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Synthesis method of nano rare-earth tetraboride and applications thereof

A technology of nano-rare earth and synthesis method, applied in the direction of boron/boride, metal boride, etc., to achieve the effects of easy removal, lower energy consumption, and lower synthesis temperature

Inactive Publication Date: 2011-05-11
苏玉长
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the past applications of rare earth borides, not much attention has been paid to the influence of particle size on their functionality. Therefore, the preparation and research of nanostructured rare earth borides and their functional applications are not only of scientific value, but also of practical significance.

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  • Synthesis method of nano rare-earth tetraboride and applications thereof
  • Synthesis method of nano rare-earth tetraboride and applications thereof
  • Synthesis method of nano rare-earth tetraboride and applications thereof

Examples

Experimental program
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Embodiment 1

[0031] Weigh chemically pure raw materials in proportion: 162.9g La 2 o 3 , 118.4g C 2 Cl 6 and 215.8g KBH 4 ,

[0032] Mix the raw materials in a planetary ball mill for 1 hour, the ball-to-material ratio is 4:1, the rotating speed is 250RPM, and all the mixed powders pass through a 100-mesh sieve; the above ball-milled mixture is molded into a disc with a diameter of 100mm, Put it into an industrial microwave oven, pre-evacuate the microwave reaction furnace to 10Pa, and then feed 99.99% Ar gas, and the gas flow rate during the synthesis process is 0.5LPM. Use microwave power to control the heating rate, heat at 200°C for 1 hour, then heat at 650°C for 4 hours, cool to room temperature with the furnace, and take out the synthesized product from the dry inert atmosphere. Put the synthetic product into the pre-prepared 800ml HCl aqueous solution with a mass concentration of 3% and stir to dissolve the by-products in the synthetic material, while the nanometer lanthanum te...

Embodiment 2

[0036] Weigh chemically pure raw materials in proportion: 181.3g Gd 2 o 3 , 118.4g C 2 Cl 6 and 151.4 g NaBH 4 ,

[0037] Mix the raw materials in a planetary ball mill for 2 hours, the ratio of balls to materials is 5:1, and the speed is 200RPM. All the mixed powders pass through a 140-mesh sieve; the above ball-milled mixture is molded into a disc with a diameter of 100mm. Put it in an industrial microwave oven, pre-evacuate the microwave reaction furnace to 5Pa, and then pass 99.99% N 2Gas, the gas flow rate during the synthesis process was 0.5 LPM. Use microwave power to control the heating rate, heat at 190°C for 2 hours, then heat at 600°C for 5 hours, cool to room temperature with the furnace, and take out the synthesized product from the dry inert atmosphere. It is the HCl aqueous solution stirring of 4% that the synthetic product is put into pre-equipped 700ml mass concentration to make the by-product dissolving in the synthetic material, and nano gadolinium tet...

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Abstract

The invention relates to a synthesis method of nano rare-earth tetraboride and applications thereof. The nano rare-earth tetraboride (ReB4) is synthesized by utilizing the high microwave absorption performance of a raw material to form a new low-temperature in-situ reaction process. The synthesis method comprises the following steps of: mixing borohydride, rare earth oxide and hexachloroethane and keeping the temperature of 180-220 DEG C for 1h under the protection of argon or N2; heating to 600-700 DEG C and keeping the temperature for 3-5h to prepare the nano rare-earth tetraboride with the grain diameter of 20-200nm and good degree of crystallinity; and washing with hydrochloride water, agglomerating, centrifugating and separating to obtain a finished product with good dispersion in an organic solvent. The method provided by the invention is simple and convenient to industrially produce and has better application prospects in the aspect of a transparent heat-insulating coating material for windows.

Description

Technical field: [0001] The invention relates to a method for synthesizing a nanometer rare earth tetraboride, and also relates to the application of the nanometer rare earth tetraboride in a transparent heat-shielding coating. Background technique: [0002] Rare Earth Borides as ReB 6 、ReB 4 (Re is La, Ce, Y, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu). There are high-temperature and low-temperature reaction preparation methods for the industrial production of rare earth borides. The high-temperature preparation methods mainly include boron carbide reduction rare earth oxide method, boron thermal reduction method, carbothermal reduction method, etc., all of which are prepared by high temperature reaction at 1300 ℃ ~ 1800 ℃. The particle size of the produced borides is coarse, more than tens of microns, and the conventional pulverization method cannot reach the nanometer particle size. Although high-energy ball milling can prepare samples for nanometer research, it is...

Claims

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Application Information

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IPC IPC(8): C01B35/04C03C17/42
Inventor 苏玉长
Owner 苏玉长
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