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A kind of preparation method of cubic phase aluminum nitride fiber

A technology of phase aluminum nitride and fiber, applied in the direction of chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., to achieve the effect of simple and feasible process

Active Publication Date: 2016-01-20
CHINA JILIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no report on the preparation of cubic AlN fibers

Method used

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  • A kind of preparation method of cubic phase aluminum nitride fiber
  • A kind of preparation method of cubic phase aluminum nitride fiber

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Experimental program
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Effect test

Embodiment 1

[0016] In a vacuum glove box, weigh 0.01mol of anhydrous aluminum chloride and 0.09mol of tetrabutylammonium azide and dissolve them in 40g of xylene to form a solution with a total mass fraction of solute of 40%, and then add 0.02mol of polyethylene glycol Diol 20000, stirred until completely dissolved to obtain a mixed solution. The mixed solution was transferred to a high-temperature reaction kettle, kept in an oven at 240° C. for 24 h, and cooled naturally to room temperature. The product in the reaction kettle was taken out, washed with xylene, and centrifuged, and repeated three times. The precipitate was collected and dried at 80°C. The dried product was calcined at 800° C. for 4 hours in a vacuum atmosphere, and then taken out and calcined at 500° C. for 4 hours in an air atmosphere to obtain cubic aluminum nitride fibers.

[0017] XRD test result shows, this product is the cubic aluminum nitride of pure phase (see figure 1 ), the SEM photo shows that the product is ...

Embodiment 2

[0019] In a vacuum glove box, weigh 0.01 mol of anhydrous aluminum chloride and 0.09 mol of tetrabutylammonium azide and dissolve them in 18 g of xylene to form a solution with a total mass fraction of solute of 60%, and then add 0.05 mol of hexadecane Alkyltrimethylammonium bromide, stirred until completely dissolved to obtain a mixed solution. The mixed solution was transferred to a high-temperature reaction kettle, kept in an oven at 280° C. for 12 hours, and naturally cooled to room temperature. The product in the reactor was taken out, washed with xylene, centrifuged, and repeated 5 times, and the precipitate was collected and dried at 100°C. The dried product was calcined at 1000° C. for 1 h under the protection of nitrogen, and then taken out and calcined at 700° C. for 1 h under air atmosphere to obtain cubic phase aluminum nitride fibers.

Embodiment 3

[0021] In a vacuum glove box, weigh 0.01 mol of anhydrous aluminum chloride and 0.09 mol of tetrabutylammonium azide and dissolve them in 27 g of xylene to form a solution with a total mass fraction of solute of 50%, and then add 0.04 mol of dodecyl ammonium Alkyl sodium sulfate, stirred until completely dissolved to obtain a mixed solution. The mixed solution was transferred to a high-temperature reaction kettle, kept in an oven at 260° C. for 18 h, and naturally cooled to room temperature. The product in the reaction kettle was taken out, washed with xylene, and centrifuged, and repeated 4 times. The precipitate was collected and dried at 90°C. The dried product was calcined at 900° C. for 2 hours in a vacuum atmosphere, and then taken out and calcined at 600° C. for 2 hours in an air atmosphere to obtain cubic aluminum nitride fibers.

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Abstract

The invention discloses a preparation method of a cubic phase aluminum nitride fiber. The method comprises the following steps: preparing a mixed solution of anhydrous aluminum chloride, tetrabutylammonium azide and a template agent; carrying out solvothermal reaction; washing, centrifuging and drying, so as to obtain a reaction product; burning in vacuum or inert atmosphere, so that the attached template agent cracks; and burning in air atmosphere to remove organic matters, so as to obtain the cubic phase aluminum nitride fiber. The cubic phase aluminum nitride fiber is directly prepared by taking azide and an inorganic salt of aluminum as raw materials and an organic matter surfactant as a template by a solvothermal method, so that the technological process is simple and feasible, and the morphology of the cubic phase aluminum nitride fiber can be regulated and controlled by controlling the temperature and time of the solvothermal reaction and adding different template agents.

Description

technical field [0001] The invention relates to a method for preparing aluminum nitride fibers, in particular to a method for preparing cubic phase aluminum nitride fibers, and belongs to the technical field of material science. Background technique [0002] Aluminum nitride has high thermal conductivity, good electrical insulation, low dielectric constant and dielectric loss, and a thermal expansion coefficient that matches silicon. It is considered to be the most ideal substrate material and electronic device packaging material today. . Aluminum nitride fiber has both the excellent characteristics of aluminum nitride material and fiber material, and has broad application prospects in the fields of electronics, metallurgy and aerospace. [0003] Aluminum nitride has two crystal phases, a stable hexagonal phase and a metastable cubic phase. For the hexagonal aluminum nitride fibers of the stable phase, its preparation technology is relatively mature, and there have been a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/072
Inventor 杨清华王焕平徐时清雷若姗邓德刚汤雨诗
Owner CHINA JILIANG UNIV
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