水热合成过渡金属氟化物和氧化物及性质研究
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摘要
本论文致力于复合氟化物的水热合成与性质表征,研究了合成条件的影响以及化合物的磁学性质,并在深入理解这些因素的基础上找到了一些水热合成复合氟化物的有效方法。
在第1章介绍了有关复合氟化物的相关基本理论知识,对复合氟化物的最新研究进展进行了总结;在第2章中,介绍了水热合成3个钾冰晶石型氟化物,同时介绍了具有锥冰晶石结构化合物K_5V_3F_(14)的合成以及磁性研究;在第3章中,介绍了冰晶石结构的六氟合钒酸盐A_3VF_6(A=K, Na, NH4)以及六氟合铁酸盐A_3FeF_6(M=K, Na, NH4)复合氟化物的水热合成与表征,并详细讨论了合成条件的改变对产物结晶的影响。在第4章中,介绍了Aurivillius结构氟氧化物的水热合成,并详细讨论了合成条件的改变对产物的影响;第5章介绍了钙钛矿结构的AgMO_3(M=Nb, Ta)和BaTaO_3以及烧绿石结构的化合物Cd_2Ta_2O_7的水热合成,结构与表征,并讨论了反应物摩尔比,反应温度和时间等对产物的影响。
本论文详细的阐述了上述化合物的合成条件和方法、结构特点以及性质,并仔细考察了各种影响产物水热稳定性的因素,为进一步研究复合氟氧化物水热合成和性质表征奠定了基础。
Fluoride compounds are usually prepared by tranditional high temperature solid-state methods which require calcination of fluoride raw materials at temperature in excess of 1000℃with frequent grindings. Aothough these methods are adequate for the synthesis of X-ray pure specimens, it is often difficult to control the total oxygen content in the mixed valence systems because of the high temperature used in products of the formation of undesirable phases. Particle size reduction by milling can introduce chemical impurities into the ceramic product, which may severely influence the final properties of fluoride compounds.
Soft chemical methods, such as the use of sol-gel precursors or molten salts as reaction media, have been adopted for the synthesis of oxide, but these methods involve often complex operating procedures. Hydrothermal technique has been widely applied to the synthesis of metastable phases and microporous solids. This method provides an attractive alternative to the synthesis fo complex oxides and fluorides, since it is carried out under relatively mild conditions (autogeneous pressure and～240℃) with controllable particle size distribution of the product. Hydrothermal method, involving heating metal salts, fluorides iin a liquid elevated temperature and pressure, offers an alternative synthesis route for the multicomponent ceramic oxides prepared using the traditional, high-temperature methods of solid-state chemistry: the use fo a solvent would permit rapid mixing fo several chemical elements, leading to homogeneous products, and also offers the potential for control of crystal growth leading to particles of desired morphologies, something rather difficult to achieve when using the high temperatures that must be employed in solid-state reactions. In particular, the hydrothermal method has great scope for the preparation of multinary fluoride phases, i.e. containing two ro more metals, where the rapid mixing fo the constituent elements would provide a great synthetic advantage, as well as potentially leading to the discovery of new materials. In this study, we focus on the hydrothermal crystal growth of fluoride compounds. In the system that has been prepared by traditional methods, a more soft synthesis route is explored and the results are compared with those obtained by other synthesis methods for the purpose to establish the relationship between the synthesis method and properties of final crystalline products.
The complex fluorides K_2NaVF_6, (NH_4)_2VF6 and (NH_4)_2NaVOF_5 with elpasolite-type structure have been synthesized under mild hydrothermal conditions. The details of hydrothermal synthesis conditions deeply discussed. We know that V2O3 is good source of V. F anions is not only a reaction material but also act as a mineralizer in the process. We found that the reducing agent K2S2O3 and (NH_4)_2S2O3 played an ed an important role for the compounds of K_2NaVF_6 and (NH_4)_2NaVF6 respectively, and also they can bring A site cations for the target products. From the experiment we concluded that the reaction condition of compound K_2NaVF_6 as follow: the molar ratio of raw material is V2O3 :NaF :(NH_4)_2S2O3 :NH4HF2 :HF=0.5:1:2:0.1,the temperature is 180℃, the reaction time is 3 days. The synthesis reaction conditions of compound (NH_4)_2NaVF6 as follows: raw materials molar ratio of V_2O_3 :NaF :(NH_4)_2S_2O_3 :NH_4HF_2 :HF=0.5:1:1:7:0.1, reaction temperature is 180℃, the reaction time is 3 days.
The chiolite-type compound of K_5V_3F_(14) was prepared for the first time from hydrothermal system, and deeply discussed the molar ratio of the reaction materials, the reaction conditions: the reaction temperature is 180℃, reaction time is 3 days, during the synthesis processes, the reducing agent of K2S_2O_3 was the critical role because of the raw material of V_2O_3 can be easily oxide by oxygen.
The hexafluoride vanadium(III) K_3VF_6, Na_3VF_6 and (NH_4)_3VF_6 with cryolite-type were prepared for the first time under the mild hydrothermal synthesis. Deeply discussed the molar ratio of the reaction materials, reaction temperature and reaction time that influence the products. Thermal stability of of (NH_4)_3VF_6 and (NH_4)_3FeF_6 were studies by TG-DTA in air. They decomposed in two steps at the first step and losses the compound of NH_4F, and the second step they loss NH_4F.
The perovskite-type oxide compounds of AgMO_3(M = Nb, Ta), BaTaO_3 and the pyrochlore-type compound of Cd_2Ta_2O_7 were prepared for the first time under the hydrothermal synthesis. Deeply discussed the reaction temperature, molar ratio of the reaction materials and reaction time that influence the products. The photocatalytic properties of the two compounds of AgNbO_3 and AgTaO_3 were investigated, the results shown that they have good photocatalytic properties for photodegradation of dyes.
在第1章介绍了有关复合氟化物的相关基本理论知识,对复合氟化物的最新研究进展进行了总结;在第2章中,介绍了水热合成3个钾冰晶石型氟化物,同时介绍了具有锥冰晶石结构化合物K_5V_3F_(14)的合成以及磁性研究;在第3章中,介绍了冰晶石结构的六氟合钒酸盐A_3VF_6(A=K, Na, NH4)以及六氟合铁酸盐A_3FeF_6(M=K, Na, NH4)复合氟化物的水热合成与表征,并详细讨论了合成条件的改变对产物结晶的影响。在第4章中,介绍了Aurivillius结构氟氧化物的水热合成,并详细讨论了合成条件的改变对产物的影响;第5章介绍了钙钛矿结构的AgMO_3(M=Nb, Ta)和BaTaO_3以及烧绿石结构的化合物Cd_2Ta_2O_7的水热合成,结构与表征,并讨论了反应物摩尔比,反应温度和时间等对产物的影响。
本论文详细的阐述了上述化合物的合成条件和方法、结构特点以及性质,并仔细考察了各种影响产物水热稳定性的因素,为进一步研究复合氟氧化物水热合成和性质表征奠定了基础。
Fluoride compounds are usually prepared by tranditional high temperature solid-state methods which require calcination of fluoride raw materials at temperature in excess of 1000℃with frequent grindings. Aothough these methods are adequate for the synthesis of X-ray pure specimens, it is often difficult to control the total oxygen content in the mixed valence systems because of the high temperature used in products of the formation of undesirable phases. Particle size reduction by milling can introduce chemical impurities into the ceramic product, which may severely influence the final properties of fluoride compounds.
Soft chemical methods, such as the use of sol-gel precursors or molten salts as reaction media, have been adopted for the synthesis of oxide, but these methods involve often complex operating procedures. Hydrothermal technique has been widely applied to the synthesis of metastable phases and microporous solids. This method provides an attractive alternative to the synthesis fo complex oxides and fluorides, since it is carried out under relatively mild conditions (autogeneous pressure and～240℃) with controllable particle size distribution of the product. Hydrothermal method, involving heating metal salts, fluorides iin a liquid elevated temperature and pressure, offers an alternative synthesis route for the multicomponent ceramic oxides prepared using the traditional, high-temperature methods of solid-state chemistry: the use fo a solvent would permit rapid mixing fo several chemical elements, leading to homogeneous products, and also offers the potential for control of crystal growth leading to particles of desired morphologies, something rather difficult to achieve when using the high temperatures that must be employed in solid-state reactions. In particular, the hydrothermal method has great scope for the preparation of multinary fluoride phases, i.e. containing two ro more metals, where the rapid mixing fo the constituent elements would provide a great synthetic advantage, as well as potentially leading to the discovery of new materials. In this study, we focus on the hydrothermal crystal growth of fluoride compounds. In the system that has been prepared by traditional methods, a more soft synthesis route is explored and the results are compared with those obtained by other synthesis methods for the purpose to establish the relationship between the synthesis method and properties of final crystalline products.
The complex fluorides K_2NaVF_6, (NH_4)_2VF6 and (NH_4)_2NaVOF_5 with elpasolite-type structure have been synthesized under mild hydrothermal conditions. The details of hydrothermal synthesis conditions deeply discussed. We know that V2O3 is good source of V. F anions is not only a reaction material but also act as a mineralizer in the process. We found that the reducing agent K2S2O3 and (NH_4)_2S2O3 played an ed an important role for the compounds of K_2NaVF_6 and (NH_4)_2NaVF6 respectively, and also they can bring A site cations for the target products. From the experiment we concluded that the reaction condition of compound K_2NaVF_6 as follow: the molar ratio of raw material is V2O3 :NaF :(NH_4)_2S2O3 :NH4HF2 :HF=0.5:1:2:0.1,the temperature is 180℃, the reaction time is 3 days. The synthesis reaction conditions of compound (NH_4)_2NaVF6 as follows: raw materials molar ratio of V_2O_3 :NaF :(NH_4)_2S_2O_3 :NH_4HF_2 :HF=0.5:1:1:7:0.1, reaction temperature is 180℃, the reaction time is 3 days.
The chiolite-type compound of K_5V_3F_(14) was prepared for the first time from hydrothermal system, and deeply discussed the molar ratio of the reaction materials, the reaction conditions: the reaction temperature is 180℃, reaction time is 3 days, during the synthesis processes, the reducing agent of K2S_2O_3 was the critical role because of the raw material of V_2O_3 can be easily oxide by oxygen.
The hexafluoride vanadium(III) K_3VF_6, Na_3VF_6 and (NH_4)_3VF_6 with cryolite-type were prepared for the first time under the mild hydrothermal synthesis. Deeply discussed the molar ratio of the reaction materials, reaction temperature and reaction time that influence the products. Thermal stability of of (NH_4)_3VF_6 and (NH_4)_3FeF_6 were studies by TG-DTA in air. They decomposed in two steps at the first step and losses the compound of NH_4F, and the second step they loss NH_4F.
The perovskite-type oxide compounds of AgMO_3(M = Nb, Ta), BaTaO_3 and the pyrochlore-type compound of Cd_2Ta_2O_7 were prepared for the first time under the hydrothermal synthesis. Deeply discussed the reaction temperature, molar ratio of the reaction materials and reaction time that influence the products. The photocatalytic properties of the two compounds of AgNbO_3 and AgTaO_3 were investigated, the results shown that they have good photocatalytic properties for photodegradation of dyes.
引文
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