Synthesis,Characterization and Properties of Solid State Phosphates and Phosphonates

• Main Authors: Wen-Chen Lin, 林文貞
• Other Authors: Ju-Hsiou Liao
• Format: Others
• Language: zh-TW
• Published: 2000
• Online Access: http://ndltd.ncl.edu.tw/handle/10721106010815275332

碩士 === 國立中正大學 === 化學研究所 === 88 === Abstract The main goal of this thesis is to explore the synthesis and structural characterization of novel solid state phosphates and phosphonates, by means of novel microwave or conventional oven heating under hydrothermal conditions. We have examined the effects of such reaction parameters as temperatures, pH values, reaction ratios and choices of counterions to optimize the reaction condition in order to improve the purity and yield of the products. The reactions were performed by heating mixtures of alkali metal (or ammonium) cations, transition metal cations and phosphates or phosphonates at elevated temperatures in sealed tubes or autoclaves. A series of products, namely, Na2Mn(O3POH)2 (1), Na2Co(O3POH)2 (2), K2Mn2(PO4)2(PO3H) (3), Cs0.5Mn3(PO4)[(PO3)(OH)][O2P(OH)2]．2H2O (4), Na2Mn(O3PC6H5)2 (5), NaCo2(OH)(O3PC6H5)2 (6), NaCo(PO4) (7), Mn5(PO4)2(PO4H)2．4H2O (8), ，(NH4)2Mn3(OH)2[P2O6(OH)]2 (9), Mn3.5(PO4)(PO4H)2 (10), (Aniline)0.33Mn0.83(HPO3) (11) were obtained. Their structures were characterized by X-ray crystallographic techniques and were examined by UV-visible-near IR and mid-IR spectroscopies. Their thermal behaviors were investigated by thermogravimetric analyzer (TGA) and differential thermal analyzer (DTA). This thesis concludes that hydrothermal reaction is a promising synthetic tool to prepare metastable solid state materials. By comparing the result of conventional oven heating and microwave heating, we found they did not necessarily give the same products. Nevertheless, microwave heating was proved to be an efficient synthetic technique that can greatly reduce reaction time from several days to 30 minutes.