发表机构
University of Applied Sciences Zwickau; Université catholique de Louvain (UCLouvain)(茨维考应用科学大学; 天主教鲁汶大学)
机构由 AI 辅助整理,请以论文原文为准。AI 中文总结
本研究通过无添加剂水溶液共沉淀法合成Fe-PBA、Co-PBA、Ni-PBA,经多种表征对比发现,三者差异不仅源于过渡金属种类,还受前驱体氧化态和洗涤效率影响。
AI 中文摘要
分别使用K₄[Fe(CN)₆]与FeCl₃、CoCl₂或NiCl₂,通过无添加剂水溶液共沉淀路线合成普鲁士蓝(Fe-PBA)及其钴、镍类似物(Co-PBA和Ni-PBA)。采用X射线衍射、ATR-FTIR、拉曼光谱、FEG-SEM/EDS及TG/SDTA对三种粉末进行系统对比。所有组成均呈现特征性的立方氰化物桥连PBA骨架,Fe-PBA、Co-PBA和Ni-PBA的表观晶格参数分别为10.10±0.02、10.01±0.02和10.10±0.03埃。在Fe-Co-Ni系列中,ATR-FTIR的主要C≡N伸缩带从2062 cm⁻¹移至2071和2087 cm⁻¹,表明局部氰化物环境存在与组成相关的变化。Fe-PBA的钾含量低于含钴和镍的粉末,且表现出明显更大的低温质量损失。在三种衍射图谱中均观察到归属于结晶KCl的尖锐反射,而Ni-PBA中存在额外的未归属反射,表明至少存在另一种结晶相。这些结果表明,Fe、Co和Ni基PBA之间的差异不能仅归因于过渡金属种类,因为前驱体氧化态和洗涤效率也会影响所得粉末的组成和热响应。
英文摘要
Prussian Blue (Fe-PBA) and its Co and Ni analogues (Co-PBA and Ni-PBA) were synthesized by an additive-free aqueous co-precipitation route using K$_4$[Fe(CN)$_6$] and FeCl$_3$, CoCl$_2$, or NiCl$_2$, respectively. The three powders were systematically compared by X-ray diffraction, ATR-FTIR and Raman spectroscopy, FEG-SEM/EDS, and TG/SDTA. All compositions exhibit the characteristic cubic cyanide-bridged PBA framework, with apparent lattice parameters of 10.10 +/- 0.02, 10.01 +/- 0.02, and 10.10 +/- 0.03 Angstrom for Fe-PBA, Co-PBA, and Ni-PBA, respectively. The dominant C$\equiv$N stretching band in ATR-FTIR shifts from 2062 to 2071 and 2087 cm$^{-1}$ across the Fe-Co-Ni series, indicating composition-dependent changes in the local cyanide environment. Fe-PBA contains less potassium than the Co- and Ni-containing powders and exhibits a substantially larger low-temperature mass loss. Sharp reflections assigned to crystalline KCl are observed in all three diffraction patterns, while additional unassigned reflections in Ni-PBA indicate the presence of at least one further crystalline phase. These results show that differences among Fe-, Co-, and Ni-based PBAs cannot be attributed solely to transition-metal identity, as precursor oxidation state and washing efficiency also influence the composition and thermal response of the resulting powders.