CN1590571A - Tungsten copper functional composite material and its preparation technology - Google Patents
Tungsten copper functional composite material and its preparation technology Download PDFInfo
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- CN1590571A CN1590571A CN 03150816 CN03150816A CN1590571A CN 1590571 A CN1590571 A CN 1590571A CN 03150816 CN03150816 CN 03150816 CN 03150816 A CN03150816 A CN 03150816A CN 1590571 A CN1590571 A CN 1590571A
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Abstract
A functional W-Cu material is prepared from W and Cu through powdering, adding inducing agent, proportionally mixing, die pressing, presintering and fusing osmosis. It has low expansibility and high thermal conductivity.
Description
Technical field
The present invention relates to a kind of alloy and preparation technology thereof, relate in particular to a kind of tungsten copper two-phase metal composite and preparation technology thereof.
Background technology
In recent years, the demand of substrate, abaculus, web member and the heat dissipation element in large-scale integrated circuit and HIGH-POWERED MICROWAVES device enlarges rapidly.By tungsten, two kinds of materials with different properties of copper tungsten-copper composite material that is composited, inherited two kinds of materials advantage separately, reach the performance that single-material can't have, and can be by changing the relative content between forming mutually, to reach above-mentioned service requirements.The high heat conduction of tungsten-copper composite material and thermotolerance can improve the use power of microelectronic device, and the thermal expansivity of tungsten-copper composite material can make the many semiconductor materials in itself and the microelectronic device be complementary.But,, cause alloy material can't satisfy service requirements because the preparation technology of tungsten-copper alloy does not reach a standard at present.
Summary of the invention
Purpose of the present invention is exactly to provide a kind of excellent material performance, the rational tungsten copper functional composite material of manufacturing process and preparation technology thereof for the defective that overcomes above-mentioned prior art existence.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of tungsten copper functional composite material is characterized in that, this matrix material comprises following component and content (weight): tungsten 70～95%, copper 5～30%.
Described component and content (weight) are: tungsten 80～90%, copper 10～20%.
The physical parameter of described matrix material is: density 15.4～17.3 gram per centimeters
3, 150～210 watts of/meter Kelvins of thermal conductivity (w/mK), thermal expansivity is 6.5～8.3ppm/ ℃.
A kind of preparation technology of tungsten copper functional composite material is characterized in that, this technology may further comprise the steps:
(1) powder treatment
Get the tungsten powder of 5～15 microns of Fei Shi mean particle sizes, through 850～1050 ℃ of dry decomposed ammonia body protections, be incubated≤60 minutes, other gets-200 purpose electrolytic copper powders, through 300～450 ℃ of dry decomposed ammonia body protections, is incubated≤60 minutes, and is stand-by;
(2) add inductor and batch mixing
Adopt granularity to mix on the powder mixer as inductor and above-mentioned tungsten powder for the thin copper powder of-500 purposes;
(3) compression moulding
Above-mentioned batch mixing is placed in the mould, and compression moulding on press, the pressure of press is 6～8 tons/centimetre 2;
(4) presintering
The green compact of above-mentioned compression moulding through 1000～1200 ℃ of presintering, and are incubated 30～120 minutes;
(5) infiltration
The electrolytic copper powder of getting ready in the step (1) is placed one-tenth parison surface through presintering, be incubated 60～180 minutes down for 1250～1400 ℃ in temperature and carry out the infiltration processing, this infiltration treating processes is carried out under the protection of exsiccant decomposed ammonia body, obtains the tungsten copper functional composite material;
The molten milliosmolarity sum of the middle electrolytic copper powder of the add-on of thin copper powder and step (5) is controlled at 5～30% (weight) that account for matrix material in the described step (2), and the add-on of tungsten powder is controlled at 70～95% (weight) that account for matrix material in the described step (2).
The add-on of thin copper powder accounts for matrix material≤5% (weight) in the described step (2).
The rotating speed of described powder mixer is in 0.6～0.75 rev/min of critical speed range, and mixing time is 8～12 hours; Described quick passage critical speed:
D is the diameter of powder mixer mixing machine in the formula, rice.
The green density of compression moulding reaches 70～75% of composite products density in the described step (3).
Tungsten-copper composite material of the present invention is a kind of two-phase pseudoalloy of forming with tungsten, two kinds of metals of copper.Tungsten and copper liquid and solid-state all be immiscible, the original physical and mechanical property of each self-sustaining behind the uniform mixing.The adding of inductor has improved the compactibility of tungsten powder green compact; Improve the infiltration efficient of copper, impelled the Tungsten-copper Composites densification; Guaranteed that copper is mutually tiny and even.For fear of sneaking into of impurity taken place in batch mixing, the present invention adopts dry type to mix.In mixing process, have only two kinds of powder of tungsten powder and copper powder, no longer add any other ball material and solvent.The adding of inductor copper powder makes the forming pressure of tungsten copper powder increase, and green density improves, and the kapillary aperture reduces, and helps the formation of tungsten copper skeleton and the infiltration of liquid phase copper.Because in the present invention, the tungsten copper blank can obtain stable size control behind infiltration copper, so, control slug press size and weight effectively, just can control the density of the finished product, the product densification is just guaranteed.Adopt infiltration method, can reach the purpose of in relative broad range, arbitrarily controlling composite material compositions and performance by changing the initial density and the granular size of low melting point skeleton metal.The low thermal coefficient of expansion of the existing tungsten of this alloy, the combining of high thermal conductivity that has copper again, can realization and the matched well sealed knot of semiconductor silicon, arsenic, gallium arsenide, aluminum oxide, beryllium oxide, can be used as the heat sink substrate of CPU, IC, the contour air-tight packaging of solid state microwave pipe.The tungsten-copper composite material that product of the present invention is used as microelectronics has high-density, high thermal conductivity, low-expansion coefficient, has satisfied service requirements.
Embodiment
Embodiment 1
A kind of tungsten copper functional composite material, this matrix material comprise following component and content (weight): tungsten 85%, copper 15%.
The preparation technology of above-mentioned tungsten copper functional composite material, this technology may further comprise the steps:
(1) powder treatment
Tungsten powder adopts and meets GB3458-1982 tungsten powder technical qualification, trade mark GW-1, the powder of Fei Shi mean particle size 5-15 micron; Electrolytic copper powder adopts and meets the GB5246-1985 electrolytic copper powder, trade mark FTD1, the powder of-200 orders (negative sign is represented the screen underflow of 200 mesh sieves).
The used powder of the present invention needs to handle through following pre-activated, and this is one of characteristics of the present invention.
Tungsten powder is incubated 30 minutes through 1000 ℃ of dry decomposed ammonia body protections; Electrolytic copper powder is incubated 30 minutes through 400 ℃ of dry decomposed ammonia body protections.
(2) add inductor and batch mixing
Adopt granularity to mix on the powder mixer as inductor and above-mentioned tungsten powder for the thin copper powder of-500 purposes, wherein, the tungsten powder consumption accounts for 85% (weight) of product population, the add-on of thin copper powder is 4% (weight) of product population, the rotating speed of powder mixer is in 0.70 rev/min of critical speed range, and mixing time is 10 hours.
(3) compression moulding
Above-mentioned batch mixing is placed in the mould, and compression moulding on press, the pressure of press is 7.5 tons/centimetre 2, and the green density of this compression moulding reaches about 73% of composite products density.
(4) presintering
The green compact of above-mentioned compression moulding through 1100 ℃ of presintering, and are incubated 60 minutes.
(5) infiltration
The electrolytic copper powder of getting ready in the step (1) is placed one-tenth parison surface through presintering; the consumption of this electrolytic copper powder accounts for 11% (weight) of product population; be incubated 120 minutes down for 1350 ℃ in temperature and carry out the infiltration processing; this infiltration treating processes is carried out under the protection of exsiccant decomposed ammonia body, obtains the tungsten copper functional composite material.
The physical parameter of the matrix material that present embodiment makes is: density 16.25 grams per cubic centimters, thermal conductivity 176w/mK, thermal expansivity are 7.2ppm/ ℃.
Embodiment 2
A kind of tungsten copper functional composite material, this matrix material comprise following component and content (weight): tungsten 80%, copper 20%.
The preparation technology of above-mentioned tungsten copper functional composite material, this technology may further comprise the steps:
(1) powder treatment
Tungsten powder adopts and meets GB3458-1982 tungsten powder technical qualification, trade mark GW-1, the powder of Fei Shi mean particle size 5-15 micron; Electrolytic copper powder adopts and meets the GB5246-1985 electrolytic copper powder, trade mark FTD1, the powder of-200 orders (negative sign is represented the screen underflow of 200 mesh sieves).
The used powder of the present invention needs to handle through following pre-activated, and this is one of characteristics of the present invention.
Tungsten powder is incubated 15 minutes through 1050 ℃ of dry decomposed ammonia body protections; Electrolytic copper powder is incubated 10 minutes through 450 ℃ of dry decomposed ammonia body protections.
(2) add inductor and batch mixing
Adopt granularity to mix on the powder mixer as inductor and above-mentioned tungsten powder for the thin copper powder of-500 purposes, wherein, the tungsten powder consumption accounts for 80% (weight) of product population, the add-on of thin copper powder is 2.5% (weight) of product population, the rotating speed of powder mixer is in 0.75 rev/min of critical speed range, and mixing time is 12 hours.
(3) compression moulding
Above-mentioned batch mixing is placed in the mould, and compression moulding on press, the pressure of press is 7.0 tons/centimetre 2, and the green density of this compression moulding reaches about 75% of composite products density.
(4) presintering
The green compact of above-mentioned compression moulding through 1200 ℃ of presintering, and are incubated 120 minutes.
(5) infiltration
The electrolytic copper powder of getting ready in the step (1) is placed one-tenth parison surface through presintering; the consumption of this electrolytic copper powder accounts for 25% (weight) of product population; be incubated 180 minutes down for 1400 ℃ in temperature and carry out the infiltration processing; this infiltration treating processes is carried out under the protection of exsiccant decomposed ammonia body, obtains the tungsten copper functional composite material.
The physical parameter of the matrix material that present embodiment makes is: density 15.52 gram per centimeters
3, thermal conductivity 200w/mK, thermal expansivity are 8.02ppm/ ℃.
Embodiment 3
A kind of tungsten copper functional composite material, this matrix material comprise following component and content (weight): tungsten 90%, copper 10%.
The preparation technology of above-mentioned tungsten copper functional composite material, this technology may further comprise the steps:
(1) powder treatment
Tungsten powder adopts and meets GB3458-1982 tungsten powder technical qualification, trade mark GW-1, the powder of Fei Shi mean particle size 5-15 micron; Electrolytic copper powder adopts and meets the GB5246-1985 electrolytic copper powder, trade mark FTD1, the powder of-200 orders (negative sign is represented the screen underflow of 200 mesh sieves).
The used powder of the present invention needs to handle through following pre-activated, and this is one of characteristics of the present invention.
Tungsten powder is incubated 60 minutes through 950 ℃ of dry decomposed ammonia body protections; Electrolytic copper powder is incubated 60 minutes through 350 ℃ of dry decomposed ammonia body protections.
(2) add inductor and batch mixing
Adopt granularity to mix on the powder mixer as inductor and above-mentioned tungsten powder for the thin copper powder of-500 purposes, wherein, the tungsten powder consumption accounts for 95% (weight) of product population, the add-on of thin copper powder is 1% (weight) of product population, the rotating speed of powder mixer is in 0.60 critical speed range, and mixing time is 8 hours.
(3) compression moulding
Above-mentioned batch mixing is placed in the mould, and compression moulding on press, the pressure of press is 8 tons/centimetre
2, the green density of this compression moulding reaches about 70% of composite products density.
(4) presintering
The green compact of above-mentioned compression moulding through 1000 ℃ of presintering, and are incubated 30 minutes.
(5) infiltration
The electrolytic copper powder of getting ready in the step (1) is placed one-tenth parison surface through presintering; the consumption of this electrolytic copper powder accounts for 4% (weight) of product population; be incubated 60 minutes down for 1250 ℃ in temperature and carry out the infiltration processing; this infiltration treating processes is carried out under the protection of exsiccant decomposed ammonia body, obtains the tungsten copper functional composite material.
The physical parameter of the matrix material that present embodiment makes is: density 16.9 gram per centimeters
3, thermal conductivity 152.3w/mK, thermal expansivity are 6.35ppm/ ℃.
Claims (7)
1. a tungsten copper functional composite material is characterized in that, this matrix material comprises following component and content (weight): tungsten 70～95%, copper 5～30%.
2. a kind of tungsten copper functional composite material according to claim 1 is characterized in that, described component and content (weight) are: tungsten 80～90%, copper 10～20%.
3. a kind of tungsten copper functional composite material according to claim 1 is characterized in that the physical parameter of described matrix material is: density 15.4～17.3 gram per centimeters
3, 150～210 watts of/meter Kelvins of thermal conductivity, thermal expansivity is 6.5～8.3ppm/ ℃.
4. the preparation technology of a tungsten copper functional composite material is characterized in that, this technology may further comprise the steps:
(1) powder treatment
Get the tungsten powder of 5～15 microns of Fei Shi mean particle sizes, through 850～1050 ℃ of dry decomposed ammonia body protections, be incubated≤60 minutes, other gets-200 purpose electrolytic copper powders, through 300～450 ℃ of dry decomposed ammonia body protections, is incubated≤60 minutes, and is stand-by;
(2) add inductor and batch mixing
Adopt granularity to mix on the powder mixer as inductor and above-mentioned tungsten powder for the thin copper powder of-500 purposes;
(3) compression moulding
Above-mentioned batch mixing is placed in the mould, and compression moulding on press, the pressure of press is 6～8 tons/centimetre
2
(4) presintering
The green compact of above-mentioned compression moulding through 1000～1200 ℃ of presintering, and are incubated 30～120 minutes;
(5) infiltration
The electrolytic copper powder of getting ready in the step (1) is placed one-tenth parison surface through presintering, be incubated 60～180 minutes down for 1250～1400 ℃ in temperature and carry out the infiltration processing, this infiltration treating processes is carried out under the protection of exsiccant decomposed ammonia body, obtains the tungsten copper functional composite material;
The molten milliosmolarity sum of the middle electrolytic copper powder of the add-on of thin copper powder and step (5) is controlled at 5～30% (weight) that account for matrix material in the described step (2), and the add-on of tungsten powder is controlled at 70～95% (weight) that account for matrix material in the described step (2).
5. the preparation technology of a kind of tungsten copper functional composite material according to claim 4 is characterized in that, the add-on of thin copper powder accounts for matrix material≤5% (weight) in the described step (2).
6. the preparation technology of a kind of tungsten copper functional composite material according to claim 4 is characterized in that, the rotating speed of described powder mixer is in 0.6～0.75 rev/min of critical speed range, and mixing time is 8～12 hours.
7. the preparation technology of a kind of tungsten copper functional composite material according to claim 4 is characterized in that, the green density of compression moulding reaches 70～75% of composite products density in the described step (3).
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| CNB031508162A CN100355924C (en) | 2003-09-05 | 2003-09-05 | Tungsten copper functional composite material and its preparation technology |
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| CN101624662B (en) * | 2009-07-08 | 2011-04-27 | 中南大学 | Method for preparing W-Cu alloy in microwave infiltration way |
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| CN101624662B (en) * | 2009-07-08 | 2011-04-27 | 中南大学 | Method for preparing W-Cu alloy in microwave infiltration way |
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| CN100355924C (en) | 2007-12-19 |
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