CN109023459B - Double-layer multi-scale enhanced boiling surface structure and preparation method thereof - Google Patents

Double-layer multi-scale enhanced boiling surface structure and preparation method thereof Download PDF

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CN109023459B
CN109023459B CN201810880776.5A CN201810880776A CN109023459B CN 109023459 B CN109023459 B CN 109023459B CN 201810880776 A CN201810880776 A CN 201810880776A CN 109023459 B CN109023459 B CN 109023459B
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scale
layer
copper
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surface structure
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CN109023459A (en
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吕树申
莫冬传
汪亚桥
罗佳利
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National Sun Yat Sen University
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—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
    • 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
    • C25D5/18—Electroplating using modulated, pulsed or reversing current
    • 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 double-layer multi-scale enhanced boiling surface structure and a preparation method thereof, wherein the double-layer multi-scale enhanced boiling surface structure comprises a forest-shaped array porous layer, and then a layer of micro-nano dual-scale honeycomb porous copper structure is deposited on the surface of the forest-shaped array porous layer; the forest-shaped array porous layer is prepared by an electrodeposition method, the average spacing of crystal branches is 1-2 mm, and the height is 1-5 mm; the cellular porous copper structure is provided with macropores with micron scale, the hole wall is formed by copper crystal branches, and gaps among the crystal branches are nano-scale gaps. The double-layer structure has the characteristics of more nucleation sites of the honeycomb structure and strong liquid absorption performance of the forest-shaped array structure, thereby having better boiling heat transfer performance. The double-layer composite multi-scale reinforced surface is obtained by an electrodeposition method, is simple to prepare and has good application prospect in large scale.

Description

Double-layer multi-scale enhanced boiling surface structure and preparation method thereof
Technical Field
The invention relates to a double-layer multi-scale enhanced boiling surface and a preparation method thereof, belonging to the field of heat and mass transfer.
Technical Field
Enhanced boiling heat transfer is one of the main methods for solving the heat dissipation problem of narrow-space and high-power microelectronic devices. Machining structures, metal powder sintering (CN 105180709 a), nanoporous structures, micro-nanostructures, and surfaces with micro-nanostructured composite porous structures are common boiling-enhanced techniques. Wherein the cellular micro-nano dual-scale porous structure surface (Wang, Y.Q.O., Luo, J.L.Heng, Y.Y., Mo, D.C., and Lyu, S.S.S., int. J.Heat Mass Transf.119, pp. 333. 342, (2018)), and the forest-like porous surface have enhanced boiling Heat exchange performance with good performance (Wang, Y.Q. Lyu, S.S., Luo, J.L.Luo, Z.Y., Fu, Y.X.Heng, Y.Zhang, J.H.and, Mo, D.C., Appl SuScirf, 422, pp. 388. 393, (2017)). The cellular micro-nano dual-scale porous surface has the characteristics of more nucleation points, low wall surface superheat degree and high heat transfer coefficient by pool boiling. The porous surface of the forest-shaped array has the characteristics of strong liquid absorption capacity and high CHF pool boiling, but in the boiling process, the nucleation points are few, and the superheat degree of the wall surface is relatively high.
Disclosure of Invention
The invention aims to provide a double-layer multi-scale enhanced boiling surface structure and a preparation method thereof, which utilize a honeycomb structure to provide more nucleation points and combine the characteristic of strong liquid absorption capacity of a dendritic array, thereby further enhancing the heat transfer effect of the boiling surface.
In order to achieve the purpose, the invention adopts the technical scheme that:
a double-layer multi-scale enhanced boiling surface structure comprises a forest-shaped array porous layer, and then a layer of micro-nano dual-scale honeycomb porous copper structure is deposited on the surface of the forest-shaped array porous layer; the forest-shaped array porous layer is prepared by an electrodeposition method, the average spacing of crystal branches is 1-2 mm, and the height is 1-5 mm; the cellular porous copper structure is provided with micro-scale macropores, the hole wall is formed by copper crystal branches, gaps of the crystal branches are nano-scale gaps, and the size of the nano-scale gaps is from several nanometers to hundreds of nanometers; the average diameter of the macropores is 1-1000 μm.
The preparation method of the double-layer multi-scale enhanced boiling surface structure comprises the following steps:
(1) treating a metal matrix: firstly, removing surface oxides by using a dilute sulfuric acid solution, then cleaning surface oil stains by using a high-concentration alkali liquor, and then washing the surface oil stains for a plurality of times by using deionized high-purity water;
(2) pre-plating a metal substrate: in order to increase the mechanical strength of the deposited porous copper, pre-plating is carried out before depositing the copper crystal branches;
(3) preparing a forest-shaped array: using a method of gradually increasing current, taking the treated metal matrix as a cathode, keeping the current acceleration rate to be certain in a solution taking sulfuric acid and copper sulfate as electrolytes, keeping the initial current density to be the same, keeping the total reaction electric quantity to be more than 0 ℃, cleaning and drying the obtained sample, and then carrying out heat treatment;
(4) depositing honeycomb micro-nano double-scale porous copper: the method adopts a constant current method, the surface of the copper crystal branch array is taken as a cathode, the electrodeposition reaction is carried out in the solution taking copper sulfate as electrolyte, and the total reaction electric quantity is more than 0C.
(5) And (3) heat treatment of the product: and carrying out heat treatment under the condition of reducing protective atmosphere to further enhance the mechanical strength of the product.
In the preparation method, in the step (3), the initial current density is 0.01-5.0A cm-2。
In the preparation method, in the step (3), the initial current density increase rate is 0.01-2000 mA cm-2 s-1。
In the preparation method, in the step (3), the molar concentration of the sulfuric acid is 0.01-10M, and the molar concentration of the copper sulfate is 0.04M-saturation.
In the preparation method, in the step (4), the constant current has a current density of 0.05-10.0A cm-2。
In the preparation method, in the step (4), the time of the electrodeposition reaction is 2-1800 s.
In the preparation method, in the step (5), the heat treatment is carried out at 400-900 ℃ in a reducing atmosphere for sintering, so that the mechanical strength of the product is increased.
Compared with the prior art, the invention has the following beneficial effects:
1. the double-layer composite multi-scale reinforced surface has the characteristics of multiple gasification cores of a honeycomb micro-nano double-scale porous structure and strong liquid absorption capacity of the surface of a forest-shaped array. Thereby leading the double-layer composite multi-scale surface to have higher boiling heat transfer performance.
2. The two layers of the double-layer composite multi-scale reinforced surface are both obtained by an electrodeposition method, the preparation is simple, and the method has good application prospect in large scale.
Drawings
FIG. 1 is a multi-scale enhanced boiling surface pore wall SEM picture (cellular micro-nano dual-scale porous copper structure);
FIG. 2 is a multi-scale enhanced boiling surface SEM image (forest-like array of the bottom layer as seen from the interior of the honeycomb structure);
fig. 3 is a pool boiling curve.
Detailed Description
Aiming at the characteristic that the temperature of the traditional honeycomb micro-nano multi-scale porous material is violently and surly increased after film boiling in the boiling process, the invention provides a double-layer composite reinforced boiling surface combining a honeycomb micro-nano double-scale porous surface and a forest-shaped array surface, and the characteristic that the honeycomb structure provides more nucleation points and combines the dendritic array with strong liquid absorption capacity is utilized, so that the boiling surface has a higher boiling reinforcing effect.
The present invention is described in further detail below with reference to the specific drawings and preferred examples.
Example 1
(1) Treating a metal matrix: firstly, dilute sulphuric acid solution is used for removing surface oxides, then high-concentration alkali liquor is used for cleaning surface greasy dirt, and then deionized high-purity water is used for washing for 3 times.
(2) Pre-plating a metal substrate: in order to increase the mechanical strength of the deposited copper dendrites, pre-plating is performed before the deposition of the copper dendrites. The pre-plating solution is the same as the solution of the copper dendrites. The pre-plating current density is 0.06A cm-2The preplating time is 3 min.
(3) And (3) deposition of a forest array layer: adopting a method of gradually increasing current, taking a treated metal matrix as a cathode, and adding 0.6M CuSO4、0.2 M H2SO4In the solution (2), the electrodeposition condition is set such that the current increase rate is 2 mA cm-2 s-1Initial current density of 0.1A cm-2The total reaction charge was 180C to carry out electrodeposition.
(4) Depositing honeycomb micro-nano double-scale porous copper: using a constant current method, the surface of the copper dendrite array is a cathode, the concentration of sulfuric acid is 1.0M, the concentration of copper sulfate is 0.4M, and the current density is 1A cm in a solution with copper sulfate as electrolyte-2The reaction time was 60 s.
(5) And (3) heat treatment of the product: sintering under the condition of reducing protective atmosphere, wherein the sintering temperature is 710 ℃, and the temperature is kept for 30 min, so that the mechanical strength of the product is further enhanced. After the treatment, the electron micrographs are shown in FIGS. 1 and 2. Wherein, fig. 1 is a honeycomb micro-nano dual-scale porous copper structure, and fig. 2 is a forest-shaped array of a bottom layer seen from the inside of the honeycomb structure. As can be seen from fig. 3, the boiling heat transfer performance of the product (double surface) is significantly better than that of a pure honeycomb surface, and a pure forest-like array surface.

Claims (7)

1. A double-layer multi-scale enhanced boiling surface structure is characterized in that: the method comprises the steps of carrying out tree forest array porous layer deposition on a layer of micro-nano dual-scale honeycomb porous copper structure on the surface of a tree forest array porous layer; the forest-shaped array porous layer is prepared by an electrodeposition method, the average spacing of crystal branches is 1-2 mm, and the height is 1-5 mm; the cellular porous copper structure is provided with micro-scale macropores, the hole wall is formed by copper crystal branches, gaps of the copper crystal branches are nano-scale gaps, and the size of the nano-scale gaps is from several nanometers to hundreds of nanometers; the average diameter of macropores is 1-1000 mu m;
the preparation method of the double-layer multi-scale enhanced boiling surface structure comprises the following steps:
(1) treating a metal matrix: firstly, removing surface oxides by using a dilute sulfuric acid solution, then cleaning surface oil stains by using a high-concentration alkali liquor, and then washing the surface oil stains for a plurality of times by using deionized high-purity water;
(2) pre-plating a metal substrate: pre-plating before depositing copper crystal branches;
(3) preparing a forest-shaped array: using a method of gradually increasing current, taking the treated metal matrix as a cathode, keeping the current acceleration rate to be certain in a solution taking sulfuric acid and copper sulfate as electrolytes, keeping the initial current density to be the same, keeping the total reaction electric quantity to be more than 0 ℃, cleaning and drying the obtained sample, and then carrying out heat treatment;
(4) depositing honeycomb micro-nano double-scale porous copper: using a constant current method, taking the surface of a copper crystal branch array as a cathode, and carrying out electrodeposition reaction in a solution taking sulfuric acid and copper sulfate as electrolytes, wherein the total reaction electric quantity is more than 0 ℃;
(5) and (3) heat treatment of the product: and carrying out heat treatment under the condition of reducing protective atmosphere.
2. The surface structure of claim 1, wherein: in the step (3), the initial current density is 0.01-5.0A-cm-2。
3. The surface structure of claim 1, wherein: in the step (3), the initial density of the current is increased by 0.01-2000 mA-cm-2·s-1。
4. The surface structure of claim 1, wherein: in the step (3), the molar concentration of the sulfuric acid is 0.01-10M, and the molar concentration of the copper sulfate is 0.04M-saturation.
5. The surface structure of claim 1, wherein: in the step (4), the current density of the constant current is 0.05-10.0A-cm-2。
6. The surface structure of claim 1, wherein: in the step (4), the step (c),
the time of the electrodeposition reaction is 2-1800 s.
7. The surface structure of claim 1, wherein: in the step (5), the temperature of the heat treatment is 400-900 ℃ for sintering in a reducing atmosphere.
CN201810880776.5A 2018-08-04 2018-08-04 Double-layer multi-scale enhanced boiling surface structure and preparation method thereof Active CN109023459B (en)

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CN110158127B (en) * 2019-05-15 2021-02-02 重庆大学 Method for strengthening critical heat flux density of heat transfer surface liquid film drying
CN110408977B (en) * 2019-06-20 2021-05-28 苏州潜寻新能源科技有限公司 Multi-scale enhanced boiling functional surface and composite preparation method
CN112176369A (en) * 2019-07-03 2021-01-05 中国科学院苏州纳米技术与纳米仿生研究所 High-efficiency boiling heat transfer copper material and preparation method thereof
CN112210802A (en) * 2019-07-10 2021-01-12 中国科学院苏州纳米技术与纳米仿生研究所 Flower-shaped boiling heat transfer structure and preparation method thereof

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