Process for microwave synthesis of rare earth compound nano rod

A technology of rare earth compound and microwave synthesis, applied in rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of long reaction time, high reaction temperature, multiple energy sources, etc., and achieve high photon quantum yield and stable chemical properties , low cost effect

Inactive Publication Date: 2007-11-07
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the hydrothermal method requires a higher reaction temperature and a longer reaction time, so it needs to consume more energy.

Method used

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  • Process for microwave synthesis of rare earth compound nano rod
  • Process for microwave synthesis of rare earth compound nano rod
  • Process for microwave synthesis of rare earth compound nano rod

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: prepare La 0.8 Ce 0.2 PO 4 Nano stave

[0017] 0.456g of La 2 o 3 powder and 0.115g of Ce 2 o 3 Powder dissolved in 50mL 10% HNO 3 A mixed solution is formed in the solution, and in the mixed solution La 3+ Ion and Ce 3+ Ion molar ratio La 3+ : Ce 3+ =80:20. Then the pH value of the mixed solution was adjusted to 2.6 with ammonia water. Add 75mL of 0.05mol / L NH under electromagnetic stirring 4 h 2 PO 4 Aqueous solution produces a colloidal precipitate. Finally the jelly thing obtained is transferred to a 250ml round-bottomed flask and placed in a microwave oven, first leading to nitrogen for 30min, then microwave heating for 20min under nitrogen protection and reflux conditions, and the microwave heating power is 80% of maximum power (maximum power is 600W), after heating, continue to pass nitrogen until cooling to room temperature, the precipitated product is fully washed with centrifugation and deionized water, and dried under vacuum at 8...

Embodiment 2

[0018] Embodiment 2: prepare La 0.5 Ce 0.5 PO 4 Nano stave

[0019] 0.815g of La 2 o 3 powder and 0.820g of Ce 2 o 3 Powder dissolved in 35mL 20% HNO 3 A mixed solution is formed in the solution, and in the mixed solution La 3+ Ion and Ce 3+ The molar ratio of ions is La 3+ : Ce 3+ =50:50. Then use ammonia water to adjust the pH value of the mixed solution to 4.5, add 70ml of 0.15M NH under electromagnetic stirring 4 h 2 PO 4 , to generate a colloidal precipitate, transfer the obtained colloid to a 250ml round-bottomed flask and place it in a microwave oven, first pass nitrogen gas for 40 minutes, then microwave for 20 minutes under nitrogen protection and reflux conditions, and the microwave heating power is the maximum power 70% (maximum power is 600W), after heating, continue to pass nitrogen until cooling to room temperature, the precipitated product is fully washed with centrifugation and deionized water, and dried under vacuum at 80°C to obtain La 0.5 Ce ...

Embodiment 3

[0020] Embodiment 3: prepare La 0.95 Eu 0.05 PO 4 Nano stave

[0021] 0.542g of La 2 o 3 powder and 0.031g of Eu 2 o 3 Powder dissolved in 50mL 10% HNO 3 A mixed solution is formed in the solution, and in the mixed solution La 3+ and Eu 3+ The molar ratio of La 3+ :Eu 3+ =95:5. Then use ammonia water to adjust the pH value of the mixed solution to 2.9, add 75ml of 0.05M NH under electromagnetic stirring 4 h 2 PO4 aqueous solution, a colloidal precipitate is formed, and finally the obtained colloid is transferred to a 250ml round-bottomed flask and placed in a microwave oven, first passed nitrogen for 30 minutes, then microwaved for 40 minutes under nitrogen protection and reflux conditions, and the microwave heating power is the maximum 60% of the power (maximum power is 600W), after heating, continue to pass nitrogen to cool to room temperature, the precipitated product is fully washed with centrifugation and deionized water, and dried under vacuum at 80°C to obt...

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Abstract

This invention discloses a micro-wave compound rare earth compound La1-xRexPO4 nanometer bar method, (Re=Ce,Eu or Tb; x=0.05-0.5), the steps as follows: 1) dissolving lanthanum oxidation powder and cerium oxidation, europium oxidation or terbium oxidation powder in nitric acid solution to form mixture solution, 2) adjusting the mixture solution's pH value to 2.5-4.5, disturbing the solution and adding NH4H2PO4 solution to produce gel sediment; 3) heating the gel sediment under the protecting of azote, and then cooling naturally, and then washing the gel sediment with centrifugal separation and ion-doffing water fully, finally collecting it and drying it. The advantage in this invention is that the method is simple, the efficient is high, and it saves energy. The average diameter and length of the nanometer bar made in this invention are 12-17 nanometer, 50-1100 nanometer respectively.

Description

technical field [0001] The invention relates to a preparation method of rare earth compound nanorods, in particular to microwave synthesis of rare earth compound La 1-x Re x PO 4 (Re=Ce, Eu or Tb; x=0.05~0.5) nanorod method. Background technique [0002] Due to the 4f electronic properties of rare earth elements, rare earth compounds have unique physical, chemical, optical, electrical and magnetic properties, and they have a wide range of applications in the fields of electronics, magnetic materials, optoelectronic materials and catalysis. my country is rich in rare earth resources, and the research and preparation of nanomaterials of rare earth compounds has important scientific significance and application value for deepening the utilization of rare earth resources and expanding their new application fields. La 1-x- Re x PO 4 (Re=Ce, Eu, Tb; 0<x<1) is an important double rare earth metal compound, which has high luminous quantum efficiency and unusual magnetic ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/22C01F17/00
Inventor 陈卫祥马琳赵杰黄思玉李翔
Owner ZHEJIANG UNIV
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