CN110284019A - A method of orienting doped graphite in a metal - Google Patents
A method of orienting doped graphite in a metal Download PDFInfo
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- CN110284019A CN110284019A CN201910624174.8A CN201910624174A CN110284019A CN 110284019 A CN110284019 A CN 110284019A CN 201910624174 A CN201910624174 A CN 201910624174A CN 110284019 A CN110284019 A CN 110284019A
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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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention discloses a kind of methods for orienting doped graphite in a metal, the following steps are included: sinter layer is mixed and is piled by the graphite composite powder of raw metal powder and/or metal-plated membrane, so that the graphite composite powder of the metal-plated membrane is in the preset position of the sinter layer with preset ratio；Under inert gas protection the sinter layer is heated to being sintered using orientation field；Accumulation sinter layer and successively sintering are repeated until material preparation is completed.The powdered graphite of metal powder and metal-plated membrane that increment is superimposed by the present invention, the metal film Flashmelt of metal powder and powdered graphite is made to be sintered to composite material using orientation field, not only with the performance of high thermal conductivity, composite material strength is improved, while meeting the demand to graphite-metal composite material complicated shape in varied situations.
Description
Technical field
The invention belongs to field of metal matrix composite, orient doped graphite in a metal more particularly, to a kind of
Method.
Background technique
With the fast development in electronic technology industry, the heat that device unit area distributes is more and more, opposite heat tube reason
The performance of material proposes more strict requirements.The exploitation of electronic package material is as an important ring, it is desirable that material has height
Thermal conductivity, low-expansion coefficient, lightweight, feature at low cost.However traditional Al/SiC composite material, Cu/W composite material and
Although the specific alloys material thermal expansion coefficient such as Cu/Mo composite material is lower, all passes through special processing, sacrifice material in heat
Performance in terms of the coefficient of conductivity and thermal diffusion coefficient；Although diamond and diamond composite thermal conductivity are high, due to gold
The ultrahigh hardness of hard rock, it is difficult to process.
Graphite-metal composite material due to the characteristics such as thermal conductivity is high, thermal expansion coefficient is small, thermal diffusion coefficient is high,
It is received more and more attention in thermal management materials application.The method of graphite-metal composite material is general are as follows:
(1) liquid phase process: it is divided into three kinds, gas pressure osmosis, squeeze casting method and pressureless penetration.Usually first pass through
The methods of hot pressing, dry-pressing and injection moulding prepare precast body, then prefabricated component is put into mould, then vacuumizes, will
It is heated to be passed through after molten state and is pressurizeed liquid metal (using gas pressure, liquid pressure or gravity, capillary
Pipe power etc.), liquid metal is penetrated into prefabricated component.
(2) solid state process: mainly powder metallurgic method, including hot pressed sintering and hot isostatic pressing etc..I.e. by powder (including
Graphite, metal etc.) be mixed in a certain ratio under suitable condition after, carry out compression moulding, then in vacuum or be passed through lazy
It is sintered under the protection of property gas.
In the above-mentioned methods, there are sintering temperature height, the demanding problems of jig, it is often more important that, can not flexibly it determine
To the control doping position of powdered graphite, doping, and the graphite-metal composite processing performance prepared is bad, causes
Graphite-metal composite material obtained is difficult during being processed into product, and yield rate is low；Especially when product has
When complex situations, preparation time length, processing difficulties.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the present invention provides one kind to orient doped graphite in a metal
Method, its object is to by orientation field increment sintering raw metal powder and graphite composite powder, realize without jig preparation appoint
Anticipating, position is adulterated, doping ratio is controllable, complex contour graphite-metallic composite, thus solves burning of the existing technology
Junction temperature height, is difficult to the technical issues of preparing the graphite-metal composite material of complicated shape at the demanding problem of jig.
To achieve the above object, according to one aspect of the present invention, it provides one kind and orients doped graphite in a metal
Method, comprising the following steps:
The graphite composite powder of raw metal powder and/or metal-plated membrane is mixed and is piled into sinter layer, so that the plating
There is the graphite composite powder of metal film to be in the preset position of the sinter layer with preset ratio；
Under inert gas protection the sinter layer is heated to being sintered using orientation field；
Accumulation sinter layer and successively sintering are repeated until material preparation is completed.
Preferably, the method for orienting doped graphite in a metal, the graphite composite powder of the metal-plated membrane are average
Partial size between 100 μm to 1000 μm, draw ratio between 20 to 80, metal-coated surface thickness 0.1 μm to 3 μm it
Between.
Preferably, the method for orienting doped graphite in a metal, graphite composite powder volume is less than in the sinter layer
Equal to 85%.
Preferably, the method for orienting doped graphite in a metal, the sinter layer, which contains or not contain, is coated with gold
Belong to the graphite composite powder of film；The graphite composite powder of metal-plated membrane described in the sinter layer of the graphite composite powder containing metal-plated membrane
Volume accounts for 20%-85%.
Preferably, the method for orienting doped graphite in a metal, the sinter layer thickness is in 40um-1000um.
Preferably, the method for orienting doped graphite in a metal, the raw metal powder and the graphite powder
The metal of the plated film in body surface face is referred to herein as requirement in terms of affinity, such as infiltration etc..
Preferably, it is described in a metal orient doped graphite method, the orientation field energy 70W- 700W it
Between.
Preferably, the method for orienting doped graphite in a metal, the orientation field are laser and/or microwave.
Preferably, the method for orienting doped graphite in a metal, described in the orientation field is scanned with pre-set velocity
Sinter layer, so that the sinter layer corresponding portion is sintered according to scan path；It is preferred that the sintered material in orientation field using pipe
Formula furnace is sintered.
Preferably, the method for orienting doped graphite in a metal, the raw metal powder are partial size in 1um-
Aluminium powder between 200um is sintered with a thickness of 40um-500um；The graphite composite powder ti coat on diamond of the metal-plated membrane, thickness exist
Between 0.1 μm to 3 μm, graphite composite powder average grain diameter is between 100 μm to 1000 μm, and draw ratio is between 20 to 80；
The orientation field is laser,
Field energy is oriented between 70W-700W.It is defeated in the location of raw metal powder spot diameter 0.2-20mm
Power 80W-500W out, scanning speed 50-100mm/s, sweep span: 0.08mm- 0.3mm；Metal film graphite composite powder and
The location of metal mixed spot diameter 0.5-40mm, output power 80W-650W W, scanning speed 0.2-10mm/s, scanning
Spacing 0.1mm-0.3mm.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, can obtain down and show
Beneficial effect:
The powdered graphite of metal powder and metal-plated membrane that increment is superimposed by the present invention makes metal using orientation field
The metal film Flashmelt of powder and powdered graphite is sintered to composite material, not only with the performance of high thermal conductivity, improves compound
The strength of materials, while meeting the demand to graphite-metal composite material complicated shape in varied situations.
Preferred embodiment has further advanced optimized the lattice of material using the method that tube furnace is sintered, and improves
Heating conduction, electric conductivity and the machining property of composite material.
Detailed description of the invention
Fig. 1 is the manufacturing process schematic diagram that the present invention prepares graphite-metal composite material；
Fig. 2 is the structural schematic diagram that the present invention prepares graphite-metal composite material；
Fig. 3 is the structural schematic diagram that the present invention prepares graphite-metal composite material；
Fig. 4 is the structural schematic diagram that the present invention prepares graphite-metal composite material.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below each other it
Between do not constitute conflict and can be combined with each other.
The method provided by the invention for orienting doped graphite in a metal, comprising the following steps:
The graphite composite powder of raw metal powder and/or metal-plated membrane is mixed and is piled into sinter layer, so that the plating
There is the graphite composite powder of metal film to be in the preset position of the sinter layer with preset ratio；The raw metal powder and the graphite
The metal of the plated film of powder surface.
The raw metal powder, partial size 1um-1000um, preferably its fusing point lower than 1600 DEG C, thermal conductance be more than 75W/
M.K, density is lower than 7.8g/cm3, intensity is more than the metal simple-substance or alloy of 60MPa, and preferable particle size 50um is 660 DEG C of fusing point, warm
The property led 240W/MK, density 2.7g/cm3, the aluminium of intensity 80MPa.The raw metal powder and the graphite composite powder surface
The metal of plated film mutually infiltrates.It is furthermore preferred that the metal energy of the raw metal powder and the plated film on the graphite composite powder surface
Alloy is formed, interphase is formed.
The graphite composite powder of the metal-plated membrane, average grain diameter between 100 μm to 1000 μm, draw ratio 20 to 80 it
Between, metal-coated surface thickness is between 0.1 μm to 3 μm.Such graphite composite powder have both good thermal conductivity and preferably
Mechanical strength.
Sinter layer thickness graphite composite powder volume in 40um-1000um, the sinter layer is less than or equal to 85%.Institute
State the graphite composite powder that sinter layer contains or not contain metal-plated membrane；The sinter layer of the graphite composite powder containing metal-plated membrane
Described in the graphite composite powder volume of metal-plated membrane account for 20%-85%.Sinter layer containing different proportion graphite composite powder can be successively
It is stitched together in stacking or horizontal direction in sintering vertical direction, forms preset anisotropic material；It is described not contain plating
There are the preferred 40um-500um of sinter layer thickness of the graphite composite powder of metal film, the preferred aluminium of material.
Under inert gas protection the sinter layer is heated to being sintered using orientation field；The orientation field energy 70W-
Between 700W, the orientation field is laser and/or microwave.The sinter layer is scanned with pre-set velocity in the orientation field, so that institute
Sinter layer corresponding portion is stated to be sintered according to scan path.
The sinter layer thickness should be matched with orientation field energy, and every layer of sinter layer can be with independent control ingredient, including metal
Powder type, metal-powder specification, graphite composite powder specification, the metal species specification of graphite composite powder plated film, therefore can be in difference
Spatial Dimension create composition proportion complexity graphite dopping metal, meet different performance requirements；It is orientable that field is oriented simultaneously
It is sintered sinter layer, prepares the composite material of complicated shape in sinter layer according to scan path.In summary two o'clock can be certainly
By the graphite dopping metal material for preparing shape and complicated component.The premise for realizing above-mentioned technology is the tool on graphite composite powder surface
Have metal coating, as long as therefore graphite surface metal and metal-powder molten sintering can form stable doping, it is sintered
Journey is metal-metal reaction, is different from metal-graphite and reacts, therefore mixed powder can be burnt rapidly under conditions of load orients field
Form type.
It is preferred that raw metal powder is aluminium powder, copper powder, iron or iron alloy powder, silver powder, and/or titanium valve, the graphite composite powder
Surface coating is copper, nickel or titanium film；It is furthermore preferred that the raw metal powder is aluminium powder, the graphite composite powder ti coat on diamond
Film, wherein titanium can improve the intensity of graphite flake, and strong chemical bonding can be formed with graphite by generating TiC with graphite, avoid
Graphite directly generates crisp phase Al with aluminium4C3, while titanium and aluminium generate alloy, interfacial contact is close.
Accumulation sinter layer and successively sintering are repeated until material preparation is completed.
It is preferred that above-mentioned material is carried out hot pressed sintering in hot pressing furnace.
The following are embodiments:
Embodiment 1:
The raw metal powder, the raw metal powder be partial size 50um, 660 DEG C of fusing point, thermal conductance 240W/MK,
The aluminum metal powder of density 2.7g/cm3, intensity 80MPa.
The graphite composite powder of the metal-plated membrane, average grain diameter is at 500 μm, draw ratio 30, and metal-coated surface is thick
Spend the graphite composite powder at 0.2 μm.The metal classification of metal film, the preparation process of plated film
The sinter layer thickness accounts for 55% in 50um, graphite composite powder volume
Under inert gas protection the sinter layer is heated to being sintered using orientation field；The orientation field be laser and/
Or microwave.
Raw metal layer: spot diameter 0.2mm, output power 100W, scanning speed 100mm/s, sweep span: 0.1mm.
Graphite and metal mixed layer: spot diameter 0.8mm, output power 80W, scanning speed 2mm/s, sweep span 0.25mm.
A kind of preparation of graphite (titanizing)-aluminium composite material
Step 1: flaky graphite powder, calcium chloride, titanium valve that partial size is 500um is taken to be uniformly mixed and mixed-powder is made, press
Mixed-powder total weight calculates, and sodium chloride accounts for 40%, and titanium valve accounts for 20%, and mixed-powder is put into vacuum tube furnace, vacuumizes
It is about 10-220Pa to vacuum degree, heating rate is 15 DEG C/min, is warming up to 1300 DEG C, keeps the temperature 100min, then furnace cooling
To room temperature.The mixed-powder that high-temperature process is crossed takes out, and is put into the beaker equipped with deionized water, will be equipped with mixed powder after processing
The beaker of end and deionized water is put into drying box, 85 DEG C of set temperature, keeps the temperature 30min, takes out beaker and outwells the water of sodium chloride
Solution is re-poured into deionized water and repeats above operation, and cleans 5 times to mixed-powder, the mixing after cleaning is finished and dried
Powder crosses 30 meshes respectively, removes superfluous silicon powder.
It is put into container A step 2: taking out and depositing aluminium powder.
Step 3: seeing that the graphite flake of first step plated film completion and aluminium powder are put into container B.
Step 4: being first uniformly laid in aluminium powder on substrate from container A, its sintering is made using laser, forms metal
Layer；The powdered graphite of container B and metal mixed powder are spread out on the metal being sintered again later, burnt using laser
Knot, repeats the above process to required thickness, finally re-sinters one layer of aluminium layer, can increase its hardness, forms metal layer-graphite linings
It is alternately present and the last layer is the laminate structure high-heat-conductive composite material (such as Fig. 2) of aluminium.The atmosphere in entire manufacturing process
For in argon atmosphere lamp protective atmosphere.
It such as needs to increase its thermal conductivity, the composite material of above-mentioned preparation can be placed in hot pressing furnace, wherein hot pressing furnace
Pressure be 40-60MPa, suction is about 10-220Pa, and heating rate is 15 DEG C/min, is warming up to 850-1050 DEG C, is protected
Warm 20-120min is sintered.Then sample is taken out after natural cooling.
Embodiment 2:
The raw metal powder, the raw metal powder be partial size 500um, 1500 DEG C of fusing point, thermal conductance 75W/MK,
Density 7.8g/cm3, intensity 170MPa metallic iron powder.
The graphite composite powder of the metal-plated membrane, average grain diameter is at 200 μm, and for draw ratio 50, metal-coated surface is thick
Spend the graphite composite powder at 2 μm.
The sinter layer thickness accounts for 70% in 200um, graphite composite powder volume.
Under inert gas protection the sinter layer is heated to being sintered using orientation field；The orientation field be laser and/
Or microwave.
Raw metal layer: spot diameter 20mm, output power 400W, scanning speed 60mm/s, sweep span: 0.1mm. stone
Ink and metal mixed layer: spot diameter 33mm, output power 600W, scanning speed 0.3mm/s, sweep span 0.2mm.
A kind of preparation of graphite (copper facing)-iron composite material
Step 1: taking partial size is the flaky graphite powder of 200um.First graphite powder is impregnated with the NaOH solution of 200g/L
40min degreasing, is then washed to neutrality；Again with the HNO of 20% (volume ratio of concentrated nitric acid and water is 1:4).Solution boils 15~
Then 20min is washed to neutrality, dry at 100 DEG C.8g CuSO is added in 800mL distilled water4·5H2O the and 15mL concentrated sulfuric acid
It is configured to electroplate liquid, 5g graphite powder is added, control current density is 9A/dm2, time 80min, and every 10min stirs 1min.
After plating, it is washed to neutrality, is passivated with 0.5% benzotriazole (BTA) as passivator, 55 DEG C of temperature, the time
5min is dried at 100 DEG C.Obtain the graphite powder for being coated with copper.
It is put into container A step 2: taking out iron deposit powder
Step 3: seeing that the graphite flake of first step plated film completion and iron powder are put into container B
Step 4: being first laid in iron powder on substrate according to the track of setting from container A, its sintering is made using laser,
Form metal layer；The powdered graphite of container B and metal mixed powder are spread out according to the track of setting again later, using laser into
Row sintering repeats the above process to required thickness, forms laminate structure high-heat-conductive composite material such as Fig. 3.It was manufactured entirely
Atmosphere is in argon atmosphere lamp protective atmosphere in journey.
It such as needs to increase its thermal conductivity, the composite material of above-mentioned preparation can be placed in hot pressing furnace, wherein hot pressing furnace
Pressure be 40-60MPa, suction is about 10-220Pa, and heating rate is 15 DEG C/min, is warming up to 850-1050 DEG C, is protected
Warm 20-120min is sintered.Then sample is taken out after natural cooling.
Embodiment 3:
The raw metal powder, the raw metal powder, partial size 800um, 1000 DEG C of fusing point, thermal conductance 397W/MK,
The metallic copper powder of density 8.9g/cm3, intensity 220MPa.
The graphite composite powder of the metal-plated membrane, average grain diameter is at 800 μm, and for draw ratio 70, metal-coated surface is thick
Degree is between 2.5 μm.
The sinter layer thickness accounts for 80% in 900um, graphite composite powder volume
Under inert gas protection the sinter layer is heated to being sintered using orientation field；The orientation field be laser and/
Or microwave.
Raw metal layer: spot diameter 20mm, output power 400W, scanning speed 60mm/s, sweep span: 0.1mm. stone
Ink and metal mixed layer: spot diameter 0.8mm, output power 150W, scanning speed 3mm/s, sweep span 0.15mm
A kind of preparation of graphite (titanizing)-carbon/carbon-copper composite material
Step 1: flaky graphite powder, calcium chloride, titanium valve that partial size is 800um is taken to be uniformly mixed and mixed-powder is made, press
Mixed-powder total weight calculates, and sodium chloride accounts for 40%, and titanium valve accounts for 30%, and mixed-powder is put into vacuum tube furnace, vacuumizes
It is about 10-220Pa to vacuum degree, heating rate is 15 DEG C/min, is warming up to 1300 DEG C, keeps the temperature 100min, then furnace cooling
To room temperature.The mixed-powder that high-temperature process is crossed takes out, and is put into the beaker equipped with deionized water, will be equipped with mixed powder after processing
The beaker of end and deionized water is put into drying box, 85 DEG C of set temperature, keeps the temperature 30min, takes out beaker and outwells the water of sodium chloride
Solution is re-poured into deionized water and repeats above operation, and cleans 5 times to mixed-powder, the mixing after cleaning is finished and dried
Powder crosses 30 meshes respectively, removes superfluous silicon powder.
It is put into container A step 2: taking out and depositing copper powder
Step 3: seeing that the graphite flake of first step plated film completion and copper powder are put into container B
Step 4: first copper powder is uniformly laid on substrate according to the position of setting from container A, later again by container
The powdered graphite and metal mixed powder of B is uniformly spread out according to the position of setting, is sintered using laser, and above-mentioned mistake is repeated
Journey is to required thickness such as Fig. 4.Atmosphere is in argon atmosphere lamp protective atmosphere in entire manufacturing process.
It such as needs to increase its thermal conductivity, the composite material of above-mentioned preparation can be placed in hot pressing furnace, wherein hot pressing furnace
Pressure be 40-60MPa, suction is about 10-220Pa, and heating rate is 15 DEG C/min, is warming up to 850-1050 DEG C, is protected
Warm 20-120min is sintered.Then sample is taken out after natural cooling.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of method for orienting doped graphite in a metal, which comprises the following steps:
The graphite composite powder of raw metal powder and/or metal-plated membrane is mixed and is piled into sinter layer, so that described be coated with gold
The graphite composite powder for belonging to film is in the preset position of the sinter layer with preset ratio；
Under inert gas protection the sinter layer is heated to being sintered using orientation field；
Accumulation sinter layer and successively sintering are repeated until material preparation is completed.
2. orienting the method for doped graphite in a metal as described in claim 1, which is characterized in that the metal-plated membrane
Graphite composite powder, average grain diameter is between 100 μm to 1000 μm, and between 20 to 80, metal-coated surface thickness exists draw ratio
Between 0.1 μm to 3 μm.
3. orienting the method for doped graphite in a metal as described in claim 1, which is characterized in that graphite in the sinter layer
Powder volume is less than or equal to 85%.
4. as described in claim 1 in a metal orient doped graphite method, which is characterized in that the sinter layer contain or
Graphite composite powder without containing metal-plated membrane；Metal is coated with described in the sinter layer of the graphite composite powder containing metal-plated membrane
The graphite composite powder volume of film accounts for 20%-85%.
5. orienting the method for doped graphite in a metal as described in claim 1, which is characterized in that the sinter layer thickness exists
40um-1000um。
6. orienting the method for doped graphite in a metal as described in claim 1, which is characterized in that the raw metal powder
Alloy can be formed with the metal of the plated film on the graphite composite powder surface.
7. orienting the method for doped graphite in a metal as described in claim 1, which is characterized in that the orientation field energy exists
Between 70W-700W.
8. orienting the method for doped graphite in a metal as claimed in claim 5, which is characterized in that the orientation field is laser
And/or microwave.
9. orienting the method for doped graphite in a metal as claimed in claim 5, which is characterized in that the orientation field is with default
Sinter layer described in velocity scanning, so that the sinter layer corresponding portion is sintered according to scan path；It is preferred that after to the sintering of orientation field
Material be sintered using tube furnace.
10. orienting the method for doped graphite in a metal as described in claim 1, which is characterized in that the raw metal powder
Body is aluminium powder of the partial size between 1um-200um, is sintered with a thickness of 40um-500um；The graphite powder body surface of the metal-plated membrane
Face titanizing, nickel and/or copper, for thickness between 0.1 μm to 3 μm, graphite composite powder average grain diameter is long between 100 μm to 1000 μm
Diameter ratio is between 20 to 80；
The orientation field is laser, orients field energy between 70W-700W.It is straight in the location of raw metal powder hot spot
Diameter 0.2-20mm, output power 80W-500W, scanning speed 50-100mm/s, sweep span: 0.08mm-0.3mm；In metal film
Graphite composite powder and the location of metal mixed spot diameter 0.5-40mm, output power 80W-650W W, scanning speed
0.2-10mm/s, sweep span 0.1mm-0.3mm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111069611A (en) * | 2019-12-23 | 2020-04-28 | 长飞光纤光缆股份有限公司 | Preparation method of graphite-graphene-metal composite material |
| CN112157965A (en) * | 2020-09-30 | 2021-01-01 | 长飞光纤光缆股份有限公司 | Graphite-metal composite material and preparation method thereof |
| CN114369739A (en) * | 2021-12-14 | 2022-04-19 | 江西理工大学 | Preparation method and device of lead-free graphite brass composite material |
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