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Method for preparing aluminum dodecaboride

A technology of aluminum dodecaboride and aluminum oxide, applied in boron/boride, metal boride, electrolysis process and other directions, can solve the problems of expensive raw materials, complicated process, low output, etc., and achieve control of production cost, low cost, Simple to use effects

Active Publication Date: 2013-03-13
NORTHEASTERN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Aluminum dodecaboride (AlB 12 ) The preparation process mainly includes: (1) with Al, B 2 o 3 As raw material, AlB was prepared by thermal shock sintering 12 ; (2) Vacuum reaction sintering with Al and B as raw materials; (3) KBF 4 , aluminum as raw material, molten salt assisted synthesis to prepare AlB 12 The disadvantages of the above methods are: method (1) complex process, more alumina impurities; method (2) expensive raw materials are limited to laboratory preparation of AlB 12 , and there are alumina impurities; method (3) yield is extremely low

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  • Method for preparing aluminum dodecaboride
  • Method for preparing aluminum dodecaboride

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Embodiment 1

[0017] (1) Preparation of Al 2 o 3 and AlB 12 Mixed powder: mix 45.6wt% aluminum powder with 54.4wt% boron oxide, ball mill for 1 hour to make a mixture, then put the mixture into a graphite crucible, then seal the graphite crucible and put it into a vacuum carbon tube furnace. The vacuum degree is controlled below 50Pa, the temperature is raised to 800°C at a rate of 10°C / min, and vacuum thermal explosion synthesis is carried out to prepare Al 2 o 3 and AlB 12 ; The prepared alumina and aluminum dodecaboride are broken, and the number of crosses is a 160 mesh sieve, so that Al 2 o 3 and AlB 12 The particle diameter of the particle is less than or equal to 96μm; then to the prepared Al 2 o 3 and AlB 12 Add 20% of its mass Al 2 o 3 powder, and mix well;

[0018] (2) Electrolytic preparation: to cryolite Na 3 AlF 6 (3NaF:AlF 3 ) by adding AlF 3 , so that NaF and AlF in cryolite 3 The molecular ratio is 2.1:1, and 1% of its mass of CaF is added to it 2 Prepare a...

Embodiment 2

[0023] (1) Preparation of Al 2 o 3 and AlB 12 Mixed powder: mix 46.9wt% aluminum powder with 53.1wt% boron oxide, ball mill for 2 hours to make a mixture, then put the mixture into a graphite crucible, then seal the graphite crucible and put it into a vacuum carbon tube furnace. The vacuum degree is controlled below 50Pa, the temperature is raised to 700°C at a rate of 10°C / min, and vacuum thermal explosion synthesis is carried out to prepare Al 2 o 3 and AlB 12 ; The prepared alumina and aluminum dodecaboride are broken, and the number of crosses is a 160 mesh sieve, so that Al 2 o 3 and AlB 12The particle diameter is less than or equal to 96μm;

[0024] (2) Electrolytic preparation: to cryolite Na 3 AlF 6 (3NaF:AlF 3 ) by adding AlF 3 , so that NaF and AlF in cryolite 3 The molecular ratio is 2.6:1, and 8% of its mass of CaF is added to it 2 Prepare an electrolyte, the total mass of the electrolyte mixture is 320g, put the electrolyte mixture in the electrolytic...

Embodiment 3

[0027] (1) Preparation of Al 2 o 3 and AlB 12 Mixed powder: mix 46wt% aluminum powder with 54wt% boron oxide, ball mill for 1.5h to make a mixture, then put the mixture into a graphite crucible, then seal the graphite crucible and put it into a vacuum carbon tube furnace, and put the The temperature is controlled below 50Pa, the temperature is raised to 400°C at a rate of 10°C / min, and vacuum thermal explosion synthesis is carried out to prepare Al 2 o 3 and AlB 12 ; The prepared alumina and aluminum dodecaboride are broken, and the number of crosses is a 160 mesh sieve, so that Al 2 o 3 and AlB 12 The particle diameter of the particle is less than or equal to 96μm; then to the prepared Al 2 o 3 and AlB 12 Adding 40% of its mass Al 2 o 3 powder, and mix well;

[0028] (2) Electrolytic preparation: to cryolite Na 3 AlF 6 (3NaF:AlF 3 ) by adding AlF 3 , so that NaF and AlF in cryolite 3 The molecular ratio is 2.4:1, and then add LiF of 12% of its mass to make an...

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Abstract

The invention belongs to the field of material preparation and particularly relates to a method for preparing aluminum dodecaboride. The method comprises the following operation steps of: mixing aluminum powder with boric oxide, carrying out ball milling on the aluminum powder and the boric oxide into mixture, putting the mixture into a graphite crucible, sealing the graphite crucible and putting the graphite crucible into a vacuum carbon tube furnace, carrying out vacuum decrepitation and synthesis, and preparing Al2O3 and AlB12; adding AlF3 into pure cryolite Na3AlF6, uniformly stirring the AlF3 and the pure cryolite Na3AlF6 into electrolyte, adding CaF2 or LiF into the electrolyte, putting mixed materials of the electrolyte into an electrolytic cell, wherein the electrolytic cell is made of high purity graphite, electrifying the electrolytic cell, and adding the Al2O3 and the AlB12 into the electrolytic cell in each 20-25 minutes; and continually taking out electrolysis products located at a negative pole, wherein the electrolysis products are mixtures of Al and the AlB12, carrying out filtering, processing dregs obtained by filtering by hydrochloric acid or sulfuric acid, and finally preparing the aluminum dodecaboride. According to the method for preparing the aluminum dodecaboride, Al powder, B2O3 powder, the Al2O3 and the cryolite which are large in yield and low in cost are taken as main raw materials, the production cost is effectively controlled, and the operation is simple; and the method for preparing the aluminum dodecaboride is suitable for continuous production.

Description

[0001] technical field [0002] The invention belongs to the field of material preparation, in particular to a method for preparing aluminum dodecaboride. Background technique [0003] Aluminum dodecaboride (AlB 12 ) The preparation process mainly includes: (1) with Al, B 2 o 3 As raw material, AlB was prepared by thermal shock sintering 12 ; (2) Vacuum reaction sintering with Al and B as raw materials; (3) KBF 4 , aluminum as raw material, molten salt assisted synthesis to prepare AlB 12 The disadvantages of the above methods are: method (1) complex process, more alumina impurities; method (2) expensive raw materials are limited to laboratory preparation of AlB 12 , and there are alumina impurities; method (3) yield is extremely low. Contents of the invention [0004] Aiming at the problems existing in the prior art, the present invention provides a kind of Al powder, B powder with large output and relatively low cost. 2 o 3 、Al 2 o 3 Aluminum dodecabori...

Claims

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Application Information

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IPC IPC(8): C25B1/00C25C3/06C01B35/04
Inventor 薛向欣王超曹晓舟张建段培宁
Owner NORTHEASTERN UNIV