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无机材料学报 2012
Rapid Synthesis of Mesoporous Nickel Phosphates under Microwave Assisted Hydrothermal ConditionDOI: 10.3724/sp.j.1077.2012.00501 Keywords: mesoporous nickel phosphate, NiPO, microwave assisted hydrothermal synthesis, Sol-Gel method Abstract: Mesostructured nickel phosphate (MW―NiPO―2) was rapidly synthesized in the presence of cationic surfactant 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 characterizations of the materials obtained by the two different procedures, Sol―Gel method and microwave assisted hydrothermal process, were carried out by ICP, FT―IR, TEM and N2 physisorption. The results show that MW―NiPO―2 can be obtained at relatively low temperature (60 par;. When the microwave radiation temperature was 100 the mesostructured phase formed in an extremely short period about 0.25 h. Ordered MW―NiPO―2 can be obtained under microwave irradiation for 1 h at 100 when OH?/P 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 comparison 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).
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