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Coprecipitation-carbothermic reduction method for preparing aluminum nitride powder

A technology of aluminum nitride and co-precipitation, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problems of difficult mixing, long reaction time, high reaction temperature, etc., achieve good dispersion performance and improve reactivity , the effect of increasing the reaction rate

Active Publication Date: 2011-02-16
厦门钜瓷科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional carbothermal reduction method usually uses alumina and carbon black as raw materials directly to prepare aluminum nitride powder. After mixing the two evenly, the aluminum nitride powder is prepared by nitriding reaction. Due to the difference in specific gravity and polarity, it is difficult to mix the two. Even, it is easy to cause incomplete reaction; in addition, the reaction temperature is high and the reaction time is long

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Weigh 0.1 mol of aluminum ammonium sulfate, 0.4 mol of ammonium bicarbonate, and 0.2 mol of carbon black. First, dissolve ammonium bicarbonate and ammonium aluminum sulfate in an appropriate amount of deionized water, then add carbon black into the aqueous solution of ammonium aluminum sulfate, stir and mix, and add an appropriate amount of stearic acid as a dispersant while stirring to obtain ammonium aluminum sulfate + carbon Black mixed solution. Then the aluminum ammonium sulfate+carbon black mixed solution is added to the ammonium bicarbonate solution, stirred, and the pH value of the solution is adjusted with ammonia water so that it remains at 9.0, and the precipitate of the obtained aluminum ammonium carbonate+carbon black is filtered through a filter cloth to remove excess water Drain as much as possible, and then place it in an oven to dry at 80°C under an air atmosphere to obtain a precursor. The precursor was reacted for 1 hour under the conditions of 1400°...

Embodiment 2

[0017] Weigh 0.1 mol of ammonium aluminum sulfate, 0.3 mol of ammonium bicarbonate, and 0.4 mol of carbon black. First, dissolve ammonium bicarbonate and ammonium aluminum sulfate in an appropriate amount of deionized water, then add carbon black into the aqueous solution of ammonium aluminum sulfate, stir and mix, and add an appropriate amount of stearic acid as a dispersant while stirring to obtain ammonium aluminum sulfate + carbon Black mixed solution. Then aluminum ammonium sulfate+carbon black mixed solution is added in the ammonium bicarbonate solution, stirred and mixed, the precipitate of boehmite+ammonium aluminum carbonate+carbon black is drained as far as possible through filter cloth, and then placed Dry in an oven at 80°C under an air atmosphere to obtain a precursor. The precursor was reacted for 2 hours under the conditions of 1500° C. and a nitrogen flow rate of 5 l / min, and the reaction product was subsequently decarburized to obtain aluminum nitride powder....

Embodiment 3

[0019] Weigh 0.1 mol of aluminum ammonium sulfate, 0.5 mol of ammonium bicarbonate, and 0.6 mol of carbon black. First, dissolve ammonium bicarbonate and ammonium aluminum sulfate in an appropriate amount of deionized water, then add carbon black into the aqueous solution of ammonium aluminum sulfate, stir and mix, and add an appropriate amount of stearic acid as a dispersant while stirring to obtain ammonium aluminum sulfate + carbon Black mixed solution. Then the aluminum ammonium sulfate+carbon black mixed solution is added to the ammonium bicarbonate solution, stirred, and the pH value of the solution is adjusted with ammonia water so that it remains at 9.0, and the precipitate of the obtained aluminum ammonium carbonate+carbon black is filtered through a filter cloth to remove excess water Drain as much as possible, and then place it in an oven to dry at 80°C under an air atmosphere to obtain a precursor. The precursor was reacted for 2 hours under the conditions of 1600...

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Abstract

The invention discloses a coprecipitation-carbothermic reduction method for preparing aluminum nitride powder, belonging to the field of ceramic powder preparation. An aluminum source is aluminum ammonium sulfate, a carbon source is carbon black, and precipitation is ammonium bicarbonate. The aluminum source and the carbon source are proportioned according to molar ratio; and the precipitation and the aluminum source are proportioned according to molar ratio. The preparation method comprises the following steps of: firstly, respectively solving the ammonium bicarbonate and the aluminum ammonium sulfate in a proper amount of deionized water, and then adding the carbon black to the aqueous solution of aluminum ammonium sulfate and stirring uniformly to obtain a mixed solution of the aluminum ammonium sulfate and the carbon black; mixing the mixed solution of the aluminum ammonium sulfate and the carbon black with the solution of ammonium bicarbonate uniformly to obtain uniform precipitation of the aluminum source and the carbon black, discharging water from the prepared precipitation of the aluminum source and the carbon black through a piece of filter cloth and drying to obtain a precursor; and reacting the precursor under a certain condition, carrying out subsequent decarbonization treatment on reaction products to obtain the aluminum nitride powder. The invention is beneficial to the synthesis of high-purity and fine-grain nanometer-level aluminum nitride ceramic powder under lower reaction temperature condition; in addition, the invention has simple device, strong process controllability and reliability and low production cost, and is suitable for the industrialized production.

Description

technical field [0001] The invention belongs to the technical field of ceramic powder preparation, and in particular provides a method for preparing aluminum nitride ceramic powder by a co-precipitation-carbothermal reduction method. Background technique [0002] Aluminum nitride ceramics have high thermal conductivity, low dielectric constant and dielectric loss, reliable electrical insulation, high temperature resistance, corrosion resistance, non-toxicity, good mechanical properties, and a thermal expansion coefficient that matches silicon. The excellent properties of the series can be applied not only as functional ceramic materials (such as substrates and packaging materials of integrated circuits), but also as structural materials (such as components used in high temperature and corrosive environments). Therefore, aluminum nitride ceramics have become one of the research hotspots in the field of modern new materials. [0003] High-quality powder raw materials are a pr...

Claims

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Application Information

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IPC IPC(8): C04B35/581C01B21/072
Inventor 曲选辉秦明礼储爱民鲁慧峰贾宝瑞
Owner 厦门钜瓷科技有限公司
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