CN110284019B - Method for directionally doping graphite in metal - Google Patents
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- CN110284019B CN110284019B CN201910624174.8A CN201910624174A CN110284019B CN 110284019 B CN110284019 B CN 110284019B CN 201910624174 A CN201910624174 A CN 201910624174A CN 110284019 B CN110284019 B CN 110284019B
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
Abstract
The invention discloses a method for directionally doping graphite in metal, which comprises the following steps: mixing and stacking metal raw material powder and/or graphite powder plated with a metal film into a sintering layer, so that the graphite powder plated with the metal film is positioned at a preset position of the sintering layer in a preset proportion; heating the sintering layer to sintering by using a directional field under the protection of inert gas; and repeatedly accumulating the sintering layers and sintering layer by layer until the material preparation is finished. The invention adopts the directional field to rapidly fuse and sinter the metal powder and the graphite powder plated with the metal film into the composite material by the metal powder and the graphite powder which are added in increments, thereby not only having high heat conduction performance and improving the strength of the composite material, but also meeting the requirements on the complex shape of the graphite-metal composite material under different conditions.
Description
Technical Field
The invention belongs to the field of metal matrix composite materials, and particularly relates to a method for directionally doping graphite in metal.
Background
With the rapid development in the electronic technology industry, more and more heat is emitted per unit area of the device, and more strict requirements are put forward on the performance of the thermal management material. The development of electronic packaging materials is an important ring, and the materials are required to have the characteristics of high thermal conductivity, low expansion coefficient, light weight and low cost. However, although the thermal expansion coefficient of the traditional Al/SiC composite material, Cu/W composite material, Cu/Mo composite material and other special alloy materials is low, the performances of the materials in the aspects of heat conduction coefficient and heat diffusion coefficient are sacrificed through special processing; diamond and diamond composites have high thermal conductivity, but are difficult to process due to the ultra-high hardness of diamond.
Graphite-metal composites have been receiving more and more attention in thermal management material applications due to their high thermal conductivity, low thermal expansion coefficient, high thermal diffusivity, and the like. The method of graphite-metal composites is generally:
(1) liquid state method: the method is divided into three types, namely a gas pressure infiltration method, an extrusion casting method and pressureless infiltration. Generally, a preform is prepared by hot pressing, dry pressing, injection molding and the like, then the preform is placed in a mold, then vacuum is drawn, the preform is heated to a molten state, and then liquid metal is pressurized (by gas pressure, liquid pressure or gravity, capillary force and the like) to infiltrate the liquid metal into the preform.
(2) Solid state method: mainly powder metallurgy methods including hot press sintering and hot isostatic pressing. The powder (including graphite, metal, etc.) is mixed in certain proportion under proper condition, pressed to form and sintered under vacuum or protection of inert gas.
In the method, the problems of high sintering temperature and high jig requirement exist, more importantly, the doping position and the doping amount of graphite powder cannot be flexibly and directionally controlled, and the prepared graphite-metal composite material has poor processing performance, so that the prepared graphite-metal composite material has great difficulty and low yield in the process of processing into products; especially, when the product has a complicated condition, the preparation time is long and the processing is difficult.
Disclosure of Invention
Aiming at the defects or the improvement requirements of the prior art, the invention provides a method for directionally doping graphite in metal, and aims to realize the preparation of graphite-metal composite materials with doping at any position, controllable doping proportion and complex appearance without a jig by using raw material metal powder and graphite powder subjected to directional field incremental sintering, thereby solving the technical problems of high sintering temperature, high jig requirement and difficulty in preparing the graphite-metal composite materials with complex shapes in the prior art.
To achieve the above object, according to one aspect of the present invention, there is provided a method for directionally doping graphite in a metal, comprising the steps of:
mixing and stacking metal raw material powder and/or graphite powder plated with a metal film into a sintering layer, so that the graphite powder plated with the metal film is positioned at a preset position of the sintering layer in a preset proportion;
heating the sintering layer to sintering by using a directional field under the protection of inert gas;
and repeatedly accumulating the sintering layers and sintering layer by layer until the material preparation is finished.
Preferably, the graphite powder coated with the metal film has an average particle size of 100 μm to 1000 μm, an aspect ratio of 20 to 80, and a surface metal coating thickness of 0.1 μm to 3 μm.
Preferably, in the method for directionally doping graphite in metal, the volume of graphite powder in the sintering layer is less than or equal to 85%.
Preferably, the sintering layer of the method for directionally doping graphite in metal contains or does not contain graphite powder plated with a metal film; the volume of the graphite powder plated with the metal film in the sintering layer containing the graphite powder plated with the metal film accounts for 20-85%.
Preferably, the sintering layer thickness of the method for directionally doping graphite in metal is 40-1000 um.
Preferably, in the method for directionally doping graphite in metal, the metal raw material powder and the metal of the plating film on the surface of the graphite powder are referred to herein as requirements in terms of affinity, such as wetting.
Preferably, the method for directionally doping graphite in metal has the directional field energy between 70W and 700W.
Preferably, the method for directionally doping graphite in metal comprises the step of directionally doping graphite in metal, wherein the directional field is laser and/or microwave.
Preferably, in the method for directionally doping graphite in metal, the directional field scans the sintering layer at a preset speed, so that the corresponding part of the sintering layer is sintered according to a scanning path; the material after the directional field sintering is preferably sintered by using a tube furnace.
Preferably, in the method for directionally doping graphite in metal, the metal raw material powder is aluminum powder with the particle size of 1-200 um, and the sintering thickness is 40-500 um; the surface of the graphite powder plated with the metal film is plated with titanium, the thickness is between 0.1 and 3 mu m, the average particle size of the graphite powder is between 100 and 1000 mu m, and the length-diameter ratio is between 20 and 80;
the directional field is a laser light and,
the directed field energy is between 70W and 700W. The spot diameter at the position of the metal raw material powder is 0.2-20mm, the output power is 80-500W, the scanning speed is 50-100mm/s, and the scanning distance is as follows: 0.08mm-0.3 mm; the spot diameter at the position where the graphite powder and the metal of the metal film are mixed is 0.5-40mm, the output power is 80W-650W W, the scanning speed is 0.2-10mm/s, and the scanning distance is 0.1mm-0.3 mm.
In general, compared with the prior art, the above technical solution contemplated by the present invention can achieve the following beneficial effects:
the invention adopts the directional field to rapidly fuse and sinter the metal powder and the graphite powder plated with the metal film into the composite material by the metal powder and the graphite powder which are added in increments, thereby not only having high heat conduction performance and improving the strength of the composite material, but also meeting the requirements on the complex shape of the graphite-metal composite material under different conditions.
According to the optimized scheme, the method of sintering by using a tube furnace is further adopted, so that the crystal lattice of the material is further optimized, and the heat-conducting property, the electric conductivity and the machining property of the composite material are improved.
Drawings
FIG. 1 is a schematic illustration of a manufacturing process for preparing a graphite-metal composite material according to the present invention;
FIG. 2 is a schematic structural view of the present invention for preparing a graphite-metal composite;
FIG. 3 is a schematic structural view of the present invention for preparing a graphite-metal composite;
FIG. 4 is a schematic structural diagram of the graphite-metal composite material prepared by the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention provides a method for directionally doping graphite in metal, which comprises the following steps:
mixing and stacking metal raw material powder and/or graphite powder plated with a metal film into a sintering layer, so that the graphite powder plated with the metal film is positioned at a preset position of the sintering layer in a preset proportion; the metal raw material powder and the metal coated on the surface of the graphite powder.
The metal raw material powder has a particle size of 1-1000 um, preferably has a melting point lower than 1600 ℃ and a thermal conductivity higher than 75W/M.K. The aluminum alloy has a density of less than 7.8g/cm3 and a strength of more than 60MPa, and preferably has a particle size of 50um, a melting point of 660 ℃, a thermal conductivity of 240W/MK, a density of 2.7g/cm3 and a strength of 80 MPa. The metal raw material powder and the metal of the coating film on the surface of the graphite powder are mutually infiltrated. More preferably, the metal raw material powder and the metal of the plating film on the surface of the graphite powder can form an alloy to form an intermetallic compound.
The graphite powder coated with the metal film has an average particle size of 100-1000 mu m, an aspect ratio of 20-80 and a surface metal coating thickness of 0.1-3 mu m. Such graphite powder has both good thermal conductivity and good mechanical strength.
The thickness of the sintering layer is 40-1000 um, and the volume of the graphite powder in the sintering layer is less than or equal to 85%. The sintering layer contains or does not contain graphite powder plated with a metal film; the volume of the graphite powder plated with the metal film in the sintering layer containing the graphite powder plated with the metal film accounts for 20-85%. Sintering layers containing graphite powder with different proportions can be sequentially sintered, stacked in the vertical direction or spliced together in the horizontal direction to form a preset anisotropic material; the thickness of the sintering layer of the graphite powder without the plated metal film is preferably 40-500 um, and the material is preferably aluminum.
Heating the sintering layer to sintering by using a directional field under the protection of inert gas; the energy of the directional field is 70W-700W, and the directional field is laser and/or microwave. The directional field scans the sintered layer at a preset speed, so that the corresponding part of the sintered layer is sintered according to a scanning path.
The thickness of the sintering layer is matched with the energy of the directional field, and the components of each sintering layer can be independently controlled, including the type of metal powder, the specification of the metal powder, the specification of graphite powder and the specification of the metal type of a graphite powder coating film, so that graphite doped metal with complex component proportion can be created in different spatial dimensions, and different performance requirements can be met; and meanwhile, the sintering layer can be sintered in an oriented mode through the oriented field, and the composite metal material with the complex shape is prepared in the sintering layer according to the scanning path. The graphite doped metal material with complex appearance and components can be freely prepared by combining the two points. The premise for realizing the technology is that the surface of the graphite powder is provided with the metal coating, so that stable doping can be formed as long as the metal on the surface of the graphite and the metal powder are fused and sintered, and the sintering process is a metal-metal reaction which is different from a metal-graphite reaction, so that the mixed powder can be rapidly sintered and molded under the condition of loading an oriented field.
Preferably, the metal raw material powder is aluminum powder, copper powder, iron or iron alloy powder, silver powder and/or titanium powder, and the surface coating of the graphite powder is a copper, nickel or titanium film; more preferably, the metal raw material powder is aluminum powder, and the surface of the graphite powder is plated with a titanium film, wherein titanium can improve the strength of the graphite flake, and can form strong chemical bonding with graphite to generate TiC, so that the graphite and aluminum are prevented from directly generating brittle phase Al4C3Meanwhile, titanium and aluminum are alloyed, and the interface contact is tight.
And repeatedly accumulating the sintering layers and sintering layer by layer until the material preparation is finished.
The above-mentioned material is preferably hot-pressed and sintered in a hot-pressing furnace.
The following are examples:
example 1:
the metal raw material powder is aluminum metal powder with the particle size of 50um, the melting point of 660 ℃, the thermal conductivity of 240W/MK, the density of 2.7g/cm3 and the strength of 80 MPa.
The graphite powder plated with the metal film has the average particle size of 500 mu m, the length-diameter ratio of 30 and the surface metal plating thickness of 0.2 mu m. Metal type of metal film, process for producing plated film
The thickness of the sintering layer is 50um, and the volume of the graphite powder is 55 percent
Heating the sintering layer to sintering by using a directional field under the protection of inert gas; the directional field is laser and/or microwave.
Metal raw material layer: spot diameter 0.2mm, output power 100W, scanning speed 100mm/s, scanning interval: 0.1mm. graphite and metal mixed layer: the diameter of a light spot is 0.8mm, the output power is 80W, the scanning speed is 2mm/s, and the scanning interval is 0.25 mm.
Preparation of graphite (titanizing) -aluminum composite material
The first step is as follows: uniformly mixing scaly graphite powder with the particle size of 500 microns, calcium chloride and titanium powder to prepare mixed powder, wherein the sodium chloride accounts for 40% and the titanium powder accounts for 20% of the total weight of the mixed powder, putting the mixed powder into a vacuum tube furnace, vacuumizing until the vacuum degree is about 10-220Pa, heating up at a rate of 15 ℃/min, heating to 1300 ℃, preserving heat for 100min, and then cooling to room temperature along with the furnace. Taking out the mixed powder treated at high temperature, putting the mixed powder into a beaker filled with deionized water, putting the beaker filled with the treated mixed powder and the deionized water into a drying oven, setting the temperature at 85 ℃, keeping the temperature for 30min, taking out the beaker, pouring out the aqueous solution of sodium chloride, pouring the deionized water again, repeating the operations, cleaning the mixed powder for 5 times, respectively sieving the cleaned and dried mixed powder with a 30-mesh sieve, and removing the excessive silicon powder.
The second step is that: taking out the aluminum powder and putting the aluminum powder into a container A.
The third step: the graphite flakes and the aluminum powder which are coated in the first step are put into a container B.
The fourth step: firstly, uniformly spreading aluminum powder on a substrate from a container A, and sintering the substrate by adopting laser to form a metal layer; then spreading the graphite powder and metal mixed powder of the container B on the sintered metal, sintering by laser, repeating the above process to the required thickness, finally sintering a layer of aluminum layer to increase the hardness, and forming the high-thermal-conductivity composite material with a laminated structure in which the metal layers and the graphite layers alternately appear and the last layer is aluminum (as shown in figure 2). The atmosphere was an argon atmosphere lamp protective atmosphere throughout the fabrication process.
If the thermal conductivity is required to be increased, the prepared composite material can be placed in a hot pressing furnace, wherein the pressure of the hot pressing furnace is 40-60MPa, the degree of vacuum pumping is about 10-220Pa, the heating rate is 15 ℃/min, the temperature is increased to 850-1050 ℃, and the temperature is maintained for 20-120min for sintering. Then the sample is taken out after natural cooling.
Example 2:
the metal raw material powder has the particle size of 500um, the melting point of 1500 ℃, the thermal conductivity of 75W/MK and the density of 7.8g/cm3And a strength of 170 MPa.
The graphite powder plated with the metal film has the average particle size of 200 mu m, the length-diameter ratio of 50 and the surface metal plating thickness of 2 mu m.
The thickness of the sintering layer is 200um, and the volume of the graphite powder is 70 percent.
Heating the sintering layer to sintering by using a directional field under the protection of inert gas; the directional field is laser and/or microwave.
Metal raw material layer: spot diameter 20mm, output power 400W, scanning speed 60mm/s, scanning pitch: 0.1mm. graphite and metal mixed layer: the diameter of a light spot is 33mm, the output power is 600W, the scanning speed is 0.3mm/s, and the scanning interval is 0.2 mm.
Preparation of graphite (copper-plated) -iron composite material
The first step is as follows: scaly graphite powder with the grain diameter of 200um is taken. Firstly, soaking graphite powder in 200g/L NaOH solution for 40min to remove grease, and then washing the graphite powder to be neutral; then 20% (the volume ratio of the concentrated nitric acid to the water is 1: 4) of HNO is added. Boiling the solution for 15-20 min, and then washing with waterDrying at 100 deg.C until neutral. 8g of CuSO was added to 800mL of distilled water4·5H2Preparing electroplating solution from O and 15mL of concentrated sulfuric acid, adding 5g of graphite powder, controlling the current density to be 9A/dm2, and stirring for 80min every 10 min. After the electroplating is finished, washing the substrate to be neutral, passivating the substrate by using 0.5% Benzotriazole (BTA) as a passivating agent at the temperature of 55 ℃ for 5min, and drying the substrate at the temperature of 100 ℃. Obtaining the graphite powder plated with copper.
The second step is that: taking out the stored iron powder and putting the iron powder into a container A
The third step: putting the graphite flakes and the iron powder which are coated in the first step into a container B
The fourth step: firstly, flatly paving iron powder on a substrate from a container A according to a set track, and sintering the iron powder by adopting laser to form a metal layer; and then spreading the graphite powder and metal mixed powder in the container B according to a set track, sintering by adopting laser, repeating the process to the required thickness, and forming the high-thermal-conductivity composite material with the laminated structure as shown in figure 3. The atmosphere was an argon atmosphere lamp protective atmosphere throughout the fabrication process.
If the thermal conductivity is required to be increased, the prepared composite material can be placed in a hot pressing furnace, wherein the pressure of the hot pressing furnace is 40-60MPa, the degree of vacuum pumping is about 10-220Pa, the heating rate is 15 ℃/min, the temperature is increased to 850-1050 ℃, and the temperature is maintained for 20-120min for sintering. Then the sample is taken out after natural cooling.
Example 3:
the metal raw material powder is metal copper powder with the particle size of 800um, the melting point of 1000 ℃, the thermal conductivity of 397W/MK, the density of 8.9g/cm3 and the strength of 220 MPa.
The graphite powder coated with the metal film has the average grain diameter of 800 microns, the length-diameter ratio of 70 and the thickness of the metal coating on the surface of 2.5 microns.
The thickness of the sintering layer is 900um, and the volume of the graphite powder is 80 percent
Heating the sintering layer to sintering by using a directional field under the protection of inert gas; the directional field is laser and/or microwave.
Metal raw material layer: spot diameter 20mm, output power 400W, scanning speed 60mm/s, scanning pitch: 0.1mm. graphite and metal mixed layer: the diameter of a light spot is 0.8mm, the output power is 150W, the scanning speed is 3mm/s, and the scanning interval is 0.15mm
Preparation of graphite (titanizing) -copper composite material
The first step is as follows: uniformly mixing scaly graphite powder with the particle size of 800 microns, calcium chloride and titanium powder to prepare mixed powder, wherein the sodium chloride accounts for 40% and the titanium powder accounts for 30% of the total weight of the mixed powder, putting the mixed powder into a vacuum tube furnace, vacuumizing until the vacuum degree is about 10-220Pa, heating up at a rate of 15 ℃/min, heating to 1300 ℃, preserving heat for 100min, and then cooling to room temperature along with the furnace. Taking out the mixed powder treated at high temperature, putting the mixed powder into a beaker filled with deionized water, putting the beaker filled with the treated mixed powder and the deionized water into a drying oven, setting the temperature at 85 ℃, keeping the temperature for 30min, taking out the beaker, pouring out the aqueous solution of sodium chloride, pouring the deionized water again, repeating the operations, cleaning the mixed powder for 5 times, respectively sieving the cleaned and dried mixed powder with a 30-mesh sieve, and removing the excessive silicon powder.
The second step is that: taking out the copper powder and putting the copper powder into a container A
The third step: putting the graphite flakes and the copper powder which are coated in the first step into a container B
The fourth step: firstly, uniformly spreading copper powder on a substrate from a container A according to a set position, then uniformly spreading graphite powder and metal mixed powder of a container B according to a set position, sintering by adopting laser, and repeating the process until the required thickness is as shown in figure 4. The atmosphere was an argon atmosphere lamp protective atmosphere throughout the fabrication process.
If the thermal conductivity is required to be increased, the prepared composite material can be placed in a hot pressing furnace, wherein the pressure of the hot pressing furnace is 40-60MPa, the degree of vacuum pumping is about 10-220Pa, the heating rate is 15 ℃/min, the temperature is increased to 850-1050 ℃, and the temperature is maintained for 20-120min for sintering. Then the sample is taken out after natural cooling.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (12)
1. A method of directionally doping graphite in a metal, comprising the steps of:
mixing and stacking metal raw material powder and graphite powder plated with a metal film into a sintering layer, so that the graphite powder plated with the metal film is positioned at a preset position of the sintering layer in a preset proportion;
heating the sintering layer to sintering by using a directional field under the protection of inert gas;
and repeatedly accumulating the sintering layers and sintering layer by layer until the material preparation is finished.
2. The method according to claim 1, wherein the graphite powder coated with the metal film has an average particle size of 100 μm to 1000 μm, an aspect ratio of 20 to 80, and a surface metallization thickness of 0.1 μm to 3 μm.
3. The method of directionally doping graphite in metals according to claim 1, wherein the volume of graphite powder in the sintered layer is 85% or less.
4. The method of directionally doping graphite in metals according to claim 1, wherein the sintered layer contains or does not contain graphite powder coated with a metal film; the volume of the graphite powder plated with the metal film in the sintering layer containing the graphite powder plated with the metal film accounts for 20-85%.
5. The method of directionally doping graphite in metal according to claim 1, wherein the sintered layer has a thickness in the range of 40um to 1000 um.
6. The method of directionally doping graphite in metals of claim 1 wherein the metal feedstock powder and the metal of the coating on the surface of the graphite powder are capable of forming an alloy.
7. The method of directionally doping graphite in metal according to claim 1, wherein said directed field energy is between 70W and 700W.
8. The method of directionally doping graphite in metal according to claim 5, wherein said directional field is laser and/or microwave.
9. The method of directionally doping graphite in metal according to claim 5, wherein said directional field scans said sintered layer at a predetermined speed such that a corresponding portion of said sintered layer is sintered in accordance with a scan path.
10. The method of directionally doping graphite in metal as claimed in claim 1 wherein the material after directional field sintering is sintered using a tube furnace.
11. The method of directionally doping graphite in metal according to claim 1, wherein the metal raw material powder is aluminum powder with a particle size of 1um-200um, and the sintering thickness is 40um-500 um; plating titanium, nickel and/or copper on the surface of the graphite powder plated with the metal film, wherein the thickness of the graphite powder is between 0.1 and 3 mu m, the average particle size of the graphite powder is between 100 and 1000 mu m, and the length-diameter ratio of the graphite powder is between 20 and 80;
the directional field is laser, and the energy of the directional field is between 70W and 700W.
12. The method for directionally doping graphite in metal as claimed in claim 11, wherein the directional field is laser, the spot diameter at the position where the metal raw material powder is located is 0.2-20mm, the output power is 80W-500W, the scanning speed is 50-100mm/s, the scanning distance is: 0.08mm-0.3 mm; the spot diameter at the position where the graphite powder and the metal of the metal film are mixed is 0.5-40mm, the output power is 80-650W, the scanning speed is 0.2-10mm/s, and the scanning distance is 0.1-0.3 mm.
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