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Method of manufacturing aluminium nitride/boron nitride multiple phase ceramic

A technology of multiphase ceramics and boron nitride, which is applied in the field of functional ceramics preparation, can solve the problems of reduced thermal conductivity, high sintering temperature, and low efficiency, and achieve the effect of short sintering time and simple process

Inactive Publication Date: 2007-08-08
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, boric acid and urea generate liquid phase and gas phase boron oxide during the reaction process to oxidize a small amount of aluminum nitride, bringing additional oxygen into the system, and the oxygen content increases from 1.1% to 5.6%, thus greatly increasing the thermal conductivity of the material. Reduced, only 37W / m·K
In addition, hot pressing sintering requires high sintering temperature (1800-1850°C) and long-term heat preservation (2-4 hours), long preparation cycle and very low efficiency, which largely limits the application of such materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Weigh aluminum nitride powder and boron nitride precursor C with an average particle size of 0.2 μm 3 N 6 h 12 B 2 o 6 , where the precursor C 3 N 6 h 12 B 2 o 6 28% by weight, fully mixed in N 2 Calcined at 1300°C for 2 hours in the atmosphere. After cooling, the oxygen content was measured to be 1.3%. Add dysprosium oxide, whose weight accounted for 3% of the final mixture, and ball milled for 3 hours. After drying, put it into a graphite mold and place it in spark plasma sintering (SPS) furnace, pre-fixed pressure 30MPa at room temperature, evacuated to 6Pa, heated up to 1600°C at a rate of 200°C / min for sintering, sintered for 20 minutes, then cooled to 1000°C and kept for 10 minutes, then turned off the power, and then The furnace is cooled to obtain aluminum nitride / boron nitride composite ceramics. The measured bending strength is σ f3 =497MPa, the thermal conductivity is 122W / m·K, and the Vickers hardness is 9.6GPa, which can be used for precision mac...

Embodiment 2

[0015] Weigh aluminum nitride powder and boron nitride precursor C with an average particle size of 0.5 μm 3 N 6 h 12 B 2 o 6 , where the precursor C 3 N 6 h 12 B 2 o 6 37.5% by weight, after mixing well in N 2 Calcined at 1400°C for 1 hour in the atmosphere, and the oxygen content was measured to be 1.5% after cooling; then add samarium oxide, whose weight accounted for 5% of the final mixture, mixed by ball milling for 5 hours, after drying, put it into a graphite mold, and place it in spark plasma sintering (SPS) furnace, pre-fixed pressure 40MPa at room temperature, evacuated to 5Pa, heated up to 1700°C at a rate of 150°C / min for sintering, sintering time was 105 minutes, then cooled to 900°C for 20 minutes and then turned off the power, then The furnace is cooled to obtain aluminum nitride / boron nitride composite ceramics. The measured bending strength is σ f3 =488MPa, the thermal conductivity is 109W / m·K, and the Vickers hardness is 7.4GPa, which can be used f...

Embodiment 3

[0017] Weigh aluminum nitride powder and boron nitride precursor C with an average particle size of 1.2 μm 3 N 6 h 12 B 2 o 6 , where the precursor C 3 N 6 h 12 B 2 o 6 37.5% by weight, after mixing well in N 2 Calcined at 1500°C for 1 hour in the atmosphere, and the oxygen content was measured to be 1.6% after cooling; then added yttrium oxide, whose weight accounted for 8% of the final mixture, mixed by ball milling for 8 hours, after drying, put it into a graphite mold, and placed it in spark plasma sintering (SPS) furnace, pre-fixed pressure 40MPa at room temperature, evacuated to 5Pa, heated up to 1800°C at a rate of 150°C / min for sintering, sintering time was 5 minutes, then cooled to 800°C for 30 minutes, then turned off the power, and then The furnace is cooled to obtain aluminum nitride / boron nitride composite ceramics. The measured bending strength is σ f3 =461MPa, the thermal conductivity is 106W / m·K, and the Vickers hardness is 6.3GPa, which can be used ...

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Abstract

The invention discloses a making method of aluminium nitride / boron nitride multiple phase ceramic in the functional ceramic domain, which comprises the following steps: sintering boron nitride pioneer C3N6H12B2O6 and aluminium nitride particle in the non-oxygen environment; adopting nitrogen or hydrogen as environmental gas; generating pure composite powder of aluminium nitride / boron nitride; dispersing boron nitride in the aluminium nitride base without block; blending the composite powder and one rare earth oxide additive completely; selecting additive from one of yttrium oxide, samarium oxide and dysprosium oxide with yttrium oxide at best; placing in the discharge plasma sintering furnace; extracting into vacuum; heating at 100-200 deg.c / min to 1600-1800 to sinter 5-20 min; insulating at 800-1000 deg.c for 10-30min; closing power; cooling.

Description

technical field [0001] A method for preparing aluminum nitride / boron nitride composite ceramics has the characteristics of high strength, high thermal conductivity and easy machining, and belongs to the technical field of functional ceramic preparation. Background technique [0002] Aluminum nitride ceramics have a series of excellent properties such as high thermal conductivity, and are ideal semiconductor substrate materials and packaging materials for high-power electronic devices. As the development of devices continues to advance toward multi-functionality and miniaturization, materials are required to have high comprehensive performance. From the simple pursuit of single high performance to multi-functionality, it is possible to take into account various performances in complex use environments. Therefore, aluminum nitride ceramics are required not only to have high thermal conductivity and excellent processing performance, but also to maintain high mechanical strength...

Claims

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Application Information

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IPC IPC(8): C04B35/581C04B35/622
Inventor 李永利张久兴
Owner BEIJING UNIV OF TECH
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