Method for preparing Aurivillius structure oxyfluoride by low-temperature liquid phase

A technology of oxyfluoride and low-temperature liquid phase, which is applied in chemical instruments and methods, niobium compounds, tantalum compounds, etc., can solve the problems of complex preparation process, high equipment requirements, and difficult synthesis, and achieve simple process and low production cost , the effect of convenient operation

Inactive Publication Date: 2017-03-15
NANCHANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Obviously, the preparation process of this method is complicated, the equipment requirements are high, and the synthesis is difficult

Method used

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  • Method for preparing Aurivillius structure oxyfluoride by low-temperature liquid phase
  • Method for preparing Aurivillius structure oxyfluoride by low-temperature liquid phase
  • Method for preparing Aurivillius structure oxyfluoride by low-temperature liquid phase

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Experimental program
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Effect test

Embodiment 1

[0025] Embodiment 1: niobium bismuth oxyfluoride (Bi 2 NbO 5 F) Preparation.

[0026] 1) Weigh 0.5 mmol of niobium pentoxide, dissolve it in 5 mL of hydrofluoric acid, remove the remaining hydrofluoric acid as much as possible by heating and evaporation, and finally dilute to 10 mL with water.

[0027] 2) Weigh 2mmol of bismuth nitrate and dissolve it in 30mL of ethylene glycol.

[0028] 3) Add the solution in step 1) dropwise to the solution in step 2) under magnetic stirring, and mix well.

[0029] 4) The obtained mixed solution was transferred to a 50mL reaction autoclave, sealed, and reacted at a constant temperature of 150°C for 12 hours, and naturally cooled to room temperature after the reaction.

[0030] 5) The reaction product was suction filtered, washed alternately with water and ethanol several times, and dried at 60°C for 5 hours to obtain Bi 2 NbO 5 F powder product.

Embodiment 2

[0031] Embodiment 2: tantalum bismuth oxyfluoride (Bi 2 TaO 5 F) Preparation.

[0032] 1) Weigh 0.5mmol tantalum pentoxide, dissolve it in 5mL hydrofluoric acid, remove the remaining hydrofluoric acid as much as possible by heating and evaporation, and finally dilute to 10mL with water.

[0033] 2) Weigh 2mmol of bismuth nitrate and dissolve it in 30mL of ethylene glycol.

[0034] 3) Add the solution in step 1) dropwise to the solution in step 2) under magnetic stirring, and mix well.

[0035] 4) The obtained mixed solution was transferred to a 50mL reaction autoclave, sealed, and reacted at a constant temperature of 150°C for 12 hours, and naturally cooled to room temperature after the reaction.

[0036] 5) The reaction product was suction filtered, washed alternately with water and ethanol several times, and dried at 60°C for 5 hours to obtain Bi 2 TaO 5 F powder product.

Embodiment 3

[0037] Embodiment 3: niobium bismuth oxyfluoride (Bi 2 NbO 5 F) Preparation.

[0038] 1) Weigh 1 mmol of niobium pentoxide, dissolve it in 7 mL of hydrofluoric acid, remove the remaining hydrofluoric acid as much as possible by heating and evaporation, and finally dilute to 20 mL with water.

[0039] 2) Weigh 4mmol of bismuth chloride and dissolve it in 20mL of ethanol.

[0040]3) Add the solution in step 1) dropwise to the solution in step 2) under magnetic stirring, and mix well.

[0041] 4) The obtained mixed solution was transferred to a 50mL reaction autoclave, sealed, and reacted at a constant temperature of 150°C for 12 hours, and naturally cooled to room temperature after the reaction.

[0042] 5) The reaction product was suction filtered, washed alternately with water and ethanol several times, and dried at 60°C for 5 hours to obtain Bi 2 NbO 5 F powder product.

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Abstract

The invention discloses a method for preparing Aurivillius structure oxyfluoride by a low-temperature liquid phase, and belongs to the field of inorganic material chemistry. The method is characterized by performing solvothermal reaction for hydrofluoric acid solution of metal oxide (Nb2O5 and Ta2O5) and alcohol solution of bismuth salt; washing the solution to form Aurivillius structure oxyfluoride. The method has the advantages that the method is simple in process, convenient in operation, low in production cost and environmentally friendly and has no special equipment requirements based on low-temperature solvothermal technology, the synthesis technology is a low-temperature liquid phase method, precursors are sufficiently and uniformly mixed, obtained products have a certain micro-nanostructure morphological characteristic, and the method has a good reference function for low-temperature liquid phase synthesis of other oxyfluoride perovskite.

Description

technical field [0001] The invention belongs to the field of inorganic material chemistry and relates to a preparation method of Oliviers type layered perovskite structure oxyfluoride. Background technique [0002] Aurivillius-type compounds are a class of layered bismuth-based oxides whose general formula can be expressed as Bi 2 o 2 (A n-1 B n o 3n+1 ), composed of perovskite [A n-1 B n o 3n+1 ] 2- layer and fluorite type [Bi 2 o 2 ] 2+ Layers are arranged alternately. In these layered perovskite materials, the chemical composition and physical properties can be widely tuned due to the good fit of cation sites. On the other hand, the anion site has a strong influence on both the crystal field and the electronic state of the metal center, and is also of great significance in changing the properties of the material. Oliveris-type oxyfluorides, such as Bi 2 NbO 5 F or Bi 2 TaO 5 F, can be regarded as Bi 2 NbO 6 or Bi 2 TaO 6 One of the oxygen atoms in is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G33/00C01G35/00B82Y40/00
CPCC01G33/006B82Y40/00C01G35/006C01P2002/72C01P2004/03
Inventor 雷水金陈秋林程荻高希杰
Owner NANCHANG UNIV
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