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Method for synthesizing hexagonal phase TbPO4 H2O nano/micron multi-stage structural material

A synthesis method and technology of structural materials, applied in the field of rare earth phosphates, can solve the problems of unfavorable large-scale production and application, non-recyclable raw materials, high synthesis temperature, etc., and achieve the effects of low raw material prices, easy industrial production, and low reaction temperature

Inactive Publication Date: 2009-07-15
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods have disadvantages such as high synthesis temperature or non-recyclable raw materials, high raw material prices, and environmental pollution, which are not conducive to large-scale production and application.

Method used

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  • Method for synthesizing hexagonal phase TbPO4 H2O nano/micron multi-stage structural material
  • Method for synthesizing hexagonal phase TbPO4 H2O nano/micron multi-stage structural material
  • Method for synthesizing hexagonal phase TbPO4 H2O nano/micron multi-stage structural material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 0.453g Tb(NO 3 ) 3 ·6H 2 O was dissolved in 10mL of distilled water and added dropwise to 10mL of 6mol / L H 3 PO 4 , making it PO 4 The / Tb molar ratio is 60, stirred for 20mim, and transferred to the reaction kettle. React at 100°C for 6 hours, wash with distilled water and absolute ethanol three times, and dry at 60°C to obtain a white powder. XRD pattern shows that the product is hexagonal phase TbPO 4 ·nH 2 O (such as figure 1 a curve in); According to the TG-DSC (thermogravimetric-scanning differential calorimetry) curve, it is calculated that 196.5 ° C loses 1mol of crystal water, and the TG-DSC curve shows that the resulting product is TbPO 4 ·H 2 O (such as figure 2 ); SEM photos show that the resulting product is a hexagonal prism with a diameter of about 700 to 800 nm and a length of several microns with better monodispersity (such as Figure 5 ).

Embodiment 2

[0023] Take 0.680g Tb(NO 3 ) 3 ·6H 2 O was dissolved in 10mL of distilled water and added dropwise to 10mL of 6mol / L H 3 PO 4 , making it PO 4 The / Tb molar ratio is 40, stirred for 20mim, and transferred to the reaction kettle. React at 100°C for 8 hours, wash with distilled water and absolute ethanol three times, and dry at 60°C to obtain a white powder. SEM photos show that the obtained product is a hexagonal prism with a diameter of about 400 to 500 nm and a length of several microns with good monodispersity (such as Image 6 ).

[0024] Spindle-shaped TbPO composed of nanorods 4 ·H 2 Preparation of O nanostructures:

[0025] Embodiment one

[0026] Take 0.680g Tb(NO 3 ) 3 ·6H 2 O was dissolved in 10mL of distilled water and added dropwise to 10mL of 6mol / L H 3 PO 4 , making it PO 4 The / Tb molar ratio is 40, after stirring for 20mim, adjust the pH value of the system to 1.4 with concentrated ammonia water, and transfer it to the reaction kettle. React at 10...

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Abstract

The invention provides a method for synthesizing a hexagonal-phase TbPO4.H2O nano / micro multi level structure material, which belongs to the field of rare-earth phosphate nano / micro multi level structure materials. In the invention, Tb(NO3) 3.6H2O dissolves in water, a certain amount of H3PO4 is added so that the mol rate of PO4Tb in reactant is between 40 and 60, the stirred mixture is transferred to a hydro-thermal reaction kettle to react for 6 to 8 hours at a temperature of 100 DEG C so as to obtain TbPO4.H2O powder in a hexagonal prism; when the mol rate of PO4Tb in the reaction system is between 40 and 60, the pH value is adjusted to between 1.4 and 1.6, the stirred mixture is transferred to the hydro-thermal reaction kettle to react for 6 to 8 hours at a temperature of 100 DEG C so as to obtain spindly TbPO4.H2O powder with a nanometer structure in an even shape. The raw material of H3PO4 can be repeatedly used without expensive surface active agent to be used as a template agent, and the invention has the characteristics that an organic solution is not necessary, the environment is not polluted, the reaction temperature is low, the energy source is saved, the converting rate is high, the industrialized production is easy, and the like.

Description

Technical field: [0001] The invention belongs to the field of rare earth phosphates and relates to a hexagonal phase TbPO 4 ·H 2 O The synthetic method of nanometer / micrometer hierarchical structure material, especially adopt low temperature, non-template agent, non-organic solvent and raw material H 3 PO 4 Reusable Synthetic Hexagonal Phase TbPO 4 ·H 2 O nanomaterials approach. Background technique: [0002] Due to the unique electron layer structure of rare earth elements, rare earth compounds exhibit many excellent optical, electrical and magnetic functions, especially rare earth elements have spectroscopic properties that cannot be compared with general elements. Due to the good chemical stability and thermal stability of rare earth phosphate, rare earth phosphate luminescent materials are widely used in various lighting, display instruments, medicine and military fields. Recently, nano / micro hierarchical structure materials are used in various fields due to their ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/26B82B3/00
Inventor 于然波宝金荣张家芸杨晓丹陈俊邢献然
Owner UNIV OF SCI & TECH BEIJING
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