Bismuth sesquioxide (\(\hbox {Bi}_2\hbox {O}_3\)) draws much attention due to wide variety of phases in which it exists depending on the temperature. Among them, \(\delta\) phase is specially interesting because of its high oxide ion conductivity and prospects of applications as an electrolyte in fuel cells. Unfortunately, it is stable only in a narrow temperature range ca. 730–830 \(^{\circ }\)C. Our group has developed a facile and reproducible two-stage method of stabilizing \(\hbox {Bi}_2\hbox {O}_3\) crystalline phases confined in nanocrystallites embedded in amorphous matrix. In the first stage, glassy materials were obtained by a routine melt-quenching method: pure \(\hbox {Bi}_2\hbox {O}_3\) powders were melted in porcelain crucibles and fast-cooled down to room temperature. In the second step, the materials were appropriately heat-treated to induce formation of crystallites of \(\beta\), \(\delta\) or \(\gamma\) \(\hbox {Bi}_2\hbox {O}_3\) phases confined in a glassy matrix, depending on the process conditions. It was found out that the vitrification of the initial \(\hbox {Bi}_2\hbox {O}_3\) and the subsequent nanocrystallization were unexpectedly possible due to the presence of some Al, and Si impurities from the crucibles. Systematic DTA, XRD, optical, Raman and SEM/EDS studies were carried out to investigate the influence of the syntheses processes and allowed us to determine conditions under which the particular phases appear and remain stable down to room temperature.

倍半氧化铋 ( \(\hbox {Bi}_2\hbox {O}_3\) ) 因温度不同而存在多种相，因此备受关注。其中，\(\delta\)相因其高氧化物离子电导率和作为燃料电池电解质的应用前景而特别受关注。不幸的是，它仅在狭窄的温度范围内稳定。730–830 \(^{\circ }\) C. 我们的小组开发了一种简便且可重复的两阶段方法来稳定限制在嵌入的纳米微晶中的\(\hbox {Bi}_2\hbox {O}_3\)晶相在无定形基质中。在第一阶段，通过常规熔融淬火方法获得玻璃态材料：纯\(\hbox {Bi}_2\hbox {O}_3\)粉末在瓷坩埚中熔化并快速冷却至室温。在第二步中，对材料进行适当的热处理以诱导形成\(\beta\)、\(\delta\)或\(\gamma\) \(\hbox {Bi}_2\hbox {O }_3\)相限制在玻璃状基质中，具体取决于工艺条件。发现初始\(\hbox {Bi}_2\hbox {O}_3\)的玻璃化由于坩埚中存在一些 Al 和 Si 杂质，随后的纳米结晶出乎意料地成为可能。进行了系统的 DTA、XRD、光学、拉曼和 SEM/EDS 研究以研究合成过程的影响，并使我们能够确定特定相出现并在室温下保持稳定的条件。