CN112210802A - Flower-shaped boiling heat transfer structure and preparation method thereof - Google Patents

Flower-shaped boiling heat transfer structure and preparation method thereof Download PDF

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CN112210802A
CN112210802A CN201910619049.8A CN201910619049A CN112210802A CN 112210802 A CN112210802 A CN 112210802A CN 201910619049 A CN201910619049 A CN 201910619049A CN 112210802 A CN112210802 A CN 112210802A
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heat transfer
flower
boiling heat
copper
cone
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高雪峰
吴菲菲
泽花姐
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Suzhou Institute of Nano Tech and Nano Bionics of CAS
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Suzhou Institute of Nano Tech and Nano Bionics of CAS
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Abstract

The invention discloses a flower-shaped boiling heat transfer structure and a preparation method thereof, wherein a micro-nano porous film covers the surface of the structure, the micro-nano porous film takes a copper micro-cone as a main body, and the surface of the micro-nano porous film is coated with a nano-cone to form a hierarchical composite cone structure; a unique micro-nano porous structure is formed between the composite cone structures. Compared with a single copper micrometer cone structure, the flower-shaped boiling heat transfer structure has the advantages of higher heat exchange area, more nucleation sites, more excellent boiling heat exchange performance, higher boiling heat transfer coefficient and critical heat flux density, and lower superheat degree corresponding to a nucleation boiling starting point. The electrolyte required by the preparation of the flower-shaped boiling heat transfer structure has simple and convenient formula, economy and easy obtainment, wide selectable range of electroplating modes and suitability for industrial scale application.

Description

Flower-shaped boiling heat transfer structure and preparation method thereof
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a flower-shaped boiling heat transfer structure and a preparation method thereof.
Background
With the development of miniaturization, integration and high power of electronic devices, a severe test is provided for high heat flow heat dissipation. The research on the micro-nano copper material with more excellent boiling heat transfer performance by utilizing the existing or developing new micro-nano processing technology has become the current research focus.
In 2008, a group of professor toprake of royal institute of technology, utilized an electrochemical deposition method to prepare a three-dimensional dendritic nano-composite microporous structure of copper material on the surface of copper material and confirmed that the structure has high boiling heat transfer performance (adv. funct. mater, 2008,18, 2215-2220). The structure is prepared by taking dynamic bubbles as a template, so that a high-density nano porous structure can be obtained, the increase of nucleation sites of the bubbles is facilitated, and the initial boiling point is greatly reduced; the nano-scale dendritic structure can increase the heat exchange area and accelerate the large-area evaporation of the micro liquid layer, the micro-scale pore structure is favorable for reducing the resistance of bubble separation, and the micro-nano structure is synergetic and is favorable for achieving the purpose of enhancing boiling heat transfer. However, the porous structure obtained by this method has a large contact area with the bubbles, and is not favorable for the detachment of the bubbles, so that the critical heat flux density cannot be further increased.
In 2017, a three-dimensional micro-Nano composite copper nanowire structure prepared by Yangronggui professor team of the university of Korolado, USA, based on a photoetching process and a porous anodic aluminum oxide template assisted electrochemical deposition technology also proves that the structure has high-efficiency boiling heat transfer performance (Nano Energy,2017,38, 59-65). The micro-cavity in the hierarchical structure can increase the nucleation density of bubbles, the nano-wires can increase the secondary wettability of liquid, and the hierarchical structure can achieve the effect of separating a vapor-liquid transmission channel. They therefore found that the critical heat flux density of the liquid was increased by 71%, the corresponding heat transfer coefficient was increased by 185% and the ONB point was advanced by 37% compared to a planar surface. Although this improved process enables in-situ growth of copper wire and has excellent boiling heat transfer properties, this process suffers from the following inevitable problems: the photoetching process and the anodic aluminum oxide template are required to assist, the operation process is complex, large-area processing cannot be realized due to the limitation of the template, and the processing cost is increased sharply along with the increase of the area of the template; mechanical interference can easily lead to template fracture and thus uncontrollable nanowire processing quality.
Therefore, how to develop the high-efficiency boiling heat transfer micro-nano copper material with real commercial value and the processing technology thereof still faces huge challenges.
Disclosure of Invention
The invention aims to provide a flower-shaped boiling heat transfer structure for solving the problem of low critical heat flux density in the prior art.
In one embodiment, the flower-shaped boiling heat transfer structure includes:
a substrate;
array needle-like micron copper structure protruding on the surface of the substrate; and
and the graded nanocones protrude out of the surface of the micron copper.
Furthermore, the metal film layer is composed of a primary cone and a grading cone, the primary cone is composed of a plurality of needle-cone-shaped micron copper structures, and the grading cone is composed of a nano cone coated on the surface of the cone. In other embodiments, the micro-cavity may be formed by directly recessing the surface of the substrate.
In another embodiment, there is provided a flower boiling heat transfer structure comprising:
a substrate;
the array is protruded on the first-level vertebral body on the surface of the substrate; and
and the grading cone protrudes out of the surface of the primary cone body.
Compared with the prior art, the micro-nano porous copper material has the advantages of higher heat exchange area, far more nucleation sites, more excellent boiling heat exchange performance, higher boiling heat transfer coefficient and critical heat flux density, and lower superheat degree corresponding to a nucleation boiling starting point. The electrolyte formula required by the preparation of the micro-nano porous copper material is economical and easy to obtain, and is suitable for industrial scale application.
The invention also aims to provide a preparation method of the flower-shaped boiling heat transfer structure, wherein the metal film layer is formed on the surface of the base material by electrodeposition in electrolyte.
The invention also aims to provide a preparation method of the flower-shaped boiling heat transfer structure, wherein the grading nanocone is formed on the surface of the main microcone through electrodeposition in electrolyte.
Compared with the prior art, the preparation method of the micro-nano porous copper material has the characteristics of simple and convenient process, cheap and easily obtained raw materials, easy regulation and control of reaction, low cost and the like.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic diagram of a preparation process of a flower-type micro-nano composite porous structure;
FIG. 2a is a scanning electron micrograph (5 μm) of a flower-type boiling heat transfer structure in example 1 of the present application;
FIG. 2b is a scanning electron micrograph (2 μm) of the flower-shaped boiling heat transfer structure in example 1 of the present application;
FIG. 2c is a scanning electron micrograph (500nm, enlarged view of a portion of FIG. 2 a) of the flower-type boiling heat transfer structure in example 1 of the present application;
FIG. 3a is a boiling heat transfer performance graph (heat flux density) of the flower-type boiling heat transfer structure in example 1 of the present application;
FIG. 3b is a boiling heat transfer performance graph (heat transfer coefficient) of the flower-type boiling heat transfer structure in example 1 of the present application;
FIG. 4a is a scanning electron micrograph (5 μm) of a flower-type boiling heat transfer structure in example 2 of the present application;
FIG. 4b is a scanning electron micrograph (2 μm) of the flower-shaped boiling heat transfer structure in example 2 of the present application;
FIG. 4c is a scanning electron micrograph (500nm, enlarged view of a portion of FIG. 4 a) of the flower-type boiling heat transfer structure in example 2 of the present application;
FIG. 5a is a boiling heat transfer performance graph (heat flux density) of the flower-shaped boiling heat transfer structure in example 2 of the present application;
FIG. 5b is a boiling heat transfer performance graph (heat transfer coefficient) of the flower-type boiling heat transfer structure in example 2 of the present application;
FIG. 6a is a scanning electron micrograph (5 μm) of a flower-shaped boiling heat transfer structure in example 3 of the present application;
FIG. 6b is a scanning electron micrograph (2 μm) of the flower-shaped boiling heat transfer structure in example 3 of the present application;
FIG. 6c is a scanning electron micrograph (500nm, enlarged view of a portion of FIG. 6 a) of the flower-type boiling heat transfer structure in example 3 of the present application;
FIG. 7a is a boiling heat transfer performance graph (heat flux density) of the flower-type boiling heat transfer structure in example 3 of the present application;
FIG. 7b is a boiling heat transfer performance graph (heat transfer coefficient) of the flower-type boiling heat transfer structure in example 3 of the present application;
FIG. 8a is a scanning electron micrograph (5 μm) of a flower-type boiling heat transfer structure in example 4 of the present application;
FIG. 8b is a scanning electron micrograph (2 μm) of the flower-shaped boiling heat transfer structure in example 4 of the present application;
FIG. 8c is a scanning electron micrograph (500nm, enlarged view of a portion of FIG. 8 a) of the flower-type boiling heat transfer structure in example 4 of the present application;
FIG. 9a is a boiling heat transfer performance graph (heat flux density) of the flower-type boiling heat transfer structure in example 4 of the present application;
FIG. 9b is a boiling heat transfer performance graph (heat transfer coefficient) of the flower-type boiling heat transfer structure in example 4 of this application.
Detailed Description
The present invention will be more fully understood from the following detailed description, which should be read in conjunction with the accompanying drawings. Detailed embodiments of the present invention are disclosed herein; however, it is to be understood that the disclosed embodiments are merely exemplary of the invention, which can be embodied in various forms. Therefore, specific functional details disclosed herein are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the present invention in virtually any appropriately detailed embodiment.
In an embodiment of the application, a flower-shaped boiling heat transfer structure is provided, which comprises a copper substrate, wherein a micro-nano porous copper film covers the surface of the copper substrate, the micro-nano porous film takes a copper micro-cone as a main body, and a nickel nano-cone covers the surface of the micro-nano porous filmForming a hierarchical composite cone structure; unique micro-nano porous structures are formed among the composite cone structures; the average height of the copper micrometer cone of the main body is 3-8 mu m, the diameter of the bottom of the copper micrometer cone is 500-2200 nm, and the diameter of the tip of the copper micrometer cone is 0-50 nm; preferably, the distribution density of the copper microcones is 1.0 × 105～1.0×107Per mm2(ii) a Preferably, the size of the porous micro-cavity structure is 1-12 μm; the height of each grading nanocone structure is more than 100nm and less than or equal to 1000nm, the diameter of the bottom is 50nm-500nm, and the diameter of the tip is more than 1nm and less than or equal to 50 nm.
In a preferred embodiment, the material of the substrate includes copper, copper alloy and other metal materials, and the shape of the copper material is not limited, and the copper material may be a flat copper sheet, a copper sheet, or a curved surface, such as the inner and outer surfaces of a copper tube.
In an embodiment of the present application, a method for preparing a flower-shaped boiling heat transfer structure is provided, including: taking copper as a working electrode, placing the copper as a counter electrode and a reference electrode in a weak alkaline copper salt electrolyte system to form a reduction system, applying a reduction current between the working electrode and the counter electrode, and electroplating to form a copper micrometer cone main body structure; and then placing the copper micrometer cone serving as a working electrode, a counter electrode and a reference electrode in a weak acid nickel salt electrolyte system to form a reduction system, applying a reduction current between the working electrode and the counter electrode, and performing an electrodeposition reaction of nickel on the copper micrometer cone to form a micro-nano porous membrane on the surface of the copper material.
In a preferred embodiment, the weakly acidic nickel salt electrolyte contains 0.5-2.0 mol/L nickel sulfate; 0.10-0.80 mol/L of boric acid; 1-4 mol/L of ethylenediamine hydrochloride.
In a preferred embodiment, the working electrode and counter electrode are spaced apart by more than 0mm but less than 60mm during the electrodeposition reaction.
In a preferred embodiment, the current density applied in the electrodeposition reaction is 0.01-0.03A/cm2。
In a preferred embodiment, the temperature of the weakly acidic nickel salt electrolyte is 55-65 ℃, and the pH value is 4.0.
In a preferred embodiment, the electrodeposition reaction time of nickel is 0-10 min, preferably 3-9min, and more preferably 5 min.
In a preferred embodiment, the material of the counter electrode can be selected from metal or semiconductor material, such as graphite, but not limited thereto. The base material comprises copper, copper alloy and other metal materials, and the shape of the copper material is not limited, and the copper material can be a flat copper sheet or a copper plate, and can also be a curved surface, such as the inner surface and the outer surface of a copper pipe.
Example 1
The embodiment relates to a flower-shaped copper-nickel micro-nano porous structure prepared by electrochemical deposition, which is used for efficient boiling heat transfer. With reference to fig. 1, the specific steps are as follows:
(1) and (3) polishing the surface of the copper test piece, washing the surface by using ultrapure water, and drying the surface by using high-purity nitrogen. This step is to remove the surface oxide layer.
(2) And (2) placing the copper test piece treated in the step (1) as a working electrode in a weak alkaline copper salt electrolyte solution, wherein a platinum electrode is used as a counter electrode, and silver/silver chloride is used as a reference electrode. The working electrode is connected through a lead, and the counter electrode and the reference electrode form a loop. Controlling the distance between the two electrodes to be 60mm, carrying out constant-voltage electrodeposition reaction in a constant-temperature water bath at 75 ℃, controlling the voltage to be-0.92V, keeping the electrodeposition time for 20min, and forming a copper micrometer cone main body structure on the surface of a copper test piece through electroplating.
The electrolyte comprises the following components: 0.03mol/L of copper sulfate, 0.24mol/L of sodium hypophosphite, 0.0024mol/L of nickel sulfate, 0.5mol/L of trisodium citrate, 0.05mol/L of boric acid and 6g/L of polyethylene glycol, and the pH value of the solution is controlled to be 8.0.
(3) The obtained copper micro-cone was placed in a weakly acidic (pH 4.0) nickel salt electrolyte solution as a working electrode, and a platinum electrode was used as a counter electrode and silver/silver chloride was used as a reference electrode. The working electrode is connected through a lead, and the counter electrode and the reference electrode form a loop. Controlling the distance between the two electrodes to be 60mm, and carrying out constant current density electrodeposition reaction in a constant temperature water bath at 60 ℃, wherein the current density is controlled to be 0.03A/cm2The electrodeposition time was 3 min.
The weakly acidic nickel salt electrolyte contains 0.84mol/L of nickel sulfate, 0.57mol/L of boric acid and 2.5mol/L of ethylenediamine hydrochloride.
The front view and the cross-sectional view of the obtained target sample are shown in fig. 2a-2c, and the structure size is as follows: the size of the main micron copper cone structure is as follows: the average height is 4.5 +/-0.2 mu m, the diameter of the bottom is 0.8 +/-0.1 mu m, and the diameter of the tip is 14.4 +/-0.3 nm; the size of the graded nickel nano cone structure is as follows: the average height is 250 + -20 nm, the diameter of the bottom is 200 + -18 nm, and the diameter of the tip is 8.1 + -0.3 nm.
(4) After the electroplating is finished, the electroplating solution is washed clean by ultrapure water and dried by high-purity nitrogen.
The boiling heat transfer performance test shows that compared with the common copper surface, the nucleation boiling starting point of the flower-shaped copper-nickel structure is advanced by 37.0 percent, the maximum heat transfer efficiency is improved by 177.4 percent, the critical heat flow density value is improved by 69.4 percent, as shown in figures 3a and 3b, the superheat degree corresponding to the nucleation boiling starting point is 7.5K, and the maximum heat transfer coefficient is 125.4kWm-2K-1The critical heat flux density was 281.0Wcm-2。
Example 2
The embodiment relates to a flower-shaped copper-nickel micro-nano porous structure prepared by electrochemical deposition and used for enhancing boiling heat transfer. The method comprises the following specific steps:
(1) and (3) polishing the surface of the copper test piece, washing the surface by using ultrapure water, and drying the surface by using high-purity nitrogen. This step is to remove the surface oxide layer.
(2) And (2) placing the copper test piece treated in the step (1) as a working electrode in a weak alkaline copper salt electrolyte solution, wherein a platinum electrode is used as a counter electrode, and silver/silver chloride is used as a reference electrode. The working electrode is connected through a lead, and the counter electrode and the reference electrode form a loop. Controlling the distance between the two electrodes to be 60mm, carrying out constant-voltage electrodeposition reaction in a constant-temperature water bath at 75 ℃, controlling the voltage to be-0.92V, keeping the electrodeposition time for 20min, and forming a copper micrometer cone main body structure on the surface of a copper test piece through electroplating.
The electrolyte comprises the following components: 0.03mol/L of copper sulfate, 0.24mol/L of sodium hypophosphite, 0.0024mol/L of nickel sulfate, 0.5mol/L of trisodium citrate, 0.05mol/L of boric acid and 6g/L of polyethylene glycol, and the pH value of the solution is controlled to be 8.0.
(3) The obtained copper micro-cone was placed in a weakly acidic (pH 4.0) nickel salt electrolyte solution as a working electrode, and a platinum electrode was used as a counter electrode and silver/silver chloride was used as a reference electrode. The working electrode is connected through a lead, and the counter electrode and the reference electrode form a loop. Controlling the distance between the two electrodes to be 60mm, and carrying out constant current density electrodeposition reaction in a constant temperature water bath at 60 ℃, wherein the current density is controlled to be 0.02A/cm2The electrodeposition time was continued for 5 min.
The weakly acidic nickel salt electrolyte contains 0.84mol/L of nickel sulfate, 0.57mol/L of boric acid and 2.5mol/L of ethylenediamine hydrochloride.
The front view and the cross-sectional view of the obtained target sample are shown in fig. 4a-4c, and the structure size is as follows: the size of the main micron copper cone structure is as follows: the average height is 4.5 +/-0.2 mu m, the diameter of the bottom is 0.8 +/-0.1 mu m, and the diameter of the tip is 14.4 +/-0.3 nm; the size of the graded nickel nano cone structure is as follows: the average height is 580 + -25 nm, the diameter of the bottom is 350 + -22 nm, and the diameter of the tip is 9.8 + -0.2 nm.
(4) After the electroplating is finished, the electroplating solution is washed clean by ultrapure water and dried by high-purity nitrogen.
The boiling heat transfer performance test shows that compared with the common copper surface, the nucleation boiling starting point of the flower-shaped copper-nickel structure is advanced by 40.3%, the maximum heat transfer efficiency is improved by 227.8%, the critical heat flow density value is improved by 71.4%, as shown in fig. 5a and 5b, the superheat degree corresponding to the nucleation boiling starting point is 7.1K, and the maximum heat transfer coefficient is 148.2kWm-2K-1The critical heat flux density was 284.4Wcm-2。
Example 3
The embodiment relates to a flower-shaped copper-nickel micro-nano porous structure prepared by electrochemical deposition and used for enhancing boiling heat transfer. The method comprises the following specific steps:
(1) and (3) polishing the surface of the copper test piece, washing the surface by using ultrapure water, and drying the surface by using high-purity nitrogen. This step is to remove the surface oxide layer.
(2) And (2) placing the copper test piece treated in the step (1) as a working electrode in a weak alkaline copper salt electrolyte solution, wherein a platinum electrode is used as a counter electrode, and silver/silver chloride is used as a reference electrode. The working electrode is connected through a lead, and the counter electrode and the reference electrode form a loop. Controlling the distance between the two electrodes to be 60mm, carrying out constant-voltage electrodeposition reaction in a constant-temperature water bath at 75 ℃, controlling the voltage to be-0.92V, keeping the electrodeposition time for 20min, and forming a copper micrometer cone main body structure on the surface of a copper test piece through electroplating.
The electrolyte comprises the following components: 0.03mol/L of copper sulfate, 0.24mol/L of sodium hypophosphite, 0.0024mol/L of nickel sulfate, 0.5mol/L of trisodium citrate, 0.05mol/L of boric acid and 6g/L of polyethylene glycol, and the pH value of the solution is controlled to be 8.0.
(3) The obtained copper micro-cone was placed in a weakly acidic (pH 4.0) nickel salt electrolyte solution as a working electrode, and a platinum electrode was used as a counter electrode and silver/silver chloride was used as a reference electrode. The working electrode is connected through a lead, and the counter electrode and the reference electrode form a loop. Controlling the distance between the two electrodes to be 60mm, and carrying out constant current density electrodeposition reaction in a constant temperature water bath at 60 ℃, wherein the current density is controlled to be 0.02A/cm2The electrodeposition time was 7 min.
The weakly acidic nickel salt electrolyte contains 0.84mol/L of nickel sulfate, 0.57mol/L of boric acid and 2.5mol/L of ethylenediamine hydrochloride.
The front view and the cross-sectional view of the obtained target sample are shown in fig. 6a-6c, and the structure size is as follows: the size of the main micron copper cone structure is as follows: the average height is 4.5 +/-0.2 mu m, the diameter of the bottom is 0.8 +/-0.1 mu m, and the diameter of the tip is 14.4 +/-0.3 nm; the size of the graded nickel nano cone structure is as follows: the average height was 860. + -.45 nm, the diameter of the base was 430. + -.36 nm, and the diameter of the tip was 11.4. + -. 0.2 nm.
(4) After the electroplating is finished, the electroplating solution is washed clean by ultrapure water and dried by high-purity nitrogen.
The boiling heat transfer performance test shows that compared with the common copper surface, the nucleation boiling starting point of the flower-shaped copper-nickel structure is advanced by 34.4%, the maximum heat transfer efficiency is improved by 187.2%, the critical heat flow density value is improved by 67.7%, as shown in fig. 7a and 7b, the superheat degree corresponding to the nucleation boiling starting point is 7.8K, and the maximum heat transfer coefficient is 121.5kWm-2K-1Critical point ofThe heat flow density was 278.3Wcm-2。
Example 4
The embodiment relates to a flower-shaped copper-nickel micro-nano structure prepared by electrochemical deposition, which is used for enhancing boiling heat transfer. The method comprises the following specific steps:
(1) and (3) polishing the surface of the copper test piece, washing the surface by using ultrapure water, and drying the surface by using high-purity nitrogen. This step is to remove the surface oxide layer.
(2) And (2) placing the copper test piece treated in the step (1) as a working electrode in a weak alkaline copper salt electrolyte solution, wherein a platinum electrode is used as a counter electrode, and silver/silver chloride is used as a reference electrode. The working electrode is connected through a lead, and the counter electrode and the reference electrode form a loop. Controlling the distance between the two electrodes to be 60mm, carrying out constant-voltage electrodeposition reaction in a constant-temperature water bath at 75 ℃, controlling the voltage to be-0.92V, keeping the electrodeposition time for 20min, and forming a copper micrometer cone main body structure on the surface of a copper test piece through electroplating.
The electrolyte used in this example consists of: 0.03mol/L of copper sulfate, 0.24mol/L of sodium hypophosphite, 0.0024mol/L of nickel sulfate, 0.5mol/L of trisodium citrate, 0.05mol/L of boric acid and 6g/L of polyethylene glycol, and the pH value of the solution is controlled to be 8.0.
(3) The obtained copper micro-cone was placed in a weakly acidic (pH 4.0) nickel salt electrolyte solution as a working electrode, and a platinum electrode was used as a counter electrode and silver/silver chloride was used as a reference electrode. The working electrode is connected through a lead, and the counter electrode and the reference electrode form a loop. Controlling the distance between the two electrodes to be 60mm, and carrying out constant current density electrodeposition reaction in a constant temperature water bath at 60 ℃, wherein the current density is controlled to be 0.02A/cm2The electrodeposition time lasted 9 min.
The weakly acidic nickel salt electrolyte contains 0.84mol/L of nickel sulfate, 0.57mol/L of boric acid and 2.5mol/L of ethylenediamine hydrochloride.
The front view and the cross-sectional view of the obtained target sample are shown in fig. 8a-8c, and the structure size is as follows: the size of the main micron copper cone structure is as follows: the average height is 4.5 +/-0.2 mu m, the diameter of the bottom is 0.8 +/-0.1 mu m, and the diameter of the tip is 14.4 +/-0.3 nm; the size of the graded nickel nano cone structure is as follows: the average height is 950 + -40 nm, the diameter of the bottom is 500 + -38 nm, and the diameter of the tip is 13.6 + -0.1 nm.
(4) After the electroplating is finished, the electroplating solution is washed clean by ultrapure water and dried by high-purity nitrogen.
The boiling heat transfer performance test shows that compared with the common copper surface, the nucleation boiling starting point of the flower-shaped copper-nickel structure is advanced by 17.6%, the maximum heat transfer efficiency is improved by 120.5%, the critical heat flow density value is improved by 47.1%, as shown in fig. 9a and 9b, the superheat degree corresponding to the nucleation boiling starting point is 9.8K, and the maximum heat transfer coefficient is 93.3kWm-2K-1The critical heat flux density was 244.0Wcm-2。
In conclusion, the invention has the following beneficial effects:
1. the invention adopts metal materials such as copper and the like, has high heat conductivity and low price. Compared with inorganic substances such as silicon and oxides such as zinc oxide used by other researchers, the material is more beneficial to enhancing boiling heat transfer, and is more expected to be applied to actual production.
2. The preparation method can directly carry out electro-deposition on the surface of the required copper material to obtain the graded composite cone structure in situ without the assistance of a template. The electrolyte formula is economical and easy to obtain, the operation process is simple, and the method is suitable for industrial scale application.
3. The stepped composite cone structure adopted by the invention is used for enhancing boiling heat transfer, has a larger effective heat transfer area and far more nucleation sites, and is an efficient boiling heat transfer interface.
The aspects, embodiments, features and examples of the present invention should be considered as illustrative in all respects and not intended to be limiting of the invention, the scope of which is defined only by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed invention.
The use of headings and chapters in this disclosure is not meant to limit the disclosure; each section may apply to any aspect, embodiment, or feature of the disclosure.
Throughout this specification, where a composition is described as having, containing, or comprising specific components or where a process is described as having, containing, or comprising specific process steps, it is contemplated that the composition of the present teachings also consist essentially of, or consist of, the recited components, and the process of the present teachings also consist essentially of, or consist of, the recited process steps.
Unless specifically stated otherwise, use of the terms "comprising", "including", "having" or "having" is generally to be understood as open-ended and not limiting.
The use of the singular herein includes the plural (and vice versa) unless specifically stated otherwise. Furthermore, the singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. In addition, where the term "about" is used before a quantity, the present teachings also include the particular quantity itself unless specifically stated otherwise.
It should be understood that the order of steps or the order in which particular actions are performed is not critical, so long as the teachings of the invention remain operable. Further, two or more steps or actions may be performed simultaneously.
In addition, the inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
While the invention has been described with reference to illustrative embodiments, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims. Moreover, unless specifically stated any use of the terms first, second, etc. do not denote any order or importance, but rather the terms first, second, etc. are used to distinguish one element from another.

Claims (10)

1. A flower boiling heat transfer structure comprising:
a substrate;
array needle-like micron copper structure protruding on the surface of the substrate; and
and the graded nanocones protrude out of the surface of the micron copper.
2. The flower-type boiling heat transfer structure of claim 1, wherein the average height of the micro copper structures is 3 to 8 μm, the diameter of the bottom is 500 to 2200nm, the diameter of the tip is 0 to 50nm, and the distribution density is 1.0 x 105～1.0×107Per mm2。
3. The flower-type boiling heat transfer structure of claim 1, wherein the micro-cavity size formed between the micron copper structures is 1-12 μm.
4. The flower type boiling heat transfer structure of claim 1, wherein the height of each of the graded nanocone structures is greater than 100nm and 1000nm or less;
the diameter of the bottom of each grading nanocone structure is 50nm-500 nm;
the diameter of the tip of each grading nano-cone structure is more than 1nm and less than or equal to 50 nm.
5. The flower-type boiling heat transfer structure of claim 1, wherein the substrate is copper or a copper alloy.
6. The flower-type boiling heat transfer structure of claim 1, wherein the graded nanocones are made of nickel, copper, gold or silver.
7. The method of producing a flower-type boiling heat transfer structure of any one of claims 1 to 6, comprising:
the micron copper structure is formed on the surface of the base material by electrodeposition or chemical plating in electrolyte;
the graded nano cone is formed on the surface of the main micro cone by electrodeposition or chemical plating in an electrolyte.
8. The method of claim 7, wherein the current density applied during the electrodeposition reaction is 0.01 to 0.03A/cm2The electrodeposition reaction time is 0-10 min, preferably 3-9min, and more preferably 5 min.
9. The method of manufacturing a flower-type boiling heat transfer structure according to claim 7, wherein the flower-type boiling heat transfer structure is applied to water, ethanol, or FC-72.
10. A flower boiling heat transfer structure comprising:
a substrate;
the array is protruded on the first-level vertebral body on the surface of the substrate; and
and the grading cone protrudes out of the surface of the primary cone body.
CN201910619049.8A 2019-07-10 2019-07-10 Flower-shaped boiling heat transfer structure and preparation method thereof Pending CN112210802A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113230530A (en) * 2021-04-30 2021-08-10 苏州大学 Preparation method of composite structure silicon microneedle

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106400067A (en) * 2016-09-18 2017-02-15 中山大学 Single-layer micro-nano double-scale enhanced boiling heat transfer copper surface structure and preparing method thereof
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106400067A (en) * 2016-09-18 2017-02-15 中山大学 Single-layer micro-nano double-scale enhanced boiling heat transfer copper surface structure and preparing method thereof
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

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
BO SHI等: ""Pool boiling heat transfer enhancement with copper nanowire arrays"", 《APPLIED THERMAL ENGINEERING》 *
HONG LI等: ""In Situ Growth of Densely Packed Single-Crystal Copper Nanocone Structure Films with Condensate Microdrop Self-Removal Function on Copper Surfaces"", 《ADV. MATER. INTERFACES》 *
WENJING ZHANG等: ""Preparation of super-hydrophobic Cu/Ni coating with micro-nano hierarchical structure"", 《MATERIALS LETTERS》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113230530A (en) * 2021-04-30 2021-08-10 苏州大学 Preparation method of composite structure silicon microneedle
CN113230530B (en) * 2021-04-30 2022-09-16 苏州大学 Preparation method of composite structure silicon microneedle

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Application publication date: 20210112