CN104630527B - A kind of method preparing copper base diamond composite - Google Patents
A kind of method preparing copper base diamond composite Download PDFInfo
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Abstract
The present invention discloses a kind of method preparing copper base diamond composite.The method is copper alloy/pure copper material to be processed into the final size of diamond/copper goods as mould, is then poured into jolt ramming in mould, then drips binder solution by diamond single crystal/coating diamond particles；Under the conditions of 200 600 DEG C, application of vacuum prepares diamond stephanoporate framework blank afterwards；Again diamond stephanoporate framework blank is loaded jacket together with copper alloy/fine copper mould and carry out hip treatment, after cooling, obtain composite.The inventive method can realize near-net-shape, post-production amount is little, simple and reliable process, the diamond/copper composite property concordance prepared is good, this material is respectively provided with preferable combination property as electronic package material and heat-radiating substrate material, its thermal conductivity can reach 700w/mk, and thermal coefficient of expansion can realize free regulation, less than 6.5*10 under room temperature condition‑6M/k, consistency reaches more than 99.9%.
Description
Technical field
The invention belongs to the technology of preparing of a kind of copper base diamond composite, be specifically related to a kind of heat etc. quiet
The method that pressure near-net-shape prepares high heat-conductive diamond/carbon/carbon-copper composite material.
Background technology
Along with improving constantly of chip integration, Electronic Packaging is to miniaturization, lightweight and high performance side
To development so that the operating temperature of circuit constantly rises, system unit volume heat generation rate constantly increases and causes
System job insecurity.In order to obtain stable performance, it is necessary to improve radiating condition, thus Electronic Packaging
Importance at microelectronic constantly promotes, along with the demand of New Materials for Electric Packing also constantly
Increase.High quality diamond is to be currently known the material that thermal conductivity is the highest in the world, can reach
2000W/ (m K), and under room temperature, diamond is insulator, also has that dielectric constant is low, thermal coefficient of expansion
The feature such as low, but single diamond is difficult to be fabricated to encapsulating material, and cost is the highest, preferably
Metal-base composites is made with it.And metallic copper has excellent electric conductivity and high heat conductivility,
Its thermal coefficient of expansion (CTE) is 17 × 10-6K, thermal conductivity (TC) is 400W/ (m K), therefore, will
Diamond and copper are compounded to form diamond/copper composite, realize height by regulation diamond volume fraction
Thermal conductance and adjustable thermal expansion, fully meet the requirement of domestic and international thermal management materials.
The preparation difficult point of diamond/copper composite is: asking of the wettability extreme difference of (1) diamond and copper
Topic.At 1150 DEG C, diamond is 145 ° with the infiltration angle of copper, and between them, high temperature does not has solid state reaction to send out
Raw, diamond and copper are difficult to sinter out the composite of densification.By Modified Diamond, as added
Strong carbon compound element (W, B, Ti, Cr), thus improve the wettability of diamond and copper.But modification
Bring the most again and increase the new problem of interface resistance, affect thermal conductivity and the heat of diamond/copper composite
The coefficient of expansion；(2) diamond graphitization problem.In atmosphere, diamond easily graphitization, 773K with
Lower it is possible to graphitization completely.Under vacuum, 970K～1670K, diamond starts part
Graphitization phenomenon, when temperature is higher than 2070K, the then complete graphitization of diamond.Therefore prepare diamond/
During carbon/carbon-copper composite material, the technique such as protection of reducing atmosphere, pressurization should be made full use of, prevent diamond
There is graphitization.
In recent years, high temperature and high pressure method, infiltration method and vacuum plating then plasma discharging in advance are mainly used
The method these three method of body sintering prepares diamond/copper composite, wherein:
High temperature and high pressure method: be exactly that composite is sintered under relatively high sintering temperature and elevated pressures effect,
The method preparation time is short, beneficially the densification of composite.The direct bonding of diamond particles, is formed
Diamond framework.High-temperature high-pressure apparatus type is many most both at home and abroad, and process conditions easily realize, composite wood
The thermal conductivity of material is higher.Thus, become recent research, apply more a kind of preparation method；
Discharge plasma sintering: discharge plasma sintering (Spark plasma sintering is called for short SPS) work
Skill, 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 programming rate is fast, organizational structure is controlled, energy-conserving and environment-protective, and prepared sintered sample is brilliant
Grain is uniform, consistency is high, and mechanical property is good.The shortcoming of this preparation method is the densification of sintered composite materials
It is not fine for changing, especially for the composite that diamond volume fraction is higher.
Powder metallurgic method: traditional powder metallurgic method
After first diamond surface being processed, in-situ preparation metallic copper on this basis, then diamond/copper is multiple
Closing powder body powder metallurgy and be prepared as composite, this heat conductivity is up to 310W/ (m K).
But the method response time is longer, and sintered density is not readily reachable by.A kind of activation as powder metallurgy is burnt
Knot mode, is the preparation method that the most abroad diamond/copper composite is most commonly seen.It it is exactly composite
Sintering under sintering temperature and pressure act on simultaneously, the method preparation time is short, beneficially composite
Densification.
Liquid infiltration: this preparation method is liquid phase forming technique, has air pressure, hydraulic pressure, soaks mutually without hydraulic fluid
Oozing, this preparation method is used more in Al based composites, and this preparation method makes reinforcement and base
Body contact gear ratio is relatively abundant, than powder metallurgy preparation technique, composite is had more preferable consistency, so that
Composite obtains higher thermal conductivity.This preparation technology is higher to equipment requirements, selects suitable equipment
And technique can realize the efficient production of this kind of composite, the production cost of material is greatly lowered.
Three of the above method prepares diamond/copper composite, owing to Preparation equipment is prohibitively expensive, and the later stage
Difficulty of processing difficulty, largely adds and limits diamond/copper composite in electronic engineering
Application.
Summary of the invention
It is an object of the invention to provide a kind of method preparing copper base diamond composite, the method is adopted
Diamond/copper composite is prepared, the diamond/copper prepared by the method by isostatic pressed near-net-shape technology
The highest ideal of the key index such as heat conductivity and thermal coefficient of expansion, and it is near to solve diamond/copper
The clean problem shaped, method is simple, and material property concordance is the best.
To achieve these goals, present invention employs techniques below scheme:
A first aspect of the present invention, it is provided that a kind of method preparing copper base diamond composite, including such as
Lower step:
Step one, according to the final size of described copper base diamond composite, with the copper containing active element
Alloy is that raw material makes mould；
Step 2, weighs the diamond weight needed, then according to the diamond tap density recorded in advance
Diamond particles is filled in the mould described in step one and jolt ramming；
Step 3, drips binding agent in the diamond particles of described step 2 mould, then will be filled with
The mould of diamond particles vacuum bakeout under the conditions of 200-600 DEG C, vacuum degree control is 0.001～0.1Pa
Scope；
Step 4, loads in jacket by the mould being filled with diamond particles after baking, laggard through soldering and sealing
Row hip treatment, wherein, hip temperature is 1100-1350 DEG C, and high temperature insostatic pressing (HIP) pressure is
20-100MPa, temperature retention time is 0.5-2h, obtains described copper base diamond composite after cooling.
In the method for first aspect present invention, as a kind of preferred implementation, described copper base diamond
In composite, the mass percent of described diamond be 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 active element
Copper alloy in, described active element is Cr or B, wherein, when described active element is Cr,
In copper alloy, the mass percentage content of Cr be 0.1-5% (such as 0.2%, 0.7%, 1.5%, 1.9%,
2.8%, 3.5%, 4.5%), remaining is copper；When described active element is B, in copper alloy, B
Mass percentage content be 0.1-3% (such as 0.2%, 0.7%, 1.5%, 1.9%, 2.3%, 2.9%),
Remaining is copper.
In the method for first aspect present invention, as a kind of preferred implementation, described diamond is gold
Hard rock monocrystalline, granularity be 80-400 μm (such as: 85 μm, 100 μm, 150 μm, 180 μm, 250 μm,
300μm、350μm、390μm)。
In the method for first aspect present invention, described binding agent can be inorganic salt solution, it is also possible to
It is water soluble organic substance, or is the mixture of above-mentioned inorganic salt solution and water soluble organic substance, as
A kind of preferred implementation, described binding agent is Na2SiO3、AlPO4, dextrin, starch and Polyethylene Glycol
In the aqueous solution of one or more mixture.
In the method for first aspect present invention, as a kind of preferred implementation, the use of described binding agent
Amount is 0.2～1mL/g diamond, such as: every g diamond dropping 0.3mL binding agent, every g Buddha's warrior attendant
Stone dropping 0.5mL binding agent, every g diamond dropping 0.7mL binding agent, every g diamond dropping 0.9
ML binding agent.
In the method for first aspect present invention, in described step 3, it is filled with the mould of diamond particles
Have 200-600 DEG C (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) under the conditions of vacuum bakeout, vacuum degree control 0.001～0.1Pa scope (such as:
0.003Pa、0.05Pa、0.08Pa、0.09Pa)；As a kind of preferred implementation, described vacuum bakeout
Temperature be 280-300 DEG C, vacuum is 0.01Pa, and baking time is 2-3 hour.
In a second aspect of the present invention, it is provided that a kind of method preparing copper base diamond composite, including
Following steps:
Step one, plates active element at diamond particle surfaces, thus obtains coating diamond；According to
The final size of described copper base diamond composite, makes mould with fine copper for raw material；
Step 2, weighs, according to the diamond tap density recorded in advance, the described coating gold that step one obtains
Hard rock weight, is then filled into described coating diamond particles in the mould described in step one and jolt ramming；
Step 3, drips binding agent in the coating diamond particles of described mould, then will be filled with plating
Mould vacuum bakeout under the conditions of 200-600 DEG C of layer diamond particles, vacuum degree control 0.001～
0.1Pa scope；
Step 4, loads in jacket by the mould being filled with coating diamond particles after baking, after soldering and sealing
Carrying out hip treatment, wherein, hip temperature is 1100-1350 DEG C, and high temperature insostatic pressing (HIP) pressure is
20-100MPa, temperature retention time is 0.5-2h, obtains described copper base diamond composite after cooling.
In the method for second aspect present invention, as a kind of preferred implementation, described at diamond table
It is vacuum evaporation, magnetron sputtering or salt bath plating that face plates the method for active element, and these three method is
This area conventional method.
In the method for second aspect present invention, as a kind of preferred implementation, described coating diamond
Thickness of coating be 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, described copper base diamond
In composite, the mass percent of described diamond be 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 gold
Hard rock monocrystalline, granularity be 80-400 μm (such as: 85 μm, 100 μm, 150 μm, 180 μm, 250 μm,
300μm、350μm、390μm)。
In the method for second aspect present invention, described binding agent can be inorganic salt solution, it is also possible to
It is water soluble organic substance, or is the mixture as above-mentioned inorganic salt solution and water soluble organic substance,
As a kind of preferred implementation, described binding agent is Na2SiO3、AlPO4, dextrin, starch and poly-second
The aqueous solution of one or more mixture in glycol.
In the method for second aspect present invention, as a kind of preferred implementation, the use of described binding agent
Amount is 0.2～1mL/g coating diamond, such as: every g coating diamond dropping 0.3mL binding agent,
Every g coating diamond dropping 0.5mL binding agent, every g coating diamond dropping 0.7mL binding agent,
Every g coating diamond dropping 0.9mL binding agent.
In the method for second aspect present invention, in described step 3, it is filled with coating diamond particles
Mould 200-600 DEG C (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) under the conditions of vacuum bakeout, vacuum degree control 0.001～0.1Pa scope (ratio
As: 0.003Pa, 0.05Pa, 0.08Pa, 0.09Pa)；As a kind of preferred implementation, described vacuum
The temperature of baking is 280-300 DEG C, and vacuum is 0.01Pa, and baking time is 2-3 hour.
In the method for first aspect present invention and second aspect, jacket can use metal or ceramic making,
Such as mild steel, Ni, Mo, glass etc..
In the method for first aspect present invention and second aspect, high temperature insostatic pressing (HIP) (high temperature insostatic pressing (HIP) (Hot
IsostaticPressing), it being called for short HIP) technique is to be placed into by goods in airtight container, to goods
Applying each to equal pressure, impose high temperature simultaneously, under the influence of high pressure and temperature, goods are sintered
And densification.High temperature insostatic pressing (HIP) condition can make suitably adjustment according to workpiece size.
The method of the present invention is the final size being processed into diamond/copper goods by copper alloy/pure copper material
As mould, this mould is utilized to pour diamond single crystal/coating diamond particles in mould jolt ramming, so
Rear dropping binder solution bonds.Under the conditions of 200-600 DEG C, application of vacuum prepares diamond porous bone again
Frame blank.Again the diamond stephanoporate framework blank handled well is loaded jacket together with copper alloy/fine copper mould
Carry out hip treatment after soldering and sealing, be cooled to room temperature and obtain diamond/copper composite.
The inventive method using copper or copper alloy as mold materials, it is achieved that the accurate control of diamond/copper size
System, processes technique by isostatic pressed, it is achieved that diamond/copper near-net-shape simultaneously, greatly reduces Buddha's warrior attendant
The post-production of stone/carbon/carbon-copper composite material, composite product consistency prepared by heat and other static pressuring processes is high, property
Energy concordance is good, and technique is simple.The method achieves diamond by pretreatment and keeps during oozing copper
In vacuum environment, it is to avoid diamond graphitization in pyroprocess.Obtained heat conductivity can
Up to 700w/mk, thermal coefficient of expansion can realize free regulation, less than 6.5*10 under room temperature condition-6M/k,
Consistency (i.e. relative density) reaches more than 99.9%.This composite is as electronic package material and dissipates
Substrate materials is respectively provided with preferable combination property.
Detailed description of the invention
Below by specific embodiment, the preparation method of the present invention is described in detail, but the present invention is not
It is limited to this.
Capital equipment used in the present invention is: vacuum drying 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 composite prepared by the present embodiment, the mass percentage content of diamond is
40%.
Preparation method is as follows:
(1) method plated surface at the diamond dust that granularity is 200 μm of magnetron sputtering is used
The Cr coating of 0.5 μm, forms plating Cr diamond single crystal；
(2) final size described in the copper base diamond composite drawing prepared according to the present embodiment,
A commercially available no-oxygen copper plate is processed into oxygen-free copper mould；
(3) according to the diamond tap density recorded in advance, calculating diamond weight according to m=ρ v is
12g, then weighs 12g plating Cr diamond and pours jolt ramming in oxygen-free copper mould into；
(4) in the plating Cr diamond of jolt ramming, the aluminum phosphate that mass percent concentration is 30% is dripped water-soluble
Liquid, consumption of binder is that about 0.5mL/g plates Cr diamond, is put by the base substrate of molding after naturally drying
Entering to be heated in vacuum drying oven maximum temperature 600 DEG C to toast, be incubated 2h, vacuum degree control is 0.005Pa
Left and right, obtains the complex of diamond framework material and copper mould；
(5) complex after baking is loaded in jacket, first the most again will with gas welding with vacuum pump evacuation
Bleeding point seals up i.e. soldering and sealing.Then the jacket after soldering and sealing is put into heating infiltration in heat isostatic apparatus, adds
Hot temperature is about 1150 DEG C, and pressure, in 50MPa, temperature retention time 1 hour, i.e. obtains this reality after cooling
Execute the diamond/copper based composites of example.
The composite obtaining the present embodiment carries out performance test, uses drainage to measure the density of material,
Density is 5.66g/cm3, consistency (relative density) is 99.91%；With the production of Nai Chi company of Germany
The thermal conductivity of composite measured by LFA447 LASER HEAT conductance/thermal diffusion coefficient analyzer, and this embodiment is multiple
The thermal conductivity of condensation material is 712W/ (m K)；NETZSCH DIL 402C thermal dilatometer is used to measure heat
The coefficient of expansion, under room temperature condition, the thermal coefficient of expansion of this embodiment composite is 5.6ppm/k.
Embodiment 2
In copper base diamond composite prepared by the present embodiment, CuB2Alloy mass degree is
38%, diamond quality degree is 62%.
(1) high-purity B powder and fine copper block being placed in melting in vacuum intermediate-frequency smelting furnace, the final B that obtains contains
Amount 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 needed, Cu-B alloy is i.e. obtained
Plate；
(3) final size described in the copper base diamond composite drawing prepared according to the present embodiment,
Above-mentioned Cu-B alloy plate is processed into mould；
(4) according to the diamond tap density recorded in advance, calculating diamond weight according to m=ρ v is
10g, weighs diamond single crystal that 10g granularity is 100 μm and is poured into jolt ramming in above-mentioned mould；
(5) dripping polyethylene glycol 6000 in the diamond of jolt ramming, consumption of binder is about 0.5mL
/ g diamond, puts into the base substrate of molding after naturally drying and is heated to maximum temperature 400 DEG C in vacuum drying oven and enters
Row baking, is incubated 1h, and vacuum degree control is about 0.005Pa, obtains diamond framework material and copper mold
The complex of tool；
(5) complex after baking is loaded in jacket, first the most again will with gas welding with vacuum pump evacuation
Bleeding point seals up i.e. soldering and sealing.Then the jacket after soldering and sealing is put into heating infiltration in heat isostatic apparatus, adds
Hot temperature is about 1150 DEG C, and pressure is in 50MPa scope, and temperature retention time 1 hour, after cooling and get final product
Diamond/copper based composites to the present embodiment.
The composite obtaining the present embodiment carries out performance test, and method of testing is with embodiment 1, and this is multiple
The density of condensation material is 5.55g/cm3, consistency is 99.9%, and thermal conductivity is 685W/ (m K), heat
The coefficient of expansion is 6.2ppm/k.
Claims (10)
1. the method preparing copper base diamond composite, it is characterised in that comprise the steps:
Step one, according to the final size of described copper base diamond composite, 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, is then filled into by diamond particles in the mould described in step one and jolt ramming；
Step 3, drips binding agent in the diamond particles of described step 2 mould, then will be filled with mould vacuum bakeout under the conditions of 200-600 DEG C of diamond particles, and vacuum degree control is in 0.001-0.1Pa scope；
Step 4, loads the mould being filled with diamond particles after baking in jacket, carries out hip treatment after soldering and sealing, wherein, hip temperature is 1100-1350 DEG C, and high temperature insostatic pressing (HIP) pressure is 20-100MPa, temperature retention time is 0.5-2h, obtains described copper base diamond composite after cooling.
Method the most according to claim 1, it is characterised in that in the described copper alloy containing 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 remaining is copper；When described active element is B, in copper alloy, the mass percentage content of B is 0.1-3%, and remaining is copper.
Method the most according to claim 1, it is characterised in that described binding agent is Na2SiO3、AlPO4, dextrin, the aqueous solution of one or more mixture in starch and Polyethylene Glycol；The consumption of described binding agent is 0.2-1mL/g diamond.
4. the method preparing copper base diamond composite, it is characterised 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 composite, make mould with fine copper for raw material；
Step 2, weighs, according to the diamond tap density recorded in advance, the described coating diamond weight that step one obtains, and is then filled in the mould described in step one by described coating diamond particles and jolt ramming；
Step 3, drips binding agent in the coating diamond particles of described mould, then will be filled with mould vacuum bakeout under the conditions of 200-600 DEG C of coating diamond particles, and 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, high temperature insostatic pressing (HIP) pressure is 20-100MPa, and temperature retention time is 0.5-2h, obtains described copper base diamond composite after cooling.
Method the most according to claim 4, it is characterised in that the thickness of coating of described coating diamond is 0.1-1 μm.
Method the most according to claim 4, it is characterised in that described active element is Cr or B.
7., according to the method described in claim 1 or 4, it is characterised in that in described copper base diamond composite, the mass percent of described diamond is 40-80%.
8., according to the method described in claim 1 or 4, it is characterised in that described diamond is diamond single crystal, granularity is 80-400 μm.
Method the most according to claim 4, it is characterised in that described binding agent is Na2SiO3、AlPO4, dextrin, the aqueous solution of one or more mixture in starch and Polyethylene Glycol；The consumption of described binding agent is 0.2～1mL/g coating diamond.
10. according to the method described in claim 1 or 4, it is characterised in that in described step 3, the temperature of described vacuum bakeout is 280-300 DEG C, and vacuum is 0.01Pa, and baking time is 2-3 hour.
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| CN106583735B (en) * | 2016-12-22 | 2018-11-27 | 北京科技大学 | A method of it prepares with high-volume fractional diamond/copper composite material parts |
| CN107937783A (en) * | 2017-11-17 | 2018-04-20 | 湖南大学 | Increase the method for binding ability between diamond and metallic matrix |
| CN108220836B (en) * | 2017-12-06 | 2019-08-20 | 浙江工贸职业技术学院 | Lightweight metal polyporous material intensifying method based on different-diameter high duty metal ball |
| CN108220835B (en) * | 2017-12-06 | 2019-08-20 | 浙江工贸职业技术学院 | Lightweight metal polyporous material intensifying method based on single diameter high duty metal ball |
| CN110951984A (en) * | 2019-12-26 | 2020-04-03 | 兰州空间技术物理研究所 | Method for improving thermal conductivity of diamond/copper composite material |
| 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 |
| CN113210611B (en) * | 2021-04-20 | 2023-05-16 | 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 |
| CN115475938B (en) * | 2022-09-23 | 2024-03-08 | 安徽工程大学 | Copper-based diamond composite board/strip 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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