CN104014921A - Method for rapidly preparing copper-molybdenum multi-layer composite material - Google Patents
Method for rapidly preparing copper-molybdenum multi-layer composite material Download PDFInfo
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- CN104014921A CN104014921A CN201410172037.2A CN201410172037A CN104014921A CN 104014921 A CN104014921 A CN 104014921A CN 201410172037 A CN201410172037 A CN 201410172037A CN 104014921 A CN104014921 A CN 104014921A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/02—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by means of a press ; Diffusion bonding
- B23K20/023—Thermo-compression bonding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/14—Preventing or minimising gas access, or using protective gases or vacuum during welding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/22—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating taking account of the properties of the materials to be welded
- B23K20/233—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating taking account of the properties of the materials to be welded without ferrous layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/24—Preliminary treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/18—Dissimilar materials
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Abstract
The invention discloses a method for rapidly preparing a copper-molybdenum multi-layer composite material. The method comprises the following steps that (1) the surfaces of copper pieces and the surfaces of molybdenum pieces are polished so that oxidation films can be removed, the polished copper pieces and the polished molybdenum pieces are washed through acetone, and the processed copper pieces and the processed molybdenum pieces are dried by cold air for later use; (2) the copper pieces and the molybdenum pieces are overlaid in an alternating mode so that a multi-layer structural plate can be formed and the multi-layer structural plate is placed in a combination mold; (3) the combination mold containing the multi-layer structural plate is placed in a plasma activation sintering furnace, demolding is conducted after sintering is conducted, and therefore the copper-molybdenum multi-layer composite material is obtained. Electrifying, heating and sintering are directly conducted on the multi-layer structural plate obtained by overlaying the copper pieces and the molybdenum pieces in the alternating mode by introducing a high-density current, rapid diffusion bonding of copper-molybdenum interfaces is achieved under the combination action of temperature and pressure, the copper-molybdenum multi-layer composite material prepared with the method is good in heat conductivity and thermal expansion coefficient, the bonding strength of the copper-molybdenum interfaces is high, the product consistency is good, and punch forming can be achieved.
Description
Technical field
The invention belongs to electronic package material technical field, be specifically related to a kind of method of preparing fast copper molybdenum multilayer materials.
Background technology
Along with the fast development of electronic information technology, semiconductor devices is constantly to the future development of high power, high integration, portability, and operating temperature constantly raises.If can not dispel the heat in time during device work, can cause performance degradation, the lost of life.Finding good electronic package material, is the important channel that solves high-power component heat dissipation problem, significant for performance, reliability and the service life of improving device.Electronic Packaging and heat sink material not only will have high thermal conductivity, and need to have the thermal coefficient of expansion matching with chip material, to avoid device be out of shape or damage because thermal strain mismatch causes in encapsulation or use procedure.Homogenous material is difficult to meet above-mentioned requirements simultaneously, and Cu/Mo/Cu laminar composite has the high-termal conductivity of Cu and the low heat expansion of Mo concurrently, and performance is adjustable, is the high-power component electronic package material that has competitiveness.
At present Cu/Mo/Cu laminar composite be take " sandwich " structure of three layers as main, and preparation method mainly contains rolling, explosion method, pressure sintering and cladding method etc.Rolling is the preparation method who is seen in the earliest report, and US Patent No. 4950554 adopts welding rolling to obtain the Cu/Mo/Cu laminar composite of " sandwich " structure the earliest; Chinese patent CN102357525 and CN1850436 adopt respectively hot rolling and cold-rolling practice to prepare Cu/Mo/Cu laminar composite; The major defect that rolling exists is that Cu and Mo are immiscible, after mill-annealed, copper molybdenum interface is mainly with the combination of mechanical engagement mode, and interface bond strength is not high, if will improve interface bond strength, must improve roll-force, but easily cause the Mo that fragility own is large to occur cracking or layering; In patent CN102371719, adopt the Cu/Mo/Cu laminar composite of blast rolling preparation " sandwich " structure, but in the technical scheme of this patent, processing step is more, and there is higher risk and noise pollution in blast composite algorithm itself, and plate shape is controlled difficulty, be unsuitable for producing continuously and to control of product quality; Patent CN1850436 adopts pressure sintering to prepare Cu/Mo laminar composite, first at Mo plate surface preplating Cu layer, then the Mo plate of plating Cu is rolled to shaping, and then, with the superimposed hot pressed sintering that carries out of Cu plate, this method technique is loaded down with trivial details, and electroplates easy contaminated environment; Patent CN1408485 adopts the Cu/Mo/Cu laminar composite of method preparation " sandwich " structure of cladding Cu layer on Mo plate, but Cu needs cold rolling shaping after cooling, the more difficult control of surface quality and bed thickness, and limited while preparing large bed thickness than composite.
Summary of the invention
Technical problem to be solved by this invention is, for above-mentioned deficiency of the prior art, to provide a kind of method of preparing fast copper molybdenum multilayer materials.The method is by the double-layer structure panel of introducing high-density current and directly the laying that is superimposed by copper sheet and molybdenum sheet the being obtained heat-agglomerating of switching on, the rapid diffusion that realizes copper molybdenum interface under the synergy of temperature and pressure connects, thereby provide a kind of operation copper molybdenum multi-layer composite materials preparation method for material simple, with short production cycle, the copper molybdenum multilayer materials that preparation technology of the present invention produces has good thermal conductivity and thermal coefficient of expansion, copper molybdenum interface bond strength is high, good product consistency, and can punch forming.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of method of preparing fast copper molybdenum multilayer materials, it is characterized in that, and the method comprises the following steps:
Step 1, grinding process is carried out to remove oxide-film in the surface of copper sheet and molybdenum sheet, then with acetone, clean copper sheet and the molybdenum sheet after polishing, cold wind dries up standby; The thickness of single described copper sheet is 0.1mm～0.65mm, and the thickness of single molybdenum sheet is 0.24mm～1.8mm;
Step 2, by the copper sheet after cleaning in step 1 and the molybdenum sheet laying that is superimposed, obtain double-layer structure panel, then described double-layer structure panel is put into assembling die; The number of plies of described double-layer structure panel is at least three layers, the outermost layer of described double-layer structure panel is copper sheet, described assembling die comprises the graphite external mold of hollow structure, the upper end of graphite external mold is provided with seaming chuck, the lower end of graphite external mold is provided with push-down head, the die cavity that is formed for placement of multiple layers structural slab between described seaming chuck, push-down head and graphite external mold inwall, the shape and size of die cavity all match with the shape and size of described double-layer structure panel;
Step 3, the assembling die that double-layer structure panel is housed in step 2 is put into plasma activated sintering stove, the vacuum that regulates described plasma activated sintering stove is 5Pa～15Pa, and current density is 300A/cm
2～500A/cm
2axial compressive force is 50MPa～100MPa, in sintering temperature, be under the condition of 800 ℃～1000 ℃ by double-layer structure panel sintering processes 10min～17min, after the temperature in plasma activated sintering stove is down to room temperature, remove axial compressive force, after the demoulding, obtain copper molybdenum multilayer materials.
A kind of above-mentioned method of preparing fast copper molybdenum multilayer materials, is characterized in that, the number of plies described in step 2 is 3～15 layers.
A kind of above-mentioned method of preparing fast copper molybdenum multilayer materials, is characterized in that, described in step 2, in double-layer structure panel, the volumn concentration of molybdenum is 40%～60%.
A kind of above-mentioned method of preparing fast copper molybdenum multilayer materials, it is characterized in that, in described double-layer structure panel, the thickness of copper sheet used all equates, the thickness of molybdenum sheet used is all equal, and the Thickness Ratio of single described copper sheet and single described molybdenum sheet is 1:(1～3).
A kind of above-mentioned method of preparing fast copper molybdenum multilayer materials, is characterized in that, seaming chuck described in step 2 and push-down head are made by carbofrax material.
A kind of above-mentioned method of preparing fast copper molybdenum multilayer materials, is characterized in that, vacuum described in step 3 is 8Pa～12Pa, and described current density is 380A/cm
2～450A/cm
2, described axial compressive force is 75MPa～100MPa, and described sintering temperature is 900 ℃～1000 ℃, and described sintering time is 12min～15min.
A kind of above-mentioned method of preparing fast copper molybdenum multilayer materials, is characterized in that, described vacuum is 10Pa, and current density is 450A/cm
2, axial compressive force is 100MPa, and sintering temperature is 950 ℃, and sintering time is 15min.
The present invention compared with prior art has the following advantages:
1, the present invention is by the double-layer structure panel of introducing high-density current and directly the laying that is superimposed by copper sheet and molybdenum sheet the being obtained heat-agglomerating of switching on, the rapid diffusion that realizes copper molybdenum interface under the synergy of temperature and pressure connects, thereby provide a kind of operation copper molybdenum multi-layer composite materials preparation method for material simple, with short production cycle, the copper molybdenum multilayer materials that preparation technology of the present invention produces has good thermal conductivity and thermal coefficient of expansion, copper molybdenum interface bond strength is high, good product consistency, and can punch forming.
2, preparation technology of the present invention is by directly to the heat-agglomerating of switching on of copper sheet to be composite and molybdenum sheet, the atom that is used for improving copper molybdenum interface that utilizes high-density current is mixed degree mutually, firing rate is exceedingly fast, can accelerate the physical contact processes such as the plastic deformation on copper sheet and molybdenum sheet surface and creep, shorten Material cladding connection procedure, electric current can promote copper molybdenum interface atom mixed mutually simultaneously, strengthens the combination of copper molybdenum metallurgical interface, to obtain the copper molybdenum laminar composite of high interfacial strength.
3, in preparation technology of the present invention by changing size, thickness and both numbers of plies that is superimposed of copper sheet and molybdenum sheet, can in a big way, regulate and control thermal conductivity and the thermal coefficient of expansion of copper molybdenum laminar composite, by increasing the molybdenum sheet number of plies, reducing molybdenum sheet thickness, can give full play to the thermal expansion effect of contraction of Mo layer to Cu layer, reduce the volumn concentration of Mo layer, thereby improve composite thermal conductivity, reduce product density and cost.
4, the preparation technology of copper molybdenum laminar composite of the present invention is one-shot forming, and this technical process is simple, and the product size scope preparing is large, high conformity, and thickness in monolayer is little, can carry out punch forming.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the structural representation of assembling die of the present invention.
Fig. 2 is the SEM photo at copper molybdenum interface in the copper molybdenum multilayer materials of the embodiment of the present invention 1 preparation.
Fig. 3 is the element distribution EDS line sweep figure at copper molybdenum interface in the copper molybdenum multilayer materials of the embodiment of the present invention 1 preparation.
Fig. 4 is the be superimposed structural representation of laying of copper sheet and molybdenum sheet in the embodiment of the present invention 2.
Description of reference numerals:
1-graphite external mold; 2-seaming chuck; 3-push-down head;
4-die cavity; 5-copper sheet; 6-molybdenum sheet.
The specific embodiment
In various embodiments of the present invention, plasma activated sintering stove used is that the model that Japanese Elenix company produces is the plasma activated sintering stove of ED-PAS III.
Embodiment 1
Step 1, with sand paper, respectively grinding process is carried out to remove oxide-film in the surface of 8 copper sheets and 7 molybdenum sheets, then with acetone, clean copper sheet and the molybdenum sheet after polishing, cold wind dries up standby; The thickness of 8 described copper sheets is respectively 0.25mm, 0.2mm, 0.1mm, 0.1mm, 0.1mm, 0.1mm, 0.2mm and 0.25mm, and the thickness of 7 described molybdenum sheets is respectively 0.3mm, 0.24mm, 0.24mm, 0.24mm, 0.24mm, 0.24mm and 0.3mm;
Step 2, by the copper sheet after cleaning in step 1 and the molybdenum sheet laying that is superimposed, obtain double-layer structure panel, then described double-layer structure panel is put into assembling die; The number of plies of described double-layer structure panel is 15 layers, the outermost layer of described double-layer structure panel is copper sheet, the order that is superimposed during according to laying, in double-layer structure panel, the thickness of copper sheet and molybdenum sheet is followed successively by 0.25mm, 0.3mm, 0.2mm, 0.24mm, 0.1mm, 0.24mm, 0.1mm, 0.24mm, 0.1mm, 0.24mm, 0.1mm, 0.24mm, 0.2mm, 0.3mm and 0.25mm, and described copper sheet and described molybdenum sheet are the disk that diameter is 60mm; As shown in Figure 1, assembling die comprises the graphite external mold 1 of hollow structure, the upper end of graphite external mold 1 is provided with seaming chuck 2, the lower end of graphite external mold 1 is provided with push-down head 3, between described seaming chuck 2, push-down head 3 and graphite external mold 1 inwall, be formed for the die cavity 4 of placement of multiple layers structural slab, the shape and size of die cavity 4 all match with the shape and size of described double-layer structure panel, and seaming chuck 2 and push-down head 3 are made by carbofrax material;
Step 3, the assembling die that double-layer structure panel is housed in step 2 is put into plasma activated sintering stove, the vacuum that regulates described plasma activated sintering stove is 10Pa, and current density is 450A/cm
2, axial compressive force is 100MPa, in sintering temperature, be under the condition of 950 ℃ by double-layer structure panel sintering processes 15min, after the temperature in plasma activated sintering stove is down to room temperature, remove axial compressive force, after the demoulding, obtain copper molybdenum multilayer materials.
Fig. 2 is the SEM photo at copper molybdenum interface in the copper molybdenum multilayer materials prepared of the present embodiment.As seen from Figure 2, in copper molybdenum multilayer materials prepared by the present embodiment, copper molybdenum interface is more straight, without obviously hole generation.
Fig. 3 is copper molybdenum interface element distribution EDS line sweep figure in the copper molybdenum multilayer materials prepared of the present embodiment.As seen from Figure 3, copper molybdenum interface in copper molybdenum multilayer materials prepared by the present embodiment is that width is the mutually mixed interface of 3 μ m～4 μ m, wherein the atomicity percentage composition of copper reaches 3.8%, much larger than limit solid solubility corresponding to Cu-Mo phasor, what this explanation effect by the present embodiment middle-high density electric current can promote copper molybdenum interface atom sneaks out journey mutually, improve the mutually mixed degree of copper molybdenum interface atom, thereby improve the bond strength at copper molybdenum interface.
In copper molybdenum multilayer materials prepared by the present embodiment, the volumn concentration of molybdenum is 58.1%, and perpendicular layers direction thermal conductivity is 221W/mk, and thermal coefficient of expansion is 8.79 * 10
-6k
-1, peel strength is 70.12N/cm.
Embodiment 2
Step 1, with sand paper, respectively grinding process is carried out to remove oxide-film in the surface of 5 copper sheets and 4 molybdenum sheets, then with acetone, clean copper sheet and the molybdenum sheet after polishing, cold wind dries up standby; The thickness of single described copper sheet and single described molybdenum sheet is 0.3mm;
Step 2, by the copper sheet after cleaning in step 1 and the molybdenum sheet laying that is superimposed, obtain double-layer structure panel, then described double-layer structure panel is put into assembling die; The number of plies of described double-layer structure panel is 9 layers, and the outermost layer of described double-layer structure panel is copper sheet, and described copper sheet and described molybdenum sheet are the disk that diameter is 50mm; As shown in Figure 1, assembling die comprises the graphite external mold 1 of hollow structure, the upper end of graphite external mold 1 is provided with seaming chuck 2, the lower end of graphite external mold 1 is provided with push-down head 3, between described seaming chuck 2, push-down head 3 and graphite external mold 1 inwall, be formed for the die cavity 4 of placement of multiple layers structural slab, the shape and size of die cavity 4 all match with the shape and size of described double-layer structure panel, and seaming chuck 2 and push-down head 3 are made by carbofrax material;
Step 3, the assembling die that double-layer structure panel is housed in step 2 is put into plasma activated sintering stove, the vacuum that regulates described plasma activated sintering stove is 12Pa, and current density is 380A/cm
2, axial compressive force is 75MPa, in sintering temperature, be under the condition of 950 ℃ by double-layer structure panel sintering processes 15min, after the temperature in plasma activated sintering stove is down to room temperature, remove axial compressive force, after the demoulding, obtain copper molybdenum multilayer materials, structure is as shown in Figure 4.
In copper molybdenum multilayer materials prepared by the present embodiment, the volumn concentration of molybdenum is 44.4%, and perpendicular layers direction thermal conductivity is 193W/mk, and thermal coefficient of expansion is 6.43 * 10
-6k
-1, peel strength is 67.18N/cm.
Embodiment 3
Step 1, with sand paper, respectively grinding process is carried out to remove oxide-film in the surface of 5 copper sheets and 4 molybdenum sheets, then with acetone, clean copper sheet and the molybdenum sheet after polishing, cold wind dries up standby; The thickness of single described copper sheet is 0.3mm, and the thickness of single described molybdenum sheet is 0.375mm;
Step 2, by the copper sheet after cleaning in step 1 and the molybdenum sheet laying that is superimposed, obtain double-layer structure panel, then described double-layer structure panel is put into assembling die; The number of plies of described double-layer structure panel is 9 layers, and the outermost layer of described double-layer structure panel is copper sheet, and described copper sheet and described molybdenum sheet are the disk that diameter is 40mm; As shown in Figure 1, assembling die comprises the graphite external mold 1 of hollow structure, the upper end of graphite external mold 1 is provided with seaming chuck 2, the lower end of graphite external mold 1 is provided with push-down head 3, between described seaming chuck 2, push-down head 3 and graphite external mold 1 inwall, be formed for the die cavity 4 of placement of multiple layers structural slab, the shape and size of die cavity 4 all match with the shape and size of described double-layer structure panel, and seaming chuck 2 and push-down head 3 are made by carbofrax material;
Step 3, the assembling die that double-layer structure panel is housed in step 2 is put into plasma activated sintering stove, the vacuum that regulates described plasma activated sintering stove is 15Pa, and current density is 300A/cm
2, axial compressive force is 50MPa, in sintering temperature, be under the condition of 800 ℃ by double-layer structure panel sintering processes 17min, after the temperature in plasma activated sintering stove is down to room temperature, remove axial compressive force, after the demoulding, obtain copper molybdenum multilayer materials.
In copper molybdenum multilayer materials prepared by the present embodiment, the volumn concentration of molybdenum is 50.0%, and perpendicular layers direction thermal conductivity is 202W/mk, and thermal coefficient of expansion is 6.72 * 10
-6k
-1, peel strength is 67.34N/cm.
Embodiment 4
Step 1, with sand paper, respectively grinding process is carried out to remove oxide-film in the surface of 5 copper sheets and 4 molybdenum sheets, then with acetone, clean copper sheet and the molybdenum sheet after polishing, cold wind dries up standby; The thickness of single described copper sheet is 0.26mm, and the thickness of single described molybdenum sheet is 0.45mm;
Step 2, by the copper sheet after cleaning in step 1 and the molybdenum sheet laying that is superimposed, obtain double-layer structure panel, then described double-layer structure panel is put into assembling die; The number of plies of described double-layer structure panel is 9 layers, and the outermost layer of described double-layer structure panel is copper sheet, and described copper sheet and described molybdenum sheet are the disk that diameter is 20mm; As shown in Figure 1, assembling die comprises the graphite external mold 1 of hollow structure, the upper end of graphite external mold 1 is provided with seaming chuck 2, the lower end of graphite external mold 1 is provided with push-down head 3, between described seaming chuck 2, push-down head 3 and graphite external mold 1 inwall, be formed for the die cavity 4 of placement of multiple layers structural slab, the shape and size of die cavity 4 all match with the shape and size of described double-layer structure panel, and seaming chuck 2 and push-down head 3 are made by carbofrax material;
Step 3, the assembling die that double-layer structure panel is housed in step 2 is put into plasma activated sintering stove, the vacuum that regulates described plasma activated sintering stove is 8Pa, and current density is 450A/cm
2, axial compressive force is 85MPa, in sintering temperature, be under the condition of 900 ℃ by double-layer structure panel sintering processes 12min, after the temperature in plasma activated sintering stove is down to room temperature, remove axial compressive force, after the demoulding, obtain copper molybdenum multilayer materials.
In copper molybdenum multilayer materials prepared by the present embodiment, the volumn concentration of molybdenum is 58.1%, and perpendicular layers direction thermal conductivity is 212W/mk, and thermal coefficient of expansion is 8.09 * 10
-6k
-1, peel strength is 68.90N/cm.
Embodiment 5
Step 1, with sand paper, respectively grinding process is carried out to remove oxide-film in the surface of 2 copper sheets and 1 molybdenum sheet, then with acetone, clean copper sheet and the molybdenum sheet after polishing, cold wind dries up standby; The thickness of single described copper sheet is 0.65mm, and the thickness of described molybdenum sheet is 1.8mm;
Step 2, by the copper sheet after cleaning in step 1 and the molybdenum sheet laying that is superimposed, obtain double-layer structure panel, then described double-layer structure panel is put into assembling die; The number of plies of described double-layer structure panel is 3 layers, and the outermost layer of described double-layer structure panel is copper sheet, and described copper sheet and described molybdenum sheet are the disk that diameter is 5mm; As shown in Figure 1, assembling die comprises the graphite external mold 1 of hollow structure, the upper end of graphite external mold 1 is provided with seaming chuck 2, the lower end of graphite external mold 1 is provided with push-down head 3, between described seaming chuck 2, push-down head 3 and graphite external mold 1 inwall, be formed for the die cavity 4 of placement of multiple layers structural slab, the shape and size of die cavity 4 all match with the shape and size of described double-layer structure panel, and seaming chuck 2 and push-down head 3 are made by carbofrax material;
Step 3, the assembling die that double-layer structure panel is housed in step 2 is put into plasma activated sintering stove, the vacuum that regulates described plasma activated sintering stove is 5Pa, and current density is 500A/cm
2, axial compressive force is 75MPa, in sintering temperature, be under the condition of 1000 ℃ by double-layer structure panel sintering processes 10min, after the temperature in plasma activated sintering stove is down to room temperature, remove axial compressive force, after the demoulding, obtain copper molybdenum multilayer materials.
In copper molybdenum multilayer materials prepared by the present embodiment, the volumn concentration of molybdenum is 58.1%, and perpendicular layers direction thermal conductivity is 219W/mk, and thermal coefficient of expansion is 7.11 * 10
-6k
-1, peel strength is 65.53N/cm.
Embodiment 6
Step 1, with sand paper, respectively grinding process is carried out to remove oxide-film in the surface of 3 copper sheets and 2 molybdenum sheets, then with acetone, clean copper sheet and the molybdenum sheet after polishing, cold wind dries up standby; The thickness of 3 described copper sheets is respectively 0.8mm, 0.1mm and 0.3mm, and the thickness of 2 described molybdenum sheets is respectively 0.3mm and 0.5mm;
Step 2, by the copper sheet after cleaning in step 1 and the molybdenum sheet laying that is superimposed, obtain double-layer structure panel, then described double-layer structure panel is put into assembling die; The number of plies of described double-layer structure panel is 5 layers, the outermost layer of described double-layer structure panel is copper sheet, the order that is superimposed during according to laying, in double-layer structure panel, the thickness of copper sheet and molybdenum sheet is followed successively by 0.8mm, 0.3mm, 0.1mm, 0.5mm and 0.3mm, and described copper sheet and described molybdenum sheet are the disk that diameter is 30mm; As shown in Figure 1, assembling die comprises the graphite external mold 1 of hollow structure, the upper end of graphite external mold 1 is provided with seaming chuck 2, the lower end of graphite external mold 1 is provided with push-down head 3, between described seaming chuck 2, push-down head 3 and graphite external mold 1 inwall, be formed for the die cavity 4 of placement of multiple layers structural slab, the shape and size of die cavity 4 all match with the shape and size of described double-layer structure panel, and seaming chuck 2 and push-down head 3 are made by carbofrax material;
Step 3, the assembling die that double-layer structure panel is housed in step 2 is put into plasma activated sintering stove, the vacuum that regulates described plasma activated sintering stove is 7Pa, and current density is 480A/cm
2, axial compressive force is 90MPa, in sintering temperature, be under the condition of 980 ℃ by double-layer structure panel sintering processes 16min, after the temperature in plasma activated sintering stove is down to room temperature, remove axial compressive force, after the demoulding, obtain copper molybdenum multilayer materials.
In copper molybdenum multilayer materials prepared by the present embodiment, the volumn concentration of molybdenum is 40%, and perpendicular layers direction thermal conductivity is 220W/mk, and thermal coefficient of expansion is 7.02 * 10
-6k
-1, peel strength is 69.50N/cm.
Embodiment 7
Step 1, with sand paper, respectively grinding process is carried out to remove oxide-film in the surface of 2 copper sheets and 1 molybdenum sheet, then with acetone, clean copper sheet and the molybdenum sheet after polishing, cold wind dries up standby; The thickness of single described copper sheet is 0.3mm, and the thickness of described molybdenum sheet is 0.9mm;
Step 2, by the copper sheet after cleaning in step 1 and the molybdenum sheet laying that is superimposed, obtain double-layer structure panel, then described double-layer structure panel is put into assembling die; The number of plies of described double-layer structure panel is 3 layers, and the outermost layer of described double-layer structure panel is copper sheet, and described copper sheet and described molybdenum sheet are the disk that diameter is 25mm; As shown in Figure 1, assembling die comprises the graphite external mold 1 of hollow structure, the upper end of graphite external mold 1 is provided with seaming chuck 2, the lower end of graphite external mold 1 is provided with push-down head 3, between described seaming chuck 2, push-down head 3 and graphite external mold 1 inwall, be formed for the die cavity 4 of placement of multiple layers structural slab, the shape and size of die cavity 4 all match with the shape and size of described double-layer structure panel, and seaming chuck 2 and push-down head 3 are made by carbofrax material;
Step 3, the assembling die that double-layer structure panel is housed in step 2 is put into plasma activated sintering stove, the vacuum that regulates described plasma activated sintering stove is 11Pa, and current density is 400A/cm
2, axial compressive force is 100MPa, in sintering temperature, be under the condition of 1000 ℃ by double-layer structure panel sintering processes 13min, after the temperature in plasma activated sintering stove is down to room temperature, remove axial compressive force, after the demoulding, obtain copper molybdenum multilayer materials.
In copper molybdenum multilayer materials prepared by the present embodiment, the volumn concentration of molybdenum is 60%, and perpendicular layers direction thermal conductivity is 218W/mk, and thermal coefficient of expansion is 6.62 * 10
-6k
-1, peel strength is 68.56N/cm.
The above; it is only preferred embodiment of the present invention; not the present invention is imposed any restrictions, every any simple modification of above embodiment being done according to the technology of the present invention essence, change and equivalent structure change, and all still belong in the protection domain of technical solution of the present invention.
Claims (7)
1. prepare fast a method for copper molybdenum multilayer materials, it is characterized in that, the method comprises the following steps:
Step 1, grinding process is carried out to remove oxide-film in the surface of copper sheet and molybdenum sheet, then with acetone, clean copper sheet and the molybdenum sheet after polishing, cold wind dries up standby; The thickness of single described copper sheet is 0.1mm～0.65mm, and the thickness of single molybdenum sheet is 0.24mm～1.8mm;
Step 2, by the copper sheet after cleaning in step 1 and the molybdenum sheet laying that is superimposed, obtain double-layer structure panel, then described double-layer structure panel is put into assembling die; The number of plies of described double-layer structure panel is at least three layers, the outermost layer of described double-layer structure panel is copper sheet, described assembling die comprises the graphite external mold (1) of hollow structure, the upper end of graphite external mold (1) is provided with seaming chuck (2), the lower end of graphite external mold (1) is provided with push-down head (3), the die cavity (4) that is formed for placement of multiple layers structural slab between described seaming chuck (2), push-down head (3) and graphite external mold (1) inwall, the shape and size of die cavity (4) all match with the shape and size of described double-layer structure panel;
Step 3, the assembling die that double-layer structure panel is housed in step 2 is put into plasma activated sintering stove, the vacuum that regulates described plasma activated sintering stove is 5Pa～15Pa, and current density is 300A/cm
2～500A/cm
2axial compressive force is 50MPa～100MPa, in sintering temperature, be under the condition of 800 ℃～1000 ℃ by double-layer structure panel sintering processes 10min～17min, after the temperature in plasma activated sintering stove is down to room temperature, remove axial compressive force, after the demoulding, obtain copper molybdenum multilayer materials.
2. according to a kind of method of preparing fast copper molybdenum multilayer materials claimed in claim 1, it is characterized in that, the number of plies described in step 2 is 3～15 layers.
3. according to a kind of method of preparing fast copper molybdenum multilayer materials claimed in claim 1, it is characterized in that, described in step 2, in double-layer structure panel, the volumn concentration of molybdenum is 40%～60%.
4. according to a kind of method of preparing fast copper molybdenum multilayer materials claimed in claim 3, it is characterized in that, in described double-layer structure panel, the thickness of copper sheet used all equates, the thickness of molybdenum sheet used is all equal, and the Thickness Ratio of single described copper sheet and single described molybdenum sheet is 1:(1～3).
5. according to a kind of method of preparing fast copper molybdenum multilayer materials claimed in claim 1, it is characterized in that, seaming chuck described in step 2 (2) and push-down head (3) are made by carbofrax material.
6. according to a kind of method of preparing fast copper molybdenum multilayer materials claimed in claim 1, it is characterized in that, vacuum described in step 3 is 8Pa～12Pa, and described current density is 380A/cm
2～450A/cm
2, described axial compressive force is 75MPa～100MPa, and described sintering temperature is 900 ℃～1000 ℃, and described sintering time is 12min～15min.
7. according to a kind of method of preparing fast copper molybdenum multilayer materials claimed in claim 5, it is characterized in that, described vacuum is 10Pa, and current density is 450A/cm
2, axial compressive force is 100MPa, and sintering temperature is 950 ℃, and sintering time is 15min.
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| CN109334162A (en) * | 2018-08-23 | 2019-02-15 | 长沙升华微电子材料有限公司 | A kind of the pseudo-alloy composite material and preparation method and application of multilayered structure |
| CN112091211A (en) * | 2020-08-20 | 2020-12-18 | 上海交通大学 | Preparation method of diffusion multi-element joint |
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