CN1676675A - Stainless Steel Electrochemical Coloring Method - Google Patents
Stainless Steel Electrochemical Coloring Method Download PDFInfo
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- CN1676675A CN1676675A CN 200510032660 CN200510032660A CN1676675A CN 1676675 A CN1676675 A CN 1676675A CN 200510032660 CN200510032660 CN 200510032660 CN 200510032660 A CN200510032660 A CN 200510032660A CN 1676675 A CN1676675 A CN 1676675A
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- 229910001220 stainless steel Inorganic materials 0.000 title claims description 85
- 239000010935 stainless steel Substances 0.000 title claims description 82
- 238000000034 method Methods 0.000 title claims description 40
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- 238000002203 pretreatment Methods 0.000 claims abstract 2
- 238000005406 washing Methods 0.000 claims description 29
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- 239000000047 product Substances 0.000 claims description 24
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- 229910019142 PO4 Inorganic materials 0.000 claims description 14
- 239000010452 phosphate Substances 0.000 claims description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
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- 239000010439 graphite Substances 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- LDMOEFOXLIZJOW-UHFFFAOYSA-N 1-dodecanesulfonic acid Chemical compound CCCCCCCCCCCCS(O)(=O)=O LDMOEFOXLIZJOW-UHFFFAOYSA-N 0.000 claims description 4
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
This invention is a kind of electro-chemstry staining method of non-corrosive steel. Firstly, pre-treatment for the semi-manufactured non-corrosive steel is essential. Molybdate water solution of 5.0-200 g/L is filled in the electrolytic bath as staining solution, and then the semi-manufactured non-corrosive steel is put into the solution to be stained. The staining electricity should be controlled between 0.02A/square decimeter and 0.6A/square decimeter, while the staining time is between 10 seconds and 60 minutes. At the same time, the temperature should be controlled between 15deg.C and 60 deg.C. After stained, the semi-manufactured non-corrosive steel is water-scrubbed. Then through desiccation, we can get stained non-corrosive steel. To sum up, the staining solution in this invention has no toxicity, has little pollution and power cost, so it does no harm to the workers' health. The technology is easy, and the stained color is stable and has high authenticity. What's more, the cost of the solution is low. You can get multi-colored, homogeneous and highly brightened product.
Description
Technical Field
The invention relates to the technical field of stainless steel electrochemical coloring for buildings, household appliances, automobiles and decoration, in particular to a stainless steel electrochemical coloring method.
Background
The first industrial production of coloured stainless steels originated from INCO company, uk in 1973, which mainly used to impregnate stainless steels in high-concentration solutions of chromic and sulphuric acids at a medium temperature of 80 ℃ to produce Cr of different thicknesses on their surfaces by controlling the length of impregnation2O3And (5) oxidizing the film. The film is semitransparent, light waves reflected by the surface of the film interfere with light waves reflected by the surface of the stainless steel through the film layer, and products with different Interference colors (Interference colors) can be produced by effectively controlling the thickness of the film. This method is also used by Xinri-Fe-Nanyang, one of the major manufacturers of Japanese color stainless steel.
Many researchers have conducted improvement studies on the above method of INCO company, and the quality of a colored film is improved by adding various additives to a coloring liquid, and the coloring temperature is 50 ℃ or higher, and a process of strengthening the colored film is required after coloring. Still some scholars adopt the alternating current square wave electrolysis method to study the coloring process of colored stainless steel, because use symmetrical alternating current square wave, the coloring temperature is between 50 ~ 55 ℃, need to carry out the process of membrane reinforcement after the coloring likewise.
At present, the coloring process for obtaining a thin colored film layer by a stainless steel chemical coloring method mainly comprises an alkaline nitrite-containing high-temperature method and an acidic chromate-acid-containing method. The alkaline high-temperature chemical method needs to be colored at the temperature of more than 100 ℃, the solution is quickly evaporated, the production environment is severe, and toxic substances, namely nitrite and high-concentration thermokalite are contained, so that the health of workers is seriously threatened; the acid chemical coloring method also needs to use 2.5 mol.L at a high temperature of 80 ℃ or higher-1Chromic acid +5.0 mol. L-1The mixed acid solution of sulfuric acid is colored, and the problems of severe production environment, quick failure of the treated solution, high waste acid treatment cost and the like exist.
Whether the chemical coloring method or the electrochemical coloring method is adopted, the pollution problem of hexavalent chromium exists in the coloring process containing chromic acid: a large amount of waste water is formed in the rinsing process, hexavalent chromium has great irritation and corrosivity to the skin, mucous membrane and respiratory system of a human body, has toxic action on central nerves, has strong carcinogenicity, and seriously affects the body health of workers. The world countries have made stricter regulations on the discharge standard of hexavalent chromium, and some developed countries have even started to legally ban hexavalent chromium plating. Our country also faces the problem of hexavalent chromium contamination, and with government control over chromic acid use, the acidic chromate acid staining process of stainless steel will inevitably be eliminated.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provide a stainless steel electrochemical coloring method. The method has simple process, less pollution of the used coloring solution, low price and stable coloring, and can produce high-quality stainless steel products with consistent color and tone which meet the performance requirements.
The purpose of the invention is realized by the following technical scheme: the stainless steel electrochemical coloring method comprises the steps of pretreating a stainless steel semi-finished product (comprising oil removal, hot water washing, flowing cold water washing, activation and flowing cold water washing), and further comprises the following steps and process conditions:
in the first step, a molybdate aqueous solution with the content of 5.0-200 g/L is used as a coloring solution and is placed in an electrolytic cell, a stainless steel semi-finished product is immersed in the coloring solution for coloring treatment, and the coloring current is controlled to be 0.02-0.6A/dm2(ii) a The coloring time is 10 seconds to 60 minutes; the coloring temperature is 15-60 ℃;
and washing the colored stainless steel semi-finished product in the second step with water, and drying to obtain a colored stainless steel finished product.
In order to better realize the invention, one or more than one mixture of phosphate, dihydric phosphate and surfactant is added into the coloring solution; the addition amount of the phosphate is 2.5-40 g/L, the addition amount of the dihydric phosphate is 5.0-50 g/L, and the addition amount of the surfactant is 10-20 ml/L; the pH value of the coloring solution is 5.0-7.0, and reagents for adjusting the pH value comprise phosphoric acid and sulfuric acid; the surfactant comprises dodecyl sulfate and dodecyl sulfonate; the anode of the electrolytic cell comprises stainless steel or graphite and the cathode comprises a coloredstainless steel semi-finished product.
The process for forming the electrochemical coloring film of the stainless steel is a cathode deposition film-forming process, wherein the possible reactions are as follows:
inner layer film: (1)
outer layer film: (2)
the thickness of the interference film formed by stainless steel in the solution is related to the coloring time, and the coloring effect of the stainless steel film is closely related to the film composition and the film thickness, so that the required film color, color uniformity and brightness can be obtained by strictly controlling the thickness of the film.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the coloring solution of the invention does not contain chromic acid, causes little pollution to the environment, has no toxicity, has low reaction temperature, can be colored at low temperature, can achieve satisfactory effect at room temperature, can obtain products with various colors, uniformity and high brightness, saves energy consumption, reduces the evaporation of the solution, and is beneficial to the health of operators.
2. The coloring method has the advantages of low cost, almost no pollution of waste liquid, simple process, stable coloring and high reliability, and can produce high-quality stainless steel products with various colors (blue, blue purple, silver gray, purplish red, golden yellow, green, yellow green, black, rainbow interference colors and the like) and consistent color tones which meet the performance requirements.
3. The invention controls the process parameters of the electrochemical coloring by adjusting, so that the color of the electrochemical coloring film is more stable, the brightness is higher and more uniform, and the higher requirements of products are met.
Drawings
FIG. 1 is a schematic diagram of a stainless steel colored film forming a color;
FIG. 2 is a process flow diagram of the coloring method of the present invention;
FIG. 3 is a schematic view showing an observation angle of an electrochemically colored film of stainless steel.
Detailed Description
The present invention will be described in further detail below with reference to the drawings and examples, but the embodiments of the present invention are not limited thereto.
As shown in fig. 1, the principle of forming a color by a stainless steel colored film is as follows: since the visible light 4 in the air 1 is incident to the surface of the colored film 2, reflection and refraction phenomena are generated, the refracted light 6 and the reflected light 5 are generated, the refracted light 6 is reflected by the stainless steel 3 and is refracted again by the colored film 2, and the formed refracted light 7 and the reflected light 5 generate interference fringes, thereby forming a color effect.
As shown in FIG. 3, the present invention uses different angle views to illustrate the interference color of the film layers. After the stainless steel is colored, the displayed color is not caused by forming a colored film on the surface of the stainless steel, but is caused by the interference of the formed transparent colored film, and the reflected light on the surface of the colored film on the surface of the stainless steel is interfered with the refracted light which passes through the colored film on the surface, so that various colors are displayed. Different stainless steels have different components, and the colors of interference colors are different due to different component solutions for forming the coloring film; the same stainless steel has different thicknesses of the formed colored films and different refractive indexes, and the colors of the interference colors are different. Even if the same stainless steel and the coloring film have the same thickness, the color of the interference color on the surface of the stainless steel changes correspondingly with the change of the incident light angle. When the stainless steel surface is observed at 90 degrees vertically, 45 degrees horizontally and 180 degrees horizontally, the color of the interference color on the stainless steel surface correspondingly changes.
As shown in fig. 2, the present invention has the following embodiments.
Example one
Firstly, pretreating a decorative 1Cr18Ni9 austenitic stainless steel plate, including removing oil; washing with hot water; washing with flowing cold water; activating; washing with flowing cold water;
and the second step of placing the coloring solution in an electrolytic cell, and immersing the stainless steel semi-finished product in the coloring solution for coloring treatment, wherein the anode is the stainless steel, and the cathode is the colored stainless steel semi-finished product. Controlling coloring current to 0.06A/dm2(ii) a Electrolytic coloring time is 4 minutes; heating to the required coloring temperature of 42 ℃ in a constant-temperature water bath (controlled by a temperature controller); the coloring solution is a molybdate aqueous solution with thecontent of 25g/L, dihydric phosphate is added according to the proportion of 12.5g/L, and the pH value of the coloring solution is adjusted to 6.5 by sulfuric acid;
and thirdly, washing the colored stainless steel semi-finished product with cold water, and drying the colored stainless steel semi-finished product with cool air to obtain a colored stainless steel finished product.
The stainless steel product obtained in this example was subjected to color observation and evaluation. The composition of the 1Cr18Ni9 stainless steel is as follows:
TABLE 11 chemical composition (in weight%) of Cr18Ni9 austenitic stainless steel
| C | Si | Mn | Ni | Cr | Cu | Mo | N |
| 0.068 | 0.57 | 1.08 | 8.64 | 18.36 | 0.08 | 0.04 | 0.027 |
S＞0.007，P＜0.025。
The method comprises the steps of depositing reaction formulas (1) and (2) of metals in the 1Cr18Ni9 stainless steel in a coloring process, forming metal oxide films on the surface of the stainless steel, and forming color films through the deposition process, wherein the film thickness ranges from 10 nm to 150nm, and the colors show various colors along with the different film thicknesses. The electrolytically colored 1Cr18Ni9 stainless steel finished product obtained a multi-color interference film which was green when viewed vertically at 90 °, purplish red when viewed at 45 °, and blue when viewed horizontally at about 180 °.
Example two
Electrochemical coloring was performed under the process conditions of example one. When the coloring time was 7.0 minutes, the color obtained was uniform and bright brown; when the coloring time is 10.0 minutes, the obtained color is uniform and bright brownish black; when the coloring time is 15.0 minutes, the obtained color is uniform and bright black; when the coloring time was 60.0 minutes, the obtained color was a uniform and bright dark black. The film layer is rubbed with an eraser at an angle of 45 degrees, and the color of the film layer is not faded for more than 1500 times and becomes brighter after being rubbed.
EXAMPLE III
The coloring current density was adjusted to 0.10A/dm2And the rest is electrochemically colored according to the process conditions of the first embodiment. When the coloring time is 10 seconds, uniform and bright bluish purple is obtained; when the coloring time is 20Second, uniform and bright silver gray is obtained; the coloring time is 30 seconds, and uniform and bright golden yellow is obtained; when the coloring time is 40 seconds, a uniform and bright colored interference film is obtained, which is yellow-green when vertically observed, blue when observed at an angle of 45 degrees and purplish-red when horizontally observed at about 180 degrees; when the coloration time was 50 seconds, a homogeneous and bright colored interference film was obtained, golden yellow when viewed vertically, blue when viewed at an angle of 45 °, and purplish red when viewed horizontally at about 180 °. It can be seen that the colors of the colorations are more varied than the colors of the conventional colorations, and the uniformity and lightness of the film color are better than those of the conventional colorations.
Example four
Firstly, pretreating a 1Cr17Ni8 austenitic stainless steel plate, including removing oil; washing with hot water; washing with flowing cold water; activating; washing with flowing cold water;
and putting the coloring solution into an electrolytic cell, and immersing the stainless steel semi-finished product into the coloring solution for coloring treatment, wherein the anode is graphite, and the cathode is the colored stainless steel semi-finished product. Controlling coloring current to 0.08A/dm2(ii) a Electrolytic coloring time was 27 minutes; the coloring temperature is 25 ℃; the coloring solution is a molybdate aqueous solution with the content of 25g/L, phosphate is added according to 5g/L, and the pH value of the coloring solution is adjusted to be 6.4 by phosphoric acid;
and thirdly, washing the colored stainless steel semi-finished product with cold water, and drying to obtain a colored stainless steel finished product.
When the stainless steel finished product obtained in this example was observed, a uniform, bright black interference film was formed on the surface of the stainless steel finished product. The film layer is rubbed with an eraser at an angle of 45 degrees, and the color of the film layer is not faded for more than 1500 times and becomes brighter after being rubbed.
EXAMPLE five
Firstly, pretreating a 1Cr17Ni7 austenitic stainless steel plate, including removing oil; washing with hot water; washing with flowing cold water; activating; washing with flowing cold water;
and putting the coloring solution into an electrolytic cell, and immersing the stainless steel semi-finished product into the coloring solution for coloring treatment, wherein the anode is graphite, and the cathode is the colored stainless steel semi-finished product. Controlling coloring current to 0.4A/dm2(ii) a Electrolytic coloring time is 12 minutes; the coloring temperature is 42 ℃; the coloring solution is a molybdate aqueous solution with the content of 25g/L, phosphate is added according to 5g/L, dodecyl sulfate is added according to 10ml/L, and the pH value of the coloring solution is adjustedto 5.5 by phosphoric acid;
and thirdly, washing the colored stainless steel semi-finished product with cold water, and drying to obtain a colored stainless steel finished product.
When the stainless steel finished product obtained in this example was observed, a uniform, bright black interference film was formed on the surface of the stainless steel finished product. The film layer is rubbed with an eraser at an angle of 45 degrees, and the color of the film layer is not faded for more than 1500 times and becomes brighter after being rubbed.
EXAMPLE six
Firstly, pretreating a 1Cr17Ni8 austenitic stainless steel plate, including removing oil; washing with hot water; washing with flowing cold water; activating; washing with flowing cold water;
and putting the coloring solution into an electrolytic cell, and immersing the stainless steel semi-finished product into the coloring solution for coloring treatment, wherein the anode is graphite, and the cathode is the colored stainless steel semi-finished product. Controlling coloring current at 0.05A/dm2(ii) a Electrolytic coloring time is 12 minutes; heating to the required coloring temperature of 15 ℃ in a constant-temperature water bath; the coloring solution is molybdate aqueous solution with the content of 5g/L, phosphate is added according to 2.5g/L, dihydric phosphate is added according to 5.0g/L, dodecyl sulfonate is added according to 10ml/L, and the pH value of the coloring solution is adjusted to 5.0 by phosphoric acid and sulfuric acid;
and thirdly, washing the colored stainless steel semi-finished product with water, and drying to obtain a colored stainless steel finished product.
When the stainless steel finished product obtained in this example was observed, a uniform, bright black interference film was formed on the surface of the stainless steel finished product. The film layer is rubbed with an eraser at an angle of 45 degrees, and the color of the film layer is not faded for more than 1500 times and becomes brighter after being rubbed.
EXAMPLE seven
Firstly, pretreating a 1Cr17Ni8 austenitic stainless steel plate, including removing oil; washing with hot water; washing with flowing cold water; activating; washing with flowing cold water;
and putting the coloring solution into an electrolytic cell, and immersing the stainless steel semi-finished product into the coloring solution for coloring treatment, wherein the anode is graphite, and the cathode is the colored stainless steel semi-finished product. Controlling coloring current to 0.6A/dm2(ii) a Electrolytic coloring time is 50 minutes; heating to 60 ℃ in a constant-temperature water bath; the coloring solution is a molybdate aqueous solution with the content of 200g/L, phosphate is added according to 40g/L, dihydric phosphate is added according to 50g/L, dodecyl sulfonate is added according to 20ml/L, and the pH value of the coloring solution is adjusted to 7.0 by phosphoric acid and sulfuric acid;
and thirdly, washing the colored stainless steel semi-finished product with water, and drying to obtain a colored stainless steel finished product.
When the stainless steel finished product obtained in this example was observed, a uniform, bright black interference film was formed on the surface of the stainless steel finished product. The film layer is rubbed with an eraser at an angle of 45 degrees, and the color of the film layer is not faded for more than 1500 times and becomes brighter after being rubbed.
Example eight
Firstly, pretreating a decorative 1Cr18Ni9 austenitic stainless steel plate, including removing oil; washing with hot water; washing with flowing cold water; activating; washing with flowing cold water;
the second step is to place the coloring solution in an electrolytic cell and to immerse the stainless steel semi-finished product in the coloring solutionAnd (5) performing coloring treatment, wherein the anode is stainless steel, and the cathode is a colored stainless steel semi-finished product. Controlling coloring current at 0.02A/dm2(ii) a Electrolytic coloring time is 60 minutes; heating to 60 ℃ in a constant-temperature water bath; the coloring solution is a molybdate aqueous solution with the content of 100g/L, and the pH value of the coloring solution is adjusted to 6.5 by using sulfuric acid;
and thirdly, washing the colored stainless steel semi-finished product with cold water, and drying the colored stainless steel semi-finished product with cool air to obtain a colored stainless steel finished product.
Claims (5)
1. The electrochemical colorizing method for stainless steel includes the pre-treatment of semi-finished stainless steel product, and features the following steps and technological conditions:
in the first step, a molybdate aqueous solution with the content of 5.0-200 g/L is used as a coloring solution and is placed in an electrolytic cell, a stainless steel semi-finished product is immersed in the coloring solution for coloring treatment, and the coloring current is controlled to be 0.02-0.6A/dm2(ii) a The coloring time is 10 seconds to 60 minutes; the coloring temperature is 15-60 ℃;
and washing the colored stainless steel semi-finished product in the second step with water, and drying to obtain a colored stainless steel finished product.
2. The method for electrochemically coloring stainless steel according to claim 1, wherein one or more of phosphate, dihydrogen phosphate and surfactant is added into the coloring solution; the addition amount of the phosphate is 2.5-40 g/L, the addition amount of the dihydric phosphate is 5.0-50 g/L, and the addition amount of the surfactant is 10-20 ml/L.
3. The method of claim 1, wherein the coloring solution has a pH of 5.0 to 7.0, and the pH adjusting agent comprises phosphoric acid and sulfuric acid.
4. The method of claim 1, wherein the anode of the electrolytic cell comprises stainless steel or graphite, and the cathode comprises a colored stainless steel blank.
5. The method as claimed in claim 2, wherein the surfactant comprises dodecyl sulfate and dodecyl sulfonate.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101173367B (en) * | 2006-10-31 | 2010-09-22 | 佛山市顺德区汉达精密电子科技有限公司 | A stainless steel electrochemical coloring process |
| CN101724878B (en) * | 2008-10-16 | 2011-11-16 | 比亚迪股份有限公司 | Electroplating solution and method for forming color plating |
| CN103866372A (en) * | 2014-03-24 | 2014-06-18 | 无锡宝顺不锈钢有限公司 | Electrochemical coloring solution for stainless steel and coloring method |
| CN105297110A (en) * | 2015-11-23 | 2016-02-03 | 佛山市高明俊品金属制品有限公司 | Environment-friendly stainless steel electrochemical coloring liquid and coloring method |
| CN110191977A (en) * | 2017-01-18 | 2019-08-30 | 株式会社杰希优 | Plating solution for coloring and coloring method |
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2005
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101173367B (en) * | 2006-10-31 | 2010-09-22 | 佛山市顺德区汉达精密电子科技有限公司 | A stainless steel electrochemical coloring process |
| CN101724878B (en) * | 2008-10-16 | 2011-11-16 | 比亚迪股份有限公司 | Electroplating solution and method for forming color plating |
| CN103866372A (en) * | 2014-03-24 | 2014-06-18 | 无锡宝顺不锈钢有限公司 | Electrochemical coloring solution for stainless steel and coloring method |
| CN105297110A (en) * | 2015-11-23 | 2016-02-03 | 佛山市高明俊品金属制品有限公司 | Environment-friendly stainless steel electrochemical coloring liquid and coloring method |
| CN110191977A (en) * | 2017-01-18 | 2019-08-30 | 株式会社杰希优 | Plating solution for coloring and coloring method |
| CN110191977B (en) * | 2017-01-18 | 2022-04-26 | 株式会社杰希优 | Plating solution for coloring and coloring method |
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