CN112247152B - Preparation method of super-hydrophilic foam copper with capillary effect and sandwich structure - Google Patents
Preparation method of super-hydrophilic foam copper with capillary effect and sandwich structure Download PDFInfo
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- CN112247152B CN112247152B CN202011147623.3A CN202011147623A CN112247152B CN 112247152 B CN112247152 B CN 112247152B CN 202011147623 A CN202011147623 A CN 202011147623A CN 112247152 B CN112247152 B CN 112247152B
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- 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
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/002—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of porous nature
- B22F7/004—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of porous nature comprising at least one non-porous part
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- 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
- B22F3/11—Making porous workpieces or articles
- B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
- B22F3/1134—Inorganic fillers
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Abstract
The invention discloses a preparation method of sandwich structure super-hydrophilic copper with capillary effect, which comprises the following steps: uniformly mixing copper powder, ammonium chloride and deionized water, and then carrying out vacuum defoaming to form a viscous mixture W1 for later use; processing a copper foil to form a flat-bottom groove in the middle of the copper foil to obtain a first plate body; pouring the viscous mixture W1 into the flat-bottom groove to completely fill the flat-bottom groove, and then uniformly paving a nano copper soldering paste layer on the copper foil part around the flat-bottom groove; two plate bodies are superposed to form a sandwich structure; and (3) heating the sandwich structure to 350-360 ℃ in a protective atmosphere environment containing hydrogen, keeping the temperature, continuously heating to 900-920 ℃ for keeping the temperature, continuously heating to 1000-1020 ℃ for keeping the temperature, and cooling to obtain the composite material. The method realizes one-step sintering molding, has simple process, short flow and low cost, can obtain the super hydrophilic copper with the sandwich structure, good product quality and structural stability, high yield and excellent capillary effect, and can be widely used as gas-liquid phase change heat transfer and radiation components, water absorption materials and the like.
Description
Technical Field
The invention relates to the technical field of heat and mass transfer, in particular to a preparation method of super-hydrophilic copper with a capillary effect and a sandwich structure.
Background
In recent years, with the breakthrough of integrated circuit technology, semiconductor technology and electronic component quality, the development of high performance, miniaturization and integration in the electronic industry is directly faced with the problem of heat dissipation. Electronic components, assemblies, circuit boards, circuits, etc. do not operate reliably at higher temperatures, even shortening their operating life. Copper is widely used in the field of heat transfer and dissipation because of its good heat-conducting property. However, pure copper as a heat sink has not been able to meet the current heat dissipation requirements. On the basis, a copper-based heat pipe and a soaking plate are developed by combining gas-liquid phase change heat transfer of working medium water.
At present, a vapor chamber mainly comprises a cavity (such as a copper pipe and a copper box), a capillary structure (a sintering layer, a silk screen or a groove) and a working medium (water, ethanol and the like), wherein the capillary structure is a key structure which directly influences heat transfer efficiency. At present, the capillary structures in the soaking plates on the market comprise wire mesh fibers, copper powder particles, foam copper and the like, and generally adopt stainless steel wire meshes as the capillary structures, but the porosity of the stainless steel wire meshes is only about 30%, and the connectivity of pores is not good, so that the stainless steel wire meshes are not beneficial to the flowing of refrigerating liquid. If pure copper or pure copper powder sintering process is adopted as the capillary structure, the porosity of more than 50 percent can be ensured, and the capillary structure has better capillary force, but the hydrophilicity is unstable. Moreover, the existing soaking plate process technology is complex, a series of process procedures such as cutting, electroplating, stamping, welding, surface treatment, high-temperature sintering, liquid injection, packaging, testing and the like are required, even two to three times of welding are required, and the excessive process procedures and technical requirements make the quality of the finished soaking plate difficult to guarantee, the stability is poor, the yield is low, and the cost is high.
Therefore, the preparation of a heat dissipation structure with low cost, simple process, high porosity and high permeability is still an urgent problem to be solved in the industry.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the preparation method of the sandwich structure super-hydrophilic copper is simple in process, short in flow, low in cost, good in product quality and structure stability, high in yield and excellent in capillary effect.
The solution of the invention is realized by the following steps:
a preparation method of super-hydrophilic copper with a capillary effect and a sandwich structure comprises the following steps:
(1) copper powder, ammonium chloride and deionized water are mixed and stirred uniformly, and then vacuum defoaming is carried out to form a viscous mixture W1 for later use;
(2) processing a copper foil to form a flat-bottom groove structure in the middle of the copper foil to obtain a first plate body, wherein an outlet is reserved on the first plate body and is used as a gas channel or a liquid injection port;
(3) pouring the viscous mixture W1 into the flat-bottom groove structure, completely filling the flat-bottom groove, compacting and flattening (middle layer), and then uniformly paving a nano copper paste layer on the copper foil part around the flat-bottom groove except the reserved outlet;
(4) a second plate body is taken to be overlapped with the first plate body, and the first plate body, the middle layer and the second plate body are overlapped to form a sandwich structure;
(5) heating the sandwich structure to 350-360 ℃ in a protective atmosphere environment containing hydrogen, preserving heat to enable water and ammonium chloride to be completely volatilized and sublimated, then continuously heating to 900-920 ℃ and preserving heat, removing an oxide layer through reaction with the hydrogen, enabling an upper plate and a lower plate to be firmly connected through copper paste, continuously heating to 1000-1020 ℃ and preserving heat to enable foamy copper formed in the middle to be fully recrystallized, and cooling to obtain the super-hydrophilic copper with the capillary effect.
In the scheme, a flat-bottom groove structure with a low middle part and high periphery can be formed by mechanically stamping a common copper foil; the shape of the part of the flat-bottom groove structure can be set according to the requirement, and the opening shape of the flat-bottom groove can be a rectangle, a square or any required special-shaped structural pattern.
Preferably, in the viscous mixture W1, the amounts of the copper powder, the ammonium chloride and the deionized water are 80-85 parts, 10-20 parts and 5-10 parts in sequence.
Preferably, the particle size of the copper powder is 200-500 nm.
Preferably, in the step (4), the temperature is slowly increased to 350-360 ℃ at the speed of 8-10 ℃/min; heating to 350-360 ℃, and then keeping the temperature for 1-2 hours; heating to 900-920 ℃, and then keeping the temperature for 1-2 hours; the temperature is raised to 1000-1020 ℃ and the heat preservation time is 1-2 hours.
Preferably, the second board body can be a plane copper foil or a copper foil with a flat-bottom stamping groove structure which is symmetrical to the first board body; and a corresponding outlet is reserved at the position of the second plate body corresponding to the outlet of the first plate body.
Preferably, when the second board body is a copper foil with a punched flat-bottom groove structure, which is symmetrical to the first board body, step (4) further includes, before the first board body and the second board body are stacked together: copper powder, ammonium chloride and deionized water are mixed and stirred uniformly, then vacuum defoaming is carried out to form a viscous mixture W2, the viscous mixture is poured into the flat-bottom groove structure of the second plate body, the groove is completely filled, and the second plate body is compacted and flattened.
Preferably, the capillary attraction of the capillary effect can be adjusted by the pore size of the copper powder in the viscous mixture, and the pore size can be adjusted by the content of ammonium chloride in the viscous mixture.
Preferably, in the step (3), the thickness of the nano-copper paste layer is 100 μm or less.
Preferably, in the step (5), the hydrogen-containing protective atmosphere contains a mixed gas of hydrogen and nitrogen; the protective atmosphere containing hydrogen is a vacuum container filled with hydrogen and nitrogen, and the vacuum container can be a vacuum tube furnace.
Preferably, the amount of the copper powder, the ammonium chloride and the deionized water in the viscous mixture W2 is 80-85 parts, 10-20 parts and 5-10 parts in sequence.
Compared with the prior art, the invention has the following advantages:
(1) the method can simultaneously realize the connection between the upper plate and the lower plate of the copper with the sandwich structure, the formation of the copper foam, the connection between the copper foam and the upper plate and the lower plate, the support between the upper plate and the lower plate, the acquisition of the super-hydrophilic and capillary forces, and the integrated sintering forming is realized, and the super-hydrophilic copper with the sandwich structure prepared by the method has excellent capillary effect, has stronger hydrophilicity compared with the sandwich structure prepared by the prior method, and the connection among the components is more stable, the product quality and the structure stability are good, the yield is high, the uniformly distributed copper foam formed in the product is a penetrating porous foam structure, has excellent hydrophilicity and capillary effect, can be widely used as a gas-liquid phase change heat-transfer heat-dissipation component, a water absorption material and the like, is integrally formed with the upper plate and the lower plate, has mechanical strength, and can play a supporting role, the upper plate and the lower plate are prevented from being contacted together due to uneven stress, so that the compression strength is better, and the overall heat transfer performance is more stable.
(2) The pore size and the pore size distribution of the interlayer of the sandwich structure copper are convenient to adjust, so that the hydrophilicity and the capillary attraction are easily adjusted according to needs, and the practicability is extremely strong.
(3) The shape of the copper in the sandwich structure can be adjusted according to the requirement without limiting the geometrical shape.
(4) Compared with the existing method, the preparation method provided by the invention has the advantages of simpler and more convenient process, low cost, strong flexibility and controllability, high practicability and suitability for large-scale production.
Drawings
Fig. 1 is a structural view of super-hydrophilic copper having a sandwich structure in which an upper plate prepared in example 1 is a planar copper foil.
Fig. 2 is a structural diagram of super-hydrophilic copper with a sandwich structure in which the upper plate and the lower plate prepared in example 2 are symmetrical groove structures.
Fig. 3 is a structural diagram of the super-hydrophilic copper with a sandwich structure, in which the upper plate and the lower plate prepared in example 3 are of symmetrical groove structures and the pore size of the middle layer of copper foam is adjustable.
Reference numerals:
firstly, a plate is arranged; ② a nano copper-tin paste layer; thirdly, the plate is arranged; and fourthly, crystallizing the foamy copper.
Detailed Description
The description is to be regarded as illustrative and explanatory only and should not be taken as limiting the scope of the invention in any way. Furthermore, those skilled in the art can combine features from the embodiments of this document and from different embodiments accordingly based on the description of this document.
Example 1:
a preparation method of super-hydrophilic copper with a capillary effect and a sandwich structure comprises the following steps:
(1) according to parts by weight, 80 parts of copper powder with the average particle size of 400nm, 10 parts of ammonium chloride and 5 parts of deionized water are mixed and stirred uniformly, and then vacuum defoaming is carried out to form a viscous mixture for later use.
(2) And mechanically stamping the common copper foil to form a flat-bottom groove structure with a low middle part and high periphery as a lower plate. An outlet is reserved on the edge of the groove structure of the lower plate and is used as a gas channel or a liquid injection port.
(3) The sticky mixture is poured into the groove of the lower plate (r), the groove is completely filled, and the mixture is compacted and flattened (middle layer).
(4) Uniformly paving a thin nano copper paste layer around the upper surface of the lower plate (except the reserved outlet); the other plane copper foil (upper plate) with the same size and without stamping is horizontally placed right above the lower plate I, so that the plane copper foil and the lower plate I are completely overlapped together, the lower plate I, the middle layer and the upper plate together form a sandwich structure, and an outlet is reserved in the position of the upper plate III corresponding to the reserved outlet of the lower plate I.
(5) Putting the sandwich structure into a vacuum tube furnace filled with nitrogen and hydrogen protective gas, slowly heating to 350-360 ℃ at the speed of 8-10 ℃/min, and keeping for 1h to completely volatilize and sublimate water and ammonium chloride; continuously heating to 900-920 ℃ in a vacuum tube furnace, preserving heat for 1-2 hours, removing an oxide layer through reaction with hydrogen, and firmly connecting an upper plate and a lower plate through copper soldering paste; continuously heating to 1000-1020 ℃ in a vacuum tube furnace and preserving heat for 1h to fully recrystallize the foamy copper formed in the middle to obtain crystalline foamy copper; cooling to room temperature, and taking out to obtain the final product with capillary effect and sandwich structure of super hydrophilic copper, with a schematic structure diagram shown in figure 1.
Example 2:
a preparation method of super-hydrophilic copper with a capillary effect and a sandwich structure comprises the following steps:
(1) according to parts by weight, 80 parts of copper powder with the average particle size of 400nm, 10 parts of ammonium chloride and 5 parts of deionized water are mixed and stirred uniformly, and then vacuum defoaming is carried out to form a viscous mixture for later use.
(2) And mechanically stamping the common copper foil to form a flat-bottom groove structure with a low middle part and high periphery as a lower plate. An outlet is reserved on the edge of the flat-bottom groove structure of the lower plate and is used as a gas channel or a liquid injection port.
(3) Pouring a viscous mixture into the groove of the lower plate I, completely filling the groove, and compacting and flattening (an intermediate layer); a thin nano copper paste layer is uniformly laid on the periphery of the upper surface of the lower plate (except the reserved outlet).
(4) Similarly, a sticky mixture is poured into the groove of the other symmetrical and punched copper foil (the upper plate III), the groove is completely filled, compacted and flattened (the middle layer), an outlet is reserved at the position corresponding to the reserved outlet of the lower plate I, and then the lower plate I, the middle layer and the upper plate III are horizontally placed right above the lower plate I to be completely overlapped with the lower plate I, so that a sandwich structure is formed by the lower plate I, the middle layer and the upper plate III.
(5) Putting the sandwich structure into a vacuum tube furnace filled with nitrogen and hydrogen protective gas, slowly heating to 350-360 ℃ at the speed of 8-10 ℃/min, and keeping for 1h to completely volatilize and sublimate water and ammonium chloride; continuously heating to 900-920 ℃ in a vacuum tube furnace, preserving heat for 1-2 hours, removing an oxide layer through reaction with hydrogen, and firmly connecting an upper plate and a lower plate through copper soldering paste; continuously heating to 1000-1020 ℃ in a vacuum tube furnace and preserving heat for 1h to fully recrystallize the foamy copper formed in the middle to obtain crystalline foamy copper; cooling to room temperature, and taking out to obtain the final product with capillary effect and sandwich structure of super hydrophilic copper, with a schematic structure diagram shown in figure 2.
Example 3:
a preparation method of super-hydrophilic copper with a capillary effect and a sandwich structure comprises the following steps:
(1) according to parts by weight, 80 parts of copper powder with the average particle size of 400nm, 10 parts of ammonium chloride and 5 parts of deionized water are mixed and stirred uniformly, and then vacuum defoaming is carried out to form a viscous mixture W1.
(2) And mechanically stamping the common copper foil to form a flat-bottom groove structure with a low middle part and high periphery as a lower plate. An outlet (the periphery of the flat-bottom groove, namely the side face) is reserved at the edge of the flat-bottom groove structure of the lower plate and is used as a gas channel or a liquid injection port.
(3) Pouring a viscous mixture W1 into the groove of the lower plate I, completely filling the groove, and compacting and flattening (an intermediate layer); a thin nano copper paste layer is uniformly laid on the periphery of the upper surface of the lower plate (except the reserved outlet).
(4) Similarly, 80 parts by weight of copper powder with the average particle size of 400nm, 20 parts by weight of ammonium chloride and 5 parts by weight of deionized water are mixed and stirred uniformly, and then vacuum defoaming is carried out to form a viscous mixture W2; pouring a viscous mixture W2 into the groove of the other symmetrical and punched copper foil (upper plate III), completely filling the groove, compacting and flattening (middle layer), reserving an outlet at the position corresponding to the reserved outlet of the lower plate I, and then horizontally placing the lower plate I right above the lower plate I to completely overlap the lower plate I, so that the lower plate I, the middle layer and the upper plate III form a sandwich structure.
(5) Putting the sandwich structure into a vacuum tube furnace filled with nitrogen and hydrogen protective gas, slowly heating to 350-360 ℃ at the speed of 8-10 ℃/min, and keeping for 1h to completely volatilize and sublimate water and ammonium chloride; continuously heating to 900-920 ℃ in a vacuum tube furnace, preserving heat for 1-2 hours, removing an oxide layer through reaction with hydrogen, and firmly connecting an upper plate and a lower plate through copper soldering paste; continuously heating to 1000-1020 ℃ in a vacuum tube furnace and preserving heat for 1h to fully recrystallize the foamy copper formed in the middle to obtain crystalline foamy copper (IV), wherein the lower part of the crystalline foamy copper (IV) is small-aperture crystalline foamy copper, and the upper part of the crystalline foamy copper (IV) is large-aperture crystalline foamy copper; cooling to room temperature, and taking out to obtain the final product with capillary effect and sandwich structure of super hydrophilic copper, with a schematic structure diagram shown in figure 3.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A preparation method of super-hydrophilic copper with a capillary effect and a sandwich structure is characterized by comprising the following steps:
(1) copper powder, ammonium chloride and deionized water are mixed and stirred uniformly, and then vacuum defoaming is carried out to form a viscous mixture W1 for later use;
(2) processing a copper foil to form a flat-bottom groove structure in the middle of the copper foil to obtain a first plate body, and reserving an outlet on the first plate body to serve as a gas channel or a liquid injection port;
(3) pouring the viscous mixture W1 into the flat-bottom groove structure, completely filling the flat-bottom groove, compacting and flattening, and then uniformly paving a nano copper soldering paste layer on the copper foil part around the flat-bottom groove; the thickness of the nano copper soldering paste layer is less than 100 mu m;
(4) a second plate body is taken to be overlapped with the first plate body to form a sandwich structure; the second plate body is a plane copper foil or a copper foil which is symmetrical to the first plate body and is provided with a flat-bottom stamping groove structure;
(5) and (3) slowly heating the sandwich structure to 350-360 ℃ at the speed of 8-10 ℃/min in a protective atmosphere environment containing hydrogen, preserving heat for 1-2 hours, then continuously heating to 900-920 ℃ and preserving heat for 1-2 hours, continuously heating to 1000-1020 ℃ and preserving heat for 1-2 hours, and cooling to obtain the super-hydrophilic copper with the sandwich structure and the capillary effect.
2. The method for preparing capillary-effect sandwich-structured super-hydrophilic copper according to claim 1, wherein the amount of the copper powder, the ammonium chloride and the deionized water in the viscous mixture W1 is 80-85 parts, 10-20 parts and 5-10 parts in sequence.
3. The method for preparing the capillary-effect sandwich-structure super-hydrophilic copper according to claim 1, wherein the particle size of the copper powder is 200-500 nm.
4. The method for preparing the super-hydrophilic copper with the capillary effect and the sandwich structure according to any one of claims 1 to 3, wherein the second plate body is provided with a corresponding outlet at a position corresponding to the outlet of the first plate body.
5. The method for preparing super-hydrophilic copper with a capillary effect sandwich structure according to claim 4, wherein when the second plate body is a copper foil with a punched flat-bottom groove structure symmetrical to the first plate body, the step (4) further comprises, before the first plate body and the second plate body are laminated together: copper powder, ammonium chloride and deionized water are mixed and stirred uniformly, then vacuum defoaming is carried out to form a viscous mixture W2, the viscous mixture is poured into the flat-bottom groove structure of the second plate body, the groove is completely filled, and the second plate body is compacted and flattened.
6. The method for preparing the sandwich structured super-hydrophilic copper with capillary effect according to any one of claims 1 to 3, wherein the protective atmosphere containing hydrogen is a vacuum container containing hydrogen and nitrogen.
7. The method for preparing capillary-effect sandwich-structured super-hydrophilic copper according to claim 5, wherein the amount of the copper powder, the ammonium chloride and the deionized water in the viscous mixture W2 is 80-85 parts, 10-20 parts and 5-10 parts in sequence.
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| CN110328367A (en) * | 2019-06-21 | 2019-10-15 | 延安速源节能科技有限公司 | A kind of preparation method of porous copper-based material |
| CN110763061A (en) * | 2019-10-31 | 2020-02-07 | 东莞市合众导热科技有限公司 | Vapor chamber and processing method thereof |
| CN111599693A (en) * | 2019-02-20 | 2020-08-28 | 中科院微电子研究所昆山分所 | Bonding method |
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2020
- 2020-10-23 CN CN202011147623.3A patent/CN112247152B/en active Active
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| WO2009049397A1 (en) * | 2007-10-19 | 2009-04-23 | Metafoam Technologies Inc. | Heat management device using inorganic foam |
| CN102818467A (en) * | 2012-09-12 | 2012-12-12 | 锘威科技(深圳)有限公司 | Flat plate heating pipe and manufacturing method thereof |
| CN105547026A (en) * | 2015-12-25 | 2016-05-04 | 江苏宏力光电科技股份有限公司 | Thermal column processing method |
| CN111599693A (en) * | 2019-02-20 | 2020-08-28 | 中科院微电子研究所昆山分所 | Bonding method |
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