CN103966643A - Method for preparing titanium-alloy super-hydrophobic surface with low roughness - Google Patents
Method for preparing titanium-alloy super-hydrophobic surface with low roughness Download PDFInfo
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Abstract
The invention provides a method for preparing a super-hydrophobic surface with low roughness on titanium alloy, belongs to the field of surface treatment on metal materials, and relates to a technical method for preparing a titanium-alloy super-hydrophobic surface by adopting electrochemical anodic oxidation in an alkaline solution. The titanium-alloy super-hydrophobic surface with the low roughness is prepared by the adoption of the electrochemical anodic oxidation in the alkaline solution, and the method comprises the following steps: adopting metallographic abrasive paper to polish the titanium alloy; putting the polished titanium alloy into acetone, ethanol and deionized water respectively for ultrasonic cleaning in order to eliminate oil stain; placing a titanium-alloy plate adopted as the anode and a graphite plate adopted as the cathode in parallel symmetrically, and connecting the titanium-alloy plate, which is connected with the positive pole, and the graphite plate, which is connected with the negative pole, with a direct current supply through conducting wires respectively; conducting anodic oxidation; after the anodic oxidation, putting the titanium alloy into the deionized water for ultrasonic cleaning. The method is economical, high-efficient, simple in technology and good in controllability; particularly, the prepared super-hydrophobic surface is low in roughness.
Description
Technical field
The invention belongs to metal material surface process field, particularly a kind of processing method of utilizing electrochemical anodic oxidation to prepare titanium alloy super-hydrophobic surface in basic solution.
Background technology
Super hydrophobic surface refers to the contact angle of water droplet and is greater than 150 °, and the surface that roll angle is less than 10 ° has the characteristics such as automatically cleaning, anticorrosive, freezing, current drag reduction.Super hydrophobic surface is applied on metallic substance, can play antifouling, antirust, anti-freeze effect; Be applied to ships shell or inner-walls of duct, can effectively reduce the friction resistance between current.That titanium alloy has is lightweight, intensity is high, the characteristic such as high temperature resistant, corrosion-resistant, in many industry such as aviation, chemical industry, transport, navigation, has very important application.Therefore, superhydrophobic characteristic is combined with titanium alloy self character, preparing titanium alloy super-hydrophobic surface has meaning of crucial importance.
At present, on metallic matrix, super hydrophobic surface is main by the micro-nano coarse structure of first structured surface, then modifies to prepare with low surface energy material.With regard to titanium or titanium alloy, conventionally prepare surface roughness by chemical process or electrochemical method, low surface energy falls in conventional silicon fluoride, stearic acid, palmitinic acid, lauric acid etc.Chemical process builds coarse structure with acid corrosion titanium alloy or by electroless plating conventionally, and then low surface energy material is modified and prepared super hydrophobic surface.The advantage of chemical process is not need special instruments and equipment, and method is simple.But because chemical corrosion is relevant with crystal formation, limited by lattice, and electroless plating is relevant to material surface activity, therefore the method is tighter to the restriction of material, and reaction controllability is poor.Electrochemical method is generally to prepare coarse structure by anode etching or anodic oxidation, and then low surface energy material is modified and prepared super hydrophobic surface.The advantage of electrochemical method is to be subject to materials limitations less, be easy to produce nano level coarse structure, and controllability is better.But because the inhomogeneous surface roughness Ra that easily causes of anode etching is larger, general roughness Ra is about 1～3 μ m.Anodic oxidation is carried out conventionally in acidic solution or organic solvent, and need to the longer reaction times.A kind of in NaCl or NaBr solution, titanium or titanium alloy carried out to anode etching and build micro-nano coarse structure as China Patent No. CN102618913A discloses, silicon fluoride makes the method for super hydrophobic surface after modifying, the method efficiency is higher, but because the inhomogeneous surfaceness that easily causes of anode etching is larger; The people such as Zhang are at F.Zhang, S.Chen, L.Dong, Y.Lei, T.Liu, Y.Yin, Appl.Surf.Sci.2011,257, in 2587, first pure titanium is put into the ethylene glycol solution that contains Neutral ammonium fluoride and carried out anodic oxidation in 5 hours, then modify to make super-hydrophobic titanium surface with low surface energy material, the method long processing time, efficiency is lower; The people such as Lin are at Y.K.Lai, C.J.Lin, J.Y.Huang, H.F.Zhuang, L.Sun, T.Nguyen, Langmuir.2008, in 24,3867, utilize electrochemistry anodic oxidation to prepare super-hydrophobic titanium surface, using platinum as negative electrode, hydrofluoric acid is electrolytic solution, because platinum is noble metal, makes the method cost higher.
Summary of the invention
The present invention is for overcoming the deficiencies in the prior art, invent a kind of method of preparing the titanium alloy super-hydrophobic surface of low roughness by anodic oxidation, the method is first in alkaline electrolyte, to construct on titanium alloy surface micron-sized pore space structure by electrochemical anodic oxidation, and recycling low surface energy material modifies to make super hydrophobic surface.This invention is simple, economical and efficient.
The technical solution used in the present invention is a kind of preparation method of titanium alloy super-hydrophobic surface of low roughness, it is characterized in that, preparation method prepares the titanium alloy super-hydrophobic surface of low roughness by electrochemical anodic oxidation in basic solution, the concrete steps of method are as follows:
1) titanium alloy sheet 3 and graphite cake 7 are all cut into 20mm × 30mm, but actual working (finishing) area is 20mm × 20mm, remainder is as clamping and conduction; Put into respectively acetone, ethanol, deionized water for ultrasonic cleaning 3min first with #1500 abrasive paper for metallograph polishing titanium alloy, then by the titanium alloy after polishing, to remove degreasing;
2) using as the titanium alloy sheet 3 of anode with as the graphite cake 7 of negative electrode, Parallel Symmetric is placed, and is connected with direct supply 1 by wire respectively, and titanium alloy connects positive pole, and graphite connects negative pole; Then negative electrode and anode are put into the alkaline electrolyte 4 being made up of NaOH and H2O2 jointly, carry out anodic oxidation 30～60min by 10～15V constant voltage, after oxidation finishes, titanium alloy is put into deionized water for ultrasonic and clean, dry up stand-by;
3) oxidized titanium alloy is put into the silicon fluoride ethanolic soln that the massfraction that configures is 1% and soaked 2h; After taking-up, put into 120 DEG C of baking ovens and toast 20min, cool to room temperature, obtains having the titanium alloy super-hydrophobic surface of low roughness.
The invention has the beneficial effects as follows and adopt NaOH and H2O2 to be general chemistry reagent, and only need just can obtain for 30 minutes the needed micro-rough structure of super hydrophobic surface; The super hydrophobic surface of preparation has the hydrophobic performance that low roughness is become reconciled, and roughness Ra is only 0.669 μ m, is 158.5 ° to the contact angle of water droplet, and roll angle is 5.3 °.Processing method is simple, without complicated processing instrument and operation steps, and suitable big area preparation, economical and efficient.
Brief description of the drawings
Fig. 1 is processing unit (plant) schematic diagram.Wherein: 1-direct supply, 2-grip device, 3-titanium alloy sheet, 4-electrolytic solution, 5-magnetic stirring apparatus, 6-stirring rotator, 7-graphite cake, 8-container.
Fig. 2 is the titanium alloy super-hydrophobic surface that the makes schematic diagram to water droplet wettability.θ and β are respectively contact angle and the roll angle of titanium alloy super-hydrophobic surface to water droplet, 1-water droplet, the super-hydrophobic titanium alloy sheet of 2-
Fig. 3 is that the titanium alloy super-hydrophobic surface that embodiment 1 makes amplifies the scanning electron microscope (SEM) photograph of 5000 times.
Embodiment
Describe specific embodiment of the invention in detail below in conjunction with technical scheme and accompanying drawing.As shown in Figure 1, titanium alloy sheet 3 is parallel with graphite cake 7 just to placing, and is fixed on grip device 2 for the required processing unit (plant) of this embodiment.Titanium alloy sheet 3 and graphite cake 7 are connected on the positive pole and negative pole of direct supply 1 by wire respectively.The effect of magnetic stirring apparatus 5 is to make the electrolytic solution in reaction more even.Titanium alloy super-hydrophobic surface to the wettability of water droplet as shown in Figure 2,5 μ L water droplets 1 are dropped on the super-hydrophobic titanium alloy sheet 2 of horizontal positioned at random, water droplet is similar to spherical, θ is the contact angle of this super hydrophobic surface to water droplet, roll angle β when making water droplet start to roll, the minimum angles of the required inclination of super-hydrophobic titanium alloy sheet 2 plate.
Embodiment 1
1) titanium alloy (Ti-6Al-4V) plate and graphite cake are all cut into 20mm × 30mm, but actual working (finishing) area is 20mm × 20mm, remainder is as clamping and conduction.Before processing, first use 1500# sand papering titanium alloy sheet, then clean 3min, wipe oil in acetone, ethanol, deionized water for ultrasonic successively.
2) by titanium alloy sheet, with graphite cake, parallel just to placing, interval 15mm, joins two plates and direct supply with wire, and titanium alloy sheet connects positive pole, and graphite cake connects negative pole.Two plates are put into and filled the NaOH of 1.5mol/L and the H2O2 mixing solutions of 0.15mol/L simultaneously, open magnetic stirring apparatus (1000r/min), connect direct supply, voltage is fixed on 10V.Oxidization time is 30min, adds man-hour solution temperature and is about room temperature (25 DEG C).
3) after machining, first titanium alloy sheet is put into deionized water for ultrasonic and cleaned 3min, dry up.The silicon fluoride ethanolic soln that exemplar to be put into the massfraction that configures be 1% again soaks 2h, finally exemplar is put into baking oven, at 120 DEG C, dries 20min.Take out exemplar cool to room temperature, can obtain titanium alloy super-hydrophobic surface.
As shown in Figure 3, surface is the pore space structure of random distribution to the electron scanning micrograph on titanium alloy super-hydrophobic surface, and pore size is 5～10 μ m.This super hydrophobic surface roughness Ra is only 0.669 μ m, and shown in accompanying drawing 2, can record this super hydrophobic surface is 158.5 ° to the contact angle of water droplet, and roll angle is 5.3 °.
Embodiment 2
Operation and the step of pressing embodiment 1, change oxidization time into 60min.The titanium alloy super-hydrophobic surface microscopic appearance obtaining, without considerable change, is pore space structure, and pore size is also 5～10 μ m.This super hydrophobic surface roughness Ra is 0.822 μ m, is 158.8 ° to the contact angle of water droplet, and roll angle is 5.1 °.
Embodiment 3
Operation and the step of pressing embodiment 1, change constant voltage into 15V.The titanium alloy super-hydrophobic surface obtaining is still the pore space structure of random distribution, and hole size is 5～10 μ m.This super hydrophobic surface roughness Ra is 0.785 μ m, is 157.8 ° to the contact angle of water droplet, and roll angle is 5.6 °.
Claims (1)
1. a preparation method for the titanium alloy super-hydrophobic surface of low roughness, is characterized in that, preparation method prepares the titanium alloy super-hydrophobic surface of low roughness by electrochemical anodic oxidation in basic solution, and the concrete steps of method are as follows:
1) titanium alloy sheet (3) and graphite cake (7) are all cut into 20mm × 30mm, but actual working (finishing) area is 20mm × 20mm, remainder is as clamping and conduction; Put into respectively acetone, ethanol, deionized water for ultrasonic cleaning 3min first with #1500 abrasive paper for metallograph polishing titanium alloy, then by the titanium alloy after polishing, to remove degreasing;
2) using as the titanium alloy sheet (3) of anode with as the graphite cake (7) of negative electrode, Parallel Symmetric is placed, and is connected with direct supply (1) by wire respectively, and titanium alloy connects positive pole, and graphite connects negative pole; Then negative electrode and anode are put into the alkaline electrolyte (4) being made up of NaOH and H2O2 jointly, carry out anodic oxidation 30～60min by 10～15V constant voltage, after oxidation finishes, titanium alloy is put into deionized water for ultrasonic and clean, dry up stand-by;
3) oxidized titanium alloy is put into the silicon fluoride ethanolic soln that the massfraction that configures is 1% and soaked 2h; After taking-up, put into 120 DEG C of baking ovens and toast 20min, cool to room temperature, obtains having the titanium alloy super-hydrophobic surface of low roughness.
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Cited By (14)
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| CN105063738A (en) * | 2015-07-29 | 2015-11-18 | 大连理工大学 | Preparation method of durable underwater ultra oleophobic surface of titanium alloy matrix |
| CN105582852A (en) * | 2016-03-28 | 2016-05-18 | 四川大学 | Wet-process rolling granulation method |
| CN105671951A (en) * | 2016-01-26 | 2016-06-15 | 苏州榕绿纳米科技有限公司 | Method for controlling wettability of substrate surface |
| CN105696055A (en) * | 2016-01-29 | 2016-06-22 | 东华大学 | Preparation method of titanium alloy self-cleaning color layer |
| CN106637316A (en) * | 2016-12-07 | 2017-05-10 | 广东工业大学 | Method for preparing super-hydrophobic surface on titanium substrate |
| CN106802095A (en) * | 2017-01-20 | 2017-06-06 | 中国石油大学(华东) | A kind of microchannel cooling |
| WO2017161920A1 (en) * | 2016-03-22 | 2017-09-28 | 苏州蓝锐纳米科技有限公司 | Aircraft wing provided with nanolayer having spontaneous condensate drop propelling function |
| CN107287640A (en) * | 2017-06-29 | 2017-10-24 | 北京石油化工学院 | A kind of preparation method of arc differential oxide ceramic layer nano surface graphite super-hydrophobic coat |
| CN108486633A (en) * | 2018-06-29 | 2018-09-04 | 四川大学 | It is a kind of that there is hydrophobic and superhydrophobic characteristic titanium or titanium alloy surface and preparation method |
| CN109056030A (en) * | 2018-08-23 | 2018-12-21 | 北方工业大学 | Super-hydrophobic titanium dioxide nanotube array film and preparation method thereof |
| US10453584B2 (en) | 2016-10-27 | 2019-10-22 | International Business Machines Corporation | Hydrophobic, conductive organic materials for metallic surfaces |
| CN110565145A (en) * | 2019-09-05 | 2019-12-13 | 华南理工大学 | Pure titanium surface super-hydrophobic anodic oxidation coloring film and preparation method and application thereof |
| CN113430486A (en) * | 2021-06-22 | 2021-09-24 | 哈尔滨工程大学 | Liquid phase plasma electrolytic infiltration device and method |
| CN114752990A (en) * | 2022-03-26 | 2022-07-15 | 四川轻化工大学 | Metal-based nest type micro-structure super-hydrophobic surface and preparation method and application thereof |
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| CN105063738A (en) * | 2015-07-29 | 2015-11-18 | 大连理工大学 | Preparation method of durable underwater ultra oleophobic surface of titanium alloy matrix |
| CN105671951A (en) * | 2016-01-26 | 2016-06-15 | 苏州榕绿纳米科技有限公司 | Method for controlling wettability of substrate surface |
| CN105696055A (en) * | 2016-01-29 | 2016-06-22 | 东华大学 | Preparation method of titanium alloy self-cleaning color layer |
| WO2017161920A1 (en) * | 2016-03-22 | 2017-09-28 | 苏州蓝锐纳米科技有限公司 | Aircraft wing provided with nanolayer having spontaneous condensate drop propelling function |
| CN105582852A (en) * | 2016-03-28 | 2016-05-18 | 四川大学 | Wet-process rolling granulation method |
| CN105582852B (en) * | 2016-03-28 | 2018-05-18 | 四川大学 | A kind of wet method rolls prilling process |
| US10453584B2 (en) | 2016-10-27 | 2019-10-22 | International Business Machines Corporation | Hydrophobic, conductive organic materials for metallic surfaces |
| US11495368B2 (en) | 2016-10-27 | 2022-11-08 | International Business Machines Corporation | Hydrophobic, conductive organic materials for metallic surfaces |
| CN106637316B (en) * | 2016-12-07 | 2018-12-21 | 广东工业大学 | A method of preparing super hydrophobic surface in titanium substrate |
| CN106637316A (en) * | 2016-12-07 | 2017-05-10 | 广东工业大学 | Method for preparing super-hydrophobic surface on titanium substrate |
| CN106802095A (en) * | 2017-01-20 | 2017-06-06 | 中国石油大学(华东) | A kind of microchannel cooling |
| CN107287640A (en) * | 2017-06-29 | 2017-10-24 | 北京石油化工学院 | A kind of preparation method of arc differential oxide ceramic layer nano surface graphite super-hydrophobic coat |
| CN108486633A (en) * | 2018-06-29 | 2018-09-04 | 四川大学 | It is a kind of that there is hydrophobic and superhydrophobic characteristic titanium or titanium alloy surface and preparation method |
| CN109056030A (en) * | 2018-08-23 | 2018-12-21 | 北方工业大学 | Super-hydrophobic titanium dioxide nanotube array film and preparation method thereof |
| CN110565145A (en) * | 2019-09-05 | 2019-12-13 | 华南理工大学 | Pure titanium surface super-hydrophobic anodic oxidation coloring film and preparation method and application thereof |
| CN113430486A (en) * | 2021-06-22 | 2021-09-24 | 哈尔滨工程大学 | Liquid phase plasma electrolytic infiltration device and method |
| CN114752990A (en) * | 2022-03-26 | 2022-07-15 | 四川轻化工大学 | Metal-based nest type micro-structure super-hydrophobic surface and preparation method and application thereof |
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