CN100595328C - Composition for surface treatment of light metal and its composite material - Google Patents
Composition for surface treatment of light metal and its composite material Download PDFInfo
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- CN100595328C CN100595328C CN200610141044A CN200610141044A CN100595328C CN 100595328 C CN100595328 C CN 100595328C CN 200610141044 A CN200610141044 A CN 200610141044A CN 200610141044 A CN200610141044 A CN 200610141044A CN 100595328 C CN100595328 C CN 100595328C
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Abstract
A combination used in surface treatment of light metal and related composite material contains water soluble rare-earth salts and oxidant, wherein, the oxidant is water soluble metavanadate. Due to adopting metavanadate as oxidant, the invention can substantially improve corrosion resistance and subsequent paint film adhesive force of the rare-earth conversion coating made by the combination.
Description
Technical field
The invention relates to a kind of surface-treated composition, especially about a kind of composition that is used for light metal and composite material surface processing thereof.
Background technology
Light metal and alloy thereof, for example aluminium, magnesium, aluminium alloy and magnesium alloy, but have that density is little, the conductive and heat-conductive ability is strong, mechanical property is excellent and advantage such as secondary processing, therefore in national economy, obtained using widely.The light metal matrix material generally makes by add the enhancing body in light metal or its alloy, except many advantages with light metal, also have outstanding advantages such as high specific tenacity, specific rigidity, wear resistance are good, therefore in fields such as space flight, aviation and automotive industry, be considered to one of the most promising type material.
But the protection against corrosion problem of light metal and matrix material thereof fails to be well solved always.Owing to exist number of drawbacks such as crystal boundary, inclusion, light metal surface to come down to a table heterogeneous, light metal and matrix material thereof are corroded when using in complex environment inevitably.And in the preparation process of light metal matrix material, having added a large amount of enhancing bodies, light metal composite inner weave construction is inhomogeneous, in use very easily forms corrosion cell, thereby makes the corrosion resistance variation of light metal matrix material.
In order to prevent the corrosion of light metal and matrix material thereof, chemical oxidization method at present commonly used and electrochemical oxidation process protect light metal and composite material surface thereof, wherein said chemical oxidization method, promptly by contacting, at the low compound rete of base metal surface formation of deposits one deck solubleness with corrosion mitigating effect with chemical pretreatment solution.Described compound is made up of oxide compound and metal-salt etc.Chemical oxidization method is little to material influence, technology is simple, with low cost, therefore obtained using widely.Traditional chemical oxidization method is mainly used chromate-containing treatment solution, though can reach anticorrosion ability preferably, this treatment solution contains toxic very big sexavalent chrome, contaminate environment, and the cost height disposes waste liquid.Methods such as the stannate processing that occurs afterwards, fluozirconate processing, cobaltates processing and molybdate processing, the rete of formation is thinner, and non-corrosibility can't reach the degree of chromate conversion coating.And phosphatizing can obtain the erosion resistance suitable with traditional chromic salt, but its shortcoming is that treatment solution consumption is fast through constantly research, and cost is higher.
Recently, occurred a kind of nontoxic, free of contamination rare-earth salts transformation processing method again, formed rare-earth conversion coatings at light metal and composite material surface thereof.For example, CN175228A discloses a kind of raising light metal and the corrosion proof rare-earth transfer film method of composite material surface thereof, this method may further comprise the steps: a, to light metal material or/and light metal-based composite material surface carries out pre-grinding handles, roughness is the 0.01-10 micron; B, will place acetone or alcohol solution that ultrasonic decontamination is carried out on its surface through the material that a step process is crossed to handle, the treatment time is 1-5 minute; C, will place basic solution to carry out oil removal treatment through the material that the b step process is crossed, solution temperature be a room temperature-60 ℃, and the treatment time is 1-5 minute; D, will place the rare earth salt aqueous solution that is added with oxygenant through the material that oil removal treatment is crossed, the concentration of rare earth salt aqueous solution is the 0.01-0.05 mol, the add-on of oxygenant be the 20-120 milliliter/liter, the temperature of mixing solutions is 20-100 ℃, treatment time is 5-20 minute, and the pH value of mixing solutions is 1-5; E, will at room temperature place at least 15 days or baking oven internal heating 1-24 hour, Heating temperature was 40-80 ℃ through the material that the d step process is crossed.Wherein, described oxygenant is H
2O
2, rare-earth salts is CeCl
3
The erosion resistance of the rare-earth conversion coatings that above-mentioned treatment process forms is relatively poor.In addition, chemical conversion film is thinner, and the erosion resistance of chemical conversion film be studies show that chemical conversion film can only slow down corrosion speed, can not effectively prevent corrosion.Therefore, in order further to prevent the corrosion of light metal and matrix material thereof, the film that chemical oxidization method forms need apply one or more layers paint film again as the surface of rare-earth conversion coatings, and the surface adhesion force of the rare-earth conversion coatings that existing treatment process obtains is lower, sticking power between paint film and the rare-earth conversion coatings is not enough, can not prevent the corrosion of light metal and matrix material thereof effectively.
Summary of the invention
The objective of the invention is to be used for the rare-earth conversion coatings corrosion-resistant that light metal and composite material surface thereof handle and the problem of follow-up paint film adhesion difference in the prior art, a kind of composition that can obtain the strong rare-earth conversion coatings of good corrosion resistance and follow-up paint film adhesion that is used for that light metal and composite material surface thereof handle is provided in order to overcome.
The invention provides a kind of composition that is used for light metal and composite material surface processing thereof, said composition contains water miscible rare-earth salts and oxygenant, and wherein, described oxygenant is water miscible metavanadate.
The composition that is used for light metal and composite material surface processing thereof provided by the invention uses metavanadate as oxygenant, can significantly improve the erosion resistance and the follow-up paint film adhesion of the rare-earth conversion coatings that is made by said composition.For example, after 8 hours, the surface corrosion area is below 1% to the magnesium alloy materials B1 that is obtained by embodiment 7 in the neutral salt spray spraying, and is more than 9% by the magnesium alloy materials BB1 that Comparative Examples 1 the obtains area that is corroded after the identical time; The follow-up paint film adhesion of the magnesium alloy materials that has adhered to chemical conversion film that is obtained by embodiment can be up to 5B, and the chemical conversion film that Comparative Examples 1 obtains has only 3B.
Embodiment
The composition that is used for light metal and composite material surface processing thereof provided by the invention contains water miscible rare-earth salts and oxygenant, and wherein, described oxygenant is water miscible metavanadate.
In composition of the present invention, the content of rare-earth salts and oxygenant can be conventional content, and for example, the content of described rare-earth salts is the 0.1-50 weight part, is preferably the 1-20 weight part; The content of described oxygenant is the 0.1-7 weight part, is preferably the 0.1-4.5 weight part.
Described metavanadate can be any water-soluble metavanadate, for example, can be in sodium metavanadate, potassium metavanadate or the ammonium meta-vanadate one or more.
The kind of described rare-earth salts has been conventionally known to one of skill in the art, can be selected from any water miscible lanthanum salt, cerium salt, praseodymium salt, bismuth salt, europium salt or the ytterbium salt one or more.For example, can be selected from Lanthanum trichloride, lanthanum bromide, lanthanum iodide, lanthanum sulfat, lanthanum nitrate, Cerium II Chloride, comprise cerium bromide, cerous iodide, cerous sulfate, cerous nitrate, praseodymium chloride, praseodymium bromide, praseodymium iodide, praseodymium sulfate, praseodymium nitrate, bismuth chloride, bismuth bromide, bismuth iodide, bismuth sulfate, Bismuth trinitrate, Europium trichloride, bromination europium, iodate europium, europium sulfate, europium nitrate, Ytterbium trichloride, ytterbium bromide, iodate ytterbium, ytterbium sulfate and the ytterbium nitrate one or more.
Under the preferable case, said composition also contains calcium salt.Calcium salt has corrosion inhibition, can act synergistically with rare-earth salts, plays the effect of the crystal grain of refinement rete, the porosity that reduces film, the erosion resistance that strengthens rete, increase sticking power, minimizing sediment, further improves the performance of the rare-earth conversion coatings of composition formation.The content of described calcium salt is the 0.1-40 weight part, is preferably the 3-9 weight part.Described calcium salt can be any water-soluble Ca salt, for example, can be in nitrocalcite, calcium chloride, Calcium Bromide and the calcium iodide one or more.
Under the preferable case, said composition also contains zinc salt.Zinc salt can quicken the formation of rare-earth conversion coatings, and can with the calcium salt codeposition, make rare-earth conversion coatings fine and close more.The content of described zinc salt is the 0.01-10 weight part, is preferably the 1-5 weight part.Described zinc salt can be any water-soluble zinc salt, for example, can be in zinc nitrate, zinc chloride, zinc bromide, zinc iodide or the zinc sulfate one or more.
Under the preferable case, said composition also contains P contained compound, and the content of described P contained compound is the 0.01-30 weight part, is preferably the 9-17 weight part.Described P contained compound can be any water-soluble P contained compound.For example, described P contained compound can be selected from one or more in phosphoric acid, phosphorous acid, Hypophosporous Acid, 50, sodium phosphate, potassiumphosphate, ammonium phosphate, sodium phosphite, potassium phosphite, ammonium phosphite, sodium hypophosphite, potassium hypophosphite and the ammonium hypophosphite.
Under the preferable case, said composition also comprises fluoroborate; Described fluoroborate can be any water-soluble fluorine borate, for example can be selected from Sodium tetrafluoroborate, potassium fluoborate and the ammonium borofluoride one or more.The content of described fluoroborate is the 0.05-25 weight part, is preferably the 3-5 weight part.
Above-mentioned fluoroborate and P contained compound can provide the acid radical anion of codeposition, make further passivation of surface, make rare-earth conversion coatings more even, fine and close.
The preparation of compositions method that the present invention is used for light metal and composite material surface processing thereof is simple, only said components need be mixed to get final product.
The described composition that is used for light metal and composite material surface processing thereof can be hybridly prepared into solution with water before using.The consumption of water is 1-50 a times of composition total weight, is preferably 5-40 doubly.Adding acid or alkali are adjusted to 1.0-3.0 with the pH value of solution value in the solution in the past, and described acid can be one or more in sulfuric acid, phosphoric acid, nitric acid or the hydrochloric acid, and described alkali can be sodium hydroxide and potassium hydroxide.The solution that can use above-mentioned preparation forms rare-earth conversion coatings according to the method for routine on the surface of light metal and matrix material thereof.Composition of the present invention is applicable to various light metals and matrix material thereof, for example, can be used for magnesium alloy, aluminium alloy etc.
Describe the present invention in detail below by embodiment.
Embodiment 1
Present embodiment is used for illustrating the composition that is used for light metal and composite material surface processing thereof provided by the invention.
1 gram lanthanum nitrate, 4.5 gram ammonium meta-vanadates, 8 gram calcium chloride, 15 gram potassiumphosphates, 3 gram zinc chloride and 4 gram potassium fluoborates are mixed, promptly get composition A1.
Embodiment 2
Present embodiment is used for illustrating the composition that is used for light metal and composite material surface processing thereof provided by the invention.
3 gram praseodymium chlorides, 2 gram sodium metavanadates, 5 gram calcium chloride, 17 gram sodium phosphites, 5 gram zinc chloride and 5 gram ammonium borofluorides are mixed, promptly get composition A2.
Embodiment 3
Present embodiment is used for illustrating the composition that is used for light metal and composite material surface processing thereof provided by the invention.
10 gram Bismuth trinitrates, 0.1 gram sodium metavanadate, 3 gram Calcium Bromides, 13 gram ammonium hypophosphites, 4 gram zinc nitrates and 5 gram Sodium tetrafluoroborates are mixed, promptly get composition A3.
Embodiment 4
Present embodiment is used for illustrating the composition that is used for light metal and composite material surface processing thereof provided by the invention.
15 gram europium nitrates, 4 gram potassium metavanadates, 7 gram nitrocalcite, 9 gram phosphoric acid, 2 gram zinc sulfate and 5 gram potassium fluoborates are mixed, promptly get composition A4.
Embodiment 5
Present embodiment is used for illustrating the composition that is used for light metal and composite material surface processing thereof provided by the invention.
20 gram ytterbium nitrates, 1 gram potassium metavanadate, 9 gram nitrocalcite, 11 gram phosphorous acid, 1 gram zinc chloride and 3 gram potassium fluoborates are mixed, promptly get composition A5.
Embodiment 6
Present embodiment is used for illustrating the composition that is used for light metal and composite material surface processing thereof provided by the invention.
5 gram Cerium II Chlorides and 4.5 gram ammonium meta-vanadates are mixed, promptly get composition A6.
Embodiment 7-12
These embodiment are used for illustrating the performance that is used for the rare-earth conversion coatings of the preparation of compositions that light metal and composite material surface thereof handle provided by the invention.
The whole of composition A1-A6 that the foregoing description 1-6 is obtained are dissolved in respectively in 1 premium on currency, regulate pH to 2 with the sulphuric acid soln of 1 mol, promptly get the rare earth chemistry conversion treating solution.
The magnesium alloy die casting that to get 6 models be AZ91D is polished to it earlier, removes unnecessary stub bar of magnesium alloy ground and burr.Place 150 ℃ baking oven to toast then 25 minutes.In 60 ℃ hot water, soaked 5 minutes again, take out, be put in 150 ℃ the baking oven baking once more 25 minutes, be cooled to normal temperature.Then, the magnesium alloy pressure-casting product after the pre-treatment is placed 45 ℃ above-mentioned rare earth conversion treating solution respectively, soaked 20 seconds, take out.Baking is 30 minutes in 150 ℃ baking oven, is cooled to normal temperature, promptly gets the magnesium alloy materials B1-B6 that has adhered to rare-earth conversion coatings.Respectively the above-mentioned magnesium alloy materials B1-B6 that makes is carried out neutral salt spray test and the test of follow-up paint film adhesion in accordance with the following methods, test result is as shown in table 1.
(1) neutral salt spray test (NSST)
In temperature is 35 ℃ testing laboratory, magnesium alloy materials B1-B6 is placed in the salt fog cabinet, under 46 ℃, spray with the air pressure of 1.0 ± 0.025 kilogram force/square centimeters with the sodium chloride brine that pH is 7.0, temperature is 35 ℃ 5 ± 0.5 weight %.At spraying sample after 8 hours, taking out and placing the another one temperature is that 22.5 ℃, relative humidity are the climatic chamber of 47.3%RH, places after 8 hours, and observation sample, the corroded area that writes down sample surfaces accounts for the per-cent of the coating total area.
(2) follow-up paint film adhesion test (GB/T 9286-1998)
Spraying a layer thickness on magnesium alloy materials B1-B6 surface with the high-pressure air spraying method is 15 microns paint film coating (KUBO KO (Kubo filial piety) company production, model is 670-065), baking is 25 minutes in 150 ℃ IR baking oven, then according to GB/T 9286-1998 test paint film adhesion.
Comparative Examples 1
This Comparative Examples is used to illustrate that documents CN175228A provides is used for the performance of the rare-earth conversion coatings of the treatment solution preparation that light metal and composite material surface thereof handle.
Embodiment 12 preparation rare-earth conversion coatings according to documents CN175228A.
5 gram Cerium II Chlorides and 100 milliliters of hydrogen peroxide are mixed, be mixed with 1 liter the aqueous solution then, regulate pH to 2.8, promptly get the rare earth chemistry conversion treating solution with the sulphuric acid soln of 1 mol.
It is existing to model to be that the magnesium alloy die casting of the magnesium alloy die casting of AZ91D carries out pre-grinding place, and roughness is 1 micron, uses deionized water rinsing then; Again above-mentioned die casting is placed acetone soln, carry out ultrasonic decontamination and handle, handled 5 minutes, use deionized water rinsing again; Place basic solution to carry out oil removal treatment then, solution temperature is 25 ℃, and the treatment time is 5 minutes, uses deionized water rinsing again; Be placed on then in the above-mentioned rare earth chemistry conversion treating solution, temperature is 25 ℃, and the treatment time is 10 minutes.The material that to handle was 80 ℃ baking oven internal heating 10 hours again.Then, it is that 2.5 weight %, pH soaked 5 minutes in 4.5 the sodium radio-phosphate,P-32 solution that this material is placed on concentration, has obtained adhering to the magnesium alloy materials BB1 of rare-earth conversion coatings.
According to the method identical with embodiment 7-12 rare-earth conversion coatings BB1 is carried out neutral salt spray test and the test of follow-up paint film adhesion, test result is as shown in table 1.
Table 1
| Numbering | B1 | B2 | B3 | B4 | B5 | B6 | BB1 |
| Neutral salt spray corroded area (area %) | ≤1 | ≤2 | ≤1 | ≤1 | ≤2 | ≤3 | ≥9 |
| Follow-up paint film adhesion (B) | 5B | 5B | 5B | 5B | 5B | 4B | 3B |
As can be seen from Table 1, the erosion resistance of the rete B1-B6 that embodiment 7-12 obtains is extremely strong, and after salt air corrosion, the surface is corroded area all below 3%, and Comparative Examples obtains rete and is corroded and amasss more than 9%; In addition, the rete B1-B6 that embodiment 7-12 obtains on follow-up doped envelope sticking power all is better than the rete that Comparative Examples 1 obtains.
Claims (12)
1, a kind of composition that is used for light metal and composite material surface processing thereof, said composition contains oxygenant and water miscible rare-earth salts or bismuth salt, it is characterized in that, described oxygenant is water miscible metavanadate, wherein, said composition also contains water-soluble P contained compound, and the content of described P contained compound is the 0.01-30 weight part, and described light metal and matrix material thereof are magnesium, aluminium, magnesium alloy or aluminium alloy.
2, composition according to claim 1, wherein, the content of described water miscible rare-earth salts or bismuth salt is the 0.1-50 weight part, the content of described oxygenant is the 0.1-7 weight part.
3, composition according to claim 2, wherein, the content of described water miscible rare-earth salts or bismuth salt is the 1-20 weight part, the content of described oxygenant is the 0.1-4.5 weight part.
4, composition according to claim 1, wherein, described metavanadate is selected from one or more in sodium metavanadate, potassium metavanadate and the ammonium meta-vanadate.
5, composition according to claim 1, wherein, described composition contains oxygenant and water-solubility rare-earth salt, and described rare-earth salts is selected from one or more in water miscible lanthanum salt, cerium salt, praseodymium salt, europium salt and the ytterbium salt.
6, composition according to claim 1, wherein, said composition also contains water-soluble Ca salt; The content of described calcium salt is the 0.1-40 weight part.
7, composition according to claim 6, wherein, described calcium salt is selected from one or more in nitrocalcite, calcium chloride, Calcium Bromide and the calcium iodide.
8, composition according to claim 1, wherein, described P contained compound is selected from one or more in phosphoric acid, phosphorous acid, Hypophosporous Acid, 50, sodium phosphate, potassiumphosphate, ammonium phosphate, sodium phosphite, potassium phosphite, ammonium phosphite, sodium hypophosphite, potassium hypophosphite and the ammonium hypophosphite.
9, composition according to claim 1, wherein, said composition also contains water-soluble zinc salt; The content of zinc salt is the 0.01-10 weight part.
10, composition according to claim 9, wherein, described zinc salt is selected from one or more in zinc nitrate, zinc chloride, zinc bromide, zinc iodide and the zinc sulfate.
11, composition according to claim 1, wherein, said composition also comprises the water-soluble fluorine borate; The content of fluoroborate is the 0.05-25 weight part.
12, composition according to claim 11, wherein, described fluoroborate is selected from one or more in Sodium tetrafluoroborate, potassium fluoborate and the ammonium borofluoride.
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101748396B (en) * | 2008-12-02 | 2011-08-31 | 中国科学院兰州化学物理研究所 | Preparation method of magnesium alloy rare-earth conversion coatings for ethylene glycol cooling system |
| CN102234799B (en) * | 2011-07-29 | 2012-12-05 | 西安建筑科技大学 | Zinc layer surface conversion film forming liquid, and application method thereof |
| CN102409330A (en) * | 2011-11-25 | 2012-04-11 | 潍坊学院 | Chromium-free passivation solution |
| CN102851659B (en) * | 2012-09-29 | 2014-06-18 | 西安建筑科技大学 | Magnesium alloy surface phosphorus-free chromium-free conversion coating and application method thereof |
| CN106854760A (en) * | 2016-12-20 | 2017-06-16 | 深圳市新合富力科技有限公司 | Superconduct film agent, preparation method and its method to Mg alloy surface treatment |
| WO2019006624A1 (en) * | 2017-07-03 | 2019-01-10 | 深圳市盈恒科技有限公司 | Chromium-free passivator, aluminum product and surface passivation process therefor |
| WO2019006674A1 (en) * | 2017-07-04 | 2019-01-10 | 深圳市长宏泰科技有限公司 | Magnesium alloy phosphating agent, metal component, and surface phosphating treatment method therefor |
| CN107557800B (en) * | 2017-09-20 | 2019-12-24 | 旌德君创科技发展有限公司 | Environment-friendly pickling solution applied to aluminum product |
| CN109233587A (en) * | 2018-08-30 | 2019-01-18 | 徐州市茗尧机械制造有限公司 | A kind of building machinery surface treating agent |
| CN110684970A (en) * | 2019-09-26 | 2020-01-14 | 博罗县东明化工有限公司 | Treatment method of magnesium alloy conversion film and conversion agent |
| CN113235077A (en) * | 2021-05-11 | 2021-08-10 | 齐齐哈尔北方集团北方化学工业有限责任公司 | Aluminum alloy vanadium-titanium-europium passivation solution and preparation and use method thereof |
| CN115305546B (en) * | 2022-08-31 | 2023-05-19 | 佛山力邦通信设备科技有限公司 | Inside-outside different oxidation process for aluminum alloy special-shaped cavity |
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