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CN103011777A - Low-temperature aluminium oxide powder and multifunctional aluminium oxide ceramic heat sink as well as manufacturing method thereof - Google Patents

Low-temperature aluminium oxide powder and multifunctional aluminium oxide ceramic heat sink as well as manufacturing method thereof Download PDF

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CN103011777A
CN103011777A CN 201210519262 CN201210519262A CN103011777A CN 103011777 A CN103011777 A CN 103011777A CN 201210519262 CN201210519262 CN 201210519262 CN 201210519262 A CN201210519262 A CN 201210519262A CN 103011777 A CN103011777 A CN 103011777A
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temperature
weight
heat sink
oxidation aluminium
ceramic heat
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李俊
丁萍
欧阳晖传
谢胜和
黄礼侃
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NANJING ZHONGJIANG NEW MATERIAL TECHNOLOGY Co Ltd
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Abstract

The invention discloses a low-temperature aluminium oxide powder. The low-temperature aluminium oxide powder comprises the following materials in weight ratio: 90-95wt% of aluminium oxide powder with the specific surface area of 3-7m<2>/g, 1-5wt% of high-thermal-conductive low-temperature aluminium oxide with the specific surface area of 12-18m<2>/g and 3-5wt% of sintering aid which comprises 27.4wt% of CaO, 32.6t% of SiO2 and 0.4wt% of TiO2. The invention also discloses a manufacturing method of a multifunctional aluminium oxide ceramic heat sink. The manufacturing method comprises the steps of blending the low-temperature aluminium oxide powder, pelleting, carrying out injection molding, degreasing and sintering at a low temperature. The invention also discloses the multifunctional aluminium oxide ceramic heat sink manufactured by the manufacturing method. According to the invention, the multifunctional aluminium oxide ceramic heat sink can keep a high theoretical density and relative density while being sintered at a low temperature so that the multifunctional aluminium oxide ceramic heat sink has preferable mechanics, electricity and thermal properties.

Description

Aluminum oxide low temperature powder and multi-functional oxidation aluminium ceramic heat sink and preparation method thereof
Technical field
The present invention relates to alumina ceramic material, alumina-ceramic and preparation method thereof, relate in particular to a kind of aluminum oxide low temperature powder, and a kind of multi-functional oxidation aluminium ceramic heat sink and preparation method thereof.
Background technology
Development along with science and technology, the particularly development of the energy, space technology, automotive industry etc., requirement for radiating element and material thereof is more and more harsher, in today of energy growing tension, in the urgent need to developing various novel radiator with high performance spares and the traditional aluminium of material substitution thereof.Alumina-ceramic is because high, high temperature resistant, the good insulating, corrosion-resistant of intensity, and has good electromechanical properties, is widely used in the industries such as electronics, machinery, chemical industry.
Radiating element with the alumina ceramic material manufacture more and more is widely used, and especially multi-functional oxidation aluminium ceramic heat sink has become the product that replaces Aluminium Radiator spare gradually.Generally prepare on the market general 95% alumina ceramic material that adopts of alumina-ceramic scatterer product material, traditional normal temperature and pressure sintering, it is inhomogeneous to exist the temperature field, and thermal stresses is larger, and efficiency is low, pollute the shortcomings such as larger.Although the HIP sintering method can reduce the sintering degree, because need to seal or presintering biscuit, pressure condition is relatively harsher, also is unsuitable for realizing suitability for industrialized production.The normal temperature and pressure sintering temperature is generally at 1560-1600 ℃, and production cost is high, and the net heat conductance becomes porcelain body density at 3.5-3.68g/cm3 generally at 20-24w/m ' k.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, and a kind of aluminum oxide low temperature powder is provided, and a kind of multi-functional oxidation aluminium ceramic heat sink and preparation method thereof also is provided.The multi-functional oxidation aluminium pottery that uses this aluminum oxide low temperature powder made is sintering at a lower temperature, can make again it keep higher theoretical density and relative density simultaneously, thereby have preferably mechanics, electricity, thermal property.The making method of this multi-functional oxidation aluminium ceramic heat sink makes the alumina-ceramic scatterer at a lower temperature when sintering, can make again it keep higher theoretical density and relative density, thereby have preferably mechanics, electricity, thermal property.This multi-functional oxidation aluminium ceramic heat sink is sintering at a lower temperature, can make again it keep higher theoretical density and relative density simultaneously, thereby have preferably mechanics, electricity, thermal property.
For solving the problems of the technologies described above, the technical scheme that the present invention takes is: aluminum oxide low temperature powder is characterized in that comprising following component:
The specific surface area of 90~95wt% (weight) is 3~7m 2/ g's is alumina powder jointed; The specific surface area of 1~5wt% (weight) is 12~18m 2The high heat conduction low-temperature oxidation aluminium powder body of/g; The sintering aid of 3-5wt% (weight);
Described combustion adjuvant comprises the SiO of CaO, the 32.6t% (weight) of 27.4wt% (weight) 2And the TiO of 0.4wt% (weight) 2
The another kind of technical scheme that the present invention takes is: the making method of multi-functional oxidation aluminium ceramic heat sink is characterized in that may further comprise the steps:
The first step, modulation aluminum oxide low temperature powder: at first, be 3~7m with specific surface area 2Alumina powder jointed and the specific surface area of/g is 12~18m 2The high heat conduction low-temperature oxidation aluminium powder body of/g mixes, and adds deionized water as medium again, then the three is evenly mixed; Then use zirconium oxide balls ball milling 2-4 hour, form mixed powder; Ball milling carries out drying treatment with mixed powder, the basis of formation powder after finishing; Secondly, in basic powder, add sintering aid, with described basic powder and both mixing of sintering aid, form aluminum oxide low temperature powder; Described aluminum oxide low temperature powder kind, specific surface area is 3~7m 2Alumina powder jointed, the specific surface area of/g are 12~18m 2The high heat conduction low-temperature oxidation aluminium powder body of/g and sintering aid three's content are respectively 90~95wt% (weight), 1~5wt% (weight) and 3-5wt% (weight); Described sintering aid is by the SiO of CaO, the 32.6t% (weight) of 27.4wt% (weight) 2And the TiO of 0.4wt% (weight) 2Mix and form;
Second step, granulation: in aluminum oxide low temperature powder, mix the crystallite high temperature paraffin of 11-15% (weight) and the oleic acid of 0.5-1% (weight), form mixture; Then under 150-200 ℃ of temperature, that mixture is evenly mixing, will through the bulk that forms after evenly mixing or sheet compound through pulverizing or extrude cutting, form the particulate state feeding again;
The 3rd step, injection molding: with the particulate state feeding under 155-165 ℃ temperature and under the pressure of 80-200MPa high speed injection in mould, after to be cooled the solidifying, form multi-functional oxidation aluminium ceramic heat sink base substrate;
The 4th step, degreasing: by type of heating, the organism in the multi-functional oxidation aluminium of the moulding ceramic heat sink base substrate is got rid of, obtained multi-functional oxidation aluminium ceramic heat sink biscuit; Described type of heating comprises warming up period, absorption phase and evaporation phase; The described evaporation phase comprises successively evaporation first phase, evaporation second phase and evaporated for three phases; With the preheating of multi-functional oxidation aluminium ceramic heat sink base substrate process preheater, then pass through resorber, finally by the pervaporation phase first; The described evaporation phase is used for the organism in the multi-functional oxidation aluminium ceramic heat sink biscuit is evaporated; In described warming up period, preheating temperature is raised to 100 ℃ gradually from room temperature, and the heating-up time is 60-120min; In described absorption phase, absorption temperature is raised to 200 ℃ gradually from 100 ℃, and the heating-up time is 120-180min, absorbs with the hot gas with multi-functional oxidation aluminium ceramic heat sink biscuit outside; In described evaporation first phase, vaporization temperature is raised to 300 ℃ gradually from 200 ℃, and the heating-up time is 180-240min; Within the evaporation second phase, vaporization temperature is raised to 600 ℃ gradually from 300 ℃, and the heating-up time is 120-180min; Within three phases of evaporation, vaporization temperature is raised to 1000 ℃ gradually from 600 ℃, and the heating-up time is 120-180min;
The 5th step, low-temperature sintering: under normal pressure, adopt energy saving and environment friendly material molecule self-friction microwave heating sintering technology, with multi-functional oxidation aluminium ceramic heat sink biscuit sintering densification, form multi-functional oxidation aluminium ceramic heat sink; Sintering temperature is 1380-1450 ℃, and sintering time is 1.5-2H.
As further improved technical scheme of the present invention, in the injection molding step, with the particulate state feeding under 160 ℃ temperature and under the pressure of 80-200MPa high speed injection in mould, after to be cooled the solidifying, form multi-functional oxidation aluminium ceramic heat sink base substrate.
As further improved technical scheme of the present invention, in the low-temperature sintering step, temperature rise rate is 3-8 ℃/min before 600 ℃., be 5-10 ℃/min at 600 ℃ of-1450 ℃ of temperature rise rates.
The third technical scheme that the present invention takes is: a kind of multi-functional oxidation aluminium ceramic heat sink that adopts the making method made of above-mentioned multi-functional oxidation aluminium ceramic heat sink.
The multi-functional oxidation aluminium pottery that uses aluminum oxide low temperature powder made of the present invention is sintering at a lower temperature, can make again it keep higher theoretical density and relative density simultaneously, thereby have preferably mechanics, electricity, thermal property.The making method of this multi-functional oxidation aluminium ceramic heat sink makes the alumina-ceramic scatterer at a lower temperature when sintering, can make again it keep higher theoretical density and relative density, thereby have preferably mechanics, electricity, thermal property.This multi-functional oxidation aluminium ceramic heat sink is sintering at a lower temperature, can make again it keep higher theoretical density and relative density simultaneously, thereby have preferably mechanics, electricity, thermal property.In a word, the present invention is take aluminum oxide low temperature powder as basic material, adopt energy saving and environment friendly material molecule self-friction microwave sintering process technology, make multi-functional oxidation aluminium ceramic heat sink at a lower temperature when sintering, can make again it keep higher theoretical density and relative density, thereby have preferably mechanics, electricity, thermal property.
Description of drawings
Fig. 1 is integrated multi-functional alumina-ceramic electric refrigeration heat radiator structural representation of the present invention.
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described further.
Embodiment
Embodiment 1
This aluminum oxide low temperature powder comprises following component:
The specific surface area of 90~95wt% (weight) is 3~7n 2/ g's is alumina powder jointed; The specific surface area of 1~5wt% (weight) is 12~18m 2The high heat conduction low-temperature oxidation aluminium powder body of/g; The sintering aid of 3-5wt% (weight);
Described combustion adjuvant comprises the SiO of CaO, the 32.6t% (weight) of 27.4wt% (weight) 2And the TiO of 0.4wt% (weight) 2
The multi-functional oxidation aluminium ceramic heat sink that uses this aluminum oxide low temperature powder made is sintering at a lower temperature, can make again it keep higher theoretical density and relative density simultaneously, thereby have preferably mechanics, electricity, thermal property.When reducing the sintering cost, the technological advantage of the multi-functional oxidation aluminium ceramic heat sink of making and product advantage are referring to table 1 and table 2.
Embodiment 2
The making method of this multi-functional oxidation aluminium ceramic heat sink is characterized in that may further comprise the steps:
The first step, modulation aluminum oxide low temperature powder: at first, be 3~7m with specific surface area 2Alumina powder jointed and the specific surface area of/g is 12~18m 2The high heat conduction low-temperature oxidation aluminium powder body of/g mixes, and adds deionized water as medium again, then the three is evenly mixed; Then use zirconium oxide balls ball milling 2-4 hour, form mixed powder; Ball milling carries out drying treatment with mixed powder, the basis of formation powder after finishing; Secondly, in basic powder, add sintering aid, with described basic powder and both mixing of sintering aid, form aluminum oxide low temperature powder; Described aluminum oxide low temperature powder kind, specific surface area is 3~7m 2Alumina powder jointed, the specific surface area of/g are 12~18m 2The high heat conduction low-temperature oxidation aluminium powder body of/g and sintering aid three's content are respectively 90~95wt% (weight), 1~5wt% (weight) and 3-5wt% (weight); Described sintering aid is by the SiO of CaO, the 32.6t% (weight) of 27.4wt% (weight) 2And the TiO of 0.4wt% (weight) 2Mix and form.
Second step, granulation: in aluminum oxide low temperature powder, mix the crystallite high temperature paraffin of 11-15% (weight) and the oleic acid of 0.5-1% (weight), form mixture; Then under 150-200 ℃ of temperature, that mixture is evenly mixing, will through the bulk that forms after evenly mixing or sheet compound through pulverizing or extrude cutting, form the particulate state feeding again;
The 3rd step, injection molding: with the particulate state feeding under 155-165 ℃ temperature and under the pressure of 80-200MPa high speed injection in mould, after to be cooled the solidifying, form multi-functional oxidation aluminium ceramic heat sink base substrate;
The 4th step, degreasing: by type of heating, the organism in the multi-functional oxidation aluminium of the moulding ceramic heat sink base substrate is got rid of, obtained multi-functional oxidation aluminium ceramic heat sink biscuit; Described type of heating comprises warming up period, absorption phase and evaporation phase; The described evaporation phase comprises successively evaporation first phase, evaporation second phase and evaporated for three phases; With the preheating of multi-functional oxidation aluminium ceramic heat sink base substrate process preheater, then pass through resorber, finally by the pervaporation phase first; The described evaporation phase is used for the organism in the multi-functional oxidation aluminium ceramic heat sink biscuit is evaporated; In described warming up period, preheating temperature is raised to 100 ℃ gradually from room temperature, and the heating-up time is 60-120min; In described absorption phase, absorption temperature is raised to 200 ℃ gradually from 100 ℃, and the heating-up time is 120-180min, absorbs with the hot gas with multi-functional oxidation aluminium ceramic heat sink biscuit outside; In described evaporation first phase, vaporization temperature is raised to 300 ℃ gradually from 200 ℃, and the heating-up time is 180-240min; Within the evaporation second phase, vaporization temperature is raised to 600 ℃ gradually from 300 ℃, and the heating-up time is 120-180min; Within three phases of evaporation, vaporization temperature is raised to 1000 ℃ gradually from 600 ℃, and the heating-up time is 120-180min;
The 5th step, low-temperature sintering: under normal pressure, adopt energy saving and environment friendly material molecule self-friction microwave heating sintering technology, with multi-functional oxidation aluminium ceramic heat sink biscuit sintering densification, form multi-functional oxidation aluminium ceramic heat sink; Sintering temperature is 1380-1450 ℃, and sintering time is 1.5-2H.
In the present embodiment, in the injection molding step, with the particulate state feeding under 160 ℃ temperature and under the pressure of 80-200MPa high speed injection in mould, after to be cooled the solidifying, form multi-functional oxidation aluminium ceramic heat sink base substrate; In the low-temperature sintering step, temperature rise rate is 3-8 ℃/min before 600 ℃., be 5-10 ℃/min at 600 ℃ of-1450 ℃ of temperature rise rates.Energy saving and environment friendly material molecule self-friction microwave heating sintering technology adopts prior art.
Compared with prior art, the present invention adopts the new prescription of homemade aluminum oxide low temperature powder as basic material, with energy saving and environment friendly material molecule self-friction microwave sintering process, and when reducing the sintering cost, its technological advantage such as table 1, property advantage such as table 2:
Table 1: the preferential comparison sheet of technique
Figure BSA00000818553700051
Table 2: the product performance comparison sheet of the multi-functional oxidation aluminium ceramic heat sink that present embodiment is made
Figure BSA00000818553700052
Embodiment 3
This multi-functional oxidation aluminium ceramic heat sink adopts the making method of 2 kinds of described multi-functional oxidation aluminium ceramic heat sinks of embodiment to be made, and no longer describes in detail.Weight is 435g before the sample moulding de-waxing; Weight is behind the sintering: 378g; Recording density with drainage is 3.73-3.85g/cm 3, the structure behind the sintering as shown in Figure 1.

Claims (5)

1. aluminum oxide low temperature powder is characterized in that comprising following component:
The specific surface area of 90~95wt% (weight) is 3~7m 2/ g's is alumina powder jointed; The specific surface area of 1~5wt% (weight) is 12~18m 2The high heat conduction low-temperature oxidation aluminium powder body of/g; The sintering aid of 3-5wt% (weight); (" wt% ")
Described combustion adjuvant comprises the SiO2 of CaO, 32.6t% (weight) of 27.4wt% (weight) and the TiO of 0.4wt% (weight) 2
2. the making method of a multi-functional oxidation aluminium ceramic heat sink is characterized in that may further comprise the steps:
The first step, modulation aluminum oxide low temperature powder: at first, be 3~7m with specific surface area 2Alumina powder jointed and the specific surface area of/g is 12~18m 2The high heat conduction low-temperature oxidation aluminium powder body of/g mixes, and adds deionized water as medium again, then the three is evenly mixed; Then use zirconium oxide balls ball milling 2-4 hour, form mixed powder; Ball milling carries out drying treatment with mixed powder, the basis of formation powder after finishing; Secondly, in basic powder, add sintering aid, with described basic powder and both mixing of sintering aid, form aluminum oxide low temperature powder; Described aluminum oxide low temperature powder kind, specific surface area is 3~7m 2Alumina powder jointed, the specific surface area of/g are 12~18m 2The high heat conduction low-temperature oxidation aluminium powder body of/g and sintering aid three's content are respectively 90~95wt% (weight), 1~5wt% (weight) and 3-5wt% (weight); Described sintering aid is by the SiO of CaO, the 32.6t% (weight) of 27.4wt% (weight) 2And the TiO of 0.4wt% (weight) 2Mix and form;
Second step, granulation: in aluminum oxide low temperature powder, mix the crystallite high temperature paraffin of 11-15% (weight) and the oleic acid of 0.5-1% (weight), form mixture; Then under 150-200 ℃ of temperature, that mixture is evenly mixing, will through the bulk that forms after evenly mixing or sheet compound through pulverizing or extrude cutting, form the particulate state feeding again;
The 3rd step, injection molding: with the particulate state feeding under 155-165 ℃ temperature and under the pressure of 80-200MPa high speed injection in mould, after to be cooled the solidifying, form multi-functional oxidation aluminium ceramic heat sink base substrate;
The 4th step, degreasing: by type of heating, the organism in the multi-functional oxidation aluminium of the moulding ceramic heat sink base substrate is got rid of, obtained multi-functional oxidation aluminium ceramic heat sink biscuit; Described type of heating comprises that warming up period, absorption phase and evaporation phase evaporate the evaporation of the organism in the product; The described evaporation phase comprises successively evaporation first phase, evaporation second phase and evaporated for three phases; With the preheating of multi-functional oxidation aluminium ceramic heat sink base substrate process preheater, then pass through resorber, finally by the pervaporation phase first; The described evaporation phase is used for the organism in the multi-functional oxidation aluminium ceramic heat sink biscuit is evaporated; In described warming up period, preheating temperature is raised to 100 ℃ gradually from room temperature, and the heating-up time is 60-120min; In described absorption phase, absorption temperature is raised to 200 ℃ gradually from 100 ℃, and the heating-up time is 120-180min, absorbs with the hot gas with multi-functional oxidation aluminium ceramic heat sink biscuit outside; In described evaporation first phase, vaporization temperature is raised to 300 ℃ gradually from 200 ℃, and the heating-up time is 180-240min; Within the evaporation second phase, vaporization temperature is raised to 600 ℃ gradually from 300 ℃, and the heating-up time is 120-180min; Within three phases of evaporation, vaporization temperature is raised to 1000 ℃ gradually from 600 ℃, and the heating-up time is 120-180min;
The 5th step, low-temperature sintering: under normal pressure, adopt energy saving and environment friendly material molecule self-friction microwave heating sintering technology, with multi-functional oxidation aluminium ceramic heat sink biscuit sintering densification, form multi-functional oxidation aluminium ceramic heat sink; Sintering temperature is 1380-1450 ℃, and sintering time is 1.5-2H.
3. the making method of multi-functional oxidation aluminium ceramic heat sink according to claim 3, it is characterized in that: in the injection molding step, with the particulate state feeding under 160 ℃ temperature and under the pressure of 80-200MPa high speed injection in mould, after to be cooled the solidifying, form multi-functional oxidation aluminium ceramic heat sink base substrate.
4. according to claim 2 or the making method of 3 described multi-functional oxidation aluminium ceramic heat sinks, it is characterized in that: in the low-temperature sintering step, temperature rise rate is 3-8 ℃/min before 600 ℃., be 5-10 ℃/min at 600 ℃ of-1450 ℃ of temperature rise rates.
5. multi-functional oxidation aluminium ceramic heat sink that adopts the making method made of claim 2 or 3 described multi-functional oxidation aluminium ceramic heat sinks.
90~95wt%'s (weight) is alumina powder jointed; The high heat conduction low-temperature oxidation aluminium powder body of 1~5wt% (weight); The sintering aid of 3-5wt% (weight);
Described combustion adjuvant comprises the SiO of CaO, the 32.6t% (weight) of 27.4wt% (weight) 2And the TiO of 0.4wt% (weight) 2
CN 201210519262 2012-12-06 2012-12-06 Low-temperature aluminium oxide powder and multifunctional aluminium oxide ceramic heat sink as well as manufacturing method thereof Pending CN103011777A (en)

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Cited By (6)

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CN103360040A (en) * 2013-07-22 2013-10-23 南京中江新材料科技有限公司 Alumina ceramic material having high thermal conductivity and low-temperature microwave sintering method thereof
CN104370546A (en) * 2014-10-28 2015-02-25 倪娟形 High-thermal conductivity ceramics for radiator connector and preparation method of high-thermal conductivity ceramics
CN105254286A (en) * 2015-09-11 2016-01-20 西宁科进工业设计有限公司 High-heat-conduction ceramic material and manufacturing method therefor
CN108025980A (en) * 2015-09-16 2018-05-11 大日精化工业株式会社 Alumina series thermal conductivity oxide and its manufacture method
CN108610026A (en) * 2018-07-11 2018-10-02 广东昭信照明科技有限公司 Aluminium oxide ceramics heat-radiating substrate preparation method and aluminium oxide ceramics heat-radiating substrate
CN110483085A (en) * 2019-08-01 2019-11-22 广东工业大学 A kind of whisker reinforcement alumina composite ceramic and the preparation method and application thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103360040A (en) * 2013-07-22 2013-10-23 南京中江新材料科技有限公司 Alumina ceramic material having high thermal conductivity and low-temperature microwave sintering method thereof
CN104370546A (en) * 2014-10-28 2015-02-25 倪娟形 High-thermal conductivity ceramics for radiator connector and preparation method of high-thermal conductivity ceramics
CN105254286A (en) * 2015-09-11 2016-01-20 西宁科进工业设计有限公司 High-heat-conduction ceramic material and manufacturing method therefor
CN108025980A (en) * 2015-09-16 2018-05-11 大日精化工业株式会社 Alumina series thermal conductivity oxide and its manufacture method
CN108025980B (en) * 2015-09-16 2021-12-21 大日精化工业株式会社 Alumina-based thermally conductive oxide and method for producing same
CN108610026A (en) * 2018-07-11 2018-10-02 广东昭信照明科技有限公司 Aluminium oxide ceramics heat-radiating substrate preparation method and aluminium oxide ceramics heat-radiating substrate
CN110483085A (en) * 2019-08-01 2019-11-22 广东工业大学 A kind of whisker reinforcement alumina composite ceramic and the preparation method and application thereof
CN110483085B (en) * 2019-08-01 2022-10-04 广东工业大学 Whisker reinforced alumina composite ceramic and preparation method and application thereof

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