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Preparation method of in-situ-synthesized composite aluminum nitride powder comprising sintering aid

A sintering aid and in-situ synthesis technology, applied in the field of ceramic powder preparation, can solve problems such as inability to compound, and achieve the effects of avoiding the introduction of oxygen and other impurities, improving sinterability, and avoiding product agglomeration

Active Publication Date: 2013-05-08
内蒙古盛和芯材科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the defect that main alloying elements such as Li and alkaline earth metal elements in the prior art cannot be compounded into sintering aids, so as to provide an in-situ preparation containing sintering aids with simple production process and large-scale production. Process method of composite aluminum nitride powder

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Using pure metal aluminum and lithium as raw materials, the binary alloy is smelted in an intermediate frequency induction furnace according to the proportion of Al-Li5wt%. Put the alloy into a corundum crucible and put it into a nitriding furnace; vacuumize the furnace cavity and feed it with NH 3 / H 2 Mixed gas, H 2 The content is 50%, and the pressure of the reaction chamber is controlled to 0.7atm, so that the oxygen partial pressure in the reaction chamber is less than 0.1Pa; the temperature is raised to 550°C, and the low-temperature nitriding is performed for 5 hours; the heating is continued to 1400°C, and the high-temperature nitriding is carried out for 5 hours; The nitriding product, after pulverization, the off-white LiAlO containing LiAlO 2 Phase AlN powder.

[0021] The composite AlN powder obtained in this example has an average particle size of 1.3 μm and a specific surface area of ​​2.4 m 2 / g.

Embodiment 2

[0023] Using pure metal aluminum and magnesium as raw materials, the binary alloy is smelted in an intermediate frequency induction furnace according to the proportion of Al-Mg0.5wt%. Put the alloy into a corundum crucible and put it into a nitriding furnace; vacuumize the furnace cavity and feed it with NH 3 / H 2 Mixed gas, H 2 The content is 70%, and the pressure of the reaction chamber is controlled to 0.8atm, so that the oxygen partial pressure in the reaction chamber is less than 0.1Pa; the temperature is raised to 750°C, and the low-temperature nitriding is carried out for 1h; the heating is continued to 850°C, and the high-temperature nitriding is carried out for 10h; The nitriding product, after pulverization, an off-white MgAl-containing 2 o 4 Phase AlN powder.

[0024] The composite AlN powder obtained in this example has an average particle size of 1.5 μm and a specific surface area of ​​2.2 m 2 / g.

Embodiment 3

[0026] Using pure metal aluminum and calcium as raw materials, the binary alloy is smelted in an intermediate frequency induction furnace according to the proportion of Al-Ca15wt%. Put the alloy into a corundum crucible and put it into a nitriding furnace; vacuumize the furnace cavity and feed it with NH 3 / H 2 Mixed gas, H 2 The content is 1%, and the pressure of the reaction chamber is controlled to be 0.5atm, so that the oxygen partial pressure in the reaction chamber is less than 0.1Pa; the temperature is raised to 650°C, and the low-temperature nitriding is carried out for 3 hours; the heating is continued to 1000°C, and the high-temperature nitriding is carried out for 5 hours; The nitrided product, after pulverization, an off-white CaAl-containing 2 o 4 Phase AlN powder.

[0027] The composite AlN powder obtained in this example has an average particle size of 1.1 μm and a specific surface area of ​​2.9 m 2 / g.

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Abstract

The invention relates to the field of ceramic powder preparation, and provides a preparation method of in-situ-synthesized composite aluminum nitride powder comprising a sintering aid. The method is characterized in that aluminum alloy is adopted as a raw material; reaction chamber gas pressure intensity is controlled, and the composite aluminum nitride powder is synthesized in-situ under a mixed atmosphere of NH3 / H2. The method mainly comprises the steps that: molten aluminum is adopted as a raw material, wherein alloying elements are Li and alkaline earth metal element; the alloy is placed in a nitriding furnace; the furnace is vacuumed, and NH3 / H2 mixed gas is delivered in; pressure intensity in the reaction chamber is controlled at 0.5-1atm; the nitriding process is divided into two steps, wherein low-temperature nitriding is carried out for 1-5h under a temperature range of 550-750 DEG C, the temperature is increased to a range of 850-1400 DEG C, and a high-temperature nitriding reaction is carried out for 1-10h; and the in-situ-synthesized composite aluminum nitride powder comprising the sintering aid is obtained after cooling. The aluminum nitride powder provided by the invention has the advantages of no agglomeration, fine particles, and good sintering performance. The method has the advantages of wide raw material source, low production cost, simple production process, and suitability for large-scale productions.

Description

technical field [0001] The invention belongs to the field of ceramic powder preparation, and in particular relates to a process method for synthesizing composite aluminum nitride powder by an in-situ method. Background technique [0002] Aluminum nitride (AlN) ceramics have a series of excellent properties such as high thermal conductivity, high electrical insulation, high strength, high hardness, corrosion resistance, non-toxicity, and thermal expansion coefficient matching silicon, and have broad application prospects. [0003] The preparation and performance of aluminum nitride ceramics are obviously affected by factors such as powder purity, particle size, and sintering performance. Therefore, the preparation of aluminum nitride powder with excellent performance is very important. At present, the preparation methods of aluminum nitride powder mainly include the direct nitriding method of aluminum powder and the carbon thermal reduction method of alumina. However, these ...

Claims

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Application Information

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IPC IPC(8): C04B35/582C04B35/626
Inventor 王群张耀辉王澈
Owner 内蒙古盛和芯材科技有限责任公司