CN106435665B - One kind having dendritic micropin wing copper surface texture of natural multi-resolution tree and preparation method thereof - Google Patents

One kind having dendritic micropin wing copper surface texture of natural multi-resolution tree and preparation method thereof Download PDF

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CN106435665B
CN106435665B CN201610828565.8A CN201610828565A CN106435665B CN 106435665 B CN106435665 B CN 106435665B CN 201610828565 A CN201610828565 A CN 201610828565A CN 106435665 B CN106435665 B CN 106435665B
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copper
dendrite arm
micropin
wing
natural multi
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CN106435665A (en
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吕树申
汪亚桥
莫冬传
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National Sun Yat Sen University
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National Sun Yat Sen University
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    • 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
    • C25D5/10Electroplating with more than one layer of the same or of different metals
    • 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
    • C25D5/16Electroplating with layers of varying thickness
    • 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

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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)
  • Electroplating Methods And Accessories (AREA)

Abstract

The invention discloses one kind to have dendritic micropin wing copper surface texture of natural multi-resolution tree and preparation method thereof.Copper dendrite arm structure is distributed on metallic copper matrix surface, the copper dendrite arm structure has natural Multi-scale model, including oikocryst branch, second level dendrite arm or three-level dendrite arm;Have gap between copper dendrite arm, copper dendrite arm is vertical, or with the inclined angle of matrix surface.The method on this easy inexpensive large scale preparation micropin wing surface, is suitble to handle the surface of any shape, and be not necessarily to valuable mechanical equipment, it is short to generate the period for energy conservation and environmental protection.And its natural Multi-scale model, can in augmentation of heat transfer, catalyst carrier, efficiently separate, microreactor, the heat and mass field such as surface hydrophobe is modified, therefore there is good prospects for commercial application.

Description

One kind having dendritic micropin wing copper surface texture of natural multi-resolution tree and preparation method thereof
Technical field
The invention belongs to materials science fields, specifically, being related to a kind of with the dendritic micropin wing copper of natural multi-resolution tree Surface texture and preparation method thereof.
Background technique
Because of its excellent heat and mass transfer performance, micropin wing (microtrabeculae group) structure is urged at microreactor (CN102202774A) Agent carrier (CN103623825-A), efficiently separates (20070227967 A of US) and electronic device is cold (CN101447466) But aspect is commonly employed.In recent years, with the development of nanosecond science and technology, show by the multiple dimensioned micropin fin structure of modification More excellent energy are gone out.Cao(Y. Cao, L. Yuan, B. Hu and J. Zhou, Nanotechnology, 2015, 26.) it in silicon micropin wing surface finish nano zinc oxide structures, becomes a kind of three-dimensional porous super thin with tertiary structure Water surface.And pass through silicon micropin fin structure (N. S. Dhillon, J. Buongiorno the and K. of applied field K. Varanasi, Nat. Commun., 2015,6,12.), effectively raise the critical heat flux density of boiling surface. Thai(D. Le Thai, D.-J. Kim, T. Tran Quang, D. Vinh Quang, B.-Y. Kim, H. K. Moon and N.-E. Lee, Adv. Funct. Mater., 2015,25,883-890.) it is modified using graphene oxide High-aspect-ratio volume micropin wing surface detects NH at room temperature3, this surface effectively raises the sensitivity of detection and reduction Detection limit and the response time.
The processing of micropin wing (microtrabeculae group) structure is usually traditional mechanical microfabrication techniques and MEMS manufacturing technology.This two Kind technology has its respective advantage and disadvantage.It is compared with MEMS, traditional micro-processing technology has maturity height and cost relatively Low advantage, but it is difficult processing dimension in 100 μm of micro-column structures below;And MEMS technology being capable of light processing micron structure And nanostructure, especially there is unique advantage in terms of high aspect ratio microstructures.But this technology is usually constructed with very long Process flow.Meanwhile both technologies require complicated mechanical equipment, and have significantly waste of material.
Summary of the invention
Traditional micropin fin structure processing difficulties are directed to, process flow is long, the single disadvantage of scale, the purpose of the present invention is It is simple to provide one kind, quickly, there is the dendritic micropin wing copper surface texture of natural multi-resolution tree.
Another object of the present invention is to provide the above-mentioned systems with the dendritic micropin wing copper surface texture of natural multi-resolution tree Preparation Method.
For achieving the above object, the present invention adopts the following technical scheme that:
One kind having the dendritic micropin wing copper surface texture of natural multi-resolution tree, and copper dendrite arm is distributed on metallic copper matrix surface Structure, the copper dendrite arm structure have natural Multi-scale model, including oikocryst branch, second level dendrite arm or three-level dendrite arm;Copper dendrite arm Between have a gap, copper dendrite arm is vertical, or with the inclined angle of matrix surface.
The above-mentioned preparation method with the dendritic micropin wing copper surface texture of natural multi-resolution tree, includes the following steps: copper After matrix processing and preplating, copper dendrite arm deposition is carried out;During the deposition process, using processed Copper substrate as cathode, with sulfuric acid and Copper sulphate is the solution of electrolyte, using the method for being gradually increased current density, carries out electrodeposit reaction;In reduction protection atmosphere Under the conditions of, it is sintered.
In the above-mentioned preparation method with the dendritic micropin wing copper surface texture of natural multi-resolution tree, sulphur in the electrolyte The molar concentration of acid is 0.2 ~ 1.0M, and the molar concentration of copper sulphate is 0.4 ~ 0.8M.
In the above-mentioned preparation method with the dendritic micropin wing copper surface texture of natural multi-resolution tree, in electrodeposition process, Current density speedup is 0.1 ~ 20 mA/ (cm2·s)。
In the above-mentioned preparation method with the dendritic micropin wing copper surface texture of natural multi-resolution tree, the sintering processes Temperature is 400 ~ 750 DEG C, is sintered in 400 ~ 750 DEG C of reducing atmospheres, and product mechanical strength is increased.
Compared with prior art, the invention has the following beneficial effects:
The present invention provides a kind of method of easy inexpensive large scale preparation micropin wing copper surface texture, it is suitble to appointing The surface of what shape is handled, and is not necessarily to valuable mechanical equipment, energy conservation and environmental protection, and it is short to generate the period, therefore is had good Prospects for commercial application.
Natural multiple dimensioned micropin wing copper surface texture prepared by the present invention is compared with traditional micropin wing surface with multiple dimensioned Structure, reference area is big, and capillary force is strong, be easy to bubble be detached from the characteristics of, effectively raise pool Boiling Heat Transfer heat exchange effect Rate, so be very suitable to apply to augmentation of heat transfer field.
Natural multiple dimensioned micropin wing copper surface texture of the invention can be wide with powder range, because of its unique three-dimensional multi-scale The heat transfers such as structure in catalyst carrier, efficiently separates, microreactor other than augmentation of heat transfer field, and surface hydrophobe is modified pass Matter field can also have good performance.
The dendroid micropin wing copper surface texture of natural Multi-scale model of the invention can be applied to heat pipe, heat exchanger, electricity The field of heat exchange such as the cooling of subcomponent can be used for other catalyst carriers, efficiently separate, the fields such as microreactor With.
Detailed description of the invention
Fig. 1 is the dendritic micropin wing copper surface texture side view of natural multi-resolution tree of embodiment 1;
Fig. 2 is the dendritic micropin wing copper surface texture side view of natural multi-resolution tree of embodiment 2;Matrix is in a constant inclination at this time Rake angle;
Fig. 3 is the copper surface texture of embodiment 1 and the pool boiling curve comparison figure of smooth copper surface.
Specific embodiment
The present invention is more specifically described in detail below with reference to specific attached drawing and preferred embodiments.
Embodiment 1:
(1) metallic matrix is handled: being removed oxide on surface using dilution heat of sulfuric acid first, is cleaned after allowing with high-concentration alkali liquor Surface and oil contaminant is then rinsed 3 times using deionization high purity water.
(2) it metallic matrix preplating: in order to increase deposited copper dendrite arm mechanical strength, is carried out before depositing copper dendrite arm pre- Plating.Pre-metallization solution is identical as the solution of copper dendrite arm.Preplating current density is 0.02A/cm2, the preplating time is 10min.
(3) copper dendrite arm deposits: using the method for being gradually increased electric current, processed metallic matrix is cathode, is in proportion 0.6MCuSO4、0.8MH2SO4Solution in, holding electric current speedup be 0.67mA/ (cm2S), initial current density is 0.1A/ cm2, reaction total electricity is 1080C.It is heat-treated after obtained sample clean drying.
(4) product is heat-treated: under reduction protection atmospheric condition, being heat-treated, further enhances product mechanical strength. For gained copper surface texture as shown in Figure 1, a series of copper dendrite arm structure is distributed on copper-based surfaces, copper dendrite arm structure has day Right Multi-scale model, including oikocryst branch, second level dendrite arm, three-level dendrite arm etc..There is gap between copper dendrite arm, copper dendrite arm has vertical , also have with matrix surface in certain inclination angle.
Embodiment 2
(1) metallic matrix is handled: being removed oxide on surface using dilution heat of sulfuric acid first, is cleaned after allowing with high-concentration alkali liquor Surface and oil contaminant is then rinsed 3 times using deionization high purity water.
(2) it metallic matrix preplating: in order to increase deposited copper dendrite arm mechanical strength, is carried out before depositing copper dendrite arm pre- Plating.Pre-metallization solution is identical as the solution of copper dendrite arm.Preplating current density is 0.02A/cm2, the preplating time is 10min.
(3) copper dendrite arm deposits: using the method for being gradually increased electric current, processed metallic matrix is cathode, is in proportion 0.6M CuSO4、0.4M H2SO4Solution in, holding electric current speedup be 2mA/ (cm2S), initial current density is 0.1A/ cm2, reaction total electricity is 180C.It is heat-treated after obtained sample clean drying.
(4) product is heat-treated: under reduction protection atmospheric condition, being heat-treated, further enhances product mechanical strength. For gained copper surface texture as shown in Fig. 2, a series of copper dendrite arm structure is distributed on copper-based surfaces, copper dendrite arm structure has day Right Multi-scale model, including oikocryst branch, second level dendrite arm, three-level dendrite arm etc..There is gap between copper dendrite arm, copper dendrite arm has vertical , also have with matrix surface in certain inclination angle.

Claims (1)

1. a kind of preparation method with the dendritic micropin wing copper surface texture of natural multi-resolution tree, which is characterized in that including as follows Step: being distributed with copper dendrite arm structure on metallic copper matrix surface, the copper dendrite arm structure has natural Multi-scale model, including Oikocryst branch, second level dendrite arm or three-level dendrite arm;There is gap between copper dendrite arm, copper dendrite arm is vertical, or with matrix surface in inclining Oblique angle;After Copper substrate processing and preplating, copper dendrite arm deposition is carried out;During the deposition process, using processed Copper substrate as cathode, Using sulfuric acid and copper sulphate as the solution of electrolyte, using the method for being gradually increased current density, electrodeposit reaction is carried out;It is restoring Under the conditions of protective atmosphere, it is sintered;The molar concentration of sulfuric acid is 0.2 ~ 1.0M, mole of copper sulphate in the electrolyte Concentration is 0.4 ~ 0.8M;In electrodeposition process, current density speedup is 0.1 ~ 20 mA/cm2·s;The temperature of the sintering processes It is 400 ~ 750 DEG C.
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US10793959B2 (en) 2017-06-19 2020-10-06 Kyung Mo Yang Method for production of metal article of manufacture and uses thereof
CN107868966B (en) * 2017-11-16 2019-08-13 中达电子(江苏)有限公司 Copper alloy porous wick structure and preparation method thereof
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
CN108364806A (en) * 2018-02-09 2018-08-03 中山大学 A kind of tree-shaped three-dimensional structure metal material and preparation method thereof and application in the battery
CN109023459B (en) * 2018-08-04 2021-03-16 中山大学 Double-layer multi-scale enhanced boiling surface structure and preparation method thereof
CN111647909A (en) * 2020-07-01 2020-09-11 中国科学技术大学 Dendritic copper electrode with hydrophobic surface and preparation method and application thereof
US20220243992A1 (en) * 2021-01-29 2022-08-04 Advanced Semiconductor Engineering, Inc. Heat transfer element, method for forming the same and semiconductor structure comprising the same
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

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101206374A (en) * 2006-12-21 2008-06-25 西北工业大学 Infrared waveband ultra-material based on dendritic structure
CN101514486A (en) * 2009-02-27 2009-08-26 华东师范大学 Cu dendritic single crystalline nano material and preparation method thereof
CN102379050A (en) * 2009-02-04 2012-03-14 应用材料公司 Porous three dimensional copper, tin, copper-tin, copper-tin-cobalt, and copper-tin-cobalt-titanium electrodes for batteries and ultra capacitors

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101206374A (en) * 2006-12-21 2008-06-25 西北工业大学 Infrared waveband ultra-material based on dendritic structure
CN102379050A (en) * 2009-02-04 2012-03-14 应用材料公司 Porous three dimensional copper, tin, copper-tin, copper-tin-cobalt, and copper-tin-cobalt-titanium electrodes for batteries and ultra capacitors
CN101514486A (en) * 2009-02-27 2009-08-26 华东师范大学 Cu dendritic single crystalline nano material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
电化学沉积金属铜的分形枝晶生长控制与性能;段涛 等;《强激光与粒子束》;20110131;第23卷(第1期);第101-106页

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