CN117862487A - Copper-molybdenum-copper composite material with bending dimension requirement and flexible deep processing method thereof - Google Patents
Copper-molybdenum-copper composite material with bending dimension requirement and flexible deep processing method thereof Download PDFInfo
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- CN117862487A CN117862487A CN202410127433.7A CN202410127433A CN117862487A CN 117862487 A CN117862487 A CN 117862487A CN 202410127433 A CN202410127433 A CN 202410127433A CN 117862487 A CN117862487 A CN 117862487A
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- 239000002131 composite material Substances 0.000 title claims abstract description 60
- BLNMQJJBQZSYTO-UHFFFAOYSA-N copper molybdenum Chemical compound [Cu][Mo][Cu] BLNMQJJBQZSYTO-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000005452 bending Methods 0.000 title claims abstract description 39
- 238000003672 processing method Methods 0.000 title claims abstract description 24
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 39
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000498 ball milling Methods 0.000 claims abstract description 34
- 229910052802 copper Inorganic materials 0.000 claims abstract description 30
- 239000010949 copper Substances 0.000 claims abstract description 30
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 26
- 239000011733 molybdenum Substances 0.000 claims abstract description 26
- 238000007639 printing Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 18
- 239000002002 slurry Substances 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000011230 binding agent Substances 0.000 claims abstract description 13
- 238000005266 casting Methods 0.000 claims abstract description 13
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 12
- 238000007650 screen-printing Methods 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 239000002562 thickening agent Substances 0.000 claims abstract description 10
- 238000007493 shaping process Methods 0.000 claims abstract description 9
- 239000012528 membrane Substances 0.000 claims abstract description 8
- 238000013035 low temperature curing Methods 0.000 claims abstract description 7
- 238000010345 tape casting Methods 0.000 claims abstract description 7
- 238000000465 moulding Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 24
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 8
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 8
- 238000003801 milling Methods 0.000 claims description 8
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 8
- 239000004677 Nylon Substances 0.000 claims description 7
- 229920001778 nylon Polymers 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 239000003292 glue Substances 0.000 claims description 6
- 238000000462 isostatic pressing Methods 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000001856 Ethyl cellulose Substances 0.000 claims description 4
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 4
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 4
- 239000004359 castor oil Substances 0.000 claims description 4
- 235000019438 castor oil Nutrition 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 4
- 229920001249 ethyl cellulose Polymers 0.000 claims description 4
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 4
- 239000004584 polyacrylic acid Substances 0.000 claims description 4
- 229940116411 terpineol Drugs 0.000 claims description 4
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 3
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 claims description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 3
- 239000002356 single layer Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 7
- 239000010410 layer Substances 0.000 description 10
- WUUZKBJEUBFVMV-UHFFFAOYSA-N copper molybdenum Chemical compound [Cu].[Mo] WUUZKBJEUBFVMV-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000005096 rolling process Methods 0.000 description 6
- 238000003754 machining Methods 0.000 description 5
- 239000011162 core material Substances 0.000 description 4
- 229910000881 Cu alloy Inorganic materials 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000005098 hot rolling Methods 0.000 description 3
- 238000003475 lamination Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005097 cold rolling Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 238000009966 trimming Methods 0.000 description 2
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000015895 biscuits Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- -1 molybdenum-copper metals Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000007514 turning Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a copper-molybdenum-copper composite material and a flexible deep processing method thereof, comprising the following steps: adding pure molybdenum metal powder into a solvent and a dispersing agent, performing primary ball milling, adding a thickening agent and a binder, performing secondary ball milling and defoaming to obtain molybdenum slurry for casting molding; placing the molybdenum slurry for tape casting on a base band, adjusting the height clearance of a scraper and the speed of the base band, and drying to obtain a molybdenum diaphragm; printing copper paste with a certain thickness on the upper surface and the lower surface of the molybdenum diaphragm through silk screen printing, and obtaining a copper-molybdenum-copper composite flexible diaphragm through drying and hot isostatic pressing; and placing the copper-molybdenum-copper composite flexible membrane into a stamping die cavity for bending, performing low-temperature curing shaping and demoulding, and performing degumming and integrated cofiring to obtain the copper-molybdenum-copper composite with the requirement on bending size. The invention has the advantages of simple process, accurate component control, good precision, high yield and the like.
Description
Technical Field
The invention relates to the technical field of copper-molybdenum-copper composite materials, in particular to a copper-molybdenum-copper composite material with bending dimension requirement and a flexible deep processing method thereof.
Background
The heat sink material is a heat dissipation material commonly applied to the combination of an integrated circuit and a chip, and is represented by typical tungsten copper alloy, molybdenum copper alloy, copper molybdenum copper flat plate composite materials, and the heat sink material has the advantages of high heat conductivity, low thermal expansion coefficient, chip matching and the like.
At present, the production method of tungsten copper and molybdenum copper heat sink materials is mainly an infiltration and liquid phase sintering method, the flat composite material is a rolling combination and thermal diffusion method of core materials and double-sided copper layers, products which are further processed into precise structural dimensions and complex shapes suitable for chips need to be processed by a machining or stamping process, and as the core materials of the flat composite material and the copper layers on the upper surface and the lower surface have large difference in plasticity, toughness and hardness, the flat composite material is deformed in a non-cooperative manner when being stressed when being stamped and bent, and the materials are broken when being stamped and bent.
In the prior art, the copper-molybdenum-copper composite material is prepared by using modes of hot pressing compounding, rolling, thermal diffusion and the like, the working procedure is complex, the component control is inaccurate, the precision is poor, and particularly, the mechanical property difference of different materials is not suitable for precision stamping hard processing.
Disclosure of Invention
In view of the defects existing at present, the invention provides a copper-molybdenum-copper composite material with bending size requirement and a flexible deep processing method thereof, the invention prepares a molybdenum blank membrane with good copper wettability through a water-based tape casting forming process, copper is sequentially coated on the upper and lower surfaces of the membrane material through copper paste in a screen printing mode, a molybdenum-copper laminated thick film material with good flexibility is prepared through hot isostatic pressing, then the flexible membrane is placed in a designed mould for solidification and shaping, degumming and integrated cofiring products, and finally shaping is carried out, flexible processing of a flat plate composite material with a precise structure and a complex shape is completed, the fracture problem of the hard composite material after firing in the punching processing is effectively solved, and the invention has the advantages of simple procedure, accurate component control, good precision, high yield and the like.
In order to achieve the above purpose, the invention provides a flexible deep processing method of a copper-molybdenum-copper composite material with bending dimension requirement, which comprises the following steps:
step 1: adding pure molybdenum metal powder into a solvent and a dispersing agent, performing primary ball milling, adding a thickening agent and a binder, performing secondary ball milling and defoaming to obtain molybdenum slurry for casting molding;
step 2: placing the molybdenum slurry for tape casting on a base band, adjusting the height clearance of a scraper and the speed of the base band, and drying to obtain a molybdenum diaphragm;
step 3: printing copper paste with a certain thickness on the upper surface and the lower surface of the molybdenum diaphragm through silk screen printing, and obtaining a copper-molybdenum-copper composite flexible diaphragm through drying and hot isostatic pressing; wherein the copper paste for printing consists of copper powder, glass powder and an organic carrier;
step 4: placing a copper-molybdenum-copper composite flexible membrane into a stamping die cavity for bending, performing low-temperature curing shaping and demoulding, and performing degumming and integrated cofiring to obtain a copper-molybdenum-copper composite with a bending size requirement; wherein the temperature of the low-temperature curing and shaping is 150-350 ℃ and the time is 2-6 h.
According to one aspect of the present invention, in step 1, the content of the pure molybdenum metal powder in the molybdenum slurry for casting is 70 to 80wt%, the content of the solvent is 11 to 25wt%, the content of the dispersant is 0.8 to 1.2wt%, the content of the thickener is 1.2 to 2.8wt%, and the content of the binder is 3 to 6wt%.
According to one aspect of the present invention, in step 1, the pure molybdenum metal powder has a particle size of 2 to 10 μm; the solvent is deionized water; the dispersing agent is polyacrylic acid or Hypermer KD-1; the thickener is at least one of glycerol and polyethylene glycol; the binder is one or more of PVA-2488, polymethyl methacrylate and ethyl acrylate.
According to one aspect of the invention, in step 1, the primary ball milling adopts a nylon ball milling tank, silicon nitride is used as a milling medium, and balls: material=1:1, ball milling time is 6-48 h, and rotating speed is 150-250 r/min; the secondary ball milling adopts a nylon ball milling tank, silicon nitride is used as a milling medium, and the balls are formed by: material=1:1, ball milling time is 6-48 h, and rotating speed is 150-250 r/min; the defoaming is to remove bubbles in vacuum for 5-20 min under the condition of 20-100 kPa.
In accordance with one aspect of the invention, in step 2, the doctor blade height gap is 5um to 0.1mm, the baseband speed is 2.0 to 2.5mm/s, and the drying temperature is 20 to 30 ℃.
According to one aspect of the present invention, in step 3, the solid content of the copper paste for printing is 50 to 80%.
According to one aspect of the invention, in step 3, the organic carrier is any one or more of terpineol, isopropanol, tributyl phthalate, ethylcellulose, toluene, terephthalic acid, castor oil.
According to one aspect of the present invention, in step 3, the screen printing method comprises: firstly, printing copper paste on one side, drying, and then printing the other side, wherein the thickness of the screen printing single layer is 0.1-10 mu m.
According to one aspect of the invention, the hot isostatic pressing is any one of a hydrothermal isostatic pressing method and an oil isostatic pressing method; the temperature of the hot isostatic pressing is 60-120 ℃, the pressure is 2000-5000 PSI, and the pressure maintaining temperature is 60-100 ℃; the degumming is carried out in the atmosphere of hydrogen or nitrogen, the temperature of glue discharging is 300-600 ℃, and the time of glue discharging is 8-24 hours; the temperature of the integrated cofiring is 800-1200 ℃, and the time of the integrated cofiring is 2-4 hours.
Based on the same inventive concept, the invention also provides the copper-molybdenum-copper composite material with bending dimension requirement prepared by any flexible deep processing method.
The invention has the beneficial effects that:
(1) The water-based casting slurry in the water-based casting forming process adopted by the invention has higher solid content and stronger inter-particle binding force, and when the particle concentration reaches the degree of mutual contact between particles, the three-dimensional space network structure of particles is deformed, and the larger the yield stress of the material is;
(2) The casting slurry is a pseudoplastic fluid, has moderate viscosity, is added with plasticizer glycerol to combine with the polar group of the PVA-2488 chain of the binder and wrap the molecular chain, increases the molecular distance of the binder, forms a large number of holes, increases the free volume, thereby reducing the glass transition temperature of the binder, leading the brittleness temperature area to be obviously lower than the room temperature, improving the flexibility of the water-based casting plain sheet and meeting the processing technology requirements of reels, cutting, lamination, bending and the like;
(3) The intrinsic brittleness of the molybdenum metal at room temperature and the insufficient strength at room temperature/high temperature limit the low-temperature processing performance of the molybdenum-copper alloy, while the preparation of the copper-molybdenum-copper composite biscuit by tape casting and lamination processes has the advantages that the interface is flat and straight, oxide impurities are not introduced, the molybdenum-copper interface combination is enhanced by a surface molybdenum-copper atomic metal bond compounding mechanism at a certain temperature, bending processing shearing force can be transmitted between the molybdenum-copper metals through good interface combination, and the two-phase deformation is consistent. The stress concentration of the interface between the copper and the molybdenum matrix is greatly relieved through the micro-scale plastic deformation of the composite material at room temperature, the cracking of the interface is delayed, and the low-temperature ductility and the good workability of the complex structure of the functionally graded composite material can be realized.
(4) The copper-molybdenum-copper composite material with the bending size requirement prepared by the processing method has high qualification rate and excellent mechanical property.
Drawings
FIG. 1 is a process flow diagram of a flexible deep processing method of a copper-molybdenum-copper composite material with bending dimension requirements according to the invention;
FIG. 2 is a front view of a copper-molybdenum-copper composite material with bending dimension requirements prepared in example 1 of the present invention;
FIG. 3 is a top view of a copper-molybdenum-copper composite material with bending dimension requirements prepared in example 1 of the present invention;
fig. 4 is a flexible processing schematic diagram of the copper-molybdenum-copper composite material with bending dimension requirement prepared in the embodiment 1 of the present invention.
Reference numerals illustrate: 1. an upper die; 2. and (5) a lower die.
Detailed Description
The present invention will be described more fully hereinafter with reference to the accompanying drawings, in which preferred embodiments are shown, for the purpose of illustrating the invention, but the scope of the invention is not limited to the specific embodiments shown.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
In order to solve the problems that in the prior art, a copper-molybdenum-copper composite material is prepared by using modes of hot pressing compounding, rolling, thermal diffusion and the like, the working procedure is complex, the component control is inaccurate, the precision is poor, and especially because the mechanical property difference of different materials is not suitable for precision stamping hard processing, the inventor of the application provides a flexible deep processing method of the copper-molybdenum-copper composite material with bending size requirement, and a process flow chart of the flexible deep processing method is shown in figure 1 and comprises the following steps:
step 1: adding pure molybdenum metal powder into a solvent and a dispersing agent, performing primary ball milling, adding a thickening agent and a binder, performing secondary ball milling and defoaming to obtain molybdenum slurry for casting molding;
step 2: placing the molybdenum slurry for tape casting on a base band, adjusting the height clearance of a scraper and the speed of the base band, and drying to obtain a molybdenum diaphragm;
step 3: printing copper paste with a certain thickness on the upper surface and the lower surface of the molybdenum diaphragm through silk screen printing, and obtaining a copper-molybdenum-copper composite flexible diaphragm through drying and hot isostatic pressing; wherein the copper paste for printing consists of copper powder, glass powder and an organic carrier;
step 4: placing a copper-molybdenum-copper composite flexible membrane into a stamping die cavity for bending, performing low-temperature curing shaping and demoulding, and performing degumming and integrated cofiring to obtain a copper-molybdenum-copper composite with a bending size requirement; wherein the temperature of the low-temperature curing and shaping is 150-350 ℃ and the time is 2-6 h.
In the step 1, the pure molybdenum metal powder in the molybdenum slurry for casting is 70-80 wt%, the solvent is 11-25 wt%, the dispersant is 0.8-1.2 wt%, the thickener is 1.2-2.8 wt%, and the binder is 3-6 wt%.
In an alternative embodiment, in step 1, the particle size of the pure molybdenum metal powder is 2-10 μm; the solvent is deionized water; the dispersing agent is polyacrylic acid or Hypermer KD-1; the thickener is at least one of glycerol and polyethylene glycol; the binder is one or more of PVA-2488, polymethyl methacrylate and ethyl acrylate.
In the step 1, as an alternative embodiment, a nylon ball milling tank is adopted for the primary ball milling, silicon nitride is used as a milling medium, and balls are used as the milling medium: material=1:1, ball milling time is 6-48 h, and rotating speed is 150-250 r/min; the secondary ball milling adopts a nylon ball milling tank, silicon nitride is used as a milling medium, and the balls are formed by: material=1:1, ball milling time is 6-48 h, and rotating speed is 150-250 r/min; the defoaming is to remove bubbles in vacuum for 5-20 min under the condition of 20-100 kPa.
In an alternative embodiment, in the step 2, the height clearance of the scraper is 5 um-0.1 mm, the speed of the base band is 2.0-2.5 mm/s, and the drying temperature is 20-30 ℃.
In an alternative embodiment, in step 3, the solid content of the copper paste for printing is 50 to 80%.
In an alternative embodiment, in step 3, the organic carrier is any one or more of terpineol, isopropanol, tributyl phthalate, ethylcellulose, toluene, terephthalic acid, castor oil.
In an optional embodiment, in step 3, the screen printing method includes: firstly, printing copper paste on one side, drying, and then printing the other side, wherein the thickness of the screen printing single layer is 0.1-10 mu m.
In the present invention, screen printing may be repeated a plurality of times depending on the thickness of the copper layer required, for example, a single printing film of 5um in thickness and a single copper layer of 20um in thickness required, and printing is required 4 times.
As an optional embodiment, the hot isostatic pressing is any one of a hydrothermal isostatic pressing method and an oil isostatic pressing method; the temperature of the hot isostatic pressing is 60-120 ℃, the pressure is 2000-5000 PSI, and the pressure maintaining temperature is 60-100 ℃; the degumming is carried out in the atmosphere of hydrogen or nitrogen, wherein the temperature of glue discharging is 300-600 ℃, and preferably 550 ℃; the glue discharging time is 8-24 hours, preferably 16 hours; the temperature of the integrated cofiring is 800-1200 ℃, preferably 950 ℃; the integrated cofiring time is 2-4 hours, preferably 2 hours.
As an optional embodiment, any of the foregoing flexible deep processing methods further includes:
step 5: and trimming the copper-molybdenum-copper composite material with the bending size requirement by machining to obtain the workpiece with precise size and complex structure.
In the present invention, the above-mentioned machining includes turning, milling, planing, drilling, grinding, and the like.
The embodiment of the invention also provides the copper-molybdenum-copper composite material with the bending dimension requirement, which is prepared by any flexible deep processing method.
The embodiments of the present application are described above, and in order to objectively explain technical effects produced by the present application, the following examples and comparative examples will be described.
Example 1
The processing part of the copper-molybdenum-copper composite material shown in the figures 2-3 comprises the following processing methods:
(1) Adding a solvent (deionized water) and a dispersing agent (polyacrylic acid) into pure molybdenum metal powder with the D50 of 2 mu m, performing primary ball milling in a nylon ball milling tank according to the mass ratio of 80:12:1, wherein the grinding balls are silicon nitride, the ball milling time is 24H, and the rotating speed is 200r/min, so as to finish primary ball milling; then adding 5wt% of PVA-2488 and 2wt% of glycerol into the ball-milling suspension, performing secondary ball milling, wherein the grinding balls are silicon nitride, the ball-material ratio is 1:1, the ball milling time is 24H, the rotating speed is 200r/min to obtain secondary ball-milling slurry, and then removing bubbles in vacuum for 10 minutes to obtain molybdenum slurry for tape casting;
(2) Regulating the gap of a scraper to 45um, injecting molybdenum slurry for water-based casting forming into a storage tank, and during casting forming, enabling the slurry to flow from the lower part of a hopper to a PET base band moving forwards, wherein the thickness of a wet band is controlled by the gap of the scraper, the speed of the base band is 2.0mm/s, and drying the cast wet band in an air medium chamber (20-30 ℃) to obtain a molybdenum film;
(3) Printing a copper layer on a molybdenum film sheet by using an automatic lamination printer, wherein the method comprises the following steps: adding printing copper paste on a printing screen plate with designed size, printing a copper layer on a membrane, drying at 80 ℃, repeatedly printing and drying four times to finish the printing of the copper layer on a single surface, and then repeating the above operation to finish the printing of the copper layer on the other surface. Performing hot isostatic pressing on the printed diaphragm on a hydrothermal pressure equalizing machine, wherein the temperature is 80 ℃, the maximum pressure is 5000PSI, and the pressure is maintained for 10 minutes to finish the preparation of the molybdenum core composite flexible thick film material with double-sided copper coating; the copper paste for printing consists of 75% of copper powder, 3% of glass powder, 22% of organic carrier (9% of ethyl cellulose, 58% of terpineol, 22% of butyl carbitol acetate, 9% of dibutyl phthalate, 0.5% of castor oil, 0.5% of polyamide wax, 0.5% of terephthalic acid and 0.5% of ethanol), and the solid content is 75+/-3%.
(4) The flexible thick film material is placed in a stamping die cavity with designed outline dimensions to finish bending processing, the bent material is placed in a drying oven with hydrogen atmosphere along with a die to be cured and shaped at low temperature (the temperature is 180 ℃ for 2 hours), then the die is removed, and the shaped composite material part is subjected to heat preservation for 2 hours at the highest sintering temperature of 950 ℃ in the hydrogen atmosphere to finish sintering, so that a sintered copper-molybdenum-copper material is obtained; wherein, referring to fig. 4, the stamping die comprises an upper die 1 and a lower die 2, and a stamping die cavity for placing a flexible thick film material.
(5) And finally, machining and trimming the appearance of the part prepared from the sintered copper-molybdenum-copper material, and completing flexible deep machining of the part with precise size and complex appearance to obtain the copper-molybdenum-copper composite material with the requirement of bending size.
The copper-molybdenum-copper composite material with the bending size requirement is detected, the mechanical properties are shown in the following table 1, and the qualification rate is more than 99% according to experimental statistics.
Table 1:
comparative example 1
The prior method for preparing the complex structure processing workpiece based on the CMC composite material shown in the figures 2-3 comprises the steps of firstly reducing and annealing core material-molybdenum metal with calculated thickness, removing stress to reduce oxygen concentration and impurities, superposing copper layers with calculated thickness on two surfaces, binding, then carrying out multi-pass hot rolling, warm rolling and cold rolling, and preparing the copper-molybdenum-copper composite material by combining heat treatment. The method comprises the following steps: calculating the thicknesses of core material molybdenum (5 mm) and double-sided copper (1.5 mm), and binding and welding the three layers of materials; and performing multi-pass hot rolling (the temperature is 700 ℃, the first pass rolling reduction is 70 percent, the second hot rolling reduction is 50 percent) and cold rolling (the rolling reduction is 20 percent, 10 percent and 10 percent in sequence) and combining with heat treatment (550 ℃) to finally finish the preparation of the copper-molybdenum-copper composite material with the thickness of 0.3 mm. And then cutting the composite material, and performing stamping forming by using a designed stamping die.
The copper-molybdenum-copper composite material with the bending size requirement is tested, the mechanical properties are shown in the following table 2, and about 60% -100% of bad occurrence (failure rate) is counted according to experiments.
Table 2:
the foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the technical scope of the present invention should be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A flexible deep processing method of a copper-molybdenum-copper composite material with bending dimension requirement is characterized by comprising the following steps:
step 1: adding pure molybdenum metal powder into a solvent and a dispersing agent, performing primary ball milling, adding a thickening agent and a binder, performing secondary ball milling and defoaming to obtain molybdenum slurry for casting molding;
step 2: placing the molybdenum slurry for tape casting on a base band, adjusting the height clearance of a scraper and the speed of the base band, and drying to obtain a molybdenum diaphragm;
step 3: printing copper paste with a certain thickness on the upper surface and the lower surface of the molybdenum diaphragm through silk screen printing, and obtaining a copper-molybdenum-copper composite flexible diaphragm through drying and hot isostatic pressing; wherein the copper paste for printing consists of copper powder, glass powder and an organic carrier;
step 4: placing a copper-molybdenum-copper composite flexible membrane into a stamping die cavity for bending, performing low-temperature curing shaping and demoulding, and performing degumming and integrated cofiring to obtain a copper-molybdenum-copper composite with a bending size requirement; wherein the temperature of the low-temperature curing and shaping is 150-350 ℃ and the time is 2-6 h.
2. The flexible deep processing method of copper-molybdenum-copper composite material with bending size requirement according to claim 1, wherein in step 1, the content of pure molybdenum metal powder in the molybdenum slurry for casting is 70-80 wt%, the content of solvent is 11-25 wt%, the content of dispersant is 0.8-1.2 wt%, the content of thickener is 1.2-2.8 wt%, and the content of binder is 3-6 wt%.
3. The flexible deep processing method of the copper-molybdenum-copper composite material with the bending dimension requirement according to claim 1, wherein in the step 1, the grain diameter of the pure molybdenum metal powder is 2-10 μm; the solvent is deionized water; the dispersing agent is polyacrylic acid or Hypermer KD-1; the thickener is at least one of glycerol and polyethylene glycol; the binder is one or more of PVA-2488, polymethyl methacrylate and ethyl acrylate.
4. The flexible deep processing method of the copper-molybdenum-copper composite material with the bending dimension requirement according to claim 1, wherein in the step 1, a nylon ball milling tank is adopted for the primary ball milling, silicon nitride is used as a milling medium, and balls are used as the balls: material=1:1, ball milling time is 6-48 h, and rotating speed is 150-250 r/min; the secondary ball milling adopts a nylon ball milling tank, silicon nitride is used as a milling medium, and the balls are formed by: material=1:1, ball milling time is 6-48 h, and rotating speed is 150-250 r/min; the defoaming is to remove bubbles in vacuum for 5-20 min under the condition of 20-100 kPa.
5. The flexible deep processing method of copper-molybdenum-copper composite material with bending dimension requirement according to claim 1, wherein in the step 2, the height clearance of the scraper is 5 um-0.1 mm, the baseband speed is 2.0-2.5 mm/s, and the drying temperature is 20-30 ℃.
6. The flexible deep processing method of copper-molybdenum-copper composite material with bending dimension requirement according to claim 1, wherein in step 3, the solid content of the copper paste for printing is 50-80%.
7. The flexible deep processing method of copper-molybdenum-copper composite material with bending dimension requirement according to claim 1, wherein in the step 3, the organic carrier is any one or more of terpineol, isopropanol, tributyl phthalate, ethylcellulose, toluene, terephthalic acid and castor oil.
8. The flexible deep processing method of copper-molybdenum-copper composite material with bending dimension requirement according to claim 1, wherein in step 3, the screen printing method is as follows: firstly, printing copper paste on one side, drying, and then printing the other side, wherein the thickness of the screen printing single layer is 0.1-10 mu m.
9. The flexible deep processing method of the copper-molybdenum-copper composite material with the bending dimension requirement according to claim 1, wherein the hot isostatic pressing is any one of a hydrothermal isostatic pressing method and an oil-medium isostatic pressing method; the temperature of the hot isostatic pressing is 60-120 ℃, the pressure is 2000-5000 PSI, and the pressure maintaining temperature is 60-100 ℃; the degumming is carried out in the atmosphere of hydrogen or nitrogen, the temperature of glue discharging is 300-600 ℃, and the time of glue discharging is 8-24 hours; the temperature of the integrated cofiring is 800-1200 ℃, and the time of the integrated cofiring is 2-4 hours.
10. A copper-molybdenum-copper composite with bending dimension requirements prepared by the flexible deep processing method of the copper-molybdenum-copper composite with bending dimension requirements of any one of claims 1-9.
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