CN108330475B - High-corrosion-resistance marine aluminum alloy surface metal-organic framework film treatment liquid and use method thereof - Google Patents
High-corrosion-resistance marine aluminum alloy surface metal-organic framework film treatment liquid and use method thereof Download PDFInfo
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
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Abstract
The invention relates to the technical field of metal surface treatment, in particular to a high-corrosion-resistance marine aluminum alloy surface metal-organic framework film treatment liquid and a using method thereof. The treatment fluid is prepared from the following components: 25-1600ppm of 45% fluorozirconic acid, 12.5-1000ppm of 50% fluotitanic acid, 5-120ppm of manganese difluoride, 25-600ppm of glucose, 5-40ppm of 50% sodium sulfate and the balance of water. And forming a metal-organic framework film by coating the treatment liquid on the surface of the aluminum alloy. According to the metal-organic framework film treatment liquid, fluozirconic acid and fluotitanic acid are used for providing metal ions, glucose is used for providing organic unsaturated bonds, and the metal ions are combined to form a framework, so that the adhesion and precipitation of aluminum oxide are facilitated, the film formation is easy, the corrosion resistance and the adhesion of the framework film are improved, and meanwhile, a chromium-free raw material is adopted, so that the metal-organic framework film treatment liquid is environment-friendly and pollution-free.
Description
Technical Field
The invention relates to the technical field of metal surface treatment, in particular to a high-corrosion-resistance marine aluminum alloy surface metal-organic framework film treatment liquid and a using method thereof.
Background
The aluminum alloy plate has better corrosion resistance, so the aluminum alloy plate is widely applied to the fields of electronic production sheets, aviation, building materials, machinery, ships and warships and the like. When the chromate is applied to ships and warships, the aluminum alloy surface is easily corroded due to long-term wet environment, and the chromate is used as a corrosion inhibitor and is applied to aluminum alloy surface treatment. The corrosion resistance of the surface of the aluminum alloy is improved by directly contacting a chromium-containing treatment liquid such as chromic acid-chromate with the surface of the metal material to precipitate a chromate film thereon, or coating the chromate film on the surface of the metal material to precipitate the chromate film thereon after drying. However, hexavalent chromium is extremely harmful to the human body and the environment, and its application is strictly limited at present. A chromium-free metal surface treatment liquid is developed, wherein in a patent with the publication number of CN101535528A, an acid solution is obtained by properly changing the concentration of zirconium, titanium or a mixture thereof and adding 0.3-3 g/L divalent zinc and controlling the pH value to be 2.2-3.8, and the chromium-free metal surface treatment liquid can be applied to the construction of a vehicle body of a motor vehicle, the manufacturing of a ship, the construction industry and the production of large household appliances. However, the converted layer obtained by this method is liable to cause a significant difference in the film layer in production due to changes in the ambient temperature and the processing time, and the adhesion property to paint or powder is thereby deteriorated. Therefore, it is an urgent technical problem to be solved in the art to provide a safe and environment-friendly aluminum alloy surface treatment solution with high corrosion resistance and adhesion.
Disclosure of Invention
The invention aims to provide a metal-organic framework film treatment solution for the surface of a marine aluminum alloy, which is safe and environment-friendly and has high corrosion resistance and adhesion, and a use method thereof.
The invention adopts the following technical scheme:
the metal-organic framework film treatment liquid for the high-corrosion-resistance marine aluminum alloy surface is prepared from the following components in parts by weight: 25-1600ppm of 45% fluorozirconic acid, 12.5-1000ppm of 50% fluotitanic acid, 5-120ppm of manganese difluoride, 25-600ppm of glucose, 5-40ppm of 50% sodium sulfate and the balance of water.
Further, the pH value of the treatment liquid is 3-6, and is adjusted by adding hydrofluoric acid, sulfuric acid, ammonia water or sodium hydroxide.
The invention also provides a use method of the high-corrosion-resistance marine aluminum alloy surface metal-organic framework film treatment liquid, which is used for forming a framework film on the surface of the marine aluminum alloy, and the specific preparation process is as follows:
(1) polishing the surface of the aluminum alloy by using silicon carbide water sand paper until the surface roughness is below 10 mu m, soaking the aluminum alloy in an acid degreasing aqueous solution for 2 to 6 minutes, washing the aluminum alloy by using clear water, repeating the operation twice, and naturally airing or air-drying the aluminum alloy;
(2) carrying out chemical conversion treatment on the aluminum alloy by using the treatment liquid for 60s-8 min;
(3) and (3) cleaning the aluminum alloy subjected to the chemical conversion treatment in the step (2) with water, and naturally airing or drying.
Further, the chemical conversion treatment in the step (2) is to soak the aluminum alloy in the treatment solution for 3-8 min.
Further, the chemical conversion treatment in the step (2) is to directly spray the treatment liquid on the surface of the aluminum alloy for 1-4min, wherein the spraying pressure is 0.01-0.12 KPa.
Further, the chemical conversion treatment in the step (2) is to coat the treatment liquid on the surface of the aluminum alloy for 60-90 s.
Further, in the cleaning process in the step (3), the aluminum alloy is chemically treated in a spraying or soaking mode, and after treatment, the surface of the aluminum alloy is washed once by clean water and then cleaned by clean water with the conductivity of less than 200 mu s/cm; the aluminum alloy chemically treated by adopting a coating mode is directly cleaned by washing after treatment.
Further, in the step (3), the drying temperature is 30-100 ℃, and the drying time is 8-12 min.
The high-corrosion-resistance marine aluminum alloy surface metal-organic framework film treatment liquid and the use method thereof have the following beneficial effects:
(1) the metal-organic framework film treatment liquid provided by the invention uses fluozirconic acid and fluotitanic acid to provide metal ions, glucose provides organic unsaturated bonds, and the metal ions are combined to form a framework, so that the adhesion and precipitation of aluminum oxide are facilitated, the film formation is easy, the corrosion resistance and the adhesion of the framework film are improved, and meanwhile, the addition of manganese difluoride and sodium sulfate provides free fluoride ions and other ions for the treatment liquid, so that the control of the reaction of the treatment liquid in the film formation direction during the reaction on the surface of the aluminum alloy is facilitated, the film formation process is accelerated, and the film formation effect is optimized
(2) The pH value of the metal-organic framework film treatment liquid is between 3 and 6, the effective process range is wide, the defect that the batch production is limited due to the narrow process range of the conventional chromium-free passivation liquid is fully overcome, and the treatment liquid can be widely applied to the surface treatment of metal materials such as aluminum alloy and the like.
(3) The application method of the metal-organic framework film treatment liquid for the high-corrosion-resistance marine aluminum alloy surface adopts a chromium-free raw material to form the framework film on the aluminum alloy surface, is environment-friendly and pollution-free, and the prepared framework film has a high corrosion-resistance effect, is favorable for ships to resist the corrosion of seawater and the influence of a humid environment in marine climate, and meanwhile, the framework film formed by the application method has good adhesion to paint, coating and the like, and is favorable for improving the aesthetic degree of the ships.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The metallic materials used in the following examples:
the domestic aluminum-magnesium alloy section 5083 with the thickness of 1mm comprises the following main components: 0.35%, Mg: 0.8 to 0.9%, Si: 0.65 to 0.75%, Cu: 0.85-0.95%, Mn: 0.15-0.25% and the balance of Al.
The surface of the above-mentioned metal material was cleaned according to the acidic degreasing aqueous solution of patent CN201010206660.7 or CN201010543878.1 and then used for the surface treatment of the following examples.
Example 1
The metal-organic framework film treatment liquid for the high-corrosion-resistance marine aluminum alloy surface is prepared from the following components in parts by weight: 1000ppm of fluorozirconic acid with a concentration of 45%, 600ppm of fluorotitanic acid with a concentration of 50%, 30ppm of manganese difluoride, 400ppm of glucose, 10ppm of sodium sulfate with a concentration of 50%, and the balance of water. The pH of the treatment solution was adjusted to 4.
The application method of the metal-organic framework film treatment liquid for the surface of the high-corrosion-resistance marine aluminum alloy in the embodiment is used for forming a framework film on the surface of the marine aluminum alloy, and the specific preparation process is as follows:
(1) polishing the surface of the aluminum alloy by using silicon carbide water sand paper until the surface roughness is below 10 mu m, soaking in an acid degreasing aqueous solution for 6 minutes, washing by using clear water, repeating the operation twice, and naturally airing or air-drying;
(2) carrying out chemical conversion treatment on the aluminum alloy by using the treatment solution, namely soaking the aluminum alloy in the treatment solution for 3 min;
(3) washing the aluminum alloy subjected to chemical conversion treatment in the step (2) with clean water for one time, and then cleaning with clean water with the conductivity of less than 200 mu s/cm; and then drying at the temperature of 30 ℃ for 12 min.
Example 2
The metal-organic framework film treatment liquid for the high-corrosion-resistance marine aluminum alloy surface is prepared from the following components in parts by weight: 100ppm of fluorozirconic acid with a concentration of 45%, 800ppm of fluorotitanic acid with a concentration of 50%, 90ppm of manganese difluoride, 100ppm of glucose, 10ppm of sodium sulfate with a concentration of 50%, and the balance of water. The pH of the treatment solution was adjusted to 3.
The application method of the metal-organic framework film treatment liquid for the surface of the high-corrosion-resistance marine aluminum alloy in the embodiment is used for forming a framework film on the surface of the marine aluminum alloy, and the specific preparation process is as follows:
(1) polishing the surface of the aluminum alloy by using silicon carbide water sand paper until the surface roughness is below 10 mu m, soaking in an acid degreasing aqueous solution for 3 minutes, washing by using clear water, repeating the operation twice, and naturally airing or air-drying;
(2) carrying out chemical conversion treatment on the aluminum alloy by using the treatment liquid, namely directly spraying the treatment liquid on the surface of the aluminum alloy for 1min, wherein the spraying pressure is 0.12 KPa;
(3) washing the surface of the aluminum alloy subjected to the chemical conversion treatment in the step (2) with clean water for one time, and then cleaning with clean water with the conductivity of less than 200 mu s/cm; and then naturally airing.
Example 3
The metal-organic framework film treatment liquid for the high-corrosion-resistance marine aluminum alloy surface is prepared from the following components in parts by weight: 1200ppm of fluorozirconic acid with a concentration of 45%, 200ppm of fluorotitanic acid with a concentration of 50%, 100ppm of manganese difluoride, 500ppm of glucose, 20ppm of sodium sulfate with a concentration of 50%, and the balance of water. The pH of the treatment solution was adjusted to 6.
The application method of the metal-organic framework film treatment liquid for the surface of the high-corrosion-resistance marine aluminum alloy in the embodiment is used for forming a framework film on the surface of the marine aluminum alloy, and the specific preparation process is as follows:
(1) polishing the surface of the aluminum alloy by using silicon carbide water sand paper until the surface roughness is below 10 mu m, soaking in an acid degreasing aqueous solution for 2 minutes, washing by using clear water, repeating the operation twice, and naturally airing or air-drying;
(2) carrying out chemical conversion treatment on the treatment liquid for the aluminum alloy, namely coating the treatment liquid on the surface of the aluminum alloy for 60 s;
(3) directly washing and cleaning the aluminum alloy subjected to chemical conversion treatment in the step (2) by using a cleaning agent; and then naturally airing.
Example 4
The metal-organic framework film treatment liquid for the high-corrosion-resistance marine aluminum alloy surface is prepared from the following components in parts by weight: 300ppm of fluorozirconic acid with a concentration of 45%, 100ppm of fluorotitanic acid with a concentration of 50%, 40ppm of manganese difluoride, 100ppm of glucose, 30ppm of sodium sulfate with a concentration of 50%, and the balance of water. The pH of the treatment solution was adjusted to 5.
The application method of the metal-organic framework film treatment liquid for the surface of the high-corrosion-resistance marine aluminum alloy in the embodiment is used for forming a framework film on the surface of the marine aluminum alloy, and the specific preparation process is as follows:
(1) polishing the surface of the aluminum alloy by using silicon carbide water sand paper until the surface roughness is below 10 mu m, soaking in an acid degreasing aqueous solution for 6 minutes, washing by using clear water, repeating the operation twice, and naturally airing or air-drying;
(2) carrying out chemical conversion treatment on the treatment liquid for the aluminum alloy, namely directly spraying the treatment liquid on the surface of the aluminum alloy for 4min, wherein the spraying pressure is 0.01 KPa;
(3) washing the surface of the aluminum alloy subjected to the chemical conversion treatment in the step (2) with clean water for one time, and then cleaning with clean water with the conductivity of less than 200 mu s/cm; and then drying at 60 ℃ for 10 min.
Example 5
The metal-organic framework film treatment liquid for the high-corrosion-resistance marine aluminum alloy surface is prepared from the following components in parts by weight: 125ppm of fluorozirconic acid with the concentration of 45 percent, 300ppm of fluotitanic acid with the concentration of 50 percent, 50ppm of manganese difluoride, 70ppm of glucose, 15ppm of sodium sulfate with the concentration of 50 percent, and the balance of water. The pH of the treatment solution was adjusted to 5.5.
The application method of the metal-organic framework film treatment liquid for the surface of the high-corrosion-resistance marine aluminum alloy in the embodiment is used for forming a framework film on the surface of the marine aluminum alloy, and the specific preparation process is as follows:
(1) polishing the surface of the aluminum alloy by using silicon carbide water sand paper until the surface roughness is below 10 mu m, soaking in an acid degreasing aqueous solution for 5 minutes, washing by using clear water, repeating the operation twice, and naturally airing or air-drying;
(2) and (3) carrying out chemical conversion treatment on the aluminum alloy treatment solution, namely coating the treatment solution on the surface of the aluminum alloy for 90 s.
(3) Cleaning the aluminum alloy subjected to chemical conversion treatment in the step (2) with water, and cleaning the aluminum alloy subjected to chemical treatment in a spraying or soaking mode by using clean water for one time after treatment and then cleaning the surface of the aluminum alloy with clean water with the conductivity of less than 200 mu s/cm; the aluminum alloy chemically treated by adopting a coating mode is directly washed clean after treatment; and then drying at 100 ℃ for 8 min.
Example 6
The metal-organic framework film treatment liquid for the high-corrosion-resistance marine aluminum alloy surface is prepared from the following components in parts by weight: 800ppm of fluorozirconic acid with a concentration of 45%, 700ppm of fluorotitanic acid with a concentration of 50%, 80ppm of manganese difluoride, 200ppm of glucose, 30ppm of sodium sulfate with a concentration of 50%, and the balance of water. The pH of the treatment solution was adjusted to 3.
The application method of the metal-organic framework film treatment liquid for the surface of the high-corrosion-resistance marine aluminum alloy in the embodiment is used for forming a framework film on the surface of the marine aluminum alloy, and the specific preparation process is as follows:
(1) polishing the surface of the aluminum alloy by using silicon carbide water sand paper until the surface roughness is below 10 mu m, soaking in an acid degreasing aqueous solution for 4 minutes, washing by using clear water, repeating the operation twice, and naturally airing or air-drying;
(2) carrying out chemical conversion treatment on the aluminum alloy by using the treatment solution, namely soaking the aluminum alloy in the treatment solution for 8 min;
(3) washing the surface of the aluminum alloy subjected to the chemical conversion treatment in the step (2) with clean water for one time, and then cleaning with clean water with the conductivity of less than 200 mu s/cm; and then naturally airing.
The aluminum alloy materials treated in examples 1 to 6 were subjected to electrostatic spraying with a three-stage powder coating, followed by curing at a curing temperature of 210 ℃ for 15 min. Respectively carrying out acid salt spray test, constant-temperature condensed water test and SO resistance on the cured material2And testing and filiform corrosion testing, wherein the specific testing conditions are as follows:
(1) acid salt spray test
The test is according to ISO 9227: 2012, test equipment is Q-FOG/SSP1100, the test duration is 2000 hours, and the technical requirements are according to QUALICOAT 14 edition: the foaming rating is according to ISO 4628-2: 2 or less (S2); penetration area along the scribe: less than or equal to 16mm210 cm; single maximum penetration length along the cross-hatch: less than or equal to 4 mm.
(2) Constant temperature condensate water test
The test is according to ISO 6270-2: 2005, test equipment liebsich K300, test duration 2000 hours, specification according to QUALICOAT version 14: the foaming rating is according to ISO 4628-2: 2 or less (S2); single maximum penetration length along the cross-hatch: less than or equal to 1 mm.
(3) SO resistance2Testing
The test is based on DIN EN ISO 3231, test equipment A-SC KBG 400Co. Liebsche, test duration 24cycles, technical requirements are based on QUALICOAT 14 edition: non-discoloring or foaming grades according to ISO 4628-2: 2 or less (S2); single maximum penetration length along the cross-hatch: less than or equal to 1 mm.
(4) Filiform corrosion test
The test was carried out according to DIN EN ISO 4623-2:2004, test equipment Climate Chamber Co Binder, test duration 1000 hours, technical requirements according to QUALICOAT version 14: maximum length of filiform corrosion: 4mm or less, average length of filiform corrosion: 2mm or less, the number of filiform corrosion: less than or equal to 20/10 cm.
The results of the tests performed in examples 1-6 are shown in Table 1.
Table 1 results of performance testing
Attached: maximum length of L-filament corrosion; m-filament corrosion length average; number of N-filiform corrosion.
As can be seen from Table 1, the skeleton film obtained by treating the surface of the aluminum alloy with the metal-organic skeleton film treatment solution for the surface of the highly-corrosion-resistant marine aluminum alloy has good corrosion resistance and high adhesion to the powder coating for the three-level powder coating, shows good corrosion resistance under long test time and various test conditions, is equivalent to or even superior to the traditional hexavalent chromate film in corrosion resistance, is more environment-friendly and pollution-free, and has wider application range.
The present invention has been further described with reference to specific embodiments, but it should be understood that the detailed description should not be construed as limiting the spirit and scope of the present invention, and various modifications made to the above-described embodiments by those of ordinary skill in the art after reading this specification are within the scope of the present invention.
Claims (8)
1. The high-corrosion-resistance marine aluminum alloy surface metal-organic framework film treatment liquid is characterized by being prepared from the following components: 800-1600ppm of 45% fluozirconic acid, 1000ppm of 50% fluotitanic acid 200, 5-120ppm of manganese difluoride, 25-600ppm of glucose, 5-40ppm of 50% sodium sulfate and the balance of water.
2. The high corrosion resistance marine aluminum alloy surface metal-organic framework film treatment solution according to claim 1, wherein the pH value of the treatment solution is 3-6, and is adjusted by adding hydrofluoric acid, sulfuric acid, ammonia water or sodium hydroxide.
3. The use method of the metal-organic framework film treatment fluid for the surface of the high-corrosion-resistance marine aluminum alloy according to any one of claims 1 to 2, which is used for forming a framework film on the surface of the marine aluminum alloy, and comprises the following specific preparation processes:
(1) polishing the surface of the aluminum alloy by using silicon carbide water sand paper until the surface roughness is below 10 mu m, soaking the aluminum alloy in an acid degreasing aqueous solution for 2 to 6 minutes, washing the aluminum alloy by using clear water, repeating the operation twice, and naturally airing or air-drying the aluminum alloy;
(2) carrying out chemical conversion treatment on the aluminum alloy by using the treatment liquid for 60s-8 min;
(3) and (3) cleaning the aluminum alloy subjected to the chemical conversion treatment in the step (2) with water, and naturally airing or drying.
4. The use method of the metal-organic framework film treatment solution for the surface of the highly corrosion-resistant marine aluminum alloy according to claim 3, wherein the chemical conversion treatment in the step (2) is to immerse the aluminum alloy in the treatment solution for 3-8 min.
5. The use method of the metal-organic framework film treatment liquid for the surface of the highly corrosion-resistant marine aluminum alloy according to claim 3, wherein the chemical conversion treatment in the step (2) is to directly spray the treatment liquid on the surface of the aluminum alloy for 1-4min, and the spraying pressure is 0.01-0.12 KPa.
6. The use method of the metal-organic framework film treatment solution for the surface of the highly corrosion-resistant marine aluminum alloy according to claim 3, wherein the chemical conversion treatment in the step (2) is to coat the treatment solution on the surface of the aluminum alloy for 60-90 s.
7. The use method of the metal-organic framework film treatment solution for the surface of the highly corrosion-resistant marine aluminum alloy according to claim 3, wherein in the step (3), the aluminum alloy is subjected to chemical treatment in a spraying or soaking manner, and after the treatment, the surface of the aluminum alloy is washed once with clean water and then is washed with clean water with the conductivity of less than 200 μ s/cm; the aluminum alloy chemically treated by adopting a coating mode is directly cleaned by washing after treatment.
8. The use method of the metal-organic framework film treatment fluid for the surface of the highly corrosion-resistant marine aluminum alloy according to claim 3, wherein the drying temperature in the step (3) is 30-100 ℃ and the drying time is 8-12 min.
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| CN111218679B (en) * | 2020-01-23 | 2022-07-05 | 广东省建筑科学研究院集团股份有限公司 | Metal-organic framework membrane preparation liquid and membrane and preparation method thereof |
| CN111218172B (en) * | 2020-01-23 | 2022-07-19 | 广东省建筑科学研究院集团股份有限公司 | Composite coating for eliminating pollution of heavy metal chromium and VOCs from source and preparation method |
| CN113151815A (en) * | 2020-12-22 | 2021-07-23 | 苏州帝航防护设施有限公司 | Corrosion-resistant metal surface treating agent |
| CN113628888B (en) * | 2021-10-09 | 2021-12-10 | 南通海星电子股份有限公司 | Preparation method of corrosion aluminum foil with high consistency of hole length |
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