CN102115902A - Surface anodization coloring treatment method for titanium and titanium alloy - Google Patents
Surface anodization coloring treatment method for titanium and titanium alloy Download PDFInfo
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- CN102115902A CN102115902A CN2009102488998A CN200910248899A CN102115902A CN 102115902 A CN102115902 A CN 102115902A CN 2009102488998 A CN2009102488998 A CN 2009102488998A CN 200910248899 A CN200910248899 A CN 200910248899A CN 102115902 A CN102115902 A CN 102115902A
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Abstract
The invention discloses a surface anodization coloring treatment method for titanium and titanium alloy, comprising the following technological process: firstly, putting titanium and titanium alloy sample pieces into an acetone solution and a caustic soda solution in sequence for cleaning oil stain, then cleaning with distilled water, drying, and putting the titanium and titanium alloy sample pieces into electrolyte for treatment, wherein the electrolyte is a mixed solution of phosphoric acid and sodium gluconate. The invention has the characteristics of simple technology, good binding force between an oxide film and a substrate, bright and uniform color and lower cost.
Description
Technical field
The present invention relates to a kind of metal surface treating method, particularly relate to the treatment process of a kind of titanium or titanium alloy surface anode oxidation coloration, belong to C25D11/26 (2006.01) the I technical field in the International Patent Classification (IPC).
Background technology
For enlarging the Application Areas of titanium alloy, must carry out modification to its surface and handle.The process for treating surface of existing titanium or titanium alloy has: laser melt cover surface treatment, surface deposition coating (CVD and PVD method),
Thermodiffusion, Surface Nanocrystalline and anodic oxidation treatment, wherein simple with anodic oxidation treatment technology, oxide film wear resisting property, anti-crevice corrosion and anti-hydrogen embrittlement performance are good, are used widely in industrial production.The titanium or titanium alloy anode oxide film is along with the variation of thicknesses of layers, and its surface can present shades of colour, is ideal ornament layer and protective layer.Though the anodised recipe ratio of titanium or titanium alloy is more, dc anodizing, pulse anodic oxidation, thick film anodic oxidation etc. are arranged, the anode oxidation process of these types scarcely possesses anodised and carries out painted ability simultaneously.Publication number is that the Chinese invention patent application of CN1844483 has provided a kind of " method of titanium or titanium alloy surface anode oxidation coloration ", its step is under 60～75 ℃ and ultrasonic wave condition, titanium or titanium alloy are handled 10～15min in soda-wash solution, put into Acidwash solution after the rinsing and handle 0.5～1min, after the rinsing at 15～35 ℃, current density 5～10Adm
-2, put into the painted 15～30min of anode oxidation coloration solution under voltage 20～90V, after the rinsing in deionized water sealing treatment 15～30min; Dry down for 110～130 ℃ and handle 30～60min.Painted anode oxide film surface hardness height, bonding force and corrosion resisting property are good though this patent application has, bright in color, the even characteristics of non-variegation, good decorating effect, and its processing step is still complicated, and cost is also higher.
Summary of the invention
The objective of the invention is to solve the above-mentioned technical problem that prior art exists, improve, a kind of treatment process of new titanium or titanium alloy surface anode oxidation coloration is provided by research.The technological process of the treatment process of this titanium or titanium alloy surface anode oxidation coloration that the present invention provides is: the titanium or titanium alloy exemplar is placed on earlier in acetone soln and the sodium hydroxide solution cleans greasy dirt earlier, clean with distilled water again, put into electrolytic solution after the drying and handle.Electrolytic solution is the mixing solutions of phosphoric acid and Sunmorl N 60S.The present invention has that technology is simple, oxide film and basal body binding force is good, all even lower-cost characteristics of bright in color.
The technical scheme that the present invention provides is: the treatment process of this titanium or titanium alloy surface anode oxidation coloration has been characterized in the following step:
1) titanium or titanium alloy are placed on processing 1-8min cleaning greasy dirt in acetone soln and the sodium hydroxide solution earlier, totally standby after taking out with distilled water flushing;
2) titanium that will be after step 1) is handled or titanium alloy are put into Acidwash solution and are handled 1-5min, and it is totally standby to take out post-flush;
3) will be through step 2) titanium or titanium alloy after handling put into anode oxidation coloration solution, at 10-30 ℃, voltage 5-90V, current density 1-10Adm
-2Under the condition, painted 1-10min, it is clean to take out post-flush, obtains bright in color, uniform anode oxide film;
4) titanium or the titanium alloy of anode oxidation coloration are put into the ebullient deionized water, sealing treatment 2-30min.
Alkaline solution of the present invention is the sodium hydroxide solution of 5-10%; Acidwash solution is the mixing solutions of hydrofluoric acid and nitric acid, and wherein, hydrofluoric acid: nitric acid: water is 1: 3: 8; Anode oxidation coloration electrolytic solution is by 50-150mlL
-1Phosphoric acid, 10-150gL
-1Sunmorl N 60S is formed.
Compared with prior art, the invention has the beneficial effects as follows:
1. processing step of the present invention is few, simple to operate, with low cost, asepsis environment-protecting;
2. by setting the anode oxide film that different magnitudes of voltage can obtain different color and lusters;
3. the prepared anode oxide film bright in color of the present invention, evenly has the excellent decoration effect;
4. prepared anode oxide film and the matrix bond of the present invention is good, in the steam more than 130 degrees centigrade 8 minutes, repeats the color no change 20 times;
Embodiment
Embodiment 1
1. after pure titanium being put into acetone soln ultrasonic cleaning 5min, put into 5% sodium hydroxide solution ultrasonic cleaning 10min, rinse well standby;
2. the pure titanium after will cleaning is put into pickle solution pickling 1min, and wherein, hydrofluoric acid: nitric acid: the ratio of water is 1: 3: 8, and it is totally standby that pickling finishes post-flush;
3. the pure titanium after will handling is put into electrolytic solution, is negative electrode with the stainless steel, and pure titanium is that anode carries out anode oxidation coloration.Coloring process is: voltage 18V, and negative electrode and positive interpolar distance are 5cm, negative electrode and annode area ratio are 5: 1, time 1min.After painted, pure titanium is rinsed well;
4 put into the ebullient deionized water, sealing treatment 15min with pure titanium; Oven dry.
Pure titanium behind the anode oxidation coloration is carried out color retentivity test: the anode oxidation coloration product is placed in the steam more than 130 degrees centigrade 8 minutes, repeats the color no change 20 times.
Claims (1)
1. the treatment process of titanium or titanium alloy surface anode oxidation coloration is characterized in that the following step is arranged:
1) titanium or titanium alloy are placed on processing 1-8min cleaning greasy dirt in acetone soln and the sodium hydroxide solution earlier, totally standby after taking out with distilled water flushing;
2) titanium that will be after step 1) is handled or titanium alloy are put into Acidwash solution and are handled 1-5min, and it is totally standby to take out post-flush;
3) will be through step 2) titanium or titanium alloy after handling put into anode oxidation coloration solution, at 10-30 ℃, voltage 5-90V, current density 1-10Adm
-2Under the condition, painted 1-10min, it is clean to take out post-flush, obtains bright in color, uniform anode oxide film;
4) titanium or the titanium alloy of anode oxidation coloration are put into the ebullient deionized water, sealing treatment 2-30min;
Wherein said alkaline solution is the sodium hydroxide solution of 5-10%; Described Acidwash solution is the mixing solutions of hydrofluoric acid and nitric acid, and wherein, hydrofluoric acid: nitric acid: water is 1: 3: 8; Described anode oxidation coloration electrolytic solution is by 50-150mlL
-1Phosphoric acid, 10-150gL
-1Sunmorl N 60S is formed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102488998A CN102115902A (en) | 2009-12-30 | 2009-12-30 | Surface anodization coloring treatment method for titanium and titanium alloy |
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|---|---|---|---|
| CN2009102488998A CN102115902A (en) | 2009-12-30 | 2009-12-30 | Surface anodization coloring treatment method for titanium and titanium alloy |
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| CN102115902A true CN102115902A (en) | 2011-07-06 |
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| CN2009102488998A Pending CN102115902A (en) | 2009-12-30 | 2009-12-30 | Surface anodization coloring treatment method for titanium and titanium alloy |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102337574A (en) * | 2011-10-08 | 2012-02-01 | 中南大学 | Anode oxidization solution and oxidization method of broad titanium plate |
| CN103266338A (en) * | 2013-05-21 | 2013-08-28 | 沈阳理工大学 | TC4 titanium alloy anodizing chromium-free blackening method |
| CN103334144A (en) * | 2013-07-18 | 2013-10-02 | 哈尔滨工业大学 | Alkaline liquid water vapor post-treatment method of micro-arc oxidation biological active coating on surface of titanium |
| CN103343375A (en) * | 2013-07-18 | 2013-10-09 | 哈尔滨工业大学 | Method for improving biological activity of composite coating on surface of titanium through micro-arc oxidation and water vapour treatment |
| CN104324974A (en) * | 2014-08-28 | 2015-02-04 | 攀钢集团成都钢钒有限公司 | Titanium alloy seamless pipe finishing method |
| CN105019001A (en) * | 2015-07-03 | 2015-11-04 | 西安理工大学 | Preparation method of NiTi alloy tooth arch wire for orthodontics |
| CN105316744A (en) * | 2015-11-30 | 2016-02-10 | 创生医疗器械（中国）有限公司 | Surface bright anodic oxidation coloring method for titanium and titanium alloy |
| CN105442019A (en) * | 2015-11-30 | 2016-03-30 | 常州奥斯迈医疗器械有限公司 | Anodic oxidation coloring method free of introducing of elements inconsistent with titanium and titanium alloy base materials |
| CN106350853A (en) * | 2016-11-03 | 2017-01-25 | 安阳工学院 | Method for electrochemical coloring of metallic titanium and titanium-based alloys |
| CN106702461A (en) * | 2016-12-28 | 2017-05-24 | 佛山市铠斯钛科技有限公司 | Titanium-magnesium alloy anodic oxidation solution |
| CN106725928A (en) * | 2016-12-12 | 2017-05-31 | 同济大学 | A kind of dental implant abutment and preparation method thereof |
| CN107236982A (en) * | 2017-06-29 | 2017-10-10 | 天津正天医疗器械有限公司 | Titanium or titanium alloy anode oxidation coloration technique |
| CN109402536A (en) * | 2018-11-05 | 2019-03-01 | 浙江飞剑科技有限公司 | A kind of titanium cup surface texture method |
| CN110191977A (en) * | 2017-01-18 | 2019-08-30 | 株式会社杰希优 | Coloring plating solution and color method |
| CN111020671A (en) * | 2020-01-16 | 2020-04-17 | 西安庄信新材料科技有限公司 | Method for forming oxide film on surface of titanium product |
| CN112425844A (en) * | 2020-12-08 | 2021-03-02 | 赵伟 | Bactericidal and bacteriostatic mask |
| CN112831817A (en) * | 2020-12-22 | 2021-05-25 | 北京钛古科技有限责任公司 | Anatase type biological titanium material and preparation method thereof |
| WO2022063230A1 (en) * | 2020-09-25 | 2022-03-31 | 北京华宇创新钽铌科技有限公司 | Method for manufacturing colored article and mobile phone case |
| CN116666581A (en) * | 2023-05-05 | 2023-08-29 | 贵州创德新能源科技有限公司 | Sodium ion battery anode material and preparation method thereof |
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| EP1199385A2 (en) * | 2000-10-19 | 2002-04-24 | CESCOR S.r.l. | Method of coloring titanium and its alloys through anodic oxidation |
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| EP1199385A2 (en) * | 2000-10-19 | 2002-04-24 | CESCOR S.r.l. | Method of coloring titanium and its alloys through anodic oxidation |
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Cited By (26)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102337574A (en) * | 2011-10-08 | 2012-02-01 | 中南大学 | Anode oxidization solution and oxidization method of broad titanium plate |
| CN103266338A (en) * | 2013-05-21 | 2013-08-28 | 沈阳理工大学 | TC4 titanium alloy anodizing chromium-free blackening method |
| CN103334144B (en) * | 2013-07-18 | 2016-06-29 | 哈尔滨工业大学 | The alkali liquor steam post-processing approach of titanium surface by micro-arc oxidation bioactivity coatings |
| CN103334144A (en) * | 2013-07-18 | 2013-10-02 | 哈尔滨工业大学 | Alkaline liquid water vapor post-treatment method of micro-arc oxidation biological active coating on surface of titanium |
| CN103343375A (en) * | 2013-07-18 | 2013-10-09 | 哈尔滨工业大学 | Method for improving biological activity of composite coating on surface of titanium through micro-arc oxidation and water vapour treatment |
| CN104324974A (en) * | 2014-08-28 | 2015-02-04 | 攀钢集团成都钢钒有限公司 | Titanium alloy seamless pipe finishing method |
| CN105019001A (en) * | 2015-07-03 | 2015-11-04 | 西安理工大学 | Preparation method of NiTi alloy tooth arch wire for orthodontics |
| CN105019001B (en) * | 2015-07-03 | 2017-11-03 | 西安理工大学 | A kind of preparation method of correction NiTi alloy dental arch filaments |
| CN105316744A (en) * | 2015-11-30 | 2016-02-10 | 创生医疗器械（中国）有限公司 | Surface bright anodic oxidation coloring method for titanium and titanium alloy |
| CN105442019A (en) * | 2015-11-30 | 2016-03-30 | 常州奥斯迈医疗器械有限公司 | Anodic oxidation coloring method free of introducing of elements inconsistent with titanium and titanium alloy base materials |
| CN105316744B (en) * | 2015-11-30 | 2017-11-14 | 创生医疗器械（中国）有限公司 | The surface-brightening method for anodizing and coloring of titanium or titanium alloy |
| CN106350853A (en) * | 2016-11-03 | 2017-01-25 | 安阳工学院 | Method for electrochemical coloring of metallic titanium and titanium-based alloys |
| CN106350853B (en) * | 2016-11-03 | 2018-10-23 | 安阳工学院 | A kind of method of Titanium and titanium-base alloy electrochemical coloring |
| CN106725928A (en) * | 2016-12-12 | 2017-05-31 | 同济大学 | A kind of dental implant abutment and preparation method thereof |
| CN106702461A (en) * | 2016-12-28 | 2017-05-24 | 佛山市铠斯钛科技有限公司 | Titanium-magnesium alloy anodic oxidation solution |
| CN110191977A (en) * | 2017-01-18 | 2019-08-30 | 株式会社杰希优 | Coloring plating solution and color method |
| CN110191977B (en) * | 2017-01-18 | 2022-04-26 | 株式会社杰希优 | Plating solution for coloring and coloring method |
| CN107236982A (en) * | 2017-06-29 | 2017-10-10 | 天津正天医疗器械有限公司 | Titanium or titanium alloy anode oxidation coloration technique |
| CN109402536B (en) * | 2018-11-05 | 2020-04-07 | 浙江飞剑科技有限公司 | Titanium cup surface texture processing method |
| CN109402536A (en) * | 2018-11-05 | 2019-03-01 | 浙江飞剑科技有限公司 | A kind of titanium cup surface texture method |
| CN111020671A (en) * | 2020-01-16 | 2020-04-17 | 西安庄信新材料科技有限公司 | Method for forming oxide film on surface of titanium product |
| WO2022063230A1 (en) * | 2020-09-25 | 2022-03-31 | 北京华宇创新钽铌科技有限公司 | Method for manufacturing colored article and mobile phone case |
| CN112425844A (en) * | 2020-12-08 | 2021-03-02 | 赵伟 | Bactericidal and bacteriostatic mask |
| CN112831817A (en) * | 2020-12-22 | 2021-05-25 | 北京钛古科技有限责任公司 | Anatase type biological titanium material and preparation method thereof |
| CN112831817B (en) * | 2020-12-22 | 2022-05-24 | 北京钛古科技有限责任公司 | Anatase type biological titanium material and preparation method thereof |
| CN116666581A (en) * | 2023-05-05 | 2023-08-29 | 贵州创德新能源科技有限公司 | Sodium ion battery anode material and preparation method thereof |
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Application publication date: 20110706 |