CN113462924A - Titanium-plated diamond copper composite material and preparation method thereof - Google Patents
Titanium-plated diamond copper composite material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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Abstract
The invention discloses a titanium-plated diamond copper composite material and a preparation method thereof. The formula of the titanium-plated diamond copper composite material comprises the following components: the copper powder and the titanium-plated diamond powder comprise the following components in parts by weight: 97.97-98.8 parts of copper powder and 1.2-2.03 parts of titanized diamond powder, the invention plates a titanium layer on the surface of diamond particles by a vacuum evaporation coating method, and carries out vacuum hot-pressing sintering on the copper powder and the titanized diamond powder to prepare titanized diamond copper alloy, the prepared titanized diamond copper alloy block is crushed, the crushed titanized diamond copper alloy granules are ball-milled, the dried and cooled titanized diamond copper alloy powder is used for producing titanized diamond copper composite material by an SLM process, and the metal powder laid by the micro laser spot melting coating layer is used for molding, thus realizing high-precision characteristic and high-complexity near-net molding.
Description
Technical Field
The invention relates to the technical field of metal matrix composite materials, in particular to a titanium-plated diamond copper composite material and a preparation method thereof.
Background
Diamond particle reinforced metal matrix composites are receiving increasing attention. However, the wettability between diamond and copper is poor, the interface bonding is weak, and the interface thermal resistance increases. There are generally two solutions to the above problem. One method is matrix alloying, i.e. introducing alloy elements such as Ti, B, Zr and Cr into the copper matrix. However, the addition amount of the alloying element is difficult to be accurately controlled, which may cause excessive amount of the element to remain in the matrix, thereby lowering the thermal conductivity of the matrix. The other is diamond surface modification, and strong carbide forming elements such as Ti, Cr, W and Mo are introduced on the surface of diamond particles. These four metal layers are not only strong carbide formers, which react with diamond, but also partially dissolve in the copper matrix. Because carbide has both a high thermal conductivity and a suitable thermal expansion coefficient. Thus, two carbides having the above properties were selected: TiC and WC. Because the free energy of formation of TiC is low, carbide is easily formed in a short time to form chemical bonding with diamond. Thus selecting a metallic titanium plating. The formed interface layer is used as a bridge for connecting copper and diamond, so that the thermal conductivity of the composite material is improved.
At present, the titanium-plated diamond copper composite material is produced in the market mostly in a Spark Plasma Sintering (SPS) mode, the production efficiency is low, the porosity of the produced material is high, the mechanical property is poor, micropores and channels in the material are difficult to produce, the quality of the product is reduced, meanwhile, the graphitization of diamond is easy to occur in the production process, and the performance of the product is greatly reduced. The titanium-plated diamond copper composite material produced by the SPS mode is cylindrical, a thermal performance test required in the later period needs to cut the cylindrical body into the size and the thickness specified by the thermal test, but diamonds with slightly larger grain sizes are difficult to cut, and the performance of diamonds with small grain sizes is poorer, so that the titanium-plated diamond copper composite material produced by the SPS mode is limited.
Disclosure of Invention
The invention aims to provide a titanium-plated diamond copper composite material and a preparation process thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
the raw materials of the titanium-plated diamond copper composite material comprise 97.97-98.8 parts by mass of copper powder and 1.2-2.03 parts by mass of titanium-plated diamond powder.
Furthermore, the copper powder is electrolytic copper powder with the purity of 99.6-99.8%.
Furthermore, the particle size of the titanium-plated diamond powder is 20-25 μm, and the thickness of the titanium-plated layer is between 140 nm and 250 nm.
A preparation method of the titanium-plated diamond copper composite material comprises the following steps:
the method comprises the following steps: weighing a certain mass part of copper powder and titanium-plated diamond powder;
step two: putting the mixture into a ball mill for ball milling, protecting the mixture by using nitrogen in the ball milling process, and preparing mixed alloy powder with the particle size of 20-25 mu m for later use after ball milling;
step three: putting the mixed alloy powder obtained after ball milling into a tungsten carbide mould for vacuum hot-pressing sintering, and cooling after sintering to obtain a titanium-plated diamond copper alloy block for later use;
step four: crushing the titanium-plated diamond copper alloy block prepared in the third step into small particles of 5-10 mm;
step five: carrying out ball milling on the titanium-plated diamond copper alloy granules obtained by crushing in the fourth step by using a ball mill, and filling nitrogen for protection during ball milling to obtain titanium-plated diamond copper alloy powder which is 25 microns and is uniformly mixed for later use;
step six: screening the titanium-plated diamond copper alloy powder prepared in the fifth step by using a 400-mesh vibrating screen, leaving fine and uniform titanium-plated diamond copper alloy powder, and then drying and cooling the screened titanium-plated diamond copper alloy powder and taking out the titanium-plated diamond copper alloy powder for later use;
step seven: and taking the titanium-plated diamond copper alloy powder dried and cooled in the sixth step, and then carrying out laser printing by using an SLM 3D printer under the protection of high-purity nitrogen to print the titanium-plated diamond copper alloy powder to prepare the titanium-plated diamond copper composite material with high density and low porosity.
Further, the method comprisesIn the third step, the process conditions of the vacuum hot-pressing sintering are as follows: the vacuum degree in the furnace is 1 multiplied by 10-3-2×10-3kPa, the hot-pressing pressure is 75-85MPa, the sintering temperature is 880-910 ℃, and the time is 55-65 min.
Further, in the sixth step, the drying temperature is 55-65 ℃, and the drying time is 240 min.
Further, in the seventh step, the concentration of the nitrogen is between 99.5 and 99.9 percent.
Further, in the seventh step, the laser power is 140-.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the copper powder and the titanized diamond powder are subjected to vacuum hot-pressing sintering to prepare the titanized diamond copper alloy, the sintering density and the tensile strength of the titanized diamond copper alloy block are greatly improved under the sintering process condition, the titanized layer is favorable for enhancing the wettability between copper and diamond, the porosity of the material is reduced by 10-20%, and the heat conductivity of the product is enhanced by 5-10%;
2. according to the invention, the SLM process is used for replacing the traditional process to produce the titanium-plated diamond copper composite material, the metal powder laid on the micro laser spot melting layer is used for forming, high-precision characteristics and high-complexity near-net forming can be realized, and no adhesive is needed to directly make a complex shape, so that the production cost is reduced, the production efficiency is improved, and the product density is high; the SLM has the advantages over the SPS that the laser has fine light spots after being focused, high power density is easy to obtain, and metal parts with higher dimensional accuracy (up to 0.1mm) and good surface roughness can be processed; the formed part has the structural characteristic of metallurgical bonding, the relative density can reach nearly 100%, and the mechanical property can be compared with that of a casting and forging piece; after a model is built by three-dimensional software, dimensions and complex structures (including porous structures capable of improving heat dissipation effect) specified by performance test are directly printed and integrally formed, and the complex structures cannot be manufactured by a traditional method (including SPS); the capability of creating complex design by the SLM is combined with the excellent performance of the metal matrix composite material, so that the performance of the diamond/copper composite material can be fully exerted, and the application of the diamond/copper composite material is remolded;
3. in the invention, nitrogen is introduced for protection in the process of multiple ball milling mixing and molding, thereby avoiding the graphitization of diamond and the oxidation of copper at high temperature and being beneficial to improving the quality of products.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, a technical solution provided by the present invention:
example 1:
the titanium-plated diamond copper composite material comprises the following components in percentage by weight: the copper powder and the titanium-plated diamond powder comprise the following components in parts by weight: 98.8 parts of copper powder and 1.2 parts of titanized diamond powder, wherein the copper powder is electrolytic copper powder with the purity of 99.8 percent, the grain diameter of the titanized diamond powder is 25 mu m, and the thickness of the titanized layer is 200 nm.
The preparation process of the titanium-plated diamond copper composite material comprises the following steps of firstly, weighing raw materials; step two, primary ball milling and mixing; step three, preparing an alloy; step four, crushing and pulverizing; step five, performing secondary ball milling and mixing; step six, screening and drying; step seven, laser forming;
in the first step, 98.8 parts of copper powder and 1.2 parts of titanizing diamond powder are respectively weighed according to the weight parts of the components;
in the second step, the copper powder and the titanium-plated diamond powder weighed in the first step are taken and put into a ball mill for ball milling at the same time, the ball milling time is 5 hours, nitrogen is used for protection in the ball milling process, and mixed alloy powder with the particle size of 25 microns is prepared for standby after ball milling;
in the third step, the mixed alloy powder obtained after ball milling in the second step is put into a tungsten carbide mould for vacuum hot-pressing sintering, and the process conditions of the vacuum hot-pressing sintering are as follows: the vacuum degree in the furnace is 1 multiplied by 10-3kPa, the hot-pressing pressure is 85MPa, the sintering temperature is 900 ℃, the time is 65min, after sintering is completed and cooling is performed, the titanium-plated diamond copper alloy block is obtained for standby, and the sintering density and the tensile strength of the titanium-plated diamond copper alloy block under the sintering process condition are both greatly improved;
in the fourth step, the titanium-plated diamond copper alloy block prepared in the third step is put into a metal crusher to be crushed, and small particles with the particle size of 10mm are obtained through crushing;
in the fifth step, the titanium-plated diamond copper alloy particles obtained by crushing in the fourth step are subjected to ball milling crushing by using a ball mill, nitrogen is filled for protection during ball milling, the ball milling time is 7 hours, unidirectional ball milling and mixing are carried out for 30min, then reverse ball milling and mixing are carried out for 30min, circulation is carried out for 7 times, and titanium-plated diamond copper alloy powder with 25 microns and uniform mixing is obtained after the ball milling is finished for later use;
screening the titanium-plated diamond copper alloy powder prepared in the fifth step by using a 400-mesh vibrating screen to leave fine and uniform titanium-plated diamond copper alloy powder, then drying the screened titanium-plated diamond copper alloy powder by using a dryer, wherein the temperature of the dryer is 60 ℃, the drying time is 120min, and taking out the titanium-plated diamond copper alloy powder for later use after drying and cooling;
and in the seventh step, the titanium-plated diamond copper alloy powder dried and cooled in the sixth step is taken, the titanium-plated diamond copper alloy powder is uniform in production standard, uniform in particle size and high in wettability, and is uniform and smooth in printing, laser printing is performed by using an SLM 3D printer under the protection of high-purity nitrogen, the concentration of the nitrogen is 99.8%, the laser power is 160W, the scanning speed is 200mm/s, the powder laying thickness is 0.025mm, and the titanium-plated diamond copper composite material is manufactured through printing and molding.
Example 2:
the titanium-plated diamond copper composite material comprises the following components in percentage by weight: the copper powder and the titanium-plated diamond powder comprise the following components in parts by weight: 97.97 parts of copper powder and 2.03 parts of titanized diamond powder, wherein the copper powder is electrolytic copper powder with the purity of 99.8 percent, the particle size of the titanized diamond powder is 25 mu m, and the thickness of the titanized layer is 200 nm.
The preparation process of the titanium-plated diamond copper composite material comprises the following steps of firstly, weighing raw materials; step two, primary ball milling and mixing; step three, preparing an alloy; step four, crushing and pulverizing; step five, performing secondary ball milling and mixing; step six, screening and drying; step seven, laser forming;
in the first step, 97.97 parts of copper powder and 2.03 parts of titanizing diamond powder are weighed according to the parts by weight of the components;
in the second step, the copper powder and the titanium-plated diamond powder weighed in the first step are taken and put into a ball mill for ball milling at the same time, the ball milling time is 5 hours, nitrogen is used for protection in the ball milling process, and mixed alloy powder with the particle size of 25 microns is prepared for standby after ball milling;
in the third step, the mixed alloy powder obtained after ball milling in the second step is put into a tungsten carbide mould for vacuum hot-pressing sintering, and the process conditions of the vacuum hot-pressing sintering are as follows: the vacuum degree in the furnace is 1 multiplied by 10-3kPa, the hot-pressing pressure is 85MPa, the sintering temperature is 900 ℃, the time is 65min, after sintering is completed and cooling is performed, the titanium-plated diamond copper alloy block is obtained for standby, and the sintering density and the tensile strength of the titanium-plated diamond copper alloy block under the sintering process condition are both greatly improved;
in the fourth step, the titanium-plated diamond copper alloy block prepared in the third step is put into a metal crusher to be crushed, and small particles with the particle size of 10mm are obtained through crushing;
in the fifth step, the titanium-plated diamond copper alloy particles obtained by crushing in the fourth step are subjected to ball milling crushing by using a ball mill, nitrogen is filled for protection during ball milling, the ball milling time is 7 hours, unidirectional ball milling and mixing are carried out for 30min, then reverse ball milling and mixing are carried out for 30min, circulation is carried out for 7 times, and titanium-plated diamond copper alloy powder with 25 microns and uniform mixing is obtained after the ball milling is finished for later use;
screening the titanium-plated diamond copper alloy powder prepared in the fifth step by using a 400-mesh vibrating screen to leave fine and uniform titanium-plated diamond copper alloy powder, then drying the screened titanium-plated diamond copper alloy powder by using a dryer, wherein the temperature of the dryer is 60 ℃, the drying time is 120min, and taking out the titanium-plated diamond copper alloy powder for later use after drying and cooling;
and in the seventh step, the titanium-plated diamond copper alloy powder dried and cooled in the sixth step is taken, the titanium-plated diamond copper alloy powder is uniform in production standard, uniform in particle size and high in wettability, and is uniform and smooth in printing, laser printing is performed by using an SLM 3D printer under the protection of high-purity nitrogen, the concentration of the nitrogen is 99.8%, the laser power is 160W, the scanning speed is 200mm/s, the powder laying thickness is 0.025mm, and the titanium-plated diamond copper composite material with high density and low porosity is manufactured by printing.
The properties of the above examples are compared and the results are given in the following table:
based on the above, the invention coats the surface of diamond particles with a titanium layer by a vacuum evaporation coating method, and carries out vacuum hot-pressing sintering on copper powder and titanium-plated diamond powder to prepare titanium-plated diamond copper alloy, the prepared titanium-plated diamond copper alloy block is put into a metal crusher to be crushed, the crushed titanium-plated diamond copper alloy granules are ball-milled by a ball mill, the dried and cooled titanium-plated diamond copper alloy powder is used for producing a titanium-plated diamond copper composite material by using an SLM (selective laser melting) process instead of the traditional process, and the metal powder laid on the micro laser spot melting layer is used for molding, so that high-precision characteristic and high-complexity near-net shape can be realized, direct molding is realized, secondary processing is not required, and the production efficiency is greatly improved. The titanium plating layer is beneficial to enhancing the wettability between copper and diamond, the density is measured by the Archimedes principle, the density is calculated by dividing the density by the theoretical density, the porosity is obtained by subtracting the density from 1, and the porosity of the product is reduced by 10-20%. The thermal diffusivity of a sample is directly measured by using a laser thermal conductivity meter and a laser flash method, the specific heat C and the density rho of the material are measured firstly, and then the thermal conductivity lambda of the material can be calculated by measuring the thermal diffusivity alpha: the heat conducting performance of the product is enhanced by 5-10%. Meanwhile, in the production process, nitrogen is used as protective gas for protecting the raw materials for many times, thereby avoiding the graphitization of diamond and the oxidation of copper at high temperature, reducing the content of impurities in the product and being beneficial to ensuring the quality of the product.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (8)
1. A titanium-plated diamond copper composite material is characterized in that: the raw materials of the titanium-plated diamond copper composite material comprise 97.97-98.8 parts of copper powder and 1.2-2.03 parts of titanium-plated diamond powder in parts by weight.
2. The titanium-plated diamond copper composite material according to claim 1, wherein: the copper powder is electrolytic copper powder with the purity of 99.6-99.8%.
3. The titanium-plated diamond copper composite material according to claim 1, wherein: the grain diameter of the titanium-plated diamond powder is 20-25 μm, and the thickness of the titanium-plated layer is between 140 nm and 250 nm.
4. A method of preparing the titanium-plated diamond copper composite material according to any one of claims 1 to 3, characterized by: the method comprises the following steps:
the method comprises the following steps: weighing a certain mass part of copper powder and titanium-plated diamond powder;
step two: putting the mixture into a ball mill for ball milling, protecting the mixture by using nitrogen in the ball milling process, and preparing mixed alloy powder with the particle size of 20-25 mu m for later use after ball milling;
step three: putting the mixed alloy powder obtained after ball milling into a tungsten carbide mould for vacuum hot-pressing sintering, and cooling after sintering to obtain a titanium-plated diamond copper alloy block for later use;
step four: crushing the titanium-plated diamond copper alloy block prepared in the third step into small particles of 5-10 mm;
step five: carrying out ball milling on the titanium-plated diamond copper alloy granules obtained by crushing in the fourth step by using a ball mill, and filling nitrogen for protection during ball milling to obtain titanium-plated diamond copper alloy powder which is 25 microns and is uniformly mixed for later use;
step six: screening the titanium-plated diamond copper alloy powder prepared in the fifth step by using a 400-mesh vibrating screen, leaving fine and uniform titanium-plated diamond copper alloy powder, and then drying and cooling the screened titanium-plated diamond copper alloy powder and taking out the titanium-plated diamond copper alloy powder for later use;
step seven: and taking the titanium-plated diamond copper alloy powder dried and cooled in the sixth step, and then carrying out laser printing by using an SLM 3D printer under the protection of high-purity nitrogen to print the titanium-plated diamond copper alloy powder to prepare the titanium-plated diamond copper composite material with high density and low porosity.
5. The method for preparing a titanium-plated diamond copper composite material according to claim 4, wherein: in the third step, the process conditions of the vacuum hot-pressing sintering are as follows: the vacuum degree in the furnace is 1 multiplied by 10-3-2×10-3kPa, the hot-pressing pressure is 75-85MPa, the sintering temperature is 880-910 ℃, and the time is 55-65 min.
6. The method for preparing a titanium-plated diamond copper composite material according to claim 4, wherein: in the sixth step, the drying temperature is 55-65 ℃, and the drying time is 240 min.
7. The method for preparing a titanium-plated diamond copper composite material according to claim 4, wherein: in the seventh step, the concentration of nitrogen is between 99.5 and 99.9 percent.
8. The method for preparing a titanium-plated diamond copper composite material according to claim 4, wherein: in the seventh step, the laser power is 140-.
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