Hybrid Cathodic/Anodic Electrosynthesis of Phase Pure Ag 4 V 2 O 7 Thin Films
Hybrid Cathodic/Anodic Electrosynthesis of Phase Pure Ag 4 V 2 O 7 Thin Films
复制标题
相纯Ag 4 V 2 O 7 薄膜的混合阴极/阳极电合成
DOI：
10.1149/1945-7111/acd149
复制
发表时间：
2023
影响因子：
3.9
通讯作者：
Rajeshwar, Krishnan
中科院分区：
文献类型：
--
作者：
Vali, Abbas;Kim, Soo Yeon;Danladi, Fahad;Rawat, Abhishek;Zhang, Chuzhong;Toth, Peter S.;Janáky, Csaba;Myung, Noseung;Meletis, Efstathios I.;Rajeshwar, Krishnan
在这里，我们展示了一个两步电合成的方法制备焦钒酸银，银4 V2 O 7薄膜的形式。在第一阴极步骤中，多晶Ag从非水浴沉积在氟掺杂的氧化锡（FTO）基底上。水焦钒酸盐物种，然后产生老化的CO2注入原钒酸钠（Na 3VO 4）溶液三周。银离子随后产生原位在该介质中使用阳极剥离的Ag/ITO膜从第一步骤。Ag+离子与焦钒酸盐物质的界面沉淀提供了相纯形式的目标产物。通过结合使用伏安法，电化学石英晶体纳米重量法（EQCN），库仑法在原位监测的各个阶段的电合成。采用X射线衍射、激光拉曼光谱、漫反射光谱、扫描电子显微镜和高分辨率透射电子显微镜等实验技术对Ag 4 V2 O 7薄膜进行了表征。表面光电压谱，环境压力光电子能谱，开尔文探针接触电位差（功函数）测量提供的信息的能带结构的p型银4 V2 O 7半导体。最后，研究了电合成的Ag 4V 2 O 7薄膜在水溶液和非水溶液中的电化学和光电化学性能。
Here, we demonstrate a two-step electrosynthesis approach for the preparation of silver pyrovanadate, Ag 4 V 2 O 7 in thin-film form. In the first, cathodic step, polycrystalline Ag was deposited on fluorine doped tin oxide (FTO) substrate from a non-aqueous bath. Aqueous pyrovanadate species were then generated by aging of a CO 2-infused sodium orthovanadate (Na 3 VO 4) solution for three weeks. Silver ions were subsequently generated in situ in this medium using anodic stripping of the Ag/ITO films from the first step. Interfacial precipitation of the Ag+ ions with the pyrovanadate species afforded the targeted product in phase pure form. The various stages of the electrosynthesis were monitored in situ via the combined use of voltammetry, electrochemical quartz crystal nanogravimetry (EQCN), and coulometry. The Ag 4 V 2 O 7 thin films were characterized by a variety of experimental techniques, including X-ray diffraction, laser Raman spectroscopy, diffuse reflectance spectroscopy, scanning electron microscopy, and high-resolution transmission electron microscopy. Surface photovoltage spectroscopy, ambient-pressure photoemission spectroscopy, and Kelvin probe contact potential difference (work function) measurements afforded information on the energy band structure of the p-type Ag 4 V 2 O 7 semiconductor. Finally, the electrochemical and photoelectrochemical properties of the electrosynthesized Ag 4 V 2 O 7 thin films were studied in both aqueous and non-aqueous electrolytes.