CN110629258A - Preparation method of porous copper liquid absorption core - Google Patents

Preparation method of porous copper liquid absorption core Download PDF

Info

Publication number
CN110629258A
CN110629258A CN201910981893.5A CN201910981893A CN110629258A CN 110629258 A CN110629258 A CN 110629258A CN 201910981893 A CN201910981893 A CN 201910981893A CN 110629258 A CN110629258 A CN 110629258A
Authority
CN
China
Prior art keywords
electrolyte
electrodeposition
substrate
porous
porous copper
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.)
Pending
Application number
CN201910981893.5A
Other languages
Chinese (zh)
Inventor
于全耀
梁平平
李学华
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.)
Dongguan Jay Metal Precision Manufacturing Technology Co Ltd
Dongguan Lingjie Metal Precision Manufacturing Technology Co Ltd
Original Assignee
Dongguan Jay Metal Precision Manufacturing Technology Co Ltd
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 Dongguan Jay Metal Precision Manufacturing Technology Co Ltd filed Critical Dongguan Jay Metal Precision Manufacturing Technology Co Ltd
Priority to CN201910981893.5A priority Critical patent/CN110629258A/en
Publication of CN110629258A publication Critical patent/CN110629258A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C25D5/34Pretreatment 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
    • C25D7/00Electroplating characterised by the article coated

Abstract

The invention discloses a preparation method of a porous copper liquid absorbing core, which comprises the following steps of A, preparing an electrodeposition electrolyte, wherein the electrolyte is an aqueous solution of copper chloride and hydrochloric acid; B. cleaning the surface of the substrate; C. and performing electrodeposition on the treated substrate in electrolyte to obtain the porous copper liquid absorbing core. The method has the beneficial effects that the electronegativity of the chlorine atom is extremely strong and is only second to the fluorine atom and the oxygen atom. The substrate can be activated in the electrodeposition process, the polarization effect is weakened, the generation of hydrogen in the pore wall structure can be reduced, a more compact pore wall structure is obtained, and the porous wall obtained by deposition is strengthened.

Description

Preparation method of porous copper liquid absorption core
Technical Field
The invention relates to the field of heat dissipation product development, in particular to a liquid absorption core structure of an ultrathin vapor chamber and a production process thereof.
Background
In the 5G era, electronic devices have been developed in the trends of integration, high frequency, high speed, etc., and the development of internal electronic chip technology has led to an increasing reduction in size and an increase in power. As semiconductor dimensions shrink, heat flux increases. The heat dissipation challenge of electronic products is becoming more serious. Heat pipes and vapor chambers, which are devices that dissipate heat by the phase change principle, are being rapidly applied to electronic products, such as high-end smart phones, LEDs, and the like.
Vapor chambers are accelerating for 5G smart phones. At present, during the manufacturing process of the vapor chamber, the wick structure usually adopts copper mesh or copper powder, and the copper mesh or copper powder is bonded with the wick structure by means of sintering. Are not optimal from both a cost and manufacturing process perspective. With the technological progress of researchers, some methods for preparing wicks in situ are gradually developed, the strength of the prepared porous wick structure is very weak, and the structure can be converted into the wick with practical application value by subsequent methods such as current deposition strengthening or sintering.
Disclosure of Invention
The invention provides a preparation method of a porous copper liquid absorbing core, which can solve one or more of the problems in the prior art.
According to one aspect of the present invention, there is provided a method of making a porous copper wick, comprising,
A. preparing an electrodeposition electrolyte, wherein the electrolyte is an aqueous solution of copper chloride and hydrochloric acid;
B. cleaning the surface of the substrate; and the combination of (a) and (b),
C. and performing electrodeposition on the treated substrate in electrolyte to obtain the porous copper liquid absorbing core.
The method has the beneficial effects that the electronegativity of the chlorine atom is extremely strong and is only second to the fluorine atom and the oxygen atom. The substrate can be activated in the electrodeposition process, the polarization effect is weakened, the generation of hydrogen in the pore wall structure can be reduced, and the porous wall obtained by deposition is strengthened.
In some embodiments, the concentration of copper chloride in the electrolyte in step A is 0.05 to 0.5mol/L and the concentration of hydrochloric acid is 1.0 to 2.0 mol/L. The concentration is too low, the deposition effect is not obvious, and a porous structure cannot be obtained. The copper ion concentration is too high, the deposition ratio is too large, and a compact film is easy to form; the hydrogen ion concentration is too high, the bubble generation rate is too high, and a three-dimensional pore structure cannot be obtained.
The invention has the beneficial effects that the invention provides a formula for preparing the porous copper liquid absorbing core by an electrochemical deposition principle, and a layer of porous metal structure with adjustable thickness and higher strength is grown on the surface of the metal in situ. Compared with the prior art that the structure can be converted into the liquid absorbing core with practical application value by further methods such as current deposition strengthening or sintering, the porous copper liquid absorbing core obtained by the method has obvious effects of cost reduction and efficiency improvement.
In some embodiments, the molar concentration ratio of hydrochloric acid to copper chloride in the electrolyte in step a is from 2:1 to 40: 1.
In some embodiments, step B comprises washing the substrate surface with a mixed solution of a surfactant and an alkaline compound, followed by washing with deionized water. The method has the advantages that the surface of the matrix is cleaned, and surface impurities are removed for several days.
In some embodiments, the electrodeposition in step C has a current density of 0.3 to 2A/cm2. The method has the beneficial effects that the current density can be controlled according to the requirement, so that the shape structure of the porous copper liquid absorption core is controlled. The current density is too high, the deposition rate and the electrolyte flowing behavior are not easy to control, and a regular porous structure cannot be obtained; the current density is too low, the deposition rate is slow, and the practical value is not high.
In some embodiments, the electrodeposition in step C has a current density of 0.5 to 1.0A/cm2
In some embodiments, in step C, the deposition time is 20-300 s.
In some embodiments, in step C, the deposition time is 30-100 s.
Drawings
Fig. 1 is a graph of porosity versus deposition time for a porous structured copper wick obtained in example 1.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
This example provides a method for making a porous copper wick, comprising,
A. preparing an electrodeposition electrolyte, wherein the electrolyte is an aqueous solution of 0.1mol/L copper chloride and 1.0mol/L hydrochloric acid;
B. cleaning the surface of the substrate by adopting a mixed solution of a surfactant and an alkaline compound, and cleaning the substrate by using deionized water;
C. the treated substrate is subjected to electrodeposition in electrolyte, and the current density of the electrodeposition is 0.8A/cm2And the deposition time is 20-180s to obtain the porous copper liquid absorbing core. The porosity of the porous structure is plotted against the deposition time as shown in FIG. 1. As can be seen from the figure, when the deposition time is 20s, the product porosity reaches about 50%; when the deposition time is 30s, the porosity of the finished product can reach more than 60 percent; after the deposition time is 50s, the porosity can reach about 80 percent and basically reaches the upper limit, and a porous structure with stable strength is formed.
Example 2
This example provides a method for making a porous copper wick, comprising,
A. preparing an electrodeposition electrolyte, wherein the electrolyte is an aqueous solution of 0.5mol/L copper chloride and 2.0mol/L hydrochloric acid;
B. cleaning the surface of the substrate by adopting a mixed solution of a surfactant and an alkaline compound, and cleaning the substrate by using deionized water;
C. the treated substrate is subjected to electrodeposition in electrolyte, and the current density of the electrodeposition is 2A/cm2And the deposition time is 300s, so that the porous copper wick is obtained.
Example 3
This example provides a method for making a porous copper wick, comprising,
A. preparing an electrodeposition electrolyte, wherein the electrolyte is an aqueous solution of 0.05mol/L copper chloride and 1.0mol/L hydrochloric acid;
B. cleaning the surface of the substrate by adopting a mixed solution of a surfactant and an alkaline compound, and cleaning the substrate by using deionized water;
C. the treated substrate is subjected to electrodeposition in electrolyte, and the current density of the electrodeposition is 1A/cm2The deposition time was 100s to obtain a porous copper wick.
Example 4
This example provides a method for making a porous copper wick, comprising,
A. preparing an electrodeposition electrolyte, wherein the electrolyte is an aqueous solution of 0.05mol/L copper chloride and 1.0mol/L hydrochloric acid;
B. cleaning the surface of the substrate by adopting a mixed solution of a surfactant and an alkaline compound, and cleaning the substrate by using deionized water;
C. the treated substrate is subjected to electrodeposition in electrolyte, and the current density of the electrodeposition is 2A/cm2And the deposition time is 200s, so that the porous copper wick is obtained.
Example 5
This example provides a method for making a porous copper wick, comprising,
A. preparing an electrodeposition electrolyte, wherein the electrolyte is an aqueous solution of 0.1mol/L copper chloride and 2mol/L hydrochloric acid;
B. cleaning the surface of the substrate by adopting a mixed solution of a surfactant and an alkaline compound, and cleaning the substrate by using deionized water;
C. the treated substrate is subjected to electrodeposition in electrolyte, and the current density of the electrodeposition is 2A/cm2And the deposition time is 300s, so that the porous copper wick is obtained.
Example 6
This example provides a method for making a porous copper wick, comprising,
A. preparing an electrodeposition electrolyte, wherein the electrolyte is an aqueous solution of 0.5mol/L copper chloride and 2.0mol/L hydrochloric acid;
B. cleaning the surface of the substrate by adopting a mixed solution of a surfactant and an alkaline compound, and cleaning the substrate by using deionized water;
C. the treated substrate is subjected to electrodeposition in electrolyte, and the current density of the electrodeposition is 1A/cm2The deposition time was 100s to obtain a porous copper wick.
Example 7
This example provides a method for making a porous copper wick, comprising,
A. preparing an electrodeposition electrolyte, wherein the electrolyte is an aqueous solution of 0.5mol/L copper chloride and 2.0mol/L hydrochloric acid;
B. cleaning the surface of the substrate by adopting a mixed solution of a surfactant and an alkaline compound, and cleaning the substrate by using deionized water;
C. the treated substrate is subjected to electrodeposition in electrolyte, and the current density of the electrodeposition is 2A/cm2And the deposition time is 200s, so that the porous copper wick is obtained.
Example 8
This example provides a method for making a porous copper wick, comprising,
A. preparing an electrodeposition electrolyte, wherein the electrolyte is an aqueous solution of 0.5mol/L copper chloride and 2mol/L hydrochloric acid;
B. cleaning the surface of the substrate by adopting a mixed solution of a surfactant and an alkaline compound, and cleaning the substrate by using deionized water;
C. the treated substrate is subjected to electrodeposition in electrolyte, and the current density of the electrodeposition is 2A/cm2And the deposition time is 300s, so that the porous copper wick is obtained.
Example 9
This example provides a method for making a porous copper wick, comprising,
A. preparing an electrodeposition electrolyte, wherein the electrolyte is an aqueous solution of 0.5mol/L copper chloride and 2mol/L hydrochloric acid;
B. cleaning the surface of the substrate by adopting a mixed solution of a surfactant and an alkaline compound, and cleaning the substrate by using deionized water;
C. the treated substrate is subjected to electrodeposition in electrolyte, and the current density of the electrodeposition is 0.5A/cm2And the deposition time is 300s, so that the porous copper wick is obtained.
What has been described above are merely some embodiments of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept thereof, and these changes and modifications can be made without departing from the spirit and scope of the invention.

Claims (8)

1. A method for preparing a porous copper wick, comprising,
A. preparing an electrodeposition electrolyte, wherein the electrolyte is an aqueous solution of copper chloride and hydrochloric acid;
B. cleaning the surface of the substrate; and the combination of (a) and (b),
C. and performing electrodeposition on the treated substrate in electrolyte to obtain the porous copper liquid absorbing core.
2. The method of claim 1, wherein the electrolyte in step a has a copper chloride concentration of 0.05 to 0.5mol/L and a hydrochloric acid concentration of 1.0 to 2.0 mol/L.
3. The method of claim 1 or 2, wherein the molar concentration ratio of hydrochloric acid to copper chloride in the electrolyte in step a is from 2:1 to 40: 1.
4. A method of making a porous copper wick according to claim 1 wherein step B comprises cleaning the surface of the substrate with a solution of a mixture of a surfactant and an alkaline compound, followed by rinsing with deionized water.
5. The method of claim 1, wherein in step C, the electrodeposition current density is between 0.3 and 2A/cm2
6. The method of claim 1, wherein in step C, the electrodeposition current density is between 0.5 and 1.0A/cm2
7. A method of making a porous copper wick according to claim 1 wherein in step C, the deposition time is from 20 to 300 seconds.
8. A method of making a porous copper wick according to claim 1 wherein in step C, the deposition time is 30-100 s.
CN201910981893.5A 2019-10-16 2019-10-16 Preparation method of porous copper liquid absorption core Pending CN110629258A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910981893.5A CN110629258A (en) 2019-10-16 2019-10-16 Preparation method of porous copper liquid absorption core

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910981893.5A CN110629258A (en) 2019-10-16 2019-10-16 Preparation method of porous copper liquid absorption core

Publications (1)

Publication Number Publication Date
CN110629258A true CN110629258A (en) 2019-12-31

Family

ID=68975158

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910981893.5A Pending CN110629258A (en) 2019-10-16 2019-10-16 Preparation method of porous copper liquid absorption core

Country Status (1)

Country Link
CN (1) CN110629258A (en)

Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5542153B2 (en) * 1974-11-06 1980-10-29
CN102185131A (en) * 2011-04-13 2011-09-14 长安大学 Preparation method of porous current collector/tin-base alloy/carbon nano-tube integrated electrode
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
CN103046088A (en) * 2012-12-20 2013-04-17 华南理工大学 Micro-nano composite porous copper surface structure and preparation method and device thereof
CN103132111A (en) * 2013-01-25 2013-06-05 重庆大学 Preparation method of three-dimensional micrometer level porous copper thin film
CN203080093U (en) * 2012-12-20 2013-07-24 华南理工大学 Electro-deposition device for manufacturing micro-nano composite porous copper surface structure
CN103406129A (en) * 2013-05-22 2013-11-27 山东大学 Preparation method of wire mesh monolithic catalyst based on surface porous structure
CN103526239A (en) * 2013-10-08 2014-01-22 昆山纯柏精密五金有限公司 Copper plating solution and hardware copper plating method
CN104975309A (en) * 2015-06-12 2015-10-14 东南大学 Method for adjusting and controlling hole diameter of open-cell foamy copper
CN105506682A (en) * 2016-01-21 2016-04-20 广州中国科学院先进技术研究所 Method for preparing copper nano-wire based on electrochemical deposition
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
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
CN109137020A (en) * 2018-09-19 2019-01-04 江西华度电子新材料有限公司 A kind of preparation method of thickness liquid-sucking core
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

Patent Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5542153B2 (en) * 1974-11-06 1980-10-29
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
CN102185131A (en) * 2011-04-13 2011-09-14 长安大学 Preparation method of porous current collector/tin-base alloy/carbon nano-tube integrated electrode
CN103046088A (en) * 2012-12-20 2013-04-17 华南理工大学 Micro-nano composite porous copper surface structure and preparation method and device thereof
CN203080093U (en) * 2012-12-20 2013-07-24 华南理工大学 Electro-deposition device for manufacturing micro-nano composite porous copper surface structure
CN103132111A (en) * 2013-01-25 2013-06-05 重庆大学 Preparation method of three-dimensional micrometer level porous copper thin film
CN103406129A (en) * 2013-05-22 2013-11-27 山东大学 Preparation method of wire mesh monolithic catalyst based on surface porous structure
CN103526239A (en) * 2013-10-08 2014-01-22 昆山纯柏精密五金有限公司 Copper plating solution and hardware copper plating method
CN104975309A (en) * 2015-06-12 2015-10-14 东南大学 Method for adjusting and controlling hole diameter of open-cell foamy copper
CN105506682A (en) * 2016-01-21 2016-04-20 广州中国科学院先进技术研究所 Method for preparing copper nano-wire based on electrochemical deposition
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
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
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
CN109137020A (en) * 2018-09-19 2019-01-04 江西华度电子新材料有限公司 A kind of preparation method of thickness liquid-sucking core

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
孙雅峰等: "氢气泡模板法电沉积制备三维多孔铜薄膜", 《电化学》 *
李云倩主编: "《化工原理 上册》", 31 October 1991, 中央广播电视大学出版社 *

Similar Documents

Publication Publication Date Title
CN106119977B (en) Fine-hair maring using monocrystalline silicon slice additive and application
TWI599060B (en) Suede structure of a crystalline silicon solar cell and its preparation method
US10411145B2 (en) Method for producing a textured structure of a crystalline silicon solar cell
JP6684856B2 (en) Porous liquid absorbent core and method for producing the same
JP4610669B2 (en) Manufacturing method of solar cell
TWI494416B (en) Acidic etching solution and method for texturing the surface of single crystal and polycrystal silicon substrates
TWI638068B (en) Copper alloy porous wick and preparation method thereof
CN103046088A (en) Micro-nano composite porous copper surface structure and preparation method and device thereof
CN106098810B (en) A kind of preparation method of crystal silicon solar energy battery suede structure
CN105304734A (en) Polycrystalline silicon wafer texturing auxiliary and application method thereof
CN101345137A (en) Anode foil corrosion technology of electrolytic capacitor
CN100347870C (en) Electro-luminescent porous silica material and its preparation method
CN102337596B (en) Monocrystalline silicon solar cell alkali texturing assistant agent and its application
Cichoszewski et al. Role of catalyst concentration on metal assisted chemical etching of silicon
CN109750353A (en) Monocrystalline silicon piece inverted pyramid making herbs into wool adjuvant and its application
TW201324833A (en) Method for manufacturing solar cell
CN112176369A (en) High-efficiency boiling heat transfer copper material and preparation method thereof
WO2017221710A1 (en) Solar cell manufacturing method
US8668840B2 (en) Solution used in the fabrication of a porous semiconductor material, and a method of fabricating said material
CN110629258A (en) Preparation method of porous copper liquid absorption core
CN103151424B (en) A kind of improvement chemical plating process prepares the method for metal electrode at porous silicon surface
CN112251817A (en) Inverted pyramid auxiliary texturing additive and application thereof
JP2015053398A (en) Manufacturing method of solar cell
CN104900488B (en) A kind of method of the stable porous silicon film physics micro-structural of energy
JP2005223180A (en) Method and apparatus for manufacturing electrode foil for aluminum electrolytic capacitor

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20191231

RJ01 Rejection of invention patent application after publication