CN115369278B - Die-casting diamond/rare earth aluminum alloy composite material and preparation method thereof - Google Patents

Die-casting diamond/rare earth aluminum alloy composite material and preparation method thereof Download PDF

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CN115369278B
CN115369278B CN202210957713.1A CN202210957713A CN115369278B CN 115369278 B CN115369278 B CN 115369278B CN 202210957713 A CN202210957713 A CN 202210957713A CN 115369278 B CN115369278 B CN 115369278B
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diamond
temperature
rare earth
aluminum alloy
alloy composite
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CN115369278A (en
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秦文波
郭晶晶
舒登峰
黄飞
孙佳晨
陈昊
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Huijing New Material Technology Hangzhou Co ltd
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1005—Pretreatment of the non-metallic additives
    • C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1094—Alloys containing non-metals comprising an after-treatment
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/223—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating specially adapted for coating particles
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering

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Abstract

The application provides a die-casting diamond/rare earth aluminum alloy composite material and a preparation method thereof, wherein a magnetron sputtering method is adopted to carry out nanocrystallization on the surfaces of one-dimensional diamond micron lines and diamond particles and design different metal coatings to improve the interface wettability with an aluminum matrix, so that the strength and the toughness of the aluminum alloy are improved; a three-dimensional foam network structure prefabricated body is constructed to improve the internal heat dissipation channel, further improve the heat conduction performance and strength of the prefabricated body, and further improve the heat conduction performance and strength of the prefabricated body; in order to further enhance the heat conductivity and toughness of the aluminum matrix, rare earth elements of lanthanum (La) and cerium (Ce) are added into the aluminum matrix system, and the aluminum matrix material is optimized from an atomic level, so that the heat conductivity and the toughness and the die-casting property of the aluminum matrix material are improved; therefore, the high heat conductivity and high toughness performance of the material are realized on the premise of light weight and high strength, and the thermal interface material with lighter weight, better heat conductivity and more optimized structure is provided for various fields.

Description

Die-casting diamond/rare earth aluminum alloy composite material and preparation method thereof
Technical Field
The invention relates to the technical field of thermal interface materials, in particular to a die-casting diamond/rare earth aluminum alloy composite material and a preparation method thereof.
Background
An ideal thermal interface material should have good properties of high thermal conductivity, high flexibility, surface wettability, high pressure sensitivity, good stability of cold and hot cycles, reusability, etc. The metal matrix composite material combines the advantages of excellent thermal conductivity and machinability of the metal matrix and the performance of high thermal conductivity and low thermal expansion of the reinforcer. The thermal conductivity of natural diamond is very high (2200 W.m < -1 > K < -1 >) and the thermophysical performance is excellent, but the preparation of the large-size block heat conduction material by pure diamond is difficult and the cost is high.
With the great popularization of artificial single crystal diamond products, the metal matrix composite material is prepared by combining diamond with extremely excellent thermal conductivity and an aluminum matrix with high thermal conductivity, so that the industrial large-scale production and application of the metal matrix composite material become possible. However, diamond is a crystal bonded by covalent bonds, and when a metal-based alloy is bonded with diamond abrasives to manufacture tools, the force interface of the diamond and complexing agent elements and the like is not infiltrated, so that the diamond abrasives can only be mechanically embedded in the complexing agent, the service performance and the service life of the diamond tools are greatly influenced, the wettability between a metal matrix and the diamond is poor, and the interface effect becomes a bottleneck restricting the performance improvement of the diamond tools. Meanwhile, on the premise of high heat conduction and high strength, the realization of high strength and high toughness and the satisfaction of special processing requirements become urgent matters for solving the thermal interface material.
Disclosure of Invention
The application provides a die-casting diamond/rare earth aluminum alloy composite material and a preparation method thereof.
According to a first aspect, there is provided a method of preparing a die cast diamond/rare earth aluminium alloy composite material comprising the steps of:
(1) Taking a proper amount of one-dimensional diamond microwires and diamond particles for washing, putting the washed diamond sample into ethanol, stirring at a low temperature until the ethanol is completely evaporated, and drying in an oven to obtain powder after dispersion treatment;
(2) Putting a proper amount of the sample treated by the powder in the step (1) into a sample chamber, and depositing nano Ti on the surface of a diamond sample on a magnetron sputtering ion plating machine; carrying out low-temperature heat treatment on the diamond with the Ti sprayed on the surface to obtain a silvery white Ti-diamond sample with a nano-sized surface;
(3) And (3) metalizing the surface of the Ti-diamond sample obtained in the step (2) by adopting the method obtained in the step (2), and plating silver and aluminum on the surface of the Ti-diamond sample to obtain the Ti-Ti-Ag-Al-diamond sample.
(4) Adding a proper amount of Ti-Ag-Al-diamond in the step (3) into the curdlan glue solution, and performing ultrasonic and electric stirring at room temperature to form a uniform colloidal solution; then slowly stirring and heating to 60 ℃, then violently stirring and slowly heating to 100 ℃, slowly fermenting to form uniform bubbles at most, and continuously stirring to improve the gel strength, so that the macromolecular chains tightly wrap the one-dimensional diamond microwires and diamond particles with the nano-sized and metallized surfaces to form a stable porous foam diamond network structure, and a three-dimensional porous network structure prefabricated body consisting of the diamond nanowires and the diamond particles is obtained; respectively carrying out low-temperature heat treatment and high-temperature heat treatment on the obtained gel, and keeping the temperature at 600 ℃;
(5) Putting the Al block into a graphite mold, heating to molten liquid aluminum, adding La-Ce rare earth chloride solution, ultrasonically stirring, and keeping the temperature in the furnace; then pouring the molten liquid rare earth aluminum alloy into a prefabricated body grinding tool with a three-dimensional porous network structure by adopting a gas pressure infiltration method, quickly applying pressure of 10MPa by using high-purity nitrogen, keeping the pressure for a proper time, returning to a lifting platform after infiltration, turning off a heating power supply, and quickly cooling a sample in a furnace under a high-temperature atmosphere to obtain the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material;
(6) Carrying out cold rolling treatment on the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material after aging treatment; before cold rolling treatment, ultrasonically cleaning the surface of a Ti-Ag-diamond/rare earth aluminum alloy composite material test block; and then carrying out solid solution treatment and cold rolling treatment on the Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block at room temperature to obtain the die-cast diamond/rare earth aluminum alloy composite material.
In some embodiments, in step (1), the type of diamond particles is HHD90, the particle size is 200 to 300 μm, the diamond microwire particle size is 400 to 800 μm, and the amount of one-dimensional diamond microwire and diamond particles is 1:1 to 3:1, uniformly mixing 100g, washing: ultrasonic washing with acetone, ethanol and deionized water for 10min.
In some embodiments, in step (2), the deposition process: using 99.99% of nano Ti as a target material, the background vacuum of 4.0-4.6 multiplied by 10 < -3 > Pa, the working gas argon (99.999%), the working pressure of 0.2-0.3 Pa, the sputtering power of 4-5 kW and the sputtering time of 100-360 s; in order to make each crystal face plating layer of the diamond uniform, an oscillation stirring device is designed automatically to obtain a silvery white diamond sample; low-temperature heat treatment: the heating speed is 5 ℃/min, the temperature is kept at 300 ℃ for 1h, and the mixture is naturally cooled to room temperature and the thickness is 80nm.
In some embodiments, in the step (3), the silver plating layer has a thickness of 130nm in order to improve its thermal conductivity, and the aluminum plating layer has a thickness of 90nm in order to ensure good bonding strength with the aluminum alloy substrate. .
In some embodiments, in the step (4), the colloidally liquid is configured as follows: naCl is added into 100mL of deionized water to prepare an alkaline solution with the pH =8, curdlan is added into the alkaline solution, and the curdlan is sheared or colloid-milled until the curdlan is completely dissolved to prepare a glue solution. Low-temperature heat treatment: keeping the temperature at 100 ℃ for 30min, increasing the temperature at the speed of 10 ℃/min, reinforcing a porous foam structure, and forming a compact three-dimensional network structure assembled by diamond nanowires and diamond particles. High-temperature heat treatment: keeping the temperature at 600 ℃ for 1h, and removing the long chain of curdlan at the heating rate of 10 ℃/min.
In some embodiments, the purity of the Al block in step (5) is 99.99%. The molar ratio of LaCl3 to CeCl3 in the La-Ce rare earth chloride solution is 1:1.
in some embodiments, in the step (5), the surface of the Ti-Ag-diamond/rare earth aluminum alloy composite test block is sequentially subjected to ultrasonic cleaning for 10min by using acetone, ethanol and deionized water before the cold rolling treatment;
the solution treatment comprises: putting the Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block into a box type resistance furnace with the temperature of 600 ℃ for heat preservation for 10-25 min, taking out and cooling to room temperature by water;
the cold rolling treatment comprises the following steps: in the cold rolling test, a phi 140-260 two-roller reversible temperature rolling mill is adopted, the rolling reduction of each pass is 0-4 mm, the plate thickness is finally rolled to be 1-5 mm, and the total rolling reduction is 20-80%; heating the box-type resistance furnace to 610 ℃, then putting the Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block with 20-80% of cold deformation into the box-type resistance furnace, preserving the temperature for 10-30 min, and quickly taking out the box-type resistance furnace for air cooling to room temperature.
According to a second aspect, there is provided a die cast diamond/rare earth aluminium alloy composite material, using the method of preparation as described in the first aspect.
According to the embodiment, the surface of the one-dimensional diamond micron line and the diamond particle is subjected to nanocrystallization by a magnetron sputtering method, and different metal coatings are designed to improve the interface wettability with an aluminum matrix, so that the strength and the toughness of the aluminum alloy are improved; a three-dimensional foam network structure prefabricated body is constructed to improve the internal heat dissipation channel, further improve the heat conduction performance and strength of the prefabricated body, and further improve the heat conduction performance and strength of the prefabricated body; in order to further enhance the heat conductivity and toughness of the aluminum matrix, rare earth elements of lanthanum (La) and cerium (Ce) are added into the aluminum matrix system, and the aluminum matrix material is optimized from an atomic level, so that the heat conductivity and the toughness and the die casting property of the aluminum matrix are improved; therefore, the high heat conduction and high toughness performance of the material is realized on the premise of light weight and high strength, and the thermal interface material with lighter weight, better heat conduction and more optimized structure is provided for various fields.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments. Wherein like elements in different embodiments are numbered with like associated elements. In the following description, numerous details are set forth in order to provide a better understanding of the present application. In some instances, certain operations related to the present application have not been shown or described in this specification in order not to obscure the core of the present application with unnecessary detail, and it is not necessary for those skilled in the art to describe these operations in detail, so that they may be fully understood from the description in the specification and the general knowledge in the art.
Furthermore, the described features, operations, or characteristics may be combined in any suitable manner to form various embodiments. Also, the various steps or actions in the method descriptions may be transposed or transposed in order, as will be apparent to one of ordinary skill in the art. Thus, the various sequences in the specification are for the purpose of clearly describing one embodiment only and are not meant to be necessarily order unless otherwise indicated where a certain order must be followed.
Example 1
(1) And (2) taking 100g of one-dimensional diamond micron line and diamond particles (the weight ratio is 1:1) for washing (acetone, ethanol and finally deionized water are used for washing and ultrasonic treatment is carried out for 10 min), then putting the washed diamond sample into ethanol, stirring at low temperature until the ethanol is completely evaporated, and drying in an oven at 60 ℃ for 10h to obtain powder for later use.
(2) And (3) putting 50g of the sample treated by the powder in the step (1) into a sample chamber, and depositing nano Ti on the surface of the diamond sample on a magnetron sputtering ion plating machine, wherein the thickness of the nano Ti is 80nm. The deposition process comprises the following steps: 99.99 percent of nano Ti is used as a target material, and the background vacuum is 4.0-4.6 multiplied by 10 -3 Pa, working gas argon (99.999%), working pressure 0.2-0.3 Pa, sputtering power 4-5 kW, and sputtering time 100-120 s. In order to make the plating layers of all crystal faces of the diamond uniform, an oscillating and stirring device is designed by self to obtain a silver-white diamond sample. And (3) carrying out low-temperature heat treatment on the diamond with the Ti sprayed on the surface, wherein the heating rate is 5 ℃/min, the heat preservation is carried out for 1h at the temperature of 300 ℃, and the diamond is naturally cooled to the room temperature to obtain the Ti-diamond sample with the nano-sized surface.
(3) And then, metalizing the surface of the Ti-diamond sample in the step (2) by adopting a method in the step (2), plating a 130nm silver coating on the surface of the Ti-diamond sample to improve the heat conductivity of the Ti-diamond sample, and plating a 90nm aluminum coating to ensure good bonding strength with an aluminum alloy matrix to prepare the Ti-Ag-Al-diamond.
(4) Adding 50g of Ti-Ag-Al-diamond in (3) into curdlan glue solution (NaCl is added into 100mL of deionized water to prepare an alkaline solution with pH =8, then adding the curdlan into the alkaline solution, and preparing the curdlan into the glue solution by shearing or colloid milling until the curdlan is completely dissolved), ultrasonically adding the curdlan at the room temperature of 25 ℃, electrically stirring for 1h, and then continuously and violently stirring for 60min to form a uniform colloidal solution. Then slowly stirring and heating to 60 ℃, continuously stirring for 30min, then violently stirring and slowly heating to 100 ℃, slowly fermenting to form uniform bubbles, and continuously stirring for 15min to improve the gel strength, so that the macromolecular chains tightly wrap the one-dimensional diamond microwires and diamond particles with the surfaces being nano-sized and metallized, and a stable porous foam diamond network structure is formed. Respectively carrying out low-temperature heat treatment and high-temperature heat treatment on the obtained gel, and reinforcing a multi-cavity foam structure by low-temperature heat treatment (keeping the temperature at 100 ℃ for 30min and increasing the temperature at a speed of 10 ℃/min) to form a compact three-dimensional network structure assembled by diamond nanowires and diamond particles; performing high-temperature heat treatment (keeping the temperature at 600 ℃ for 1h, and increasing the temperature at a speed of 10 ℃/min), removing the long chain of curdlan to obtain a three-dimensional porous network structure preform consisting of diamond microwires and diamond particles, and keeping the temperature at 600 ℃ for later use.
(5) Putting Al (purity 99.99%) blocks into a graphite mould, heating to molten liquid aluminum, and adding La-Ce rare earth chloride solution (LaCl) 3 ：CeCl 3 In a molar ratio of 1: 1) Ultrasonic stirring is carried out for 5-6 s, and the temperature in the furnace is kept at 700 ℃ for 30 min. Pouring molten liquid rare earth aluminum alloy into a prefabricated body grinding tool with a three-dimensional porous network structure by adopting a gas pressure infiltration method, quickly applying pressure of 10MPa by using high-purity nitrogen with the purity of 99.99 percent, keeping for 20min, returning to a lifting platform after infiltration, closing a heating power supply, and quickly cooling a sample in a furnace under a high-temperature atmosphere to obtain the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material.
(6) And (3) carrying out cold rolling treatment on the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material after aging treatment. And (3) carrying out cold rolling treatment, and carrying out ultrasonic cleaning on the surface of the Ti-Ag-diamond/rare earth aluminum alloy composite material test block for 10min by using acetone, ethanol and deionized water in sequence. And (3) putting the Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block into a box-type resistance furnace with the temperature of 600 ℃ for heat preservation for 15min, taking out and cooling to room temperature by water. And (3) carrying out cold rolling treatment on the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material test block subjected to the solution treatment at room temperature, and finally rolling the plate to be 5mm by adopting a phi 140/260 two-roller reversible temperature rolling mill in a cold rolling test. And then heating the box-type resistance furnace to 610 ℃, then keeping the temperature of the Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block with the thickness of 5mm for 25min, quickly taking out the test block and cooling the test block to room temperature in an air cooling mode, and finally obtaining the die-casting diamond/rare earth aluminum alloy composite material with high heat conductivity, high strength and high toughness, wherein the pattern size of the die-casting diamond/rare earth aluminum alloy composite material is 120mm multiplied by 60mm multiplied by 5mm.
Example 2
(1) And (2) taking 100g of one-dimensional diamond micron line and diamond particles (the weight ratio is 2:1) for washing (acetone, ethanol and finally deionized water are used for washing and ultrasonic treatment is carried out for 10 min), then putting the washed diamond sample into ethanol, stirring at low temperature until the ethanol is completely evaporated, and drying in an oven at 60 ℃ for 10h to obtain powder for later use.
(2) And (3) putting 50g of the sample treated by the powder in the step (1) into a sample chamber, and depositing nano Ti on the surface of the diamond sample on a magnetron sputtering ion plating machine, wherein the thickness of the nano Ti is 80nm. The deposition process comprises the following steps: 99.99 percent of nano Ti is taken as a target material, and the background vacuum is 4.0-4.6 multiplied by 10 -3 Pa, working gas argon (99.999%), working pressure 0.2-0.3 Pa, sputtering power 4-5 kW, and sputtering time 100-120 s. In order to make the plating layers of all crystal faces of the diamond uniform, an oscillating and stirring device is designed by self to obtain a silvery white diamond sample. And carrying out low-temperature heat treatment on the diamond with the Ti sprayed on the surface, wherein the heating speed is 5 ℃/min, the heat preservation is carried out for 1h at the temperature of 300 ℃, and naturally cooling to the room temperature to obtain the Ti-diamond sample with the nano-sized surface.
(3) And then, metalizing the surface of the Ti-diamond sample in the step (2) by adopting a method in the step (2), plating a 130nm silver coating on the surface of the Ti-diamond sample to improve the heat conductivity of the Ti-diamond sample, and plating a 90nm aluminum coating to ensure good bonding strength with an aluminum alloy matrix to prepare the Ti-Ag-Al-diamond.
(4) Adding 50g of Ti-Ag-Al-diamond in (3) into curdlan glue solution (NaCl is added into 100mL of deionized water to prepare an alkaline solution with pH =8, then adding the curdlan into the alkaline solution, and preparing the curdlan into the glue solution by shearing or colloid milling until the curdlan is completely dissolved), ultrasonically adding the curdlan at the room temperature of 25 ℃, electrically stirring for 1h, and then continuously and violently stirring for 60min to form a uniform colloidal solution. Then slowly stirring and heating to 60 ℃, continuously stirring for 30min, then violently stirring and slowly heating to 100 ℃, slowly fermenting to form uniform bubbles, and continuously stirring for 15min to improve the gel strength, so that the macromolecular chains tightly wrap the one-dimensional diamond microwires and diamond particles with the surfaces being nano-sized and metallized, and a stable porous foam diamond network structure is formed. Respectively carrying out low-temperature heat treatment and high-temperature heat treatment on the obtained gel, and reinforcing a multi-cavity foam structure by low-temperature heat treatment (keeping the temperature at 100 ℃ for 30min and increasing the temperature at a speed of 10 ℃/min) to form a compact three-dimensional network structure assembled by diamond nanowires and diamond particles; and (4) performing high-temperature heat treatment (keeping the temperature at 600 ℃ for 1h, and increasing the temperature at a speed of 10 ℃/min), removing the long chain of curdlan to obtain a three-dimensional porous network structure preform consisting of diamond nanowires and diamond particles, and keeping the temperature at 600 ℃ for later use.
(5) Putting Al (purity 99.99%) blocks into a graphite mold, heating to molten liquid aluminum, and adding La-Ce rare earth chloride solution (LaCl) 3 ：CeCl 3 In a molar ratio of 1: 1) Ultrasonic stirring is carried out for 5-6 s, and the temperature in the furnace is kept at 700 ℃ for 30 min. Pouring molten liquid rare earth aluminum alloy into a prefabricated body grinding tool with a three-dimensional porous network structure by adopting a gas pressure infiltration method, quickly applying pressure of 10MPa by using high-purity nitrogen with the purity of 99.99 percent, keeping for 20min, returning to a lifting platform after infiltration, closing a heating power supply, and quickly cooling a sample in a furnace under a high-temperature atmosphere to obtain the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material.
(6) And carrying out cold rolling treatment on the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material after aging treatment. And in the cold rolling treatment, the surface of the Ti-Ag-diamond/rare earth aluminum alloy composite material test block is sequentially cleaned by acetone, ethanol and deionized water for 10min in an ultrasonic manner. And (3) putting the Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block into a box type resistance furnace with the temperature of 600 ℃ for heat preservation for 15min, taking out and cooling to room temperature by water. And (3) carrying out cold rolling treatment on the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material test block subjected to the solution treatment at room temperature, and finally rolling the plate to be 5mm by adopting a phi 140 x 260 two-roller reversible temperature rolling mill in a cold rolling test. And then heating the box-type resistance furnace to 610 ℃, then keeping the temperature of the Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block with the thickness of 5mm for 25min, quickly taking out the test block and cooling the test block to room temperature in an air cooling mode, and finally obtaining the die-casting diamond/rare earth aluminum alloy composite material with high heat conductivity, high strength and high toughness, wherein the pattern size of the die-casting diamond/rare earth aluminum alloy composite material is 120mm multiplied by 60mm multiplied by 5mm.
Embodiment 3
(1) And (2) taking 100g of one-dimensional diamond micron line and diamond particles (the weight ratio is 3:1) for washing (acetone, ethanol and finally deionized water are used for washing and ultrasonic treatment is carried out for 10 min), then putting the washed diamond sample into ethanol, stirring at low temperature until the ethanol is completely evaporated, and drying in an oven at 60 ℃ for 10h to obtain powder for later use.
(2) And (3) putting 50g of the sample treated by the powder in the step (1) into a sample chamber, and depositing nano Ti on the surface of the diamond sample on a magnetron sputtering ion plating machine, wherein the thickness of the nano Ti is 80nm. The deposition process comprises the following steps: 99.99 percent of nano Ti is taken as a target material, and the background vacuum is 4.0-4.6 multiplied by 10 -3 Pa, working gas argon (99.999%), working pressure of 0.2-0.3 Pa, sputtering power of 4-5 kW, and sputtering time of 100-120 s. In order to make the plating layers of all crystal faces of the diamond uniform, an oscillating and stirring device is designed by self to obtain a silver-white diamond sample. And (3) carrying out low-temperature heat treatment on the diamond with the Ti sprayed on the surface, wherein the heating rate is 5 ℃/min, the heat preservation is carried out for 1h at the temperature of 300 ℃, and the diamond is naturally cooled to the room temperature to obtain the Ti-diamond sample with the nano-sized surface.
(3) And then, metalizing the surface of the Ti-diamond sample in the step (2) by adopting a method in the step (2), plating a 130nm silver coating on the surface of the Ti-diamond sample to improve the heat conductivity of the Ti-diamond sample, and plating a 90nm aluminum coating to ensure good bonding strength with an aluminum alloy matrix to prepare the Ti-Ag-Al-diamond.
(4) Adding 50g of Ti-Ag-Al-diamond in (3) into curdlan glue solution (NaCl is added into 100mL of deionized water to prepare an alkaline solution with pH =8, then adding the curdlan into the alkaline solution, and preparing the curdlan into the glue solution by shearing or colloid milling until the curdlan is completely dissolved), ultrasonically adding the curdlan at the room temperature of 25 ℃, electrically stirring for 1h, and then continuously and violently stirring for 60min to form a uniform colloidal solution. Then slowly stirring and heating to 60 ℃, continuously stirring for 30min, then violently stirring and slowly heating to 100 ℃, slowly fermenting to form uniform bubbles, and continuously stirring for 15min to improve the gel strength, so that the macromolecular chains tightly wrap the one-dimensional diamond microwires and diamond particles with the surfaces being nano-sized and metallized, and a stable porous foam diamond network structure is formed. Respectively carrying out low-temperature heat treatment and high-temperature heat treatment on the obtained gel, and reinforcing a multi-cavity foam structure by the low-temperature heat treatment (keeping the temperature at 100 ℃ for 30min and increasing the temperature at a speed of 10 ℃/min) to form a compact three-dimensional network structure assembled by diamond microwires and diamond particles; and (4) performing high-temperature heat treatment (keeping the temperature at 600 ℃ for 1h, and increasing the temperature at a speed of 10 ℃/min), removing the long chain of curdlan to obtain a three-dimensional porous network structure preform consisting of diamond nanowires and diamond particles, and keeping the temperature at 600 ℃ for later use.
(5) Putting Al (purity 99.99%) blocks into a graphite mold, heating to molten liquid aluminum, and adding La-Ce rare earth chloride solution (LaCl) 3 ：CeCl 3 In a molar ratio of 1: 1) Ultrasonic stirring is carried out for 5-6 s, and the temperature in the furnace is kept at 700 ℃ for 30 min. Pouring molten liquid rare earth aluminum alloy into a prefabricated body grinding tool with a three-dimensional porous network structure by adopting a gas pressure infiltration method, quickly applying pressure of 10MPa by using high-purity nitrogen with the purity of 99.99 percent, keeping for 20min, returning to a lifting platform after infiltration, closing a heating power supply, and quickly cooling a sample in a furnace under a high-temperature atmosphere to obtain the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material.
(6) And (3) carrying out cold rolling treatment on the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material after aging treatment. And (3) carrying out cold rolling treatment, and carrying out ultrasonic cleaning on the surface of the Ti-Ag-diamond/rare earth aluminum alloy composite material test block for 10min by using acetone, ethanol and deionized water in sequence. And (3) putting the Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block into a box type resistance furnace with the temperature of 600 ℃ for heat preservation for 15min, taking out and cooling to room temperature by water. And (3) carrying out cold rolling treatment on the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material test block subjected to the solution treatment at room temperature, and finally rolling the plate to be 5mm by adopting a phi 140/260 two-roller reversible temperature rolling mill in a cold rolling test. And then heating the box-type resistance furnace to 610 ℃, then keeping the temperature of the Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block with the thickness of 5mm for 25min, quickly taking out the test block, and air-cooling the test block to room temperature to obtain the die-casting diamond/rare earth aluminum alloy composite material with the characteristics of high heat conductivity, high strength and high toughness, wherein the pattern size of the die-casting diamond/rare earth aluminum alloy composite material is 120mm multiplied by 60mm multiplied by 5mm.
Example 4
(1) And (2) taking 100g of one-dimensional diamond micron line and diamond particles (the weight ratio is 3:1) for washing (acetone, ethanol and finally deionized water are used for washing and ultrasonic treatment is carried out for 10 min), then putting the washed diamond sample into ethanol, stirring at low temperature until the ethanol is completely evaporated, and drying in an oven at 60 ℃ for 10h to obtain powder for later use.
(2) And (3) putting 50g of the sample treated by the powder in the step (1) into a sample chamber, and depositing nano Ti on the surface of the diamond sample on a magnetron sputtering ion plating machine, wherein the thickness of the nano Ti is 80nm. The deposition process comprises the following steps: 99.99 percent of nano Ti is taken as a target material, and the background vacuum is 4.0-4.6 multiplied by 10 -3 Pa, working gas argon (99.999%), working pressure 0.2-0.3 Pa, sputtering power 4-5 kW, and sputtering time 100-120 s. In order to make the plating layers of all crystal faces of the diamond uniform, an oscillating and stirring device is designed by self to obtain a silver-white diamond sample. And (3) carrying out low-temperature heat treatment on the diamond with the Ti sprayed on the surface, wherein the heating rate is 5 ℃/min, the heat preservation is carried out for 1h at the temperature of 300 ℃, and the diamond is naturally cooled to the room temperature to obtain the Ti-diamond sample with the nano-sized surface.
(3) And then, metalizing the surface of the Ti-diamond sample in the step (2) by adopting a method in the step (2), plating a 130nm silver coating on the surface of the Ti-diamond sample to improve the heat conductivity of the Ti-diamond sample, and plating a 90nm aluminum coating to ensure good bonding strength with an aluminum alloy matrix to prepare the Ti-Ag-Al-diamond.
(4) Adding 50g of Ti-Ag-Al-diamond in (3) into curdlan glue solution (NaCl is added into 100mL of deionized water to prepare an alkaline solution with pH =8, then adding the curdlan into the alkaline solution, and preparing the curdlan into the glue solution by shearing or colloid milling until the curdlan is completely dissolved), ultrasonically adding the curdlan at the room temperature of 25 ℃, electrically stirring for 1h, and then continuously and violently stirring for 60min to form a uniform colloidal solution. And then slowly stirring and heating to 60 ℃, continuously stirring for 30min, then violently stirring and slowly heating to 100 ℃, slowly fermenting to form uniform bubbles at most, and continuously stirring for 15min to improve the gel strength, so that the surface nano and metallized one-dimensional diamond microwires and diamond particles are tightly wrapped by macromolecular chains to form a stable porous foam diamond network structure. Respectively carrying out low-temperature heat treatment and high-temperature heat treatment on the obtained gel, and reinforcing a porous foam structure by low-temperature heat treatment (keeping the temperature at 100 ℃ for 30min and increasing the temperature at a speed of 10 ℃/min) to form a compact three-dimensional network structure assembled by diamond microwires and diamond particles; performing high-temperature heat treatment (keeping the temperature at 600 ℃ for 1h, and increasing the temperature at the speed of 10 ℃/min), removing the long chains of curdlan to obtain a three-dimensional porous network structure preform consisting of diamond microwires and diamond particles, and keeping the temperature at 600 ℃ for later use.
(5) Putting Al (purity 99.99%) blocks into a graphite mold, heating to molten liquid aluminum, and adding La-Ce rare earth chloride solution (LaCl) 3 ：CeCl 3 In a molar ratio of 1: 1) Ultrasonic stirring is carried out for 5-6 s, and the temperature in the furnace is kept at 700 ℃ for 30 min. Pouring molten liquid rare earth aluminum alloy into a prefabricated body grinding tool with a three-dimensional porous network structure by adopting a gas pressure infiltration method, quickly applying pressure of 10MPa by using high-purity nitrogen with the purity of 99.99 percent, keeping for 20min, returning to a lifting platform after infiltration, closing a heating power supply, and quickly cooling a sample in a furnace under a high-temperature atmosphere to obtain the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material.
(6) And (3) carrying out cold rolling treatment on the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material after aging treatment. And before cold rolling treatment, the surface of the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material test block is sequentially cleaned by acetone, ethanol and deionized water for 10min in an ultrasonic mode. And (3) putting the Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block into a box-type resistance furnace with the temperature of 600 ℃ for heat preservation for 15min, taking out and cooling to room temperature by water. And (2) carrying out cold rolling treatment on the Ti-Ag-diamond/rare earth aluminum alloy composite material test block subjected to the solution treatment at room temperature, wherein a phi 140/260 two-roller reversible temperature rolling mill is adopted in a cold rolling test, the rolling reduction of each pass is 1mm, the plate thickness is finally rolled to be 4mm, and the total rolling reduction is 20%. Heating a box-type resistance furnace to 610 ℃, then putting a 20% cold-deformed Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block, preserving the heat for 25min, quickly taking out the test block and cooling the test block to room temperature in air, thus obtaining the die-cast diamond/rare earth aluminum alloy composite material with high heat conductivity, high strength and high toughness, wherein the pattern size of the die-cast diamond/rare earth aluminum alloy composite material is 120mm multiplied by 60mm multiplied by 4mm.
Example 5
(1) And (2) taking 100g of one-dimensional diamond micron line and diamond particles (the weight ratio is 3:1) to wash (acetone, ethanol and finally deionized water are used for washing and ultrasonic processing for 10 min), then putting the washed diamond sample into ethanol, stirring at a low temperature until the ethanol is completely evaporated, and drying in an oven at a temperature of 60 ℃ for 10h to obtain powder for later use.
(2) And (3) putting 50g of the sample treated by the powder in the step (1) into a sample chamber, and depositing nano Ti on the surface of the diamond sample on a magnetron sputtering ion plating machine, wherein the thickness of the nano Ti is 80nm. The deposition process comprises the following steps: 99.99 percent of nano Ti is taken as a target material, and the background vacuum is 4.0-4.6 multiplied by 10 -3 Pa, working gas argon (99.999%), working pressure 0.2-0.3 Pa, sputtering power 4-5 kW, and sputtering time 100-120 s. In order to make the plating layers of all crystal faces of the diamond uniform, an oscillating and stirring device is designed by self to obtain a silver-white diamond sample. And (3) carrying out low-temperature heat treatment on the diamond with the Ti sprayed on the surface, wherein the heating rate is 5 ℃/min, the heat preservation is carried out for 1h at the temperature of 300 ℃, and the diamond is naturally cooled to the room temperature to obtain the Ti-diamond sample with the nano-sized surface.
(3) And then, metalizing the surface of the Ti-diamond sample in the step (2) by adopting a method in the step (2), plating a 130nm silver coating on the surface of the Ti-diamond sample to improve the heat conductivity of the Ti-diamond sample, and plating a 90nm aluminum coating to ensure good bonding strength with an aluminum alloy matrix to prepare the Ti-Ag-Al-diamond.
(4) Adding 50g of Ti-Ag-Al-diamond in (3) into curdlan glue solution (NaCl is added into 100mL of deionized water to prepare an alkaline solution with pH =8, then adding the curdlan into the alkaline solution, and preparing the curdlan into the glue solution by shearing or colloid milling until the curdlan is completely dissolved), ultrasonically adding the curdlan at the room temperature of 25 ℃, electrically stirring for 1h, and then continuously and violently stirring for 60min to form a uniform colloidal solution. Then slowly stirring and heating to 60 ℃, continuously stirring for 30min, then violently stirring and slowly heating to 100 ℃, slowly fermenting to form uniform bubbles, and continuously stirring for 15min to improve the gel strength, so that the macromolecular chains tightly wrap the one-dimensional diamond microwires and diamond particles with the surfaces being nano-sized and metallized, and a stable porous foam diamond network structure is formed. Respectively carrying out low-temperature heat treatment and high-temperature heat treatment on the obtained gel, and reinforcing a multi-cavity foam structure by the low-temperature heat treatment (keeping the temperature at 100 ℃ for 30min and increasing the temperature at a speed of 10 ℃/min) to form a compact three-dimensional network structure assembled by diamond microwires and diamond particles; performing high-temperature heat treatment (keeping the temperature at 600 ℃ for 1h, and increasing the temperature at the speed of 10 ℃/min), removing the long chains of curdlan to obtain a three-dimensional porous network structure preform consisting of diamond microwires and diamond particles, and keeping the temperature at 600 ℃ for later use.
(5) Putting Al (purity 99.99%) blocks into a graphite mould, heating to molten liquid aluminum, and adding La-Ce rare earth chloride solution (LaCl) 3 ：CeCl 3 In a molar ratio of 1: 1) Ultrasonic stirring is carried out for 5-6 s, and the temperature in the furnace is kept at 700 ℃ for 30 min. Pouring molten liquid rare earth aluminum alloy into a prefabricated body grinding tool with a three-dimensional porous network structure by adopting a gas pressure infiltration method, quickly applying pressure of 10MPa by using high-purity nitrogen with the purity of 99.99 percent, keeping for 20min, returning to a lifting platform after infiltration, closing a heating power supply, and quickly cooling a sample in a furnace under a high-temperature atmosphere to obtain the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material.
(6) And carrying out cold rolling treatment on the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material after aging treatment. And (3) before cold rolling treatment, the surface of the Ti-Ag-diamond/rare earth aluminum alloy composite material test block is subjected to ultrasonic cleaning for 10min by using acetone, ethanol and deionized water in sequence. And (3) putting the Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block into a box type resistance furnace with the temperature of 600 ℃ for heat preservation for 15min, taking out and cooling to room temperature by water. And (3) carrying out cold rolling treatment on the Ti-Ag-diamond/rare earth aluminum alloy composite material test block subjected to solution treatment at room temperature, wherein in a cold rolling test, a phi 140-260 two-roller reversible temperature rolling mill is adopted, the rolling reduction of each pass is 2mm, the plate thickness is finally rolled to be 3mm, and the total rolling reduction is 40%. Heating a box-type resistance furnace to 610 ℃, then putting a 40% cold-deformed Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block, preserving the heat for 25min, quickly taking out the test block and cooling the test block to room temperature in air, thus obtaining the die-cast diamond/rare earth aluminum alloy composite material with high heat conductivity, high strength and high toughness, wherein the pattern size of the die-cast diamond/rare earth aluminum alloy composite material is 120mm multiplied by 60mm multiplied by 3mm.
Example 6
(1) And (2) taking 100g of one-dimensional diamond micron line and diamond particles (the weight ratio is 3:1) to wash (acetone, ethanol and finally deionized water are used for washing and ultrasonic processing for 10 min), then putting the washed diamond sample into ethanol, stirring at a low temperature until the ethanol is completely evaporated, and drying in an oven at a temperature of 60 ℃ for 10h to obtain powder for later use.
(2) 50g of the sample treated with the powder in (1) was placed in a sample chamber and subjected to magnetic controlAnd (4) depositing the nano Ti on the surface of the diamond sample on a sputtering ion coating machine, wherein the thickness of the nano Ti is 80nm. The deposition process comprises the following steps: 99.99 percent of nano Ti is taken as a target material, and the background vacuum is 4.0-4.6 multiplied by 10 -3 Pa, working gas argon (99.999%), working pressure 0.2-0.3 Pa, sputtering power 4-5 kW, and sputtering time 100-120 s. In order to make the plating layers of all crystal faces of the diamond uniform, an oscillating and stirring device is designed by self to obtain a silvery white diamond sample. And carrying out low-temperature heat treatment on the diamond with the Ti sprayed on the surface, wherein the heating speed is 5 ℃/min, the heat preservation is carried out for 1h at the temperature of 300 ℃, and naturally cooling to the room temperature to obtain the Ti-diamond sample with the nano-sized surface.
(3) And then, metalizing the surface of the Ti-diamond sample in the step (2) by adopting a method in the step (2), plating a 130nm silver coating on the surface of the Ti-diamond sample to improve the heat conductivity of the Ti-diamond sample, and plating a 90nm aluminum coating to ensure good bonding strength with an aluminum alloy matrix to prepare the Ti-Ag-Al-diamond.
(4) Adding 50g of Ti-Ag-Al-diamond in (3) into curdlan glue solution (NaCl is added into 100mL of deionized water to prepare an alkaline solution with pH =8, then adding the curdlan into the alkaline solution, and preparing the curdlan into the glue solution by shearing or colloid milling until the curdlan is completely dissolved), ultrasonically adding the curdlan at the room temperature of 25 ℃, electrically stirring for 1h, and then continuously and violently stirring for 60min to form a uniform colloidal solution. Then slowly stirring and heating to 60 ℃, continuously stirring for 30min, then violently stirring and slowly heating to 100 ℃, slowly fermenting to form uniform bubbles, and continuously stirring for 15min to improve the gel strength, so that the macromolecular chains tightly wrap the one-dimensional diamond microwires and diamond particles with the surfaces being nano-sized and metallized, and a stable porous foam diamond network structure is formed. Respectively carrying out low-temperature heat treatment and high-temperature heat treatment on the obtained gel, and reinforcing a multi-cavity foam structure by the low-temperature heat treatment (keeping the temperature at 100 ℃ for 30min and increasing the temperature at a speed of 10 ℃/min) to form a compact three-dimensional network structure assembled by diamond microwires and diamond particles; performing high-temperature heat treatment (keeping the temperature at 600 ℃ for 1h, and increasing the temperature at a speed of 10 ℃/min), removing the long chain of curdlan to obtain a three-dimensional porous network structure preform consisting of diamond microwires and diamond particles, and keeping the temperature at 600 ℃ for later use.
(5) Mixing Al (purity 99.99%) blocksHeating in graphite mold to molten liquid aluminum, adding La-Ce rare earth chloride solution (LaCl) 3 ：CeCl 3 In a molar ratio of 1: 1) Ultrasonic stirring is carried out for 5-6 s, and the temperature in the furnace is kept at 700 ℃ for 30 min. Pouring molten liquid rare earth aluminum alloy into a prefabricated body grinding tool with a three-dimensional porous network structure by adopting a gas pressure infiltration method, quickly applying pressure of 10MPa by using high-purity nitrogen with the purity of 99.99 percent, keeping for 20min, returning to a lifting platform after infiltration, closing a heating power supply, and quickly cooling a sample in a furnace under a high-temperature atmosphere to obtain the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material.
(6) And (3) carrying out cold rolling treatment on the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material after aging treatment. And (3) before cold rolling treatment, the surface of the Ti-Ag-diamond/rare earth aluminum alloy composite material test block is subjected to ultrasonic cleaning for 10min by using acetone, ethanol and deionized water in sequence. And (3) putting the Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block into a box type resistance furnace with the temperature of 600 ℃ for heat preservation for 15min, taking out and cooling to room temperature by water. And (3) carrying out cold rolling treatment on the Ti-Ag-diamond/rare earth aluminum alloy composite material test block subjected to solution treatment at room temperature, wherein in a cold rolling test, a phi 140-260 two-roller reversible temperature rolling mill is adopted, the rolling reduction is 3mm, the plate thickness is finally rolled to be 2mm, and the total rolling reduction is 60%. Heating a box-type resistance furnace to 610 ℃, then putting a 60% cold-deformed Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block, preserving the heat for 25min, quickly taking out the test block and cooling the test block to room temperature in air, thus obtaining the die-cast diamond/rare earth aluminum alloy composite material with high heat conductivity, high strength and high toughness, wherein the pattern size of the die-cast diamond/rare earth aluminum alloy composite material is 120mm multiplied by 60mm multiplied by 2mm.
Example 7
(1) And (2) taking 100g of one-dimensional diamond micron line and diamond particles (the weight ratio is 3:1) for washing (acetone, ethanol and finally deionized water are used for washing and ultrasonic treatment is carried out for 10 min), then putting the washed diamond sample into ethanol, stirring at low temperature until the ethanol is completely evaporated, and drying in an oven at 60 ℃ for 10h to obtain powder for later use.
(2) And (3) putting 50g of the sample treated by the powder in the step (1) into a sample chamber, and depositing nano Ti on the surface of the diamond sample on a magnetron sputtering ion plating machine, wherein the thickness of the nano Ti is 80nm. The deposition process comprises the following steps: at 99.99% of nano Ti is used as target material, the background vacuum is 4.0-4.6 x 10 -3 Pa, working gas argon (99.999%), working pressure 0.2-0.3 Pa, sputtering power 4-5 kW, and sputtering time 100-120 s. In order to make the plating layers of all crystal faces of the diamond uniform, an oscillating and stirring device is designed by self to obtain a silvery white diamond sample. And (3) carrying out low-temperature heat treatment on the diamond with the Ti sprayed on the surface, wherein the heating rate is 5 ℃/min, the heat preservation is carried out for 1h at the temperature of 300 ℃, and the diamond is naturally cooled to the room temperature to obtain the Ti-diamond sample with the nano-sized surface.
(3) And then, metalizing the surface of the Ti-diamond sample in the step (2) by adopting a method in the step (2), plating a 130nm silver coating on the surface of the Ti-diamond sample to improve the heat conductivity of the Ti-diamond sample, and plating a 90nm aluminum coating to ensure good bonding strength with an aluminum alloy matrix to prepare the Ti-Ag-Al-diamond.
(4) Adding 50g of Ti-Ag-Al-diamond in (3) into curdlan glue solution (NaCl is added into 100mL of deionized water to prepare an alkaline solution with the pH =8, then adding the curdlan into the alkaline solution, and preparing the curdlan into the glue solution by shearing or colloid milling until the curdlan is completely dissolved), ultrasonically adding electricity at the room temperature of 25 ℃ and stirring for 1 hour, and then continuously stirring vigorously for 60min to form a uniform colloidal solution. Then slowly stirring and heating to 60 ℃, continuously stirring for 30min, then violently stirring and slowly heating to 100 ℃, slowly fermenting to form uniform bubbles, and continuously stirring for 15min to improve the gel strength, so that the macromolecular chains tightly wrap the one-dimensional diamond microwires and diamond particles with the surfaces being nano-sized and metallized, and a stable porous foam diamond network structure is formed. Respectively carrying out low-temperature heat treatment and high-temperature heat treatment on the obtained gel, and reinforcing a multi-cavity foam structure by the low-temperature heat treatment (keeping the temperature at 100 ℃ for 30min and increasing the temperature at a speed of 10 ℃/min) to form a compact three-dimensional network structure assembled by diamond microwires and diamond particles; performing high-temperature heat treatment (keeping the temperature at 600 ℃ for 1h, and increasing the temperature at a speed of 10 ℃/min), removing the long chains of curdlan to obtain a three-dimensional porous network structure preform consisting of diamond microwires and diamond particles, and keeping the temperature at 600 ℃ for later use.
(5) Putting Al (purity 99.99%) blocks into a graphite mould, heating to molten liquid aluminum, and adding La-Ce rare earth chloride solution (LaCl) 3 ：CeCl 3 In a molar ratio of 1: 1) Ultrasonic stirring is carried out for 5-6 s, and the temperature in the furnace is kept at 700 ℃ for 30 min. Pouring molten liquid rare earth aluminum alloy into a prefabricated body grinding tool with a three-dimensional porous network structure by adopting a gas pressure infiltration method, quickly applying pressure of 10MPa by using high-purity nitrogen with the concentration of 99.99 percent, keeping for 20min, returning to a lifting platform after infiltration, closing a heating power supply, and quickly cooling a sample in a furnace under a high-temperature atmosphere to obtain the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material.
(6) And (3) carrying out cold rolling treatment on the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material after aging treatment. And before cold rolling treatment, the surface of the Ti-Ag-diamond/rare earth aluminum alloy composite material test block is sequentially cleaned by acetone, ethanol and deionized water for 10min in an ultrasonic mode. And (3) putting the Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block into a box type resistance furnace with the temperature of 600 ℃ for heat preservation for 15min, taking out and cooling to room temperature by water. And (3) carrying out cold rolling treatment on the Ti-Ag-diamond/rare earth aluminum alloy composite material test block subjected to solution treatment at room temperature, wherein in a cold rolling test, a phi 140-260 two-roller reversible temperature rolling mill is adopted, the rolling reduction is 4mm, the plate thickness is finally rolled to be 1mm, and the total rolling reduction is 80%. Heating a box-type resistance furnace to 610 ℃, then putting an 80% cold-deformed Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block, preserving heat for 25min, quickly taking out and air-cooling to room temperature to obtain the die-cast diamond/rare earth aluminum alloy composite material with high heat conductivity, high strength and high toughness, wherein the pattern size of the die-cast diamond/rare earth aluminum alloy composite material is 120mm multiplied by 60mm multiplied by 1mm.
The heat conductivity coefficient in the thickness direction of the die-cast diamond/rare earth aluminum alloy composite material with high heat conductivity, high strength and high toughness prepared in the above embodiment 1-7 is measured according to ASTM D5470; the tensile strength is measured on a universal testing machine; performing fracture toughness test on a sample on an MTS810-100kN type testing machine according to HB5142-96 standard (before the test, the yield strength selection load of the 7475 aluminum alloy plate in the transverse direction (thickness direction) is referred to, prefabricating a fatigue crack of 2mm, and then calculating to obtain the plane strain fracture toughness K IC Value of (d).
The heat conductivity and mechanical properties of the die-cast diamond/rare earth aluminum alloy composite material with high heat conductivity, high strength and high toughness prepared in the above examples 1 to 7 are measured as shown in the following table 1:
Figure BDA0003792029890000161
the present invention has been described in terms of specific examples, which are provided to aid understanding of the invention and are not intended to be limiting. For a person skilled in the art to which the invention pertains, several simple deductions, modifications or substitutions may be made according to the idea of the invention.

Claims (6)

1. The preparation method of the die-cast diamond/rare earth aluminum alloy composite material is characterized by comprising the following steps:
(1) Taking a proper amount of one-dimensional diamond microwires and diamond particles for washing, putting the washed diamond sample into ethanol, stirring at a low temperature until the ethanol is completely evaporated, and drying in an oven to obtain powder after dispersion treatment; the one-dimensional diamond micron line and the diamond particles are mixed according to different weight ratios of 1:1 to 3:1, uniformly mixing 100g of the mixture; the type of the diamond particles is HHD90, the particle size is 200-300 mu m, and the particle size of the diamond micron line is 400-800 mu m;
(2) Putting a proper amount of the sample treated by the powder in the step (1) into a sample chamber, and depositing nano Ti on the surface of the diamond sample on a magnetron sputtering ion plating machine; carrying out low-temperature heat treatment on the diamond with the Ti sprayed on the surface to obtain a silvery white Ti-diamond sample with a nano-sized surface;
(3) Metallizing the surface of the Ti-diamond sample in the step (2) by adopting the method in the step (2), and plating silver and aluminum on the surface of the Ti-diamond sample to prepare a Ti-Ag-Al-diamond sample;
(4) Adding a proper amount of Ti-Ag-Al-diamond in the step (3) into the curdlan glue solution, and performing ultrasonic and electric stirring at room temperature to form a uniform colloidal solution; then slowly stirring and heating to 60 ℃, then violently stirring and slowly heating to 100 ℃, slowly fermenting to form uniform bubbles at most, continuously stirring to improve the gel strength, so that the macromolecular chains tightly wrap the one-dimensional diamond microwires and diamond particles with the nano-sized and metallized surfaces to form a stable porous foam diamond network structure, and obtaining a three-dimensional porous network structure prefabricated body consisting of the diamond nanowires and the diamond particles; respectively carrying out low-temperature heat treatment and high-temperature heat treatment on the obtained gel, and keeping the temperature at 600 ℃;
(5) Putting the Al block into a graphite mould, heating to molten liquid aluminum, adding La-Ce rare earth chloride solution, ultrasonically stirring, and keeping the temperature in the furnace; then pouring the molten liquid rare earth aluminum alloy into a prefabricated body grinding tool provided with a three-dimensional porous network structure by adopting a gas pressure infiltration method, quickly applying pressure of 10MPa by using high-purity nitrogen, keeping for a proper time, returning to a lifting platform after infiltration, turning off a heating power supply, and quickly cooling a sample in a furnace under a high-temperature atmosphere to obtain the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material;
before cold rolling treatment, the surface of the Ti-Ag-diamond/rare earth aluminum alloy composite material test block is sequentially cleaned by acetone, ethanol and deionized water for 10min in an ultrasonic mode;
the solution treatment comprises the following steps: putting the Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block into a box type resistance furnace with the temperature of 600 ℃ for heat preservation for 10-25 min, taking out and cooling to room temperature by water;
the cold rolling treatment comprises the following steps: in the cold rolling test, a phi 140-260 two-roller reversible temperature rolling mill is adopted, the rolling reduction of each pass is 0-4 mm and does not contain 0mm, the plate is finally rolled to be 1-5 mm, and the total rolling reduction is 20-80%; heating a box-type resistance furnace to 610 ℃, then putting the Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block with 20-80% of cold deformation into the box-type resistance furnace, preserving the heat for 10-30 min, and quickly taking out the box-type resistance furnace and cooling the box-type resistance furnace to room temperature;
(6) Carrying out cold rolling treatment on the Ti-Ag-Al-diamond/rare earth aluminum alloy composite material after aging treatment; before cold rolling treatment, ultrasonically cleaning the surface of a Ti-Ag-diamond/rare earth aluminum alloy composite material test block; and then carrying out solid solution treatment and cold rolling treatment on the Ti-Ag-Al-diamond/rare earth aluminum alloy composite test block at room temperature to obtain the die-cast diamond/rare earth aluminum alloy composite material.
2. As claimed in claimThe preparation method according to claim 1, wherein in the step (2), the deposition process comprises: 99.99 percent of nano Ti is taken as a target material, and the background vacuum is 4.0-4.6 multiplied by 10 -3 Pa,99.999 percent of working gas argon, 0.2-0.3 Pa of working pressure, 4-5 kW of sputtering power and 100-360 s of sputtering time; in order to make each crystal face plating layer of the diamond uniform, an oscillating and stirring device is designed automatically to obtain a silvery white diamond sample; low-temperature heat treatment: the temperature rise speed is 5 ℃/min, the temperature is kept at 300 ℃ for 1h, and the mixture is naturally cooled to room temperature with the thickness of 80nm.
3. The manufacturing method of claim 1, wherein in the step (3), the silver plating layer has a thickness of 130nm in order to improve thermal conductivity thereof, and the aluminum plating layer has a thickness of 90nm in order to ensure good bonding strength with the aluminum alloy substrate.
4. The preparation method according to claim 1, wherein in the step (4), the curdlan glue solution is prepared by: adding NaCl into 100mL of deionized water to prepare an alkaline solution with the pH =8, then adding curdlan into the alkaline solution, and preparing a glue solution by shearing or colloid milling until the curdlan is completely dissolved; low-temperature heat treatment: keeping the temperature at 100 ℃ for 30min, and increasing the temperature at the speed of 10 ℃/min, and reinforcing a porous foam structure to form a compact three-dimensional network structure assembled by diamond nanowires and diamond particles; high-temperature heat treatment: keeping the temperature at 600 ℃ for 1h, and removing the long chain of curdlan at the heating rate of 10 ℃/min.
5. The method according to claim 1, wherein in the step (5), the Al mass has a purity of 99.99%; laC in La-Ce rare earth chloride solution l3 And CeC l3 In a molar ratio of 1:1.
6. a die-cast diamond/rare earth aluminum alloy composite material obtained by the production method according to any one of claims 1 to 5.
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