CN104651818A - Method for preparing super-hydrophobic surface with ultrahigh adhesion - Google Patents

Method for preparing super-hydrophobic surface with ultrahigh adhesion Download PDF

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CN104651818A
CN104651818A CN201510101568.7A CN201510101568A CN104651818A CN 104651818 A CN104651818 A CN 104651818A CN 201510101568 A CN201510101568 A CN 201510101568A CN 104651818 A CN104651818 A CN 104651818A
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surface
adhesion
cobalt
superhydrophobic
super
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CN201510101568.7A
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李健
景治娇
阎龙
王庆涛
雷自强
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西北师范大学
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/54Contact plating, i.e. electroless electrochemical plating
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/02Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using non-aqueous solutions
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D

Abstract

The invention provides a method for preparing a super-hydrophobic surface with ultrahigh adhesion. With cobalt sulfate heptahydrate as a reaction substrate, a zinc plate as a base and water as a solvent, the method comprises the following steps: firstly depositing cobalt on the surface of the zinc plate according to a chemical precipitation method, then immersing the zinc plate with cobalt deposited on the surface in an absolute ethanol solution of stearic acid to graft the stearic acid to the cobalt surface to obtain the super-hydrophobic surface. Contact angle measurement finds that the super-hydrophobic surface prepared according to the method disclosed by the invention has the contact angle of bigger than 150 degrees and the roll angle of 90 degrees to deionized water, and keeps good adhesion property as water drops can be firmly adhered to the surface of the zinc plate even if the zinc plate is inverted; and as a result, as a super-hydrophobic material, the super-hydrophobic surface prepared according to the method disclosed by the invention used has higher adhesion property, plays an important role in lossless delivery of a trace amount of liquid, and has great commercial prospect in the technical field of special infiltration interfaces.

Description

超高黏附性超疏水表面的制备方法 The method of preparing ultrahigh superhydrophobic surface adhesion

技术领域 FIELD

[0001] 本发明属于特殊浸润性界面技术领域,涉及一种超高黏附性超疏水表面的制备方法。 [0001] The present invention belongs to the technical field of special interface wettability, a method for preparing ultra high adhesion of superhydrophobic surfaces.

技术背景 technical background

[0002] 超疏水表面是指与水滴的接触角大于150°的表面,比如大自然中一些玫瑰花、荷叶、蝴蝶、壁虎、苍蝇、蝗虫、蜜蜂等等。 [0002] superhydrophobic surface refers to a surface contact angle with water droplet is larger than 150 °, such as the nature, the roses, leaves, butterflies, gecko, flies, grasshoppers, bees and the like. 在这许许多多的超疏水表面中,尤其以荷叶最为特殊,显示了不同寻常的超疏水性能和自清洁性能,这种现象称之为“荷叶效应”,是由于荷叶表面低表面能的蜡状物质和微纳米的粗糙结构共同作用的结果。 In many of these super-hydrophobic surface, particularly in the most special lotus leaf, showing the extraordinary performance of superhydrophobic and self-cleaning properties, a phenomenon known as the "lotus effect" is due to the lower surface of the lotus leaf surface the results of the interaction energy of waxy material and micro roughness nm. 不同与低黏附的超疏水荷叶表面,高黏附性超疏水表面具有较高的黏附力和摩擦力。 Different Lotus superhydrophobic surface with low adhesion, high adhesion superhydrophobic surface having a high adhesion and friction forces. 由于表面黏附力的存在,在水滴与高黏附性超疏水表面的接触角大于150°的情况下,将表面倾斜90°或者180°,水滴仍能黏附在表面而不脱落。 Due to the presence of the adhesion surfaces, the contact angle of water droplet in the case of high adhesion superhydrophobic surface is greater than 150 °, the inclined surface 90 ° or 180 °, still adhered to the surface without drops off. 这些表面具有很强的黏附性,因而称之为高黏附超疏水表面。 These surfaces have a strong adhesion, so called super high adhesion of hydrophobic surfaces. 高黏附性超疏水表面虽然不具有自清洁功能,单从微米尺度上操纵液滴方面具有奇妙的应用,可以在微流体系统,液体无损转移和生物技术等方面发挥重大的作用。 Although the high adhesion superhydrophobic surface having no self-cleaning function, a single droplet from the aspect of manipulation has wonderful micron scale applications, can play a major role in the microfluidic system, the lossless transfer liquid and biotechnology.

[0003]目前对于高黏附超疏水表面的制备,主要是通过调节表面的微观结构,增大固液接触面积,提高水滴在表面的黏附力。 [0003] At present, for preparing a superhydrophobic surface of high adhesion, mainly by regulating the surface microstructure of the solid-liquid contact area is increased to improve the adhesion of water droplets on the surface. 或者是通过调节表面亲疏化学成分的比例,在表面引入一定比例的亲水点,增大水滴在表面的黏附力。 Or by adjusting the ratio of the surface chemical composition of closeness, a certain proportion of the hydrophilic surface of the introduction point, increasing the adhesion of water droplets on the surface. 近年来,科学家们通过很多方法制备出了高黏附性超疏水表面,但其制备过程复杂,制备周期较长而不易大规模生产,并且主要集中在极端高黏附超疏水表面的制备,对可控高黏附性超疏水表面的制备研宄极少。 In recent years, scientists have made by many ways a high adhesion superhydrophobic surfaces, but the preparation process is complex, long and difficult period of preparation for mass production and are mainly concentrated preparation of extremely high adhesion of superhydrophobic surfaces in, controllable preparation of a Subsidiary high adhesion superhydrophobic surface is minimal. 因此,在表面化学成分不变的前提下,通过简单的化学方法实现对高黏附超疏水表面形貌的控制,从而实现对高黏附超疏水表面的黏附性的有效调控,可以拓宽超疏水表面在实际生产生活中的应用,具有很好的商业化前景。 Thus, the lower surface without changing the chemical composition, is achieved by simple chemical method for the control of high adhesion superhydrophobic surface morphology, thereby achieving efficient regulation of adhesion high adhesion superhydrophobic surface, the surface can be widened superhydrophobic application of real-life production, has good commercial prospects.

发明内容 SUMMARY

[0004] 本发明的目的是提供一种超高黏附性超疏水表面的制备方法。 [0004] The object of the present invention is to provide an ultra high adhesion superhydrophobic surface preparation.

[0005] —、超尚黏附性超疏水表面的制备 [0005] - Preparation of ultra still superhydrophobic surface adhesion

本发明超尚黏附性超疏水表面的制备,是以七水合硫酸钻为反应底物,梓片为基底,水为溶剂,先通过化学沉积法使钴沉积在锌片表面;再将沉积钴的锌片浸泡到硬脂酸的无水乙醇溶液中,使得低表面能的硬脂酸接枝到钴表面,得到超疏水表面。 Preparation superhydrophobic surface adhesion still present invention over, is cobalt sulfate heptahydrate as the reaction substrate, the substrate sheet is a Zi, water as a solvent, the first cobalt is deposited on the surface of a zinc sheet by a chemical deposition method; then deposited cobalt zinc sheet to soak in the acid solution in absolute ethanol, such that the low surface energy of the stearic acid grafted to the surface of the cobalt to give a superhydrophobic surface. 其具体制备工艺为:先将锌片依次用丙酮、无水乙醇、去离子水超声清洗,于硫酸钴水溶液中浸泡20~30 min,使钴沉积在锌片表面;取出并用去离子水和无水乙醇清洗、晾干;再于硬脂酸的无水乙醇溶液中浸泡30~40 min,然后用去离子水和无水乙醇清洗、晾干,即得超高黏附性能的超疏水表面。 Specific preparation process: first zinc sheets successively with acetone, ethanol, deionized water, ultrasonic cleaning, immersion 20 ~ 30 min to the aqueous solution of cobalt sulfate, cobalt zinc sheet deposited on the surface; deionized water and removed without water, ethanol, dried; stearic acid in ethanol and then immersed in a solution of 30 ~ 40 min, and then with deionized water and absolute ethanol is washed and dried, to obtain the adhesion of the ultra super hydrophobic surface.

[0006] 所述硫酸钴水溶液的浓度为0.005-0.05 mo I/L ;硫酸钴水溶液与锌片的体积面积比为5:1~10:1 mL/cm2。 [0006] The concentration of the aqueous solution of cobalt sulfate is 0.005-0.05 mo I / L; aqueous cobalt sulfate solution volume ratio of the area of ​​the zinc sheet was 5: 1 ~ 10: 1 mL / cm2.

[0007] 所述硬脂酸的无水乙醇溶液中,硬脂酸的浓度为0.002-0.005 mo I/L ;硬脂酸的无水乙醇溶液与锌片的体积面积比为5:1-10:1 mL/cm2。 [0007] The stearic acid solution in absolute ethanol, the concentration of stearic acid 0.002-0.005 mo I / L; the area ratio of the volume of absolute ethanol stearate and zinc sheet was 5: 1-10 : 1 mL / cm2.

[0008] 一、超尚黏附性超疏水表面的结构表征1、X射线衍射(XRD)分析 [0008] First, the adhesion is still super super hydrophobic surface structure characterization 1, X-ray diffraction (XRD) analysis

图1为本发明所制备的超高黏附性超疏水表面的XRD谱图。 XRD spectrum of ultra adhesion superhydrophobic surface in FIG. 1 prepared in the present invention. 从XRD的谱图可以看出,2 Θ =20.9。 As can be seen from the XRD spectrum, 2 Θ = 20.9. ,32.5° ,33.7° ,37.0° 和58.4。 , 32.5 °, 33.7 °, 37.0 °, and 58.4. 分别对应钴的(110)、(210)、(004)、(212)和(410)晶面衍射峰(JCPDS N0.65-9722) ο 而2Θ =36.0°、38.6°、42.9 °、54.0°和69.7。 Corresponding cobalt (110), (210), (004), (212) and (410) plane diffraction peak (JCPDS N0.65-9722) ο and 2Θ = 36.0 °, 38.6 °, 42.9 °, 54.0 ° and 69.7. 分别归属于锌基底的(002)、(100)、(101)、(102)和(103)晶面衍射峰(JCPDSN0.04-0831)。 They are attributed to a zinc base (002), (100), (101), (102) and (103) plane diffraction peak (JCPDSN0.04-0831). 因此,在锌基底上成功的制备出了钴表面。 Thus, the substrate on the zinc cobalt successfully prepared surface.

[0009] 2、能谱(EDX)分析 [0009] 2, spectroscopy (EDX) analysis

图2为本发明制备的超高黏附性超疏水表面的EDX谱图。 EDX spectra ultrahigh adhesion superhydrophobic surfaces 2 of the present invention was prepared. 从能谱图中可以看出,在锌基底上制备的超疏水表面上主要含有碳、氧、钴和锌元素。 As it can be seen in the energy spectrum, mainly containing carbon, oxygen, cobalt and zinc on superhydrophobic surfaces produced on a zinc substrate. 谱图中所检测到的金元素,是因为样品做能谱分析时,经辉光放射喷金处理后留在了超疏水表面上。 Spectra detected alloying elements, is made as the sample energy spectrum, the radiation after glow discharge treatment gold is left on the super-hydrophobic surface. 结合XRD分析,可以推断出锌片将硫酸钴溶液中的钴成功地置换并沉积在其表面上。 Based on XRD analysis, the sheet can be inferred that the zinc sulphate solution Cobalt successfully replaced and deposited on the surface thereof.

[0010] 3、扫描电镜(SEM)分析 [0010] 3, scanning electron microscopy (SEM) analysis

图3为本发明中不同浓度硫酸钴所制备的超疏水表面的SEM图。 FIG 3 is a SEM image of a super-hydrophobic surface of the present invention in various concentrations of cobalt sulfate prepared. (a、b)0.005 mo I Γ1硫酸钴水溶液所制备的超疏水表面的SEM图,(c、d)0.01 mo IL—1硫酸钴水溶液所制备的超疏水表面的SEM图,(e、f) 0.05 mo IL—1硫酸钴水溶液所制备的超疏水表面的SEM图。 (A, b) SEM FIGS 0.005 mo superhydrophobic surfaces produced I Γ1 cobalt sulfate aqueous solution, (c, d) 0.01 mo IL-1 SEM FIG superhydrophobic surfaces produced cobalt sulfate aqueous solution, (e, f) 0.05 mo IL-1 SEM FIG superhydrophobic surfaces produced cobalt sulfate aqueous solution. 其中,(a、c、e)是低倍数的SEM图,(b、d、f)是高倍数的SEM图。 Wherein, (a, c, e) is the SEM image of low multiples, (b, d, f) is the SEM image of high expansion. 比较不同浓度的SEM图,可以看出沉积的钴表面是由许多的“鳞片”组成的,片与片之间有较多的不规则孔洞。 SEM images of different concentrations, it can be seen from the cobalt is deposited on the surface of many of the "scale" of the composition, there are more irregular pores between the sheet and the sheet. 通过肉眼可以看出,随着硫酸钴浓度的增加,这些“鳞片”的密度也在逐渐的增大,从而使得孔洞越来越多。 As can be seen by the naked eye, as the sulfuric acid concentration of cobalt increases, these "scales" density is gradually increased, so that more and more holes. 从高倍数的SEM图中可以看出,钴表面中的“鳞片”厚度在10~50 nm之间。 SEM can be seen from FIG high-expansion, the cobalt surface "scale" thickness between 10 ~ 50 nm.

[0011] 二、超尚黏附性超疏水材料的润湿性能测试1、接触角和黏附性分析 [0011] Second, the adhesion is still super super hydrophobic material 1 test wettability, adhesion and contact angle analysis

图4为本发明所制备超高黏附性超疏水表面对水滴的接触角和黏附量的光学照片。 FIG 4 superhydrophobic surface adhesion ultrahigh optical photograph of a water droplet contact angle and the amount of the adhesive of the present invention was prepared. (a、d、g)为接触角,纳米级的“鳞片”经硬脂酸修饰后,对水滴的接触角均高于150°。 (A, d, g) is the contact angle, nanoscale "scales" was modified after stearate, the contact angle of water droplet is higher than 150 °. (b、e、h)超疏水表面翻转180°时所悬挂最大体积的水滴,超疏水表面对水滴表现出了很强的黏附力,水滴可以牢牢地固定在其表面上,无论将该表面旋转至90°或180°,水滴都不会滚落或掉落下来。 The maximum volume of the suspended when (b, e, h) superhydrophobic surfaces 180 ° in water droplets, the water droplets on the superhydrophobic surface exhibits a strong adhesion, the water droplets can be firmly fixed on the surface thereof, regardless of the surface rotated to 90 ° or 180 °, the water droplets will not tumble or fall. (c、f、i)超疏水表面倾斜30°时所黏附的最大体积的液滴,随着“鳞片”密度的增大,超疏水表面能够悬挂液滴的最大体积在不断增加。 (C, f, i) when the super-hydrophobic surface is inclined by 30 ° Adhesion maximum volume droplets increases as "scale" density superhydrophobic surface can be suspended droplet increasing maximum volume.

[0012] 图5为本发明所制备的超尚黏附性超疏水表面对水滴的黏附量图。 Super adhesion still adhering amount superhydrophobic surfaces produced [0012] FIG. 5 of the present invention, FIG droplets. 从图5中可以看出,黏附量随着硫酸钴浓度的增大而呈增大趋势,并且同一浓度时,倾斜角度越大,黏附量越大。 As it can be seen from FIG. 5, as the adhering amount increases cobalt sulfate concentration tended to increase, and when the same density, the larger the inclination angle, the greater the amount of adhesion. 倾斜180°时,黏附量从8 μ L逐渐增大到24 μ L和28 μ L ;倾斜45°时,黏附量从14 μ L逐渐增大到36 μ L和40 yL ;倾斜30°时,黏附量从28 μ L逐渐增大到60 μ L和78 μ L0 Tilt 180 °, the amount of adhesion is gradually increased from 8 μ L to 24 μ L and 28 μ L; tilt 45 °, the adhesion is gradually increased from the amount of 14 μ L to 36 μ L and 40 yL; tilt 30 °, adhering amount is gradually increased from 28 μ L to 60 μ L and 78 μ L0

[0013] 图6为本发明所制备的超尚黏附性超疏水表面的黏附力图。 Adhesion is still trying super adhesion superhydrophobic surfaces produced [0013] FIG. 6 of the present invention. 从图6中可以看出,随着硫酸钴浓度的增大,黏附力从109.6 μ N逐渐增大到146.8 μ N和163.4 μ N。 As can be seen from Figure 6, as the cobalt concentration of sulfuric acid is increased, the adhesion is gradually increased to 109.6 μ N 146.8 μ N and 163.4 μ N. 因此,超疏水表面对水滴的黏附量越来越大,这与图4和图5的结论相符合。 Therefore, the super-hydrophobic surface adhesion amount of water droplets growing, which coincide with the conclusion of Figures 4 and 5.

[0014] 2、超尚黏附性超疏水表面的应用 [0014] 2, yet ultra-adhesion superhydrophobic surface application

图7为本发明所制备的超高黏附性超疏水表面的应用。 Application of ultra-high adhesion prepared superhydrophobic surface 7 of the present invention FIG. 将一滴20 μ L的水滴轻轻地滴在低黏附的超疏水表面上,然后用我们制备的超高黏附的超疏水表面轻轻地挤压水滴,水滴变形并最终黏附到超疏水表面上,然后轻轻地升高超疏水表面,水滴从低黏附的超疏水表面转移到超高黏附性超疏水表面上;接着让水滴与亲水的不锈钢块接触,水滴立刻从超高黏附的超疏水表面转移到亲水的不锈钢块上,整个过程如图7所示。 A drop of 20 μ L drops gently dropped on the surface of the superhydrophobic low adhesion, and adhesion with the ultra super hydrophobic surface we prepared gently squeeze water droplets, water droplets adhere to deform and ultimately the superhydrophobic surface, then gently raised superhydrophobic surface, the superhydrophobic surface of the water droplet is transferred from the low adhesion to the ultra super hydrophobic surface adhesion; then let the water droplets to the hydrophilic block of stainless steel in contact, immediately transferred from the water droplet adhesion superhydrophobic surface ultrahigh hydrophilic block to the stainless steel, the entire process as shown in FIG. 超高黏附的超疏水表面的这种转移作用将在微量液体无损失输送中扮演重要的角色。 This shift effect ultra-high adhesion super-hydrophobic surface will play an important role in the transport of trace amounts of liquid without loss.

[0015] 综上所述,本发明制备的超尚黏附性超疏水表面,有着$父好的超疏水性能和$父大的黏附性。 [0015] In summary, the adhesion is still super superhydrophobic surface of the present invention is prepared, the parent has a good $ $ large superhydrophobic properties and adhesion of the parent. 通过选择不同浓度的硫酸钴溶液,可以实现对超疏水表面黏附性的调控。 By selecting different concentrations of cobalt sulfate solution, may be regulated to achieve adhesion of superhydrophobic surfaces. 另外,本发明所制备的超疏水表面的制备工艺简单,原料易得,安全环保,在特殊浸润性界面技术领域有很大的商业化前景。 Further, the preparation process of the superhydrophobic surface of the present invention prepared in a simple, readily available raw materials, safety and environmental protection, there is great commercial prospects special interface wettability art.

附图说明 BRIEF DESCRIPTION

[0016] 图1为本发明所制备的超高黏附性超疏水表面的XRD谱图。 [0016] FIG. 1 XRD spectrum of ultra adhesion superhydrophobic surface of the present invention are prepared.

[0017] 图2为本发明所制备的超高黏附性超疏水表面的EDX谱图。 EDX spectra ultrahigh adhesion superhydrophobic surfaces produced [0017] FIG. 2 of the present invention.

[0018] 图3为本发明中不同浓度硫酸钻所制备的超尚黏附性超疏水表面的SEM图。 [0018] FIG 3 is a SEM image of super-adhesion still superhydrophobic surfaces invention various concentrations of cobalt sulfate prepared.

[0019]图4为本发明所制备的超尚黏附性超疏水表面对水滴的接触角和黏附量的光学照片。 Optical Photo [0019] FIG. 4 of the present invention is prepared is still super adhesion of superhydrophobic surfaces and the contact angle of water droplet adhesion amount.

[0020] 图5为本发明所制备的超尚黏附性超疏水表面对水滴的黏附量图。 Super adhesion still adhering amount superhydrophobic surfaces produced [0020] FIG. 5 of the present invention, FIG droplets.

[0021] 图6为本发明所制备的超尚黏附性超疏水表面的黏附力图。 Adhesion is still trying super adhesion superhydrophobic surfaces produced [0021] FIG. 6 of the present invention.

[0022] 图7为本发明所制备的超尚黏附性超疏水表面的应用。 Application of Ultra still adhesion superhydrophobic surfaces produced [0022] FIG. 7 of the present invention.

具体实施方式 Detailed ways

[0023] 下面通过具体实施例对本发明所制备的超尚黏附性超疏水表面的制备和性能作进一步说明。 [0023] The following Preparation and Properties of Ultra still adhesion superhydrophobic surfaces prepared by the specific embodiments of the present invention will be further described.

[0024] 实施例一 [0024] Example a

将锌片裁剪出1X1 Cm2大小,然后压平。 The zinc sheet cut-out size 1X1 Cm2, and then flatten. 依次用丙酮,无水乙醇及去离子水超声清洗,以便除去锌片表面的污染物。 Washed successively with acetone, ethanol and deionized water ultrasonic cleaning, to remove surface contaminants zinc sheet. 将干净锌片光亮的一面向上浸入装有10 mL的CoSO4水溶液的烧杯中(CoSO4水溶液的浓度0.005 mo IL—1),浸泡30 min,使钴沉积在锌片表面。 The beaker was immersed CoSO4 solution side up with 10 mL clean bright zinc sheet (concentration of the aqueous solution CoSO4 0.005 mo IL-1), soaked 30 min, cobalt zinc sheet deposited on the surface. 反应结束后,倾出溶液,依次用大量的去离子水和无水乙醇清洗锌片,室温晾干。 After completion of the reaction, the solution was decanted, washed with plenty of deionized water and ethanol washing zinc sheet, drying at room temperature. 接着将沉积钴的锌片在硬脂酸的无水乙醇溶液(硬脂酸的浓度0.005 mo I I71)中浸泡30 min,使硬脂酸接枝到钴表面。 Cobalt is then deposited zinc sheet soaked for 30 min in absolute ethanol stearic acid (stearic acid concentration of 0.005 mo I I71) in the cobalt stearate grafted to the surface. 浸泡结束后,用大量的无水乙醇清洗锌片,室温晾干,得超疏水表面。 After soaking, washing with a large amount of zinc sheet ethanol, dried at room temperature to give a superhydrophobic surface.

[0025] 将4 μ L的去离子水水滴静置于该表面上,对水滴的接触角高达155.1 °。 [0025] Static μ L of 4 drops of deionized water are placed on the surface, the water droplet contact angle of up to 155.1 °. 将该沉积钴的锌片翻转180°时,可以黏附水滴的最大体积是8 μ L ;倾斜45°时,可以黏附的水滴的最大体积是14 μ L ;倾斜30°时,可以黏附的水滴的最大体积是28 μ L0 The zinc sheet deposited cobalt rollover 180 °, the maximum volume of water droplet adhesion can be 8 μ L; tilt 45 °, the maximum volume of the water droplets adhesion may be 14 μ L; tilt 30 °, water droplets may adhere The maximum volume of 28 μ L0

[0026] 实施例二 [0026] Second Embodiment

将锌片裁剪出1X1 Cm2大小,然后压平。 The zinc sheet cut-out size 1X1 Cm2, and then flatten. 依次用丙酮,无水乙醇及去离子水超声清洗,以便除去锌片表面的污染物。 Washed successively with acetone, ethanol and deionized water ultrasonic cleaning, to remove surface contaminants zinc sheet. 将干净锌片光亮的一面向上浸入装有10 mL的CoSO4水溶液的烧杯中(CoSO4水溶液的浓度0.01 mo IL ―1),浸泡30 min,使钴沉积在锌片表面。 The beaker was immersed CoSO4 solution side up with 10 mL clean zinc sheet of light (concentration of the aqueous solution of CoSO4 0.01 mo IL -1), soak 30 min, cobalt zinc sheet deposited on the surface. 反应结束后,倾出溶液,依次用大量的去离子水和无水乙醇清洗锌片,室温晾干。 After completion of the reaction, the solution was decanted, washed with plenty of deionized water and ethanol washing zinc sheet, drying at room temperature. 接着将沉积钴的锌片在硬脂酸的无水乙醇溶液(硬脂酸的浓度0.004 mo I I71)中浸泡30 min,使硬脂酸接枝到钴表面。 Cobalt is then deposited zinc sheet soaked for 30 min in absolute ethanol stearic acid (stearic acid concentration of 0.004 mo I I71) in the cobalt stearate grafted to the surface. 浸泡结束后,用大量的无水乙醇清洗锌片,室温晾干,得超疏水表面。 After soaking, washing with a large amount of zinc sheet ethanol, dried at room temperature to give a superhydrophobic surface.

[0027] 将4 μ L的去离子水水滴静置于该表面上,对水滴的接触角是153.8°。 [0027] A droplet 4 Static μ L of deionized water was placed on the surface of the water droplet contact angle is 153.8 °. 将该沉积钴的锌片翻转180°时,可以黏附水滴的最大体积是24 UL ;倾斜45°时,可以黏附的水滴的最大体积是36 μ L ;倾斜30°时,可以黏附的水滴的最大体积是60 μ L。 The maximum tilt 30 °, adhesion may droplets; when the zinc sheet deposited cobalt flipped 180 °, the maximum volume of the water droplets can be adhered is 24 UL; tilt 45 °, the maximum volume of the water droplets can be adhered is 36 μ L volume was 60 μ L.

[0028] 实施例三 [0028] Example three

将锌片裁剪出1X1 Cm2大小,然后压平。 The zinc sheet cut-out size 1X1 Cm2, and then flatten. 依次用丙酮,无水乙醇及去离子水超声清洗,以便除去锌片表面的污染物。 Washed successively with acetone, ethanol and deionized water ultrasonic cleaning, to remove surface contaminants zinc sheet. 将干净锌片光亮的一面向上浸入装有10 mL的CoSO4水溶液的烧杯中(CoSO4水溶液的浓度0.05 mo IL ―1)浸泡30 min,使钴沉积在锌片表面。 The beaker was immersed CoSO4 solution side up with 10 mL clean zinc sheet of light (concentration of the aqueous solution of CoSO4 0.05 mo IL -1) soaked 30 min, cobalt zinc sheet deposited on the surface. 结束后倾出溶液,依次用大量的去离子水和无水乙醇清洗锌片,室温晾干。 After the solution was decanted, washed with plenty of deionized water and ethanol washing zinc sheet, drying at room temperature. 接着将沉积钴的锌片在硬脂酸的无水乙醇溶液(硬脂酸的浓度0.002 mo I I71)中浸泡40 min,使硬脂酸接枝到钴表面。 Cobalt is then deposited zinc sheet soaked 40 min in absolute ethanol solution of stearic acid (stearic acid concentration of 0.002 mo I I71) in the cobalt stearate grafted to the surface. 浸泡结束后,用大量的无水乙醇清洗锌片,室温晾干,得超疏水表面。 After soaking, washing with a large amount of zinc sheet ethanol, dried at room temperature to give a superhydrophobic surface.

[0029] 将4 yL的去离子水水滴静置于该表面上,对水滴的接触角高达157°。 [0029] The 4 yL deionized water drop placed on the surface of the static contact angle of water droplet up to 157 °. 将该沉积钴的锌片翻转180°时,可以黏附水滴的最大体积是28 μ L ;倾斜45°时,可以黏附的水滴的最大体积是40 μ L ;倾斜30°时,可以黏附的水滴的最大体积是78 μ L。 The zinc sheet deposited cobalt rollover 180 °, the maximum volume of the water droplets can be adhered is 28 μ L; tilt 45 °, the maximum volume of the water droplets adhesion may be 40 μ L; tilt 30 °, water droplets may adhere The maximum volume was 78 μ L.

Claims (6)

1.超尚黏附性能超疏水表面的制备方法,是以七水合硫酸钻为反应底物,梓片为基底,水为溶剂,先通过化学沉积法使钴沉积在锌片表面;再将沉积钴的锌片浸泡到硬脂酸的无水乙醇溶液中,使得低表面能的硬脂酸接枝到钴表面,得到超高黏附性超疏水表面。 1. Preparation method of adhesion of super still superhydrophobic surfaces, is cobalt sulfate heptahydrate as the reaction substrate, the substrate sheet is a Zi, water as a solvent, the first cobalt is deposited on the surface of a zinc sheet by a chemical deposition method; then depositing cobalt the zinc sheet immersed in absolute ethanol was stearate, stearic acid so that the low surface energy of the grafted surface cobalt, ultra-high adhesion superhydrophobic surface.
2.如权利要求1所述超高黏附性超疏水表面的制备方法,其特征在于:其具体制备工艺为:先将锌片依次用丙酮、无水乙醇、去离子水超声清洗,于硫酸钴水溶液中浸泡20~30min,使钴沉积在锌片表面;取出并用去离子水和无水乙醇清洗、晾干;再于硬脂酸的无水乙醇溶液中浸泡30~40 min,然后用去离子水和无水乙醇清洗、晾干,即得超高黏附性能的超疏水表面。 2. The method of preparing an ultra-high surface adhesion superhydrophobic claim, wherein: the specific preparation process: first zinc sheets successively with acetone, ethanol, de-ionized water ultrasonic cleaning, to cobalt sulfate immersed aqueous 20 ~ 30min, cobalt zinc sheet deposited on the surface; and extracted with deionized water and absolute ethanol wash, dry; stearic acid in ethanol and then immersed in a solution of 30 ~ 40 min, and then washed with deionized water and ethanol washing, drying, to obtain the adhesion of the ultra super hydrophobic surface.
3.如权利要求1或2所述超高黏附性超疏水表面的制备方法,其特征在于:所述硫酸钴水溶液的浓度为0.005-0.05 mol/Lo 3. The ultra-high adhesion superhydrophobic surface preparation as claimed in claim 1 or 2, wherein: the concentration of the aqueous solution of cobalt sulfate is 0.005-0.05 mol / Lo
4.如权利要求1或2所述超高黏附性超疏水表面的制备方法,其特征在于:所述硬脂酸的无水乙醇溶液中,硬脂酸的浓度为0.002-0.005 mol/Lo 4. The method of claim 1 or 2 preparing ultra superhydrophobic surface adhesion claim, wherein: said absolute ethanol stearic acid, a stearic acid concentration of 0.002-0.005 mol / Lo
5.如权利要求1或2所述超高黏附性超疏水表面的制备方法,其特征在于:所述硫酸钴水溶液与锌片的体积面积比为5:1~10:1 mL/cm2。 5. The method of claim 1 or 2 preparing ultra superhydrophobic surface adhesion claim, wherein: the area ratio of the volume of the aqueous solution of cobalt sulfate and zinc sheet was 5: 1 ~ 10: 1 mL / cm2.
6.如权利要求1或2所述超高黏附性超疏水表面的制备方法,其特征在于:所述硬脂酸的无水乙醇溶液与锌片的体积面积比为5:1~10:1 mL/cm2。 6. The method of claim 1 or 2 preparing ultra superhydrophobic surface adhesion claim, wherein: the area ratio of the volume of absolute ethanol and stearic acid zinc film is 5: 1 to 10: 1 mL / cm2.
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CN102615036A (en) * 2012-04-08 2012-08-01 大连理工大学 Method for preparing steel matrix high-adhesion super-hydrophobic surface
CN102615037A (en) * 2012-04-19 2012-08-01 大连理工大学 Method for preparing super-hydrophobic green film on magnesium alloy substrate
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101517125A (en) * 2006-09-20 2009-08-26 英国贝尔法斯特女王大学 Method of coating a metallic article with a surface of tailored wettability
CN101967663A (en) * 2010-08-27 2011-02-09 中国科学院海洋研究所 Method for preparing super-hydrophobic alloy film on surface of metal matrix
CN102615036A (en) * 2012-04-08 2012-08-01 大连理工大学 Method for preparing steel matrix high-adhesion super-hydrophobic surface
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