CN104694775A - SiC/Al2(WO4)3/Al composite material with adjustable thermal expansion - Google Patents

SiC/Al2(WO4)3/Al composite material with adjustable thermal expansion Download PDF

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CN104694775A
CN104694775A CN201510123392.5A CN201510123392A CN104694775A CN 104694775 A CN104694775 A CN 104694775A CN 201510123392 A CN201510123392 A CN 201510123392A CN 104694775 A CN104694775 A CN 104694775A
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thermal expansion
powder
matrix material
composite material
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CN104694775B (en
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程晓农
张琰琰
陈敏
郭丽萍
杨娟
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Jiangsu Hy Times Electronic Technology Co Ltd
Jiangsu University
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Jiangsu Hy Times Electronic Technology Co Ltd
Jiangsu University
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Abstract

The invention belongs to the technical field of composite materials, and specifically relates to a SiC/Al2(WO4)3/Al composite material with an adjustable thermal expansion. Al is used as a matrix; a low thermal expansion material SiC is used as a reinforcement; meanwhile, a certain amount of Al2(WO4)3 powder is added in for achieving a reduction of the thermal expansion coefficient. Al2(WO4)3 is a negative thermal expansion material that is able to resist a high temperature and is stable in property. On one aspect, Al2(WO4)3 is added in for reducing the thermal expansion coefficient of the original SiC/Al composite material; on the other aspect, Al2(WO4)3 is added in for reducing the content of the highly hard abrasive SiC and increasing the subsequent processing performance of the composite material. The SiC/Al2(WO4)3/Al composite material with the adjustable thermal expansion is prepared by a powder metallurgy technology. The thermal expansion coefficient of the SiC/Al2(WO4)3/Al composite material is significantly lower than that of the SiC/Al composite material. Accordingly, the requirement to the thermal expansion coefficient of electronic packaging materials is met better.

Description

A kind of SiC/Al of adjustable thermal expansion 2(WO 4) 3/ Al matrix material
Technical field
The invention belongs to technical field of composite materials, refer in particular to a kind of SiC/Al of adjustable thermal expansion 2(WO 4) 3/ Al matrix material, by changing low thermal expansion material SiC and negative thermal expansion material Al 2(WO 4) 3mass ratio regulate the thermal expansivity of matrix material.
Background technology
Along with microelectronic device is to high-performance, lightweight and miniaturization development, microelectronics proposes more and more harsher requirement to packaged material, matrix material used for electronic packaging generally uses under the environment of certain temperature change, therefore the thermal dimensional stability in this temperature range will ensure well, and thermal expansivity is a very important parameter; SiC/Al matrix material is a kind of novel electronic package material, its advantage is that the prices of raw and semifnished materials are cheap, only can be shaped as complicated shape, there is high heat conductance simultaneously, high specific strength, high ratio modulus, wear-resistant, the features such as density is low, concerning SiC/Al matrix material, modal method is exactly increase the content of reinforcement SiC to regulate the thermal expansivity of material, and the thermal expansivity of matrix material can be made by 23 × 10 of aluminium -6k -1drop to 7.5 × 10 -6k -1left and right, investigation of materials persons are to this has been large quantity research and report, and achievement in research have also been obtained certain application in Electronic Packaging field; But SiC itself is a kind of high-hardness grinding material, fragility is large, and the volume fraction of SiC is larger, and the machinability of matrix material will decline, and this has a great impact the follow-up machining of material, and the development of SiC/Al matrix material is hindered; Under lower packing volume mark, how to realize the low bulk of matrix material, high thermal conductance, stability and workability is the key issue solving such material practical application, this kind of problem of solution that is found to be of negative thermal expansion material provides possibility, at present, Thermal expansion coefficient of composites is regulated also seldom to have report by negative thermal expansion material and Al base compound.
The present invention is when Al base content is constant, changes SiC content, is filled into negative thermal expansion material Al 2(WO 4) 3, prepare the SiC/ Al that thermal expansivity is adjustable 2(WO 4) 3/ Al matrix material.
Summary of the invention
The object of the invention is when Al base content is constant, change the content of reinforcement SiC, be filled into negative thermal expansion material Al 2(WO 4) 3, prepare the SiC/ Al of adjustable thermal expansion 2(WO 4) 3/ Al matrix material.The thermal expansivity of the matrix material of gained obtains further reduction compared with SiC/Al matrix material, achieves adjustable simultaneously, more close to the thermal expansivity of chip material.
A kind of SiC/ Al of adjustable thermal expansion 2(WO 4) 3/ Al matrix material, raw material used is: SiC, pure Al powder, Al 2(WO 4) 3powder.
Preparation technology is:
(1) SiC powder is claimed in proportion, pure Al powder, Al 2(WO 4) 3powder; Pure Al powder accounts for 40%, SiC and Al of three kinds of powder total masses 2(WO 4) 3account for 60% of three kinds of powder total masses, wherein Al 2(WO 4) 3account for 10 ~ 30% of three kinds of powder total masses; Powder mixes by different ratios.
(2) put in mould by the powder after mixing, suppress on oil press after vibrating compacting, pressure is 5 ~ 7 Mpa, and the dwell time is 1 ~ 3 min, and sample is taken out in the demoulding.
(3) compressing tablet sinters after completing and makes its densification in vacuum tube furnace; Using argon gas and hydrogen as protective atmosphere in stove, the flow of Ar is 1 ~ 1.5 ml/s, H 2flow be 0.3 ~ 0.5 ml/s, sintering temperature is 400 ~ 650 DEG C, and soaking time 1 ~ 3 h, furnace cooling obtains sample.
The median size of described SiC is 20 um.
The diameter of described mould is 10mm.
Al in step 1 2(WO 4) 3optimum quality ratio be 30%.
Optimum pressure in step 2 is 6 Mpa, and the dwell time is 2 min.
Optimal sintering temperature in step 3 is 600 DEG C, and the flow of insulation 3h, shielding gas Ar is 1.5ml/s, H 2flow be 0.3ml/s.
Advantage of the present invention is passing through to add negative thermal expansion material Al 2(WO 4) 3prepare the SiC/ Al of adjustable thermal expansion 2(WO 4) 3/ Al matrix material, its thermal expansivity is (8.6 ~ 4.9) × 10 -6k -1, thermal expansivity is adjustable, and technique is simple.
Take Al as matrix, while low thermal expansion material SiC is reinforcement, by adding appropriate Al 2(WO 4) 3powder realizes the reduction of thermal expansivity; Al 2(WO 4) 3be negative thermal expansion material, high temperature resistant, stable in properties, on the one hand by adding the thermal expansivity that it reduces original SiC/Al matrix material, reducing the content of this high-hardness grinding material of SiC on the other hand, improving the processing characteristics that matrix material is follow-up; The present invention is the SiC/Al being prepared adjustable thermal expansion by the preparation technology of powder metallurgy 2(WO 4) 3al matrix material, SiC/Al 2(WO 4) 3/ Al matrix material compares obvious reduction with the thermal expansivity of SiC/Al matrix material, has better met the needs of electronic package material to thermal expansivity.
Accompanying drawing explanation
Fig. 1 is the thermal dilatometry figure of comparative example 1 matrix material.
Fig. 2 is the thermal dilatometry figure of example 2 matrix material.
Fig. 3 is the thermal dilatometry figure of example 3 matrix material.
Fig. 4 is the thermal dilatometry figure of example 4 matrix material.
Embodiment
comparative example 1
Raw material: Al powder, mass percent is 40%, SiC powder, and mass ratio is 60%.
Get said ratio and powder 0.5 g mixed, loading into diameter is the mould of 10 mm, and suppress on tabletting machine after vibrating compacting, pressure is 6 Mpa, demoulding sampling after pressurize 2 min; Put in vacuum tube furnace after having suppressed and sinter, vacuum oven heats up with 5 DEG C/min temperature rise rate, and when being elevated to 600 DEG C, be incubated 3 h, the flow of shielding gas Ar is 1.5 ml/s, H 2flow be 0.3 ml/s, furnace cooling.
After testing, as shown in Figure 1, the mean thermal expansion coefficients calculating matrix material in 25 ~ 230 DEG C of intervals through linear fit is 9.4 × 10 to thermal dilatometry to gained sample -6k -1.
embodiment 2
Raw material: Al powder, mass percent is 40%, SiC powder, and mass ratio is 50%, Al 2(WO 4) 3powder, mass ratio is 10%.
Get said ratio and powder 0.5 g mixed, loading into diameter is the mould of 10 mm, and suppress on tabletting machine after vibrating compacting, pressure is 6 Mpa, demoulding sampling after pressurize 2 min; Put in vacuum tube furnace after having suppressed and sinter, vacuum oven heats up with 5 DEG C/min temperature rise rate, and when being elevated to 600 DEG C, be incubated 3 h, the flow of shielding gas Ar is 1.5 ml/s, H 2flow be 0.3 ml/s, furnace cooling.
After testing, as shown in Figure 2, the mean thermal expansion coefficients calculating matrix material in 25 ~ 230 DEG C of intervals through linear fit is 8.6 × 10 to thermal dilatometry to gained sample -6k -1.
embodiment 3
Raw material: Al powder, mass percent is 40%, SiC powder, and mass ratio is 40%, Al 2(WO 4) 3powder, mass ratio is 20%.
Get said ratio and powder 0.5 g mixed, loading into diameter is the mould of 10 mm, and suppress on tabletting machine after vibrating compacting, pressure is 6 Mpa, demoulding sampling after pressurize 2 min; Put in vacuum tube furnace after having suppressed and sinter, vacuum oven heats up with 5 DEG C/min temperature rise rate, and when being elevated to 600 DEG C, be incubated 3 h, the flow of shielding gas Ar is 1.5 ml/s, H 2flow be 0.3 ml/s, furnace cooling.
After testing, as shown in Figure 3, the mean thermal expansion coefficients calculating matrix material in 25 ~ 230 DEG C of intervals through linear fit is 7.7 × 10 to thermal dilatometry to gained sample -6k -1.
embodiment 4
Raw material: Al powder, mass percent is 40%, SiC powder, and mass ratio is 30%, Al 2(WO 4) 3powder, mass ratio is 30%.
Get said ratio and powder 0.5 g mixed, loading into diameter is the mould of 10 mm, and suppress on tabletting machine after vibrating compacting, pressure is 6 Mpa, demoulding sampling after pressurize 2 min; Put in vacuum tube furnace after having suppressed and sinter, vacuum oven heats up with 5 DEG C/min temperature rise rate, and when being elevated to 600 DEG C, be incubated 3 h, the flow of shielding gas Ar is 1.5 ml/s, H 2flow be 0.3 ml/s, furnace cooling.
After testing, as shown in Figure 3, the mean thermal expansion coefficients calculating matrix material in 25 ~ 230 DEG C of intervals through linear fit is 4.9 × 10 to thermal dilatometry to gained sample -6k -1.
comparative example 2
Raw material: Al powder, mass percent is 40%, SiC powder, and mass ratio is 20%, Al 2(WO 4) 3powder, mass ratio is 40%.
Get said ratio and powder 0.5 g mixed, loading into diameter is the mould of 10 mm, and suppress on tabletting machine after vibrating compacting, pressure is 6 Mpa, demoulding sampling after pressurize 2 min; Put in vacuum tube furnace after having suppressed and sinter, vacuum oven heats up with 5 DEG C/min temperature rise rate, and when being elevated to 600 DEG C, be incubated 3 h, the flow of shielding gas Ar is 1.5 ml/s, H 2flow be 0.3 ml/s, furnace cooling.
After testing, the mean thermal expansion coefficients that heat calculates matrix material in 25 ~ 230 DEG C of intervals through linear fit is 9.6 × 10 to gained sample -6k -1.

Claims (7)

1. the SiC/Al of an adjustable thermal expansion 2(WO 4) 3/ Al matrix material, is characterized in that:
(1) SiC powder is claimed in proportion, pure Al powder, Al 2(WO 4) 3powder; Pure Al powder accounts for 40%, SiC and Al of three kinds of powder total masses 2(WO 4) 3account for 60% of three kinds of powder total masses, wherein Al 2(WO 4) 3account for 10 ~ 30% of three kinds of powder total masses; Powder mixes by different ratios;
(2) put in mould by the powder after mixing, suppress on oil press after vibrating compacting, pressure is 5 ~ 7 Mpa, and the dwell time is 1 ~ 3 min, and sample is taken out in the demoulding;
(3) compressing tablet sinters after completing and makes its densification in vacuum tube furnace; Using argon gas and hydrogen as protective atmosphere in stove, the flow of Ar is 1 ~ 1.5 ml/s, H 2flow be 0.3 ~ 0.5 ml/s, sintering temperature is 400 ~ 650 DEG C, and soaking time 1 ~ 3 h, furnace cooling obtains sample.
2. the SiC/Al of a kind of adjustable thermal expansion as claimed in claim 1 2(WO 4) 3/ Al matrix material, is characterized in that: the median size of described SiC is 20 um.
3. the SiC/Al of a kind of adjustable thermal expansion as claimed in claim 1 2(WO 4) 3/ Al matrix material, is characterized in that: the diameter of described mould is 10mm.
4. the SiC/Al of a kind of adjustable thermal expansion as claimed in claim 1 2(WO 4) 3/ Al matrix material, is characterized in that: Al in step 1 2(WO 4) 3mass ratio be 30%.
5. the SiC/Al of a kind of adjustable thermal expansion as claimed in claim 1 2(WO 4) 3/ Al matrix material, is characterized in that: the pressure in step 2 is 6 Mpa, and the dwell time is 2 min.
6. the SiC/Al of a kind of adjustable thermal expansion as claimed in claim 1 2(WO 4) 3/ Al matrix material, is characterized in that: the sintering temperature in step 3 is 600 DEG C, and the flow of insulation 3h, shielding gas Ar is 1.5ml/s, H 2flow be 0.3ml/s.
7. the SiC/Al of a kind of adjustable thermal expansion as claimed in claim 1 2(WO 4) 3/ Al matrix material, is characterized in that: its thermal expansivity is 8.6 ~ 4.9 × 10 -6k -1.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106756163A (en) * 2016-11-24 2017-05-31 江苏时代华宜电子科技有限公司 A kind of preparation method of the adjustable composite of thermal expansion
CN111376625A (en) * 2018-12-28 2020-07-07 卡西欧计算机株式会社 Thermally expandable sheet, method for producing thermally expandable sheet, and molded article
CN112410623A (en) * 2019-08-21 2021-02-26 天津大学 High-damping aluminum-silicon-based composite material and preparation method thereof

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106756163A (en) * 2016-11-24 2017-05-31 江苏时代华宜电子科技有限公司 A kind of preparation method of the adjustable composite of thermal expansion
CN111376625A (en) * 2018-12-28 2020-07-07 卡西欧计算机株式会社 Thermally expandable sheet, method for producing thermally expandable sheet, and molded article
CN111376625B (en) * 2018-12-28 2022-01-07 卡西欧计算机株式会社 Thermally expandable sheet, method for producing thermally expandable sheet, and molded article
CN112410623A (en) * 2019-08-21 2021-02-26 天津大学 High-damping aluminum-silicon-based composite material and preparation method thereof
CN112410623B (en) * 2019-08-21 2022-01-07 天津大学 High-damping aluminum-silicon-based composite material and preparation method thereof

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