CN106636719B - A kind of preparation method of Aluminum Matrix Composites Strengthened by SiC - Google Patents

A kind of preparation method of Aluminum Matrix Composites Strengthened by SiC Download PDF

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CN106636719B
CN106636719B CN201611064911.6A CN201611064911A CN106636719B CN 106636719 B CN106636719 B CN 106636719B CN 201611064911 A CN201611064911 A CN 201611064911A CN 106636719 B CN106636719 B CN 106636719B
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matrix composites
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CN106636719A (en
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周乐平
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Jiangxi Fu Fu Military Equipment Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1005Pretreatment of the non-metallic additives
    • C22C1/101Pretreatment of the non-metallic additives by coating
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/04Pretreatment of the material to be coated
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/08Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of metallic material

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Abstract

The invention discloses a kind of preparation method of Aluminum Matrix Composites Strengthened by SiC, including preliminary alkali cleaning:For removing Si, SiO2The SiO that slag inclusion and surface of SiC are formed2Film;Etching:Silicon-carbide particle surface is performed etching;Impregnate precursor solution:Obtain the silicon-carbide particle of surface attachment presoma phase;Thermal decomposition:Obtain the silicon-carbide particle of surface attachment Ir Cu oxide composite layers;Pressureless penetration:Aluminum Matrix Composites Strengthened by SiC is made.Pass through the preparation method of Aluminum Matrix Composites Strengthened by SiC of the present invention, it can realize and first form one layer of Ir Cu oxide composite layers in surface of SiC before pressureless penetration, it can effectively improve the degree of adhesion of reinforced phase granular boundary and aluminum alloy melt boundary, and then the hole of two alternate generations is reduced, the thermal conductivity for macroscopically showing as composite material improves.

Description

A kind of preparation method of Aluminum Matrix Composites Strengthened by SiC
Technical field
The invention belongs to field of metal matrix composite, more particularly to a kind of preparation of Aluminum Matrix Composites Strengthened by SiC Method.
Background technology
With the high speed development of hyundai electronics information technology, electronic component inside chip integrated level improves rapidly, power Quick increase, heat caused by electronic device work increased dramatically, and the demand to electronic package material heat conductivility is increasingly It is high;Simultaneously as the raising of chip integration, electronic product internal structure tend to complicate, become more meticulous, this is to Electronic Packaging material Material is also higher and higher with the thermally matched performance requirement of chip and other semiconductor devices.In recent years, it is particulate reinforced metal-based compound The advantage that material is used as electronic package material is gradually recognized by people, wherein with enhancing aluminum-base composite material by silicon carbide particles SiCp/Al) for representative particle enhanced aluminum-based composite material have become New Materials for Electric Packing important developing way it One.
In the course of work of electronic component, the raising of operating temperature increases the probability of electronic component failure, because And require electronic package material that should have good heat conductivility.Therefore, thermal conductivity is SiCp/Al composite woods used for electronic packaging Expect mostly important performance indicator.Current SiCp/Al composite material and preparation method thereofs can be mainly divided into:(1) solid state process, such as powder Last metallurgy method, pressure sintering;(2) liquid metal method, such as squeeze casting method, stirring casting method, liquid metal method of impregnation;(3) it is spontaneous Into method and other preparation methods, such as self-propagating high-temperature synthesis, heat release disperse method.Wherein, liquid metal method is because its is relatively low Cost and can be mass produced and with broader practice prospect.Liquid metal and solid phase in liquid metal method increase Wetting and attachment behavior between strong phase play a crucial role, and the hole and phase boundary surface state of two alternate generations are to compound Mechanical performance, thermophysical property and the corrosion resistance of material have very intuitive influence, but at present to liquid metal The research that legal system makes the drawbacks described above of composite material is less, in composite material preparation process, solid phase surface and liquid phase gap Larger, two-phase cannot fully infiltrate during hot melt oozes, in two alternate very easy formation Residual Pores, SiC particulate and aluminium base The faults in material such as micro-crack are easily formed between body, causes the electronic component performance prepared insufficient, it is compound to constrain SiCp/Al The development of material.
Invention content
To solve the disadvantage that the prior art and deficiency, the present invention provides a kind of systems of Aluminum Matrix Composites Strengthened by SiC Preparation Method so that more abundant using the composite material solid-liquid two-phase infiltration of liquid metal method manufacture, the alternate porosity significantly subtracts Few, composite material thermal conductivity improves.
To achieve the above object, the technical solution adopted by the present invention is:A kind of system of Aluminum Matrix Composites Strengthened by SiC Preparation Method, the specific steps are:
1) preliminary alkali cleaning:Due to containing a large amount of Si and SiO in silicon carbide (SiC) particle2Slag inclusion, and surface of SiC is easy Form SiO2Film, affects the formation and attachment of Ir-Cu oxide composite layers in thermal decomposition process, therefore should be gone It removes.Due to silicon and SiO2It can react with highly basic, but SiC is more stable in strong base solution, so selection highly basic is made To remove Si and SiO in silicon-carbide particle2Cleaning agent, Si and SiO2Reaction equation in highly basic is:
Si+2OH-+H2O→SiO3 2-+2H2
SiO2+2OH-→SiO3 2-+H2O
The strong base solution that configuration substance withdrawl syndrome is 2~5mol/L first, then heats the strong base solution being configured To 60~80 DEG C of heat preservations, silicon-carbide particle is immersed in strong base solution, soaking time is 2~4 hours, constantly right in soaking process Solution is stirred.Lye is diluted with tap water after the completion of alkali cleaning and be separated by filtration silicon-carbide particle and solution, after filtering Silicon-carbide particle embathes the lye of removal particle surface remaining with clear water again, and then filtering drying obtains the silicon carbide after alkali cleaning Grain.
2) it etches:In order to obtain the Ir-Cu oxide composite layers that adhesive force is good, need to carry out silicon-carbide particle surface On the one hand etching can improve the specific surface area of particle surface, so as to increase the surface area of Ir-Cu oxide composite layers;It is another Aspect can improve silicon-carbide particle surface-active, the certain crystalline substances conducive to the attachment of Ir-Cu oxide composite layers of exposure by etching Face so that in follow-up thermal decomposition process, Ir-Cu oxide composite layers can be with matrix close attachment.Since SiC particulate is strong It is all very stable in sour highly basic, but corrode relatively acutely in HF, therefore select etching agents of the HF as SiC powder, reaction equation is:
SiC+4HF=SiF4+CH4
Configuration quality score is 4%~10%HF solution first, solution is sufficiently stirred in configuration process so that in solution HF is evenly distributed.Then it etches, etches in the HF solution silicon-carbide particle immersion after the alkali cleaning obtained by step 1) being configured Temperature is room temperature, and etch period is 1.5~2.5h.Reaction solution in ultrasonic oscillator is shaken into 10min after the completion of etching, is made The reactant of silicon carbide deposition is fully dissolved into solution, then with tap water dilute reaction solution and be separated by filtration carbonization Silicon-carbide particle after filtering is embathed the reaction solution of removal powder surface remaining, then mistake by silicon particle and solution with clear water again The silicon-carbide particle after being etched is dried in filter.
3) precursor solution is impregnated:Precursor solution of the present invention, refer to be configured before thermal decomposition be used for synthesizing, The chemical reagent batch of Ir-Cu oxide composite layers is prepared, the precursor solution that the present invention selects is chloro-iridic acid (H2IrCl6· 6H2O) solution, ethyl alcohol and copper chloride (CuCl2) solution mixed liquor.According to volume ratio Chloroiridic Acid solution (wherein iridium quality percentage 35%) content is:Ethyl alcohol:Copper chloride solution (CuCl220%)=1 mass fraction is:1~2:5~10 measurement chloro-iridic acid is molten Liquid, ethyl alcohol and copper chloride solution, and mixed liquor is stirred evenly;Then the silicon-carbide particle after the etching obtained by step 2) is soaked Bubble stirs 5~10min in above-mentioned precursor solution.Precursor solution is poured out after stirring, silicon carbide is avoided during pouring out Particle is flowed out with precursor solution.Then it by the silicon-carbide particle drawout after immersion, equably tiles on stainless steel And move into drying 10min in drying box;Silicon-carbide particle after drying is again dipped into the above-mentioned precursor solution poured out and stirs 5~10min is mixed, again pours out precursor solution after stirring, and again by the silicon-carbide particle drawout after immersion, equably It is laid on stainless steel plate and moves into drying 10min in drying box;Repeat above procedure totally 3~5 times, last time impregnates presoma The technique of solution is:5~10min is first stirred, then stands 30~60min.Finally obtain the carbonization of surface attachment presoma phase Silicon particle.
4) it thermally decomposes:By horse of the silicon-carbide particle of surface attachment presoma phase obtained in step 3) at 450~500 DEG C 1~2h is not thermally decomposed in stove, then takes out and is air-cooled to room temperature, obtains the silicon carbide of surface attachment Ir-Cu oxide composite layers Grain.
5) pressureless penetration:The silicon-carbide particle and penetration-assisting agent that step 4) is obtained compare silicon carbide according to quality:Penetration-assisting agent is 25~35:1 ratio is uniformly mixed, and the addition of penetration-assisting agent can destroy the oxidation film in aluminum alloy melt, moreover it is possible to promote aluminium alloy Liquid is infiltrated with reinforced phase.First by mixed powder accumulation in cast mould, then by alusil alloy at 800~900 DEG C Liquid is fused into, then liquid aluminium alloy is poured into mould, mould is transferred to 800~900 DEG C of Muffle immediately after cast 0.5~1h is kept the temperature in stove.After heat preservation after air-cooled to less than 400 DEG C water coolings to room temperature.Aluminum Matrix Composites Strengthened by SiC is made.
Preferably, the highly basic is sodium hydroxide or potassium hydroxide.
Preferably, in order to make preliminary alkali cleaning more abundant, in soaking process, solution is stirred using magnetic agitation method It mixes.
Preferably, the granularity of silicon-carbide particle is 50~200 μm.
Preferably, it detaches for convenience, the separation process of silicon carbide and precursor solution, which may be used suction filtration machine and filter, to be divided From.
Preferably, the penetration-assisting agent is the one of which in aluminium powder, magnesium powder, silica flour.
Preferably, the ingredient of the alusil alloy is:Si 6.5%~13%;Fe≤0.7%;Cu≤0.3%;Mn≤ 0.5%;Surplus is Al.
Preferably, the shape of the cast mould inner chamber body can be designed according to the shape of required product.
The beneficial effects of the invention are as follows:One layer of Ir-Cu oxide composite layers first are formed in surface of SiC before pressureless penetration, The degree of adhesion of reinforced phase granular boundary and aluminum alloy melt boundary is can effectively improve, and then reduces the hole of two alternate generations, The thermal conductivity for macroscopically showing as composite material improves.
Specific embodiment
With reference to embodiment, the present invention will be further described, it should be understood that these embodiments are only used for illustration Purpose, be in no way intended to limit protection scope of the present invention.
Embodiment 1
A kind of preparation method of Aluminum Matrix Composites Strengthened by SiC, the specific steps are:
1) preliminary alkali cleaning:The strong base solution that configuration substance withdrawl syndrome is 2mol/L first, the highly basic that then will be configured Solution is heated to 60 DEG C of heat preservations, silicon-carbide particle is immersed in strong base solution, soaking time 2h, constantly to molten in soaking process Liquid is stirred.Lye is diluted with tap water after the completion of alkali cleaning and be separated by filtration silicon-carbide particle and solution, by the carbon after filtering Silicon carbide particle embathes the lye of removal particle surface remaining with clear water again, and then filtering drying obtains the silicon carbide after alkali cleaning Grain.
2) it etches:Configuration quality score is 4%HF solution first, solution is sufficiently stirred in configuration process so that solution Middle HF is evenly distributed.Then it etches, carves in the HF solution silicon-carbide particle immersion after the alkali cleaning obtained by step 1) being configured Erosion temperature be room temperature, etch period 1.5h.Reaction solution is shaken into 10min in ultrasonic oscillator after the completion of etching so that The reactant of silicon carbide deposition is fully dissolved into solution, then with tap water dilute reaction solution and is separated by filtration silicon carbide Silicon-carbide particle after filtering with clear water is embathed the reaction solution of removal powder surface remaining, then filtered by particle and solution again Dry the silicon-carbide particle after being etched.
3) precursor solution is impregnated:According to volume ratio Chloroiridic Acid solution (wherein iridium mass percentage is 35%):Ethyl alcohol: Copper chloride solution (CuCl220%)=1 mass fraction is:1:5 measurement Chloroiridic Acid solution, ethyl alcohol and copper chloride solution, and will Mixed liquor stirs evenly;Then the silicon-carbide particle after the etching obtained by step 2) is immersed in above-mentioned precursor solution, stirred Mix 5min.Precursor solution is poured out after stirring, silicon-carbide particle is avoided to be flowed out with precursor solution during pouring out.Then By the silicon-carbide particle drawout after immersion, equably tile on stainless steel and move into and 10min is dried in drying box;Drying Silicon-carbide particle afterwards is again dipped into the above-mentioned precursor solution poured out and stirs 5min, again by precursor solution after stirring It pours out, and the silicon-carbide particle drawout after immersion is equably laid in move into drying box on stainless steel plate and be dried again 10min;Repeat above procedure totally 3 times, the technique that last time impregnates precursor solution is:5min is first stirred, is then stood 30min.Finally obtain the silicon-carbide particle of surface attachment presoma phase.
4) it thermally decomposes:By Muffle furnace of the silicon-carbide particle of surface attachment presoma phase obtained in step 3) at 450 DEG C Middle thermal decomposition 1h, then takes out and is air-cooled to room temperature, obtains the silicon-carbide particle of surface attachment Ir-Cu oxide composite layers.
5) pressureless penetration:The silicon-carbide particle and penetration-assisting agent that step 4) is obtained compare silicon carbide according to quality:Penetration-assisting agent is 25:1 ratio is uniformly mixed, and the addition of penetration-assisting agent can destroy the oxidation film in aluminum alloy melt, moreover it is possible to promote aluminum alloy melt with Reinforced phase infiltrates.First then alusil alloy is fused into liquid by mixed powder accumulation in cast mould at 800 DEG C State, then liquid aluminium alloy is poured into mould, mould is transferred in 800 DEG C of Muffle furnace immediately after cast and keeps the temperature 0.5h. After heat preservation after air-cooled to less than 400 DEG C water coolings to room temperature.Aluminum Matrix Composites Strengthened by SiC is made.
Shone the thermal diffusion coefficient of thermal conductivity instrument test compound material using laser, and composite material thermal conductivity is obtained passing through conversion Rate, the results are shown in Table 1.
Embodiment 2:
A kind of preparation method of Aluminum Matrix Composites Strengthened by SiC, the specific steps are:
1) preliminary alkali cleaning:The strong base solution that configuration substance withdrawl syndrome is 3mol/L first, the highly basic that then will be configured Solution is heated to 70 DEG C of heat preservations, and silicon-carbide particle is immersed in strong base solution, and soaking time is 3 hours, in soaking process constantly Solution is stirred.Lye is diluted with tap water after the completion of alkali cleaning and be separated by filtration silicon-carbide particle and solution, after filtering Silicon-carbide particle again with clear water embathe removal particle surface remaining lye, then filtering drying acquisition alkali cleaning after silicon carbide Particle.
2) it etches:Configuration quality score is 8%HF solution first, solution is sufficiently stirred in configuration process so that solution Middle HF is evenly distributed.Then it etches, carves in the HF solution silicon-carbide particle immersion after the alkali cleaning obtained by step 1) being configured Erosion temperature be room temperature, etch period 2h.Reaction solution is shaken into 10min in ultrasonic oscillator after the completion of etching so that carbon The reactant of SiClx surface deposition is fully dissolved into solution, then with tap water dilute reaction solution and is separated by filtration silicon carbide Silicon-carbide particle after filtering is embathed the reaction solution of removal powder surface remaining by grain and solution with clear water again, and then filtering is dried Do the silicon-carbide particle after being etched.
3) precursor solution is impregnated:According to volume ratio Chloroiridic Acid solution (wherein iridium mass percentage is 35%):Ethyl alcohol: Copper chloride solution (CuCl220%)=1 mass fraction is:1.5:8 measurement Chloroiridic Acid solution, ethyl alcohol and copper chloride solution, and Mixed liquor is stirred evenly;Then the silicon-carbide particle after the etching obtained by step 2) is immersed in above-mentioned precursor solution, Stir 8min.Precursor solution is poured out after stirring, silicon-carbide particle is avoided to be flowed out with precursor solution during pouring out.So Afterwards by the silicon-carbide particle drawout after immersion, equably tile on stainless steel and move into and 10min is dried in drying box;It dries Silicon-carbide particle after dry, which is again dipped into the above-mentioned precursor solution poured out, stirs 8min, again that presoma is molten after stirring Liquid is poured out, and the silicon-carbide particle drawout after immersion is equably laid in move into drying box on stainless steel plate and be dried again Dry 10min;Repeat above procedure totally 4 times, the technique that last time impregnates precursor solution is:8min is first stirred, is then stood 50min.Finally obtain the silicon-carbide particle of surface attachment presoma phase.
4) it thermally decomposes:By Muffle furnace of the silicon-carbide particle of surface attachment presoma phase obtained in step 3) at 480 DEG C Middle thermal decomposition 1.5h, then takes out and is air-cooled to room temperature, obtains the silicon-carbide particle of surface attachment Ir-Cu oxide composite layers.
5) pressureless penetration:The silicon-carbide particle and penetration-assisting agent that step 4) is obtained compare silicon carbide according to quality:Penetration-assisting agent is 30:1 ratio is uniformly mixed, and the addition of penetration-assisting agent can destroy the oxidation film in aluminum alloy melt, moreover it is possible to promote aluminum alloy melt with Reinforced phase infiltrates.First then alusil alloy is fused into liquid by mixed powder accumulation in cast mould at 850 DEG C State, then liquid aluminium alloy is poured into mould, mould is transferred in 850 DEG C of Muffle furnace immediately after cast and keeps the temperature 0.7h. After heat preservation after air-cooled to less than 400 DEG C water coolings to room temperature.Aluminum Matrix Composites Strengthened by SiC is made.
Shone the thermal diffusion coefficient of thermal conductivity instrument test compound material using laser, and composite material thermal conductivity is obtained passing through conversion Rate, the results are shown in Table 1.
Embodiment 3:
A kind of preparation method of Aluminum Matrix Composites Strengthened by SiC, the specific steps are:
1) preliminary alkali cleaning:The strong base solution that configuration substance withdrawl syndrome is 5mol/L first, the highly basic that then will be configured Solution is heated to 80 DEG C of heat preservations, and silicon-carbide particle is immersed in strong base solution, and soaking time is 4 hours, in soaking process constantly Solution is stirred.Lye is diluted with tap water after the completion of alkali cleaning and be separated by filtration silicon-carbide particle and solution, after filtering Silicon-carbide particle again with clear water embathe removal particle surface remaining lye, then filtering drying acquisition alkali cleaning after silicon carbide Particle.
2) it etches:Configuration quality score is 10%HF solution first, solution is sufficiently stirred in configuration process so that solution Middle HF is evenly distributed.Then it etches, carves in the HF solution silicon-carbide particle immersion after the alkali cleaning obtained by step 1) being configured Erosion temperature be room temperature, etch period 2.5h.Reaction solution is shaken into 10min in ultrasonic oscillator after the completion of etching so that The reactant of silicon carbide deposition is fully dissolved into solution, then with tap water dilute reaction solution and is separated by filtration silicon carbide Silicon-carbide particle after filtering with clear water is embathed the reaction solution of removal powder surface remaining, then filtered by particle and solution again Dry the silicon-carbide particle after being etched.
3) precursor solution is impregnated:According to volume ratio Chloroiridic Acid solution (wherein iridium mass percentage is 35%):Ethyl alcohol: Copper chloride solution (CuCl220%)=1 mass fraction is:2:10 measurement Chloroiridic Acid solution, ethyl alcohol and copper chloride solution, and will Mixed liquor stirs evenly;Then the silicon-carbide particle after the etching obtained by step 2) is immersed in above-mentioned precursor solution, stirred Mix 10min.Precursor solution is poured out after stirring, silicon-carbide particle is avoided to be flowed out with precursor solution during pouring out.So Afterwards by the silicon-carbide particle drawout after immersion, equably tile on stainless steel and move into and 10min is dried in drying box;It dries Silicon-carbide particle after dry, which is again dipped into the above-mentioned precursor solution poured out, stirs 10min, again by presoma after stirring Solution is poured out, and the silicon-carbide particle drawout after immersion is equably laid on stainless steel plate and is moved into drying box again Dry 10min;Repeat above procedure totally 5 times, the technique that last time impregnates precursor solution is:First stir 10min, Ran Houjing Put 60min.Finally obtain the silicon-carbide particle of surface attachment presoma phase.
4) it thermally decomposes:By Muffle furnace of the silicon-carbide particle of surface attachment presoma phase obtained in step 3) at 500 DEG C Middle thermal decomposition 2h, then takes out and is air-cooled to room temperature, obtains the silicon-carbide particle of surface attachment Ir-Cu oxide composite layers.
5) pressureless penetration:The silicon-carbide particle and penetration-assisting agent that step 4) is obtained compare silicon carbide according to quality:Penetration-assisting agent is 35:1 ratio is uniformly mixed, and the addition of penetration-assisting agent can destroy the oxidation film in aluminum alloy melt, moreover it is possible to promote aluminum alloy melt with Reinforced phase infiltrates.First then alusil alloy is fused into liquid by mixed powder accumulation in cast mould at 900 DEG C State, then liquid aluminium alloy is poured into mould, mould is transferred in 900 DEG C of Muffle furnace immediately after cast and keeps the temperature 1h.It protects After temperature after air-cooled to less than 400 DEG C water coolings to room temperature.Aluminum Matrix Composites Strengthened by SiC is made.
Shone the thermal diffusion coefficient of thermal conductivity instrument test compound material using laser, and composite material thermal conductivity is obtained passing through conversion Rate, the results are shown in Table 1.
1 each embodiment testing result list of table
Refer to be omitted pair of the step 3) with step 4) of the present invention described in table without Ir-Cu oxide composite layers control groups According to group, that is to say, that the SiC particulate surface used in 2 pressureless penetration of control group 1 and control group does not have Ir-Cu oxide composite layers, Other techniques are as described in embodiment.As can be seen from Table 1, one layer of Ir- is covered on SiC particulate surface by thermal decomposition method Cu oxide composite layers can significantly improve the thermal conductivity of Aluminum Matrix Composites Strengthened by SiC, this is primarily due to Ir-Cu oxidations The presence of object composite bed improves the activity on SiC particulate surface so that reinforced phase is easier mutually to infiltrate with aluminium alloy liquid phase, compound When the two alternate porositys and defect formation rate reduce, result in the raising of thermal conductivity.

Claims (8)

1. a kind of preparation method of Aluminum Matrix Composites Strengthened by SiC, which is characterized in that the specific steps are:
1)Preliminary alkali cleaning:The strong base solution that configuration substance withdrawl syndrome is 2~5mol/L first, it is then that the highly basic being configured is molten Liquid is heated to 60~80 DEG C of heat preservations, and silicon-carbide particle is immersed in strong base solution, and soaking time is 2~4 hours, in soaking process Constantly solution is stirred, dilute lye with tap water after the completion of alkali cleaning and is separated by filtration silicon-carbide particle and solution, incited somebody to action Silicon-carbide particle after filter embathes the lye of removal particle surface remaining with clear water again, and then filtering drying obtains the carbon after alkali cleaning Silicon carbide particle;
2)Etching:Configuration quality score is 4%~10% HF solution first, solution is sufficiently stirred in configuration process so that solution Middle HF is evenly distributed, then by step 1)It etches, carves in the HF solution that silicon-carbide particle immersion after the alkali cleaning of gained has been configured Erosion temperature is room temperature, and etch period is 1.5~2.5h, and after the completion of etching, reaction solution is shaken in ultrasonic oscillator 10min so that the reactant of silicon carbide deposition is fully dissolved into solution, then with tap water dilute reaction solution and is filtered Silicon-carbide particle and solution are detached, the silicon-carbide particle after filtering is embathed into removal silicon-carbide particle surface remaining with clear water again Reaction solution, the silicon-carbide particle after then filtering drying is etched;
3)Impregnate precursor solution:According to volume ratio Chloroiridic Acid solution:Ethyl alcohol:Copper chloride solution=1:1~2:5~10 measurement Chloroiridic Acid solution, ethyl alcohol and copper chloride solution, and mixed liquor is stirred evenly, wherein, the quality of iridium in above-mentioned Chloroiridic Acid solution Percentage composition is 35%, and the mass fraction of copper chloride is 20% in copper chloride solution, then by step 2)Carbon after the etching of gained Silicon carbide particle is immersed in above-mentioned precursor solution, is stirred 5~10min, is poured out precursor solution after stirring, during pouring out Silicon-carbide particle is avoided to be flowed out with precursor solution, then by the silicon-carbide particle drawout after immersion, is equably laid in On stainless steel plate and the interior drying 10min of drying box is moved into, the silicon-carbide particle after drying is again dipped into the above-mentioned forerunner poured out 5~10min is stirred in liquid solution, again pours out precursor solution after stirring, and again spreads the silicon-carbide particle after immersion Expansion is equably laid on stainless steel plate and moves into drying 10min in drying box;Repeat above procedure totally 3~5 times, last It is secondary impregnate precursor solution technique be:5~10min is first stirred, then stands 30~60min, before finally obtaining surface attachment Drive the silicon-carbide particle of body phase;
4)Thermal decomposition:By step 3)Muffle furnace of the silicon-carbide particle of the surface attachment presoma phase of middle acquisition at 450~500 DEG C 1~2h of middle thermal decomposition, then takes out and is air-cooled to room temperature, obtains the silicon-carbide particle of surface attachment Ir-Cu oxide composite layers;
5)Pressureless penetration:By step 4)The silicon-carbide particle and penetration-assisting agent of acquisition compare silicon carbide according to quality:Penetration-assisting agent for 25~ 35:1 ratio is uniformly mixed, and the addition of penetration-assisting agent can destroy the oxidation film in aluminum alloy melt, moreover it is possible to promote aluminum alloy melt with Reinforced phase infiltrates, and first mixed silicon-carbide particle and penetration-assisting agent mixed-powder is deposited in cast mould, then by aluminium silicon Alloy is fused into liquid at 800~900 DEG C, then liquid aluminium alloy is poured into mould, immediately shifts mould after cast 0.5~1h is kept the temperature into 800~900 DEG C of Muffle furnaces, to room temperature, carbonization is made in water cooling after air-cooled to less than 400 DEG C after heat preservation Silicon reinforced aluminum matrix composites.
2. the preparation method of a kind of Aluminum Matrix Composites Strengthened by SiC according to claim 1, which is characterized in that described Highly basic is sodium hydroxide or potassium hydroxide.
3. the preparation method of a kind of Aluminum Matrix Composites Strengthened by SiC according to claim 1, which is characterized in that impregnate In the process, solution is stirred using magnetic agitation method.
A kind of 4. preparation method of Aluminum Matrix Composites Strengthened by SiC according to claim 1, which is characterized in that carbonization The granularity of silicon particle is 50~200 μm.
A kind of 5. preparation method of Aluminum Matrix Composites Strengthened by SiC according to claim 1, which is characterized in that carbonization The separation process of silicon and precursor solution filters separation using suction filtration machine.
6. the preparation method of a kind of Aluminum Matrix Composites Strengthened by SiC according to claim 1, which is characterized in that described Penetration-assisting agent is aluminium powder, the one of which in magnesium powder, silica flour.
7. the preparation method of a kind of Aluminum Matrix Composites Strengthened by SiC according to claim 1, which is characterized in that described The ingredient of alusil alloy is:Si 6.5%~13%;Fe ≤0.7%;Cu ≤0.3%;Mn ≤0.5%;Surplus is Al.
8. a kind of preparation method of Aluminum Matrix Composites Strengthened by SiC according to claim 1, which is characterized in that according to The shape of the shape design cast mould inner chamber body of required product.
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CN104451240A (en) * 2014-12-30 2015-03-25 南昌航空大学 Preparation method of electronic packaging silicon carbide reinforced aluminum-based composite material
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