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Publication numberCN101705488 A
Publication typeApplication
Application numberCN 200910212774
Publication date12 May 2010
Filing date9 Nov 2009
Priority date9 Nov 2009
Also published asCN101705488B
Publication number200910212774.X, CN 101705488 A, CN 101705488A, CN 200910212774, CN-A-101705488, CN101705488 A, CN101705488A, CN200910212774, CN200910212774.X
Inventors余新泉, 周荃卉, 张友法, 李康宁, 陈锋
Applicant东南大学
Export CitationBiBTeX, EndNote, RefMan
External Links: SIPO, Espacenet
Surface processing method of super-hydrophobic ice-covering-proof aluminum and steel with rough surface
CN 101705488 A
Abstract
The invention relates to a surface processing method of super-hydrophobic ice-covering-proof aluminum and steel with rough surfaces. The method comprises the following steps: performing ultrasonic cleaning to aluminum and steel plates with acetone and deionized water, drying, suspending the aluminum and steel plates in a sealed container with 20vol.%-80vol.% of hydrochloric acid solution, then etching aluminum and steel plates with volatile hydrochloric acid for 15min-1h in a water bath under the temperature of boiling water, namely 100 DEG C; after the etching, placing the aluminum and steel plates in the normal hexane solution of fluorosilane to performing evaporation and modification of fluorosilane at 200-300 DEG C for 1-2h, and finally taking out the samples to keep temperature in the air at 180-300 DEG C for 1-2h; and in the fluorosilane solution, the weight ratio of fluorosilane to normal hexane is 1-5%, and the pH value of the added acetic acid aqueous solution is 3 and the content is 2-4% of the normal hexane solution of fluorosilane.
Claims(1)  translated from Chinese
  1. 一种超疏水低粘着性防覆冰铜表面的制备方法,其特征在于所述制备方法包括下列步骤:(1)前处理:将铝片和钢片依次用丙酮、去离子水超声波清洗并烘干;(2)湿化学刻蚀:将铝片或钢片悬挂于盛有盐酸溶液的密闭装置中,然后将密闭装置置于恒温水浴槽中,100℃沸水温度下使盐酸挥发,并用挥发的盐酸刻蚀铝片或钢片,取出铝片或钢片后用清水冲洗并烘干;所述盐酸的体积分数为20%-80%,刻蚀时间为15min-1h;(3)氟化处理:将刻蚀后的铝片和钢片放入盛有氟硅烷正己烷溶液的密闭容器内,并一同放入箱式电炉中200-300℃下保温1-2h,实现铝片和钢片表面的氟硅烷修饰;随后取出样品,于180-300℃下在空气中保温1-2h,即可得到具备超疏水特性的铝和钢表面;制备的铝和钢表面的结霜实验表明,这种表面有很好的防覆冰性能;所述氟硅烷溶液的配制过程为:将氟硅烷溶于正己烷溶剂中,氟硅烷与正己烷溶剂的重量百分比为1-5%,再加入氟硅烷正己烷溶液重量的2-4%、pH值为3的醋酸水溶液,充分搅拌后即可使用。 A method of preparing a superhydrophobic low viscosity anti-icing copper surface, characterized in that said process comprising the steps of: (1) pre-treatment: The aluminum and steel successively with acetone, deionized water, ultrasonic cleaning and drying dry; (2) wet chemical etching: The aluminum or steel suspension in a sealed device containing hydrochloric acid solution, and then the device is placed in a sealed thermostatic water bath, so that the temperature of boiling water at 100 ℃ volatile hydrochloric acid, and with volatile hydrochloric acid etching of aluminum or steel, aluminum or steel after removing rinse with water and dried; the hydrochloric acid volume fraction of 20% -80%, the etching time was 15min-1h; (3) the fluorination treatment : The etched aluminum and steel into fluorine containing silane-hexane solution within a closed container, and placed in a box with electric furnace 200-300 ℃ incubated 1-2h, realized aluminum and steel surfaces The fluorosilane modification; samples were then removed, incubated 1-2h at 180-300 ℃ in air, can be obtained with super hydrophobic surface characteristics of aluminum and steel; frost experimental aluminum and steel surfaces prepared show that this surface has a good anti-icing properties; preparation process for the fluoro silane solution: The fluorosilane dissolved in a solvent of n-hexane, and n-hexane fluorosilane weight percentage of 1-5% of the solvent, and then adding n-hexyl fluorosilane 2-4% by weight dioxane solution, pH value of the aqueous solution of acetic acid 3, can be used after sufficiently stirring.
Description  translated from Chinese

具有粗糙表面的超疏水防覆冰铝和钢的表面处理方法 With a rough surface super-hydrophobic surface treatment method the anti-icing aluminum and steel

技术领域 Technical Field

[0001] 本发明涉及一种具有粗糙表面的超疏水防覆冰铝和钢的表面处理方法。 [0001] The present invention relates to a rough surface anti-icing superhydrophobic surface treatment of aluminum and steel have.

背景技术 Background

[0002] 结霜现象广泛存在于制冷和低温运行设备的金属零部件中,例如热泵机组的空气盘管、航空航天器的机翼和表面、空调、冰箱内表面等,给设备的稳定工作带来了不同程度的危害。 [0002] frost is widespread in the metal parts of refrigeration and cryogenic equipment operation, such as an air coil heat pump units, wing and surface aerospace vehicles, air conditioners, refrigerators, surface, etc., to bring stability equipment to varying degrees of damage.

[0003] 传统的工程材料表面防结冰技术多利用机械或加热技术除冰、融冰,如热力融冰、 过电流融冰、短路融冰、带负荷融冰等。 [0003] The traditional engineering materials technology multi-surface anti-icing heating technology using mechanical or de-icing, melt the ice, such as heat melting ice, melting ice over current, short melting ice, melting ice with a load. 现有的一些发明技术也是基于"融冰"的思路,如:采用高频脉冲电流加热振荡法对输配电线路防覆冰除融冰,采用与输配电的导线一同敷设的导体发热来防覆冰。 Some of the existing technology is also based on the invention "ice-melting" ideas, such as: the use of high-frequency pulse current heating oscillation method for transmission and distribution lines in addition to the anti-icing melting ice, use and transmission and distribution wires with conductor heating to lay Anti-icing. 但这些方法不能从根本上解决问题,且在除冰时需停止设备,并配以专门的除冰系统和装备。 However, these methods do not solve the problem fundamentally, and the need to stop at the de-icing equipment, and with a special de-icing systems and equipment. 这无疑给生产带来了不便,同时也消耗了大量的能源,增加了成本。 This is undoubtedly the inconvenience to the production, but also consumes a lot of energy, increasing the cost. 为此,部分研究人员以抑制结冰为出发点,探索出了一些抑制结冰的方法。 For this reason, some researchers to inhibit freezing as a starting point to explore a number of inhibiting freezing method. 如在冷表面涂以亲水性抑霜涂料[0koroafor EU, J Phy.D_App.Phy. ,1999,32(18) :2454-2461 ;0koroafor EU,Newborough M,App. Thermal Eng. , 2000, 20 (8) :737-758],可降低霜的厚度达10-30% , 但这种涂层较厚,约0. 77mm,影响到冷表面空气流通,且涂料中的有机成分易挥发,使得其使用寿命较低;北京工业大学刘中良等开发了一种强亲水性抑霜涂料,该涂料含有吸水性树脂,可吸收大量水分,且添加的氯化钠或氯化钾颗粒可有效降低水的冰点,使吸收涂料内的水分长时间保持不冻结,从而抑制初始霜晶的出现,起到抑霜的作用,但这种强亲水性表面吸收的水分不易快速挥发,由于只是降低水的冰点,所以在温度更低时反而会促进霜晶的形成,加剧表面的结霜。 As the cold surface coated with hydrophilic coatings suppress cream [0koroafor EU, J Phy.D_App.Phy, 1999,32 (18):. 2454-2461; 0koroafor EU, Newborough M, App Thermal Eng, 2000, 20.. (8): 737-758], can be reduced up to 10-30% of the thickness of the cream, but this coating thicker, about 0. 77mm, the impact surface to the cold air flow, and the paint volatile organic components, such its life is low; Beijing University Liu Zhongliang, etc. have developed a strong suppression hydrophilic cream coatings that contain water-absorbing resin, can absorb large amounts of water, and add sodium chloride or potassium chloride particles can effectively reduce the water the freezing point, the moisture absorbent coating remains frozen for a long time, thus inhibiting the initial frost crystals appeared, played the role of frost suppression, but this strongly hydrophilic surface moisture absorbed easily evaporate quickly, since only reduce water freezing point, so at lower temperatures it will promote the formation of frost crystals, increasing frost surface.

[0004] 仿照具有"荷叶效应(Lotus Effect)"生物体特殊的表面微观结构,可在金属表面构筑类似的特殊结构,得到具有超疏水特性的金属表面。 [0004] modeled with the "lotus effect (Lotus Effect)" special surface microstructure of the organism, can build a special structure similar to the metal surface to give a super-hydrophobic properties of the metal surface. 这种超疏水金属表面在自净、减阻、耐腐蚀、抗结冰等领域有着极其巨大的应用潜力和广阔的应用前景。 This super-hydrophobic metal surface purification, drag reduction, corrosion resistance, anti-icing and other fields has a very great potential and broad prospects. 以此为启发,一些疏水性防结冰涂料和镀膜技术相继被开发。 This was inspired by some of the anti-icing coating and the hydrophobic coating technology have been being developed. 如将有机硅烷和/或氟硅树脂、快干性溶剂、主体溶剂室温搅拌后,相继加入聚氧化乙烯、硅烷偶联剂促进剂、氧化硅和/或氧化铝颗粒搅拌,最后涂覆在试样表面固化得到防结冰涂层,可使结霜量减少40%,但这种技术对形状复杂的设备和零件的一些部位不易涂覆,使得防护不均匀,且涂料中的有机溶剂易挥发,使用寿命较低,结霜层也需在机械振动下去除,对一些需防结冰但不能进行振动的精密仪器、设备和零件有一定的局限性;通过真空蒸镀方式,在输电电缆表面涂镀正三十六烷疏水层也可延迟初始霜晶的形成,形成的霜晶结构疏松,较易去除,但需要指出的是,这种镀膜方法需要在真空度小于1. 3X10—5的真空条件下进行,显然不易进行大规模生产。 As the organic silane and / or fluorine silicone, quick-drying solvent, stirring at room temperature after the principal solvent, were added successively polyoxyethylene, silane coupling accelerator, silica and / or alumina particles was stirred, and finally coated test like anti-icing coating obtained by curing the surface, it can reduce by 40% the amount of frost, but this technique for some parts of the equipment and parts of complex shape is not easily applied, so uneven protection and paint volatile organic solvent life is low, frost layer also need to be removed in mechanical vibration, for some to be anti-icing but not vibrate precision instruments, equipment and spare parts have some limitations; the way by vacuum evaporation, the surface of the transmission cable n Hexatriacontane hydrophobic coating layer may delay the initial frost crystals form, frost crystal structure formed loose, easily removed, but should be noted that this coating method requires a vacuum of less than 1. 3X10-5 under vacuum conditions, apparently difficult for mass production. [0005] 研究表明[Byeongchul N, Ralph LW, Int. J Hea備ass Transfer, 2003, 46, 3797-3808],固体表面的粗糙度会降低水蒸气的过饱和度,从而降低水珠的成核率和成核速度,延缓初始霜晶的形成,起到抑霜的作用。 [0005] Studies have shown that [Byeongchul N, Ralph LW, Int. J Hea prepare ass Transfer, 2003, 46, 3797-3808], the roughness of the solid surface will reduce the over-saturation of water vapor, thereby reducing the water droplets nucleation rate and nucleation rate, delay initial frost crystals form, played the role of suppressing frost. 同时,疏水性表面形成水珠的势垒比亲水性表面大,因此疏水性表面上凝结成液核的数量较亲水性表面小。 Meanwhile, the formation of water droplets in the hydrophobic surface hydrophilic surface barrier than large, so condensed into liquid on a hydrophobic surface number of smaller nuclear hydrophilic surface. 因此,在固体表面,尤其是 Thus, the solid surface, especially

3应用广泛的铝和钢的表面同时构筑粗糙度和疏水性,将会更有效的延缓初始霜晶的出现, 显著提高铝和钢表面的抗结冰性能。 Extensive application of aluminum and steel surface 3 while constructing roughness and hydrophobicity, will be more effectively delay the initial frost crystals appear significantly improve the anti-icing properties of aluminum and steel surfaces. 但基于这种思路,且针对铝和钢表面的疏水性防结冰技术尚未见有报道。 But based on this idea, and hydrophobic anti-icing technology for aluminum and steel surfaces it has not been reported.

发明内容 DISCLOSURE

[0006] 本发明提供一种超疏水防覆冰粗糙铝和钢表面的处理方法。 [0006] The present invention provides a super-hydrophobic anti-clad aluminum and steel rough treatment of the ice surface. [0007] 本发明采用如下技术方案: [0007] The present invention adopts the following technical solution:

[0008] —种超疏水防覆冰粗糙铝和钢表面的处理方法,处理的步骤如下: [0008] - the kind of super-hydrophobic anti-icing treatment of rough aluminum and steel surface treatment steps are as follows:

[0009] (1)前处理:将铝片和钢片依次用丙酮、去离子水超声波清洗并烘干; [0009] (1) pre-treatment: The aluminum and steel successively with acetone, deionized water, ultrasonic cleaning and drying;

[0010] (2)湿化学刻蚀:将铝片或钢片悬挂于盛有盐酸溶液的密闭装置中,然后将密闭 [0010] (2) wet chemical etching: The aluminum or steel suspended in a solution containing hydrochloric acid in a closed system, then closed

装置置于恒温水浴槽中,10(TC沸水温度下使盐酸挥发,并用挥发的盐酸刻蚀铝片或钢片, Device placed in a constant temperature water bath, 10 hydrochloride (TC boiling temperature at the volatile and volatile hydrochloric acid etching with aluminum or steel,

取出铝片或钢片后用清水冲洗并烘干;所述盐酸的体积分数为20% _80%,刻蚀时间为 After removing aluminum or steel rinse with water and dried; the volume fraction of hydrochloric acid 20% _80%, the etching time

15min-lh ; 15min-lh;

[0011] (3)氟化处理:将刻蚀后的铝片和钢片放入盛有氟硅烷正己烷溶液的密闭容器内,并一同放入箱式电炉中200-30(TC下保温l-2h,实现铝片和钢片表面的氟硅烷修饰;随后取出样品,于180-30(TC下在空气中保温l-2h,即可得到具备超疏水特性的铝和钢表面; 制备的铝和钢表面的结霜实验表明,这种表面有很好的防覆冰性能;所述氟硅烷溶液的配制过程为:将氟硅烷溶于正己烷溶剂中,氟硅烷与正己烷溶剂的重量百分比为1_5%,再加入氟硅烷正己烷溶液重量的2-4X、pH值为3的醋酸水溶液,充分搅拌后即可使用。 [0012] 本发明制备得到了具有粗糙表面的超疏水防覆冰铝和钢的表面。首先,铝和钢表面的粗糙度会降低水蒸气的过饱和度,从而降低水滴的成核率和成核速度,延缓初始霜晶的形成,起到抑霜的作用。其次,这种表面对水具有优良的超疏水性能和很低的粘滞力,与水滴接触时,具有很高的接触角(> 150 )和极低的滚动角(1 )。超疏水性表面不但会增大形成水珠的势垒,减小表面水滴凝结成液核的数量,同时会在与水滴接触时,在接触界面截留空气形成"气垫",显著减小水珠与固体表面的实际接触面积(< 10% ),从而在低温时有效降低表面与水滴间的热量交换,增大水珠凝结所需的能量,最终使得水滴难以凝结成核形成初始霜晶,并抑制在初始霜晶基础上生长的霜层的形成和生长。需要指出的是,由于制备的铝和钢表面对水滴的粘滞性较低,水滴在这种表面极易滚落,轻微的振动,甚至是风吹都有可能使得水滴滚落,从而不易吸附冻结形成霜晶,即使形成,也由于粘滞性较低而极易滑落,从而不但起到了抑制结冰的作用,还起到了除冰的效果,真正实现铝和钢表面的防覆冰。因此,在应用广泛的铝和钢表面制备具有一定粗糙度的超疏水防覆冰表面,不但会更有效的延缓初始霜晶的出现,显著提高铝和钢表面的抗结冰性能,还可以利用表面的低粘滞性来除冰,实现真正的铝和钢表面防覆冰。如在潜艇或舰船的外壳上制备这种超疏水防覆冰表面,不但可保持表面的自清洁、提高航行速度和耐海水腐蚀性,还可使外壳在低温条件下没有覆冰,从而为它们在低温条件下,如在南极、北极或其它高寒地区的航行,提供保障。 [0011] (3) fluoride treatment: etched aluminum and steel into the fluorine containing silane-hexane solution within a closed container, and placed in a box with electric furnace 200-30 (TC incubated l -2h, aluminum and steel surfaces to achieve fluorosilanes modification; then a sample was taken at 180-30 (TC incubated for l-2h in the air, you can get with the super-hydrophobic surface properties of aluminum and steel; aluminum prepared and frost steel surface experiments show that the surface has a good anti-icing properties; the preparation process of the fluorine silane solution is: will fluorosilanes dissolved in hexane solvent, the weight percentage of n-hexane solvent fluorosilanes to 1_5% n-hexane solution was added fluorosilanes weight 2-4X, pH value of an aqueous solution of acetic acid 3 can be used after stir. [0012] The present invention has been prepared with a rough surface super-hydrophobic anti-icing aluminum and the surface of the steel. First, the surface roughness of the aluminum and steel will reduce the over-saturation of water vapor, thereby reducing the droplet nucleation rate and nucleation rate, delaying initial frost crystals form, played the role of suppressing frost Second , the surface of the water with excellent superhydrophobic properties and low viscous forces, when in contact with water droplets, with a high contact angle (> 150 ) and low rolling angle (1 ). superhydrophobic not only will increase the formation of water droplets surface barrier, reducing the surface condenses into liquid droplets the number of cores, and it will in contact with water droplets, the contact interface trapped air to form "cushion" significantly reduce water drops and solid surface The actual contact area (<10%), so that at low temperature to reduce the heat exchange between the surface and the water droplets, dew condensation increases the energy required, ultimately making it difficult to condense into water droplets initially formed frost crystal nucleation and suppressed initial Cream Based on the crystal growth of frost layer formation and growth. It should be noted that, due to aluminum and steel surfaces prepared to lower the viscosity of the water droplets, water droplets in this surface easily rolled, slight vibration, even the wind Blow are likely to make water drops rolled so easily adsorbed freeze frost crystals form, even if formed, but also due to the low viscosity and can easily fall, thereby inhibiting ice not only played a role, but also played a deicing effect, real anti-icing aluminum and steel surfaces. Therefore, widely used aluminum and steel surface has some roughness prepared superhydrophobic surface anti-icing, not only will more effectively delay the initial frost crystals appeared significantly improved aluminum and anti-icing properties of steel surface can also be used in low-viscosity surface deicing, real aluminum and steel surface anti-icing as this super-hydrophobic surface anti-icing prepared on a submarine or a ship shell , not only to keep the surface self-cleaning, improve navigation speed and resistance to seawater corrosion, but also the housing no icing in cold conditions, so as they are at low temperatures, such as sailing in the Antarctic, the Arctic and other cold regions, provide protection.

[0013] 本发明提供的制备工艺基于湿化学刻蚀法,所需原材料为丙酮、盐酸、氟硅烷、正己烷、醋酸等常见溶剂,所需设备为超声波清洗机、恒温水浴槽、密闭容器、箱式电炉等常见设备,工艺步骤和设备作十分简单,且根据生产规模的需求,通过适当调整即可满足要求,效率高、成本低。 [0013] The preparation process of the present invention provides a method based on wet chemical etching, the raw materials needed for the common solvents such as acetone, hydrochloric acid, fluorine silane, n-hexane, acetic acid, etc., required equipment for ultrasonic cleaning machine, constant temperature water bath, airtight container, common box-type furnace and other equipment, process steps and equipment for the very simple, and according to the needs of production scale, through appropriate adjustments to meet the requirements, high efficiency and low cost. 此外,这种铝和钢表面超疏水防覆冰的处理方法,对铝和钢本身没有特殊要求,且对复杂产品的一些不易涂镀的部位也能进行有效处理。 In addition, this aluminum and steel surfaces superhydrophobic anti-icing treatment, aluminum and steel does not have special requirements, and some of the difficult parts of a complex product coating can be effectively addressed. 因此,本发明提供的具有粗糙表面的超疏水防覆冰铝和钢的表面处理方法适用性较广,易工业化应用。 Accordingly, the present invention provides a rough surface super-hydrophobic surface treatment of aluminum and steel anti-icing wider applicability, easy to industrial applications.

附图说明: Brief description:

[0014] 图1为制备的超疏水防覆冰粗糙铝表面的扫描电镜图及表面水珠形态。 [0014] FIG. 1 is prepared superhydrophobic anti-icing rough aluminum surface scanning electron micrographs and surface water droplets form.

[0015] 图2为未经处理的铝表面在结霜实验条件下的结霜形态(二值化处理后)。 [0015] Figure 2 is untreated aluminum surface under the experimental conditions of frost frost forms (binarized treatment).

[0016] 图3为制备的超疏水防覆冰粗糙铝表面在结霜实验条件下的结霜形态(二值化处理后)。 [0016] FIG. 3 is prepared superhydrophobic aluminum rough anti-icing frosting frost forms in experimental conditions (binarization processing).

[0017] 图4制备的超疏水防覆冰粗糙钢表面的扫描电镜图及表面水珠形态。 [0017] FIG. 4 SEM preparation of superhydrophobic anti-icing rough steel surface morphology and surface water drops.

[0018] 图5为未经处理的钢表面在结霜实验条件下的结霜形态(二值化处理后)。 [0018] FIG. 5 is untreated steel surface under the experimental conditions of frost frost forms (binarized treatment).

[0019] 图6为制备的超疏水防覆冰粗糙钢表面在结霜实验条件下的结霜形态(二值化处理后)。 [0019] FIG. 6 (binarization processing) super-hydrophobic anti-icing rough steel surface morphology of prepared frosting frost under experimental conditions.

具体实施方式 DETAILED DESCRIPTION

[0020] —种超疏水防覆冰粗糙铝和钢表面的处理方法: [0020] - the kind of super-hydrophobic anti-icing rough aluminum and steel surface treatment:

[0021] (1)前处理:将铝片和钢片依次用丙酮、去离子水超声波清洗并烘干; [0021] (1) pre-treatment: The aluminum and steel successively with acetone, deionized water, ultrasonic cleaning and drying;

[0022] (2)湿化学刻蚀:将铝片或钢片悬挂于盛有盐酸溶液的密闭装置中,然后将密闭 [0022] (2) wet chemical etching: The aluminum or steel suspended in a solution containing hydrochloric acid in a closed system, then closed

装置置于恒温水浴槽中,10(TC沸水温度下使盐酸挥发,并用挥发的盐酸刻蚀铝片或钢片, Device placed in a constant temperature water bath, 10 hydrochloride (TC boiling temperature at the volatile and volatile hydrochloric acid etching with aluminum or steel,

取出铝片或钢片后用清水冲洗并烘干;所述盐酸的体积分数为20% _80%,刻蚀时间为 After removing aluminum or steel rinse with water and dried; the volume fraction of hydrochloric acid 20% _80%, the etching time

15min-lh ;在本实施例中,盐酸的体积分数选用20%、80%或68%,刻蚀时间15min、lh或 15min-lh; in the present embodiment, the selection of hydrochloric acid of 20% volume fraction of 80% or 68%, the etching time 15min, lh or

37min ; 37min;

[0023] (3)氟化处理:将刻蚀后的铝片或钢片放入盛有氟硅烷正己烷溶液的密闭容器内,并一同放入箱式电炉中200-30(TC下保温l-2h,实现铝片和钢片表面的氟硅烷修饰;随后取出样品,于180-30(TC下在空气中保温l-2h,即可得到具备超疏水特性的铝和钢表面; 制备的铝和钢表面的结霜实验表明,这种表面有很好的防覆冰性能;所述氟硅烷溶液的配制过程为:将氟硅烷溶于正己烷溶剂中,氟硅烷与正己烷溶剂的重量百分比为1_5%,再加入氟硅烷正己烷溶液重量的2-4%、 pH值为3的醋酸水溶液,充分搅拌后即可使用;在本实施例中,氟化用的氟硅烷正己烷溶液中,氟硅烷与正己烷溶剂的重量百分比为1%、5% 或3. 2%,加入的醋酸水溶液为氟硅烷正己烷溶液重量的2%、4%或3. 3%,密闭容器放入箱式电炉中加热至20(TC、30(rC或148t:,并保温lh、2h或1. 4h,铝片或钢片样品最后在180。C、300。C或247。C下的空气中保温lh、2h或1. 7h。 [0024] 实例1 [0023] (3) fluoride treatment: after etching of aluminum or steel into fluorine containing silane-hexane solution within a closed container, and placed in a box with electric furnace 200-30 (TC incubated l -2h, aluminum and steel surfaces to achieve fluorosilanes modification; then a sample was taken at 180-30 (TC incubated for l-2h in the air, you can get with the super-hydrophobic surface properties of aluminum and steel; aluminum prepared and frost steel surface experiments show that the surface has a good anti-icing properties; the preparation process of the fluorine silane solution is: will fluorosilanes dissolved in hexane solvent, the weight percentage of n-hexane solvent fluorosilanes of 1_5%, adding 2-4% by weight of n-hexane solution fluorosilane, pH value of the aqueous solution of acetic acid 3, can be used after sufficiently stirring; in the present embodiment, the fluorinated fluorosilane with n-hexane solution, fluorosilane weight percent n-hexane with 1%, 5% or 3.2% aqueous solution of acetic acid was added 2% by weight of n-hexane solution fluorosilane, 4%, or 3.3%, placed in a sealed container box furnace heated to 20 (TC, 30 (rC or 148t :, and incubated lh, 2h, or 1. 4h, aluminum or steel sample finally 180.C, 300.C or 247.C lh incubation under air , 2h or 1. 7h. [0024] Example 1

[0025] 首先用丙酮、去离子水超声波清洗铝片并烘干;随后用浓度为40%的盐酸水溶液,在沸水槽内的密闭容器中,蒸汽法刻蚀铝片lh,取出后清水冲洗并烘干;用pH值为3的醋酸水溶液调节氟硅烷正己烷溶剂,其中氟硅烷与正己烷的重量百分比为2%,醋酸水溶液与氟硅烷正己烷溶液的重量百分比也为2% ;将刻蚀后的铝片悬挂于上述氟硅烷正己烷溶液上方,密闭后一同放入箱式电炉中25(TC下保温2h,实现铝片表面的氟硅烷修饰;随后取出样品,继续于25(TC下保温0. 5h,得到的具备超疏水特性的粗糙铝表面的形貌及表面水 [0025] First with acetone, deionized water, ultrasonic cleaning aluminum sheet and dried; then an aqueous solution of hydrochloric acid at a concentration of 40%, in boiling water bath in a closed container, steam etching aluminum lh, rinse with water after removing and drying; pH 3 with aqueous acetic acid adjusted fluorosilane hexane solvent, wherein the weight percentage of n-hexane fluorosilane with 2% aqueous acetic acid solution and the weight percentage of n-hexane solution fluorosilane also 2%; the etching After aluminum suspension in n-hexane solution above said fluorosilanes together into the closed box-shaped electric furnace after 25 (TC incubated 2h, achieve fluorosilane modified aluminum surfaces; then a sample was taken and continue to 25 (TC incubated 0. 5h, morphology and surface water obtained have superhydrophobic properties of the aluminum surface rough

5滴形态如图1所示,相应数据如表1所示。 5 drops of Form 1, the corresponding data is shown in Table 1. 从表1可见,同未处理的铝片表面相比,制备得到的铝表面超疏水性能较好,且水滴极易滚落。 From Table 1, compared with untreated aluminum surface, preferably superhydrophobic properties of the aluminum surface prepared, and drop easily rolled.

[0026] 试样结霜实验的条件如下:环境温度5C ,冷表面温度_5C ,相对湿度77% ,采用半导体制冷方式制冷,每2min通过图像采集系统对结霜的过程进行实时采集,并对采集的图像进行二值化处理,最后从二值化图像中获取霜层高度等相关信息,并以此来衡量试样的抗结冰性能。 Conditions [0026] frost test sample as follows: ambient temperature of 5 C, cold surface temperature _5 C, relative humidity of 77%, the use of semiconductor refrigeration cooling mode, by image acquisition system for real-time process of frost every 2min collection, and the collection of binary image processing, and finally get frost layer height and other relevant information from the binary image, and as a measure of anti-icing properties of the sample.

[0027] 对于未经处理的铝片表面,其结霜实验结果如图2所示,结霜试验进行2min时, 未经处理的铝片表面已形成霜层,且分布均匀(图2中l所指);随着结霜试验的进行,表面上的霜层不断生长,霜层高度不断增加,10min时结霜严重(图2中5所指),霜高达到0. 1542mm,显示出较差的防结冰性能。 [0027] For the aluminum surface untreated, the results shown in Figure 2 frost, frost trials 2min, the aluminum surface untreated frost layer has been formed, and uniform distribution (Figure 2 l meaning); As the frost tests, frost layer on the surface continue to grow, increasing the height of the frost layer, when severe frost 10min (Figure 2 5 above), reaching a high frost 0. 1542mm, showing relatively poor anti-icing properties. 对于制备的超疏水防覆冰粗糙铝表面,其结霜实验结果如图3所示。 For the super-hydrophobic anti-icing rough aluminum surface preparation, the frost results shown in Figure 3. 这种表面的结霜速度明显降低,在最初的4min里几乎没有霜晶形成(图3 中1和2所指),随后虽有少量初始霜晶形成(图3中3和4所指),但速度较低,至10min 时,也仅有少量初始霜晶,仍未形成霜层(图3中5所指),霜晶的平均高度仅为0. 0354mm。 This surface frost significantly reduced rate, in the first 4min almost no frost crystals formed (Fig. 1 and 2 within the meaning of 3), although a small amount of initial frost crystals then formed (Fig. 3 and 4 within the meaning of 3), but the speed is low, to 10min when there was only a small amount of initial frost crystals, yet frost layer is formed (Fig. 3 5 above), the average height of frost crystals only 0. 0354mm. [0028] 表1制备的铝片表面与水的接触角、滚动角及防覆冰性能[0029] [0028] The contact angle of the aluminum surface in Table 1 was prepared with water, roll angle and anti-icing properties [0029]

<table>table see original document page 6</column></row> <table> <Table> table see original document page 6 </ column> </ row> <table>

[0030] 实例2 [0030] Example 2

[0031] 将钢片依次用丙酮、去离子水超声波清洗并烘干;将浓度为75%的盐酸溶液和悬 [0031] The steel sheet was washed successively with acetone, deionized water, ultrasonic cleaning and drying; the hydrochloric acid concentration of 75% and a suspension

挂有钢片的密闭容器置于沸水槽内30min,随后取出,清水冲洗并烘干;用pH值为3的醋酸 Hanging steel sealed container in a boiling water bath 30min, then removed, rinse and dry; pH 3 with acetic acid

水溶液调节氟硅烷正己烷溶剂,其中氟硅烷与正己烷的重量百分比为2%,醋酸水溶液与氟 Adjusting fluorosilane aqueous solvent of n-hexane, and wherein the weight percent of n-hexane fluorosilane 2% aqueous acetic acid and fluorine

硅烷正己烷溶液的重量百分比也为2% ;将刻蚀后的钢片放入盛有上述氟硅烷正己烷溶液 Weight percent n-hexane solution of silane is also 2%; the steel etched into the fluorine-containing silane-n-hexane solution

的密闭容器内,并一同放入箱式电炉中25(TC下保温2h,实现钢片表面的氟硅烷修饰;随后 In the sealed container, and placed in a box with electric furnace 25 (TC incubated for 2h, achieve fluorosilane modified steel surface; then

取出样品,继续于25(TC下保温0. 5h,得到的具备超疏水特性的粗糙钢表面的形貌及表面 Samples were removed, continue to 25 (TC incubated 0. 5h, morphology and surface characteristics obtained have superhydrophobic rough steel surface

水滴形态如图4所示,相应数据如表2所示。 As shown in Figure 4 forms droplets, the corresponding data are shown in Table 2. 从表2可见,同未处理的钢片表面相比,制备 From Table 2, compared with the untreated steel surface preparation

得到的钢表面超疏水性能较好,且水滴极易滚落。 Steel surface was super good hydrophobic properties, and drop easily rolled.

[0032] 表2制备的钢片表面与水的接触角、滚动角及防覆冰性能 [0032] Table 2, the contact angle of the steel surface was prepared with water, roll angle and anti-icing performance

[0033]<table>table see original document page 7</column></row> <table>[0034] 钢片表面结霜实验条件与铝片表面结霜实验相同,相应的结果如图5和图6所示。 [0033] <table> table see original document page 7 </ column> </ row> <table> [0034] steel and aluminum experimental conditions frosting frosting same experiment, and the corresponding results are shown in FIG. 5 and FIG 6. 未经处理的钢片表面的结霜情况与未经处理的铝片类似,结霜实验2min就开始出现霜晶,但分布稀疏,4min时出现了霜层,且随着结霜试验的进行,霜层不断增高,如图5所示, lOmin时达到了O. 14mm,结冰现象严重。 Similar situations without frost aluminum treated with untreated steel surfaces, frost experiment 2min frost crystals began to appear, but sparse, 4min event of a frost layer, and with frost to be tested, frost layer continues to grow, as shown in Figure 5, lOmin reached O. 14mm, severe icing. 同制备的超疏水防覆冰粗糙铝表面类似,制备的超疏水防覆冰粗糙钢表面在结霜实验的10min里只出现很稀疏的霜晶,一直未形成霜层,如图6所示,且10min时的平均霜晶高只有0. 0108mm,显示出优异的防覆冰效果。 Preparation of the superhydrophobic with anti-icing similar rough aluminum surfaces superhydrophobic anti-icing rough steel surface preparation experiment appear in frost in only very sparse 10min frost crystals frost layer has not formed, as shown in Figure 6, and 10min, average frost crystal high only 0. 0108mm, exhibit excellent anti-icing effect.

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Classifications
International ClassificationC23C22/34, C23F1/30, C23F1/20
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