CN107868966A - Copper alloy porous wick structure and preparation method thereof - Google Patents

Copper alloy porous wick structure and preparation method thereof Download PDF

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Publication number
CN107868966A
CN107868966A CN201711136869.9A CN201711136869A CN107868966A CN 107868966 A CN107868966 A CN 107868966A CN 201711136869 A CN201711136869 A CN 201711136869A CN 107868966 A CN107868966 A CN 107868966A
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substrate
current density
preparation
porous wick
wick structure
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CN201711136869.9A
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CN107868966B (en
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于全耀
李柏霖
王治平
邱俊隆
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In Reach Electronics (jiangsu) Co Ltd
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In Reach Electronics (jiangsu) Co Ltd
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Priority to TW106144627A priority patent/TWI638068B/en
Publication of CN107868966A publication Critical patent/CN107868966A/en
Priority to US15/956,719 priority patent/US20190145015A1/en
Priority to JP2018109099A priority patent/JP6704432B2/en
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/60Electroplating characterised by the structure or texture of the layers
    • C25D5/623Porosity of the layers
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/38Electroplating: Baths therefor from solutions of copper
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/18Electroplating using modulated, pulsed or reversing current
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34Pretreatment of metallic surfaces to be electroplated
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48After-treatment of electroplated surfaces
    • C25D5/50After-treatment of electroplated surfaces by heat-treatment
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28DHEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D15/00Heat-exchange apparatus with the intermediate heat-transfer medium in closed tubes passing into or through the conduit walls ; Heat-exchange apparatus employing intermediate heat-transfer medium or bodies
    • F28D15/02Heat-exchange apparatus with the intermediate heat-transfer medium in closed tubes passing into or through the conduit walls ; Heat-exchange apparatus employing intermediate heat-transfer medium or bodies in which the medium condenses and evaporates, e.g. heat pipes
    • F28D15/04Heat-exchange apparatus with the intermediate heat-transfer medium in closed tubes passing into or through the conduit walls ; Heat-exchange apparatus employing intermediate heat-transfer medium or bodies in which the medium condenses and evaporates, e.g. heat pipes with tubes having a capillary structure
    • F28D15/046Heat-exchange apparatus with the intermediate heat-transfer medium in closed tubes passing into or through the conduit walls ; Heat-exchange apparatus employing intermediate heat-transfer medium or bodies in which the medium condenses and evaporates, e.g. heat pipes with tubes having a capillary structure characterised by the material or the construction of the capillary structure

Abstract

The preparation method of one Albatra metal porous wick structure is provided, comprised the following steps:A) electrolyte is prepared, is the aqueous solution liquid for including 0.5 1.8mol/L sulfuric acid and 0.1 0.5mol/L copper sulphate;B) copper alloy substrate surface is cleaned using the mixed solution of surfactant and alkali compounds, then activated with watery hydrochloric acid, then cleaned up;C) by the substrate after processing in the electrolyte electro-deposition to form loose structure on the substrate;And product d) obtained to step c) is washed, after drying, sintering.Loose structure with specific configuration, with excellent capillary force and permeability can be directly obtained in substrate surface by the inventive method, be advantageous to working medium transmission.

Description

Copper alloy porous wick structure and preparation method thereof
Technical field
The present invention relates to soaking plate structure liquid sucting core structure, more particularly to a kind of through hole soaking prepared by soft template method Plate liquid-sucking core preparation method.
Background technology
With the development of science and technology, electronic product gradually tends to microminiaturization, because the function of electronic product is more and more, Its heat dissipation element is increasingly concentrated in smaller scope.Therefore the radiating of electronic product is product design and production and assembly process In an important issue must take into consideration.
The heat sinks electronic products parts such as the heat pipe invented by phase-change heat, soaking plate also arise at the historic moment, and in product Radiating well is provided in function to ensure.Also therefore, such radiating element creates high valency to manufacturer Value and profit.The heat radiation power of the radiating elements such as soaking plate is also urgently further to be improved.CN103542749A discloses one kind Bionical soaking plate liquid-sucking core, the liquid sucting core structure are advantageous to the transmission of working medium, improve the heat-sinking capability of soaking plate, but due to knot Structure is complex, it is necessary to use the complicated and expensive equipment such as photoetching.Patent of invention CN106435665A passes through electrochemical deposition Prepare it is a kind of have the dendritic micropin wing copper surface texture of natural multi-resolution tree as heat pipe or the liquid sucting core structure of soaking plate, but this Structure easily causes working medium and carried by air-flow, reduces heat transfer efficiency.And by electrochemical deposition method prepare loose structure with Substrate caking power is weak, and the problems such as mechanical strength difference, huge challenge is brought in terms of the reliability and life-span to product.
The content of the invention
To overcome disadvantage mentioned above and deficiency, it is an object of the invention to invent the preparation side of an Albatra metal porous wick structure Method, comprise the following steps:A) electrolyte is prepared, is include 0.5-1.8mol/L sulfuric acid and 0.1-0.5mol/L copper sulphate water-soluble Liquid liquid;B) copper alloy substrate surface is cleaned using the mixed solution of surfactant and alkali compounds, then with dilute salt Acid activation, then clean up;C) by the substrate after processing, electro-deposition is more to be formed on the substrate in the electrolyte Pore structure;And product d) obtained to step c) is washed, after drying, sintering.
According to an embodiment of the present invention, electro-deposition is carried out using constant current density mode, constant current density is 0.5-5A/cm2, sedimentation time 20s-10min.
According to another embodiment of the present invention, the current density is 0.8-1.5A/cm2, sedimentation time 50-90s.
According to another embodiment of the present invention, electro-deposition, starting electricity are carried out by the way of gradually increase current density Current density is 0.01-0.1A/cm2, current density speedup be 0.001-0.05A/cm2S, sedimentation time is 10s-10min.
According to another embodiment of the present invention, electro-deposition, starting electricity are carried out by the way of current density is gradually reduced Current density is 0.5-5A/cm2, current density reduce speed be 0.001-0.05A/cm2S, sedimentation time is 10s-10min.
According to another embodiment of the present invention, the substrate be brass, one-ton brass, ledrite, aldubra, nickel brass or Iron brass.
According to another embodiment of the present invention, the sintering is in protective atmosphere, reducing atmosphere or vacuum environment, temperature Sintered at 450-750 DEG C.
According to another embodiment of the present invention, the protective atmosphere is selected from least one of nitrogen, argon gas.It is described Reducing atmosphere is the gaseous mixture of nitrogen and hydrogen.
The present invention also provides an Albatra metal porous wick structure, is made up of the above method.
The porous wick structure that the present invention is prepared using the complex method of electro-deposition and sintering, fine copper prepared by electro-deposition are porous Structure passes through high-temperature process, and nanostructured has been carried out into rearrangement using nano effect, has enhanced its structural strength.The present invention Method can be used on variously-shaped heat pipe and soaking panel products, loose structure thickness can be adjusted in 10 μm of any of the above, New direction is provided for the personalized designs of product.It can be directly obtained by the inventive method in substrate surface with given row Cloth, there is the loose structure of excellent capillary force and permeability, be advantageous to working medium transmission.
Brief description of the drawings
Figure 1A is the stereoscan photograph that porous wick structure prepared by embodiment 1 inlays section.
Figure 1B is the Zn distribution diagram of element of porous wick structure prepared by embodiment 1.
Fig. 1 C are the Cu distribution diagram of element of porous wick structure prepared by embodiment 1.
Fig. 1 D are the component content distribution maps of porous wick structure prepared by embodiment 1.
Fig. 2A with Fig. 2 B are the stereoscan photographs of porous wick structure difference enlargement ratio prepared by embodiment 1.
Embodiment
The present invention is elaborated with reference to specific embodiment.But protection scope of the present invention is not limited to following realities Apply example.
Embodiment 1
A certain amount of copper sulphate is weighed, copper sulphate dissolving is formed into copper-bath in deionized water, then to sulfuric acid The proper amount of concentrated sulfuric acid is added in copper solution, obtains the electrolyte of 0.5mol/L sulfuric acid and 0.1mol/L copper sulphate.
Using H70 brass as substrate, substrate is cleaned using the mixed solution of surfactant and alkali compounds, then Activated with watery hydrochloric acid, then cleaned up with deionized water.
Substrate after processing is subjected to electro-deposition in the solution of preparation using constant current density mode, with substrate Loose structure is formed, wherein electrodeposition temperature is 20 DEG C, current density 0.5A/cm2, time 10min.
Loose structure by substrate and thereon is washed, after drying, 450 DEG C of sintering in vacuum sintering furnace.
Embodiment 2
Electrolyte is prepared in the same manner as in Example 1, except the concentration of sulfuric acid is 1.8mol/L, the concentration of copper sulphate For 0.5mol/L.
Using iron brass as substrate, precondition substrate in the same manner as in Example 1.
Substrate after processing is subjected to electro-deposition in the solution of preparation using constant current density mode, with substrate Loose structure is formed, wherein electrodeposition temperature is room temperature, current density 0.8A/cm2, time 90s.
Loose structure by substrate and thereon is washed, after drying, 500 DEG C of sintering in vacuum sintering furnace.
Embodiment 3
Electrolyte is prepared in the same manner as in Example 1, except the concentration of sulfuric acid is 1.0mol/L, the concentration of copper sulphate For 0.2mol/L.
Using ledrite as substrate, precondition substrate in the same manner as in Example 1.
Substrate after processing is subjected to electro-deposition in the solution of preparation using constant current density mode, with substrate Loose structure is formed, wherein electrodeposition temperature is 20 DEG C, current density 1.5A/cm2, time 50s.
Loose structure by substrate and thereon is washed, after drying, 600 DEG C of sintering in vacuum sintering furnace.
Embodiment 4
Electrolyte is prepared in the same manner as in Example 1, except the concentration of sulfuric acid is 0.8mol/L, the concentration of copper sulphate For 0.2mol/L.
Using aldubra as substrate, precondition substrate in the same manner as in Example 1.
Substrate after processing is subjected to electro-deposition in the solution of preparation using constant current density mode, with substrate Loose structure is formed, wherein electrodeposition temperature is 20 DEG C, current density 5A/cm2, time 20s.
Loose structure by substrate and thereon is washed, after drying, 750 DEG C of sintering in vacuum sintering furnace.
Embodiment 5
Electrolyte is prepared in the same manner as in Example 1, except the concentration of sulfuric acid is 0.7mol/L, the concentration of copper sulphate For 0.3mol/L.
Using H68 brass as substrate, precondition substrate in the same manner as in Example 1.
Substrate after processing is subjected to electro-deposition in the solution of preparation using constant current density mode, with substrate Loose structure is formed, wherein electrodeposition temperature is 20 DEG C, current density 1A/cm2, time 1min.
Loose structure by substrate and thereon is washed, after drying, 700 DEG C of sintering in vacuum sintering furnace.
Embodiment 6
Electrolyte is prepared in the same manner as in Example 1, except the concentration of sulfuric acid is 0.5mol/L, the concentration of copper sulphate For 0.1mol/L.
Using H70 brass as substrate, precondition substrate in the same manner as in Example 1.
Substrate after processing is subjected to electro-deposition in the solution of preparation by the way of current density is gradually reduced, with Loose structure is formed in substrate, wherein electrodeposition temperature is 20 DEG C, and initial current density is 0.5A/cm2, current density, which is slowed down, is 0.05A/cm2S, time 10s.
Loose structure by substrate and thereon is washed, after drying, 450 DEG C of sintering in vacuum sintering furnace.
Embodiment 7
Electrolyte is prepared in the same manner as in Example 1, except the concentration of sulfuric acid is 0.5mol/L, the concentration of copper sulphate For 0.1mol/L.
Using H70 brass as substrate, precondition substrate in the same manner as in Example 1.
Substrate after processing is subjected to electro-deposition in the solution of preparation by the way of current density is gradually reduced, with Loose structure is formed in substrate, wherein electrodeposition temperature is 20 DEG C, and initial current density is 2A/cm2, current density, which is slowed down, is 0.002A/cm2S, time 5min.
Loose structure by substrate and thereon is washed, after drying, 600 DEG C of sintering in vacuum sintering furnace.
Embodiment 8
Electrolyte is prepared in the same manner as in Example 1, except the concentration of sulfuric acid is 0.5mol/L, the concentration of copper sulphate For 0.1mol/L.
Using H70 brass as substrate, precondition substrate in the same manner as in Example 1.
Substrate after processing is subjected to electro-deposition in the solution of preparation by the way of current density is gradually reduced, with Loose structure is formed in substrate, wherein electrodeposition temperature is 20 DEG C, and initial current density is 5A/cm2, current density, which is slowed down, is 0.001A/cm2S, time 10min.
Loose structure by substrate and thereon is washed, after drying, 450 DEG C of sintering in vacuum sintering furnace.
Embodiment 9
Electrolyte is prepared in the same manner as in Example 1, except the concentration of sulfuric acid is 0.5mol/L, the concentration of copper sulphate For 0.1mol/L.
Using H70 brass as substrate, precondition substrate in the same manner as in Example 1.
By the substrate after processing in the solution of preparation using gradually increase current density by the way of carry out electro-deposition, with Loose structure is formed in substrate, wherein electrodeposition temperature is 20 DEG C, and initial current density is 0.01A/cm2, current density speedup For 0.05A/cm2S, time 10s.
Loose structure by substrate and thereon is washed, after drying, 450 DEG C of sintering in vacuum sintering furnace.
Embodiment 10
Electrolyte is prepared in the same manner as in Example 1, except the concentration of sulfuric acid is 0.5mol/L, the concentration of copper sulphate For 0.1mol/L.
Using H70 brass as substrate, precondition substrate in the same manner as in Example 1.
By the substrate after processing in the solution of preparation using gradually increase current density by the way of carry out electro-deposition, with Loose structure is formed in substrate, wherein electrodeposition temperature is 20 DEG C, and initial current density is 0.1A/cm2, current density speedup is 0.001A/cm2S, time 10min.
Loose structure by substrate and thereon is washed, after drying, 450 DEG C of sintering in vacuum sintering furnace.
Embodiment 11
Electrolyte is prepared in the same manner as in Example 1, except the concentration of sulfuric acid is 0.5mol/L, the concentration of copper sulphate For 0.1mol/L.
Using H70 brass as substrate, precondition substrate in the same manner as in Example 1.
By the substrate after processing in the solution of preparation using gradually increase current density by the way of carry out electro-deposition, with Loose structure is formed in substrate, wherein electrodeposition temperature is 20 DEG C, and initial current density is 0.2A/cm2, current density speedup is 0.005A/cm2S, time 5min.
Loose structure by substrate and thereon is washed, after drying, 450 DEG C of sintering in vacuum sintering furnace.
Figure 1A is the stereoscan photograph of porous wick structure prepared by embodiment 1, it can be seen that bright gray parts For liquid-sucking core agent structure;The distribution for element zinc that Figure 1B is shown, the distribution and presence of white dot representative element;Figure 1C is the distribution of elemental copper, the distribution and presence of gray corrosion representative element;Figure 1B and 1C illustrates that the porous wick structure is Ormolu form;Fig. 1 D are the component contents of the structure, can further prove the presence of ormolu.Above results proved that Zn-ef ficiency after oversintering in substrate, which is diffused into loose structure, forms ormolu.Fig. 2A and 2B is that embodiment 1 is made respectively The stereoscan photograph of standby porous wick structure surface difference enlargement ratio, Fig. 2A can be seen that the loose structure of liquid-sucking core;Figure 2B finds out that prism structure occurs in surface, and this proves that the Zn-ef ficiency diffusion after sintering in substrate causes.Due to substrate in sintering process In Zn-ef ficiency be diffused into loose structure and form ormolu, therefore increase the surface hydrophilicity of loose structure, so as to have Beneficial to transmission of the working medium in loose structure, and then improve radiating efficiency.
For other embodiments provided by the invention, products obtained therefrom result is same as Example 1 or similar, not another herein One repeats.
Certainly, the present invention can also have other various embodiments, ripe in the case of without departing substantially from spirit of the invention and its essence Know those skilled in the art when can be made according to the present invention it is various it is corresponding change and deformation, but these corresponding change and become Shape should all belong to the protection domain of appended claims of the invention.

Claims (9)

1. the preparation method of an Albatra metal porous wick structure, it is characterised in that comprise the following steps:
A) electrolyte is prepared, is the aqueous solution liquid for including 0.5-1.8mol/L sulfuric acid and 0.1-0.5mol/L copper sulphate;
B) copper alloy substrate surface is cleaned using the mixed solution of surfactant and alkali compounds, then uses watery hydrochloric acid Activation, is then cleaned up;
C) by the substrate after processing in the electrolyte electro-deposition to form loose structure on the substrate;And
D) product obtained to step c) is washed, after drying, sintering.
2. the preparation method of copper alloy porous wick structure according to claim 1, it is characterised in that close using constant current Degree mode carries out electro-deposition, constant current density 0.5-5A/cm2, sedimentation time 20s-10min.
3. the preparation method of copper alloy porous wick structure according to claim 2, it is characterised in that the current density is 0.8-1.5A/cm2, sedimentation time 50-90s.
4. the preparation method of copper alloy porous wick structure according to claim 1, it is characterised in that using gradually increase electricity The mode of current density carries out electro-deposition, and initial current density is 0.01-0.1A/cm2, current density speedup be 0.001-0.05A/ cm2S, sedimentation time is 10s-10min.
5. the preparation method of copper alloy porous wick structure according to claim 1, it is characterised in that use and be gradually reduced electricity The mode of current density carries out electro-deposition, and initial current density is 0.5-5A/cm2, current density reduce speed be 0.001- 0.05A/cm2S, sedimentation time is 10s-10min.
6. the preparation method of copper alloy porous wick structure according to claim 1, it is characterised in that the substrate is Huang Copper, one-ton brass, ledrite, aldubra, nickel brass or iron brass.
7. the preparation method of copper alloy porous wick structure according to claim 1, it is characterised in that the sintering is to protect Sintered at shield atmosphere, reducing atmosphere or vacuum environment, 450-750 DEG C of temperature.
8. the preparation method of copper alloy porous wick structure according to claim 7, it is characterised in that the protective atmosphere is Selected from least one of nitrogen, argon gas;The reducing atmosphere is the gaseous mixture of nitrogen and hydrogen.
A 9. Albatra metal porous wick structure, it is characterised in that be made up of the either method described in claim 1-8.
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CN201711136869.9A CN107868966B (en) 2017-11-16 2017-11-16 Copper alloy porous wick structure and preparation method thereof
TW106144627A TWI638068B (en) 2017-11-16 2017-12-19 Copper alloy porous wick and preparation method thereof
US15/956,719 US20190145015A1 (en) 2017-11-16 2018-04-18 Method for preparing porous copper alloy wick and product prepared by the same
JP2018109099A JP6704432B2 (en) 2017-11-16 2018-06-07 Copper alloy porous liquid absorbent core and method for producing the same

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CN108914178A (en) * 2018-09-19 2018-11-30 江西华度电子新材料有限公司 A method of it is uneven to solve galvanoplastic preparation wick thickness
CN112522747A (en) * 2020-11-19 2021-03-19 瑞声科技(南京)有限公司 Preparation method of upper cover plate of vapor chamber and vapor chamber
CN113388753A (en) * 2021-06-22 2021-09-14 沈伟 Alloy with capillary structure and preparation method thereof
CN113587693A (en) * 2021-08-09 2021-11-02 中山大学 Ultrathin bionic forest-shaped liquid absorption core structure with high capillary performance and preparation method thereof
CN113954494A (en) * 2021-10-19 2022-01-21 江西广信新材料股份有限公司 Preparation method and application of liquid absorption core

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CN108914178A (en) * 2018-09-19 2018-11-30 江西华度电子新材料有限公司 A method of it is uneven to solve galvanoplastic preparation wick thickness
CN112522747A (en) * 2020-11-19 2021-03-19 瑞声科技(南京)有限公司 Preparation method of upper cover plate of vapor chamber and vapor chamber
CN112522747B (en) * 2020-11-19 2022-01-07 瑞声科技(南京)有限公司 Preparation method of upper cover plate of vapor chamber and vapor chamber
CN113388753A (en) * 2021-06-22 2021-09-14 沈伟 Alloy with capillary structure and preparation method thereof
CN113388753B (en) * 2021-06-22 2022-01-04 沈伟 Alloy with capillary structure and preparation method thereof
CN113587693A (en) * 2021-08-09 2021-11-02 中山大学 Ultrathin bionic forest-shaped liquid absorption core structure with high capillary performance and preparation method thereof
CN113954494A (en) * 2021-10-19 2022-01-21 江西广信新材料股份有限公司 Preparation method and application of liquid absorption core

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