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a k 3 zrf 7 Preparation methods of nanocrystals

A nanocrystalline and drying technology, which is applied in the direction of nanotechnology, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as unfavorable to low-cost large-scale industrial production, complicated procedures, etc., achieve crystal stability, shorten reaction time, and easily washing effect

Active Publication Date: 2020-04-03
三亚哈尔滨工程大学南海创新发展基地
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Problems solved by technology

The method is complex in operation and is unfavorable for low-cost and large-scale industrial production of products

Method used

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  • a k  <sub>3</sub> zrf  <sub>7</sub> Preparation methods of nanocrystals
  • a k  <sub>3</sub> zrf  <sub>7</sub> Preparation methods of nanocrystals
  • a k  <sub>3</sub> zrf  <sub>7</sub> Preparation methods of nanocrystals

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Embodiment Construction

[0020] K of the present invention 3 ZrF 7 A method for preparing nanocrystals, comprising the steps of:

[0021] Step 1: According to the ratio of parts by mass (30-50): (40-55), weigh lithium chloride and potassium chloride, mix them evenly, and put them into a dry crucible. The crucible containing lithium chloride and potassium chloride was dried in a muffle furnace at 300°C for 24h. Add K with a mass ratio of 1 / 100 to 1 / 14 to the mixed molten salt after pre-electrolytic dehydration 2 ZrF 6 .

[0022] Step 2: Heat the sample obtained in Step 1 to 650-800° C. under the protection of nitrogen for 3-5 hours to form a precipitate. After the reaction was completed, the upper layer of molten salt was poured out, and the precipitated product was naturally cooled to room temperature.

[0023] Step 3: Take out the reaction product obtained in step 2, wash it with deionized water for 2 to 5 times, and filter it with suction, then take out the washed product and put it in a vacuu...

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Abstract

The invention provides a preparation method of a K3ZrF7 nanocrystalline. The preparation method comprises the steps that (1) LiCl and KCl are added into a crucible to be mixed and stirred uniformly atthe mass part ratio of (30-50) to (40-55), the mixture is placed into a muffle furnace to be dried for 24 hours, and then preelectrolysis dehydration is conducted at the temperature of 500 DEG C to obtain mixed fused salt; (2) K2ZrF6 with the mass ratio of 1 / 100-1 / 14 of the mixed fused salt is added into the crucible and then placed in a heating furnace to be heated till the temperature is 650-800 DEG C, sediment is generated, supernatant fused salt is poured out, and a sedimentary product is obtained; and (3) cooling, washing and drying are conducted. K3ZrF7 prepared by adopting the method is high in purity and fineness, can be used as a base material of rare earth luminescent materials, and has the advantages of being low in price, convenient to prepare and the like.

Description

technical field [0001] What the present invention relates to is a kind of preparation method of nanometer material, specifically a kind of K 3 ZrF 7 Methods of preparing nanocrystals. Background technique [0002] Fluoride nanocrystals are an important class of inorganic functional materials, which are widely used in many frontier fields. K 3 ZrF 7 As a typical representative, due to its inherent low phonon energy (<350cm -1 ) and proved to be the most efficient host material for rare-earth ion-doped conversion (UC), resulting in a reduced nonradiative relaxation rate and enhanced UC efficiency. [0003] At present, it is used internationally to prepare K 3 ZrF 7 The method is: combine KOH and Zr(AC) 4 Put together and heat to 160°C under the protection of nitrogen, add NH after cooling to room temperature 4 F and then heated to 60 ℃, insulation for 30 minutes. Then reheat to 260-300°C, keep warm for 40 minutes, and cool to room temperature. Finally, it was was...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/04B82Y40/00
CPCB82Y40/00C01G25/006C01G25/04C01P2002/72C01P2004/03C01P2004/64
Inventor 杨晓光李春月韩伟李梅王伟杨大伟
Owner 三亚哈尔滨工程大学南海创新发展基地