Static observation of the interphase between NaBH4 and LiI during the conversion reaction
Static observation of the interphase between NaBH4 and LiI during the conversion reaction
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转化反应过程中NaBH4和LiI之间界面的静态观察
DOI：
10.1016/j.jssc.2021.122496
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发表时间：
2021
影响因子：
3.3
通讯作者：
Hihara Takehiko
中科院分区：
文献类型：
--
作者：
Miyazaki Reona;Onishi Keita;Miyagawa Reina;Hihara Takehiko
为了确定单相NaI-NaBH 4-LiI固溶体的合成条件，通过制备NaBH 4/LiI混合颗粒，研究了NaBH 4 + LiI → NaI + LiBH 4的转化反应。在不同的反应温度和压力下，反应的程度进行了研究。虽然在本研究中不可能完全抑制转化反应，但低温和高压条件显示出有利于避免LiBH 4的存在。一个重要的一点是，转化反应是在静态条件下以颗粒的形式进行研究的，而大多数金属硼氢化物-卤化物复合材料是通过球磨制备的。采用扫描电镜（SEM）、俄歇电子能谱（AES）、波长色散X射线谱（WDS）和飞行时间二次离子质谱（ToF-SIMS）等分析手段，研究了不同时效时间下NaBH 4/LiI混合芯块的微观结构。分析表明，NaBH 4与LiI之间的反应界面按LiI/NaI/LiBH 4/NaBH 4的顺序发生。可以清楚地证实，即使在室温下，NaI层的生长也随着时间而持续。结合界面相的排列，Na+在LiBH 4中的扩散似乎是NaI层生长的必要条件。这些结果表明，对其它金属硼化物与卤化物（如CeCl_3/LiBH_4，ZrCl_4/KBH_4等）之间的转化反应的详细研究是有益的。在静态条件下可能会揭示新离子在现有化合物中的扩散。
To determine the synthesis conditions for NaI–NaBH4–LiI solid solutions in a single phase, the conversion reaction of NaBH4+ LiI → NaI + LiBH4was investigated by preparing mixed pellets of NaBH4/LiI. The extent of the reaction was investigated under different reaction temperatures and pressures. Although it was not possible to completely suppress the conversion reaction in this study, the low temperature and high-pressure conditions were shown to be favorable to avoid the presence of LiBH4. A significant point is that the conversion reaction was investigated in a static condition in the form of pellets, whereas most of the metal borohydride-halide composites have been fabricated by ball-milling. The microstructure of NaBH4/LiI mixed pellets at different ageing times was observed by scanning electron microscope (SEM), Auger electron spectroscopy (AES), wavelength dispersive X-ray spectroscopy (WDS) and time of flight secondary ion mass spectroscopy (ToF-SIMS). The analysis revealed that the reaction interphase between NaBH4and LiI occurs in the order of LiI/NaI/LiBH4/NaBH4. It was clearly confirmed that the growth of the NaI layer continued with time even at room temperature. In conjunction with the array of the interphase, the diffusion of Na+in LiBH4appears to be a necessary condition for the growth of the NaI layer. The present results suggest that a detailed investigation of the conversion reaction between other metal borohydrides and halides (for example, CeCl3/LiBH4, ZrCl4/KBH4,etc.) in the static condition would likely reveal the diffusion of the new ions in the existing compounds.
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