CN104014921B - A kind of method preparing copper molybdenum multilayer materials fast - Google Patents
A kind of method preparing copper molybdenum multilayer materials fast Download PDFInfo
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- CN104014921B CN104014921B CN201410172037.2A CN201410172037A CN104014921B CN 104014921 B CN104014921 B CN 104014921B CN 201410172037 A CN201410172037 A CN 201410172037A CN 104014921 B CN104014921 B CN 104014921B
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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 kind of method preparing copper molybdenum multilayer materials fast, comprise the following steps: one, grinding process is carried out to remove oxide-film in the surface of copper sheet and molybdenum sheet, then with the copper sheet after acetone cleaning polishing and molybdenum sheet, cold wind dries up for subsequent use; Two, be superimposed copper sheet and molybdenum sheet laying, obtains double-layer structure panel, then double-layer structure panel is put into assembling die; Three, the assembling die that double-layer structure panel is housed is put into plasma activated sintering stove, after sintering, the demoulding obtains copper molybdenum multilayer materials.The present invention directly carries out electrified regulation sintering to the double-layer structure panel that the laying that is superimposed by copper sheet and molybdenum sheet obtains by introducing high-density current, the rapid diffusion realizing copper molybdenum interface under the synergy of temperature and pressure connects, 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.
Description
Technical field
The invention belongs to electronic package material technical field, be specifically related to a kind of method preparing copper molybdenum multilayer materials fast.
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 devices function, performance degradation, the lost of life can be caused.Finding excellent electronic package material, is the important channel solving high-power component heat dissipation problem, and for improving, the performance of device, reliability and service life are significant.Electronic Packaging and heat sink material not only will have high thermal conductivity, and need the thermal coefficient of expansion matched with chip material, to avoid device in encapsulation or use procedure because thermal strain mismatch causes distortion or damage.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 having competitiveness.
Current Cu/Mo/Cu laminar composite is based on " sandwich " structure of three layers, and preparation method mainly contains rolling, explosion method, pressure sintering and cladding method etc.Rolling is the preparation method being seen in report the earliest, 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 adopts hot rolling and cold-rolling practice to prepare Cu/Mo/Cu laminar composite respectively; The major defect that rolling exists is that Cu and Mo is immiscible, after mill-annealed, copper molybdenum interface mainly combines in mechanical engagement mode, and interface bond strength is not high, to improve interface bond strength, roll-force must be improved, but there is cracking or layering in the Mo easily causing fragility own large; The Cu/Mo/Cu laminar composite of blast rolling preparation " sandwich " structure is adopted in patent CN102371719, but processing step is more in the technical scheme of this patent, and itself there is higher risk and noise pollution in Explosion composite method, and Strip Shape Control is difficult, be unsuitable for continuous seepage 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 shaping, then superimposedly with Cu plate carries out hot pressed sintering, and 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 needs cold rolling shaping, surface quality and the more difficult control of thickness after Cu cooling, and limited when preparing large Thickness ratio 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 preparing copper molybdenum multilayer materials fast.The method directly carries out electrified regulation sintering to the double-layer structure panel that the laying that is superimposed by copper sheet and molybdenum sheet obtains by introducing high-density current, the rapid diffusion realizing copper molybdenum interface under the synergy of temperature and pressure connects, thus the copper molybdenum multi-layer composite materials preparation method for material providing a kind of operation 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 preparing copper molybdenum multilayer materials fast, and it is characterized in that, the method comprises the following steps:
Step one, grinding process is carried out to remove oxide-film in the surface of copper sheet and molybdenum sheet, then with the copper sheet after acetone cleaning polishing and molybdenum sheet, cold wind dries up for subsequent use; 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, the copper sheet after cleaning in step one and molybdenum sheet to be superimposed laying, to 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, described seaming chuck, formed be used for the die cavity of placement of multiple layers structural slab between 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, regulate the vacuum of described plasma activated sintering stove to be 5Pa ~ 15Pa, current density is 300A/cm
2~ 500A/cm
2axial compressive force is 50MPa ~ 100MPa, be by double-layer structure panel sintering processes 10min ~ 17min under the condition of 800 DEG C ~ 1000 DEG C in sintering temperature, be down to after room temperature until the temperature in plasma activated sintering stove and remove axial compressive force, after the demoulding, obtain copper molybdenum multilayer materials.
A kind of above-mentioned method preparing copper molybdenum multilayer materials fast, is characterized in that, the number of plies described in step 2 is 3 ~ 15 layers.
A kind of above-mentioned method preparing copper molybdenum multilayer materials fast, is characterized in that, in double-layer structure panel described in step 2, the volumn concentration of molybdenum is 40% ~ 60%.
A kind of above-mentioned method preparing copper molybdenum multilayer materials fast, it is characterized in that, in described double-layer structure panel, the thickness of copper sheet used is all equal, and 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 preparing copper molybdenum multilayer materials fast, it 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 preparing copper molybdenum multilayer materials fast, it is characterized in that, vacuum described in step 3 is 8Pa ~ 12Pa, described current density is 380A/cm
2~ 450A/cm
2, described axial compressive force is 75MPa ~ 100MPa, and described sintering temperature is 900 DEG C ~ 1000 DEG C, and described sintering time is 12min ~ 15min.
A kind of above-mentioned method preparing copper molybdenum multilayer materials fast, it is characterized in that, described vacuum is 10Pa, current density is 450A/cm
2, axial compressive force is 100MPa, and sintering temperature is 950 DEG C, and sintering time is 15min.
The present invention compared with prior art has the following advantages:
1, the present invention directly carries out electrified regulation sintering to the double-layer structure panel that the laying that is superimposed by copper sheet and molybdenum sheet obtains by introducing high-density current, the rapid diffusion realizing copper molybdenum interface under the synergy of temperature and pressure connects, thus the copper molybdenum multi-layer composite materials preparation method for material providing a kind of operation 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 carrying out electrified regulation sintering to copper sheet to be composite and molybdenum sheet, utilize the atom being used for improving copper molybdenum interface of high-density current mixed degree mutually, firing rate is exceedingly fast, the physical contact process such as plastic deformation and creep on copper sheet and molybdenum sheet surface can be accelerated, shorten Material cladding connection procedure, electric current can promote that copper molybdenum interface atoms mixes mutually simultaneously, strengthens copper molybdenum metallurgical interface and combines, to obtain the copper molybdenum laminar composite of high interfacial strength.
3, the size of change copper sheet and molybdenum sheet, thickness and both numbers of plies that is superimposed is passed through in preparation technology of the present invention, thermal conductivity and the thermal coefficient of expansion of copper molybdenum laminar composite can be regulated and controled in a big way, by increasing the molybdenum sheet number of plies, reducing molybdenum sheet thickness, the thermal expansion effect of contraction of Mo layer to Cu layer can be given full play to, reduce the volumn concentration of Mo layer, thus raising heat 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 prepared is large, and uniformity is good, 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 Elemental redistribution 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 that in the embodiment of the present invention 2, copper sheet and molybdenum sheet are superimposed the structural representation of laying.
Description of reference numerals:
1-graphite external mold; 2-seaming chuck; 3-push-down head;
4-die cavity; 5-copper sheet; 6-molybdenum sheet.
Detailed description of the invention
In various embodiments of the present invention, plasma activated sintering stove used is the model that Japanese Elenix company produces is the plasma activated sintering stove of ED-PAS III.
Embodiment 1
Step one, respectively grinding process is carried out to remove oxide-film in the surface of 8 copper sheets and 7 molybdenum sheets with sand paper, then with the copper sheet after acetone cleaning polishing and molybdenum sheet, cold wind dries up for subsequent use; 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, the copper sheet after cleaning in step one and molybdenum sheet to be superimposed laying, to 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, according to the order that is superimposed during 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, described seaming chuck 2, formed between push-down head 3 and graphite external mold 1 inwall and be used 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, regulate the vacuum of described plasma activated sintering stove to be 10Pa, current density is 450A/cm
2, axial compressive force is 100MPa, is by double-layer structure panel sintering processes 15min under the condition of 950 DEG C in sintering temperature, is down to after room temperature and removes axial compressive force, obtain copper molybdenum multilayer materials after the demoulding until the temperature in plasma activated sintering stove.
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, generates without obvious hole.
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, to be width be at copper molybdenum interface in copper molybdenum multilayer materials prepared by the present embodiment mixed mutually interface of 3 μm ~ 4 μm, wherein the atomicity percentage composition of copper reaches 3.8%, much larger than the limit solid solubility that Cu-Mo phasor is corresponding, this illustrate can promote copper molybdenum interface atoms by the effect of the present embodiment middle-high density electric current sneak out journey mutually, improve the mixed mutually degree of copper molybdenum interface atoms, thus 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 one, respectively grinding process is carried out to remove oxide-film in the surface of 5 copper sheets and 4 molybdenum sheets with sand paper, then with the copper sheet after acetone cleaning polishing and molybdenum sheet, cold wind dries up for subsequent use; The thickness of single described copper sheet and single described molybdenum sheet is 0.3mm;
Step 2, the copper sheet after cleaning in step one and molybdenum sheet to be superimposed laying, to 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, described seaming chuck 2, formed between push-down head 3 and graphite external mold 1 inwall and be used 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, regulate the vacuum of described plasma activated sintering stove to be 12Pa, current density is 380A/cm
2, axial compressive force is 75MPa, is by double-layer structure panel sintering processes 15min under the condition of 950 DEG C in sintering temperature, and be down to after room temperature until the temperature in plasma activated sintering stove and remove axial compressive force, obtain copper molybdenum multilayer materials after the demoulding, structure 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 one, respectively grinding process is carried out to remove oxide-film in the surface of 5 copper sheets and 4 molybdenum sheets with sand paper, then with the copper sheet after acetone cleaning polishing and molybdenum sheet, cold wind dries up for subsequent use; The thickness of single described copper sheet is 0.3mm, and the thickness of single described molybdenum sheet is 0.375mm;
Step 2, the copper sheet after cleaning in step one and molybdenum sheet to be superimposed laying, to 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, described seaming chuck 2, formed between push-down head 3 and graphite external mold 1 inwall and be used 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, regulate the vacuum of described plasma activated sintering stove to be 15Pa, current density is 300A/cm
2, axial compressive force is 50MPa, is by double-layer structure panel sintering processes 17min under the condition of 800 DEG C in sintering temperature, is down to after room temperature and removes axial compressive force, obtain copper molybdenum multilayer materials after the demoulding until the temperature in plasma activated sintering stove.
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 one, respectively grinding process is carried out to remove oxide-film in the surface of 5 copper sheets and 4 molybdenum sheets with sand paper, then with the copper sheet after acetone cleaning polishing and molybdenum sheet, cold wind dries up for subsequent use; The thickness of single described copper sheet is 0.26mm, and the thickness of single described molybdenum sheet is 0.45mm;
Step 2, the copper sheet after cleaning in step one and molybdenum sheet to be superimposed laying, to 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, described seaming chuck 2, formed between push-down head 3 and graphite external mold 1 inwall and be used 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, regulate the vacuum of described plasma activated sintering stove to be 8Pa, current density is 450A/cm
2, axial compressive force is 85MPa, is by double-layer structure panel sintering processes 12min under the condition of 900 DEG C in sintering temperature, is down to after room temperature and removes axial compressive force, obtain copper molybdenum multilayer materials after the demoulding until the temperature in plasma activated sintering stove.
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 one, respectively grinding process is carried out to remove oxide-film in the surface of 2 copper sheets and 1 molybdenum sheet with sand paper, then with the copper sheet after acetone cleaning polishing and molybdenum sheet, cold wind dries up for subsequent use; The thickness of single described copper sheet is 0.65mm, and the thickness of described molybdenum sheet is 1.8mm;
Step 2, the copper sheet after cleaning in step one and molybdenum sheet to be superimposed laying, to 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, described seaming chuck 2, formed between push-down head 3 and graphite external mold 1 inwall and be used 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, regulate the vacuum of described plasma activated sintering stove to be 5Pa, current density is 500A/cm
2, axial compressive force is 75MPa, is by double-layer structure panel sintering processes 10min under the condition of 1000 DEG C in sintering temperature, is down to after room temperature and removes axial compressive force, obtain copper molybdenum multilayer materials after the demoulding until the temperature in plasma activated sintering stove.
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 one, respectively grinding process is carried out to remove oxide-film in the surface of 3 copper sheets and 2 molybdenum sheets with sand paper, then with the copper sheet after acetone cleaning polishing and molybdenum sheet, cold wind dries up for subsequent use; 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, the copper sheet after cleaning in step one and molybdenum sheet to be superimposed laying, to 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, according to the order that is superimposed during 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, described seaming chuck 2, formed between push-down head 3 and graphite external mold 1 inwall and be used 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, regulate the vacuum of described plasma activated sintering stove to be 7Pa, current density is 480A/cm
2, axial compressive force is 90MPa, is by double-layer structure panel sintering processes 16min under the condition of 980 DEG C in sintering temperature, is down to after room temperature and removes axial compressive force, obtain copper molybdenum multilayer materials after the demoulding until the temperature in plasma activated sintering stove.
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 one, respectively grinding process is carried out to remove oxide-film in the surface of 2 copper sheets and 1 molybdenum sheet with sand paper, then with the copper sheet after acetone cleaning polishing and molybdenum sheet, cold wind dries up for subsequent use; The thickness of single described copper sheet is 0.3mm, and the thickness of described molybdenum sheet is 0.9mm;
Step 2, the copper sheet after cleaning in step one and molybdenum sheet to be superimposed laying, to 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, described seaming chuck 2, formed between push-down head 3 and graphite external mold 1 inwall and be used 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, regulate the vacuum of described plasma activated sintering stove to be 11Pa, current density is 400A/cm
2, axial compressive force is 100MPa, is by double-layer structure panel sintering processes 13min under the condition of 1000 DEG C in sintering temperature, is down to after room temperature and removes axial compressive force, obtain copper molybdenum multilayer materials after the demoulding until the temperature in plasma activated sintering stove.
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 above embodiment is done according to the technology of the present invention essence any simple modification, change and equivalent structure change, all still belong in the protection domain of technical solution of the present invention.
Claims (6)
1. prepare a method for copper molybdenum multilayer materials fast, it is characterized in that, the method comprises the following steps:
Step one, grinding process is carried out to remove oxide-film in the surface of copper sheet and molybdenum sheet, then with the copper sheet after acetone cleaning polishing and molybdenum sheet, cold wind dries up for subsequent use; 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, the copper sheet after cleaning in step one and molybdenum sheet to be superimposed laying, to 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), described seaming chuck (2), the die cavity (4) being used for placement of multiple layers structural slab is formed between 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, in described double-layer structure panel, the volumn concentration of molybdenum is 40% ~ 60%,
Step 3, the assembling die that double-layer structure panel is housed in step 2 is put into plasma activated sintering stove, regulate the vacuum of described plasma activated sintering stove to be 5Pa ~ 15Pa, current density is 300A/cm
2~ 500A/cm
2axial compressive force is 50MPa ~ 100MPa, be by double-layer structure panel sintering processes 10min ~ 17min under the condition of 800 DEG C ~ 1000 DEG C in sintering temperature, be down to after room temperature until the temperature in plasma activated sintering stove and remove axial compressive force, after the demoulding, obtain copper molybdenum multilayer materials.
2. according to a kind of method preparing copper molybdenum multilayer materials fast according to 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 preparing copper molybdenum multilayer materials fast according to claim 1, it is characterized in that, in described double-layer structure panel, the thickness of copper sheet used is all equal, 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).
4. according to a kind of method preparing copper molybdenum multilayer materials fast according to claim 1, it is characterized in that, seaming chuck described in step 2 (2) and push-down head (3) are made by carbofrax material.
5. according to a kind of method preparing copper molybdenum multilayer materials fast according to 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 DEG C ~ 1000 DEG C, and described sintering time is 12min ~ 15min.
6. according to a kind of method preparing copper molybdenum multilayer materials fast according to 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 DEG C, and sintering time is 15min.
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| CN105946312A (en) * | 2016-06-24 | 2016-09-21 | 佛山华智新材料有限公司 | Multilayered metal rapid compounding process |
| CN107096987A (en) * | 2017-03-22 | 2017-08-29 | 华南理工大学 | A kind of quick diffusion welding method of metal bar based on pulsed current annealing |
| CN109334162B (en) * | 2018-08-23 | 2021-08-13 | 长沙升华微电子材料有限公司 | Pseudo alloy composite material with multilayer structure and preparation method and application thereof |
| CN112091211B (en) * | 2020-08-20 | 2021-09-10 | 上海交通大学 | Preparation method of diffusion multi-element joint |
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| CN103402690A (en) * | 2011-03-02 | 2013-11-20 | 株式会社拓科浩 | Method for fabricating slidable member |
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