Preparation method of dispersed fluffy MB6 nano low-heat-transfer powder material

A kind of powder material and nanotechnology, which is applied in the field of preparation of evacuated and fluffy MB6 nanometer low heat transfer powder material, can solve the problems of difficult separation and purification of powder, long atomic diffusion path, incomplete reaction, etc., and achieve high added value of products , controllable particle size and low cost of raw materials

Active Publication Date: 2022-05-24
TIANJIN BAOGANG RES INST OF RARE EARTHS
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  • Application Information

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Problems solved by technology

These methods all belong to the category of solid-state reaction methods, which have disadvantages such as high reaction temperature (1500-2000°C), high energy consumption, long atomic diffusion path, incomplete reaction, etc., which easily lead to large particle size, uneven particles, impurities, etc. Many, low surface activity, etc.
CN106395843B discloses a kind of molten salt method synthetic LaB 6 The method of nano-powder, when the synthetic powder is prepared in batches by this method, it takes a long time and the efficiency is low, it is difficult to break the molten salt after solidification, and it is difficult to separate and purify the powder from the molten salt

Method used

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  • Preparation method of dispersed fluffy MB6 nano low-heat-transfer powder material
  • Preparation method of dispersed fluffy MB6 nano low-heat-transfer powder material
  • Preparation method of dispersed fluffy MB6 nano low-heat-transfer powder material

Examples

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Effect test

Embodiment 1

[0036] An evacuated fluffy CaB 6 The preparation method of nanometer low heat transfer powder material comprises the following steps:

[0037] (1) According to the ratio of Ca:B molar ratio of 1:6, weigh CaCO 3 1010g, B 2 O 3 2089g put it and 6kg deionized water into a sand mill and grind for 8 hours to obtain a 146nm powder precursor;

[0038](2) The precursor is loaded into the rotary furnace, and the filling height of the precursor is 3 cm. After the sealed rotary furnace is filled with 8% hydrogen-nitrogen gas at a rate of 100 mL / min for 1 min, the temperature starts to rise. The first heating stage: room temperature To 200°C, the heating rate is 7°C / min, keep warm for 30min, the ventilation rate is 2mL / min, the inclination angle of the rotary furnace is 15°, and the rotation rate is 10rpm; the second heating stage: from 200°C to 470°C, the heating rate is 7°C / min, heat preservation 30min, ventilation rate 5mL / min, rotary furnace inclination angle 10°, rotation spee...

Embodiment 2

[0042] An evacuated fluffy EuB 6 The preparation method of nanometer low heat transfer powder material comprises the following steps:

[0043] (1) According to the ratio of Eu:B molar ratio of 1:6, weigh Eu(NO 3 ) 3 3380g, B2O3 2089g, put it and 6kg deionized water into a sand mill and grind for 8 hours to obtain a 142nm powder precursor;

[0044] (2) The precursor is loaded into the rotary furnace, and the filling height of the precursor is 3 cm. After the sealed rotary furnace is filled with 8% hydrogen-nitrogen gas at a rate of 100 mL / min for 1 min, the temperature starts to rise. The first heating stage: room temperature To 200°C, the heating rate is 7°C / min, keep warm for 30min, the ventilation rate is 2mL / min, the inclination angle of the rotary furnace is 15°, and the rotation rate is 10rpm; the second heating stage: from 200°C to 470°C, the heating rate is 7°C / min, heat preservation 30min, ventilation rate 5mL / min, rotary furnace inclination angle 10°, rotation sp...

Embodiment 3

[0048] A loose fluffy SmB 6 The preparation method of nanometer low heat transfer powder material comprises the following steps:

[0049] (1) According to the ratio of Sm:B molar ratio of 1:6, weigh SmCl respectively 3 2567.2g, B 2 o 3 2089g put it and 6kg deionized water into a sand mill and grind for 8.5 hours to obtain a 143nm powder precursor;

[0050] (2) The precursor is loaded into the rotary furnace, and the filling height of the precursor is 3 cm. After the sealed rotary furnace is filled with 8% hydrogen-nitrogen gas at a rate of 100 mL / min for 1 min, the temperature starts to rise. The first heating stage: room temperature To 200°C, the heating rate is 7°C / min, keep warm for 30min, the ventilation rate is 2mL / min, the inclination angle of the rotary furnace is 15°, and the rotation rate is 10rpm; the second heating stage: from 200°C to 470°C, the heating rate is 7°C / min, heat preservation 30min, ventilation rate 5mL / min, rotary furnace inclination angle 10°, ...

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Abstract

The invention provides a preparation method of a dispersed fluffy MB6 nano low-heat-transfer powder material. The preparation method comprises the following steps: step 1, grinding metal M cations and a boron source to obtain an MB6 precursor; 2, the MB6 precursor is loaded into a rotary furnace to be calcined, hydrogen and nitrogen mixed gas is introduced into the rotary furnace, the temperature is increased to 850-1200 DEG C, heat preservation is conducted for 30-450 min, and a head product is obtained after cooling; and step 3, removing impurities from the primary product to obtain the dispersed and fluffy MB6 nano low-heat-transfer powder material. The powder material disclosed by the invention is loose and fluffy in powder, small in particle size, relatively low in required temperature, low in energy consumption, low in cost of required raw materials, simple in batch preparation and suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of thermal insulation powder materials, in particular to an evacuated fluffy MB 6 The invention relates to a preparation method of a nano low heat transfer powder material. Background technique [0002] Metal borides are used in many fields due to their unique structures and properties. MB 6 (M=Mg, Ca, Sr, Ba, La, etc.) has a CsCl-type crystal structure, in which the metal atoms are located at the center of the cube, and the 8 corner positions are occupied by regular octahedrons composed of B atoms. These metal borides have the advantages of high melting point, high hardness, low work function, low evaporation rate, stable chemical properties and resistance to ion bombardment, as well as good thermal conductivity and electrical conductivity. And M x B 6 Nanoparticles have excellent near-infrared absorption properties due to the small size effect, surface effect, quantum effect and macroscopic quantum tunneling ef...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/04B82Y40/00
CPCC01B35/04B82Y40/00C01P2004/62C01P2004/32C01P2002/72C01P2004/52Y02P20/10
Inventor 邓冠南张光睿尹健秦晓婷刘金龙彭维李璐
Owner TIANJIN BAOGANG RES INST OF RARE EARTHS
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