CN103266315A - Preparation method of aluminum alloy cobalt salt chemical conversion coating treating fluid - Google Patents
Preparation method of aluminum alloy cobalt salt chemical conversion coating treating fluid Download PDFInfo
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- CN103266315A CN103266315A CN2013102121472A CN201310212147A CN103266315A CN 103266315 A CN103266315 A CN 103266315A CN 2013102121472 A CN2013102121472 A CN 2013102121472A CN 201310212147 A CN201310212147 A CN 201310212147A CN 103266315 A CN103266315 A CN 103266315A
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Abstract
The invention relates to a preparation method of aluminum alloy cobalt salt chemical conversion coating treating fluid, belonging to the field of aluminum alloy surface treatment. A porous chemical conversion coating formed by treating aluminum alloy through treating fluid has the characteristics of no chromium, environment friendliness, and good corrosion resistance property, and the like, the treating fluid is prepared from cobalt salt, oxidant, ligand and water, wherein per liter of cobalt salt chemical conversion treating fluid contains the following compositions by weight: 20-50g of cobalt salt, 1-50g of an oxidant, and 2-7g of ligand, and the PH value of the treating fluid ranges from 3 to 4; the cobalt salt is selected from one or two of cobalt-nitrate hydrate and cobalt-chloride hydrate; the oxidant is selected from one or more of lithium permanganate, sodium permanganate, ammonia permanganate and calcium permanganate; and the ligand is selected from one or two of sodium nitrite or sodium acetate.
Description
Technical field
The present invention relates to the processing of aviation alloyed aluminium decoration and protective coating.Be specially a kind for the treatment of process of aviation alloyed aluminium environment-friendly chromium-free chemical conversion film, formed multi-hole type chemical conversion film has good solidity to corrosion and coating adhesion after sealing, can replace traditional chromic salts chemical conversion treatment process.
Background technology
Fine aluminium and aluminium alloy are exposed in the air can form the natural oxidation film layer of one deck, but thinner thickness is damaged easily, and solidity to corrosion is relatively poor.Need to handle with coating, existing two classes transform rete and are used for coating, adopt porous anode method and chemical oxidization method to handle respectively and obtain for this reason.
Chemical oxidation treatment is at a certain temperature, makes metallic aluminium and oxidizing solution generation chemical reaction, generates the technology of insoluble oxide film on the surface.Chemical oxide film is bigger 100～200 times than natural oxidation film thickness, compares with anode oxide film, has advantages such as simple to operate, that equipment is simple, cost is low, formation speed is fast, tack is good, can make protective layer separately or as the application bottom.Shortcoming is that the rete quality is soft, wears no resistance, and the carrying occasion is destroyed easily.
The chemical method for treating surface of aluminium and aluminium alloy is mainly the chromate conversion embrane method.Formed chromic acid conversion film has that film formation time is short, thinner, the anti-corrosion type of rete is good, to advantages such as the influence of substrate anti-fatigue performance are little; but not only can producing in treating processes, chromate treating technology pollutes; and the hexavalent chromium compound that uses in the conversion of chromic salt chemistry is extremely malicious chemical substance; have strong toxicity and carcinogenesis; be that the WEES of European Union and RoHS instruction clearly propose strictness and limit its use at be ranked first 7 highly toxic material of USEPA (ERA).China also announced in 2003, and chromic salt is carried out uses of limiting the quantity of, and sought replacing of chromic salt and treated this work of thing oneself is imperative.
The research and development of aluminium alloy non-chromium transformation technology mainly concentrate on following several big system: the conversion of titanium zirconates, molybdate conversion, organic acid chemical conversion, the conversion of high-valency metal salt, the conversion of lithium hydrochlorate, rare-earth salts chemical conversion etc.Wherein cobalt salt conversion processing development is later, belongs to Chrome-free and transforms new technology, is characterized in that the rete contact resistance is low, solidity to corrosion good, and is combined goodly with coating, has been applied to the surface treatment of aerospace, electronics and communication products.
Chinese patent literature CN93101737.8 discloses a kind of preparation method of aluminum alloy surface cobalt salt chemical conversion film.Wherein oxygenant is selected hydrogen peroxide for use.
Originally discover and adopt hydrogen peroxide as oxygenant following shortcoming to be arranged, the strong impulse smell is arranged, and consumption is big, and the compound method complexity is not suitable for extensive use.
For this this research improves the method for cobalt salt chemical conversion, select for use permanganate as oxidation promotor, be mixed with a kind of new cobalt salt chemical conversion treatment solution, it has advantages such as consumption is few, and film layer structure is flexible adjustable.
Summary of the invention
The objective of the invention is to overcome the problem that prior art exists, as the harm of sexavalent chrome to environment and human body, provide a kind of low cost to form the cobalt salt chemical conversion processing method of flexible film layer structure in aluminum alloy surface.
Purpose of the present invention can realize by following technical solution.
A kind of aluminium alloy cobalt salt chemical conversion membrane processing method said method comprising the steps of:
1, aluminum alloy surface pre-treatment;
2, handle with the cobalt salt chemical conversion treatment solution;
3, ultrasonic washing with clean water, oven dry.
Wherein, step 1, described pre-treatment, method is as follows:
(1) soak oil removing with degreaser, soak time is 10～30min, to remove the greasy dirt that machining surface adds man-hour;
(2) clear water washing;
(3) put into 60～80 ℃ of basic solutions and soaked 30～60 seconds, removing surperficial thin native oxide layer,
(4) clear water washing,
(5) soaked 30～60 seconds neutralization with dilute nitric acid solution;
(6) clear water washing again.
Wherein said degreaser is selected from: dehydrated alcohol, acetone and other organic solvent.
Described basic solution is: yellow soda ash and sodium hydroxide solution, every liter of basic solution contains 10～20g yellow soda ash and 15～30g sodium hydroxide.
Described dilute nitric acid solution is: the dilute nitric acid solution of 10～30% volume percent.
Wherein, step 2, described processing, method is as follows:
Will be through step 1, pretreated aluminium alloy is put into the cobalt salt chemical conversion treatment solution, soaks under 40～70 ℃ temperature, and the time is 10～30min.Wherein said cobalt salt chemical conversion treatment solution is by cobalt salt, oxygenant, part, and water is formulated, and wherein, every liter of cobalt salt chemical conversion treatment solution contains 20～50g cobalt salt, 1～50g oxygenant, and 2～7g part, the pH value for the treatment of solution is between 3～4.Wherein said cobalt salt is selected from one or both in nitric hydrate cobalt and the hydration cobaltous chlorate; Described oxygenant is selected from one or more in high manganese lithium, sodium permanganate, potassium permanganate, ammonium permanganate, the calcium permanganate; Described part is selected from one or both in Sodium Nitrite or the sodium acetate; The compound method of cobalt salt chemical conversion treatment solution is as follows: dissolve cobalt salt earlier, dissolved oxidant adds part at last then.Adopt nitric acid or sodium hydroxide that the pH value for the treatment of solution is reconciled between 3～4.
The present invention is with respect to prior art, and its advantage is as follows:
(1) the present invention is applicable to the aviation alloyed aluminium surface conversion treatment.Do not contain sexavalent chrome and trivalent chromium to environment and human body harmful in the coating.
(2) adopting permanganate is oxygenant, and when oxygenate content was 1～10g/L, the film layer structure that forms in aluminum alloy surface was multi-hole type, identical with in the past cobalt salt conversion film structure, must carry out the secondary sealing; When accelerator content was 10～50g/L, film layer structure was dense form, need not to seal.
For further specifying advantage of the present invention, now provide of the present invention and contrast experiment prior art:
Prior art: Chinese patent literature CN93101737.8 disclosed method,
The technology of the present invention: the method for the embodiment of the invention 1,
Handle same batch 10 kilograms of aluminum alloy materials with above-mentioned two kinds of methods, result such as following table:
| ? | Treatment effect | The treatment solution consumption | Treatment time | Solution | Cost |
| Prior art | Outward appearance is inhomogeneous, and aberration is arranged | 50L | 20min | Produce a large amount of foams, the solution instability | 1983.25 unit/ton |
| The technology of the present invention | Outward appearance is even, no color differnece | 30L | 20min | Solution-stabilized | 1887.5 unit/ton |
Through above contrast experiment, prove that method treatment effect of the present invention is good, more superior than prior art.
Description of drawings
The scanning electron microscope diagram of Fig. 1 embodiment 1.
The scanning electron microscope diagram of Fig. 2 embodiment 3.
Embodiment
The present invention will be further described below in conjunction with example.
Embodiment 1:
1060 aluminum alloy surface cobalt salt chemical conversion process comprise the steps:
(1) aluminum alloy surface pretreatment process
At first 1060 aluminum alloy specimens are put into the degreaser oil removing, to remove the greasy dirt that machining surface adds man-hour, soak time is 10min;
Put into 70 ℃ of basic solution 40s after the clear water washing and remove surperficial thin native oxide layer, every liter of basic solution is made up of 10g yellow soda ash and 25g sodium hydroxide; After the clear water washing, put into the dilute nitric acid solution dipping 40s neutralization of 25% volume percent; Last clear water washing.
(2) configuration of cobalt salt chemical conversion treatment solution: every liter of cobalt salt chemical conversion treatment solution contains 30g hydration cobaltous chlorate, the 2g high manganese lithium, and the 2g sodium permanganate, 3g part Sodium Nitrite, the pH value for the treatment of solution are 3.
(3) chemical conversion of aluminum alloy surface cobalt salt is handled, and is that the sample that pre-treatment is good is put into 50 ℃ of cobalt salt chemical conversion treatment solutions that configure, and the time is 20min, takes out the back running water wash, ultrasonic washing with clean water 5min then, hot-air seasoning.
Embodiment 2:
2117 aluminum alloy surface cobalt salt chemical conversion process comprise the steps:
(1) the aluminum alloy surface pretreatment process is with embodiment 1
(2) configuration of cobalt salt chemical conversion treatment solution: every liter of cobalt salt chemical conversion treatment solution contains 30g hydration cobaltous chlorate, the 6g high manganese lithium, and the 6g sodium permanganate, 3g part Sodium Nitrite, the pH value for the treatment of solution are 3.
(3) chemical conversion of aluminum alloy surface cobalt salt is handled, and is that the sample that pre-treatment is good is put into 50 ℃ of cobalt salt chemical conversion treatment solutions that configure, and the time is 20min, takes out the back running water wash, ultrasonic washing with clean water 5min then, hot-air seasoning.
Embodiment 3:
7050 aluminum alloy surface cobalt salt chemical conversion process comprise the steps:
(1) aluminum alloy surface pretreatment process
At first 7050 aluminum alloy specimens are put into the degreaser oil removing, to remove the greasy dirt that machining surface adds man-hour, soak time is 20min;
Put into 60 ℃ of basic solution 30s after the clear water washing and remove surperficial thin native oxide layer, every liter of basic solution is made up of 20g yellow soda ash and 15g sodium hydroxide; After the clear water washing, put into the dilute nitric acid solution dipping 30s neutralization of 35% volume percent; Last clear water washing.
(2) configuration of cobalt salt chemical conversion treatment solution: every liter of cobalt salt chemical conversion treatment solution contains, 20g hydration cobaltous chlorate, and 10g nitric hydrate cobalt, the 20g high manganese lithium, the 10g sodium permanganate, 3g part Sodium Nitrite, the pH value for the treatment of solution are 4.
(3) chemical conversion of aluminum alloy surface cobalt salt is handled, and is that the sample that pre-treatment is good is put into 60 ℃ of cobalt salt chemical conversion treatment solutions that configure, and the time is 15min, takes out the back running water wash, ultrasonic washing with clean water 6min then, hot-air seasoning.
Claims (4)
1. cobalt salt chemical conversion treatment solution, by cobalt salt, oxygenant, part, water is formulated, and wherein, every liter of cobalt salt chemical conversion treatment solution contains 20～50g cobalt salt, 1～50g oxygenant, 2～7g part, the pH value for the treatment of solution is between 3～4; Wherein said cobalt salt is selected from one or both in nitric hydrate cobalt and the hydration cobaltous chlorate; Described oxygenant is selected from one or more in high manganese lithium, sodium permanganate, potassium permanganate, ammonium permanganate, the calcium permanganate; Described part is selected from one or both in Sodium Nitrite or the sodium acetate.
2. according to the treatment solution of claim 1, it is characterized in that: it consists of: every liter of cobalt salt chemical conversion treatment solution contains 30g hydration cobaltous chlorate, the 2g high manganese lithium, and the 2g sodium permanganate, 3g part Sodium Nitrite, the pH value for the treatment of solution are 3.
3. according to the treatment solution of claim 1, it is characterized in that: it consists of: every liter of cobalt salt chemical conversion treatment solution contains 30g hydration cobaltous chlorate, the 6g high manganese lithium, and the 6g sodium permanganate, 3g part Sodium Nitrite, the pH value for the treatment of solution are 3.
4. according to the treatment solution of claim 1, it is characterized in that: it consists of: every liter of cobalt salt chemical conversion treatment solution contains, 20g hydration cobaltous chlorate, and 10g nitric hydrate cobalt, the 20g high manganese lithium, the 10g sodium permanganate, 3g part Sodium Nitrite, the pH value for the treatment of solution are 4.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756969A (en) * | 2017-01-23 | 2017-05-31 | 江苏理工学院 | A kind of cobalt salt black chemical oxidation liquid and its application for aluminium and aluminium alloy |
| CN108103493A (en) * | 2018-01-03 | 2018-06-01 | 江苏理工学院 | A kind of aluminum alloy cobalt salt chemical conversion solution circulation utilization method |
| CN108165973A (en) * | 2018-01-03 | 2018-06-15 | 江苏理工学院 | A kind of recycling method of cobalt salt chemical conversion solution |
| CN108179408A (en) * | 2018-01-03 | 2018-06-19 | 江苏理工学院 | A kind of cobalt salt chemical conversion solution and its application |
| CN108220947A (en) * | 2018-01-03 | 2018-06-29 | 江苏理工学院 | A kind of cobalt salt chemical conversion solution recycling method |
| CN108330481A (en) * | 2016-08-14 | 2018-07-27 | 深圳市创汇信息科技有限公司 | A kind of preparation method of the aqueous solution containing cobalt |
| CN109972131A (en) * | 2019-03-27 | 2019-07-05 | 江苏理工学院 | A kind of preparation method of aluminum alloy surface cobalt salt conversion film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1090338A (en) * | 1992-06-25 | 1994-08-03 | 波音公司 | The non-chromate oxide membranous layer of aluminum substrate |
| CN101693995A (en) * | 2009-09-08 | 2010-04-14 | 上海波平航空科技有限公司 | Preparation method of aluminum alloy corrosion resistant coating |
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2013
- 2013-05-31 CN CN201310212147.2A patent/CN103266315B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1090338A (en) * | 1992-06-25 | 1994-08-03 | 波音公司 | The non-chromate oxide membranous layer of aluminum substrate |
| CN101693995A (en) * | 2009-09-08 | 2010-04-14 | 上海波平航空科技有限公司 | Preparation method of aluminum alloy corrosion resistant coating |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108330481A (en) * | 2016-08-14 | 2018-07-27 | 深圳市创汇信息科技有限公司 | A kind of preparation method of the aqueous solution containing cobalt |
| CN106756969A (en) * | 2017-01-23 | 2017-05-31 | 江苏理工学院 | A kind of cobalt salt black chemical oxidation liquid and its application for aluminium and aluminium alloy |
| CN108103493A (en) * | 2018-01-03 | 2018-06-01 | 江苏理工学院 | A kind of aluminum alloy cobalt salt chemical conversion solution circulation utilization method |
| CN108165973A (en) * | 2018-01-03 | 2018-06-15 | 江苏理工学院 | A kind of recycling method of cobalt salt chemical conversion solution |
| CN108179408A (en) * | 2018-01-03 | 2018-06-19 | 江苏理工学院 | A kind of cobalt salt chemical conversion solution and its application |
| CN108220947A (en) * | 2018-01-03 | 2018-06-29 | 江苏理工学院 | A kind of cobalt salt chemical conversion solution recycling method |
| CN109972131A (en) * | 2019-03-27 | 2019-07-05 | 江苏理工学院 | A kind of preparation method of aluminum alloy surface cobalt salt conversion film |
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Address after: 226602 No. 88 Hainan Road, Haian Town, Haian City, Nantong City, Jiangsu Province Patentee after: Haian Shenling Electrical Appliance Manufacturing Co., Ltd. Address before: 226600 No. 8 Hainan Road, Haian High-tech Zone, Haian County, Jiangsu Province Patentee before: Haian Shenling Electrical Appliance Manufacturing Co., Ltd. |