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CN109023459A - A kind of multiple dimensioned surface texture and preparation method thereof for strengthening boiling of bilayer - Google Patents

A kind of multiple dimensioned surface texture and preparation method thereof for strengthening boiling of bilayer Download PDF

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CN109023459A
CN109023459A CN201810880776.5A CN201810880776A CN109023459A CN 109023459 A CN109023459 A CN 109023459A CN 201810880776 A CN201810880776 A CN 201810880776A CN 109023459 A CN109023459 A CN 109023459A
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CN109023459B (en
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吕树申
莫冬传
汪亚桥
罗佳利
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Sun Yat Sen University
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10Electroplating with more than one layer of the same or of different metals
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • 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
    • C25D5/18Electroplating using modulated, pulsed or reversing current
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48After-treatment of electroplated surfaces
    • C25D5/50After-treatment of electroplated surfaces by heat-treatment

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Abstract

本发明公开了一种双层多尺度强化沸腾的表面结构及其制备方法,包括树林状阵列多孔层,然后在其表面沉积一层具有微纳双尺度的蜂窝状多孔铜结构;所述树林状阵列多孔层采用电沉积法制备,晶枝的平均间距为1μm~2mm,高度为1μm~5mm;所述蜂窝状多孔铜结构具有微米尺度的大孔,孔壁由铜晶枝构成,晶枝的间隙是纳米级缝隙。这种双层结构兼具蜂窝状结构成核位点多和树林状阵列结构吸液性能强的特性,从而具有更好的沸腾传热性能。双层复合多尺度强化表面是由电沉积法得到,制备简单,有很好的规模化运用的前景。

The invention discloses a double-layer multi-scale enhanced boiling surface structure and a preparation method thereof, which comprises a forest-like array porous layer, and then deposits a layer of micro-nano double-scale honeycomb porous copper structure on its surface; the forest-like The array porous layer is prepared by electrodeposition, the average spacing of crystal dendrites is 1 μm~2mm, and the height is 1 μm~5mm; the honeycomb porous copper structure has macropores with micron scale, and the hole walls are composed of copper crystal dendrites, and the gap between crystal dendrites is nanometer level gap. This double-layer structure combines the characteristics of many nucleation sites of the honeycomb structure and the strong liquid absorption performance of the tree-like array structure, thus having better boiling heat transfer performance. The double-layer composite multi-scale strengthened surface is obtained by electrodeposition, which is easy to prepare and has good prospects for large-scale application.

Description

一种双层多尺度强化沸腾的表面结构及其制备方法A surface structure of double-layer multi-scale enhanced boiling and its preparation method

技术领域technical field

本发明涉及一种双层多尺度强化沸腾表面及其制备方法,属于传热传质领域。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.

技术背景technical background

强化沸腾传热是解决窄空间、大功率微电子器件散热问题的主要方法之一。机械加工结构、金属粉末烧结(CN 105180709 A)、纳米多孔结构、微纳米结构以及具有微纳复合多孔结构表面是常用的强化沸腾的技术方法。其中蜂窝状的微纳双尺度多孔结构表面(Wang, Y.-Q., Luo, J.-L., Heng, Y., Mo, D.-C., and Lyu, S.-S., Int. J. HeatMass Transf., 119, pp. 333-342, (2018))、和树林状的多孔表面都具有良好性能的强化沸腾换热性能(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 Surf Sci, 422, pp. 388-393,(2017).)。蜂窝状的微纳双尺度多孔表面具有成核点多,壁面过热度低、传热系数高的池沸腾特点。而树林状阵列的多孔表面具有吸液能力强,CHF高的池沸腾特点,但是在沸腾过程中,其成核点较少,壁面过热度相对较高。Enhancing boiling heat transfer is one of the main methods to solve the heat dissipation problem of narrow space and high power microelectronic devices. Machining structures, metal powder sintering (CN 105180709 A), nano-porous structures, micro-nano structures, and surfaces with micro-nano composite porous structures are commonly used technical methods to enhance boiling. Among them, the honeycomb micro-nano dual-scale porous structure surface (Wang, Y.-Q., Luo, J.-L., Heng, Y., Mo, D.-C., and Lyu, S.-S., Int. J. HeatMass Transf., 119, pp. 333-342, (2018)), and forest-like porous surfaces have good performance of enhanced boiling heat transfer 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 Surf Sci, 422, pp. 388-393, (2017).). The honeycomb micro-nano dual-scale porous surface has the characteristics of pool boiling with many nucleation points, low wall superheat and high heat transfer coefficient. The porous surface of the tree-like array has the characteristics of strong liquid absorption and high CHF pool boiling, but in the boiling process, its nucleation points are few, and the superheat of the wall is relatively high.

发明内容Contents of the invention

本发明的目的在于提出一种双层多尺度强化沸腾的表面结构及其制备方法,利用蜂窝状结构提供更多的成核点同时结合树枝状阵列吸液能力强的特点,从而进一步强化沸腾表面的传热效果。The purpose of the present invention is to propose a double-layer multi-scale enhanced boiling surface structure and its preparation method, using the honeycomb structure to provide more nucleation points and combining the characteristics of dendritic arrays with strong liquid absorption, thereby further strengthening the boiling surface heat transfer effect.

为了达到上述目的,本发明采取的技术方案是:In order to achieve the above object, the technical scheme that the present invention takes is:

一种双层多尺度强化沸腾的表面结构,包括树林状阵列多孔层,然后在其表面沉积一层具有微纳双尺度的蜂窝状多孔铜结构;所述树林状阵列多孔层采用电沉积法制备,晶枝的平均间距为1μm ~2 mm,高度为1μm ~5mm;所述蜂窝状多孔铜结构具有微米尺度的大孔,孔壁由铜晶枝构成,晶枝的间隙是纳米级缝隙,纳米级缝隙尺寸为数纳米到数百纳米之间;大孔的平均直径在1~1000 μm。A double-layer multi-scale enhanced boiling surface structure, including a forest-like array porous layer, and then depositing a layer of micro-nano double-scale honeycomb porous copper structure on its surface; the forest-like array porous layer is prepared by electrodeposition , the average spacing of crystal dendrites is 1 μm ~ 2 mm, and the height is 1 μm ~ 5mm; the honeycomb porous copper structure has macropores on a micron scale, and the hole walls are composed of copper crystal dendrites. The gaps between crystal dendrites are nanoscale gaps, and the nanoscale gap size It is between a few nanometers and hundreds of nanometers; the average diameter of macropores is between 1 and 1000 μm.

上述双层多尺度强化沸腾的表面结构的制备方法,包括如下步骤:The preparation method of the above-mentioned double-layer multi-scale enhanced boiling surface structure comprises the following steps:

(1)金属基体处理:首先使用稀硫酸溶液除去表面氧化物,然后用高浓度碱液清洗表面油污,接着使用去离子高纯水冲洗若干次;(1) Metal substrate treatment: first use dilute sulfuric acid solution to remove surface oxides, then use high-concentration lye to clean the surface oil, and then use deionized high-purity water to rinse several times;

(2)金属基体预镀:为了增加所沉积的多孔铜机械强度,在沉积铜晶枝前进行预镀;(2) Metal substrate pre-plating: In order to increase the mechanical strength of the deposited porous copper, pre-plating is performed before depositing copper dendrites;

(3)树林状阵列制备:使用逐渐增大电流的方法,处理过的金属基体为阴极,在硫酸和硫酸铜为电解质的溶液中,保持电流增速一定,起始电流密度相同,反应总电量大于0 C,得到的样品清洗吹干后进行热处理;(3) Forest-like array preparation: using the method of gradually increasing the current, the treated metal substrate is used as the cathode, and in the solution of sulfuric acid and copper sulfate as the electrolyte, the current growth rate is kept constant, the initial current density is the same, and the total reaction power If the temperature is greater than 0 C, the obtained sample is cleaned and dried and then heat-treated;

(4)蜂窝状微纳双尺度多孔铜沉积:使用恒电流的方法,铜晶枝阵列表面为阴极,在硫酸硫酸铜为电解质的溶液中,进行电沉积反应,反应总电量大于0 C。(4) Honeycomb micro-nano dual-scale porous copper deposition: using a constant current method, the surface of the copper dendrite array is the cathode, and the electrodeposition reaction is carried out in a solution of copper sulfate as the electrolyte, and the total reaction electricity is greater than 0 C.

(5)产品热处理:在还原保护气氛条件下,进行热处理,进一步增强产品机械强度。(5) Product heat treatment: Under the condition of reducing protective atmosphere, heat treatment is carried out to further enhance the mechanical strength of the product.

在上述的制备方法,步骤(3)中,电流起始密度为0.01~5.0 A cm-2In the above preparation method, in step (3), the initial current density is 0.01-5.0 A cm -2 .

在上述的制备方法,步骤(3)中,电流起始密度增速为0.01 ~ 2000 mA cm-2 s-1In the above preparation method, in step (3), the current initial density increases from 0.01 to 2000 mA cm -2 s -1 .

在上述的制备方法,步骤(3)中,所述硫酸的摩尔浓度为0.01~10 M,硫酸铜的摩尔浓度为0.04 M~饱和。In the above preparation method, in step (3), the molar concentration of the sulfuric acid is 0.01-10 M, and the molar concentration of copper sulfate is 0.04 M-saturated.

在上述的制备方法,步骤(4)中,所述恒电流的电流密度为0.05 ~ 10.0 A cm-2In the above preparation method, in step (4), the current density of the constant current is 0.05-10.0 A cm -2 .

在上述的制备方法,步骤(4)中,所述电沉积反应的时间为2 ~ 1800 s。In the above preparation method, in step (4), the electrodeposition reaction time is 2 to 1800 s.

在上述的制备方法,步骤(5)中,所述热处理的温度为400~900 ℃还原气氛中烧结,增加产品机械强度。In the above preparation method, in step (5), the temperature of the heat treatment is sintering in a reducing atmosphere at 400-900° C. to increase the mechanical strength of the product.

与现有技术相比,本发明具有如下有益效果:Compared with the prior art, the present invention has the following beneficial effects:

1、双层复合多尺度强化表面既具有蜂窝状微纳双尺度多孔结构气化核心多的特点,同时也具有树林状阵列表面吸液能力强的特点。从而使得双层复合多尺度表面具有更高的沸腾传热性能。1. The double-layer composite multi-scale reinforced surface not only has the characteristics of a honeycomb micro-nano dual-scale porous structure with many gasification cores, but also has the characteristics of a forest-like array surface with a strong liquid absorption capacity. Therefore, the double-layer composite multi-scale surface has higher boiling heat transfer performance.

2、双层复合多尺度强化表面的两层都是由电沉积法得到,制备简单,有很好的规模化运用的前景。2. The two layers of the double-layer composite multi-scale strengthening surface are obtained by electrodeposition, which is easy to prepare and has a good prospect for large-scale application.

附图说明Description of drawings

图1为多尺度强化沸腾表面孔壁SEM图(蜂窝状微纳双尺度多孔铜结构);Figure 1 is the SEM image of the multi-scale enhanced boiling surface pore wall (honeycomb micro-nano dual-scale porous copper structure);

图2为多尺度强化沸腾表面SEM图(从蜂窝状结构内部看到的底层的树林状阵列);Figure 2 is the SEM image of the multi-scale enhanced boiling surface (the underlying forest-like array seen from the inside of the honeycomb structure);

图3为池沸腾曲线。Figure 3 shows the pool boiling curve.

具体实施方式Detailed ways

针对传统蜂窝状微纳多尺度多孔材料在沸腾过程中膜沸腾后温度剧烈飙升的特性,本发明提出一种蜂窝状微纳双尺度多孔表面与树林状阵列表面相结合双层复合强化沸腾表面,利用蜂窝状结构提供更多的成核点结合树枝状阵列吸液能力强的特点,从而达到沸腾表面具有更高的沸腾强化效果。In view of the characteristics of the traditional honeycomb micro-nano multi-scale porous material in the boiling process, the temperature soars sharply after film boiling, the present invention proposes a double-layer composite enhanced boiling surface combining a honeycomb micro-nano dual-scale porous surface and a tree-like array surface, The use of the honeycomb structure to provide more nucleation points combined with the characteristics of the strong liquid absorption capacity of the dendritic array achieves a higher boiling enhancement effect on the boiling surface.

下面结合具体附图和较佳实例对本发明作进一步具体详细描述。The present invention will be described in further detail below in conjunction with specific drawings and preferred examples.

实施例1Example 1

(1)金属基体处理:首先使用稀硫酸溶液除去表面氧化物,让后用高浓度碱液清洗表面油污,接着使用去离子高纯水冲洗3次。(1) Metal substrate treatment: first use dilute sulfuric acid solution to remove surface oxides, then use high-concentration lye to clean the surface oil, and then use deionized high-purity water to rinse 3 times.

(2)金属基体预镀:为了增加所沉积的铜晶枝机械强度,在沉积铜晶枝前进行预镀。预镀溶液与铜晶枝的溶液相同。预镀电流密度为0.06 A cm-2,预镀时间为3 min。(2) Metal substrate pre-plating: In order to increase the mechanical strength of the deposited copper dendrites, pre-plating is performed before depositing copper dendrites. The preplating solution is the same as that of copper dendrites. The pre-plating current density was 0.06 A cm -2 , and the pre-plating time was 3 min.

(3)树林状阵列层沉积:采用逐渐增大电流的方法,以处理过的金属基体为阴极,在配比为0.6 M CuSO4、0.2 M H2SO4的溶液中,设置电沉积条件为电流增速为2 mA cm-2 s-1,起始电流密度为0.1 A cm-2,反应总电量为180 C,来进行电沉积。(3) Wood-like array layer deposition: using the method of gradually increasing the current, using the treated metal substrate as the cathode, in a solution with a ratio of 0.6 M CuSO 4 and 0.2 MH 2 SO 4 , set the electrodeposition condition as current Electrodeposition was carried out with a growth rate of 2 mA cm -2 s -1 , an initial current density of 0.1 A cm -2 , and a total reaction charge of 180 C.

(4)蜂窝状微纳双尺度多孔铜沉积:使用恒电流的方法,铜晶枝阵列表面为阴极,在硫酸硫酸铜为电解质的溶液中,硫酸浓度为1.0 M,硫酸铜浓度为0.4 M保持电流密度为1A cm-2,反应时间为60 s。(4) Honeycomb micro-nano dual-scale porous copper deposition: using the constant current method, the surface of the copper dendrite array is the cathode, in the solution of copper sulfate as the electrolyte, the concentration of sulfuric acid is 1.0 M, and the concentration of copper sulfate is 0.4 M to maintain the current The density is 1A cm -2 , and the reaction time is 60 s.

(5)产品热处理:在还原保护气氛条件下,进行烧结,烧结温度为710 ℃,保温30min,进一步增强产品机械强度。处理完成后,其电镜图如图1和图2所示。其中,图1为蜂窝状微纳双尺度多孔铜结构,图2为从蜂窝状结构内部看到的底层的树林状阵列。从图3可以看到,该产品(双层表面)的沸腾传热性能要明显优于单纯的蜂窝表面,以及单纯的树林状阵列表面。(5) Product heat treatment: Sintering is carried out under the condition of reducing protective atmosphere, the sintering temperature is 710 ℃, and the temperature is kept for 30 minutes to further enhance the mechanical strength of the product. After the processing is completed, its electron micrographs are shown in Figure 1 and Figure 2. Among them, Figure 1 is a honeycomb micro-nano dual-scale porous copper structure, and Figure 2 is a forest-like array at the bottom layer seen from inside the honeycomb structure. It can be seen from Figure 3 that the boiling heat transfer performance of this product (double-layer surface) is significantly better than that of a simple honeycomb surface and a simple tree-like array surface.

Claims (8)

1.一种双层多尺度强化沸腾的表面结构,其特征是:包括树林状阵列多孔层,然后在其表面沉积一层具有微纳双尺度的蜂窝状多孔铜结构;所述树林状阵列多孔层采用电沉积法制备,晶枝的平均间距为1μm ~2 mm,高度为1μm ~5mm;所述蜂窝状多孔铜结构具有微米尺度的大孔,孔壁由铜晶枝构成,晶枝的间隙是纳米级缝隙,纳米级缝隙尺寸为数纳米到数百纳米之间;大孔的平均直径在1~1000 μm。1. A double-layer multi-scale enhanced boiling surface structure is characterized in that: it includes a forest-like array porous layer, and then deposits a layer of honeycomb porous copper structure with micro-nano double-scale on its surface; the forest-like array is porous The layer is prepared by electrodeposition, the average spacing of crystal dendrites is 1 μm ~ 2 mm, and the height is 1 μm ~ 5 mm; the honeycomb porous copper structure has macropores on a micron scale, and the hole walls are composed of copper crystal dendrites, and the gap between crystal dendrites is nanoscale Slits, nanoscale slits range in size from a few nanometers to hundreds of nanometers; the average diameter of macropores is 1-1000 μm. 2.权利要求1所述双层多尺度强化沸腾的表面结构的制备方法,其特征在于包括如下步骤:2. the preparation method of the surface structure of double-layer multi-scale enhanced boiling described in claim 1, is characterized in that comprising the steps: (1)金属基体处理:首先使用稀硫酸溶液除去表面氧化物,然后用高浓度碱液清洗表面油污,接着使用去离子高纯水冲洗若干次;(1) Metal substrate treatment: first use dilute sulfuric acid solution to remove surface oxides, then use high-concentration lye to clean the surface oil, and then use deionized high-purity water to rinse several times; (2)金属基体预镀:在沉积铜晶枝前进行预镀;(2) Metal substrate pre-plating: pre-plating is performed before depositing copper dendrites; (3)树林状阵列制备:使用逐渐增大电流的方法,处理过的金属基体为阴极,在硫酸和硫酸铜为电解质的溶液中,保持电流增速一定,起始电流密度相同,反应总电量大于0 C,得到的样品清洗吹干后进行热处理;(3) Forest-like array preparation: using the method of gradually increasing the current, the treated metal substrate is used as the cathode, and in the solution of sulfuric acid and copper sulfate as the electrolyte, the current growth rate is kept constant, the initial current density is the same, and the total reaction power If the temperature is greater than 0 C, the obtained sample is cleaned and dried and then heat-treated; (4)蜂窝状微纳双尺度多孔铜沉积:使用恒电流的方法,铜晶枝阵列表面为阴极,在硫酸硫酸铜为电解质的溶液中,进行电沉积反应,反应总电量大于0 C;(4) Honeycomb micro-nano dual-scale porous copper deposition: using the constant current method, the surface of the copper crystal dendrite array is the cathode, and the electrodeposition reaction is carried out in the solution of copper sulfate as the electrolyte, and the total reaction electricity is greater than 0 C; (5)产品热处理:在还原保护气氛条件下,进行热处理。(5) Product heat treatment: heat treatment is carried out under the condition of reducing protective atmosphere. 3.如权利要求2所述的制备方法,其特征在于:步骤(3)中,电流起始密度为0.01~5.0 Acm-23 . The preparation method according to claim 2 , wherein in step (3), the initial current density is 0.01-5.0 Acm -2 . 4.如权利要求2所述的制备方法,其特征在于:步骤(3)中,电流起始密度增速为0.01 ~2000 mA cm-2 s-14. The preparation method according to claim 2, characterized in that: in step (3), the initial current density increases from 0.01 to 2000 mA cm -2 s -1 . 5.如权利要求2所述的制备方法,其特征在于:步骤(3)中,所述硫酸的摩尔浓度为0.01~10 M,硫酸铜的摩尔浓度为0.04 M~饱和。5. The preparation method according to claim 2, characterized in that: in step (3), the molar concentration of the sulfuric acid is 0.01-10 M, and the molar concentration of copper sulfate is 0.04 M-saturated. 6.如权利要求2所述的制备方法,其特征在于:步骤(4)中,所述恒电流的电流密度为0.05 ~ 10.0 A cm-26. The preparation method according to claim 2, characterized in that: in step (4), the current density of the constant current is 0.05-10.0 A cm -2 . 7.如权利要求2所述的制备方法,其特征在于:步骤(4)中,所述电沉积反应的时间为2~ 1800 s。7. The preparation method according to claim 2, characterized in that: in step (4), the electrodeposition reaction time is 2-1800 s. 8.如权利要求2所述的制备方法,其特征在于:步骤(5)中,所述热处理的温度为400~900 ℃还原气氛中烧结。8. The preparation method according to claim 2, characterized in that: in step (5), the temperature of the heat treatment is sintering in a reducing atmosphere at 400-900°C.
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CN110158127A (en) * 2019-05-15 2019-08-23 重庆大学 A kind of method for the critical heat flux density that enhanced heat transfer surfaces liquid film dryouies
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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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