CN102691089A - Electrochemical method for preparing superhydrophobic surface on copper substrates by using aqueous electrolyte - Google Patents
Electrochemical method for preparing superhydrophobic surface on copper substrates by using aqueous electrolyte Download PDFInfo
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Abstract
The invention discloses an electrochemical method for preparing a superhydrophobic surface on copper substrates by using an aqueous electrolyte. The method comprises the steps of: I, dissolving potassium hydroxide and potassium peroxydisulfate into distilled water to obtain a solution A; II, dissolving tetradecanoic acid into anhydrous ethanol to obtain a solution B; III, polishing the two copper substrates by using waterproof abrasive paper, then cleanly washing the two copper substrates by sequentially using the distilled water and the anhydrous ethanol, and drying for later use; IV, placing the solution A, as an electrolyte, into an electrolytic cell, and utilizing the two dried copper substrates as an anode and a cathode respectively to electrolyze; and V, cleanly washing the electrolyzed anode copper substrate by sequentially using the distilled water and the anhydrous ethanol, then uniformly smearing the solution B to a surface of the cleanly washed anode copper substrate, and airing to obtain the copper substrates with the super-hydrophobic surface. A contact angle of the super-hydrophobic surface prepared on the copper substrates by using the method can reach more than 152 degrees, and the super-hydrophobic performance keeps stable after the copper substrates are placed in a normal condition for one year.
Description
Technical field
The invention belongs to the material technology field, be specifically related to a kind of electrochemical method that adopts water electrolysis liquid on the copper matrix, to prepare super hydrophobic surface.
Background technology
Natural a lot of plant for example lotus leaf has all been showed extraordinary ultra-hydrophobicity, and its contact angle is up to being lower than 3 ° with roll angle more than 150 °.Excited by this, the researcher has carried out the research of superhydrophobic characteristic, and this direction has developed into a research hot issue of Surface Science at present.The result finds that superhydrophobic characteristic depends primarily on chemical constitution and microtexture, generally is employed in to modify the low surface energy material on the uneven surface or make up coarse structure on the super hydrophobic material surface to make up ultraphobic surface.At present; The preparation method who forms has mainly contained galvanic deposit, chemical vapour deposition, plasma etching, anodic oxidation, chemical corrosion, laser treatment, electric spinning, collosol and gel or the like; Yet; Also there are some shortcomings in these methods, and for example expensive material, complicated technology controlling and process and needs use template, and these have all seriously hindered its large-scale application in engineering.Therefore, adopt a kind of efficient, inexpensive, method is constructed suitable coarse surface tissue simply and easily, in the application of industrial big scale, has tangible application prospect.
Summary of the invention
Technical problem to be solved by this invention is the deficiency to above-mentioned prior art; Provide a kind of method simple; Preparation time is short, and cost is low, is easy to realize that employing water electrolysis liquid that the suitability for industrialized production of big scale requires prepares the electrochemical method of super hydrophobic surface on the copper matrix.Adopt the copper sulfate that this method prepares on the copper matrix and the super hydrophobic surface of TETRADECONIC ACID copper micro, contact angle can reach more than 152 °.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of electrochemical method that adopts water electrolysis liquid on the copper matrix, to prepare super hydrophobic surface is characterized in that this method may further comprise the steps:
Step 1, Pottasium Hydroxide and Potassium Persulphate are dissolved in the zero(ppm) water, obtain solution A after stirring; The concentration of Pottasium Hydroxide is 0.03mol/L～0.2mol/L in the said solution A, and the concentration of Potassium Persulphate is 0.035mol/L～0.1mol/L;
Step 2, TETRADECONIC ACID is dissolved in the absolute ethyl alcohol, obtains solution B after stirring; The concentration of TETRADECONIC ACID is 0.01mol/L～0.4mol/L in the said solution B;
Step 3, two copper matrixes are used liquid honing, to remove the zone of oxidation of copper matrix surface, two copper matrixes after will polishing are then rinsed well with zero(ppm) water and absolute ethyl alcohol successively, dry up for use;
Step 4, place electrolyzer as electrolytic solution solution A described in the step 1; Two copper matrixes after drying up in the step 3 are connected with the positive and negative electrode of direct supply with negative electrode as anode respectively; And to regulate two copper matrixes be 25mm～35mm over against the distance between parallel placement and the two copper matrixes; Opening direct supply, is electrolysis 5s～120s under the condition of 5V～15V at voltage;
Step 5, the anode copper matrix after electrolysis in the step 4 is rinsed well with zero(ppm) water and absolute ethyl alcohol successively; Then solution B described in the step 2 evenly is applied in the anode copper matrix surface after rinsing well; Dry, obtain having the copper matrix that surface contact angle reaches the super hydrophobic surface more than 152 °.
Above-mentioned employing water electrolysis liquid prepares the electrochemical method of super hydrophobic surface on the copper matrix, described in the step 1 in the solution A concentration of Pottasium Hydroxide be 0.1mol/L.
Above-mentioned employing water electrolysis liquid prepares the electrochemical method of super hydrophobic surface on the copper matrix, described in the step 1 in the solution A concentration of Potassium Persulphate be 0.05mol/L.
Above-mentioned employing water electrolysis liquid prepares the electrochemical method of super hydrophobic surface on the copper matrix, described in the step 2 in the solution B concentration of TETRADECONIC ACID be 0.1mol/L.
Above-mentioned employing water electrolysis liquid prepares the electrochemical method of super hydrophobic surface on the copper matrix, the distance between two copper matrixes described in the step 4 is 30mm.
The present invention compared with prior art has the following advantages:
1, method of the present invention is simple, and preparation time is short, and cost is low, and efficient is high, and the present invention adopts the solvent of zero(ppm) water as electrolytic solution, and is than adopting other reagent (like absolute ethyl alcohol) more economically, convenient; In addition, adopt the solvent of zero(ppm) water as electrolytic solution, required voltage is low in the electrolytic process, operates safer.
2, the present invention has broken through the restriction that in the past needs acid electrolyte, in basic soln, constructs the super hydrophobic surface of copper sulfate and TETRADECONIC ACID copper micro first, is easy to realize the low-cost industrial production requirement of big scale.
3, method of the present invention is than quicker based on the electrochemical method of absolute ethyl alcohol electrolytic solution, and electrolysis 5s～120s gets final product.
4, adopt the copper sulfate that method of the present invention prepares and the super hydrophobic surface of TETRADECONIC ACID copper micro on the copper matrix, contact angle can reach more than 152 °, and the normal condition held after 1 year ultra-hydrophobicity keep stable.
Below in conjunction with accompanying drawing and embodiment technical scheme of the present invention is done further detailed description.Figure of description
Fig. 1 is the sem photograph of the super hydrophobic surface of the embodiment of the invention 2 preparations.
Fig. 2 is the sem photograph of the super hydrophobic surface of the embodiment of the invention 5 preparations.
Embodiment
Embodiment 1
Step 1, with 0.56g Pottasium Hydroxide and 1.35g Potassium Persulphate powder dissolution in zero(ppm) water, be settled to 100mL, obtaining concentration of potassium hydroxide after stirring is 0.1mol/L, Potassium Persulphate concentration is the solution A of 0.05mol/L;
Step 2, the TETRADECONIC ACID of 2.28g is dissolved in the absolute ethyl alcohol, is settled to 100mL, obtain the solution B that TETRADECONIC ACID concentration is 0.1mol/L after stirring;
Step 3, be that the copper matrix of 50mm * 25mm * 1.5mm is used liquid honing with two piece sizes, to remove the zone of oxidation of copper matrix surface, two copper matrixes after will polishing are then rinsed well with zero(ppm) water and absolute ethyl alcohol successively, dry up for use;
Step 4, place electrolyzer as electrolytic solution solution A described in the step 1; Two copper matrixes after drying up in the step 3 are inserted in the electrolytic solution; And be connected with the positive and negative electrode of direct supply with negative electrode as anode respectively; Regulating two copper matrixes is 30mm over against the distance between parallel placement and the two copper matrixes, opens direct supply, is electrolysis 20s under the condition of 5V at voltage;
Step 5, the anode copper matrix after electrolysis in the step 4 is rinsed well with zero(ppm) water and absolute ethyl alcohol successively; Then solution B described in the step 2 evenly is applied in the anode copper matrix surface after rinsing well; Dry, obtain having the copper matrix of super hydrophobic surface.
Embodiment 2
Step 1, with 0.56g Pottasium Hydroxide and 1.35g Potassium Persulphate powder dissolution in zero(ppm) water, be settled to 100mL, obtaining concentration of potassium hydroxide after stirring is 0.1mol/L, Potassium Persulphate concentration is the solution A of 0.05mol/L;
Step 2, the TETRADECONIC ACID of 2.28g is dissolved in the absolute ethyl alcohol, is settled to 100mL, obtain the solution B that TETRADECONIC ACID concentration is 0.1mol/L after stirring;
Step 3, be that the copper matrix of 50mm * 25mm * 1.5mm is used liquid honing with two piece sizes, to remove the zone of oxidation of copper matrix surface, two copper matrixes after will polishing are then rinsed well with zero(ppm) water and absolute ethyl alcohol successively, dry up for use;
Step 4, place electrolyzer as electrolytic solution solution A described in the step 1; Two copper matrixes after drying up in the step 3 are inserted in the electrolytic solution; And be connected with the positive and negative electrode of direct supply with negative electrode as anode respectively; Regulating two copper matrixes is 30mm over against the distance between parallel placement and the two copper matrixes, opens direct supply, is electrolysis 50s under the condition of 5V at voltage;
Step 5, the anode copper matrix after electrolysis in the step 4 is rinsed well with zero(ppm) water and absolute ethyl alcohol successively; Then solution B described in the step 2 evenly is applied in the anode copper matrix surface after rinsing well; Dry, obtain having the copper matrix of super hydrophobic surface.
Fig. 1 is the sem photograph of the super hydrophobic surface of present embodiment preparation; As can be seen from the figure; Stochastic distribution sparse tiny flocculent structure on substrate surface, the coarse structure of these floccule mass bunch complicacy of formation, and this has greatly increased the ability of stored air.This structure combines with the TETRADECONIC ACID of low surface energy, thereby has realized the ultra-hydrophobicity of copper matrix surface.
Embodiment 3
Step 1, with 0.168g Pottasium Hydroxide and 2.7g Potassium Persulphate powder dissolution in zero(ppm) water, be settled to 100mL, obtaining concentration of potassium hydroxide after stirring is 0.03mol/L, Potassium Persulphate concentration is the solution A of 0.1mol/L;
In step 2, the TETRADECONIC ACID adding absolute ethyl alcohol, be settled to 100mL, obtain the solution B that TETRADECONIC ACID concentration is 0.01mol/L after stirring 0.228g;
Step 3, be that the copper matrix of 50mm * 25mm * 1.5mm is used liquid honing with two piece sizes, to remove the zone of oxidation of copper matrix surface, two copper matrixes after will polishing are then rinsed well with zero(ppm) water and absolute ethyl alcohol successively, dry up for use;
Step 4, place electrolyzer as electrolytic solution solution A described in the step 1; Two copper matrixes after drying up in the step 3 are inserted in the electrolytic solution; And be connected with the positive and negative electrode of direct supply with negative electrode as anode respectively; Regulating two copper matrixes is 25mm over against the distance between parallel placement and the two copper matrixes, opens direct supply, is electrolysis 90s under the condition of 5V at voltage;
Step 5, the anode copper matrix after electrolysis in the step 4 is rinsed well with zero(ppm) water and absolute ethyl alcohol successively; Then solution B described in the step 2 evenly is applied in the anode copper matrix surface after rinsing well; Dry, obtain having the copper matrix of super hydrophobic surface.
Embodiment 4
Step 1, with 1.12g Pottasium Hydroxide and 0.945g Potassium Persulphate powder dissolution in zero(ppm) water, be settled to 100mL, obtaining concentration of potassium hydroxide after stirring is 0.2mol/L, Potassium Persulphate concentration is the solution A of 0.035mol/L;
In step 2, the TETRADECONIC ACID adding absolute ethyl alcohol, be settled to 100mL, obtain the solution B that TETRADECONIC ACID concentration is 0.4mol/L after stirring 9.12g;
Step 3, be that the copper matrix of 50mm * 25mm * 1.5mm is used liquid honing with two piece sizes, to remove the zone of oxidation of copper matrix surface, two copper matrixes after will polishing are then rinsed well with zero(ppm) water and absolute ethyl alcohol successively, dry up for use;
Step 4, place electrolyzer as electrolytic solution solution A described in the step 1; Two copper matrixes after drying up in the step 3 are inserted in the electrolytic solution; And be connected with the positive and negative electrode of direct supply with negative electrode as anode respectively; Regulating two copper matrixes is 35mm over against the distance between parallel placement and the two copper matrixes, opens direct supply, is electrolysis 120s under the condition of 5V at voltage;
Step 5, the anode copper matrix after electrolysis in the step 4 is rinsed well with zero(ppm) water and absolute ethyl alcohol successively; Then solution B described in the step 2 evenly is applied in the anode copper matrix surface after rinsing well; Dry, obtain having the copper matrix of super hydrophobic surface.
Embodiment 5
Step 1, with 0.56g Pottasium Hydroxide and 1.35g Potassium Persulphate powder dissolution in zero(ppm) water, be settled to 100mL, obtaining concentration of potassium hydroxide after stirring is 0.1mol/L, Potassium Persulphate concentration is the solution A of 0.05mol/L;
Step 2, the TETRADECONIC ACID of 2.28g is dissolved in the absolute ethyl alcohol, is settled to 100mL, obtain the solution B that TETRADECONIC ACID concentration is 0.1mol/L after stirring;
Step 3, be that the copper matrix of 50mm * 25mm * 1.5mm is used liquid honing with two piece sizes, to remove the zone of oxidation of copper matrix surface, two copper matrixes after will polishing are then rinsed well with zero(ppm) water and absolute ethyl alcohol successively, dry up for use;
Step 4, place electrolyzer as electrolytic solution solution A described in the step 1; Two copper matrixes after drying up in the step 3 are inserted in the electrolytic solution; And be connected with the positive and negative electrode of direct supply with negative electrode as anode respectively; Regulating two copper matrixes is 30mm over against the distance between parallel placement and the two copper matrixes, opens direct supply, is electrolysis 5s under the condition of 10V at voltage;
Step 5, the anode copper matrix after electrolysis in the step 4 is rinsed well with zero(ppm) water and absolute ethyl alcohol successively; Then solution B described in the step 2 evenly is applied in the anode copper matrix surface after rinsing well; Dry, obtain having the copper matrix of super hydrophobic surface.
Fig. 2 is the sem photograph of the super hydrophobic surface of present embodiment preparation, and as can be seen from the figure, its microtexture is too smooth, and this structure has increased water droplet and copper coin surface contact area, also makes its hydrophobic performance descend greatly.Yet this structure further combines with the TETRADECONIC ACID of low surface energy, has also realized the ultra-hydrophobicity of copper matrix surface.
Embodiment 6
Step 1, with 0.28g Pottasium Hydroxide and 2.16g Potassium Persulphate powder dissolution in zero(ppm) water, be settled to 100mL, obtaining concentration of potassium hydroxide after stirring is 0.05mol/L, Potassium Persulphate concentration is the solution A of 0.08mol/L;
In step 2, the TETRADECONIC ACID adding absolute ethyl alcohol, be settled to 100mL, obtain the solution B that TETRADECONIC ACID concentration is 0.2mol/L after stirring 4.56g;
Step 3, be that the copper matrix of 50mm * 25mm * 1.5mm is used liquid honing with two piece sizes, to remove the zone of oxidation of copper matrix surface, two copper matrixes after will polishing are then rinsed well with zero(ppm) water and absolute ethyl alcohol successively, dry up for use;
Step 4, place electrolyzer as electrolytic solution solution A described in the step 1; Two copper matrixes after drying up in the step 3 are inserted in the electrolytic solution; And be connected with the positive and negative electrode of direct supply with negative electrode as anode respectively; Regulating two copper matrixes is 35mm over against the distance between parallel placement and the two copper matrixes, opens direct supply, is electrolysis 15s under the condition of 10V at voltage;
Step 5, the anode copper matrix after electrolysis in the step 4 is rinsed well with zero(ppm) water and absolute ethyl alcohol successively; Then solution B described in the step 2 evenly is applied in the anode copper matrix surface after rinsing well; Dry, obtain having the copper matrix of super hydrophobic surface.
Embodiment 7
Step 1, with 0.84g Pottasium Hydroxide and 1.89g Potassium Persulphate powder dissolution in zero(ppm) water, be settled to 100mL, obtaining concentration of potassium hydroxide after stirring is 0.15mol/L, Potassium Persulphate concentration is the solution A of 0.07mol/L;
In step 2, the TETRADECONIC ACID adding absolute ethyl alcohol, be settled to 100mL, obtain the solution B that TETRADECONIC ACID concentration is 0.15mol/L after stirring 3.42g;
Step 3, be that the copper matrix of 50mm * 25mm * 1.5mm is used liquid honing with two piece sizes, to remove the zone of oxidation of copper matrix surface, two copper matrixes after will polishing are then rinsed well with zero(ppm) water and absolute ethyl alcohol successively, dry up for use;
Step 4, place electrolyzer as electrolytic solution solution A described in the step 1; Two copper matrixes after drying up in the step 3 are inserted in the electrolytic solution; And be connected with the positive and negative electrode of direct supply with negative electrode as anode respectively; Regulating two copper matrixes is 28mm over against the distance between parallel placement and the two copper matrixes, opens direct supply, is electrolysis 5s under the condition of 15V at voltage;
Step 5, the anode copper matrix after electrolysis in the step 4 is rinsed well with zero(ppm) water and absolute ethyl alcohol successively; Then solution B described in the step 2 evenly is applied in the anode copper matrix surface after rinsing well; Dry, obtain having the copper matrix of super hydrophobic surface.
The copper matrix with super hydrophobic surface to the embodiment of the invention 1 to embodiment 7 preparation carries out contact angle detection, and the result sees the following form:
The contact angle of the copper matrix with super hydrophobic surface of table 1 embodiment 1 to embodiment 7 preparation
| Sample | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 |
| Contact angle (°) | 158 | 165 | 161 | 159 | 152 | 158 | 158 |
Can find out from table 1; Adopt method of the present invention on the copper matrix, to prepare super hydrophobic surface; The contact angle on surface reaches more than 152 °, has greatly reduced the contact area of drop and matrix surface, thereby has further improved the performance such as not sticking, antifouling and anticorrosion of super hydrophobic surface.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any restriction, every technical spirit changes any simple modification, change and the equivalent structure that above embodiment did according to the present invention, all still belongs in the protection domain of technical scheme of the present invention.
Claims (5)
1. electrochemical method that adopts water electrolysis liquid on the copper matrix, to prepare super hydrophobic surface is characterized in that this method may further comprise the steps:
Step 1, Pottasium Hydroxide and Potassium Persulphate are dissolved in the zero(ppm) water, obtain solution A after stirring; The concentration of Pottasium Hydroxide is 0.03mol/L～0.2mol/L in the said solution A, and the concentration of Potassium Persulphate is 0.035mol/L～0.1mol/L;
Step 2, TETRADECONIC ACID is dissolved in the absolute ethyl alcohol, obtains solution B after stirring; The concentration of TETRADECONIC ACID is 0.01mol/L～0.4mol/L in the said solution B;
Step 3, two copper matrixes are used liquid honing, to remove the zone of oxidation of copper matrix surface, two copper matrixes after will polishing are then rinsed well with zero(ppm) water and absolute ethyl alcohol successively, dry up for use;
Step 4, place electrolyzer as electrolytic solution solution A described in the step 1; Two copper matrixes after drying up in the step 3 are connected with the positive and negative electrode of direct supply with negative electrode as anode respectively; And to regulate two copper matrixes be 25mm～35mm over against the distance between parallel placement and the two copper matrixes; Opening direct supply, is electrolysis 5s～120s under the condition of 5V～15V at voltage;
Step 5, the anode copper matrix after electrolysis in the step 4 is rinsed well with zero(ppm) water and absolute ethyl alcohol successively; Then solution B described in the step 2 evenly is applied in the anode copper matrix surface after rinsing well; Dry, obtain having the copper matrix that surface contact angle reaches the super hydrophobic surface more than 152 °.
2. employing water electrolysis liquid according to claim 1 prepares the electrochemical method of super hydrophobic surface on the copper matrix, it is characterized in that, described in the step 1 in the solution A concentration of Pottasium Hydroxide be 0.1mol/L.
3. employing water electrolysis liquid according to claim 1 prepares the electrochemical method of super hydrophobic surface on the copper matrix, it is characterized in that, described in the step 1 in the solution A concentration of Potassium Persulphate be 0.05mol/L.
4. employing water electrolysis liquid according to claim 1 prepares the electrochemical method of super hydrophobic surface on the copper matrix, it is characterized in that, described in the step 2 in the solution B concentration of TETRADECONIC ACID be 0.1mol/L.
5. employing water electrolysis liquid according to claim 1 prepares the electrochemical method of super hydrophobic surface on the copper matrix, it is characterized in that, the distance between two copper matrixes described in the step 4 is 30mm.
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| CN107779848A (en) * | 2017-09-22 | 2018-03-09 | 浙江海洋大学 | It is a kind of to prepare super-hydrophobic and oleophobic surface method by replacing reaction on steel matrix surface |
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| CN102943246A (en) * | 2012-11-26 | 2013-02-27 | 四川材料与工艺研究所 | Method for preparing metal surface super-hydrophobicity aluminum coating |
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| CN105568327A (en) * | 2015-12-18 | 2016-05-11 | 西安科技大学 | Electrochemical method for preparing super-hydrophobic surface of copper dendritic crystal |
| CN105568327B (en) * | 2015-12-18 | 2018-06-29 | 西安科技大学 | A kind of electrochemical method for preparing copper dendrite super hydrophobic surface |
| CN107779848A (en) * | 2017-09-22 | 2018-03-09 | 浙江海洋大学 | It is a kind of to prepare super-hydrophobic and oleophobic surface method by replacing reaction on steel matrix surface |
| CN111218712A (en) * | 2020-01-09 | 2020-06-02 | 大连理工大学 | Preparation method of super-hydrophobic surface of electrolytic copper matrix |
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