CN101886285A - Method for preparing stainless steel with antibacterial surface - Google Patents
Method for preparing stainless steel with antibacterial surface Download PDFInfo
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- CN101886285A CN101886285A CN 201010212158 CN201010212158A CN101886285A CN 101886285 A CN101886285 A CN 101886285A CN 201010212158 CN201010212158 CN 201010212158 CN 201010212158 A CN201010212158 A CN 201010212158A CN 101886285 A CN101886285 A CN 101886285A
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Abstract
The invention discloses a method for preparing stainless steel with an antibacterial surface. In the method, a porous oxide film is made on the surface of the stainless steel by an anodic oxidation method; then the porous oxide film is used as a carrier to perform alternating current electrolytic deposition in an electrolyte which contains antibacterial metal ions, so that under the electrolytic reduction action of the antibacterial metal ions in the holes in the oxide film, an antibacterial metal element can be implanted into the holes in the oxide film to make the oxide film have an antibacterial property; and thus, an antibacterial outer layer is prepared on the surface of the stainless steel. The surface antibacterial layer prepared by the method is in metallurgical combination with the substrate, so stripping problem is solved. In addition, the preparation process is simple; and the cost is low.
Description
Technical field
The present invention relates to a kind of preparation method of stainless steel with antibacterial surface, be specifically related to a kind of method for preparing stainless steel with antibacterial surface based on anodic oxidation porous oxide film implantation antibacterial metal element
Background technology
Stainless steel is used very extensive in human daily life, carrying case, dining car, food-shelf, food processing machinery as foodstuffs industry, medicine equipment such as operation tool, Operation trolley, communal facility such as elevator ﹠ stairs handrail, railing, household supplies such as tank, cabinet, kitchen cabinet, washing machine inner bag, shower, water tank, door handle, handle etc.Common stainless steel does not have antibacterial, and unwanted bacteria is easily multiplied on Stainless Steel Products, causes the contact transmission of bacterium easily, brings hidden danger to HUMAN HEALTH.On the Stainless Steel Products of the daily contact of the mankind, adopt anti-bacteria stainless steel, can suppress bacterium and multiply, avoid contact transmission.The whole anti-bacteria stainless steel of the cupric of now having developed or argentiferous antibiotic lasting, be not afraid of wearing and tearing, but owing to use a large amount of silver or copper, material cost height.Because what play anti-microbial effect under most of occasion all is stainless steel surface, utilize technologies such as spraying, roller coat, sol-gel, compound plating, magnetron sputtering to apply anti-biotic material and can reduce the anti-bacteria stainless steel cost at stainless steel surface, but mainly be that machinery is chimeric between antimicrobial coating and matrix, bonding force is not high enough, peels off easily in the use.
Summary of the invention
The present invention is directed to the problem of peeling off that existing stainless steel surface antimicrobial coating exists, propose a kind of method for preparing the stainless steel surface antibiotic layer based on stainless steel surface anodic oxidation porous oxide film implantation antibacterial metal element.The antibacterial metal element of implanting can be the metallic element that silver, copper etc. have antibacterial.
A kind of method for preparing stainless steel with antibacterial surface provided by the invention: adopt anonizing to prepare porous oxide film at stainless steel surface earlier, be carrier then with the porous oxide film, in containing the electrolytic solution of antibacterial metal ions, carry out the alternating current electrolysis deposition, utilize antibacterial metal ions in the intrapore electrolytic reduction effect of oxide film, the antibacterial metal element is implanted in the hole of oxide film, make oxide film have germ resistance, thereby prepare antibiotic skin at stainless steel surface.
Above-mentioned stainless steel is the SUS304 stainless steel, carries out anodic oxidation after electropolishing, oil removing, activation; Anodic oxidation equipment adopts the WYK-15010K dc current regulator power supply, is counter electrode with stereotype, and electrolytic solution adopts sulfuric acid deionized water solution, oxalic acid deionized water solution or citric acid deionized water solution respectively; Oxidation voltage 10～100V, current density 1～2A/dm
2, 24～35 ℃ of electrolyte temperatures, oxidization time 30～60min.
Above-mentioned electrolytic solution is the deionized water solution of sulfuric acid, oxalic acid or citric acid, wherein sulfuric acid concentration 150～300gL
-1, concentration of oxalic acid 40～100gL
-1, citric acid concentration 100～400gL
-1
Adopt SVC-500VA full-automatic alternating current stabilized voltage supply antianode oxidation porous oxide film to carry out the antibacterial metal element deposition, the electrolytic solution that the alternating current electrolysis deposition adopts adopts Silver Nitrate and vitriolic mixed solution, adopts copper sulfate and vitriolic mixed solution when deposited copper when depositing silver; The processing parameter that depositing silver adopts is: depositing current density 1.5A/dm
2, deposition voltage 25V, 30 ℃ of electrolyte temperatures, depositing time 20～60min; The processing parameter that deposited copper adopts is: depositing current density 1.0A/dm
2, deposition voltage 15V, 25 ℃ of electrolyte temperatures, depositing time 20～70min.
In above-mentioned Silver Nitrate and the vitriolic mixed solution, silver nitrate concentration 10gL
-1, sulfuric acid concentration 20gL
-1
In above-mentioned copper sulfate and the vitriolic mixed solution, concentration of copper sulfate 15gL
-1, sulfuric acid concentration 18gL
-1
Antibiotic requirement according to Stainless Steel Products, implantable different antibacterial metal element, and the pore dimension of porous oxide film, void density can be controlled by change anodic oxidation liquid formula, anode oxidation process, and the implantation amount of antibacterial metal element can be controlled by changing the alternating current electrolysis depositing operation.
The stainless steel with antibacterial surface of the present invention's preparation is compared with existing anti-bacteria stainless steel, and beneficial effect is:
(1) antibiotic layer and basal body binding force are strong.Because between the porous oxide film of anodic oxidation preparation and the matrix is metallurgical binding, so compare with the coating anti-bacteria stainless steel, there is not the problem of peeling off in the antibacterial surface layer of this technology preparation.
(2) cost is low.The whole anti-bacteria stainless steel of argentiferous or cupric is to add precious metal element silver or copper in integral material, and the addition of copper is generally 1.5%～3.8%, and the addition of silver is generally about 0.4%, and noble metal dosage is big, the cost height.The thickness of the stainless steel surface antibiotic layer of this technology preparation has only tens microns, so the consumption of silver or copper reduces greatly.Simultaneously, because antibiotic layer is to form, can replace fine silver or fine copper metal in argentiferous or copper-containing solution with the Silver Nitrate or the copper sulfate of cheapness.So the antibiotic layer cost of this technology preparation reduces greatly.
(3) technology is simple.Operations such as anodic oxidation and alternating current electrolysis deposition are all carried out in the common electrical coating bath, and this technology is promoted easily.This technology also can be used for aluminium alloy, titanium alloy, Mg alloy surface and prepares antibiotic layer.
(4) antibiotic layer solidity to corrosion, wear resistance are good.Anode oxide film has good solidity to corrosion and wear resistance, and the antibiotic layer that is based upon on the anodic oxidation porous oxide film basis has good solidity to corrosion and wear resistance equally.
Description of drawings
Fig. 1 is the structure iron of stainless steel surface anodic oxidation porous oxide film of the present invention.
Fig. 2 is the structure iron of the stainless steel surface antibiotic layer based on the anodic oxidation porous oxide film of the present invention.
Number in the figure explanation: 1-anodic oxidation porous oxide film; The 2-hole; The 3-stainless steel base; 4-antibacterial metal element.
Embodiment
Embodiment
With the SUS304 stainless steel is body material, and line cuts into the sample of 20mm * 20mm * 1mm, after electropolishing, oil removing, activation, carries out anodic oxidation.Anodic oxidation equipment adopts WYK-15010K dc current regulator power supply (voltage 0～150V, electric current 0～10A), with the stereotype that is of a size of 25mm * 25mm * 3.6mm is counter electrode, and electrolytic solution adopts sulfuric acid deionized water solution, oxalic acid deionized water solution, citric acid deionized water solution respectively.Table 1 is segment anode oxidizing process parameter and porous oxide film structural parameter.
Adopt SVC-500VA full-automatic alternating current stabilized voltage supply (output voltage 220V) antianode oxidation porous oxide film to carry out the antibacterial metal element deposition, electrolytic solution adopts the deionized water solution that contains Silver Nitrate.Sedimentary silver is simple substance silver, is cylindric, and diameter is identical with the aperture of porous-film, and length depends on depositing time.Table 2 is the structural parameter of the interior silver of fenestra behind the partially porous oxide film deposition silver; Table 3 is the structural parameter of the interior silver of fenestra behind the partially porous oxide film deposition copper.
Adopt " the antibiotic fabricated product of JISZ2801-2000----antibacterial tests method and antibacterial effect " standard detecting method, detect the anti-microbial property of antibiotic oxide film intestinal bacteria, streptococcus aureus, Pseudomonas aeruginosa.
Table 4 is the anti-microbial property of the antibiotic oxide film of part.
Table 1 anode oxidation process parameter and oxide film structural parameter
The structural parameter of depositing silver in table 2 alternating current electrolysis depositing operation and the fenestra
The structural parameter of deposited copper in table 3 alternating current electrolysis depositing operation and the fenestra
The anti-microbial property of the antibiotic oxide film of table 4
Claims (6)
1. method for preparing stainless steel with antibacterial surface, it is characterized in that: adopt anonizing to prepare porous oxide film at stainless steel surface earlier, be carrier then with the porous oxide film, in containing the electrolytic solution of antibacterial metal ions, carry out the alternating current electrolysis deposition, utilize antibacterial metal ions in the intrapore electrolytic reduction effect of oxide film, the antibacterial metal element is implanted in the hole of oxide film, makes oxide film have germ resistance, thereby prepare antibiotic skin at stainless steel surface.
2. preparation method according to claim 1 is characterized in that: above-mentioned stainless steel is 304 stainless steels, carries out anodic oxidation after electropolishing, oil removing, activation; Anodic oxidation equipment adopts dc current regulator power supply, is counter electrode with stereotype, and electrolytic solution adopts sulfuric acid deionized water solution, oxalic acid deionized water solution or citric acid deionized water solution respectively; Oxidation voltage 10～100V, current density 1～2A/dm
2, 24～35 ℃ of electrolyte temperatures, oxidization time 30～60min.
3. preparation method according to claim 2 is characterized in that: above-mentioned electrolytic solution is the deionized water solution of sulfuric acid, oxalic acid or citric acid, wherein sulfuric acid concentration 150～300gL
-1, concentration of oxalic acid 40～100gL
-1, citric acid concentration 100～400gL
-1
4. preparation method according to claim 1, it is characterized in that: adopt full-automatic alternating current stabilized voltage supply antianode oxidation porous oxide film to carry out the antibacterial metal element deposition, the electrolytic solution that the alternating current electrolysis deposition adopts adopts Silver Nitrate and vitriolic mixed solution, adopts copper sulfate and vitriolic mixed solution when deposited copper when depositing silver; The processing parameter that depositing silver adopts is: depositing current density 1.5A/dm
2, deposition voltage 25V, 30 ℃ of electrolyte temperatures, depositing time 20～60min; The processing parameter that deposited copper adopts is: depositing current density 1.0A/dm
2, deposition voltage 15V, 25 ℃ of electrolyte temperatures, depositing time 20～70min.
5. preparation method according to claim 4 is characterized in that: in above-mentioned Silver Nitrate and the vitriolic mixed solution, and silver nitrate concentration 10gL
-1, sulfuric acid concentration 20gL
-1
6. preparation method according to claim 4 is characterized in that: in above-mentioned copper sulfate and the vitriolic mixed solution, and concentration of copper sulfate 15gL
-1, sulfuric acid concentration 18gL
-1
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102268713A (en) * | 2011-06-29 | 2011-12-07 | 武汉科技大学 | Stainless steel surface nano-pore array film and preparation method thereof |
| CN104651899A (en) * | 2014-12-11 | 2015-05-27 | 温州大学 | Anodizing process of metal substrate for carbon nanotube growth |
| CN105100317A (en) * | 2015-08-18 | 2015-11-25 | 上海交通大学 | Antimicrobial self-cleaning mobile phone housing and preparation method of antimicrobial film layer thereof |
| CN105200466A (en) * | 2015-09-25 | 2015-12-30 | 中国科学院金属研究所 | Production method of antibacterial colored stainless steel |
| CN105603410A (en) * | 2015-12-22 | 2016-05-25 | 唐艺峰 | Manufacturing method of bacteriostatic stainless steel dish |
| CN108716015A (en) * | 2018-06-05 | 2018-10-30 | 浙江苏泊尔股份有限公司 | A method of improving the discoloration of stainless steel work-piece high temperature resistance |
| CN109852960A (en) * | 2019-03-12 | 2019-06-07 | 姜水英 | A kind of method of antibacterial functionalized-corrosion-resistant modification of aluminum alloy surface |
| CN110552044A (en) * | 2019-10-14 | 2019-12-10 | 四川轻化工大学 | Steel anodic oxidation electrolyte and anodic oxidation method thereof |
| CN112160001A (en) * | 2020-09-25 | 2021-01-01 | 同曦集团有限公司 | Antibacterial, mildewproof and antiviral oxidized stainless steel and preparation method thereof |
| CN112522773A (en) * | 2020-11-04 | 2021-03-19 | 东南大学 | Preparation method of stainless steel with antibacterial surface |
| CN112575355A (en) * | 2019-09-30 | 2021-03-30 | 浙江绍兴苏泊尔生活电器有限公司 | Cooking utensil and surface treatment method thereof |
| CN113293421A (en) * | 2021-04-15 | 2021-08-24 | 光科真空科技(泰兴)有限公司 | Electrolytic process and electrolyte for inner wall protection plate of vacuum cavity |
| CN114232053A (en) * | 2021-11-15 | 2022-03-25 | 中国科学院金属研究所 | Anticorrosive and antibacterial surface treatment method for stainless steel |
| CN114395912A (en) * | 2021-06-29 | 2022-04-26 | 台湾塑胶工业股份有限公司 | Method for producing antibacterial fiber |
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| KR20060087127A (en) * | 2005-01-28 | 2006-08-02 | 이상훈 | Method to attach nano silver to stainless steel |
| CN101748470A (en) * | 2009-12-28 | 2010-06-23 | 常州佳得顺抗菌材料科技有限公司 | Antibacterial stainless steel with electrochemical oxidation film |
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| JPH10121222A (en) * | 1996-10-15 | 1998-05-12 | Nisshin Steel Co Ltd | Stainless steel sheet having photocatalistic action and its production |
| CN1745200A (en) * | 2003-01-30 | 2006-03-08 | 日本氧化铝加工株式会社 | Method for forming anodic oxide coating on surface of aluminum or aluminum alloy |
| KR20060087127A (en) * | 2005-01-28 | 2006-08-02 | 이상훈 | Method to attach nano silver to stainless steel |
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Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102268713B (en) * | 2011-06-29 | 2013-10-23 | 武汉科技大学 | Stainless steel surface nano-pore array film and preparation method thereof |
| CN102268713A (en) * | 2011-06-29 | 2011-12-07 | 武汉科技大学 | Stainless steel surface nano-pore array film and preparation method thereof |
| CN104651899A (en) * | 2014-12-11 | 2015-05-27 | 温州大学 | Anodizing process of metal substrate for carbon nanotube growth |
| CN105100317A (en) * | 2015-08-18 | 2015-11-25 | 上海交通大学 | Antimicrobial self-cleaning mobile phone housing and preparation method of antimicrobial film layer thereof |
| CN105100317B (en) * | 2015-08-18 | 2019-01-11 | 上海交通大学 | The preparation method of antibiotic self-cleaning phone housing and its antibacterial film layer |
| CN105200466A (en) * | 2015-09-25 | 2015-12-30 | 中国科学院金属研究所 | Production method of antibacterial colored stainless steel |
| CN105603410A (en) * | 2015-12-22 | 2016-05-25 | 唐艺峰 | Manufacturing method of bacteriostatic stainless steel dish |
| CN108716015A (en) * | 2018-06-05 | 2018-10-30 | 浙江苏泊尔股份有限公司 | A method of improving the discoloration of stainless steel work-piece high temperature resistance |
| CN109852960A (en) * | 2019-03-12 | 2019-06-07 | 姜水英 | A kind of method of antibacterial functionalized-corrosion-resistant modification of aluminum alloy surface |
| CN112575355A (en) * | 2019-09-30 | 2021-03-30 | 浙江绍兴苏泊尔生活电器有限公司 | Cooking utensil and surface treatment method thereof |
| CN112575355B (en) * | 2019-09-30 | 2023-11-14 | 浙江绍兴苏泊尔生活电器有限公司 | Cooking appliance and surface treatment method thereof |
| CN110552044A (en) * | 2019-10-14 | 2019-12-10 | 四川轻化工大学 | Steel anodic oxidation electrolyte and anodic oxidation method thereof |
| CN112160001A (en) * | 2020-09-25 | 2021-01-01 | 同曦集团有限公司 | Antibacterial, mildewproof and antiviral oxidized stainless steel and preparation method thereof |
| CN112160001B (en) * | 2020-09-25 | 2021-07-27 | 同曦集团有限公司 | Antibacterial, mildewproof and antiviral oxidized stainless steel and preparation method thereof |
| CN112522773B (en) * | 2020-11-04 | 2022-01-28 | 东南大学 | Preparation method of stainless steel with antibacterial surface |
| CN112522773A (en) * | 2020-11-04 | 2021-03-19 | 东南大学 | Preparation method of stainless steel with antibacterial surface |
| CN113293421A (en) * | 2021-04-15 | 2021-08-24 | 光科真空科技(泰兴)有限公司 | Electrolytic process and electrolyte for inner wall protection plate of vacuum cavity |
| CN114395912A (en) * | 2021-06-29 | 2022-04-26 | 台湾塑胶工业股份有限公司 | Method for producing antibacterial fiber |
| CN114395912B (en) * | 2021-06-29 | 2024-04-16 | 台湾塑胶工业股份有限公司 | Method for manufacturing antibacterial fiber |
| CN114232053A (en) * | 2021-11-15 | 2022-03-25 | 中国科学院金属研究所 | Anticorrosive and antibacterial surface treatment method for stainless steel |
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Open date: 20101117 |