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Preparation method for synthesizing nano rare earth boride material at low temperature by microwave heating

A nano-rare earth, microwave heating technology, applied in boron compounds, chemical instruments and methods, chemical/physical/physical-chemical processes of applying energy, etc. The effect of increasing productivity

Active Publication Date: 2022-08-09
TIANJIN BAOGANG RES INST OF RARE EARTHS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In summary, there is still a lack of a synthesis process in the prior art that has simple process conditions, is suitable for scale-up production, and at the same time, has a low synthesis temperature and can produce nano-scale rare earth borides in one step.

Method used

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  • Preparation method for synthesizing nano rare earth boride material at low temperature by microwave heating
  • Preparation method for synthesizing nano rare earth boride material at low temperature by microwave heating
  • Preparation method for synthesizing nano rare earth boride material at low temperature by microwave heating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Nano rare earth boride Sm 0.4 Eu 0.6 B 6 The preparation method specifically comprises the following steps:

[0043] It is to weigh 29.1g of europium chloride hexahydrate, 43.5g of samarium chloride hexahydrate, 27.4g of magnesium diboride and 200g of water and put it into a ball milling jar for ball milling, rotating speed 150r / min, ball milling for 24h, and pour the slurry after completion. Put it into a tray and then put it into an 80°C oven for drying. After drying, it is put into a pulverizer and pulverized to obtain a precursor powder. Put the precursor powder into a quartz crucible, then put it into a vacuum microwave oven, and evacuate it to -0.1MPa. Then turn on the vacuum microwave oven 2350MHz for microwave heating, the temperature is 150°C, and the reaction time is 3min. After the reaction is completed, the crude powder is obtained, and then acid-washed twice with 3 mol / L dilute hydrochloric acid, and then washed twice with water until the pH value reac...

Embodiment 2

[0046] Nano rare earth boride LaB 6 The preparation method specifically comprises the following steps:

[0047] It is to weigh 19.5kg of lanthanum bromide heptahydrate, 6.76kg of magnesium diboride and 10kg of water and put it into a ball mill tank for ball milling, the rotation speed is 300r / min, and the ball milling is 24h. Dry. After drying, it is put into a pulverizer and pulverized to obtain a precursor powder. Put the precursor powder into a quartz crucible, then put it into a vacuum microwave oven, and evacuate it to -0.1MPa. Then turn on the vacuum microwave oven 8000MHz for microwave heating, the temperature is 160°C, and the reaction time is 60min. After the reaction is completed, a crude powder is obtained, which is then acid washed twice with 3 mol / L dilute hydrochloric acid, and then washed twice with water until the pH value reaches 7, and then freeze-dried at -8 °C to obtain pure nanometers. LaB 6 Powder 6kg.

[0048] for the obtained nano-LaB 6 The powde...

Embodiment 3

[0050] Nano rare earth boride Gd 0.2 Ce 0.8 B 6 The preparation method specifically comprises the following steps:

[0051] It is to weigh 2.42kg of gadolinium bromide hexahydrate, 2.55kg of cerium chloride hexahydrate, 3.3kg of magnesium diboride and 3kg of water and put it into a ball mill tank for ball milling, rotating speed 300r / min, ball milling for 24h, and pouring the slurry after completion. Put it into a tray and then put it into a 120°C oven for drying. After drying, it is put into a pulverizer and pulverized to obtain a precursor powder. The precursor powder was placed in a ceramic container, then placed in a vacuum microwave oven, and evacuated to -0.1MPa. Then turn on the vacuum microwave oven 6000MHz for microwave heating, the temperature is 160°C, and the reaction time is 30min. After the reaction is completed, a crude powder is obtained, which is then acid washed twice with 3 mol / L dilute hydrochloric acid, and then washed twice with water until the pH va...

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Abstract

The invention provides a preparation method for synthesizing a nano rare earth boride material at low temperature by microwave heating, which comprises the following steps: (1) weighing a rare earth source and a boron source according to a stoichiometric ratio, putting the rare earth source and the boron source into a ball milling tank for ball milling for 12-48 hours, then drying, and crushing for later use after drying; (2) putting the powder crushed in the step (1) into a container, and carrying out microwave reaction at the reaction temperature of 100-180 DEG C for 3-60 minutes to obtain coarse powder; and (3) carrying out acid pickling and water washing on the coarse powder obtained by the reaction, and drying to obtain the pure rare earth hexaboride. Compared with the existing method for synthesizing the rare earth boride, the preparation method disclosed by the invention has the advantages of simpler raw material composition, more simplified process conditions, short process period, low equipment requirement, high production efficiency, high product yield, high purity and no generation of any dangerous raw materials and byproducts, and is more suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of rare earth boride materials, in particular to a preparation method for synthesizing nanometer rare earth boride materials at low temperature by microwave heating. Background technique [0002] Rare earth boride materials are well-known cathode materials that have been studied theoretically and experimentally for decades. In rare earth borides, metal atoms are embedded in a network of boron cages interconnected by B-B covalent bonds. This unique cage-like structure, the special 4f orbital of rare earth elements and the electron-deficient characteristics of boron element make the material exhibit many excellent properties: low work function, high electrical conductivity, high emission current density, high hardness, Young's High modulus, high melting point, high chemical stability, strong thermal radiation resistance, etc. Rare earth boride materials are widely used and have been successfully used in radar, aerospa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/18B82Y40/00B01J19/12
CPCC01B35/04B82Y40/00B01J19/126C01P2002/72C01P2004/03C01P2004/51B01J2219/00141Y02P20/10
Inventor 秦晓婷刘金龙尹健李璐彭维张光睿赵长玉王安丽
Owner TIANJIN BAOGANG RES INST OF RARE EARTHS
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