CN106435665A - Natural multi-scale dendritic micro-pinfin copper surface structure and preparation method thereof - Google Patents

Natural multi-scale dendritic micro-pinfin copper surface structure and preparation method thereof Download PDF

Info

Publication number
CN106435665A
CN106435665A CN201610828565.8A CN201610828565A CN106435665A CN 106435665 A CN106435665 A CN 106435665A CN 201610828565 A CN201610828565 A CN 201610828565A CN 106435665 A CN106435665 A CN 106435665A
Authority
CN
China
Prior art keywords
copper
natural multi
micropin
wing
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201610828565.8A
Other languages
Chinese (zh)
Other versions
CN106435665B (en
Inventor
吕树申
汪亚桥
莫冬传
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
National Sun Yat Sen University
Original Assignee
National Sun Yat Sen University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by National Sun Yat Sen University filed Critical National Sun Yat Sen University
Priority to CN201610828565.8A priority Critical patent/CN106435665B/en
Publication of CN106435665A publication Critical patent/CN106435665A/en
Application granted granted Critical
Publication of CN106435665B publication Critical patent/CN106435665B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • 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
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • 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
    • C25D5/16—Electroplating with layers of varying thickness
    • 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

Abstract

The invention discloses a natural multi-scale dendritic micro-pinfin copper surface structure and a preparation method thereof. A copper dendrite structure is distributed on the surface of a metal copper substrate, is provided with a natural multi-scale structure body and comprises primary dendritic crystals and second-level or third-level dendritic crystals; clearances are formed among copper dendritic crystals, the copper dendritic crystals are vertical, or inclined angles are formed between the dendritic crystals and the surface of the substrate. The simple low-cost method for preparing micro-pinfin surfaces on a large scale is suitable for processing surfaces of any shapes without valuable mechanical equipment, energy is saved, the environment is protected, and the generating period is short; and in addition, through the natural multi-scale structure body, the natural multi-scale dendritic micro-pinfin copper surface structure can be applied to strengthened heat transferring, catalyst carriers, efficient separation, microreactors, surface hydrophilic and hydrophobic modification and other heat and mass transfer fields and thereby having very good industrial application prospects.

Description

One kind has natural multi-resolution tree dendritic micropin wing copper surface texture and preparation method thereof
Technical field
The invention belongs to material science, specifically, it is related to one kind and there is natural multi-resolution tree dendritic micropin wing copper Surface texture and preparation method thereof.
Background technology
Because of its excellent heat and mass transfer performance, micropin wing（Microtrabeculae group）Structure is in microreactor（CN102202774A）, urge Agent carrier（CN103623825-A）, efficiently separate（US 20070227967 A）And electronic device is cold（CN101447466） But aspect is commonly employed.In recent years, with the development of nanosecond science and technology, the multiple dimensioned micropin fin structure through modifying represents More excellent energy are gone out.Cao(Y. Cao, L. Yuan, B. Hu and J. Zhou, Nanotechnology, 2015, 26.) so as to become a kind of, there is the three-dimensional porous super thin of tertiary structure in silicon micropin wing surface finish nano zinc oxide structures Water surface.And the silicon micropin fin structure through applied field（N. S. Dhillon, J. Buongiorno and K. 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.）Modified using graphene oxide High-aspect-ratio volume micropin wing surface detects NH at ambient temperature3, this surface effectively raises the sensitivity of detection and reduces Test limit and the response time.
Micropin wing（Microtrabeculae group）The processing of structure is usually traditional mechanical microfabrication techniques and MEMS manufacturing technology.This two The technology of kind has its respective pluses and minuses.Compare with MEMS, traditional micro-processing technology has maturity height, and cost is relatively Low advantage, but it is difficult to micro-column structure below 100 μm for the processing dimension；And MEMS technology being capable of light processing micron structure And nanostructured, in terms of high aspect ratio microstructures, particularly there is the advantage of uniqueness.But this technology is usually constructed with very long Technological process.Meanwhile, both technology are required for the plant equipment of complexity, and have significantly waste of material.
Content of the invention
It is directed to traditional micropin fin structure processing difficulties, technological process is long, the single shortcoming of yardstick, the purpose of the present invention is There is provided a kind of simple, quickly, there is natural multi-resolution tree dendritic micropin wing copper surface texture.
Another object of the present invention is to providing the above-mentioned system with natural multi-resolution tree dendritic micropin wing copper surface texture Preparation Method.
For achieving the above object, the present invention adopts the following technical scheme that：
One kind has natural multi-resolution tree dendritic micropin wing copper surface texture, and copper dendrite arm knot is distributed with metallic copper matrix surface Structure, described copper dendrite arm structure has natural Multi-scale model, including oikocryst branch, two grades of dendrite arms or three-level dendrite arm；Copper dendrite arm it Between have gap, copper dendrite arm is vertical, or the inclined angle with matrix surface.
The above-mentioned preparation method with natural multi-resolution tree dendritic micropin wing copper surface texture, comprises the steps：By copper After matrix process and preplating, carry out copper dendrite arm deposition；In deposition process, with the Copper substrate that processed as negative electrode, with sulfuric acid and Copper sulphate is the solution of electrolyte, and the method using 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 natural multi-resolution tree dendritic micropin wing copper surface texture, sulphur in described 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 natural multi-resolution tree dendritic micropin wing copper surface texture, in electrodeposition process, Current density speedup is 0.1 ~ 20 mA/ (cm2·s).
In the above-mentioned preparation method with natural multi-resolution tree dendritic micropin wing copper surface texture, described sintering processes Temperature is 400 ~ 750 DEG C, sinters in 400 ~ 750 DEG C of reducing atmospheres, increases product mechanical strength.
Compared with prior art, the present invention has the advantages that：
The invention provides a kind of method that easy low cost prepares micropin wing copper surface texture on a large scale, it is suitable for any shape The surface of shape is processed, and need not be valuable plant equipment, energy-conserving and environment-protective, generate cycle is short, therefore there is good industry Application prospect.
The present invention preparation natural multiple dimensioned micropin wing copper surface texture and tradition micropin wing surface compare have multiple dimensioned Structure, reference area is big, capillary force strong it is easy to the feature of bubble disengagement, effectively raise the heat exchange effect of pool Boiling Heat Transfer Rate, so be especially suitable for applying to augmentation of heat transfer field.
The natural multiple dimensioned micropin wing copper surface texture of the present invention can be wide with powder scope, because of its unique three-dimensional multi-scale Structure, in addition to augmentation of heat transfer field, in catalyst carrier, efficiently separates, microreactor, and the heat transfer such as surface hydrophobe modification passes Matter field also can have good performance.
The dendroid micropin wing copper surface texture of the natural Multi-scale model of the present invention can be applicable to heat pipe, heat exchanger, electricity The field of heat exchange such as the cooling of subcomponent it is also possible to for other catalyst carriers, efficiently separate, the field such as microreactor With.
Brief description
Fig. 1 is the natural multi-resolution tree dendritic micropin wing copper surface texture side view of embodiment 1；
Fig. 2 is the natural multi-resolution tree dendritic micropin wing copper surface texture side view of embodiment 2；Now matrix is in certain inclination angle Degree；
Fig. 3 is the pool boiling curve comparison figure with smooth copper surface for the copper surface texture of embodiment 1.
Specific embodiment
With reference to concrete accompanying drawing and preferred embodiments, the present invention is more specifically described in detail.
Embodiment 1：
（1）Metallic matrix is processed：Remove oxide on surface first by dilution heat of sulfuric acid, after allowing, clean surface with high-concentration alkali liquor Greasy dirt, is then used by deionization high purity water and rinses 3 times.
（2）Metallic matrix preplating：In order to increase deposited copper dendrite arm mechanical strength, carry out pre- before deposition copper dendrite arm Plating.Pre-metallization solution is same with the solution of copper dendrite arm.Preplating current density is 0.02A/cm2, the preplating time is 10min.
（3）Copper dendrite arm deposits：Method using being gradually increased electric current, the metallic matrix processing is negative electrode, in proportioning is 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.The sample clean obtaining is heat-treated after drying up.
（4）Product is heat-treated：Under reduction protection atmospheric condition, it is heat-treated, further enhanced product mechanical strength. As shown in figure 1, a series of copper dendrite arm structure is distributed with copper-based surfaces, copper dendrite arm structure has sky to gained copper surface texture Right Multi-scale model, including oikocryst branch, two grades of dendrite arms, three-level dendrite arms etc..There is gap, copper dendrite arm has vertically between copper dendrite arm , also having with matrix surface is in certain inclination angle.
Embodiment 2
（1）Metallic matrix is processed：Remove oxide on surface first by dilution heat of sulfuric acid, after allowing, clean surface with high-concentration alkali liquor Greasy dirt, is then used by deionization high purity water and rinses 3 times.
（2）Metallic matrix preplating：In order to increase deposited copper dendrite arm mechanical strength, carry out pre- before deposition copper dendrite arm Plating.Pre-metallization solution is same with the solution of copper dendrite arm.Preplating current density is 0.02A/cm2, the preplating time is 10min.
（3）Copper dendrite arm deposits：Method using being gradually increased electric current, the metallic matrix processing is negative electrode, in proportioning is 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.The sample clean obtaining is heat-treated after drying up.
（4）Product is heat-treated：Under reduction protection atmospheric condition, it is heat-treated, further enhanced product mechanical strength. As shown in Fig. 2 a series of copper dendrite arm structure is distributed with copper-based surfaces, copper dendrite arm structure has sky to gained copper surface texture Right Multi-scale model, including oikocryst branch, two grades of dendrite arms, three-level dendrite arms etc..There is gap, copper dendrite arm has vertically between copper dendrite arm , also having with matrix surface is in certain inclination angle.

Claims (5)

1. one kind has natural multi-resolution tree dendritic micropin wing copper surface texture it is characterised in that dividing on metallic copper matrix surface It is furnished with copper dendrite arm structure, described copper dendrite arm structure has natural Multi-scale model, brilliant including oikocryst branch, two grades of dendrite arms or three-level Branch；There is gap, copper dendrite arm is vertical between copper dendrite arm, or the inclined angle with matrix surface.
2. there is described in claim 1 preparation method of natural multi-resolution tree dendritic micropin wing copper surface texture it is characterised in that Comprise the steps：After Copper substrate process and preplating, carry out copper dendrite arm deposition；In deposition process, copper-based with processed Body is negative electrode, the solution with sulfuric acid and copper sulphate as electrolyte, and the method using being gradually increased current density carries out electro-deposition anti- Should；Under reduction protection atmospheric condition, it is sintered.
3. there is the preparation method of natural multi-resolution tree dendritic micropin wing copper surface texture, its feature as claimed in claim 2 It is：In described electrolyte, the molar concentration of sulfuric acid is 0.2 ~ 1.0M, and the molar concentration of copper sulphate is 0.4 ~ 0.8M.
4. there is the preparation method of natural multi-resolution tree dendritic micropin wing copper surface texture, its feature as claimed in claim 2 It is：In electrodeposition process, current density speedup is 0.1 ~ 20 mA/cm2·s.
5. there is the preparation method of natural multi-resolution tree dendritic micropin wing copper surface texture, its feature as claimed in claim 2 It is：The temperature of described sintering processes is 400 ~ 750 DEG C.
CN201610828565.8A 2016-09-18 2016-09-18 One kind having dendritic micropin wing copper surface texture of natural multi-resolution tree and preparation method thereof Active CN106435665B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610828565.8A CN106435665B (en) 2016-09-18 2016-09-18 One kind having dendritic micropin wing copper surface texture of natural multi-resolution tree and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610828565.8A CN106435665B (en) 2016-09-18 2016-09-18 One kind having dendritic micropin wing copper surface texture of natural multi-resolution tree and preparation method thereof

Publications (2)

Publication Number Publication Date
CN106435665A true CN106435665A (en) 2017-02-22
CN106435665B CN106435665B (en) 2019-04-05

Family

ID=58167967

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610828565.8A Active CN106435665B (en) 2016-09-18 2016-09-18 One kind having dendritic micropin wing copper surface texture of natural multi-resolution tree and preparation method thereof

Country Status (1)

Country Link
CN (1) CN106435665B (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107868966A (en) * 2017-11-16 2018-04-03 中达电子(江苏)有限公司 Copper alloy porous wick structure and preparation method thereof
CN107937943A (en) * 2017-11-16 2018-04-20 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
CN109023459A (en) * 2018-08-04 2018-12-18 中山大学 A kind of multiple dimensioned surface texture and preparation method thereof for strengthening boiling of bilayer
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
US10793959B2 (en) 2017-06-19 2020-10-06 Kyung Mo Yang Method for production of metal article of manufacture and uses 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
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

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
段涛 等: "电化学沉积金属铜的分形枝晶生长控制与性能", 《强激光与粒子束》 *

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10793959B2 (en) 2017-06-19 2020-10-06 Kyung Mo Yang Method for production of metal article of manufacture and uses thereof
US11608562B2 (en) 2017-06-19 2023-03-21 Kyung Mo Yang Method for production of metal article of manufacture and uses thereof
CN107868966A (en) * 2017-11-16 2018-04-03 中达电子(江苏)有限公司 Copper alloy porous wick structure and preparation method thereof
CN107937943A (en) * 2017-11-16 2018-04-20 中达电子(江苏)有限公司 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
CN109023459A (en) * 2018-08-04 2018-12-18 中山大学 A kind of multiple dimensioned surface texture and preparation method thereof for strengthening boiling of bilayer
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

Also Published As

Publication number Publication date
CN106435665B (en) 2019-04-05

Similar Documents

Publication Publication Date Title
CN106435665B (en) One kind having dendritic micropin wing copper surface texture of natural multi-resolution tree and preparation method thereof
TWI642814B (en) Porous wick and preparation method thereof
CN107868966B (en) Copper alloy porous wick structure and preparation method thereof
Wang et al. Copper vertical micro dendrite fin arrays and their superior boiling heat transfer capability
CN105293427A (en) Preparation method of super-hydrophobic surface based on limited local plating of meniscus
CN102447011A (en) Method for manufacturing solar battery photoanode and product thereof
CN103046088A (en) Micro-nano composite porous copper surface structure and preparation method and device thereof
CN105390702B (en) A kind of nickel foam base carbon nanotube doping Sn/SnO/SnO2Three-dimensional porous negative electrode material of stratiform and preparation method thereof
CN106222694B (en) Sponge structure alloy loads the preparation method of ternary oxide layer hydrogen evolution electrode material
CN102070120A (en) Preparation method for high-density interposer for microelectronic system-in-package
Wang et al. Morphologies and wetting properties of copper film with 3D porous micro-nano hierarchical structure prepared by electrochemical deposition
Nicaise et al. Control of zinc oxide nanowire array properties with electron-beam lithography templating for photovoltaic applications
CN105668505B (en) A kind of processing method of complex three-dimensional structure microchannel
CN106400067A (en) Single-layer micro-nano double-scale enhanced boiling heat transfer copper surface structure and preparing method thereof
CN103481583B (en) A kind of surface has the preparation method processing Copper Foil of loose structure
CN105603469A (en) CuO/Ni core-shell nanowire and preparation method thereof
Mackay et al. Template-free electrochemical synthesis of tin nanostructures
CN109023459B (en) Double-layer multi-scale enhanced boiling surface structure and preparation method thereof
CN107502945A (en) A kind of graphene aluminium alloy conductor and preparation method
CN110387565A (en) A kind of surface preparation method that can prepare a variety of nanowire structures
Gryzunova et al. Preparation of materials with a developed surface by thermal treatment and chemical etching of electrodeposited icosahedral small copper particles
CN112176369A (en) High-efficiency boiling heat transfer copper material and preparation method thereof
CN104726920A (en) Method for preparing and transferring ultrathin perforated anode alumina template
CN100548871C (en) 3 D semiconductor Nano structured array and preparation method thereof
CN104846411B (en) The method and its product of flower-like nanometer metal cobalt are prepared using anodic oxidation aluminium formwork

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant