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A kind of high-entropy rare earth co-doped nanometer low heat transfer powder material and preparation method thereof

A powder material and co-doping technology, which is applied in nanotechnology, chemical instruments and methods, sustainable manufacturing/processing, etc., can solve the problems of short and narrow near-infrared absorption wavelengths, and achieve controllable particle size and crystal grain size. Uniform distribution and single phase effect

Active Publication Date: 2022-07-12
TIANJIN BAOGANG RES INST OF RARE EARTHS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of this, the present invention proposes a high-entropy rare earth co-doped nanometer low heat transfer powder material and its preparation method to solve the problem of existing LaB 6 The problem of short and narrow near-infrared absorption wavelengths of powder materials

Method used

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  • A kind of high-entropy rare earth co-doped nanometer low heat transfer powder material and preparation method thereof
  • A kind of high-entropy rare earth co-doped nanometer low heat transfer powder material and preparation method thereof
  • A kind of high-entropy rare earth co-doped nanometer low heat transfer powder material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] A preparation method of high-entropy rare earth co-doped nanometer low heat transfer powder material, comprising the following steps:

[0053] (1) Set Y 2 (CO 3 ) 3 358g, La 2 (CO 3 ) 3 1373g, EuCl 3 258g, Ce 2 (CO 3 ) 3 460g, Sm 2 (CO 3 ) 3 487g, B 2 O 3 2089g, Na 552g and SiO 2 720g (Y:La:Eu:Ce:Sm:B:Na:SiO 2 The molar ratio was 0.1:0.6:0.1:0.1:0.1:6:24:12) into the autoclave, 15 moles of hydrogen was poured in, the temperature was raised to 320°C and fully stirred for 2 hours, and the obtained product was extracted and fractionated. layer, the precipitation was washed 5 times with suction filtration, dried at 110 °C for 5 hours, then dropped into a sand mill together with 6kg of deionized water to grind a 506-nanometer slurry for 12 hours, and the slurry was sprayed and granulated to obtain a 754-nanometer slurry. The spherical powder is finely granulated by using a high-energy jet mill to obtain an R1 of 246 nm. x R2 y R3 z R4 w R5 n B 6 Pre...

Embodiment 2

[0058] A preparation method of high-entropy rare earth co-doped nanometer low heat transfer powder material, comprising the following steps:

[0059] (1) Ce (NO 3 ) 3 326g, La 2 (CO 3 ) 3 1373g, EuCl 3 258g, NdCl 3 256g, Sm 2 (CO 3 ) 3 487g, B 2 O 3 2089g, Na 552g, SiO 2 720g (Ce:La:Eu:Nd:Sm:B:Na:SiO 2 The molar ratio was 0.1:0.6:0.1:0.1:0.1:6:24:12) into the autoclave, 15 moles of hydrogen was poured in, the temperature was raised to 320°C and fully stirred for 2 hours, and the obtained product was extracted and fractionated. layer, the precipitation was washed with suction filtration water 5 times, dried at 110 ° C for 5 hours, then dropped into a sand mill and ground for 12 hours with 6kg deionized water, the obtained 508-nanometer slurry was sprayed and granulated, and the obtained 781 The nano-sized spherical powder is subjected to secondary grinding with a high-energy jet mill, and the obtained 152-nanometer R1 x R2 y R3 z R4 w R5 n B 6 The precu...

Embodiment 3

[0064] A preparation method of high-entropy rare earth co-doped nanometer low heat transfer powder material, comprising the following steps:

[0065] (1) The EuCl 3 258g, La 2 (CO 3 ) 3 1373g, Sm 2 (CO 3 ) 3 487g, GdCl 3 264g, Ce(NO 3 ) 3 326g, B 2 O 3 2089g, Na 552g, SiO 2 720g (Eu:La:Sm:Gd:Ce:B:Na:SiO 2 The molar ratio was 0.1:0.6:0.1:0.1:0.1:6:24:12) into the autoclave, 15 moles of hydrogen was poured in, the temperature was raised to 320°C and fully stirred for 2 hours, and the obtained product was extracted and fractionated. layer, the precipitation was washed with suction filtration water 5 times, dried at 110 ° C for 5 hours, then dropped into a sand mill together with 6kg of deionized water and ground for 12 hours, the obtained 594-nanometer slurry was sprayed and granulated, and the obtained The spherical powder of 782 nanometers is ground using an air mill, and the obtained R1 of 166 nanometers is x R2 y R3 z R4 w R5 n B 6 The precursor, the pr...

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Abstract

The invention provides a high-entropy rare earth co-doped nanometer low heat transfer powder material and a preparation method thereof, comprising the following steps: (1) putting rare earth source, boron source and intermediate into a high pressure reaction kettle, and flushing hydrogen , heat up to 320-340 ℃ and fully stir for activation, extract and layer the obtained product, carry out suction filtration washing, drying, then wet grinding, spray granulation of the obtained slurry, and granulate the obtained slurry. The spherical powder is dry-milled to obtain a precursor; (2) the precursor is loaded into a rotary kiln for calcination, a hydrogen-nitrogen mixture is introduced into the rotary kiln, the temperature is raised to 900-1200°C, the temperature is kept for 30-450min, and the temperature is lowered. and (3) removing impurities from the initial product to obtain the high-entropy rare earth co-doped nanometer low heat transfer powder material. The high-entropy rare earth co-doped nanometer low heat transfer powder material of the present invention has small scattered and fluffy particle size, low required temperature and low energy consumption.

Description

technical field [0001] The invention belongs to the field of heat insulating powder materials, in particular to a high-entropy rare earth co-doped nanometer low heat transfer powder material and a preparation method thereof. Background technique [0002] The patent of 103663482A discloses a full wet process and a method for synthesizing LaB6 powder in a closed loop. This method obtains the LaB6 bulk material, which needs to be mechanically crushed and then subjected to hydrometallurgy and sulfuric acid leaching to obtain LaB6 powder. The method has low yield and large pollution, and is not suitable for industrial production. [0003] Patent No. 101372340A discloses a multi-element rare earth boride (LaxRe1-x) B6 cathode material and a preparation method thereof. The method adopts SPS sintering and densification to obtain polycrystalline bulk. The preparation process has complex technology, high technical difficulty, expensive equipment, high energy consumption, and requir...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/18B82Y40/00
CPCC01B35/04B82Y40/00C01P2002/72C01P2004/32C01P2004/62Y02P20/10
Inventor 邓冠南刘金龙尹健秦晓婷彭维李璐张光睿
Owner TIANJIN BAOGANG RES INST OF RARE EARTHS
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