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摘要: 以化学水解法合成的-FeOOH纳米微粉(平均粒径在12 nm左右)为原料,分别在0.0~4.5 GPa和200~350 ℃的压力和温度范围进行冷压和热压处理。实验结果表明,冷压对-FeOOH纳米固体的结构没有明显影响,但却使它的热致相变(从-FeOOH相到-Fe2O3相)温度从常压下的203.8 ℃提高到4.5 GPa压力下的274 ℃,接近常规体相材料的相变温度。而在一定的热压条件处理下,首次发现了从-FeOOH相到-FeOOH相的结构转变,并在4.5 GPa、200 ℃的热压条件下得到了转变过程中的一个新的亚稳相。从压力和温度对纳米微粒的作用角度,对上述实验结果进行了讨论。Abstract: It is well known that the research on nanometer solid has brought to people's great interest in recent years, but only a few works has been done so far about the properties of nanocrystalline under high pressure. In the present paper, we have synthesized a series of -FeOOH nanometer solid by treating the ultrafine powder under the pressure range of 0.0~4.5 GPa and the temperature range of 200~350 ℃. The ultrafine powder was synthesized by using chemical hydrolysis method and its average diameter is 12 nm. Using X-ray diffraction (XRD) and differential thermal analysis (TG-DTA), we investigated the structural transformation of these nanometer solids. The results of XRD and TG-DTA experiments show that under cold pressure of 0.0~4.5 GPa, the structure of the nanometer solids do not change considerably, but on the other hand, the temperature of the heat-induced phase transformation (from -FeOOH phase to -Fe2O3 phase) in these -FeOOH nanometer solids is raised obviously with increasing pressure, from 203.8 ℃ at normal pressure to 274 ℃ at 4.5 GPa. This variation can be interpreted by the effect of pressure on the coordinate state of the OH- group in the interface of nanometer solid. After treating under hot pressure, both the formation and temperature of the structural transformation of -FeOOH nanometer solid are very different from the results under cold pressure. Under the hot pressure of 4.5 GPa, the temperature of the structural transformation from -FeOOH phase to -Fe2O3 phase is far above 350 ℃. However under the condition of 3.0 GPa, 200 ℃ and 4.5 GPa, 350 ℃, we firstly observe the structural transformation, from -FeOOH phase to -FeOOH phase. It is more interesting that we obtain a new metastable phase of FeOOH in the above structural transformation at the condition of 4.5 GPa and 200 ℃. These special variation can be interpreted by considering the effect of pressure combining temperature on the OH- group in the nanometer solid at the same time.
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