摘要
以KMnO4与MnSO4为原料,采用水热法制备了α-MnO2纳米线;采用XRD、IR、SEM、EDS、DTA-TG等对样品的物相、结构、形貌、成分及热稳定性进行了表征;初步研究了反应温度、水热时间及溶剂种类对纳米结构MnO2合成的影响,并探讨了MnO2的晶型转变和-αMnO2纳米线的生长过程。结果表明:①所得α-MnO2纳米线粗细均匀,分散度好,其直径约为50~60 nm;②在水体系中,温度较低和反应时间较短时生成具有层状结构的锰的羟基化合物和-δMnO2,随着反应温度的升高(180~220℃)和水热时间的延长(6~48 h)产物转化为-αMnO2;③将溶剂改为正丙醇,在与②相同的条件下得不到MnO2;④α-MnO2纳米线的生长过程为:MnO4-与Mn2+反应生成MnO(OH),MnO(OH)发生氧化反应生成Mn(OH)4,Mn(OH)4发生脱水反应生成MnO2,产物由无规则球形纳米颗粒最终转化为纳米线。实验中通过控制反应参数达到调控MnO2物相和形貌的目的,为氧化物的可控制备及性能调控提供思路。
The α-MnO2 nanowires with the diameter of 50~60 nm were successfully synthesized by hydrothermal reaction between KMnO4 and MnSO4.The samples were characterized by XRD,IR,SEM,EDS and DTA-TG techniques to determine their phase,structure,morphology,composition and thermal stability.And the influence of experimental parameters,such as reaction temperature and hydrothermal time and solvents,were studies,implying that the crystal structures and morphologies of the as-obtained samples depend on the temperature and time.The results show that lamellar-structured δ-MnO2 and manganese hydroxyl compounds are obtained at 140℃ for 6 h,which are transformed into α-MnO2 while the temperatures are increased and the hydrothermal times are prolonged.When the solvent is changed into water and propanol with the 1∶1 volumn ratio,MnO2 can not be obtained.
出处
《实验室研究与探索》
CAS
北大核心
2011年第6期33-36,43,共5页
Research and Exploration In Laboratory
基金
中南大学博士后基金项目(1332/74341015511)
湖南科技大学博士启动基金(E51079)
湖南科技大学教育科研项目(G30953)
关键词
水热法
MNO2
纳米线
生长机理
hydrothermal method
MnO2
nanowires
formation mechanism