网络首发时间: 2019-11-13 16:58

稀有金属 2021,45(03),306-311 DOI:10.13373/j.cnki.cjrm.xy19080026

镓基液体金属在不同介质表面的润湿性研究

郎玉婧 郝洁 杜秀征 毛华 李金宝

中国兵器科学研究院宁波分院

宁波中星新材料研究院有限公司

摘 要：

以Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5(质量分数)五元镓基液体金属为基础,用综合热分析仪、导热系数测试仪以及高温电镜研究了其基本物理性能和在常用散热组元材料表面上的润湿行为,研究结果表明该镓基液体金属的熔点为3.1℃,20℃时的密度为6.67 g·cm^-3、导热系数为21.5W·m^-1·℃^-1、比热容为504 J·kg^-1·℃^-1、导电率为3.46×10⁶S·m^-1,相对于纯镓和镓铟锡合金其热导特性明显提高。在3.1～100℃的温度范围内,该镓基液体金属在聚氯乙烯塑料(PVC)、硅、铜合金、铝合金等基体表面的润湿性是依次提高的,即PVC<硅<铜合金<铝合金,随着温度升高接触角随之降低,分别从3.1℃的147°,133°,135°,131°降低到100℃时的107°,62°,45°,37°,分别减小了40°,61°,90°,94°。在所研究的温区内,不同温度下得到的接触角数据能够很好地展现接触角随温度的变化情况,同时也展示了液态镓独特的润湿特性。结果表明该五元镓基液体金属可以与常规散热器件组元材料匹配良好,可实现大功率、高热量器件的快速散热。

关键词：

镓合金;液体金属;润湿性;接触角;

中图分类号： TG146.43

作者简介：郎玉婧(1983-),女,辽宁营口人,博士,副研究员,研究方向:铝合金、非晶合金,电话:0574-87902404,E-mail:yj.lang@163.com;

收稿日期：2019-08-20

基金：宁波市自然科学基金项目(2016A610242)资助;

Wettability of Gallium-Based Liquid Metals on Different Media Surfaces

Lang Yujing Hao Jie Du Xiuzheng Mao Hua Li Jinbao

Ningbo Branch of China Academy of Ordnance Science

Ningbo Zhong Xing New Materials Research Institute Co.,Ltd.

Abstract：

In recent years,with the rapid development of science and technology,there were more and more serious heat dissipation problems of high-power and high-heat-flow devices in many industries. The first and foremost was the field of electronics,information and optoelectronic technology. At present,the liquid metal thermal conductive materials were considered as one of the best high performance heat dissipation materials in the future because of their high heat conduction rate,large heat absorption capacity,high heat transfer capacity and stable and controllable physical chemistry properties. In recent years,many researchers had studied low-meltingpoint gallium-based liquid metal from the research of material preparation,performance and application,and obtained many valuable research results. But the wettability of liquid metal on the surface of different media was not involved,and the wettability of liquid metal would determine the structure,the heat dissipation efficiency and the overall efficiency of the radiator. Therefore,the wetting behavior of five-element gallium-based liquid metal(such as copper alloy,aluminum alloy,silicon,polyvinyl chloride(PVC),etc.)on the surface of common heat dissipation materials was involved. The wettability of gallium-based liquid metal on different surfaces was analyzed,and the flow and heat transfer characteristics of gallium-based liquid metal in these channels were evaluated here. On the basis of GaInSn ternary alloy,zinc and bismuth were introduced to further reduce the melting point of the alloy to obtain the system of GaInSnBiZn five-element alloy with specific compositions such as Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5(mass fraction). The raw materials were indium 99.96%,gallium 99.999%,tin 99.996% and bismuth 99.95%,zinc 99.99%. Gallium was first heated by an alcohol lamp in a nickel crucible in argon atmosphere to melt it at temperature of 200～250 ℃,then indium,tin,bismuth and zinc were added in turn and stirred with a glass rod until the alloy was completely dissolved,the gallium-based liquid metal was obtained by soaking at 200-250 ℃for 10 min. The specific heat capacity(C_p)and melting point(T_m)of liquid gallium were measured with a comprehensive thermal analyzer(STA449C,Nietzsche,Germany). The specific heat capacity(dH/dT)and differential scanning calorimetry(DSC)curves of gallium-based liquid metal(10-20 mg)were obtained in an open argon atmosphere from-10 to 200 ℃ at 10 ℃·min^-1,to get C_p,T_m,respectively. The conductivity of liquid gallium was measured by conductivity Tester(EC-4110,Kuosi,Shanghai). The thermal conductivity of liquid gallium was measured by the DRL-ii(Xiangtan Instrument,Hunan). The physical morphology of gallium-based liquid metal with 5 mm square on different carriers was observed by high temperature electron microscope(RDS-04,Northeastern University,China)from-30 to 100 ℃,the temperature dependence of the wetting angle between liquid metal and carrier surface was observed. Based on Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5 five-element gallium liquid metal,the wetting behavior on the surface of common heat dissipation materials was studied,the wettability of liquid gallium metal on different surfaces was analyzed. The results were as follows:the melting point of Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5 five-element liquid gallium metal was 3.1 ℃,the density was 6.67 g·cm^-3,the thermal conductivity was 21.5 W·m^-1·℃^-1,the specific heat capacity was 504 J·kg^（-1）·K^（-1）,the conductivity was 3.46×10⁶ S·m^-1,and the thermal conductivity was significantly higher than that of pure gallium and indium tin alloys. The contact angle of Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5 liquid gallium on the substrates of PVC,silicon,copper alloy and aluminum alloy decreased with the increase of temperature from 147°,133°,135°and 131° at 3.1 ℃ to 107°,62°,45° and 37° at 100 ℃ with the reduction of 40°,61°,90° and 94°,respectively. Compared with pure gallium and gallium indium tin alloy,the thermal conductivity of the gallium alloy was obviously improved. In the temperature range of 3.1～100 ℃,the wettability of the gallium base liquid metal on the matrix surface of polyvinyl chloride(PVC),silicon,copper alloy,aluminum alloy,was increased in turn with the order of PVC<silicon alloy<copper alloy<aluminum alloy,and with the rising of temperature. In the temperature range of this study,the contact angle data obtained at different temperatures could show the change of contact angle with temperature well and also showed the unique wetting characteristics of liquid gallium. From the analysis results,it could be seen that the gallium base liquid metal could match the conventional heat dissipation device component material well,and could dissipate the heats quickly for the high probability and high energy devices.

Keyword：

gallium alloy; liquid metal; wettability; contact angle;

Received： 2019-08-20

近年来，随着科技飞速发展，各行各业都存在日趋严峻的大功率、高热流设备器件的散热问题 ^{[1,2,3,4,5,6]} 。首当其冲是电子、信息、光电技术领域，计算机、光电芯片一直是朝着提高集成度、减小尺寸的趋势发展，散热问题越发严峻，按照实际发展速度推算，计算处理芯片上的晶体管数量每十年翻一倍，由晶体管发热带来的过高温度将降低芯片的工作稳定性，增加出错率，同时模块内部与其外部环境间所形成的热应力会直接影响到芯片的电性能、工作频率、机械强度及可靠性，据统计由晶体管发热导致电子计算机通讯行业领域的直接经济损失达到几十亿。其次在国防军事领域，武器装备朝着高威力、大范围、信息化的趋势发展，所消耗的功率越来越高，致使关键部件散热问题越来越严重，导致武器装备性能的快速降低，造成人力、物力、财力的极大浪费，同时使作战效能降低并危及国家安全。事实上，不仅对于电子计算机通讯领域、国防军事领域，对于其他领域中大量功率器件、高发热仪器设备也存在着类似的广泛而迫切的散热冷却需要，有的情况下甚至要求更高。这些态势都表明，目前对高性能散热介质材料的需求已提到了前所未有的层面。

目前液体金属热导介质材料因其具有高的导热速率、大的吸纳热量能力、高的热传输能力以及稳定可控的物理化学性能被认为是未来最佳的高性能散热介质材料之一。近年来国内外众多学者分别从材料制备研究 ^[7,8,9] 、性能研究 ^{[10,11,12,13]} 、应用研究 ^[14,15,16] 入手对低熔点镓基液体金属进行了研究，得到了很多有价值的研究结果 ^{[17,18,19,20,21]} 。但是对液体金属在不同介质表面的润湿行为没有涉及，而液体金属的润湿性能将会决定散热器件的结构、散热器件的散热效率以及其综合效能。

因此，本文以五元镓基液体金属为基础，研究其在常用散热材料（如铜合金、铝合金、硅、聚氯乙烯塑料（PVC）等）表面上的润湿行为，分析镓基液体金属在不同材质表面的润湿性，并评估分析镓基液体金属在这些材料流道内的流动特性和热交换特性。

1实验

本实验镓基液体金属的名义成分为Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5（质量分数）所用原料分别为：纯度为99.96%的铟，纯度为99.999%的高纯镓，纯度为99.996%的锡，纯度为99.95%的高纯铋，纯度为99.99%的高纯锌。按配比首先将镓放入到镍坩埚中，在氩气保护气氛下，用酒精灯加热使镓融化，并使温度维持在200～250℃，随后依次加入铟、锡，铋、锌，用玻璃棒搅拌直至合金成分完全相溶，并混合均匀，在200～250℃保温10 min即得镓基液态金属。

用综合热分析仪（STA449C，德国耐驰仪器制造有限公司，德国）分析测量镓基液体金属的比热容（C_p）、熔点（T_m）。在敞开的氩气气氛下，把10～20 mg的镓基液体金属放入热分析仪中，以10℃·min^-1，从-10℃升到200℃，得到其比热容（d H/d T）、差示扫描量热仪记录到的曲线（DSC曲线），分别得到C_p,T_m。再用电导率测试仪（EC-4110，上海阔思电子有限公司，上海）测量镓基液体金属的电导率。再用导热系数测试仪（DRL-Ⅱ，湘潭湘仪仪器有限公司，湖南）测量镓基液体金属的导热系数。再用高温电镜（RDS-04,Northeastern University,China）观察5 mm见方的镓基液体金属在不同载体上从-30℃升到100℃的物理形态变化规律，研究其在不同载体上不同温度下的物理状态，观察镓基液体金属与载体表面的润湿角随温度的变化情况。所有载体表面都经过2000号砂纸打磨、超声清洗、烘干等过程，确保试验结果的可对比性。

2结果与讨论

2.1镓基液体金属的物理性能

制备出的Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5的主要物理性质如表1所示。本镓基合金的熔点为3.1℃，20℃时的密度为6.67 g·cm^-3、导热系数为21.5 W·m^-1·℃^-1、比热容为504 J·kg^-1·K^-1、导电率为3.46×10⁶S·m^-1。较纯镓和镓铟锡合金而言 ^[11] ，其熔点接近镓铟锡合金，而密度较前两者有明显增加，导热系数介于镓和镓铟锡合金之间，其比热容在这三者中是最大的，这些热特性表明该镓基合金具有大吸纳热量能力、高热传输能力的理想功能，是理想的高性能散热介质材料之一。

2.2不同温度下镓基液体金属的物理形态

在不同载体上，随温度变化镓基液体金属与载体之间的相互作用也会随之变化。图1～4是Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5液态金属在PVC、硅、铜合金、铝合金等基板上随温度升高其物理形态的变化情况。

表1 20℃下Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5的基本物理性能  下载原图

Table 1 Basic physical properties of Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5at 20℃

图1是Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5液态金属在PVC基板上其形态随温度升高的变化情况。该镓基液态金属在-10℃呈固体立方状态，在3.1℃时溶解成球体液体颗粒，熔点与表1中的数据一致，此时该镓基液态金属液滴与PVC基板呈钝角粘接。当温度升高到50℃，镓基液态金属与PVC基板的接触角逐渐降低，但依然是钝角状态，说明镓基液态金属与PVC基板接触属于非润湿型接触，这样有利于镓基液体金属在PVC管内流动，减小驱动阻力。随着温度进一步升高到100℃，该镓基液态金属与PVC基板接触角进一步减小，但仍然处于非润湿型接触状态，表明该镓基液体金属与PVC基板可以在大多数散热环境中实现散热通道的流畅，从而保证热量传输快速运输以及散热系统的高效循环。进一步说明PVC等有机塑料管道可以用作冷热源间的回路管道。

图1 不同温度下镓基液体金属在PVC塑料表面的润湿性

Fig.1 Moisture of gallium-based liquid metals on PVC plastic surfaces at different temperatures

图2是该镓基液态金属在硅基板上其形态随温度升高的变化情况。该镓基液态金属熔点以下是固体立方状，在3.1℃时溶解成球体液体颗粒，该镓基液态金属液滴与硅基板也呈钝角粘接，但接触角较图1相应温度有所减小，说明该镓基液态金属液滴在硅基板上的润湿性有所提高。当温度升高到50℃，镓基液态金属与硅基板的接触角逐渐降低，接近90°接触，说明镓基液态金属与硅基板开始由非润湿型向润湿型转变，表明该镓基液体金属与硅基板可以实现高效接触，有利于两者间的热传导效率，即实现液体金属对半导体材料的散热。随着温度进一步升高到高100℃，该镓基液态金属与硅基板接触角进一步减小，转变成润湿型接触特征，热子传导通道会进一步增加，镓基液态金属可快速从硅基板中带走热量，实现散热。

图3是该镓基液态金属在铜合金基板上其形态随温度升高的变化情况。该镓基液态金属熔点以下是固体立方状，在3.1℃时溶解成球体液滴，该镓基液态金属液滴与铜合金也呈钝角粘接，但接触角较图1和图2相应温度有进一步减小，说明该镓基液态金属液滴在铜合金上的润湿性较前面两种基板材料更好。随温度升高其接触角减小趋势更加明显，其非润湿型向润湿型转变的温度出现在50℃以下。在50℃时已经呈锐角接触状态，说明镓基液态金属与铜合金的润湿类型可能是反应润湿 ^[11] ，表明该镓基液体金属与铜合金可以实现高效热传输。随着温度进一步升高到100℃，该镓基液态金属与硅基板接触角进一步减小，该镓基液体金属在铜合金表面可呈铺展润湿状态，热子传导通道会进一步增加。而铜合金常常作为散热器的热交换器材料与液体金属一起将器件的热量快速导出，实现大功率器件的快速降温。

图2 不同温度下镓基液体金属在硅表面的润湿性

Fig.2 Moisture of gallium-based liquid metals on silicon sur-faces at different temperatures

图3 不同温度下镓基液体金属在铜合金表面的润湿性

Fig.3 Moisture of gallium-based liquid metals on copper alloy surface at different temperatures

图4是该镓基液态金属在铝合金基板上其形态随温度升高的变化情况。其在铝合金基板上的状态与其在铜合金基板上的状态类似，非润湿型向润湿型转变的温度也在50℃以下。但镓基液态金属在铝合金板上的润湿性较铜合金有一定的提升。在相同的温度下，其接触角都小于在铜合金表面上的接触角，说明该镓基液态金属液滴在铝合金上的润湿性较前面3种基板材料更佳。该镓基液态金属与铝合金的润湿类型也可能是反应润湿 ^[11] ，表明该镓基液体金属与铝合金可以实现高效热传输。铝合金也是常用热交换器材料，同时也是电子元器件的封装材料，可与镓基液体金属一起实现功率器件一体化散热。

图4 不同温度下镓基液体金属在铝合金表面的润湿性

Fig.4 Moisture of gallium-based liquid metals on aluminum alloy surface at different temperatures

2.3镓基液体金属在不同载体上的润湿性

为了进一步直观分析不同温度下镓基液体金属在以上基板上的润湿行为，对3.1,30,50,70和100℃下的润湿角进行了测量，结果列于表2中。对于Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5液体金属而言，其熔点温度下，其在PVC、硅、铜合金、铝合金等基板上的接触角分别为147°，133°，135°，131°。随着温度升高接触角都随之降低，到100℃时分别减小了40°，61°，90°，94°。且在各个温度下该镓基液体金属的润湿性依次是PVC<硅<铜合金<铝合金，与前面2.2部分的结果一致。

表2 镓基液体金属在不同材料体表面的接触角  下载原图

Table 2 Contact angles of gallium-based liquid metals on surfaces of different materials（°）

以上结果表明，3.1～100℃的温度范围内，Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5液体金属在PVC、硅、铜合金、铝合金等基体表面的润湿性是依次提高的，即该镓基液体金属在金属基板上的润湿性，也优于在陶瓷半导体基板上的润湿性以及在塑料基板上的润湿性。从以上结果还可以看出，在所研究的温区内，不同温度下得到的接触角数据能够很好地展现接触角随温度的变化情况，同时也展示了液态镓独特的润湿特性。可以根据结果选用相应材料作为散热器相应部件的组成材料，即塑料材料做循环通道材料，铜合金和铝合金可以作为热交换器材料，镓基液体金属作为导热介质材料。

3结论

以Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5五元镓基液体金属为基础，研究了其在常用散热材料表面上的润湿行为，分析了镓基液体金属在不同材质表面的润湿性得到结论如下：

1.Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5五元镓基液体金属的熔点为3.1℃，20℃时的密度为6.67 g·cm^-3、导热系数为21.5 W·m^-1·℃^-1、比热容为504 J·kg^-1·K^-1、导电率为3.46×10⁶S·m^-1，相对于纯镓和镓铟锡合金其热导特性明显提高。

2.Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5五元镓基液体金属在PVC、硅、铜合金、铝合金等基板上的接触角随着温度升高接触角随之降低，分别从3.1℃的147°，133°，135°，131°降低到100℃时的107°，62°，45°，37°，分别减小了40°，61°，90°，94°。

3.在3.1～100℃的温度范围内，Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5五元镓基液体金属在PVC、硅、铜合金、铝合金等基体表面的润湿性是依次提高的，即PVC<硅<铜合金<铝合金。

4.从分析结果可以看出，该Ga₆₆In₂₀Sn₁₀Bi_3.5Zn_0.5五元镓基液体金属可以与常规散热器件组元材料匹配良好，实现大概率、高热量功能器件的快速散热。

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