CN107868966B - Copper alloy porous wick structure and preparation method thereof - Google Patents
Copper alloy porous wick structure and preparation method thereof Download PDFInfo
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- CN107868966B CN107868966B CN201711136869.9A CN201711136869A CN107868966B CN 107868966 B CN107868966 B CN 107868966B CN 201711136869 A CN201711136869 A CN 201711136869A CN 107868966 B CN107868966 B CN 107868966B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/60—Electroplating characterised by the structure or texture of the layers
- C25D5/623—Porosity of the layers
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/18—Electroplating using modulated, pulsed or reversing current
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
- F28D15/00—Heat-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
- F28D15/02—Heat-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
- F28D15/04—Heat-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
- F28D15/046—Heat-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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Sustainable Development (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The preparation method of one Albatra metal porous wick structure is provided, includes the following steps: a) to prepare electrolyte, 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 is activated with dilute hydrochloric acid, then cleaned up;C) will treated substrate in the electrolyte electro-deposition to form porous structure on the substrate;And after d) washing to the product that step c) is obtained, be dry, sintering.Porous structure with specific configuration, with excellent capillary force and permeability can be directly obtained in substrate surface by the method for the invention, be conducive to working medium transmission.
Description
Technical field
The present invention relates to soaking plate structure liquid sucting core structure, in particular to a kind of through-hole soaking prepared by soft template method
Plate liquid-sucking core preparation method.
Background technique
With the development of science and technology, electronic product gradually tends to microminiaturization, since the function of electronic product is more and more,
Its heat dissipation element increasingly concentrates in smaller range.Therefore the heat dissipation of electronic product is product design and production and assembly process
In an important issue must be taken into consideration.
The heat sinks electronic products part such as heat pipe, soaking plate for inventing by phase-change heat also comes into being, and in product
Heat dissipation well is provided in function to guarantee.Also therefore, suchlike radiating element creates high valence 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 conducive to the transmission of working medium, improve the heat-sinking capability of soaking plate, but due to knot
Structure is complex, needs to use the complicated and expensive equipment such as photoetching.Patent of invention CN106435665A passes through electrochemical deposition
Prepare it is a kind of with 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 should
Structure be easy to cause working medium to be carried by air-flow, reduces heat transfer efficiency.And by electrochemical deposition method prepare porous structure with
The problems such as substrate caking power is weak, and mechanical strength is poor, reliability and service life aspect to product bring huge challenge.
Summary 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 includes the following steps: a) to prepare electrolyte, 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
Then acid activation cleans up;C) by treated, substrate electro-deposition in the electrolyte is more to be formed on the substrate
Pore structure;And after d) washing to the product that step c) is obtained, be dry, 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.
Another embodiment according to the present invention, the current density are 0.8-1.5A/cm2, sedimentation time 50-90s.
Another embodiment according to the present invention carries out electro-deposition, starting electricity by the way of being gradually increased current density
Current density is 0.01-0.1A/cm2, current density speedup be 0.001-0.05A/cm2S, sedimentation time is 10s-10min.
Another embodiment according to the present invention carries out electro-deposition, starting electricity by the way of being gradually reduced current density
Current density is 0.5-5A/cm2, current density reduce speed be 0.001-0.05A/cm2S, sedimentation time is 10s-10min.
Another embodiment according to the present invention, the substrate be brass, one-ton brass, ledrite, aldubra, nickel brass or
Iron brass.
Another embodiment according to the present invention, the sintering is in protective atmosphere, reducing atmosphere or vacuum environment, temperature
It is sintered at 450-750 DEG C.
Another embodiment according to the present invention, the protective atmosphere are 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 structures, are made of the above method.
The fine copper of the porous wick structure that the present invention is prepared using the complex method of electro-deposition and sintering, electro-deposition preparation is porous
Structure passes through high-temperature process, and nanostructure has been carried out rearrangement using nano effect, has enhanced its structural strength.The present invention
Method can be used on heat pipe of various shapes and soaking panel products, porous 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 directly obtain by the method for the invention in substrate surface with given row
Cloth, porous structure with excellent capillary force and permeability are conducive to working medium transmission.
Detailed description of the invention
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 is the Cu distribution diagram of element of porous wick structure prepared by embodiment 1.
Fig. 1 D is the component content distribution map of porous wick structure prepared by embodiment 1.
Fig. 2A with Fig. 2 B is the stereoscan photograph of porous wick structure difference enlargement ratio prepared by embodiment 1.
Specific embodiment
The present invention will be described in detail below with reference to specific embodiments.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 dissolution 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
It is activated with dilute hydrochloric acid, is then cleaned up with deionized water.
By treated, substrate carries out electro-deposition using constant current density mode in the solution of preparation, in substrate
Porous structure is formed, wherein electrodeposition temperature is 20 DEG C, current density 0.5A/cm2, time 10min.
After porous structure by substrate and thereon is washed, is dry, 450 DEG C of sintering in vacuum sintering furnace.
Embodiment 2
Electrolyte is prepared in the same manner as in Example 1, in addition to 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.
By treated, substrate carries out electro-deposition using constant current density mode in the solution of preparation, in substrate
Porous structure is formed, wherein electrodeposition temperature is room temperature, current density 0.8A/cm2, time 90s.
After porous structure by substrate and thereon is washed, is dry, 500 DEG C of sintering in vacuum sintering furnace.
Embodiment 3
Electrolyte is prepared in the same manner as in Example 1, in addition to 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.
By treated, substrate carries out electro-deposition using constant current density mode in the solution of preparation, in substrate
Porous structure is formed, wherein electrodeposition temperature is 20 DEG C, current density 1.5A/cm2, time 50s.
After porous structure by substrate and thereon is washed, is dry, 600 DEG C of sintering in vacuum sintering furnace.
Embodiment 4
Electrolyte is prepared in the same manner as in Example 1, in addition to 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.
By treated, substrate carries out electro-deposition using constant current density mode in the solution of preparation, in substrate
Porous structure is formed, wherein electrodeposition temperature is 20 DEG C, current density 5A/cm2, time 20s.
After porous structure by substrate and thereon is washed, is dry, 750 DEG C of sintering in vacuum sintering furnace.
Embodiment 5
Electrolyte is prepared in the same manner as in Example 1, in addition to 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.
By treated, substrate carries out electro-deposition using constant current density mode in the solution of preparation, in substrate
Porous structure is formed, wherein electrodeposition temperature is 20 DEG C, current density 1A/cm2, time 1min.
After porous structure by substrate and thereon is washed, is dry, 700 DEG C of sintering in vacuum sintering furnace.
Embodiment 6
Electrolyte is prepared in the same manner as in Example 1, in addition to 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 treated, substrate carries out electro-deposition in the solution of preparation by the way of being gradually reduced current density, with
Porous 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.
After porous structure by substrate and thereon is washed, is dry, 450 DEG C of sintering in vacuum sintering furnace.
Embodiment 7
Electrolyte is prepared in the same manner as in Example 1, in addition to 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 treated, substrate carries out electro-deposition in the solution of preparation by the way of being gradually reduced current density, with
Porous 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.
After porous structure by substrate and thereon is washed, is dry, 600 DEG C of sintering in vacuum sintering furnace.
Embodiment 8
Electrolyte is prepared in the same manner as in Example 1, in addition to 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 treated, substrate carries out electro-deposition in the solution of preparation by the way of being gradually reduced current density, with
Porous 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.
After porous structure by substrate and thereon is washed, is dry, 450 DEG C of sintering in vacuum sintering furnace.
Embodiment 9
Electrolyte is prepared in the same manner as in Example 1, in addition to 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 treated, substrate carries out electro-deposition in the solution of preparation by the way of being gradually increased current density, with
Porous 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.
After porous structure by substrate and thereon is washed, is dry, 450 DEG C of sintering in vacuum sintering furnace.
Embodiment 10
Electrolyte is prepared in the same manner as in Example 1, in addition to 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 treated, substrate carries out electro-deposition in the solution of preparation by the way of being gradually increased current density, with
Porous 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.
After porous structure by substrate and thereon is washed, is dry, 450 DEG C of sintering in vacuum sintering furnace.
Embodiment 11
Electrolyte is prepared in the same manner as in Example 1, in addition to 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 treated, substrate carries out electro-deposition in the solution of preparation by the way of being gradually increased current density, with
Porous 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.
After porous structure by substrate and thereon is washed, is dry, 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 from the figure that bright gray parts
For liquid-sucking core main structure;Figure 1B show be element zinc distribution, 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 is the component content 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 porous 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 porous structure of liquid-sucking core;Figure
2B finds out that prism structure occurs in surface, this proves that the Zn-ef ficiency diffusion after being sintered in substrate causes.Due to substrate in sintering process
In Zn-ef ficiency be diffused into porous structure and form ormolu, therefore increase the surface hydrophilicity of porous structure, to have
Conducive to transmission of the working medium in porous 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, without deviating from the spirit and substance of the present invention, ripe
It knows those skilled in the art and makes various corresponding changes and modifications, but these corresponding changes and change in accordance with the present invention
Shape all should fall within the scope of protection of the appended claims of the present invention.
Claims (3)
1. a kind of preparation method of ormolu porous wick structure, which comprises the steps of:
A) electrolyte is prepared, is the aqueous solution for including 0.5-1.8mol/L sulfuric acid and 0.1-0.5mol/L copper sulphate;
B) ormolu substrate surface is cleaned using the mixed solution of surfactant and alkali compounds, then with dilute salt
Then acid activation cleans up;
C) will treated substrate in the electrolyte electro-deposition to form porous structure on the substrate;And
D) after washing to the product that step c) is obtained, be dry, sintering;
Wherein the electro-deposition is carried out by the way of being gradually increased current density, and initial current density is 0.01-0.1A/cm2、
Current density speedup is 0.001-0.05A/cm2S, sedimentation time is 10s-10min;It is described to be sintered in vacuum environment, temperature
It is sintered at 450-750 DEG C of degree.
2. the preparation method of ormolu porous wick structure according to claim 1, which is characterized in that the substrate is Huang
Copper, one-ton brass, ledrite, aldubra, nickel brass or iron brass.
3. a kind of ormolu porous wick structure, which is characterized in that be made of either method claimed in claims 1-2.
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
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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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CN201711136869.9A CN107868966B (en) | 2017-11-16 | 2017-11-16 | Copper alloy porous wick structure and preparation method thereof |
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CN107868966B true CN107868966B (en) | 2019-08-13 |
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JP (1) | JP6704432B2 (en) |
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Cited By (1)
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CN110629258A (en) * | 2019-10-16 | 2019-12-31 | 东莞领杰金属精密制造科技有限公司 | Preparation method of porous copper liquid absorption core |
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CN107937943B (en) * | 2017-11-16 | 2019-04-26 | 中达电子(江苏)有限公司 | Porous wick structure and preparation method thereof |
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 |
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 |
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 |
CN114086229B (en) * | 2021-10-27 | 2022-11-25 | 中山市仲德科技有限公司 | Groove liquid for preparing liquid absorption core and preparation method of liquid absorption core |
CN113930807B (en) * | 2021-11-11 | 2023-03-31 | 中南大学 | Method for preparing copper-arsenic alloy by pulse electrodeposition |
CN115161647B (en) * | 2022-07-13 | 2023-07-21 | 江苏富乐华半导体科技股份有限公司 | Method for improving oxidation of copper surface of copper-clad ceramic substrate after welding |
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JP2012516941A (en) * | 2009-02-04 | 2012-07-26 | アプライド マテリアルズ インコーポレイテッド | Three-dimensional porous electrodes of copper, tin, copper tin, copper tin cobalt, and copper tin cobalt titanium for batteries and ultracapacitors |
CN103046088B (en) * | 2012-12-20 | 2015-08-26 | 华南理工大学 | A kind of micro-nano compound porous copper surface tissue and preparation method thereof and device |
CN103542749B (en) * | 2013-10-15 | 2015-10-28 | 华南理工大学 | A kind of bionical soaking plate liquid-sucking core |
CN103994682B (en) * | 2014-05-07 | 2016-01-13 | 江苏科技大学 | A kind of heat pipe and preparation method thereof |
CN205373480U (en) * | 2015-12-14 | 2016-07-06 | 上海利正卫星应用技术有限公司 | Ultra -thin heat pipe of high -efficient imbibition core |
CN105403085B (en) * | 2015-12-14 | 2018-05-04 | 上海利正卫星应用技术有限公司 | Variable element liquid-sucking core ultrathin heat pipe |
CN106435665B (en) * | 2016-09-18 | 2019-04-05 | 中山大学 | One kind having dendritic micropin wing copper surface texture of natural multi-resolution tree and preparation method thereof |
-
2017
- 2017-11-16 CN CN201711136869.9A patent/CN107868966B/en active Active
- 2017-12-19 TW TW106144627A patent/TWI638068B/en active
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2018
- 2018-04-18 US US15/956,719 patent/US20190145015A1/en not_active Abandoned
- 2018-06-07 JP JP2018109099A patent/JP6704432B2/en not_active Expired - Fee Related
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110629258A (en) * | 2019-10-16 | 2019-12-31 | 东莞领杰金属精密制造科技有限公司 | Preparation method of porous copper liquid absorption core |
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CN107868966A (en) | 2018-04-03 |
JP2019090100A (en) | 2019-06-13 |
US20190145015A1 (en) | 2019-05-16 |
TWI638068B (en) | 2018-10-11 |
JP6704432B2 (en) | 2020-06-03 |
TW201923155A (en) | 2019-06-16 |
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