CN102815048B - AlSiC composite material, preparation method thereof, and Ni-plated AlSiC composite material - Google Patents
AlSiC composite material, preparation method thereof, and Ni-plated AlSiC composite material Download PDFInfo
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Abstract
The invention discloses an AlSiC composite material and a preparation method thereof. The AlSiC composite material comprises an SiC carrier having a porous structure, wherein Al is filled in the pores of the SiC carrier, and the surface of the SiC carrier is covered with an Al layer having a thickness of 30-150mum; and the Al layer and the Al matrix filled in the pores of the SiC carrier are a continuous distribution phase. The invention also provides an Ni-plated AlSiC composite material. The AlSiC composite material provided by the invention has a good surface chemical-coating homogeneity.
Description
Technical field
The invention belongs to field of research of metal, particularly relate to a kind of AlSiC composite and moulding process thereof.
Background technology
AlSiC(aluminium silicon carbide) composite has the advantage of low thermal coefficient of expansion, high heat conductance, high strength and good anti-wear performance, be used as the base of high power module and heat sink, the plate core of printed circuit board (PCB), microprocessor cover plate, electronic device chassis and encapsulating housing etc., demonstrate huge Application and Development potentiality.But because in AlSiC composite, SiC grain volume fraction is higher, its welding performance is poor, and is easily oxidized in welding process, higher to protective gas purity requirement.Due to the difference of AlSiC composite material surface material, there is SiC, Al two-phase, bring difficulty to chemical plating, difficulty is to be difficult to form even, smooth coating.
SiC(carborundum is used in prior art) powder prepares green compact, binder removal, pre-burning, then aluminising, finally in material surface nickel plating.Due to the difference of composite material surface material, there is SiC, Al two-phase, be difficult to during chemical plating form even, smooth coating.
Summary of the invention
For the difference solving composite material surface material SiC, Al two-phase causes being difficult to during chemical plating the problem of even, the smooth coating of formation, the invention provides a kind of AlSiC composite, make subsequent chemistry nickel plating more easy to operate, the surface chemical plating nickel dam homogeneity obtained is largely increased.
The invention provides a kind of AlSiC composite, comprise the Carboround with loose structure, be filled with aluminium in the porous of described Carboround, described Carboround surface coverage has a layer thickness to be the aluminium lamination of 30-150 μm (micron); The aluminum substrate be filled with in aluminium lamination and Carboround porous is continuous distributed phase.
The invention provides a kind of nickel plating AlSiC composite, it comprises base material and nickel dam, and described base material is AlSiC composite provided by the invention, and described nickel dam is arranged on described aluminium lamination upper surface.
Aluminium lamination of the present invention comprises upper surface and lower surface, and wherein, what contact with nickel dam is aluminium lamination upper surface, and what contact with silicon carbide porous carrier is aluminium lamination lower surface.
Present invention also offers above-mentioned AlSiC composite material and preparation method thereof, comprise following processing step: 1) raw material preparation: with carborundum quality for benchmark, take modifier 0.8-1.2wt%, decentralized medium 8.5-14wt%, three is directly heated, is mixed to get slurry; 2) preparation of porous preform: carry out hot die-casting molding to slurry, obtain green compact, carries out binder removal, presintering to gained green compact, obtains silicon carbide porous precast body; 3) pressure infiltration: adopt aluminium alloy solution to carry out pressure infiltration process to silicon carbide porous precast body, obtain surface and there is the AlSiC composite that a layer thickness is 30-150 μm of aluminium lamination.
The Carboround with loose structure of the present invention is by the step 1) in AlSiC composite material and preparation method thereof of the present invention and step 2) the silicon carbide porous precast body for preparing.
The present inventor is surprised to find that by great many of experiments, and when pressure infiltration process is when the aluminum layer thickness that silicon carbide porous precast body surface is formed is 30-150 μm, the AlSiC composite material surface nickel plating finally prepared is homogeneous.If the aluminum layer thickness that pressure infiltration process is formed on silicon carbide porous precast body surface is too small, after the AlSiC composite chemical plating obtained, coating planarization cannot improve, and thus cannot solve the problem that AlSiC composite chemical plating coating homogeneity is good; If pressure infiltration process is when the aluminum layer thickness > 150 μm that silicon carbide porous precast body surface is formed, the AlSiC composite obtained easily occurs that aluminium lamination peels off in the thermal shock experiment in later stage, and the linear expansion coefficient that aluminium lamination is relative and composite is larger will reduce the service life of product.
A kind of AlSiC composite provided by the invention and preparation method thereof, a kind of nickel plating AlSiC composite solve the problem of chemical deposit planarization after AlSiC composite material surface chemical plating, make AlSiC composite material surface chemical deposit homogeneity good.
Accompanying drawing explanation
Fig. 1 is AlSiC composite material process planning schematic diagram of the present invention.
1 is aluminium alloy solution, and 2 is aluminium alloy solution main-inlet, and 3 is graphite jig, and 4 is charging aperture.
Detailed description of the invention
The invention provides a kind of AlSiC composite, comprise the Carboround with loose structure, be filled with aluminium in the porous of described Carboround, described Carboround surface coverage has a layer thickness to be the aluminium lamination of 30-150 μm; The aluminum substrate be filled with in aluminium lamination and Carboround porous is continuous distributed phase.
According to the present invention, the aluminum layer thickness of described AlSiC composite material surface is preferably 50-100 μm.The present inventor is by a large amount of experiments, be surprised to find that, when the aluminum layer thickness of AlSiC composite material surface is within the scope of this, both can ensure the planarization on subsequent chemistry coated coating surface, its coefficient of expansion also can not be caused because aluminium lamination is blocked up to embody obviously, cause aluminium lamination and composite body to be peeled off.
The invention provides a kind of nickel plating AlSiC composite, it comprises base material and nickel dam, and described base material is AlSiC composite provided by the invention, and described nickel dam is arranged on described aluminium lamination upper surface.According to the present invention, described aluminium lamination comprises upper surface and lower surface, and wherein, what contact with nickel dam is aluminium lamination upper surface, and what contact with silicon carbide porous carrier is aluminium lamination lower surface.This nickel plating AlSiC composite is by obtaining with the aluminium lamination upper surface of conventional aluminum alloys nickel plating liquid medicine process AlSiC composite provided by the invention, conventional aluminum alloys nickel plating liquid medicine mentioned here is known to the skilled person, can directly by commercially available, the chemical nickel plating liquid medicine of such as Lyceum Lai Si company, the chemical nickel plating liquid medicine of moral star chemical industry (Suzhou) Co., Ltd, the nickel plating liquid medicine Niccol-201 of Tianjin Nie Kai Surface Treat Technologies Inc. (US).
According to the present invention, control chemical nickel plating time 5-15min, nickel plating temperature 45-70 DEG C, the thickness of described nickel dam is 2-5 μm.
Present invention also offers above-mentioned AlSiC composite material and preparation method thereof, comprise following processing step: 1) raw material preparation: with carborundum quality for benchmark, take modifier 0.8-1.2wt%, decentralized medium 8.5-14wt%, three is directly heated, is mixed to get slurry; 2) preparation of porous preform: carry out hot die-casting molding to slurry, obtain green compact, carries out binder removal, presintering to gained green compact, obtains silicon carbide porous precast body; 3) pressure infiltration: adopt aluminium alloy solution to carry out pressure infiltration process to silicon carbide porous precast body, obtain surface and there is the AlSiC composite that a layer thickness is 30-150 μm of aluminium lamination.
According to the present invention, described aluminium alloy solution is known to the skilled person, can directly by commercially available, the such as trade mark is the aluminium alloy solution of 2024-T351,5052-H112,5083-H112,6061-T651,7050-T7451,7075-T651, zl101 aluminium alloy (ZAlSi7Mg, alloy designations: ZL101, standard: GB/T 1173-1995).
According to the present invention, described modifier is stearic acid, and described decentralized medium is paraffin.Paraffin is as organic part of slurry, and SiC is scattered in wherein; Stearic acid is powder surface modifier, carries out modification to powder, is conducive to improving the loading of powder in paraffin, thus the linear expansion coefficient of AlSiC composite when reducing subsequent treatment.Stearic acid dosage depending on powder specific surface, generally with carborundum quality for benchmark, modifier stearic acid content is between 0.5%-1.5wt%, and stearic acid content is preferably 0.8-1.2wt% in the present invention.According to the present invention, step 1) gained slurry is the cerul slurry of SiC.
According to the present invention, described stearic acid is the conventional stearic acid in this area, can directly by commercially available, and such as Shijiazhuang Mao Feng chemical industry, Guangzhou good fortune foreignize the stearic acid product of work.
The present invention's paraffin used is the conventional paraffin in this area, can directly by commercially available, such as, in Panjin sky paraffin chemical industry 50#, 52#, 54#, 56#, the paraffin wax product of Wuhan Bo Anda.
According to the present invention, the heating-up temperature in described step 1) is 80-130 DEG C, and heating-up temperature is depending on SiC volume fraction, and SiC volume fraction is about 65% time, and heating-up temperature is 80 DEG C, and when SiC volume fraction reaches about 75%, heating-up temperature rises to 130 DEG C.
According to the present invention, described step 2) in hot die-casting molding pressure be 0.5-0.8MPa, obtain green compact after hot die-casting molding completes.
According to the present invention, described step 2) in binder removal program be warming up to 50 DEG C-60 DEG C with the speed of 5-10 DEG C/min, be then warming up to 150 DEG C with the speed of 0.2-0.5 DEG C/min, at 150 DEG C, be incubated 1-3h, be warming up to 300 DEG C with the speed of 0.2-0.5 DEG C/min again, at 300 DEG C, be incubated 1-3h; Be warming up to 1000-1200 DEG C of presintering process with the speed of 10 DEG C/min after binder removal program completes, the presintering time is 1-3h, obtains silicon carbide porous precast body.
According to the present invention, the pressure infiltration in described step 3) carries out in graphite jig, first vacuumizes whole cavity body of mould, is then docked with mould by the container filling aluminum alloy melt, under the pressure of 10-15MPa, aluminum alloy melt is injected cavity.Reserving thickness, the 30-150 μm larger than the porous preform size prepared that make the size on its thickness direction by controlling graphite jig, controlling the aluminum layer thickness that gained makes AlSiC composite material surface thus.Select graphite jig to be because aluminum alloy melt is comparatively active, can soak with most material generation chemical reaction, physics, although graphite and Al can react, the Al generated
4c
3for brittle substance, after pressure has been oozed, brushing technique is used to be removed easily.First whole cavity body of mould is vacuumized during pressure infiltration, aluminum or aluminum alloy can be avoided like this to enter cavity rear oxidation, vacuumize simultaneously and a negative pressure can be provided suitably to reduce pressure needed for external pressure infiltration.
According to the present invention, described SiC is SiC conventional in this area, can directly by commercially available, and W5, W14, W28 product of such as Beijing micro-nano company, the SiC product of moral is found in Zhengzhou.
At composite material surface plating layer of metal protective layer, the metal level of its surface coverage will be combined firmly with matrices of composite material, himself must have the characteristics such as high temperature resistant, anti-oxidant again, also good with solder wettability.Thus make to be widely used in the method for SiC/Al surface chemistry deposition Ni coating.The present invention in composite preparation process namely at the aluminium lamination that Surface Creation one deck is smooth, so subsequent chemistry plating will be same thing mutually on carry out, can be easier to like this prepare homogeneous coating.
A kind of AlSiC composite provided by the invention and preparation method thereof solves chemical deposit planarization problem after AlSiC composite material surface chemical plating, makes the homogeneity of AlSiC composite material surface chemical plating coating good.
Below in conjunction with specific embodiment, the present invention is described in detail, and following examples can more contribute to the present invention is described, should be understood that these embodiments are further explanation of the present invention, do not constitute any limitation the present invention.
The partial response parameter of table 1: embodiment 1-3.
| SiC/g | Stearic acid/g | Paraffin/g | Slurry temperature/DEG C | Pressure/MPa during injection moulding | |
| Embodiment 1 | 100 | 1 | 14 | 80 | 0.5 |
| Embodiment 2 | 100 | 0.8 | 12 | 100 | 0.7 |
| Embodiment 3 | 100 | 1.2 | 8.5 | 130 | 0.8 |
According to table 1, take the SiC of corresponding weight, stearic acid and paraffin, then each component weighed up is carried out slurry in hot injection moulding machine, slurry temperature is as described in Table 1, and after slurry is even, die cast (concrete pressure is as shown in table 1) obtains green compact under a certain pressure.Then the green compact of gained are placed in resistance furnace carry out binder removal, presintering process obtains silicon carbide porous precast body.Preparation graphite jig as shown in Figure 1, is placed in mould by the above-mentioned silicon carbide porous precast body prepared, to cavity extracting vacuum, then carries out pressure infiltration: aluminum alloy melt is injected mould, control certain pressure, obtain AlSiC composite.Then process is polished to gained AlSiC composite material surface; Finally, carry out this surface of chemical nickel plating process (with conventional aluminum alloys nickel plating liquid medicine in composite material surface Nickel Plating Treatment), obtain product S.The design parameter of binder removal program, preprocessing process and pressure infiltration process is arranged in following specific embodiment to be mentioned.
Raw material used in following examples and device all with describe in epimere consistent.
[embodiment 1]
A) raw material preparation, design parameter is in table 1;
B) porous preform preparation: the green compact of gained are placed in resistance furnace and carry out binder removal, presintering process, binder removal program: be warming up to 50 DEG C with the speed of 5 DEG C/min, then 150 DEG C are warming up to the speed of 0.3 DEG C/min, 2h is incubated at 150 DEG C, be warming up to 300 DEG C with the speed of 0.2 DEG C/min again, at 300 DEG C, be incubated 1h.Presintering process: after binder removal completes, be warming up to 1100 DEG C of presintering process with the speed of 10 DEG C/min, the presintering time is 2h, obtains SiC porous preform;
C) pressure infiltration: preparation graphite jig as shown in Figure 1, controls reserved thickness (size on thickness direction is larger than porous preform size) 30 μm, porous preform is placed in mould, to cavity extracting vacuum.Finally, 1000 DEG C of aluminium alloy solutions (the domestic trade mark is 6061-T651) are injected mould, and pressure used is 12MPa, obtains the AlSiC composite that there are one deck 30 μm of thick aluminium laminations on surface; D) chemical nickel plating process composite material surface: with aluminum alloy nickel plated liquid medicine (Tianjin Nie Kai Surface Treat Technologies Inc. (US), the liquid medicine trade mark: Niccol-201) at AlSiC composite material surface Nickel Plating Treatment 5min, controlling nickel plating temperature is 45 DEG C, and nickel layer thickness is 2 μm, obtains product S1.
[embodiment 2]
A) raw material preparation, design parameter is in table 1;
B) porous preform preparation: the green compact of gained are placed in resistance furnace and carry out binder removal, presintering process.Binder removal program: be warming up to 60 DEG C with the speed of 7 DEG C/min, is then warming up to 150 DEG C with the speed of 0.2 DEG C/min, at 150 DEG C, be incubated 3h, then is warming up to 300 DEG C with the speed of 0.5 DEG C/min, at 300 DEG C, be incubated 2h.Presintering process: after binder removal completes, be warming up to 1000 DEG C of presintering process with the speed of 10 DEG C/min, the presintering time is 1h, obtains SiC porous preform;
C) pressure infiltration: preparation graphite jig as shown in Figure 1, controls reserved thickness (size on thickness direction is large compared with porous prefabrication size) 120 μm, porous preform is placed in mould, to cavity extracting vacuum.Finally, 900 DEG C of aluminum alloy melts are injected mould, and pressure used is 15MPa, obtains the AlSiC composite that there are one deck 120 μm of thick aluminium laminations on surface;
D) chemical nickel plating process composite material surface: with aluminum alloy nickel plated liquid medicine (Tianjin Nie Kai Surface Treat Technologies Inc. (US), the liquid medicine trade mark: Niccol-201) at AlSiC composite material surface Nickel Plating Treatment 5min, controlling nickel plating temperature is 45 DEG C, and nickel layer thickness is 2 μm, obtains product S2.
[embodiment 3]
A) raw material preparation, design parameter is in table 1;
B) porous preform preparation: the green compact of gained are placed in resistance furnace and carry out binder removal, presintering process.Binder removal program: be warming up to 55 DEG C with the speed of 10 DEG C/min, is then warming up to 150 DEG C with the speed of 0.5 DEG C/min, at 150 DEG C, be incubated 1h, then is warming up to 300 DEG C with the speed of 0.4 DEG C/min, at 300 DEG C, be incubated 3h.Presintering process: after binder removal completes, be warming up to 1200 DEG C of presintering process with the speed of 10 DEG C/min, the presintering time is 3h, obtains SiC porous preform;
C) pressure infiltration: preparation graphite jig as shown in Figure 1, controls the reserved thickness (size on thickness direction is large compared with porous preform size) 150 μm of mould, precast body is placed in mould, to cavity extracting vacuum.Finally, 1100 DEG C of aluminum alloy melts are injected mould, and pressure used is 10MPa, obtains the surperficial AlSiC composite having one deck 150 μm of thick aluminium laminations;
D) chemical nickel plating process composite material surface: with aluminum alloy nickel plated liquid medicine (Tianjin Nie Kai Surface Treat Technologies Inc. (US), the liquid medicine trade mark: Niccol-201) at AlSiC composite material surface Nickel Plating Treatment 5min, controlling nickel plating temperature is 45 DEG C, and nickel layer thickness is 2 μm, obtains product S3.
[embodiment 4]
C by embodiment 3) graphite jig in this step of pressure infiltration reserves thickness (size on thickness direction is large compared with porous preform size) and changes 50 μm into, the AlSiC composite that there are one deck 50 μm of thick aluminium laminations on surface is obtained after step c), other finally obtain product S4 all in the same manner as in Example 3.
[embodiment 5]
C by embodiment 3) graphite jig in this step of pressure infiltration reserves thickness (size on thickness direction is large compared with porous preform size) and changes 100 μm into, the AlSiC composite that there are one deck 100 μm of thick aluminium laminations on surface is obtained after step c), other finally obtain product S5 all in the same manner as in Example 3.
[comparative example 1]
This comparative example prepares AlSiC composite for illustration of employing method of the prior art;
A) taking 100g SiC(particle diameter is 20 μm), 1g SA, 14g PW; Lower slurry in hot injection moulding machine, slurry temperature 100 DEG C, slurry evenly casts green compact at the pressure of 0.7MPa afterwards.The green compact of gained are carried out binder removal, preheating in resistance furnace, binder removal process: be warming up to 50 DEG C with the speed of 5 DEG C/min, is then warming up to 150 DEG C with the speed of 0.2 DEG C/min, at 150 DEG C, be incubated 1h, be warming up to 300 DEG C with the speed of 0.2 DEG C/min again, at 300 DEG C, be incubated 1h.Burn-in process: be warming up to 1000 DEG C with the speed of 10 DEG C/min after binder removal completes and carry out preheating, burn-in time is 1h, obtains SiC porous ceramic preforms;
B) under N2 protective atmosphere, aluminium alloy is infiltrated porous preform by infiltration or infiltration mode;
C) grinding residue, obtains Al-SiCp composite;
D) use aluminum alloy nickel plated liquid medicine (Tianjin Nie Kai Surface Treat Technologies Inc. (US), the liquid medicine trade mark: Niccol-201) at above-mentioned Al-SiCp composite material surface Nickel Plating Treatment 5min, controlling nickel plating temperature is 45 DEG C, and nickel layer thickness is 2 μm, obtains product DS1.
[performance test]
The product F 1-F5 obtained and G is done following performance test:
1. roughness test standard (GB131-2006)
Tester: roughmeter (Britain Taylor roughmeter);
2. thermal cycle testing standard: Δ T=80 DEG C, circulates 2000 times; Test result is visually observed after thermal cycling test; Tester: thermal shock test chamber;
Table 2: test result
| Project | S1 | S2 | S3 | S4 | S5 | DS1 |
| Surface roughness (μm) | 0.05 | 0.1 | 0.1 | 0.05 | 0.05 | 0.2 |
| Thermal cycle | Without significant change | Without significant change | Without significant change | Without significant change | Without significant change | There is partial exfoliation in coating |
The degree of roughness of chemical plating coating is related to size, the uniformity of follow-up solder side cohesive force; The thickness of aluminium lamination is meeting under bright and clean, the smooth prerequisite of chemical deposit, unsuitable blocked up.
Be easy to get by table 2, the good and chemical plating coating of the AlSiC composite products coating smoothness prepared by the present invention and composite material surface bond strength high, plating nickel on surface is homogeneous.
Those skilled in the art easily know; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.Protection scope of the present invention is determined by claims.
Claims (8)
1. a preparation method for AlSiC composite, is characterized in that, comprises processing step: 1) raw material preparation: with carborundum quality for benchmark, take modifier 0.8-1.2wt%, decentralized medium 8.5-14wt%, three directly heated, be mixed to get slurry; 2) preparation of porous preform: carry out hot die-casting molding to slurry, obtain green compact, carries out binder removal, presintering to gained green compact, obtains silicon carbide porous precast body; 3) pressure infiltration: adopt aluminium alloy solution to carry out pressure infiltration process to silicon carbide porous precast body, obtain surface and there is the AlSiC composite that a layer thickness is 30-150 μm of aluminium lamination;
Described AlSiC composite, comprises the Carboround with loose structure, is filled with aluminium, it is characterized in that in the porous of described Carboround, and described Carboround surface coverage has a layer thickness to be the aluminium lamination of 30-150 μm; The aluminum substrate be filled with in aluminium lamination and Carboround porous is continuous distributed phase.
2. preparation method according to claim 1, is characterized in that, described aluminum layer thickness is 50-100 μm.
3. preparation method according to claim 1, is characterized in that, the heating-up temperature in described step 1) is 80-130 DEG C.
4. preparation method according to claim 1, is characterized in that, in described step 1), modifier is stearic acid, and decentralized medium is paraffin.
5. preparation method according to claim 1, is characterized in that, described step 2) in hot die-casting molding pressure be 0.5-0.8MPa.
6. preparation method according to claim 1, it is characterized in that, described step 2) in binder removal program be warming up to 50 DEG C-60 DEG C with the speed of 5-10 DEG C/min, then 150 DEG C are warming up to the speed of 0.2-0.5 DEG C/min, 1-3h is incubated at 150 DEG C, be warming up to 300 DEG C with the speed of 0.2-0.5 DEG C/min again, at 300 DEG C, be incubated 1-3h; Be warming up to 1000-1200 DEG C of presintering process with the speed of 10 DEG C/min after binder removal program completes, the presintering time is 1-3h.
7. AlSiC composite material and preparation method thereof according to claim 1, is characterized in that, the pressure infiltration of described step 3) carries out in graphite jig.
8. AlSiC composite material and preparation method thereof according to claim 1, is characterized in that, the pressure infiltration of described step 3), and control pressure is 10-15MPa.
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| CN1060979C (en) * | 1998-09-02 | 2001-01-24 | 华中理工大学 | Pressureless penetration casting method for aluminium-base composite material |
| CN1864895A (en) * | 2005-05-17 | 2006-11-22 | 上海众汇泡沫铝材有限公司 | Process for preparing through-hole foam aluminium plate |
| CN101361184B (en) * | 2006-01-13 | 2011-04-13 | 电气化学工业株式会社 | Aluminum/silicon carbide composite and heat radiation part making use of the same |
| JP4996600B2 (en) * | 2006-04-26 | 2012-08-08 | 電気化学工業株式会社 | Aluminum-silicon carbide composite and heat dissipation component using the same |
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