核壳结构Ta₂O₅@Ta₃N₅纳米花控制合成工艺研究  

Controllable Synthesis of Core-Shell Structure Ta2O5@Ta3N5 Nanoflowers

作　　者：董鑫 

机构地区：[1]哈尔滨师范大学化学化工学院,黑龙江 哈尔滨

出　　处：《材料科学》2023年第4期253-260,共8页Material Sciences

摘　　要：以TaCl5为钽源,采用水热–高温氮化法合成核壳结构Ta2O5@Ta3N5纳米花。首先,利用场发射扫描电子显微镜(SEM)测试评价样品形貌,研究溶剂种类、异丙醇用量、盐酸用量、水热时间等条件因素对样品形貌调控规律;异丙醇溶剂有利于促进棒状结构生成,当异丙醇用量为14 mL,浓盐酸用量为400 µL,经160℃水热4 h制得Ta2O5纳米花,组成纳米花的棒状结构直径约50 nm,长约200 nm。再利用高温氮化技术,在50 mL∙min−1 NH3气流下,经850℃氮化3 h,Ta2O5纳米花经拓扑转换制得核壳结构Ta2O5@Ta3N5纳米花。XRD分析证实样品具有Ta2O5和Ta3N5双相结构,晶化度较高;HRTEM分析表明样品形成Ta2O5/Ta3N5;BET比表面积为21.9 m2∙g−1。本文为进一步开展Ta2O5@Ta3N5基纳米材料的制备及应用性能研究奠定实验技术基础。Ta2O5@Ta3N5 nanoflowers were synthesized by a combination of hydrothermal and high-tempe- rature nitridation method, using TaCl5 as the tantalum source. Based on the morphology evaluated by field emission scanning electron micros-copy (SEM), the preparation process of Ta2O5 nanoflowers was optimized by regulating process conditions including solvent type, amount of isopropanol, amount of hydrochloric acid, and hydrother-mal time. Isopropanol solvent is beneficial to promote the formation of rod-like structure. When the amount of isopropanol is 14 mL and the amount of concentrated hydrochloric acid is 400 µL, Ta2O5 nanoflowers are prepared by hydrothermal treatment at 160˚C for 4 h. The rod-like structure of nanoflowers is about 50 nm in diameter and about 200 nm in length. Then, Ta2O5@Ta3N5 nanoflowers were prepared by topological transformation of Ta2O5 nanoflowers, using high-temperature nitriding technology, under 50 mL∙min−1 NH3 gas flow, after nitriding at 850˚C for 3 h. XRD analysis confirmed that the sample possessed both Ta2O5 and Ta3N5 phases with a high crystallization de-gree. HRTEM analysis indicated that the sample exhibited core-shell structure Ta2O5@Ta3N5. Its BET specific area was 21.9 m2∙g−1. This work lays an experimental technical foundation for further research on preparation and application properties of Ta2O5@Ta3N5-based nanomaterials.

关 键 词：纳米花 棒状结构 TA2O5 核壳结构 水热时间 高温氮化 测试评价 盐酸用量 

分 类 号：TB3[一般工业技术—材料科学与工程]