CN104694775B - A kind of SiC/Al of adjustable thermal expansion2(WO4)3/ Al composite - Google Patents
A kind of SiC/Al of adjustable thermal expansion2(WO4)3/ Al composite Download PDFInfo
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- CN104694775B CN104694775B CN201510123392.5A CN201510123392A CN104694775B CN 104694775 B CN104694775 B CN 104694775B CN 201510123392 A CN201510123392 A CN 201510123392A CN 104694775 B CN104694775 B CN 104694775B
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Abstract
The invention belongs to technical field of composite materials, refer in particular to a kind of SiC/Al of adjustable thermal expansion2(WO4)3/ Al composite.With Al as matrix, while low thermal expansion material SiC is reinforcement, by adding appropriate Al2(WO4)3Powder is realizing the reduction of thermal coefficient of expansion；Al2(WO4)3It is negative thermal expansion material, high temperature resistant, stable in properties, on the one hand by adding the thermal coefficient of expansion that it reduces original SiC/Al composite, on the other hand reduce the content of this high-hardness grinding material of SiC, improve the follow-up processing characteristics of composite；The present invention is to prepare the SiC/Al of adjustable thermal expansion by the preparation technology of powder metallurgy2(WO4)3Al composite, SiC/Al2(WO4)3Obvious reduction compared by/Al composite with the thermal coefficient of expansion of SiC/Al composite, has better met the needs to thermal coefficient of expansion for the electronic package material.
Description
Technical field
The invention belongs to technical field of composite materials, refer in particular to a kind of SiC/Al of adjustable thermal expansion2(WO4)3/ Al composite wood
Material, by changing low thermal expansion material SiC and negative thermal expansion material Al2(WO4)3Mass ratio swollen come the heat to adjust composite
Swollen coefficient.
Background technology
With microelectronic component to high-performance, lightweight and miniaturization develop, and microelectronics proposes to encapsulating material
Increasingly harsher requirement, composite used for electronic packaging typically uses, therefore at this in the environment of uniform temperature change
Thermal dimensional stability in individual temperature range will ensure well, and thermal coefficient of expansion is a critically important parameter；SiC/Al is combined
Material is a kind of new electronic package material, and its advantage is that the prices of raw materials are cheap, can only be shaped as complicated shape, have simultaneously
There is a high heat conductance, high specific strength, high ratio modulus, wear-resistant, the low feature of density, for SiC/Al composite, most common
Method be just to increase the content of the reinforcement SiC thermal coefficient of expansion to adjust material, the thermal expansion system of composite can be made
Count by the 23 × 10 of aluminum-6K-1Drop to 7.5 × 10-6K-1Left and right, investigation of materials person have carried out numerous studies and report to this, grind
Study carefully achievement and also obtain certain application in Electronic Packaging field；But SiC is a kind of high-hardness grinding material in itself, fragility is big, SiC
Volume fraction bigger, the machinability of composite will decline, and this is subsequently machined with very big shadow to material
Ring, make the development of SiC/Al composite hindered；How to realize the low swollen of composite under relatively low packing volume fraction
Swollen, highly thermally conductive, stability and machinability are the key issues solving such material practical application, negative thermal expansion material
Such issues that be found to be solution provides possibility, at present, is combined with negative thermal expansion material and Al base that to adjust composite heat swollen
Swollen coefficient also seldom has been reported that.
The present invention is in the case that Al base content is constant, changes SiC content, is filled into negative thermal expansion material Al2
(WO4)3, prepare the adjustable SiC/Al of thermal coefficient of expansion2(WO4)3/ Al composite.
Content of the invention
The purpose of the present invention is in the case that Al base content is constant, changes the content of reinforcement SiC, is filled into negative heat swollen
Swollen materials A l2(WO4)3, prepare the SiC/Al of adjustable thermal expansion2(WO4)3/ Al composite.The heat of the composite of gained is swollen
Swollen coefficient has obtained reducing further compared with SiC/Al composite, is simultaneously achieved adjustable, is more nearly chip material
Thermal coefficient of expansion.
A kind of SiC/Al of adjustable thermal expansion2(WO4)3/ Al composite, raw material used is：SiC, pure Al powder, Al2
(WO4)3Powder.
Preparation technology is：
(1) SiC powder, pure Al powder, Al are claimed in proportion2(WO4)3Powder；Pure Al powder account for three kinds of powder gross masses 40%, SiC and
Al2(WO4)3Account for the 60% of three kinds of powder gross masses, wherein Al2(WO4)3Account for the 10～30% of three kinds of powder gross masses；Powder is pressed
Different proportion mix homogeneously.
(2) by after mix homogeneously powder put into mould in, after vibrating compacting on hydraulic press suppress, pressure be 5～
7MPa, the dwell time is 1～3min, and sample is taken out in the demoulding.
(3) after the completion of tabletting, in vacuum tube furnace, sintering makes its densification；Using argon and hydrogen as shielding gas in stove
Atmosphere, the flow of Ar is 1～1.5ml/s, H2Flow be 0.3～0.5ml/s, sintering temperature is 400～650 DEG C, temperature retention time 1
～3h, furnace cooling is obtained sample.
The mean diameter of described SiC is 20um.
A diameter of 10mm of described mould.
Al in step 12(WO4)3Optimum quality ratio be 30%.
Optimum pressure in step 2 is 6MPa, and the dwell time is 2min.
Optimal sintering temperature in step 3 is 600 DEG C, is incubated 3h, the flow of protective gas Ar is 1.5ml/s, H2Stream
Measure as 0.3ml/s.
It is an advantage of the invention that by adding negative thermal expansion material Al2(WO4)3Prepare the SiC/Al of adjustable thermal expansion2
(WO4)3/ Al composite, its thermal coefficient of expansion is (8.6～4.9) × 10-6K-1, thermal coefficient of expansion is adjustable, and process is simple.
With Al as matrix, while low thermal expansion material SiC is reinforcement, by adding appropriate Al2(WO4)3Powder comes real
The reduction of existing thermal coefficient of expansion；Al2(WO4)3Negative thermal expansion material, high temperature resistant, stable in properties, on the one hand by add it Lai
Reduce the thermal coefficient of expansion of original SiC/Al composite, on the other hand reduce the content of this high-hardness grinding material of SiC, improve multiple
The follow-up processing characteristics of condensation material；The present invention is to prepare the SiC/Al of adjustable thermal expansion by the preparation technology of powder metallurgy2
(WO4)3/ Al composite, SiC/Al2(WO4)3/ Al composite is compared substantially with the thermal coefficient of expansion of SiC/Al composite
Reduce, better met the needs to thermal coefficient of expansion for the electronic package material.
Brief description
Fig. 1 is the thermal dilatometry figure of comparative example 1 composite.
Fig. 2 is the thermal dilatometry figure of example 2 composite.
Fig. 3 is the thermal dilatometry figure of example 3 composite.
Fig. 4 is the thermal dilatometry figure of example 4 composite.
Specific embodiment
Comparative example 1
Raw material：Al powder, mass percent is 40%, SiC powder, and mass ratio is 60%.
Take the powder 0.5g of said ratio and mix homogeneously, load the mould into a diameter of 10mm, in pressure after vibrating compacting
Suppress on piece machine, pressure is 6MPa, demoulding sampling after pressurize 2min；Put in vacuum tube furnace after the completion of compacting and be sintered,
Vacuum drying oven is heated up with 5 DEG C/min heating rate, when being increased to 600 DEG C, is incubated 3h, the flow of protective gas Ar is 1.5ml/s,
H2Flow be 0.3ml/s, furnace cooling.
After testing, thermal dilatometry is as shown in figure 1, be calculated 25～230 DEG C of intervals through linear fit for gained sample
The mean thermal expansion coefficients of interior composite is 9.4 × 10-6K-1.
Embodiment 2
Raw material：Al powder, mass percent is 40%, SiC powder, and mass ratio is 50%, Al2(WO4)3Powder, mass ratio is
10%.
Take the powder 0.5g of said ratio and mix homogeneously, load the mould into a diameter of 10mm, in pressure after vibrating compacting
Suppress on piece machine, pressure is 6MPa, demoulding sampling after pressurize 2min；Put in vacuum tube furnace after the completion of compacting and be sintered,
Vacuum drying oven is heated up with 5 DEG C/min heating rate, when being increased to 600 DEG C, is incubated 3h, the flow of protective gas Ar is 1.5ml/s,
H2Flow be 0.3ml/s, furnace cooling.
After testing, thermal dilatometry is as shown in Fig. 2 be calculated 25～230 DEG C of intervals through linear fit for gained sample
The mean thermal expansion coefficients of interior composite is 8.6 × 10-6K-1.
Embodiment 3
Raw material：Al powder, mass percent is 40%, SiC powder, and mass ratio is 40%, Al2(WO4)3Powder, mass ratio is
20%.
Take the powder 0.5g of said ratio and mix homogeneously, load the mould into a diameter of 10mm, in pressure after vibrating compacting
Suppress on piece machine, pressure is 6MPa, demoulding sampling after pressurize 2min；Put in vacuum tube furnace after the completion of compacting and be sintered,
Vacuum drying oven is heated up with 5 DEG C/min heating rate, when being increased to 600 DEG C, is incubated 3h, the flow of protective gas Ar is 1.5ml/s,
H2Flow be 0.3ml/s, furnace cooling.
After testing, thermal dilatometry is as shown in figure 3, be calculated 25～230 DEG C of intervals through linear fit for gained sample
The mean thermal expansion coefficients of interior composite is 7.7 × 10-6K-1.
Embodiment 4
Raw material：Al powder, mass percent is 40%, SiC powder, and mass ratio is 30%, Al2(WO4)3Powder, mass ratio is
30%.
Take the powder 0.5g of said ratio and mix homogeneously, load the mould into a diameter of 10mm, in pressure after vibrating compacting
Suppress on piece machine, pressure is 6MPa, demoulding sampling after pressurize 2min；Put in vacuum tube furnace after the completion of compacting and be sintered,
Vacuum drying oven is heated up with 5 DEG C/min heating rate, when being increased to 600 DEG C, is incubated 3h, the flow of protective gas Ar is 1.5ml/s,
H2Flow be 0.3ml/s, furnace cooling.
After testing, thermal dilatometry is as shown in figure 3, be calculated 25～230 DEG C of intervals through linear fit for gained sample
The mean thermal expansion coefficients of interior composite is 4.9 × 10-6K-1.
Comparative example 2
Raw material：Al powder, mass percent is 40%, SiC powder, and mass ratio is 20%, Al2(WO4)3Powder, mass ratio is
40%.
Take the powder 0.5g of said ratio and mix homogeneously, load the mould into a diameter of 10mm, in pressure after vibrating compacting
Suppress on piece machine, pressure is 6MPa, demoulding sampling after pressurize 2min；Put in vacuum tube furnace after the completion of compacting and be sintered,
Vacuum drying oven is heated up with 5 DEG C/min heating rate, when being increased to 600 DEG C, is incubated 3h, the flow of protective gas Ar is 1.5ml/s,
H2Flow be 0.3ml/s, furnace cooling.
After testing, the evenly heat being calculated composite in 25～230 DEG C of intervals through linear fit is swollen for gained sample
Swollen coefficient is 9.6 × 10-6K-1.
Claims (7)
1. a kind of SiC/Al of adjustable thermal expansion2(WO4)3/ Al composite it is characterised in that：
(1) SiC powder, pure Al powder, Al are claimed in proportion2(WO4)3Powder；Pure Al powder accounts for 40%, the SiC and Al of three kinds of powder gross masses2
(WO4)3Account for the 60% of three kinds of powder gross masses, wherein Al2(WO4)3Account for the 10～30% of three kinds of powder gross masses；Powder presses difference
Ratio mix homogeneously；
(2) powder after mix homogeneously is put in mould, suppress on hydraulic press after vibrating compacting, pressure is 5～7MPa, protects
The pressure time is 1～3min, and sample is taken out in the demoulding；
(3) after the completion of tabletting, in vacuum tube furnace, sintering makes its densification；Using argon and hydrogen as protective atmosphere, Ar in stove
Flow be 1～1.5ml/s, H2Flow be 0.3～0.5ml/s, sintering temperature is 400～650 DEG C, temperature retention time 1～3h,
Furnace cooling is obtained sample.
2. a kind of SiC/Al of adjustable thermal expansion as claimed in claim 12(WO4)3/ Al composite it is characterised in that：Institute
The mean diameter stating SiC is 20 μm.
3. a kind of SiC/Al of adjustable thermal expansion as claimed in claim 12(WO4)3/ Al composite it is characterised in that：Institute
State a diameter of 10mm of mould.
4. a kind of SiC/Al of adjustable thermal expansion as claimed in claim 12(WO4)3/ Al composite it is characterised in that：Step
Al in rapid 12(WO4)3Mass ratio be 30%.
5. a kind of SiC/Al of adjustable thermal expansion as claimed in claim 12(WO4)3/ Al composite it is characterised in that：Step
Pressure in rapid 2 is 6MPa, and the dwell time is 2min.
6. a kind of SiC/Al of adjustable thermal expansion as claimed in claim 12(WO4)3/ Al composite it is characterised in that：Step
Sintering temperature in rapid 3 is 600 DEG C, is incubated 3h, the flow of protective gas Ar is 1.5ml/s, H2Flow be 0.3ml/s.
7. a kind of SiC/Al of adjustable thermal expansion as claimed in claim 12(WO4)3/ Al composite it is characterised in that：Its
Thermal coefficient of expansion is (8.6～4.9) × 10-6K-1.
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| 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 |
| JP2020104455A (en) * | 2018-12-28 | 2020-07-09 | カシオ計算機株式会社 | Thermally expansive sheet, production method therefor and molded article |
| 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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| JP2012057252A (en) * | 2010-08-12 | 2012-03-22 | Denki Kagaku Kogyo Kk | Aluminum-silicon carbide composite material |
| JP5602566B2 (en) * | 2010-09-30 | 2014-10-08 | 日本ファインセラミックス株式会社 | Heat transfer member made of aluminum-silicon carbide composite |
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