晶化温度对H-TiO2纳米管阵列微观结构及电化学储锂性能的影响  

Influence of annealing temperature on microstructure and electrochemical lithium storage performances of hydrogenated TiO2 nanotube arrays

作　　者：李天赐 李靖巍 戴梦嘉 许俊 刘家琴 张琪 吴玉程 LI Tian-ci;LI Jing-wei;DAI Meng-jia;XU Jun;LIU Jia-qin;ZHANG Qi;WU Yu-cheng(Institute of Industry ＆ Equipment Technology, Hefei University of Technology, Hefei 230009, China;School of Electronic Science ＆ Applied Physics, Hefei University of Technology, Hefei 230009, China;Key Laboratory of Advanced Functional Materials and Devices of Anhui Province, Hefei 230009, China;School of Materials Science and Engineering, Hefei University of Technology, Hefei 230009, China)

机构地区：[1]合肥工业大学工业与装备技术研究院,安徽合肥230009 [2]合肥工业大学电子科学与应用物理学院,安徽合肥230009 [3]先进功能材料与器件安徽省重点实验室,安徽合肥230009 [4]合肥工业大学材料科学与工程学院,安徽合肥230009

出　　处：《材料热处理学报》2018年第6期140-147,共8页Transactions of Materials and Heat Treatment

基　　金：国家自然科学基金(51402078);合肥工业大学学术新人提升计划B项目(JZ2016HGTB0711);安徽省有色金属材料与加工工程实验室青年学术团队能力提升计划项目(HFUT-AZ-2017-035-1)

摘　　要：采用阳极氧化法制备TiO2纳米管阵列薄膜（TNTAs）,在不同热处理温度下对其进行晶化处理,然后采用电化学氢化法对TNTAs实施氢化改性,获得导电性显著提高的H-TNTAs。利用场发射扫描电镜、X射线衍射、X射线光电子能谱、显微共焦激光拉曼光谱研究了晶化温度对TNTAs和H-TNTAs微观结构的影响,利用电池测试系统,探究晶化温度对TNTAs和H-TNTAs作为锂电负极的电化学性能影响。结果表明：当晶化温度从400℃升高至700℃时,非晶TiO2逐渐晶化为锐钛矿相,在600℃时发生锐钛矿向晶红石相转变,700℃时管状结构发生破坏;随着晶化温度的升高,TNTAs电极的比容量不断降低;氢化改性后HTNTAs的比容量和倍率特性均有提升,但是不同晶化温度的H-TNTAs比容量和倍率特性提升幅度不一,主要是由于氢化时引入的Ti^3＋在不同晶体结构TiO2中浓度和稳定性不同,其中晶化温度为500℃时,单一锐钛矿相、结晶良好的H-TNTAs-500的电化学性能最优,比容量和倍率特性提升最为显著。Highly-ordered and well-separated TiO2 nanotube arrays（ TNTAs） were fabricated by anodization and then annealed at different temperatures. Subsequently,the TNTAs were hydrogenated by a facile electrochemical hydrogenation technique to obtain highly-conductive H-TNTAs. The morphology and microstructure of as-prepared TNTAs and H-TNTAs annealled at different temperatures were characterized by means of field emission scanning electron microscopy（ FESEM）,X-ray diffraction（ XRD）,X-ray photoelectron spectroscopy（ XPS）,and Raman spectroscopy（ Raman）,and the electrochemical performances of the TNTAs and H-TNTAs electrodes annealled at different temperatures for lithium ion battery were tested by using a cell testing system. The results show that when the annealing temperature increases from 400 ℃ to 700 ℃,the amorphous TiO2 gradually crystalizes into anatase phase,and anatase to rutile phase transforms at 600 ℃,and the tube-structure of the TNTAs is destroyed at 700 ℃. With the increasing of annealing temperature,the discharge capacityof the TNTAs electrodes gradually decreases,while the discharge capacity and rate performance of the H-TNTAs electrodes are greatly improved to different degrees at different annealing temperatures,which is mainly due to the different concentration and stability of intentionally introduced Ti^3＋ in different TiO2 crystal structure during hydrogenation. When the annealing temperature is 500 ℃,the single anatase phase and the well-crystallized H-TNTAs-500 have the best electrochemical performance and the most significant enhancement of discharge capacity and rate performance.

关 键 词：晶化温度 TIO2纳米管阵列 氢化 微观结构 储锂性能 

分 类 号：TB383[一般工业技术—材料科学与工程] TM911[电气工程—电力电子与电力传动]