Method for preparing hexagonal rare earth tetrafluoride sodium salt material through low-temperature molten salt fluorination

A technology of rare earth tetrafluoride and low temperature molten salt, which is applied in chemical instruments and methods, luminescent materials, rare earth metal compounds, etc., can solve the problems of requiring a large amount of organic solvents and surfactants, complicated preparation methods, etc., and achieve rich raw materials. , The reaction principle is simple, and the particle size is uniform.

Inactive Publication Date: 2020-02-18
黄新阳
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a simple and environment-friendly preparation method of rare earth tetrafluoride sodium salt material in order to solve the technical problem that the existing fluoride material preparation method is complex and requires a large amount of organic solvents and surfactants in the preparation process

Method used

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  • Method for preparing hexagonal rare earth tetrafluoride sodium salt material through low-temperature molten salt fluorination
  • Method for preparing hexagonal rare earth tetrafluoride sodium salt material through low-temperature molten salt fluorination
  • Method for preparing hexagonal rare earth tetrafluoride sodium salt material through low-temperature molten salt fluorination

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Embodiment 1

[0044] A method for preparing a hexagonal phase rare earth tetrafluoride sodium salt material by fluorination of low-temperature molten salt, comprising the following steps:

[0045] (1) Weigh 2mmol Na with an electronic balance 2 CO3 , 1.56 mmol Y 2 o 3 , 0.40mmolYb 2 o 3 , 0.04mmolEr 2 o 3 , pour the weighed medicine into the agate crucible and grind it evenly;

[0046] (2) Then weigh 8mmol NH 4 HF 2 Pour into the grinding in step 1, and grind again until all the medicines are ground evenly to obtain the reaction substance;

[0047] (3) Pour the reaction substance ground in step 2 into a 25ml polytetrafluoroethylene liner, and place it in a water heating tank, seal and tighten the water heating tank, and then put the water heating tank into a blast drying oven , set the reaction temperature to 250 o C, the reaction time is 36h, obtains reaction product;

[0048] (4) After the reaction is over, take out the water heat tank and allow it to cool down to room temperat...

Embodiment 2

[0051] A method for preparing a hexagonal phase rare earth tetrafluoride sodium salt material by fluorination of low-temperature molten salt, comprising the following steps:

[0052] (1) Weigh 2mmol Na with an electronic balance 2 CO 3 , 1.56 mmol Gd 2 o 3 , 0.40mmolYb 2 o 3 , 0.04mmolEr 2 o 3 , pour the weighed medicine into the agate crucible and grind it evenly;

[0053] (2) Then weigh 8mmol NH 4 HF 2 Pour into the grinding in step 1, and grind again until all the medicines are ground evenly to obtain the reaction substance;

[0054] (3) Pour the medicine that has been ground in step 2 into a 25ml polytetrafluoroethylene liner, and place it in a water heating tank, seal and tighten the water heating tank, then put the water heating tank into a blast drying oven, Set the reaction temperature to 270 o C, the reaction time is 36h, obtains reaction product;

[0055] (4) After the reaction is over, take out the water heat tank and allow it to cool down to room temper...

Embodiment 3

[0058] A method for preparing a hexagonal phase rare earth tetrafluoride sodium salt material by fluorination of low-temperature molten salt, comprising the following steps:

[0059] (1) Weigh 2mmol Na with an electronic balance 2 CO 3 , 1.56 mmol Lu 2 o 3 , 0.40mmolYb 2 o 3 , 0.04mmolEr 2 o 3 , pour the weighed medicine into the agate crucible and grind it evenly;

[0060] (2) Then weigh 8mmol NH 4 HF 2 Pour into the grinding in step 1, and grind again until all the medicines are ground evenly to obtain the reaction substance;

[0061] (3) Pour the reaction substance ground in step 2 into a 25ml polytetrafluoroethylene liner, and place it in a water heating tank, seal and tighten the water heating tank, and then put the water heating tank into a blast drying oven , set the reaction temperature to 270 o C, the reaction time is 36h, obtains reaction product;

[0062] (4) After the reaction is over, take out the water heating tank and allow it to cool down to room te...

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Abstract

The invention discloses a method for preparing a rare earth tetrafluoride sodium salt material through low-temperature molten salt fluorination, and belongs to the field of inorganic material preparation. The method is simple and convenient to operate, common cheap substances are used as raw materials, sodium carbonate and sodium bicarbonate are used as sodium sources, and ammonium hydrogen fluoride is used as a fluorinating agent and a fluxing agent. According to the method, the hexagonal rare earth tetrafluoride sodium salt material with uniform size and regular morphology can be prepared. The prepared rare earth doped luminescent fluoride material has strong upconversion fluorescence performance and pure photochromaticity, and has potential application value in the fields of bioluminescence imaging, 3D display and photocatalysis. The preparation method has low requirements on environmental equipment, can be used for large-scale production and is expected to be used for industrial production.

Description

technical field [0001] The invention belongs to the technical field of inorganic micro-nano materials, and in particular relates to a method for preparing a hexagonal phase rare earth tetrafluoride sodium salt material by fluorination of a low-temperature molten salt. [0002] technical background [0003] Rare-earth upconversion inorganic materials have attracted extensive attention in recent decades. Up-conversion luminescent materials can absorb lower-energy photons and radiate higher-energy photons through a multi-photon conversion mechanism. Compared with semiconductor quantum dots, upconversion materials have the following advantages: less toxicity, large Stokes shift, clear emission band, high quantum yield, long lifetime, weak background luminescence, resistance to photobleaching, scintillation and photochemical degradation Therefore, it has broad application prospects in laser, display, anti-counterfeiting, biological imaging, solar cells and other fields. Among th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85C09K11/74B82Y20/00B82Y40/00C01F17/36
CPCB82Y20/00B82Y40/00C01P2002/72C01P2004/03C09K11/7435C09K11/7705C09K11/7733C09K11/7757C09K11/7763
Inventor 黄新阳
Owner 黄新阳
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