表面纳米多孔结构制备及其强化沸腾传热性能研究
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摘要
沸腾传热技术被广泛应用于热能动力、核电、地热能、太阳能、石油化工、食品及低温工程等传统工业领域以及空间技术和微电子散热等高新技术领域。强化沸腾关键技术的突破可有效提高能源利用率和解决狭小空间内高热流密度的散热难题。纳米多孔铜表面具有高比表面积、优异的热导率、良好的浸润性以及极高的潜在汽泡核心密度，是极具前景的强化沸腾传热表面。本文提出一种基于热浸镀锌/脱合金的表面纳米多孔铜的简易制备方法，对该表面多孔结构与强化沸腾传热应用相关的关键物化特性进行了系统分析，并通过饱和池内沸腾实验研究了表面纳米多孔铜结构的强化沸腾传热性能和作用机理。主要研究内容如下：
1.热浸镀锌及镀层组分控制
采用热浸镀锌作为铜基体表面合金化的方法，以满足Cu/Zn脱合金体系对前驱体的组分要求为目标，利用热力学平衡相图和反应扩散理论作为指导对热浸镀锌工艺参数进行了优化。借助金相、SEM等表征手段对热浸镀形成的Cu-Zn化合物相层的组织形貌和生长规律进行了分析，发现在热浸镀锌铜块样品表面形成的镀层存在明显的相界面，表面热浸镀锌过程中各相层的生长受扩散控制。对镀层进行XRD分析发现γ相（Cu5Zn8）和β′相（CuZn）是镀层的主要组成，且γ相是镀层的主体。
2.表面纳米多孔铜结构的脱合金制备
以铜基热浸镀锌形成的表面Cu-Zn合金层作为研究对象，对该多相合金体系的脱合金过程进行了系统研究，讨论了外加电势、腐蚀时间、电解质溶液及浓度等脱合金条件对脱合金成形孔径结构和微裂纹的影响。Cu-Zn合金镀层在碱性脱合金溶液环境可获得孔径较均一的纳米多孔铜结构，而高于10wt.%的盐酸环境会破坏多孔铜结构。电化学腐蚀较化学腐蚀具有更高的脱合金速率，然而也会加剧裂纹的产生。对镀层进行了线性扫描伏安分析，通过扫描电势窗内氧化峰的分布情况可推断镀层的主要组分γ-CuZn和β'-CuZn都可参与选择性溶解的脱合金过程。
3. NPC水热环境稳定性及孔径尺度效应
以熔炼法制备的Cu0.4Mn0.6作为脱合金前驱体，分别通过电化学和自由腐蚀脱合金方法制备了孔径均一的纳米多孔铜材料（NPC）。通过沸水实验研究了纳米多孔铜材料在水热工作环境中的稳定性及孔径演化规律。采用SEM和EDS表征手段，对纳米多孔铜的孔径粗化规律和化学稳定性进行分析。研究表明，NPC在水热环境下的粗化过程由表面扩散机理控制，孔径结构的稳定性具有明显的尺度效应。另外，采用接触角测量仪和红外成像技术研究了孔径变化对多孔材料表面浸润性和毛细现象的影响。
4.纳米多孔表面强化沸腾传热性能研究
通过可视化饱和池内沸腾实验研究了热浸镀锌/脱合金工艺（HDGD）制备的纳米多孔铜表面(NPCS)与无强化结构表面(US)的沸腾传热性能差异，并通过表面物化性能表征结果和汽泡动力学现象分析了纳米多孔金属表面的强化沸腾传热机理。由于加热壁面浸润性的改善、汽化核心密度的提高和表面捕获载气量的增加等因素，纳米多孔铜表面展示了显著的沸腾强化作用。另外，纳米多孔表面与光滑表面在饱和池内核沸腾实验中的汽泡动力学特征有显著的差异，纳米多孔表面的汽泡脱离直径更小，脱离频率更高。文中将实验结果与相关文献报道的实验数据进行了对比分析，讨论了壁面热物理性质对核态沸腾传热性能的影响。
Boiling heat transfer technology is widely used in traditional industrial areas, likethermal power, nuclear engineering, solar energy, chemical, food engineering and cryogenicengineering, as well as space technology and microelectronics cooling. The development ofboiling enhancement technology can improve heat transfer efficiency and provide a solutionfor the heat dispersing problem in small space with high heat flux. The nanoporous coppersurface with high specific surface area, excellent thermal conductivity, good wettability aswell as a high density of potential bubble nucleate sites, is a promising heating wall forenhancing boiling heat transfer. In this thesis, a simple method which combined hot-dipgalvanized and dealloying was proposed for the fabrication of nanoporous copper surface.The key physical and chemical characteristics related to boiling heat transfer applications ofthe porous surface were analyzed. Finally, the enhancement of boiling heat transferperformance of the nanoporous copper surface was studied. The main contents of this thesisinclude:
1. Hot-dip galvanizing and component control of the coating
Hot-dip galvanizing was selected for the surface alloying on copper substrate. With theobjective of getting a Cu/Zn layer which meets the component requirement for dealloying, theoperation parameters of the hot-dipping process were optimized based on the thermodynamicequilibrium phase diagram and reaction-diffusion theory. The microstructure of the coatinglayer and the growth pattern of Cu-Zn intermetallic compounds were analyzed by means ofmetallography and SEM. Two obvious phase interfaces were found in the coating layer. Thegrowth rates of the phase layers are different, and are all controlled by diffusion. The XRDanalysis indicates γ-CuZn and β′-CuZn are the main components of the coating layer.
2. Fabrication of nanoporous copper surface by dealloying
The dealloying process of the multiphase Cu-Zn alloy layer formatted by hot-dipgalvanizing was systematically studied. The effects of electrolytes, the concentration ofelectrolyte solution, corrosion time and the anodic potential employed in dealloying on theformation of nanoporous structure and cracks were discussed. Homogeneous nanoporous copper structure can be obtained by free corrosion in an alkaline environment. It was foundthat nanoporous copper would be destroyed in a hydrochloric acid environment beyond10wt.%in concentration. A higher dealloying rate can be obtained by using electrochemical corrosioncompared to that of chemical corrosion, however, more cracks on the dealloyed surface.According to the linear sweep voltammetry analysis, the γ-CuZn and β'-CuZn phases whichmainly compose the coating layer can be selectively dissolved during the dealloying process.
3. Stability of NPC in hydrothermal environment and scale effect of porosity
Cu0.4Mn0.6was prepared by a process involved melting and solution treatment. NPCmaterials with uniform porosity were obtained by electrochemical and free dealloying,respectively. The stability and evolution of the nanoporous-copper structure in saturatedboiling water were experimentally investigated by means of SEM. Meanwhile, the changes inchemical composition of the nanoporous materials before and after boiled were analyzed byEDS. The NPC structure shows excellent chemical stability, however, keeps coarsening in thehydrothermal environment. The coarsening process shows high dependence on porosity scale,and is controlled by the surface diffusion mechanism. In addition, the contact anglemeasurement and infrared imaging technology were employed to reveal the changes insurface wettability and capillarity resulted from the scale effect of the porous structures.
4. Boiling heat transfer performance on the nanoporous copper surface
Saturated pool boiling experiments were conducted on a visualization platform. Thenucleate boiling heat transfer performance of nanoporous copper surface prepared by HDGDprocess was investigated compared to that of unstructured surface. The mechanism of theenhancement of boiling heat transfer was discussed based on the physical and chemicalproperties of the nanoporous surface and the observations of bubble dynamics phenomena.The improvement of wettability, higher nucleation sites density, and more entrapped gasvolume of the nanoporous surface contribute to the significant enhancement of boiling heattransfer. Furthermore, the bubble kinetic characteristics on the nanoporous copper surface andthe smooth surface show significant differences in the saturated pool-boiling tests. Bubbleswith smaller departure diameter and higher departure frequency were observed on nanoporous surface. The experimental data was compared with the reported results, and the effect ofthermal properties of the heating wall on the boiling heat transfer performance was discussed.
1.热浸镀锌及镀层组分控制
采用热浸镀锌作为铜基体表面合金化的方法，以满足Cu/Zn脱合金体系对前驱体的组分要求为目标，利用热力学平衡相图和反应扩散理论作为指导对热浸镀锌工艺参数进行了优化。借助金相、SEM等表征手段对热浸镀形成的Cu-Zn化合物相层的组织形貌和生长规律进行了分析，发现在热浸镀锌铜块样品表面形成的镀层存在明显的相界面，表面热浸镀锌过程中各相层的生长受扩散控制。对镀层进行XRD分析发现γ相（Cu5Zn8）和β′相（CuZn）是镀层的主要组成，且γ相是镀层的主体。
2.表面纳米多孔铜结构的脱合金制备
以铜基热浸镀锌形成的表面Cu-Zn合金层作为研究对象，对该多相合金体系的脱合金过程进行了系统研究，讨论了外加电势、腐蚀时间、电解质溶液及浓度等脱合金条件对脱合金成形孔径结构和微裂纹的影响。Cu-Zn合金镀层在碱性脱合金溶液环境可获得孔径较均一的纳米多孔铜结构，而高于10wt.%的盐酸环境会破坏多孔铜结构。电化学腐蚀较化学腐蚀具有更高的脱合金速率，然而也会加剧裂纹的产生。对镀层进行了线性扫描伏安分析，通过扫描电势窗内氧化峰的分布情况可推断镀层的主要组分γ-CuZn和β'-CuZn都可参与选择性溶解的脱合金过程。
3. NPC水热环境稳定性及孔径尺度效应
以熔炼法制备的Cu0.4Mn0.6作为脱合金前驱体，分别通过电化学和自由腐蚀脱合金方法制备了孔径均一的纳米多孔铜材料（NPC）。通过沸水实验研究了纳米多孔铜材料在水热工作环境中的稳定性及孔径演化规律。采用SEM和EDS表征手段，对纳米多孔铜的孔径粗化规律和化学稳定性进行分析。研究表明，NPC在水热环境下的粗化过程由表面扩散机理控制，孔径结构的稳定性具有明显的尺度效应。另外，采用接触角测量仪和红外成像技术研究了孔径变化对多孔材料表面浸润性和毛细现象的影响。
4.纳米多孔表面强化沸腾传热性能研究
通过可视化饱和池内沸腾实验研究了热浸镀锌/脱合金工艺（HDGD）制备的纳米多孔铜表面(NPCS)与无强化结构表面(US)的沸腾传热性能差异，并通过表面物化性能表征结果和汽泡动力学现象分析了纳米多孔金属表面的强化沸腾传热机理。由于加热壁面浸润性的改善、汽化核心密度的提高和表面捕获载气量的增加等因素，纳米多孔铜表面展示了显著的沸腾强化作用。另外，纳米多孔表面与光滑表面在饱和池内核沸腾实验中的汽泡动力学特征有显著的差异，纳米多孔表面的汽泡脱离直径更小，脱离频率更高。文中将实验结果与相关文献报道的实验数据进行了对比分析，讨论了壁面热物理性质对核态沸腾传热性能的影响。
Boiling heat transfer technology is widely used in traditional industrial areas, likethermal power, nuclear engineering, solar energy, chemical, food engineering and cryogenicengineering, as well as space technology and microelectronics cooling. The development ofboiling enhancement technology can improve heat transfer efficiency and provide a solutionfor the heat dispersing problem in small space with high heat flux. The nanoporous coppersurface with high specific surface area, excellent thermal conductivity, good wettability aswell as a high density of potential bubble nucleate sites, is a promising heating wall forenhancing boiling heat transfer. In this thesis, a simple method which combined hot-dipgalvanized and dealloying was proposed for the fabrication of nanoporous copper surface.The key physical and chemical characteristics related to boiling heat transfer applications ofthe porous surface were analyzed. Finally, the enhancement of boiling heat transferperformance of the nanoporous copper surface was studied. The main contents of this thesisinclude:
1. Hot-dip galvanizing and component control of the coating
Hot-dip galvanizing was selected for the surface alloying on copper substrate. With theobjective of getting a Cu/Zn layer which meets the component requirement for dealloying, theoperation parameters of the hot-dipping process were optimized based on the thermodynamicequilibrium phase diagram and reaction-diffusion theory. The microstructure of the coatinglayer and the growth pattern of Cu-Zn intermetallic compounds were analyzed by means ofmetallography and SEM. Two obvious phase interfaces were found in the coating layer. Thegrowth rates of the phase layers are different, and are all controlled by diffusion. The XRDanalysis indicates γ-CuZn and β′-CuZn are the main components of the coating layer.
2. Fabrication of nanoporous copper surface by dealloying
The dealloying process of the multiphase Cu-Zn alloy layer formatted by hot-dipgalvanizing was systematically studied. The effects of electrolytes, the concentration ofelectrolyte solution, corrosion time and the anodic potential employed in dealloying on theformation of nanoporous structure and cracks were discussed. Homogeneous nanoporous copper structure can be obtained by free corrosion in an alkaline environment. It was foundthat nanoporous copper would be destroyed in a hydrochloric acid environment beyond10wt.%in concentration. A higher dealloying rate can be obtained by using electrochemical corrosioncompared to that of chemical corrosion, however, more cracks on the dealloyed surface.According to the linear sweep voltammetry analysis, the γ-CuZn and β'-CuZn phases whichmainly compose the coating layer can be selectively dissolved during the dealloying process.
3. Stability of NPC in hydrothermal environment and scale effect of porosity
Cu0.4Mn0.6was prepared by a process involved melting and solution treatment. NPCmaterials with uniform porosity were obtained by electrochemical and free dealloying,respectively. The stability and evolution of the nanoporous-copper structure in saturatedboiling water were experimentally investigated by means of SEM. Meanwhile, the changes inchemical composition of the nanoporous materials before and after boiled were analyzed byEDS. The NPC structure shows excellent chemical stability, however, keeps coarsening in thehydrothermal environment. The coarsening process shows high dependence on porosity scale,and is controlled by the surface diffusion mechanism. In addition, the contact anglemeasurement and infrared imaging technology were employed to reveal the changes insurface wettability and capillarity resulted from the scale effect of the porous structures.
4. Boiling heat transfer performance on the nanoporous copper surface
Saturated pool boiling experiments were conducted on a visualization platform. Thenucleate boiling heat transfer performance of nanoporous copper surface prepared by HDGDprocess was investigated compared to that of unstructured surface. The mechanism of theenhancement of boiling heat transfer was discussed based on the physical and chemicalproperties of the nanoporous surface and the observations of bubble dynamics phenomena.The improvement of wettability, higher nucleation sites density, and more entrapped gasvolume of the nanoporous surface contribute to the significant enhancement of boiling heattransfer. Furthermore, the bubble kinetic characteristics on the nanoporous copper surface andthe smooth surface show significant differences in the saturated pool-boiling tests. Bubbleswith smaller departure diameter and higher departure frequency were observed on nanoporous surface. The experimental data was compared with the reported results, and the effect ofthermal properties of the heating wall on the boiling heat transfer performance was discussed.
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