微波辅助水热法快速合成介孔磷酸镍  

Rapid Synthesis of Mesoporous Nickel Phosphates under Microwave Assisted Hydrothermal Condition

作　　者：李旭影[1] 谭涓[1] 杨建华[1] 刘靖[1] 杨菲[1] 

机构地区：[1]大连理工大学化工与环境生命学部,化工学院,大连116024

出　　处：《无机材料学报》2012年第5期501-506,共6页Journal of Inorganic Materials

基　　金：国家自然科学基金(20803004)~~

摘　　要：采用微波辅助水热法快速合成了介孔磷酸镍(MW-NiPO-2),详细研究了在微波水热条件下微波晶化温度、微波辐射时间、碱度及Ni/P摩尔比对MW-NiPO-2合成的影响,优化了合成条件.并利用ICP、FT-IR、TEM和N2吸附等手段对比研究了溶胶凝胶法和微波水热法合成样品的结构组成、比表面和孔道特征.研究结果表明:在微波辅助水热条件下,在较低温度下(60℃)即可形成MW-NiPO-2;在100℃下,0.25 h即有MW-NiPO-2生成.在微波辐射1 h,碱度(OH-/P)为2.0、原料Ni/P比为0.7条件下,能够合成有序度较高的MW-NiPO-2.MW-NiPO-2和SG-NiPO-2具有相似的骨架结构和组成,但其纳米管簇结构特征不明显,表现出类似虫孔结构的状态.微波辅助水热法合成的MW-NiPO-2较溶胶凝胶法合成样品具有更大的比表面和孔容,分别为334.4 m2/g和0.318 cm3/g.Mesostructured nickel phosphate （MW-NiPO-2） was rapidly synthesized in the presence of cationic sur- factant by a microwave assisted hydrothermal process. The synthesis parameters, microwave irradiation temperature and time, OH/P and Ni/P molar ratios of the precursor, were systematically investigated and optimized. The charac- terizations of the materials obtained by the two different procedures, Sol-Gel method and microwave assisted hydro- thermal process, were carried out by ICE FT-IR, TEM and N2 physisorption. The results show that MW-NiPO-2 can be obtained at relatively low temperature （60℃）. When the microwave radiation temperature was 100℃, the mesostruc- tured phase formed in an extremely short period about 0.25 h. Ordered MW-NiPO-2 can be obtained under micro- wave irradiation for 1 h at 100℃, when OH-if＇ and the Ni/P molar ratios of the precursor are 2.0 and 0.7, respectively. In contrast, it took at least 24 h for completion via Sol-Gel method. MW-NiPO-2 and SG-NiPO-2 possess similar structure and composition while MW-NiPO-2 exhibites a worm-like appearance other than piled nanotubes. In com- parison with the sample synthesized via Sol-Gel method, MW-NiPO-2 possesses a relatively high BET surface area （334.4 m2/g） and pore volume （0.318 cm3/g）.

关 键 词：介孔磷酸镍 NiPO 微波辅助水热合成 溶胶凝胶法 

分 类 号：TQ426[化学工程]