CN113564404A - Aluminum-based graphite particle reinforced composite material and method and heat dissipation adaptor - Google Patents
Aluminum-based graphite particle reinforced composite material and method and heat dissipation adaptor Download PDFInfo
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Abstract
The invention provides an aluminum-based graphite particle reinforced composite material, a method and a heat dissipation adapter, wherein the method comprises the following steps: respectively activating the metal surfaces of graphite powder with different particle sizes, and then pretreating the raw materials according to the design parameters of the raw materials; uniformly mixing the pretreated graphite particles, and filling the mixture into a mold; putting the mould into a heating furnace, and heating the mould uniformly; then putting the aluminum alloy into an aluminum melting furnace for melting casting and refining, and vacuumizing and stirring; moving the heated mould to a hot press platform, and injecting molten aluminum alloy in an aluminum melting furnace into the mould; adjusting the pressure of a hot press to the required pressure and pressure maintaining time, carrying out hot pressing, and then demoulding; and carrying out heat treatment and surface metallization plating processes on the forged casting to obtain the aluminum-based graphite particle reinforced composite material. The product prepared by the invention has the advantages of compactness, excellent performance, simple operation and low cost.
Description
Technical Field
The invention belongs to the technical field of new material preparation and heat dissipation adapter, and particularly discloses an aluminum-based graphite particle reinforced composite material, a method and a heat dissipation adapter.
Background
The particle reinforced aluminum matrix composite material has excellent performance and lower cost than fiber reinforced aluminum matrix composite material. The addition of graphite particles can not only obviously improve the wear resistance, self-lubricating property and cutting processing property of the material, but also greatly improve the shock absorption property of the material and reduce the thermal expansion coefficient of the material, so that the material is suitable for manufacturing wear-resistant parts such as pistons, cylinder sleeves, bearing bushes and bushings, can also be used as a heat-dissipation adapter of high-power electronic components and has wide application prospect.
However, it is difficult to mix graphite into an aluminum melt because the solubility of graphite in aluminum is less than 0.05%, graphite is not wet to aluminum, its contact angle is 157 °, and it is still greater than 90 ° at 1000 ℃. Even if the graphite is mixed, the wettability of the graphite and the graphite is poor, so that the graphite is unevenly distributed, and the performance of the material is influenced.
At present, the preparation method of the aluminum-based graphite composite material comprises a powder metallurgy method, a spray deposition method, a stirring casting method and the like, the process methods all have certain defects, the powder metallurgy method can be used for preparing the composite material with high volume fraction, but the preparation process and equipment of the method are complex, the mechanical property of the composite material is low due to an oxide film on the surface of aluminum powder particles and pores of the material, the shape and the size of a product are limited, overlarge and overlarge parts are not suitable to be manufactured, particularly, the cost is extremely high, and the price is up to $ 100/kg, so that the aluminum-carbon (graphite) composite material prepared by the powder metallurgy method is difficult to be widely applied. The technological parameters of the spray deposition method are difficult to control, the prepared material has high porosity, the relative density is usually between 95 percent and 98 percent, secondary processing and forming are generally needed, and the cost is high. The stirring casting method has the defects of poor carbon (graphite) wettability, difficult uniform particle aggregation and distribution and interface reaction between graphite and a melt.
The methods cannot completely obtain higher volume fraction, density, thermal conductivity and mechanical strength of graphite, and the linear expansion coefficient of the formed aluminum-doped graphite is unstable, so that the large-scale application of the aluminum-doped graphite in the fields of thermal management materials such as electronic packaging, aviation, aerospace and the like with higher requirements on thermal stability is limited.
Disclosure of Invention
The technical problem to be solved by the invention is to provide an aluminum-based graphite particle reinforced composite material, a method and a heat dissipation adaptor aiming at the defects in the prior art, and solve the problems of complex process, high cost, difficult demoulding, low heat conductivity coefficient and dimensional stability, long production period, low yield and the like of the conventional heat conducting, heat dissipating and wear resistant material of a high-power electronic component and the heat dissipation adaptor of the aluminum-graphite composite material prepared by the conventional process in the forming process.
The technical scheme adopted by the invention is that,
a preparation method of an aluminum-based graphite particle reinforced composite material heat dissipation adapter comprises the following steps:
respectively activating the metal surfaces of graphite powder with different particle sizes, and then preprocessing raw materials according to the raw material design parameters of the heat dissipation adapter;
uniformly mixing the pretreated graphite particles, and then filling the mixture into a mold; putting the mould into a heating furnace, and heating the mould uniformly;
putting the aluminum alloy into an aluminum melting furnace for melting casting and refining, and vacuumizing and stirring to obtain an aluminum alloy melt;
moving the heated mould to a hot press platform, and injecting molten aluminum alloy into the mould; adjusting the pressure of a hot press to the required pressure and pressure maintaining time, carrying out hot pressing, and then demoulding; forging the demolded casting;
and carrying out heat treatment and surface metallization plating processes on the forged casting to obtain the aluminum-based graphite particle reinforced composite material.
As a further improvement of the invention, the particle size distribution of the graphite is 180#, and the mass ratio of 90# to 5# is 11: 5: 3.
as a further improvement of the invention, the element components of the aluminum alloy satisfy the following conditions: the Mg and Si contents are adjusted in the refining process, so that the Mg and the Si contents are respectively increased to 0.3 to 0.7 percent.
As a further improvement of the invention, the method comprises the following steps of respectively activating the metal surfaces of graphite powder with different particle sizes, and then pretreating the raw materials according to the design parameters of the raw materials:
selecting graphite particles with corresponding particle size distribution according to a grading theory, and respectively carrying out metal Cu surface coating on graphite powder with different particle sizes to obtain a mixture;
mixing polyvinyl alcohol, sodium carboxymethylcellulose and water according to a mass ratio of 8% to 4% to 88%, heating at 150 ℃ and keeping the mixture fully dissolved to prepare a colloid;
the mixture and the colloid are mixed according to the mass ratio of (18-20%): mixing 80% of the raw materials, granulating, drying, sieving, and drying to water content of 3%; adding 20% of glue into the dried powder, and continuing to carry out artificial granulation; drying, sieving, and continuously drying to water content of 1.5%; obtaining the powder.
As a further improvement of the invention, the method comprises the following steps of putting the mould into a heating furnace, uniformly heating the mould by heating:
putting the mould into a heating furnace, uniformly heating the mould at the speed of 50 ℃/min, and heating to 650 ℃.
As a further improvement of the invention, the specific steps of putting the aluminum alloy into an aluminum melting furnace for melting and casting are as follows:
adding ZL101A aluminum alloy into a smelting furnace, and smelting at the temperature of 650-750 ℃ to obtain aluminum alloy melt; controlling the temperature at 700 ℃, adding a refining agent for refining, and removing ash residues on the surface of the aluminum alloy solution to obtain a purer aluminum alloy solution.
As a further improvement of the invention, the hot pressing specific process comprises the following steps:
adjusting the pressure of a hot press to 2MPa, starting pressing, applying pressure at a constant speed of 3MPa/min up, down, left, right, front and back, keeping the pressure when the pressure reaches 15MPa, naturally releasing pressure, and cooling to room temperature.
As a further improvement of the invention, the surface metallization plating process specifically comprises:
removing oil: HTL-310 medicament with the concentration of 35g/L, and ultrasonic cleaning is carried out at the temperature of 20-30 ℃;
② weak etching: soaking 70g/L HTL-310 in water at 50-60 deg.C;
thirdly, washing for one time: washing with deionized water at 20-30 deg.C;
activation: soaking HT-AC600 medicament with concentration of 500ml/L at 20-30 ℃;
secondary washing: washing with deionized water at 20-30 deg.C;
sixthly, electroplating nickel: electrolyzing 3-6um nickel in ferrous sulfate solution, with voltage of 3V and current of 0.3A;
chemical nickel: soaking HT-EN800 medicament with concentration of 150ml/L at pH of 4.8-5.5 and temperature of 85-90 deg.C;
eighthly, three times of water washing: washing with deionized water at 20-30 deg.C;
ninthly, drying: blowing by circulating hot air at the temperature of 120 ℃ and 150 ℃;
and (c) dehydrogenation: preserving heat at 120-250 ℃, and cooling to room temperature along with the furnace.
An aluminum-based graphite particle reinforced composite material is prepared by the method.
A heat dissipation adaptor is prepared by adopting the aluminum-based graphite particle reinforced composite material.
Compared with the prior art, the invention has the following advantages:
the invention sequentially passes through five steps of powder surface activation, filling, mold heating, aluminum injection and surface metal plating technology, avoids the defects of complex working procedure, expensive equipment, long production period and high energy consumption, has the advantages of compact product, excellent performance, simple operation, low cost and wide application range, and can be implemented in the preparation process of metal composite materials such as aluminum base, magnesium base, titanium base and the like. The preparation method improves the heat-conducting property of the aluminum-graphite composite material; the heat conductivity coefficient can be adjusted according to the grain composition of the graphite powder; the material has stable structure and prolonged service life; simple preparation method and the like.
Further, a graphite powder metal surface coating technology is adopted, and preheating treatment is carried out before graphite particles and aluminum are compounded, so that volatile matters and adsorbed gas on the surface of graphite can be effectively removed, a coating which can be wetted with aluminum melt is generated on the surface of the graphite particles, the activation energy of the surface of graphite is improved, and meanwhile, magnesium blocks are added into the aluminum melt, so that the surface tension of the aluminum alloy is reduced, the wettability of the aluminum alloy and aluminum is improved, and the stability of an interface of the graphite and the aluminum melt is improved.
Further, the technological process of accumulating and compacting graphite powder with surface activated in mold heated continuously and pouring aluminum includes adding some elements capable of preventing graphite from floating, such as Ti, Cr, Zr, Ni, V, Co, Mn, Nb, P, etc. into aluminum melt, and ultrasonic vibration to speed the compounding of graphite grain and aluminum melt4C3Phase and particle aggregation and the like, greatly reduces the rejection rate, greatly shortens the production period, and can form parts with relatively complex structures.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a picture of the appearance of sample S210511090 of example 2;
FIG. 3 is a picture of the appearance of sample S210511091 of example 3.
Detailed Description
At present, the heat dissipation adaptor of the high-power electronic component mostly adopts aluminum alloy, copper alloy, tungsten copper, molybdenum copper, CMC copper and pure ceramic materials, the aluminum alloy and the copper alloy materials are soft, the strength is low, the linear expansion coefficient is large, and the deformation is serious under the working conditions of heating and stress, so that the stress concentration, the cracking and the failure of the electronic component connected with the aluminum alloy and the copper alloy materials are caused; tungsten copper, molybdenum copper and CMC copper have high density, belong to heavy metal, can not be used in the field with high requirement on density, and have certain harm effect on human body and environment; the pure ceramic material is brittle and fragile, has high processing cost, cannot be processed into a product with a complex shape, is easy to scratch and crack in the using and transporting processes, and increases the risk of failure of electronic components. The aluminum silicon carbide composite material is limited by mechanical processing and cannot be used in large-size complex parts. The aluminum-based graphite has good cutting processing performance and higher shock absorption, is suitable for various heat dissipation and self-lubricating parts, and provides favorable conditions for adapters of high-power electronic components.
The first purpose of the invention is to provide a preparation method of an aluminum-based graphite particle reinforced composite material, which comprises the following steps:
firstly, calculating design parameters of the aluminum-graphite raw material, including graphite volume, graphite particle composition, graphite outline, aluminum alloy element components and the like, which meet technical indexes such as high strength, high elastic modulus, high thermal conductivity, high dimensional stability and the like by combining theoretical calculation with a digital simulation technology;
secondly, respectively activating the metal surfaces of graphite powder with different particle sizes, and then performing raw material pretreatment by the steps of material preparation, ball milling mixing, granulation and the like according to the design parameters of the raw materials; preheating the special die at the same time;
uniformly mixing the pretreated graphite particles, and filling the mixture into a mold; putting the mould into a heating furnace, and uniformly heating the mould according to the corresponding heating rate;
putting the aluminum alloy into an aluminum melting furnace for melting and casting, and vacuumizing and stirring; moving the heated mould to a hot press platform, and injecting molten aluminum alloy in an aluminum melting furnace into the mould; adjusting the pressure of a hot press to a certain pressure and pressure maintaining time, carrying out hot pressing, and then demoulding; forging the demolded casting to obtain the aluminum-graphite composite material with high specific stiffness, high heat conductivity and high dimensional stability;
and finally, carrying out surface metallization plating process treatment on the aluminum-carbon (graphite) finished product to ensure that the aluminum-graphite product has certain corrosion resistance and packaging and welding properties, thereby forming a final product meeting the requirements.
The preparation method improves the heat-conducting property of the aluminum-graphite composite material; the heat conductivity coefficient can be adjusted according to the grain composition of the graphite powder; the material has stable structure and prolonged service life; simple preparation method and the like.
A second object is to provide an aluminum-based graphite particle-reinforced composite material, which is obtained by the method.
The third purpose is to provide a heat dissipation adaptor, which is prepared by adopting the aluminum-based graphite particle reinforced composite material.
The preparation method comprises the following steps:
s1, according to the technical index requirements of thermal conductivity, dimensional stability, bending strength and the like corresponding to the corresponding heat dissipation adaptor and the heat conduction and bending strength principle of the microstructure of the aluminum-graphite composite material, the grain size distribution is pertinently and custom designed to be 180#, and the mass ratio of 90# to 5# is 11: 5: 3; in order to improve the wettability of the aluminum alloy, the contents of Mg and Si are adjusted in the refining process of ZL101A and are respectively increased to 0.3-0.7%.
S2, selecting graphite particles with corresponding particle size distribution according to the grading theory, respectively coating films on the surfaces of the metal Cu on the graphite powder with different particle sizes, and mixing.
S3, mixing the polyvinyl alcohol PVA, the sodium carboxymethylcellulose CMC and the water according to the mass ratio of 8% to 4% to 88%, adding into a stirring tank, heating at 150 ℃, keeping for 5 hours until the materials are fully dissolved to prepare colloid, and naturally cooling to below 35 ℃ for later use.
S4, mixing the mixture obtained in the step S2 with the colloid obtained in the step S3 according to the mass ratio of 18-20%: mixing 80% of the raw materials, granulating, then putting the granulated powder into a baking oven, baking for 2.5-3.5 h at 80-120 ℃, sieving by a 40-mesh sieve until all the granules are sieved, and continuously drying until the water content is 3%; adding 20% of glue into the dried powder, and continuing to carry out artificial granulation; drying in an oven at 80-120 ℃ for 2h, sieving with a 40-mesh sieve until all the materials are sieved, and continuously drying until the water content is 1.5%; putting the sieved powder into a sealed bag, and placing the sealed bag in a shade place for 5-10 h;
s5, putting the special die into a heating furnace, uniformly heating the die at a speed of 50 ℃/min, and heating to 650 ℃;
s6, adding ZL101A aluminum alloy into a smelting furnace, and smelting at the controlled temperature of 650-750 ℃ to obtain aluminum alloy melt; controlling the temperature at 700 ℃, adding a refining agent for refining, removing ash residues on the surface of the aluminum alloy solution to obtain a purer aluminum alloy solution, and vacuumizing and stirring;
s7, filling the graphite powder prepared in the step S4 into a preheated mold S5, and keeping the mold vibrating to ensure that the powder is uniformly compacted; moving the heated mould to a hot press platform, injecting molten aluminum alloy in an S6 aluminum melting furnace into the mould, adjusting the hot press, starting pressing at 2MPa, applying pressure at a constant speed of 3MPa/min up, down, left, right, front and back, keeping the pressure for 10min when the pressure reaches 15MPa, naturally releasing the pressure, and demoulding after the temperature is cooled to room temperature;
s8, carrying out heat treatment on the aluminum-graphite composite material prepared in the step S7, heating the aluminum-graphite composite material casting blank to 400-450 ℃ (preferably 450 ℃) at a heating rate of 30-50 ℃/h, preserving heat for 3-6 h, then carrying out water bath quenching and cooling to room temperature, then heating to 150-180 ℃ at a heating rate of 10-30 ℃/h, preserving heat for 2-3 h (preferably 2.5 h), and then naturally cooling to room temperature in air.
S9, performing a surface metallization plating process on the aluminum-graphite finished product prepared in the step S8, removing oil: cleaning with 35g/L HTL-310 agent at 20-30 deg.C by ultrasonic wave for 3 min; ② weak etching: soaking 70g/L HTL-310 in water at 50-60 deg.C for 7 min; washing with water: washing with deionized water at 20-30 deg.C for 1-3 min; activation: soaking HT-AC600 medicament with concentration of 500ml/L at 20-30 deg.C for 1-1.5 min; washing with water: washing with deionized water at 20-30 deg.C for 1-3 min; sixthly, electroplating nickel: electrolyzing 3-6um nickel in ferrous sulfate solution, with voltage of 3V and current of 0.3A; chemical nickel: soaking 150ml/L HT-EN800 preparation at pH4.8-5.5 and 85-90 deg.C for 75-95 min; and (b) washing with water: washing with deionized water at 20-30 deg.C for 1-3 min; ninthly, drying: blowing by circulating hot air at the temperature of 120 ℃ and 150 ℃ for 10-20 min; and (c) dehydrogenation: preserving heat for 2-5h at 120-250 ℃, and cooling to room temperature along with the furnace.
And S10, sealing, plastically packaging the aluminum-graphite product prepared in the step S9.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention. The present invention will be described in detail with reference to specific examples.
Example 1
S1, according to the technical index requirements of thermal conductivity, dimensional stability, bending strength and the like corresponding to the corresponding heat dissipation adaptor and the heat conduction and bending strength principle of the microstructure of the aluminum-graphite composite material, the grain size distribution is pertinently and custom designed to be 180#, and the mass ratio of 90# to 5# is 11: 5: 3; in order to improve the wettability of the aluminum alloy, the contents of Mg and Si are adjusted in the refining process of ZL101A and are respectively increased to 0.3 percent and 0.7 percent.
S2, selecting graphite particles with corresponding particle size distribution according to the grading theory, respectively coating films on the surfaces of the metal Cu on the graphite powder with different particle sizes, and mixing.
S3, mixing the polyvinyl alcohol PVA, the sodium carboxymethylcellulose CMC and the water according to the mass ratio of 8% to 4% to 88%, adding into a stirring tank, heating at 150 ℃, keeping for 5 hours until the materials are fully dissolved to prepare colloid, and naturally cooling to below 35 ℃ for later use.
S4, mixing the mixture obtained in the step S2 with the colloid obtained in the step S3 according to the mass ratio of 19%: mixing 81% of the raw materials according to a proportion, granulating, then putting the granulated powder into an oven, baking for 3.5 hours at 80 ℃, sieving by a 40-mesh sieve until all the granulated powder is sieved, and continuously drying until the moisture content is 3%; adding 20% of glue into the dried powder, and continuing to carry out artificial granulation; drying in an oven at 80 deg.C for 2 hr, sieving with 40 mesh sieve, and drying to water content of 1.5%; putting the sieved powder into a sealed bag, and placing the sealed bag in a shade place for 10 hours;
s5, putting the special die into a heating furnace, uniformly heating the die at a speed of 50 ℃/min, and heating to 650 ℃;
s6, adding ZL101A aluminum alloy into a smelting furnace, and smelting at 650 ℃ to obtain aluminum alloy melt; controlling the temperature at 700 ℃, adding a refining agent for refining, removing ash residues on the surface of the aluminum alloy solution to obtain a purer aluminum alloy solution, and vacuumizing and stirring;
s7, filling the graphite powder prepared in the step S4 into a preheated mold S5, and keeping the mold vibrating to ensure that the powder is uniformly compacted; moving the heated mould to a hot press platform, injecting molten aluminum alloy in an S6 aluminum melting furnace into the mould, adjusting the hot press, starting pressing at 2MPa, applying pressure at a constant speed of 3MPa/min up, down, left, right, front and back, keeping the pressure for 10min when the pressure reaches 15MPa, naturally releasing the pressure, and demoulding after the temperature is cooled to room temperature;
s8, carrying out heat treatment on the aluminum-graphite composite material prepared in the step S7, heating a casting blank of the aluminum-graphite composite material to 400 ℃ at a heating rate of 30-50 ℃/h, preserving heat for 6 hours, carrying out water bath quenching and cooling to room temperature, then heating to 150 ℃ at a heating rate of 10 ℃/h, preserving heat for 2 hours, and then naturally cooling to room temperature in the air.
S9, performing a surface metallization plating process on the aluminum-graphite finished product prepared in the step S8, removing oil: cleaning with 35g/L HTL-310 agent at 20 deg.C by ultrasonic wave for 3 min; ② weak etching: soaking 70g/L HTL-310 in water at 50 deg.C for 7 min; washing with water: washing with deionized water at 20 ℃ for 1; activation: soaking HT-AC600 medicament with concentration of 500ml/L at 20 deg.C for 1 min; washing with water: cleaning with deionized water at 20 deg.C for 1 min; sixthly, electroplating nickel: electrolyzing 3um nickel in ferrous sulfate solution, wherein the voltage is 3V and the current is 0.3A; chemical nickel: soaking HT-EN800 medicament with concentration of 150ml/L at pH of 4.8 and 85 deg.C for 75 min; and (b) washing with water: cleaning with deionized water at 20 deg.C for 1 min; ninthly, drying: circulating hot air blowing at 120 deg.C for 20 min; and (c) dehydrogenation: preserving the heat for 5 hours at the temperature of 120 ℃, and cooling to the room temperature along with the furnace.
And S10, sealing, plastically packaging the aluminum-graphite product prepared in the step S9.
Example 2
S1, according to the technical index requirements of thermal conductivity, dimensional stability, bending strength and the like corresponding to the corresponding heat dissipation adaptor and the heat conduction and bending strength principle of the microstructure of the aluminum-graphite composite material, the grain size distribution is pertinently and custom designed to be 180#, and the mass ratio of 90# to 5# is 11: 5: 3; in order to improve the wettability of the aluminum alloy, the contents of Mg and Si are adjusted in the refining process of ZL101A and are respectively increased to 0.4 percent and 0.6 percent.
S2, selecting graphite particles with corresponding particle size distribution according to the grading theory, respectively coating films on the surfaces of the metal Cu on the graphite powder with different particle sizes, and mixing.
S3, mixing the polyvinyl alcohol PVA, the sodium carboxymethylcellulose CMC and the water according to the mass ratio of 8% to 4% to 88%, adding into a stirring tank, heating at 150 ℃, keeping for 5 hours until the materials are fully dissolved to prepare colloid, and naturally cooling to below 35 ℃ for later use.
S4, mixing the mixture obtained in the step S2 with the colloid obtained in the step S3 according to a mass ratio of 18%: mixing 82% of the raw materials according to a proportion, granulating, then putting the granulated powder into a baking oven, baking for 3 hours at 100 ℃, sieving by a 40-mesh sieve until the granulated powder is completely sieved, and continuously drying until the moisture content is 3%; adding 20% of glue into the dried powder, and continuing to carry out artificial granulation; drying in an oven at 100 deg.C for 2 hr, sieving with 40 mesh sieve, and drying to water content of 1.5%; putting the sieved powder into a sealed bag, and placing the sealed bag in a shade place for 8 hours;
s5, putting the special die into a heating furnace, uniformly heating the die at a speed of 50 ℃/min, and heating to 650 ℃;
s6, adding ZL101A aluminum alloy into a smelting furnace, and smelting at 700 ℃ to obtain aluminum alloy melt; controlling the temperature at 700 ℃, adding a refining agent for refining, removing ash residues on the surface of the aluminum alloy solution to obtain a purer aluminum alloy solution, and vacuumizing and stirring;
s7, filling the graphite powder prepared in the step S4 into a preheated mold S5, and keeping the mold vibrating to ensure that the powder is uniformly compacted; moving the heated mould to a hot press platform, injecting molten aluminum alloy in an S6 aluminum melting furnace into the mould, adjusting the hot press, starting pressing at 2MPa, applying pressure at a constant speed of 3MPa/min up, down, left, right, front and back, keeping the pressure for 10min when the pressure reaches 15MPa, naturally releasing the pressure, and demoulding after the temperature is cooled to room temperature;
s8, carrying out heat treatment on the aluminum-graphite composite material prepared in the step S7, heating the aluminum-graphite composite material casting blank to 420 ℃ at a heating rate of 40 ℃/h, preserving heat for 5 hours, carrying out water bath quenching and cooling to room temperature, heating to 160 ℃ at a heating rate of 20 ℃/h, preserving heat for 2.5 hours, and naturally cooling to room temperature in the air.
S9, performing a surface metallization plating process on the aluminum-graphite finished product prepared in the step S8, removing oil: cleaning with 35g/L HTL-310 agent at 25 deg.C by ultrasonic wave for 3 min; ② weak etching: soaking 70g/L HTL-310 in 55 deg.C for 7 min; washing with water: washing with deionized water at 25 deg.C for 1.5 min; activation: soaking HT-AC600 agent with concentration of 500ml/L at 25 deg.C for 1.2 min; washing with water: washing with deionized water at 25 deg.C for 2.5 min; sixthly, electroplating nickel: electrolyzing 4um of nickel in a ferrous sulfate solution, wherein the voltage is 3V and the current is 0.3A; chemical nickel: soaking HT-EN800 medicament with concentration of 150ml/L at pH 5 and 86 deg.C for 80 min; and (b) washing with water: washing with deionized water at 25 deg.C for 2.5 min; ninthly, drying: blowing with circulating hot air at 130 deg.C for 15 min; and (c) dehydrogenation: keeping the temperature at 200 ℃ for 2.5h, and cooling to room temperature along with the furnace.
And S10, sealing, plastically packaging the aluminum-graphite product prepared in the step S9.
Example 3
S1, according to the technical index requirements of thermal conductivity, dimensional stability, bending strength and the like corresponding to the corresponding heat dissipation adaptor and the heat conduction and bending strength principle of the microstructure of the aluminum-graphite composite material, the grain size distribution is pertinently and custom designed to be 180#, and the mass ratio of 90# to 5# is 11: 5: 3; in order to improve the wettability of the aluminum alloy, the contents of Mg and Si are adjusted in the refining process of ZL101A and are respectively increased to 0.7 percent and 0.5 percent.
S2, selecting graphite particles with corresponding particle size distribution according to the grading theory, respectively coating films on the surfaces of the metal Cu on the graphite powder with different particle sizes, and mixing.
S3, mixing the polyvinyl alcohol PVA, the sodium carboxymethylcellulose CMC and the water according to the mass ratio of 8% to 4% to 88%, adding into a stirring tank, heating at 150 ℃, keeping for 5 hours until the materials are fully dissolved to prepare colloid, and naturally cooling to below 35 ℃ for later use.
S4, mixing the mixture obtained in the step S2 with the colloid obtained in the step S3 according to the mass ratio of 20%: mixing 80% of the raw materials, granulating, baking the granulated powder in a baking oven at 120 ℃ for 2.5h, sieving with a 40-mesh sieve until all the granules are sieved, and continuously drying until the water content is 3%; adding 20% of glue into the dried powder, and continuing to carry out artificial granulation; drying in an oven at 120 deg.C for 2h, sieving with 40 mesh sieve, and drying to water content of 1.5%; putting the sieved powder into a sealed bag, and placing the sealed bag in a shade place for 5 hours;
s5, putting the special die into a heating furnace, uniformly heating the die at a speed of 50 ℃/min, and heating to 650 ℃;
s6, adding ZL101A aluminum alloy into a smelting furnace, and smelting at 750 ℃ to obtain aluminum alloy melt; controlling the temperature at 700 ℃, adding a refining agent for refining, removing ash residues on the surface of the aluminum alloy solution to obtain a purer aluminum alloy solution, and vacuumizing and stirring;
s7, filling the graphite powder prepared in the step S4 into a preheated mold S5, and keeping the mold vibrating to ensure that the powder is uniformly compacted; moving the heated mould to a hot press platform, injecting molten aluminum alloy in an S6 aluminum melting furnace into the mould, adjusting the hot press, starting pressing at 2MPa, applying pressure at a constant speed of 3MPa/min up, down, left, right, front and back, keeping the pressure for 10min when the pressure reaches 15MPa, naturally releasing the pressure, and demoulding after the temperature is cooled to room temperature;
s8, carrying out heat treatment on the aluminum-graphite composite material prepared in the step S7, heating a casting blank of the aluminum-graphite composite material to 450 ℃ at a heating rate of 50 ℃/h, preserving heat for 3 hours, carrying out water bath quenching and cooling to room temperature, heating to 180 ℃ at a heating rate of 30 ℃/h, preserving heat for 3 hours, and naturally cooling to room temperature in the air.
S9, performing a surface metallization plating process on the aluminum-graphite finished product prepared in the step S8, removing oil: cleaning with 35g/L HTL-310 agent at 30 deg.C by ultrasonic wave for 3 min; ② weak etching: soaking 70g/L HTL-310 in water at 60 deg.C for 7 min; washing with water: cleaning with deionized water at 30 deg.C for 3 min; activation: soaking HT-AC600 medicament with concentration of 500ml/L at 30 deg.C for 1 min; washing with water: cleaning with deionized water at 30 deg.C for 1 min; sixthly, electroplating nickel: electrolyzing 3um nickel in ferrous sulfate solution, wherein the voltage is 3V and the current is 0.3A; chemical nickel: soaking HT-EN800 medicament with concentration of 150ml/L at pH 5.5 and 90 deg.C for 95 min; and (b) washing with water: cleaning with deionized water at 30 deg.C for 1 min; ninthly, drying: circulating hot air blowing at 150 deg.C for 10 min; and (c) dehydrogenation: keeping the temperature at 250 ℃ for 5h, and cooling to room temperature along with the furnace.
And S10, sealing, plastically packaging the aluminum-graphite product prepared in the step S9.
Two sets of samples prepared according to examples 2 and 3, respectively, were tested and the appearance pictures of the two sets of samples are shown in fig. 2.
TABLE 1 detection results of thermal conductivity of aluminum-based graphite particle reinforced composite material
According to the test result, the aluminum-based graphite particle reinforced composite material prepared by the embodiment of the invention has good thermal conductivity and meets the test requirement of the heat dissipation adapter.
Example 4
S1, according to the technical index requirements of thermal conductivity, dimensional stability, bending strength and the like corresponding to the corresponding heat dissipation adaptor and the heat conduction and bending strength principle of the microstructure of the aluminum-graphite composite material, the grain size distribution is pertinently and custom designed to be 180#, and the mass ratio of 90# to 5# is 11: 5: 3; in order to improve the wettability of the aluminum alloy, the contents of Mg and Si are adjusted in the refining process of ZL101A and are respectively increased to 0./7 percent and 0.3 percent.
S2, selecting graphite particles with corresponding particle size distribution according to the grading theory, respectively coating films on the surfaces of the metal Cu on the graphite powder with different particle sizes, and mixing.
S3, mixing the polyvinyl alcohol PVA, the sodium carboxymethylcellulose CMC and the water according to the mass ratio of 8% to 4% to 88%, adding into a stirring tank, heating at 150 ℃, keeping for 5 hours until the materials are fully dissolved to prepare colloid, and naturally cooling to below 35 ℃ for later use.
S4, mixing the mixture obtained in the step S2 with the colloid obtained in the step S3 according to the mass ratio of 20%: mixing 80% of the raw materials, granulating, then putting the granulated powder into a baking oven, baking for 3 hours at 110 ℃, sieving by a 40-mesh sieve until all the granules are sieved, and continuously drying until the water content is 3%; adding 20% of glue into the dried powder, and continuing to carry out artificial granulation; drying in an oven at 100 deg.C for 2 hr, sieving with 40 mesh sieve, and drying to water content of 1.5%; putting the sieved powder into a sealed bag, and placing the sealed bag in a shade place for 5-10 h;
s5, putting the special die into a heating furnace, uniformly heating the die at a speed of 50 ℃/min, and heating to 650 ℃;
s6, adding ZL101A aluminum alloy into a smelting furnace, and smelting at 700 ℃ to obtain aluminum alloy melt; controlling the temperature at 700 ℃, adding a refining agent for refining, removing ash residues on the surface of the aluminum alloy solution to obtain a purer aluminum alloy solution, and vacuumizing and stirring;
s7, filling the graphite powder prepared in the step S4 into a preheated mold S5, and keeping the mold vibrating to ensure that the powder is uniformly compacted; moving the heated mould to a hot press platform, injecting molten aluminum alloy in an S6 aluminum melting furnace into the mould, adjusting the hot press, starting pressing at 2MPa, applying pressure at a constant speed of 3MPa/min up, down, left, right, front and back, keeping the pressure for 10min when the pressure reaches 15MPa, naturally releasing the pressure, and demoulding after the temperature is cooled to room temperature;
s8, carrying out heat treatment on the aluminum-graphite composite material prepared in the step S7, heating a casting blank of the aluminum-graphite composite material to 450 ℃ at a heating rate of 30-50 ℃/h, preserving heat for 4h, carrying out water bath quenching and cooling to room temperature, heating to 160 ℃ at a heating rate of 26 ℃/h, preserving heat for 2.5h, and naturally cooling to room temperature in the air.
S9, performing a surface metallization plating process on the aluminum-graphite finished product prepared in the step S8, removing oil: cleaning with 35g/L HTL-310 agent at 26 deg.C by ultrasonic wave for 3 min; ② weak etching: soaking 70g/L HTL-310 in 55 deg.C for 7 min; washing with water: cleaning with deionized water at 26 deg.C for 2 min; activation: soaking HT-AC600 medicament with concentration of 500ml/L at 26 deg.C for 1.5 min; washing with water: cleaning with deionized water at 26 deg.C for 2 min; sixthly, electroplating nickel: electrolyzing 5um nickel in ferrous sulfate solution, wherein the voltage is 3V and the current is 0.3A; chemical nickel: soaking HT-EN800 medicament with concentration of 150ml/L at pH 5.2 and 86 deg.C for 86 min; and (b) washing with water: cleaning with deionized water at 26 deg.C for 2 min; ninthly, drying: circulating hot air blowing at 130 deg.C for 10-20 min; and (c) dehydrogenation: keeping the temperature at 220 ℃ for 4h, and cooling to room temperature along with the furnace.
And S10, sealing, plastically packaging the aluminum-graphite product prepared in the step S9.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered by the claims.
Claims (10)
1. The preparation method of the aluminum-based graphite particle reinforced composite material is characterized by comprising the following steps:
respectively activating the metal surfaces of graphite powder with different particle sizes, and then preprocessing raw materials according to the raw material design parameters of the heat dissipation adapter;
uniformly mixing the pretreated graphite particles, and then filling the mixture into a mold; putting the mould into a heating furnace, and heating the mould uniformly;
putting the aluminum alloy into an aluminum melting furnace for melting casting and refining, and vacuumizing and stirring to obtain an aluminum alloy melt;
moving the heated mould to a hot press platform, and injecting molten aluminum alloy into the mould; adjusting the pressure of a hot press to the required pressure and pressure maintaining time, carrying out hot pressing, and then demoulding; forging the demolded casting;
and carrying out heat treatment and surface metallization plating processes on the forged casting to obtain the aluminum-based graphite particle reinforced composite material.
2. The method of claim 1,
the grain composition of the graphite is 180#, and the mass ratio of 90# to 5# is 11: 5: 3;
the element components of the aluminum alloy meet the following conditions: the Mg and Si contents are adjusted in the refining process, so that the Mg and the Si contents are respectively increased to 0.3 to 0.7 percent.
3. The method of claim 1,
respectively activating the metal surfaces of graphite powder with different particle sizes, and then performing raw material pretreatment according to raw material design parameters, wherein the raw material pretreatment specifically comprises the following steps:
selecting graphite particles with corresponding particle size distribution according to a grading theory, and respectively carrying out metal Cu surface coating on graphite powder with different particle sizes to obtain a mixture;
mixing polyvinyl alcohol, sodium carboxymethylcellulose and water according to a mass ratio of 8% to 4% to 88%, heating at 150 ℃ and keeping the mixture fully dissolved to prepare a colloid;
the mixture and the colloid are mixed according to the mass ratio of (18-20%): mixing 80% of the raw materials, granulating, drying, sieving, and drying to water content of 3%; adding 20% of glue into the dried powder, and continuing to carry out artificial granulation; drying, sieving, and continuously drying to water content of 1.5%; obtaining the powder.
4. The method of claim 1,
putting the mould into a heating furnace, uniformly heating the mould by heating, and comprising the following specific steps:
putting the mould into a heating furnace, uniformly heating the mould at the speed of 50 ℃/min, and heating to 650 ℃.
5. The method of claim 1,
the method comprises the following steps of putting an aluminum alloy into an aluminum melting furnace for melting and casting:
adding ZL101A aluminum alloy into a smelting furnace, and smelting at the temperature of 650-750 ℃ to obtain aluminum alloy melt; controlling the temperature at 700 ℃, adding a refining agent for refining, and removing ash residues on the surface of the aluminum alloy solution to obtain a purer aluminum alloy solution.
6. The method of claim 1,
the hot pressing specific process comprises the following steps:
adjusting the pressure of a hot press to 2MPa, starting pressing, applying pressure at a constant speed of 3MPa/min up, down, left, right, front and back, keeping the pressure when the pressure reaches 15MPa, naturally releasing pressure, and cooling to room temperature.
7. The method of claim 1,
the heat treatment specifically includes:
heating the aluminum-graphite composite material casting blank to 400-450 ℃ at the heating rate of 30-50 ℃/h, preserving heat for 3-6 h, then quenching in water bath and cooling to room temperature, then heating to 150-180 ℃ at the heating rate of 10-30 ℃/h, preserving heat for 2-3 h, and then naturally cooling to room temperature in air.
8. The method of claim 1,
the surface metallization plating process specifically comprises:
removing oil: HTL-310 medicament with the concentration of 35g/L, and ultrasonic cleaning is carried out at the temperature of 20-30 ℃;
② weak etching: soaking 70g/L HTL-310 in water at 50-60 deg.C;
thirdly, washing for one time: washing with deionized water at 20-30 deg.C;
activation: soaking HT-AC600 medicament with concentration of 500ml/L at 20-30 ℃;
secondary washing: washing with deionized water at 20-30 deg.C;
sixthly, electroplating nickel: electrolyzing 3-6um nickel in ferrous sulfate solution, with voltage of 3V and current of 0.3A;
chemical nickel: soaking HT-EN800 medicament with concentration of 150ml/L at pH of 4.8-5.5 and temperature of 85-90 deg.C;
eighthly, three times of water washing: washing with deionized water at 20-30 deg.C;
ninthly, drying: blowing by circulating hot air at the temperature of 120 ℃ and 150 ℃;
and (c) dehydrogenation: preserving heat at 120-250 ℃, and cooling to room temperature along with the furnace.
9. An aluminum-based graphite particle-reinforced composite material, characterized by being produced by the method according to any one of claims 1 to 9.
10. A heat-dissipating adaptor produced from the aluminum-based graphite particle-reinforced composite material according to claim 9.
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