti_3AlC_2 was synthesized by self-propagating high-temperature synthesis method from Ti, Al and C powders with different initial ratios. The thermal stability of Ti_3AlC_2 in Ar atmosphere was studied. X-ray diffraction results show the products consists of TiC and/or Ti-Al intermetallics besides Ti_3AlC_2. The maximum content of Ti_3AlC_2 is estimated to be 96.7% by k-value method. The inductively coupled plasma-atomic emission spectrometry(ICP-AES) result shows that the highest-purity product contains 74.2% Ti and 13.7% Al, which is very close to those in Ti_3AlC_2. The fracture surfaces were observed by scanning electron microscope, where layered morphology is apparent. Thermal gravimetric-differential thermal analysis result shows no obvious heat effect was observed during heating highly pure as-synthesized Ti_3AlC_2, which indicates the as-synthesized product is almost in its equilibrium condition. The decomposition temperature of Ti_3AlC_2 is determined to be 1370 ℃ and the mass increased slightly because of oxidation.
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