CN104630527A - Method for preparing copper-based diamond composite material - Google Patents
Method for preparing copper-based diamond composite material Download PDFInfo
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- CN104630527A CN104630527A CN201410842734.4A CN201410842734A CN104630527A CN 104630527 A CN104630527 A CN 104630527A CN 201410842734 A CN201410842734 A CN 201410842734A CN 104630527 A CN104630527 A CN 104630527A
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Abstract
The invention discloses a method for preparing a copper-based diamond composite material. The method comprises the following steps: processing a copper alloy/pure copper material into a final size of a diamond/copper product to serve as a mold, then pouring diamond single crystal/coated diamond granules into the mold, jolt ramming, and dripping an adhesive solution; vacuum treating at 200-600 DEG C to prepare a porous diamond skeleton blank; filling the porous diamond skeleton blank and the copper alloy/pure copper mold in a sheath, carrying out hot isostatic pressure treatment, and cooling to obtain the composite material. The method disclosed by the invention can be used for achieving near-net forming, the post processing capacity is small, the process is simple and reliable, the prepared diamond/copper composite material is good in performance uniformity, the material has good comprehensive performance with being used as an electronic package material and a radiating substrate material, the thermal conductivity of the material can reach 700w/mk, the thermal expansion coefficient can be freely adjusted and is not less than 6.5*10<-6> m/l at a room temperature condition, and the density is higher than 99.9%.
Description
Technical field
The invention belongs to a kind of technology of preparing of copper base diamond matrix material, be specifically related to a kind of method that hot isostatic pressing near-net-shape prepares high heat-conductive diamond/carbon/carbon-copper composite material.
Background technology
Along with improving constantly of chip integration, Electronic Packaging, to miniaturization, lightweight and high performance future development, makes the working temperature of circuit constantly rise, and system unit volume heat generation rate constantly increases and causes system works unstable.In order to obtain stable performance, radiating condition must be improved, thus Electronic Packaging constantly promotes in the importance of microelectronic, along with the demand of New Materials for Electric Packing also in continuous increase.High quality diamond is the material that current known thermal conductivity is the highest in the world, 2000W/ (mK) can be reached, and diamond is isolator under room temperature, also there is the features such as specific inductivity is low, thermal expansivity is low, but single diamond is not easily made into packaged material, and cost is very high, comparatively ideal is make metal-base composites with it.And metallic copper has excellent conductivity and high heat conductivility, its thermal expansivity (CTE) is 17 × 10
-6k, thermal conductivity (TC) is 400W/ (mK), therefore, diamond and copper is compounded to form diamond/copper matrix material, by regulating diamond volume fraction to realize high thermal conductance and adjustable thermal expansion, meet the requirement of domestic and international thermal management materials completely.
The preparation difficult point of diamond/copper matrix material is: the problem of the wettability extreme difference of (1) diamond and copper.At 1150 DEG C, the infiltration angle of diamond and copper is 145 °, and between them, high temperature does not have solid state reaction to occur, and diamond and copper are difficult to sinter out fine and close matrix material.By Modified Diamond, as added strong carbon compound element (W, B, Ti, Cr), thus improve the wettability of diamond and copper.But bring again the new problem increasing interface resistance while modification, affect thermal conductivity and the thermal expansivity of diamond/copper matrix material; (2) diamond graphitization problem.In atmosphere, diamond is greying very easily, and below 773K just may complete greying.Under vacuum, 970K ~ 1670K, diamond starts generating portion greying phenomenon, when temperature is higher than 2070K, then the complete greying of diamond.Therefore in the process preparing diamond/copper matrix material, the technique such as protection of reducing atmosphere, pressurization should be made full use of, prevent diamond generation greying.
In recent years, mainly adopt high temperature and high pressure method, infiltration method and in advance vacuum plating then discharge plasma sintering these three kinds of methods of method prepare diamond/copper matrix material, wherein:
High temperature and high pressure method: be exactly that matrix material is sintered under comparatively high sintering temperature and elevated pressures effect, the method preparation time is short, is conducive to the densification of matrix material.The direct Cheng Jian of diamond particles, forms diamond framework.High-temperature high-pressure apparatus type is many both at home and abroad at present, and processing condition easily realize, and the thermal conductivity of matrix material is higher.Thus, become recent research, apply more a kind of preparation method;
Discharge plasma sintering: discharge plasma sintering (Spark plasma sintering, be called for short SPS) technique is that development in recent years is got up a kind of novel material preparation method.Compared with traditional sintering method, SPS has the advantages such as heat-up rate is fast, weave construction is controlled, energy-conserving and environment-protective, and obtained sintered sample uniform crystal particles, density are high, and mechanical property is good.The shortcoming of this preparation method is the densification of sintered composite materials is not fine, especially for the matrix material that diamond volume fraction is higher.
Powder metallurgic method: traditional powder metallurgic method
First after diamond surface process, in-situ preparation metallic copper on this basis, then diamond/copper composite granule powder metallurgy is prepared into matrix material, this heat conductivity can reach 310W/ (mK).But the method reaction times is longer, sintered density is not easy to reach.As a kind of activated sintering mode of powder metallurgy, be the preparation method that external diamond/copper matrix material is the most common at present.Be exactly that matrix material sinters under sintering temperature and pressure act on simultaneously, the method preparation time is short, is conducive to the densification of matrix material.
Liquid infiltration: this preparation method is liquid phase forming technique, there are air pressure, hydraulic pressure, liguid infiltration with no pressure, this preparation method uses more in Al based composites, this preparation method make reinforcement and substrate contact more abundant, there is better density than powder metallurgy preparation technique to matrix material, thus make matrix material obtain higher thermal conductivity.This preparation technology is higher to equipment requirements, selects suitable instrument and supplies can realize the High-efficient Production of this kind of matrix material, significantly reduces the production cost of material.
Above three kinds of methods prepare diamond/copper matrix material, and because Preparation equipment is too expensive, post-production difficulty difficulty, adds to a great extent and limit the application of diamond/copper matrix material in electronic engineering.
Summary of the invention
The object of the present invention is to provide a kind of method preparing copper base diamond matrix material, the method adopts isostatic pressed near-net-shape technology to prepare diamond/copper matrix material, the all higher ideals of key index such as the diamond/copper heat conductivity prepared by the method and thermal expansivity, and solve the problem of diamond/copper near-net-shape, method is simple, and material property consistence is very good.
To achieve these goals, present invention employs following technical scheme:
A first aspect of the present invention, provides a kind of method preparing copper base diamond matrix material, comprises the steps:
Step one, according to the final size of described copper base diamond matrix material, makes mould with the copper alloy containing active element for raw material;
Step 2, weighs the diamond weight needed according to the diamond tap density recorded in advance, then diamond particles is filled into also jolt ramming in the mould described in step one;
Step 3, drips caking agent in the diamond particles of described step 2 mould, and then will be filled with mould vacuum bakeout under 200-600 DEG C of condition of diamond particles, vacuum degree control is in 0.001 ~ 0.1Pa scope;
Step 4, the mould being filled with diamond particles after baking is loaded in jacket, hip treatment is carried out after soldering and sealing, wherein, hip temperature is 1100-1350 DEG C, hot isostatic pressing pressure is 20-100MPa, and soaking time is 0.5-2h, obtains described copper base diamond matrix material after cooling.
In the method for first aspect present invention, as a kind of preferred implementation, in described copper base diamond matrix material, described adamantine mass percent is 40-80% (such as 45%, 55%, 60%, 70%, 75%, 78%).
In the method for first aspect present invention, as a kind of preferred implementation, described containing in the copper alloy of active element, described active element is Cr or B, wherein, when described active element is Cr, in copper alloy, the mass percentage content of Cr is 0.1-5% (such as 0.2%, 0.7%, 1.5%, 1.9%, 2.8%, 3.5%, 4.5%), and all the other are copper; When described active element is B, in copper alloy, the mass percentage content of B is 0.1-3% (such as 0.2%, 0.7%, 1.5%, 1.9%, 2.3%, 2.9%), and all the other are copper.
In the method for first aspect present invention, as a kind of preferred implementation, described diamond is diamond single crystal, and granularity is 80-400 μm (such as: 85 μm, 100 μm, 150 μm, 180 μm, 250 μm, 300 μm, 350 μm, 390 μm).
In the method for first aspect present invention, described caking agent can be inorganic salt solution, also can be water soluble organic substance, or is the mixture of above-mentioned inorganic salt solution and water soluble organic substance, and as a kind of preferred implementation, described caking agent is Na
2siO
3, AlPO
4, dextrin, one or more mixtures in starch and polyoxyethylene glycol the aqueous solution.
In the method for first aspect present invention, as a kind of preferred implementation, the consumption of described binding agent is 0.2 ~ 1mL/g diamond, such as: every g diamond drips 0.3mL binding agent, every g diamond drips 0.5mL binding agent, every g diamond drips 0.7mL binding agent, and every g diamond drips 0.9mL binding agent.
In the method for first aspect present invention, in described step 3, be filled with mould vacuum bakeout under 200-600 DEG C of (such as 210 DEG C, 250 DEG C, 300 DEG C, 340 DEG C, 400 DEG C, 450 DEG C, 500 DEG C, 520 DEG C, 580 DEG C) condition of diamond particles, vacuum degree control is 0.001 ~ 0.1Pa scope (such as: 0.003Pa, 0.05Pa, 0.08Pa, 0.09Pa); As a kind of preferred implementation, the temperature of described vacuum bakeout is 280-300 DEG C, and vacuum tightness is 0.01MPa, and baking time is 2-3 hour.
In a second aspect of the present invention, a kind of method preparing copper base diamond matrix material is provided, comprises the steps:
Step one, plates active element at diamond particle surfaces, thus obtains coating diamond; According to the final size of described copper base diamond matrix material, be that raw material makes mould with fine copper;
Step 2, the described coating diamond weight obtained according to the diamond tap density weighing step one recorded in advance, is then filled into also jolt ramming in the mould described in step one by described coating diamond particles;
Step 3, drips caking agent in the coating diamond particles of described mould, and then will be filled with mould vacuum bakeout under 200-600 DEG C of condition of coating diamond particles, vacuum degree control is in 0.001 ~ 0.1Pa scope;
Step 4, the mould being filled with coating diamond particles after baking is loaded in jacket, hip treatment is carried out after soldering and sealing, wherein, hip temperature is 1100-1350 DEG C, hot isostatic pressing pressure is 20-100MPa, and soaking time is 0.5-2h, obtains described copper base diamond matrix material after cooling.
In the method for second aspect present invention, as a kind of preferred implementation, the described method plating active element at diamond surface is vacuum evaporation, magnetron sputtering or salt bath plating, and these three kinds of methods are this area ordinary method.
In the method for second aspect present invention, as a kind of preferred implementation, the adamantine thickness of coating of described coating is 0.1-1 μm (such as 0.2 μm, 0.4 μm, 0.6 μm, 0.8 μm, 0.9 μm).
In the method for second aspect present invention, as a kind of preferred implementation, in described copper base diamond matrix material, described adamantine mass percent is 40-80% (such as 45%, 55%, 60%, 70%, 75%, 78%).
In the method for second aspect present invention, as a kind of preferred implementation, described active element is Cr or B.
In the method for second aspect present invention, as a kind of preferred implementation, described diamond is diamond single crystal, and granularity is 80-400 μm (such as: 85 μm, 100 μm, 150 μm, 180 μm, 250 μm, 300 μm, 350 μm, 390 μm).
In the method for second aspect present invention, described caking agent can be inorganic salt solution, also can be water soluble organic substance, or is the mixture as above-mentioned inorganic salt solution and water soluble organic substance, and as a kind of preferred implementation, described caking agent is Na
2siO
3, AlPO
4, dextrin, one or more mixtures in starch and polyoxyethylene glycol the aqueous solution.
In the method for second aspect present invention, as a kind of preferred implementation, the consumption of described binding agent is 0.2 ~ 1mL/g coating diamond, such as: every g coating diamond drips 0.3mL binding agent, every g coating diamond drips 0.5mL binding agent, every g coating diamond drips 0.7mL binding agent, and every g coating diamond drips 0.9mL binding agent.
In the method for second aspect present invention, in described step 3, be filled with mould vacuum bakeout under 200-600 DEG C of (such as 210 DEG C, 250 DEG C, 300 DEG C, 340 DEG C, 400 DEG C, 450 DEG C, 500 DEG C, 520 DEG C, 580 DEG C) condition of coating diamond particles, vacuum degree control is 0.001 ~ 0.1Pa scope (such as: 0.003Pa, 0.05Pa, 0.08Pa, 0.09Pa); As a kind of preferred implementation, the temperature of described vacuum bakeout is 280-300 DEG C, and vacuum tightness is 0.01MPa, and baking time is 2-3 hour.
In the method for first aspect present invention and second aspect, jacket can adopt metal or ceramic making, such as soft steel, Ni, Mo, glass etc.
In the method for first aspect present invention and second aspect, hot isostatic pressing (hot isostatic pressing (Hot IsostaticPressing), being called for short HIP) technique is placed into by goods in airtight container, apply each to equal pressure to goods, impose high temperature simultaneously, under the influence of high pressure and temperature, goods are sintered and densification.Hot isostatic pressing condition can make suitable adjustment according to workpiece size.
Method of the present invention is processed into the final size of diamond/copper goods as mould by copper alloy/pure copper material, utilizes this mould to pour diamond single crystal/coating diamond particles in mould jolt ramming, then drips adhesive solution bonding.Under 200-600 DEG C of condition, vacuum-treat obtains diamond stephanoporate framework blank again.Carry out hip treatment after again the diamond stephanoporate framework blank handled well being loaded jacket soldering and sealing together with copper alloy/fine copper mould, be cooled to room temperature and obtain diamond/copper matrix material.
The inventive method using copper or copper alloy as moulding stock, achieve the accurate control of diamond/copper size, simultaneously by isostatic pressed treatment process, achieve diamond/copper near-net-shape, greatly reduce the post-production of diamond/copper matrix material, composite product density prepared by heat and other static pressuring processes is high, and consistency of performance is good, and technique is simple.The method achieves diamond oozing in copper process by pre-treatment and remains on vacuum environment, avoids diamond graphitization in pyroprocess.Obtained heat conductivity can up to 700w/mk, and thermal expansivity can realize free adjustment, lower than 6.5*10 under room temperature condition
-6m/k, density (i.e. relative density) reaches more than 99.9%.This matrix material all has good over-all properties as electronic package material and heat-radiating substrate material.
Embodiment
Below by specific embodiment, preparation method of the present invention is described in detail, but the present invention is not limited to this.
Major equipment used in the present invention is: vacuum oven, heat isostatic apparatus, vacuum intermediate-frequency smelting furnace, magnetron sputtering stove etc.These equipment are this area conventional equipment.
Embodiment 1
In copper base diamond matrix material prepared by the present embodiment, adamantine mass percentage content is 40%.
Preparation method is as follows:
(1) method of employing magnetron sputtering is the Cr coating of the plated surface 0.5 μm of the diamond powder of 200 μm in granularity, forms plating Cr diamond single crystal;
(2) final size recorded in the copper base diamond matrix material drawing prepared according to the present embodiment, is processed into oxygen free copper mould by a commercially available no-oxygen copper plate;
(3) according to the diamond tap density recorded in advance, calculating diamond weight according to m=ρ v is 12g, then takes 12g plating Cr diamond and pours jolt ramming in oxygen free copper mould into;
(4) in the plating Cr diamond of jolt ramming, the aluminium phosphate aqueous solution that mass percent concentration is 30% is dripped, consumption of binder is that about 0.5mL/g plates Cr diamond, naturally after drying, shaping base substrate is put into vacuum oven to be heated to top temperature 600 DEG C and to toast, insulation 2h, vacuum degree control is about 0.005Pa, obtains the complex body of diamond framework material and copper mould;
(5) complex body after baking is loaded in jacket, first with vacuum pump evacuation and then with gas welding, bleeding point is sealed up i.e. soldering and sealing.Then the jacket after soldering and sealing is put into heat isostatic apparatus heating infiltration, Heating temperature is about 1150 DEG C, and pressure is at 50MPa, and soaking time 1 hour, namely obtains the diamond/copper based composites of the present embodiment after cooling.
Carry out performance test to the matrix material that the present embodiment obtains, adopt drainage to measure the density of material, density is 5.66g/cm
3, density (relative density) is 99.91%; The thermal conductivity of matrix material measured by the LFA447 LASER HEAT conductance of producing with German Nai Chi company/thermal diffusivity determinator, and the thermal conductivity of this embodiment matrix material is 712W/ (mK); Adopt NETZSCH DIL 402C thermal dilatometer to measure thermal expansivity, under room temperature condition, the thermal expansivity of this embodiment matrix material is 5.6ppm/k.
Embodiment 2
In copper base diamond matrix material prepared by the present embodiment, CuB
2alloy mass degree is 38%, and diamond quality degree is 62%.
(1) high-purity B powder and fine copper block are placed in the melting of vacuum intermediate-frequency smelting furnace, final acquisition B content is the Cu-B alloy ingot of 2wt%;
(2) by the rolling of above-mentioned Cu-B alloy ingot to be thinned to the thickness of needs, namely obtain Cu-B alloy plate;
(3) final size recorded in the copper base diamond matrix material drawing prepared according to the present embodiment, is processed into mould by above-mentioned Cu-B alloy plate;
(4) according to the diamond tap density recorded in advance, calculating diamond weight according to m=ρ v is 10g, takes 10g granularity and is the diamond single crystal of 100 μm and is poured into jolt ramming in above-mentioned mould;
(5) in the diamond of jolt ramming, polyethylene glycol 6000 is dripped, consumption of binder is about 0.5mL/g diamond, naturally after drying, shaping base substrate is put into vacuum oven to be heated to top temperature 400 DEG C and to toast, insulation 1h, vacuum degree control is about 0.005Pa, obtains the complex body of diamond framework material and copper mould;
(5) complex body after baking is loaded in jacket, first with vacuum pump evacuation and then with gas welding, bleeding point is sealed up i.e. soldering and sealing.Then the jacket after soldering and sealing is put into heat isostatic apparatus heating infiltration, Heating temperature is about 1150 DEG C, and pressure is in 50MPa scope, and soaking time 1 hour, namely obtains the diamond/copper based composites of the present embodiment after cooling.
Carry out performance test to the matrix material that the present embodiment obtains, testing method is with embodiment 1, and the density of this matrix material is 5.55g/cm
3, density is 99.9%, and thermal conductivity is 685W/ (mK), and thermal expansivity is 6.2ppm/k.
Claims (10)
1. prepare a method for copper base diamond matrix material, it is characterized in that, comprise the steps:
Step one, according to the final size of described copper base diamond matrix material, makes mould with the copper alloy containing active element for raw material;
Step 2, weighs the diamond weight needed according to the diamond tap density recorded in advance, then diamond particles is filled into also jolt ramming in the mould described in step one;
Step 3, drips caking agent in the diamond particles of described step 2 mould, and then will be filled with mould vacuum bakeout under 200-600 DEG C of condition of diamond particles, vacuum degree control is in 0.001-0.1Pa scope;
Step 4, the mould being filled with diamond particles after baking is loaded in jacket, hip treatment is carried out after soldering and sealing, wherein, hip temperature is 1100-1350 DEG C, hot isostatic pressing pressure is 20-100MPa, and soaking time is 0.5-2h, obtains described copper base diamond matrix material after cooling.
2. method according to claim 1, is characterized in that, described containing in the copper alloy of active element, described active element is Cr or B, and wherein, when described active element is Cr, in copper alloy, the mass percentage content of Cr is 0.1-5%, and all the other are copper; When described active element is B, in copper alloy, the mass percentage content of B is 0.1-3%, and all the other are copper.
3. method according to claim 1, is characterized in that, described caking agent is Na
2siO
3, AlPO
4, dextrin, one or more mixtures in starch and polyoxyethylene glycol the aqueous solution; Preferably, the consumption of described binding agent is 0.2-1mL/g diamond.
4. prepare a method for copper base diamond matrix material, it is characterized in that, comprise the steps:
Step one, plates active element at diamond particle surfaces, thus obtains coating diamond; According to the final size of described copper base diamond matrix material, be that raw material makes mould with fine copper;
Step 2, the described coating diamond weight obtained according to the diamond tap density weighing step one recorded in advance, is then filled into also jolt ramming in the mould described in step one by described coating diamond particles;
Step 3, drips caking agent in the coating diamond particles of described mould, and then will be filled with mould vacuum bakeout under 200-600 DEG C of condition of coating diamond particles, vacuum degree control is in 0.001-0.1Pa scope;
Step 4, the mould being filled with coating diamond particles after baking is loaded in jacket, hip treatment is carried out after soldering and sealing, wherein, hip temperature is 1100-1350 DEG C, hot isostatic pressing pressure is 20-100MPa, and soaking time is 0.5-2h, obtains described copper base diamond matrix material after cooling.
5. method according to claim 4, is characterized in that, the adamantine thickness of coating of described coating is 0.1-1 μm.
6. method according to claim 4, is characterized in that, described active element is Cr or B.
7. the method according to claim 1 or 4, is characterized in that, in described copper base diamond matrix material, described adamantine mass percent is 40-80%.
8. the method according to claim 1 or 4, is characterized in that, described diamond is diamond single crystal, and granularity is 80-400 μm.
9. method according to claim 4, is characterized in that, described caking agent is Na
2siO
3, AlPO
4, dextrin, one or more mixtures in starch and polyoxyethylene glycol the aqueous solution; Preferably, the consumption of described binding agent is 0.2 ~ 1mL/g coating diamond.
10. the method according to claim 1 or 4, is characterized in that, in described step 3, the temperature of described vacuum bakeout is 280-300 DEG C, and vacuum tightness is 0.01MPa, and baking time is 2-3 hour.
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| CN111826542B (en) * | 2020-06-30 | 2022-01-04 | 长沙新材料产业研究院有限公司 | Copper-based diamond gradient heat dissipation material and preparation method thereof |
| CN111826542A (en) * | 2020-06-30 | 2020-10-27 | 长沙新材料产业研究院有限公司 | Copper-based diamond gradient heat dissipation material and preparation method thereof |
| CN113210611A (en) * | 2021-04-20 | 2021-08-06 | 湖南浩威特科技发展有限公司 | Copper-diamond composite material with metal layer coated on surface and preparation method and application thereof |
| CN113718127A (en) * | 2021-08-16 | 2021-11-30 | 安泰科技股份有限公司 | High-performance copper-based solid self-lubricating composite material and preparation method thereof |
| CN115475938A (en) * | 2022-09-23 | 2022-12-16 | 安徽工程大学 | Copper-based diamond composite board/strip and preparation method thereof |
| CN115475938B (en) * | 2022-09-23 | 2024-03-08 | 安徽工程大学 | Copper-based diamond composite board/strip and preparation method thereof |
| CN117020209A (en) * | 2023-10-09 | 2023-11-10 | 赣州金顺科技有限公司 | Heat dissipation substrate and preparation method thereof |
| CN117020209B (en) * | 2023-10-09 | 2024-01-26 | 赣州金顺科技有限公司 | Heat dissipation substrate and preparation method thereof |
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