改进共沉淀法制备高比表面积钒酸镍负极材料及其电化学性能  

Nickel vanadate anode material with high specific surface area through improved co‑precipitation method:Preparation and electrochemical properties

作　　者：张宇婷 刘尊义 李宁[1] 张栋强[1] 赵仕玲 赵鹬[1] ZHANG Yuting;LIU Zunyi;LI Ning;ZHANG Dongqiang;ZHAO Shiling;ZHAO Yu(School of Petrochemical Engineering,Lanzhou University of Technology,Lanzhou 730050,China)

机构地区：[1]兰州理工大学石油化工学院,兰州730050

出　　处：《无机化学学报》2024年第11期2163-2174,共12页Chinese Journal of Inorganic Chemistry

基　　金：国家自然科学基金(No.21763016)资助。

摘　　要：以去离子水为绿色溶剂,Ni(NO_(3))_(2)·6H_(2)O为镍源,NH_(4)VO_(3)为钒源,通过碳酸钠溶液调节沉淀pH值,正丁醇干燥提高比表面积及颗粒分散度,采用改进的共沉淀法制备了相对廉价的钒酸镍负极材料(NVO-NBA)。通过对其微观形貌、比表面积、孔径大小及表面元素分布进行测试,探究了改进共沉淀法对钒酸镍电极材料织构性质的影响。结果表明,沉淀过程中溶液pH值的精准调节及后续加入表面张力较小的醇类溶剂的干燥方式对材料的比表面积、孔径大小、微观结构及颗粒分散度有显著的影响,其中在pH=8的条件下沉淀、后续加入正丁醇辅助干燥得到的样品NVO-8-NBA具有最大的比表面积(86 m2·g^(-1)),同时材料形貌为分散度较高、直径较小的球形纳米颗粒。加入乙醇、正丁醇、正己醇等醇类溶剂进行后续干燥得到的钒酸盐材料比表面积均比未加醇处理的样品显著提高,而正丁醇处理的样品效果最好,表明表面张力较小的醇类溶剂可以有效保护共沉淀过程生成的孔道体系,并可使颗粒分散更均匀,同时醇类的碳链长度对其性质也具有显著的影响。未加醇处理的样品NVO-8比表面积仅为20 m2·g^(-1),形貌为聚集的大块状。将制备的钒酸镍材料作为锂离子电池的负极材料,其在0.3 A·g^(-1)的电流密度下,NVO-8-NBA的首圈放电容量可以达到1519 mAh·g^(-1),而NVO-8仅为536 mAh·g^(-1)。NVO-8-NBA在0.3 A·g^(-1)的电流密度下循环100次后容量保持在223 mAh·g^(-1),而NVO-8仅为70 mAh·g^(-1)且仍有继续下降的趋势。The relatively cheap nickel vanadate anode material(NVO-NBA)was prepared through an improved co-precipitation method with Ni(NO_(3))2·6H_(2)O as nickel source,NH_(4)VO_(3) as vanadium source,and deionized water as a green solvent.The specific surface area and particle dispersion were improved by adjusting the pH value of precipi-tation with sodium carbonate solution and drying with n-butanol.The effects of the enhanced co-precipitation meth-od on the texture properties of nickel vanadate electrode materials were investigated by testing the microstructure,specific surface area,pore size,and surface element distribution.The results show that the specific surface area,pore size,microstructure,and particle dispersion of the material are significantly affected by the precise adjustment of the pH value of the solution during the precipitation process and the drying method of the subsequent addition of alcohol solvents with smaller surface tension.The typical sample NVO-8-NBA obtained by precipitation at pH=8 and subsequent addition of n-butanol-assisted drying possessed the largest specific surface area(86 m2·g^(-1)),and the material's morphology was spherical nanoparticles with higher dispersion and a smaller diameter.The specific sur-face area of the vanadate materials obtained by adding alcohol solvents such as ethanol,n-butanol,and n-hexanol for subsequent drying was significantly higher than that of the sample without alcohol treatment,while the samples treated with n-butanol had the best effect,indicating that the alcohol solvent with smaller surface tension can effec-tively protect the pore system generated by the co-precipitation process and can make the particles disperse more evenly,and the carbon chain length of the alcohol also has a significant effect on its properties.The specific surface area of the sample NVO-8 without alcohol treatment was only 20 m2·g^(-1),and its morphology was a large block of aggregation.The prepared nickel vanadate material was used as the anode material of the lithium-ion batt

关 键 词：改进共沉淀法 钒酸镍 锂离子电池 电化学性能 

分 类 号：TQ152[化学工程—电化学工业] O614.511[理学—无机化学] O614.813[理学—化学]