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Rapid microwave synthetic method of high-quality aluminium nitride powder

A synthesis method, aluminum nitride technology, applied in the direction of nitrogen compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of incomplete reaction, difficult production and application, complex equipment, etc., achieve short holding time, easy maintenance, and synthesis The effect of low temperature

Inactive Publication Date: 2013-10-23
HENGYANG KAIXIN SPECIAL MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the main disadvantages are low efficiency, complex equipment, incomplete reaction, and difficulty in production and application.

Method used

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  • Rapid microwave synthetic method of high-quality aluminium nitride powder
  • Rapid microwave synthetic method of high-quality aluminium nitride powder
  • Rapid microwave synthetic method of high-quality aluminium nitride powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Using aluminum powder with a D50 particle size of 50.4 μm as raw material, 100g of aluminum powder and 3g of ammonium fluoride were evenly mixed, and then mixed with 3g of zinc particles with a diameter of 1mm. figure 1 The positions shown are put into the silicon nitride ceramic sagger 1 successively. Place the silicon nitride ceramic sagger 1 in an intermittent industrial microwave oven for microwave synthesis, inject high-purity nitrogen gas, the pressure is normal pressure, the heating rate is 80°C / min, the synthesis temperature is 1050°C, and the temperature is kept for 0.5 hours to obtain a composite After cooling, it is the finished aluminum nitride powder. The powder color is off-white. After determination, the finished aluminum nitride product contains 33.4% nitrogen, and the XRD analysis phase structure is AlN, such as figure 2 shown.

Embodiment 2

[0030] Use aluminum powder with a particle size of D50 of 0.1mm as raw material, mix 500g of aluminum powder with 25g of ammonium bicarbonate, and press with 25g of zinc block whose length×width×height is 2mm×0.5mm×0.5mm figure 1 The positions shown are put into the silicon nitride ceramic sagger 1 successively. Place the silicon nitride ceramic sagger 1 in a continuous industrial microwave oven for microwave synthesis, inject nitrogen-hydrogen mixed gas containing 5% hydrogen, the pressure is normal pressure, the heating rate is 70°C / min, the synthesis temperature is 1000°C, and the temperature is kept After 1.5 hours, the resulting composition is cooled to become the finished aluminum nitride powder. The powder color is off-white. After determination, the finished aluminum nitride product contains 32.5% nitrogen, and the XRD analysis phase structure is AlN, such as image 3 shown.

Embodiment 3

[0032] Use aluminum powder with a particle size of D50 of 20 μm as raw material, mix 100g of aluminum powder with 4g of ammonium chloride evenly, and press with 2g of zinc particles with a diameter of 2mm figure 1 The positions shown are put into the silicon nitride ceramic sagger 1 successively. Place the silicon nitride ceramic sagger 1 in an intermittent industrial microwave oven for microwave synthesis, inject high-purity nitrogen gas, the pressure is normal pressure, the heating rate is 90°C / min, the synthesis temperature is 1025°C, and the temperature is kept for 1 hour to obtain a composite After cooling, it is the finished aluminum nitride powder. The powder color is off-white. After determination, the finished aluminum nitride product contains 33.2% nitrogen, and the XRD analysis phase structure is AlN.

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Abstract

The invention discloses a rapid microwave synthetic method of a high-quality aluminium nitride powder. According to the method, the aluminium powder is used as a raw material for microwave synthesis. The method provided by the invention comprises the following steps: uniformly mixing D50 aluminium powder with granularity being less than 0.5mm and a certain proportion of ammonium salt in cooperation of a certain proportion of zinc granules or zinc slab of a certain size, firstly placing the zinc granules or zinc slab (3) at the bottom of a silicon nitride ceramic saggar (1), covering the zinc granules or zinc slab (3) with the mixture (2) of aluminium powder and ammonium salt, putting the silicon nitride ceramic saggar filled with the material into a microwave synthesis reaction chamber, blowing a nitrogen-containing gas at normal pressure to carry out microwave synthesis at the heating rate of 10-100 DEG C / min and at the synthesis temperature of 600-1200 DEG C, keeping warm for 0-5h, and cooling an obtained compound so as to obtain the high-quality finished product aluminium nitride powder. Different from a traditional convection, conduction or radiation heating mode, the method provided by the invention is characterized in that heat is generated by coupling of special wave band of microwaves and an infrastructure of the materials, and the whole materials are heated by dielectric loss of the materials. The method provided by the invention has advantages of low synthesis temperature, short time, low energy consumption, good quality, high efficiency, no requirement of subsequent processing and the like.

Description

technical field [0001] The invention relates to a preparation method of inorganic non-metal material aluminum nitride powder, in particular to a microwave rapid synthesis method of high-quality aluminum nitride powder. Background technique [0002] The sintered body of aluminum nitride is a new type of ceramic material. It has a series of excellent properties such as high thermal conductivity, low thermal expansion coefficient, low dielectric constant and dielectric loss, non-toxic, and insulation. It is not only considered It is an ideal material for a new generation of semiconductor substrates and semiconductor packaging, and its application in the electronics industry has been increasingly valued, and it can also be used in components used in high temperature and corrosive environments. Aluminum nitride ceramics have become one of the research hotspots in the field of modern new materials. [0003] However, high-quality aluminum nitride powder is a key factor in determin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/072C04B35/581C04B35/626
Inventor 曾小锋徐助要李勇全
Owner HENGYANG KAIXIN SPECIAL MATERIAL TECH CO LTD
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