为了研究纳米氮化硼在溶剂热条件下的物相转变规律,利用三氯化硼(BCl3)和氮化锂(Li3N)为原料,吡啶作为溶剂合成了纳米氮化硼.在实验过程中,系统研究了反应温度、压力以及反应时间的影响,发现在吡啶热反应体系中,首先形成的是结构无序的无定形纳米氮化硼(aBN).随着反应温度和压力的提高以及时间的延长,纳米氮化硼中的原子排列有序度不断提高,逐渐出现了结构部分有序的湍层氮化硼(tBN)和结构有序的六方氮化硼(hBN).在反应温度和压力提高时,样品中首先是tBN的含量提高,然后是hBN的含量明显增加,说明在合成反应过程中存在aBN→tBN→hBN的物相转变.
In order to investigate the phase transformation of boron nitride nanoparticles in solvothermal solutions, BN was synthesized by reacting BCl3 and Li3N in pyridine under a rather mild condition. During the synthesis process, the influences of reaction temperature, pressure and duration were intensively investigated, finding that the earliest BN phase appearing in the solution was aBN, in which B and N atoms arranged in a random way. After that, the order degree of B and N atom arrangement was improved gradually with increasing the temperature and pressure and prolonging the reaction duration, thus tBN and hBN formed. Besides, the content of tBN increased at first when the temperature and pressure increased, followed by the increase of hBN and the decrease of tBN. This result reveals that a phase transformation of aBN→tBN→hBN happened in the reaction solution under such a circumstance.