CN102230169A - Method for constructing super-hydrophobic membrane on surface of copper matrix - Google Patents
Method for constructing super-hydrophobic membrane on surface of copper matrix Download PDFInfo
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Abstract
The invention relates to a method for constructing a super-hydrophobic membrane on the surface of a copper matrix, and relates to a method for constructing a super-hydrophobic membrane, which solves the problems of complex steps of constructing the super-hydrophobic surface and large toxicity of raw materials in the conventional method. In the method, a sliver layer with a micro-nanometer structure is generated by replacement reaction of copper and silver nitrate, a rough surface is constructed on the copper matrix, and a self-assembly membrane is formed on a silver surface by utilizing long-chain carboxylic acid to reduce surface energy. When the method is used, the construction of the rough surface and surface modification are completed in one step, equipment and a process is simple, and the method is easy to operate; and the toxicity of the raw materials is low, and environmental pollution is small. The method is suitable for the large-scale industrial production of the super-hydrophobic membrane.
Description
Technical field
The present invention relates to a kind of method that makes up based superhydrophobic thin films.
Background technology
Super hydrophobic material be meant with water contact angle greater than 150 °, roll angle is less than 5 ° material, is one of focus of Surface Science and membrane science research in recent years.Super hydrophobic material is in daily life, and industrial production is widely used in the national defence, makes up the resistance to corrosion that based superhydrophobic thin films can strengthen metal in the metallic surface.
Super hydrophobic surface has two big indispensable elements: the one, and will there be micro-nano coarse structure on the surface, and the 2nd, surface mass has low surface energy.Usually make up micro-nano coarse structure and the surface is carried out in two steps with the modification of low surface energy material at matrix surface, such as Liu Weimin etc. in " method that on copper surface, prepares super hydrophobic surface " (patent No. CN201010161832.3), earlier place the supersaturation copper-bath to soak 10～15 days metal copper plate, make up coarse structure on the copper surface, carry out finishing with the method that end-vinyl-polydimethylsiloxane is spun to the metal copper plate surface then.The strong grade of beam generation adopts following method to make the matrix roughen in " a kind of method for preparing copper substrate superhydrophobic surface " (patent No. CN200910081996.2): the copper base is immersed in HNO
3Etching is taken out for a moment in the solution, and the water flushing dries up; Evenly spray acetic acid, under the room temperature, relative humidity more than 50%, spray acetic acid once more after drying in the shade, treat to form on the copper primary surface upper layer that spreads all over green spot; With the copper base put into baking oven in 300 ± 50 ℃ down baking take out, place air to cooling, the matrix of roughening is immersed in the ethanolic soln of the ethanolic soln of positive stearylmercaptan or Dodecyl Mercaptan and carries out finishing to reduce surface energy.As can be seen matrix surface roughening and finishing are divided into the method steps very complicated that two steps made up super hydrophobic surface by above two examples, and raw material such as the end-vinyl-polydimethylsiloxane toxicity used are bigger, cost is higher relatively, is unfavorable for large-scale commercial production.
Summary of the invention
The objective of the invention is to make up the bigger problem of material toxicity that the super hydrophobic surface complex steps is complicated and use, the invention provides a kind of method that makes up based superhydrophobic thin films at the copper matrix surface in order to solve existing method.
A kind of method that makes up based superhydrophobic thin films at the copper matrix surface of the present invention, realize by following steps: one, with the copper matrix put into mass concentration be 0.1%～30% hydrochloric acid or mass concentration be above-mentioned two kinds of sour equal-volumes of 0.1%～70% sulfuric acid or two kinds of acid mix soak the oxide compound that 0.2～120min removes the copper matrix surface after, with deionized water the copper matrix is cleaned 1～3 time, and then, obtain cleaning the copper matrix with alcohol flushing 1～3 time; Two, Silver Nitrate is dissolved in methyl alcohol, ethanol or the acetone, obtains solution A; The carboxylic acid that adds backbone c atoms several 9～20 then in solution A makes its dissolving, obtains solution B; In the solution B, the concentration of Silver Nitrate is 1～30mmol/L, and the concentration of carboxylic acid is 1～40mmol/L; Three, the cleaning copper matrix that obtains in the step 1 is put into the solution B that step 2 obtains and soaked 0.5～5min, perhaps the solution B that step 2 is obtained is sprayed on the cleaning copper matrix surface that obtains in the step 1, carry out drying then, 50 ℃～90 ℃ of drying temperatures, 0.5～48h finished at the copper matrix surface and made up based superhydrophobic thin films time of drying.
The present invention generates the silver layer with micro nano structure by the replacement(metathesis)reaction of copper and Silver Nitrate, makes up uneven surface on the copper matrix, utilizes the long-chain carboxylic acid to form self-assembled film to reduce surface energy at silver surface; The based superhydrophobic thin films that makes up at the copper matrix surface has good super-hydrophobicity, and film and matrix bond are good, stable performance.And structure uneven surface and one step of finishing finish, and equipment and technology are simple, easy handling; The use material toxicity is low, and environmental pollution is little.
Description of drawings
Fig. 1 is the contact angle figure of the copper surface super hydrophobic thin film that obtains of embodiment 20.Fig. 2 is that the copper surface super hydrophobic thin film that embodiment 21 obtains amplifies 20000 times SEM figure.
Embodiment
The technology of the present invention method is not limited to following cited embodiment, also comprises the arbitrary combination that each concrete enforcement is seen.
Embodiment one: a kind of method that makes up based superhydrophobic thin films at the copper matrix surface in the present embodiment, realize by following steps: one, putting into mass concentration with the copper matrix is that 0.1%～30% hydrochloric acid or mass concentration are after 0.1%～70% sulfuric acid or above-mentioned two kinds of sour equal-volume blended mixed solutions soak the oxide compound that 0.2～120min removes the copper matrix surface, with deionized water the copper matrix is cleaned 1～3 time, and then, obtain cleaning the copper matrix with alcohol flushing 1～3 time; Two, Silver Nitrate is dissolved in methyl alcohol, ethanol or the acetone, obtains solution A; The carboxylic acid that adds backbone c atoms several 9～20 then in solution A makes its dissolving, obtains solution B; In the solution B, the concentration of Silver Nitrate is 1～30mmol/L, and the concentration of carboxylic acid is 1～40mmol/L; Three, the cleaning copper matrix that obtains in the step 1 is put into the solution B that step 2 obtains and soaked 0.5～5min, perhaps the solution B that step 2 is obtained is sprayed on the cleaning copper matrix surface that obtains in the step 1, carry out drying then, 50 ℃～90 ℃ of drying temperatures, 0.5～48h finished at the copper matrix surface and made up based superhydrophobic thin films time of drying.
The copper matrix is a fine copper or to contain copper mass be copper alloy more than 50% in the present embodiment step 1;
The contained functional group of carboxylic acid is carbochain and a carboxyl in the present embodiment step 2;
Present embodiment makes up uneven surface and one step of finishing finishes, and equipment and technology are simple, easy handling; The use material toxicity is low, and environmental pollution is little.
Embodiment two: what present embodiment and embodiment one were different is that the described hydrochloric acid mass concentration of step 1 is 1%～25%, and h 2 so 4 concentration is 1%～60%, and soak time is 0.5～100min.Other step and parameter are identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is that the described hydrochloric acid mass concentration of step 1 is 10%, and h 2 so 4 concentration is 5%, and soak time is 50min.Other step and parameter are identical with embodiment one.
Embodiment four: what present embodiment and embodiment one to three were different is with deionized water matrix to be cleaned 2 times in the step 1, and then with alcohol flushing 2 times.Other step and parameter are identical with embodiment one to three.
Embodiment five: what present embodiment and embodiment one to four were different is the carboxylic acid that adds backbone c atoms several 10～19 in the step 2.Other step and parameter are identical with embodiment one to four.
Embodiment six: what present embodiment and embodiment one to four were different is the carboxylic acid that adds backbone c atoms several 12 in the step 2.Other step and parameter are identical with embodiment one to four.
Embodiment seven: present embodiment and embodiment one to six are different is that the concentration of Silver Nitrate in the step 2 is 5～25mmol/L.Other step and parameter are identical with embodiment one to six.
Embodiment eight: present embodiment and embodiment one to six are different is that the concentration of Silver Nitrate in the step 2 is 15mmol/L.Other step and parameter are identical with embodiment one to six.
Embodiment nine: present embodiment and embodiment one to eight are different is that the concentration of carboxylic acid in the step 2 is 5～35mmol/L.Other step and parameter are identical with embodiment one to eight.
Embodiment ten: present embodiment and embodiment one to eight are different is that the concentration of carboxylic acid in the step 2 is 20mmol/L.Other step and parameter are identical with embodiment one to eight.
Embodiment 11: what present embodiment and embodiment one to ten were different is to soak 1～4min in the step 3.Other step and parameter are identical with embodiment one to ten.
Embodiment 12: what present embodiment and embodiment one to ten were different is to soak 2min in the step 3.Other step and parameter are identical with embodiment one to ten.
Embodiment 13: present embodiment and embodiment one to 12 are different is 55 ℃～85 ℃ of drying temperatures in the step 3, time of drying 1～40h.Other step and parameter are identical with embodiment one to 12.
Embodiment 14: present embodiment and embodiment one to 12 are different is 60 ℃ of drying temperatures in the step 3, time of drying 20h.Other step and parameter are identical with embodiment one to 12.
Embodiment 15: a kind of method that makes up based superhydrophobic thin films at the copper matrix surface in the present embodiment, realize by following steps: it is after 1% hydrochloric acid soaks 5min that the copper sheet that, will be of a size of 3cm * 3cm * 0.2cm is put into the 500ml mass concentration, with washed with de-ionized water copper sheet 2 times, and then with alcohol flushing 2 times, dry up copper sheet surface ethanol, obtain cleaning copper sheet; Two, 0.1～0.3g Silver Nitrate is put into beaker, add 100ml ethanol, magnetic agitation makes its dissolving, obtains solution A, adds 0.05～0.22g TETRADECONIC ACID in solution A, and magnetic agitation makes the TETRADECONIC ACID dissolving, obtains solution B; Three, the cleaning copper sheet that obtains in the step 1 is put into the solution B that step 2 obtains, soak 0.5～1min, put it into then and carry out drying in the baking oven, 50 ℃～90 ℃ of drying temperatures, 0.5～48h finished on the copper surface and made up based superhydrophobic thin films time of drying.
Embodiment 16: a kind of method that makes up based superhydrophobic thin films at the copper matrix surface in the present embodiment, realize by following steps: it is after 1% hydrochloric acid soaks 5min that the copper sheet that, will be of a size of 3cm * 3cm * 0.2cm is put into the 500ml mass concentration, with washed with de-ionized water copper sheet 2 times, and then with alcohol flushing 2 times, dry up copper sheet surface ethanol, obtain cleaning copper sheet; Two, 0.1～0.3g Silver Nitrate is put into beaker, add 100ml acetone, magnetic agitation makes its dissolving, obtains solution A, adds 0.05～0.1g palmitic acid in solution A, and magnetic agitation makes the palmitic acid dissolving, obtains solution B; Three, the solution B that step 2 is obtained is sprayed on the cleaning copper sheet surface that obtains in the step 1, put it into then to carry out drying in the baking oven, and 50 ℃～90 ℃ of drying temperatures, 0.5～48h finished on the copper surface and made up based superhydrophobic thin films time of drying.
Embodiment 17: a kind of method that makes up based superhydrophobic thin films at the copper matrix surface in the present embodiment, realize by following steps: it is that 10% sulfuric acid soaks 5min and removes the oxide compound on copper sheet surface that the copper sheet that, will be of a size of 3cm * 3cm * 0.2cm is put into the 500ml mass concentration, with deionized water copper sheet is cleaned 2 times then, and then, obtain cleaning copper sheet with alcohol flushing 2 times; Two, 0.1～0.3g Silver Nitrate is dissolved in the methyl alcohol, obtains solution A; In solution A, add 0.05～0.1g, 20 acid then and make its dissolving, obtain solution B; Three, the cleaning copper sheet that obtains in the step 1 is put into the solution B that step 2 obtains and soaked 0.5～1min, perhaps the solution B that step 2 is obtained is sprayed on the cleaning copper sheet surface that obtains in the step 1, carry out drying then, 50 ℃～90 ℃ of drying temperatures, 0.5～48h finished on the copper surface and made up based superhydrophobic thin films time of drying.
Embodiment 18: a kind of method that makes up based superhydrophobic thin films at the copper matrix surface in the present embodiment, realize by following steps: it is that 5% hydrochloric acid and mass concentration are that 10% sulfuric acid equal-volume blended mixed solution soaks 5min and removes the oxide compound on copper sheet surface that the copper sheet that, will be of a size of 3cm * 3cm * 0.2cm is put into the 500ml mass concentration, with deionized water copper sheet is cleaned 2 times, and then, obtain cleaning copper sheet with alcohol flushing 2 times; Two, 0.1～0.3g Silver Nitrate is dissolved in the ethanol, obtains solution A; In solution A, add 0.05～0.1g nonadecanoic acid then and make its dissolving, obtain solution B; Three, the cleaning copper sheet that obtains in the step 1 is put into the solution B that step 2 obtains and soaked 0.5～1min, perhaps the solution B that step 2 is obtained is sprayed on the cleaning copper sheet surface that obtains in the step 1, carry out drying then, 50 ℃～90 ℃ of drying temperatures, 0.5～48h finished on the copper surface and made up based superhydrophobic thin films time of drying.
Embodiment 19: a kind of method that makes up based superhydrophobic thin films at the copper matrix surface in the present embodiment, realize by following steps: it is after 1% hydrochloric acid soaks 5min that the copper sheet that, will be of a size of 3cm * 3cm * 0.2cm is put into the 500ml mass concentration, with washed with de-ionized water copper sheet 2 times, and then with alcohol flushing 2 times, dry up copper sheet surface ethanol, obtain cleaning copper sheet; Two, the 0.17g Silver Nitrate is put into beaker, add 100ml acetone, magnetic agitation makes its dissolving, obtains solution A, adds the 02g lauric acid in solution A, and magnetic agitation makes the lauric acid dissolving, obtains solution B; Three, the cleaning copper sheet that obtains in the step 1 is put into the solution B that step 2 obtains, soak 0.5min, put it into then and carry out drying in the baking oven, 60 ℃ of drying temperatures, 5h finished on the copper surface and made up based superhydrophobic thin films time of drying.
The copper surface super hydrophobic thin film that present embodiment obtains and the contact angle of water are 155 ± 4 °.
Embodiment 20: a kind of method that makes up based superhydrophobic thin films at the copper matrix surface in the present embodiment, realize by following steps: it is after 1% hydrochloric acid soaks 5min that the copper sheet that, will be of a size of 3cm * 3cm * 0.2cm is put into the 500ml mass concentration, with washed with de-ionized water copper sheet 2 times, and then with alcohol flushing 2 times, dry up copper sheet surface ethanol, obtain cleaning copper sheet; Two, the 0.085g Silver Nitrate is put into beaker, add 100ml ethanol, magnetic agitation makes its dissolving, obtains solution A, adds the 0.3g TETRADECONIC ACID in solution A, and magnetic agitation makes the TETRADECONIC ACID dissolving, obtains solution B; Three, the solution B that step 2 is obtained is sprayed on the cleaning copper sheet surface that obtains in the step 1, put it into then to carry out drying in the baking oven, and 70 ℃ of drying temperatures, 3h finished on the copper surface and made up based superhydrophobic thin films time of drying.
The contact angle figure of the copper surface super hydrophobic thin film that obtains in the present embodiment as shown in Figure 1.As can be seen from Figure 1, water droplet is spherical shape on the copper surface, and nearly 160 ℃ of contact angle has good hydrophobicity.
Embodiment 21: a kind of method that makes up based superhydrophobic thin films at the copper matrix surface in the present embodiment, realize by following steps: it is after 1% hydrochloric acid soaks 5min that the copper sheet that, will be of a size of 3cm * 3cm * 0.2cm is put into the 500ml mass concentration, with washed with de-ionized water copper sheet 2 times, and then with alcohol flushing 2 times, dry up copper sheet surface ethanol, obtain cleaning copper sheet; Two, the 0.085g Silver Nitrate is put into beaker, add 100ml methyl alcohol, magnetic agitation makes its dissolving, obtains solution A, adds the 0.2g lauric acid in solution A, and magnetic agitation makes the lauric acid dissolving, obtains solution B; Three, the cleaning copper sheet that obtains in the step 1 is put into the solution B that step 2 obtains, soak 1min, put it into then and carry out drying in the baking oven, 50 ℃ of drying temperatures,, 6h finished on the copper surface and made up based superhydrophobic thin films time of drying.
The SEM figure that the copper surface super hydrophobic thin film amplification that obtains in the present embodiment is 20000 times as shown in Figure 2.Can observe the micro-nano coarse structure on copper surface from Fig. 2.
Claims (8)
1. method that makes up based superhydrophobic thin films at the copper matrix surface, it is characterized in that a kind of method that makes up based superhydrophobic thin films at the copper matrix surface realizes by following steps: after one, putting into mass concentration and be 0.1%～30% hydrochloric acid or mass concentration and be 0.1%～70% sulfuric acid or above-mentioned two kinds of sour equal-volume blended mixed solutions and soaking the oxide compound that 0.2～120min removes the copper matrix surface with the copper matrix, with deionized water the copper matrix is cleaned 1～3 time, and then, obtain cleaning the copper matrix with alcohol flushing 1～3 time; Two, Silver Nitrate is dissolved in methyl alcohol, ethanol or the acetone, obtains solution A; The carboxylic acid that adds backbone c atoms several 9～20 then in solution A makes its dissolving, obtains solution B; In the solution B, the concentration of Silver Nitrate is 1～30mmol/L, and the concentration of carboxylic acid is 1～40mmol/L; Three, the cleaning copper matrix that obtains in the step 1 is put into the solution B that step 2 obtains and soaked 0.5～5min, perhaps the solution B that step 2 is obtained is sprayed on the cleaning copper matrix surface that obtains in the step 1, carry out drying then, 50 ℃～90 ℃ of drying temperatures, 0.5～48h finished at the copper matrix surface and made up based superhydrophobic thin films time of drying.
2. a kind of method at copper matrix surface structure based superhydrophobic thin films according to claim 1 is characterized in that the described hydrochloric acid mass concentration of step 1 is 1%～25%, and h 2 so 4 concentration is 1%～60%, and soak time is 0.5～100min.
3. according to claim 1ly a kind ofly make up the method for based superhydrophobic thin films, it is characterized in that with deionized water matrix being cleaned 2 times in the step 1 at the copper matrix surface, and then with alcohol flushing 2 times.
4. according to claim 1 and 2ly a kind ofly make up the method for based superhydrophobic thin films, it is characterized in that adding in the step 2 carboxylic acid of backbone c atoms several 10～19 at the copper matrix surface.
5. a kind of method at copper matrix surface structure based superhydrophobic thin films according to claim 4, the concentration that it is characterized in that Silver Nitrate in the step 2 is 5～25mmol/L.
6. according to claim 2 or 3 described a kind of methods at copper matrix surface structure based superhydrophobic thin films, the concentration that it is characterized in that carboxylic acid in the step 2 is 5～35mmol/L.
7. a kind of method at copper matrix surface structure based superhydrophobic thin films according to claim 6 is characterized in that soaking in the step 3 1～4min.
8. according to claim 6ly a kind ofly make up the method for based superhydrophobic thin films, it is characterized in that in the step 3 55 ℃～85 ℃ of drying temperatures at the copper matrix surface, time of drying 1～40h.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102626686A (en) * | 2012-04-19 | 2012-08-08 | 大连理工大学 | Method for preparing low-adhesion super-hydrophobic surface on steel substrate |
| CN102877047A (en) * | 2012-10-25 | 2013-01-16 | 武汉工程大学 | Method for preparing super hydrophobic coating on copper or copper alloy net |
| CN103469184A (en) * | 2013-09-27 | 2013-12-25 | 武汉工程大学 | Preparation method of super-hydrophobic bismuth coating |
| CN103567456A (en) * | 2013-10-08 | 2014-02-12 | 上海交通大学 | Metallic silver surface super-hydrophobicity material and preparation method thereof |
| CN103588164A (en) * | 2013-10-08 | 2014-02-19 | 上海交通大学 | Copper-silver micro-nano multi-stage structure super-hydrophobic surface and production method thereof |
| CN103817059A (en) * | 2012-11-19 | 2014-05-28 | 深圳富泰宏精密工业有限公司 | Preparation method for aluminum super-hydrophobic surface and product |
| CN105239066A (en) * | 2015-11-13 | 2016-01-13 | 上海理工大学 | Preparation method of self-cleaning coating on copper surface |
| CN105671523A (en) * | 2016-01-17 | 2016-06-15 | 西安科技大学 | Replacement reaction method for preparation of silver dendritic super-hydrophobic surface |
| CN106283133A (en) * | 2016-09-06 | 2017-01-04 | 吉林大学 | A kind of preparation method of bionical oil-water separation copper foam |
| CN108530657A (en) * | 2018-02-27 | 2018-09-14 | 广东工业大学 | A kind of highly sensitive strain sensing macromolecule and preparation method thereof with self-healing and super thin water resistance |
| CN111019148A (en) * | 2019-12-10 | 2020-04-17 | 河南科技学院 | Modified foamed copper material and preparation method and application thereof |
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| CN102626686A (en) * | 2012-04-19 | 2012-08-08 | 大连理工大学 | Method for preparing low-adhesion super-hydrophobic surface on steel substrate |
| CN102877047A (en) * | 2012-10-25 | 2013-01-16 | 武汉工程大学 | Method for preparing super hydrophobic coating on copper or copper alloy net |
| CN103817059A (en) * | 2012-11-19 | 2014-05-28 | 深圳富泰宏精密工业有限公司 | Preparation method for aluminum super-hydrophobic surface and product |
| CN103469184A (en) * | 2013-09-27 | 2013-12-25 | 武汉工程大学 | Preparation method of super-hydrophobic bismuth coating |
| CN103469184B (en) * | 2013-09-27 | 2015-09-09 | 武汉工程大学 | A kind of preparation method of super-hydrophobic bismuth coating |
| CN103567456B (en) * | 2013-10-08 | 2016-04-13 | 上海交通大学 | A kind of Metallic silver surface super-hydrophobicitymaterial material and preparation method thereof |
| CN103588164A (en) * | 2013-10-08 | 2014-02-19 | 上海交通大学 | Copper-silver micro-nano multi-stage structure super-hydrophobic surface and production method thereof |
| CN103567456A (en) * | 2013-10-08 | 2014-02-12 | 上海交通大学 | Metallic silver surface super-hydrophobicity material and preparation method thereof |
| CN105239066A (en) * | 2015-11-13 | 2016-01-13 | 上海理工大学 | Preparation method of self-cleaning coating on copper surface |
| CN105671523A (en) * | 2016-01-17 | 2016-06-15 | 西安科技大学 | Replacement reaction method for preparation of silver dendritic super-hydrophobic surface |
| CN105671523B (en) * | 2016-01-17 | 2018-05-25 | 西安科技大学 | A kind of displacement reaction method for preparing silver tree branch super hydrophobic surface |
| CN106283133A (en) * | 2016-09-06 | 2017-01-04 | 吉林大学 | A kind of preparation method of bionical oil-water separation copper foam |
| CN108530657A (en) * | 2018-02-27 | 2018-09-14 | 广东工业大学 | A kind of highly sensitive strain sensing macromolecule and preparation method thereof with self-healing and super thin water resistance |
| CN108530657B (en) * | 2018-02-27 | 2021-03-09 | 广东工业大学 | High-sensitivity strain sensing polymer with self-healing and super-hydrophobic waterproof properties and preparation method thereof |
| CN111019148A (en) * | 2019-12-10 | 2020-04-17 | 河南科技学院 | Modified foamed copper material and preparation method and application thereof |
| CN111019148B (en) * | 2019-12-10 | 2021-10-01 | 河南科技学院 | Modified foamed copper material and preparation method and application thereof |
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Application publication date: 20111102 |