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Preparation method of rare earth fluoride in air

A rare earth fluoride and fluoride technology, applied in the field of rare earth fluoride, can solve the problems of danger, expensive raw materials, high pressure, etc., achieve good water and acid resistance and stability, simple preparation method, and reduce the effect of sintering temperature

Inactive Publication Date: 2012-10-24
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the sol-gel method has disadvantages: the reaction takes a long time, the raw material is expensive, the sintering property between the gel particles is poor, and the product shrinks greatly when it is dried.
The hydrothermal method is a new method for the synthesis of ultrafine powder developed in recent years. The main difference between the hydrothermal method and other soft chemical methods such as sol-gel method and co-precipitation method is that the temperature is lower and the pressure is higher, and high pressure resistance is required. The equipment is used to complete the experiment, which is potentially dangerous and not easy for industrial mass production

Method used

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  • Preparation method of rare earth fluoride in air
  • Preparation method of rare earth fluoride in air
  • Preparation method of rare earth fluoride in air

Examples

Experimental program
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Effect test

Embodiment 1

[0032] The molecular formula of synthetic fluoride is NaYbF 4 . Weigh 2.1731 g Yb 2 o 3 , dissolved with nitric acid to form a rare earth salt solution, and ammonium bicarbonate was added to adjust the pH value of the rare earth salt solution to 6. Then weigh 1.8873 grams of precipitant NH 4 F, and dissolved in deionized water to prepare a precipitant solution. Add excess precipitant solution to rare earth salt solution at room temperature, and magnetically stir the mixed solution. Stop stirring, stand still, get rare earth fluoride YbF 3 precipitation. Wash the precipitate by adding deionized water several times by decantation until the pH value of the washing solution is 7. Precipitate YbF 3 Add to distilled water and stir magnetically to form a suspension. Add 0.4631 g of NaF solution to the suspension to obtain a mixed solution. In an atmosphere without hydrogen fluoride in the air, and magnetically stirred, the mixture was heated at 80°C for 36 hours to obtain n...

Embodiment 2

[0034] The molecular formula of synthetic fluoride is LiYbF 4 . Weigh 2.3093 g Yb 2 o 3 , dissolved with hydrochloric acid to form a rare earth salt solution, adding ammonia water to adjust the pH value of the rare earth salt solution to 6.5. Then weigh 1.2 g of precipitant NH 4 HF 2 , and dissolved in deionized water to prepare a precipitant solution. Add excess precipitant solution to rare earth salt solution at room temperature, and magnetically stir the mixed solution. Stop stirring, stand still, get rare earth fluoride YbF 3 precipitation. Use a high-speed centrifuge to separate and wash the precipitate until the pH of the washing solution is 7. Precipitate YbF 3 Add to distilled water and stir magnetically to form a suspension. Add 0.3040 g of liF solution to the suspension to obtain a mixed solution. In the air without hydrogen fluoride atmosphere, and magnetic stirring, the mixture was heated at 120°C for 72 hours to obtain nano-sized LiYbF with a particle s...

Embodiment 3

[0036] The molecular formula of synthetic fluoride is NaYb 0.92 Er 0.08 f 4 . Weigh 2.0026 g Yb 2 o 3 and 0.1691 g Er 2 o 3 , Dissolve with hydrochloric acid, and heat the solution to evaporate water to make it close to dryness, then add deionized water to dilute to form a rare earth salt solution. Then weigh 1.8905 g of precipitant NH 4 HF 2 , and dissolved in deionized water to prepare a precipitant solution. Add excess precipitant solution to rare earth salt solution at room temperature, and magnetically stir the mixed solution. Stop stirring, stand still, get rare earth fluoride Yb 0.92 Er 0.08 f 3 precipitation. Use a high-speed centrifuge to separate and wash the precipitate until the pH of the washing solution is 7. Precipitate Yb 0.92 Er 0.08 f 3 Add to distilled water and stir magnetically to form a suspension. Add 0.4639 g of NaF solution to the suspension to obtain a mixed solution. In an atmosphere without hydrogen fluoride in the air, and magnet...

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Abstract

The invention discloses a preparation method of rare earth fluoride in air, which comprises the following steps of dissolving rare earth element oxide by using acid and deionized water to form a rare earth salt solution; adding a precipitator into the rare earth salt solution and stirring to obtain a rare earth fluoride precipitate; adding deionized water into the precipitate and stirring to forma turbid liquid; and adding fluoride solution of M element in the turbid solution to obtain a liquid mixture. The method can not only realize uniform doping of rare earth ions without high-temperature sintering under an atmosphere of hydrogen fluoride, but also can avoid the problem of proportion mismatching of rare earth ions and other ions during the synthesis, has simple operation and good repeatability, can be used for synthesizing hundreds of sizes of rare earth fluorides and can carry out the batch production. The obtained product has uniform grain distribution, good dispersity and highstability, can be widely applied to the laser technology, fiber optical amplifiers, anti-counterfeiting materials, three primary color display materials, light conversion films of solar cells, and fluorescent marks for biological detection and analysis.

Description

technical field [0001] The invention relates to the technical field of rare earth material synthesis, in particular to a method for synthesizing rare earth fluorides of different sizes in air at 80-120°C. Background technique [0002] Due to its special 4f electronic structure, rare earth elements have optical, electrical, magnetic and thermal properties that many other elements do not have, so they can be made into many new materials that can be used in high-tech, known as the "treasure house" of new materials " and the "vitamins" of human industry. my country is rich in rare earth resources, and the research and preparation of rare earth compounds has important strategic scientific significance and application value for deepening the utilization of rare earth resources and expanding their new application fields. At present, the rare earth materials involved in the application include rare earth fluorine (chloride) compounds, rare earth oxides, rare earth composite oxides ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/622C04B35/50
Inventor 颜晓红王祥夫
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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