Molten salt synthesis method of rare earth oxyfluoride with cubic crystal form

A technology of rare earth oxides and synthesis methods, which is applied in the direction of rare earth metal halide oxides, rare earth metal compounds, rare earth metal halides, etc., can solve the problems of difficult operation and inapplicability of large-quality samples, and reduce production costs, The synthesis conditions are not harsh and the reaction rate is fast

Active Publication Date: 2020-06-12
INNER MONGOLIA UNIV OF SCI & TECH
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  • Abstract
  • Description
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The rapid cooling technique is difficult to operate a...

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  • Molten salt synthesis method of rare earth oxyfluoride with cubic crystal form
  • Molten salt synthesis method of rare earth oxyfluoride with cubic crystal form

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Embodiment 1

[0045] This embodiment provides a method for synthesizing a molten salt with a cubic rare earth oxyfluoride, comprising the following steps:

[0046] Lithium fluoride, calcium fluoride, neodymium fluoride, and neodymium oxide were uniformly mixed according to the molar ratio of 4:1:3.6:3.6, and placed in a graphite crucible. Then put the graphite crucible into a box-type resistance furnace, control the temperature at 850° C., keep the temperature for 10 minutes, and then cool down with the furnace to obtain the product.

[0047] Result verification: the obtained powder is subjected to X-ray diffractometer (XRD) measurement, and after comparing the obtained X-ray diffraction pattern with the PDF card, it is determined that the generated powder is a cubic NdOF powder, and the result is as follows figure 1 as shown, figure 1 (a) is the X-ray diffraction pattern after comparison of neodymium oxyfluoride and PDF card in Example 1.

Embodiment 2

[0049] This embodiment provides a method for synthesizing a molten salt with a cubic rare earth oxyfluoride, comprising the following steps:

[0050] Lithium fluoride, potassium fluoride, neodymium fluoride, and neodymium oxide were uniformly mixed according to the molar ratio of 1:1:1:1, and placed in a graphite crucible. Then put the graphite crucible into a box-type resistance furnace, control the temperature at 900°C, keep the temperature for 20 minutes, and then cool down with the furnace to obtain the product.

[0051]Result verification: the obtained powder is subjected to X-ray diffractometer (XRD) measurement, and after comparing the obtained X-ray diffraction pattern with the PDF card, it is determined that the generated powder is a cubic NdOF powder, and the result is as follows figure 1 as shown, figure 1 (b) is the X-ray diffraction pattern after comparing the neodymium oxyfluoride and the PDF card in Example 2.

Embodiment 3

[0053] This embodiment provides a method for synthesizing a molten salt with a cubic rare earth oxyfluoride, comprising the following steps:

[0054] Lithium fluoride, sodium fluoride, neodymium fluoride, and neodymium oxide were uniformly mixed according to the molar ratio of 3:2:2:2, and placed in a graphite crucible. Then put the graphite crucible into a box-type resistance furnace, control the temperature at 800° C., keep the temperature for 10 minutes, and then cool down with the furnace to obtain the product.

[0055] Result verification: the obtained powder is subjected to X-ray diffractometer (XRD) measurement, and after comparing the obtained X-ray diffraction pattern with the PDF card, it is determined that the generated powder is a cubic NdOF powder, and the result is as follows figure 1 as shown, figure 1 (c) is the X-ray diffraction pattern after comparison between neodymium oxyfluoride and PDF card in Example 1.

[0056] figure 1 The analysis results in (a)-(c...

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Abstract

The invention discloses a molten salt synthesis method of rare earth oxyfluoride with a cubic crystal form. The method comprises the following steps: mixing rare earth oxide and rare earth fluoride toobtain a rare earth mixture, uniformly mixing the rare earth mixture with alkali metal fluoride and/or alkaline-earth metal fluoride, heating to a temperature higher than the melting point of the mixed fluoride, keeping the temperature for a preset time, and cooling to obtain the rare earth oxyfluoride with the cubic crystal form. According to the synthesis method of rare earth oxyfluoride, the cubic crystal structure of the rare earth oxyfluoride at high temperature can be reserved without quenching, inert atmosphere or reducing atmosphere is not needed as protective atmosphere, the molten salt synthesis reaction rate is far higher than the traditional solid-phase synthesis reaction rate, and the method has the characteristics of simple synthesis process, high synthesis efficiency and low cost.

Description

technical field [0001] The invention relates to a preparation method of rare earth materials, in particular to a method for synthesizing molten salt with cubic rare earth oxyfluoride. Background technique [0002] Rare earth oxyfluoride has attracted much attention because of its stable chemical and thermal properties and low phonon energy. It has been widely used in many fields such as luminescent materials, magnetic materials, microwave absorbing materials, and solid electrolyte materials. It has these unique properties The essential reason is that rare earth oxyfluoride has both REO + cations and O 2- , F - Advantages of anions. [0003] As we all know, the structure of rare earth oxyfluoride is mainly cubic crystal and hexagonal crystal, and the common preparation methods of rare earth oxyfluoride, such as high-temperature solid-phase synthesis, mechanochemical synthesis, solvent synthesis, etc., cannot retain rare earth fluoride oxidation. Cubic crystal structure of...

Claims

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Application Information

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IPC IPC(8): C01F17/259
CPCC01F17/00C01P2002/72Y02E60/10
Inventor 杨育圣赵增武白庆伟
Owner INNER MONGOLIA UNIV OF SCI & TECH
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