CN108330475A - A kind of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid and its application method - Google Patents
A kind of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid and its application method Download PDFInfo
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- CN108330475A CN108330475A CN201711476600.5A CN201711476600A CN108330475A CN 108330475 A CN108330475 A CN 108330475A CN 201711476600 A CN201711476600 A CN 201711476600A CN 108330475 A CN108330475 A CN 108330475A
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- C—CHEMISTRY; METALLURGY
- 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 present invention relates to field of metal surface treatment technology more particularly to a kind of improved corrosion marine aluminium alloy surface metal organic framework film treatment fluid and its application methods.The treatment fluid is prepared from the following components：A concentration of 45% fluorine zirconic acid 25 1600ppm, a concentration of 50% 12.5 1000ppm of fluotitanic acid, 5 120ppm of manganese difluoride, 25 600ppm of glucose, a concentration of 50% 5 40ppm of sodium sulphate, surplus is water.Metal organic framework film is formed by the way that the treatment fluid is coated in aluminum alloy surface.The metal organic framework film treatment fluid of the present invention, metal ion is provided with fluorine zirconic acid, fluotitanic acid, glucose provides organic unsaturated bond, it is combined to form skeleton with metal ion, it is precipitated convenient for the attachment of aluminum oxide, is easy to form a film, and be conducive to improve the corrosion resistance and adhesion of framework film, chromium free raw material is used simultaneously, it is environment friendly and pollution-free.
Description
Technical field
The present invention relates to field of metal surface treatment technology more particularly to a kind of improved corrosion marine aluminium alloy surface gold
Category-organic framework film treatment fluid and its application method.
Background technology
Aluminum alloy plate materials due to having preferable corrosion resistance, be widely used in electronics production piece, aviation, building materials, machinery,
The fields such as naval vessel.And since, in application, being chronically at wet environment, aluminum alloy surface is easy to be corroded in naval vessel, chromate
As corrosion inhibitor, it is applied to aluminum alloy surface processing.By the way that the treatment fluid containing chromium such as chromic acid-chromate is in direct contact
It to make it that chromate film be precipitated, or is coated on metal surface, chromate film is precipitated after dry by metal material surface
Method improves the corrosion resistance of aluminum alloy surface.But since Cr VI is highly unwanted to human body and environment, it is applied at present
Receive stringent limitation.People start to develop the metal surface treating liquid of Chrome-free, wherein Publication No. CN101535528A's
In patent, by suitably changing the concentration of or mixtures thereof zirconium, titanium, and 0.3~3 grams per liter divalent zinc, control ph are added
The acid solution obtained between 2.2-3.8 can be applied to construction, shipbuilding, building trade and the application of motor vehicle body
In production large household appliance.But conversion coating is obtained in production easily because of the variation of environment temperature and processing time with the method
So that film layer generates notable difference, therefore the adhesion performance of paint or powder can be declined.Therefore it provides a kind of safety
Environmental protection with the aluminum alloy surface treatment fluid compared with high corrosion resistance and adhesion is that this field technology urgently to be resolved hurrily is asked
Topic.
Invention content
The purpose of the present invention is to provide a kind of safety and environmental protection, with the marine aluminium alloy compared with high corrosion resistance and adhesion
Surface metal-organic framework film treatment fluid and its application method.
The present invention uses following technical scheme：
A kind of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid, the treatment fluid are matched by following components
It makes：A concentration of 45% fluorine zirconic acid 25-1600ppm, a concentration of 50% fluotitanic acid 12.5-1000ppm, manganese difluoride 5-
120ppm, glucose 25-600ppm, a concentration of 50% sodium sulphate 5-40ppm, surplus is water.
Further, the pH value for the treatment of fluid is 3-6, is adjusted by adding hydrofluoric acid, sulfuric acid, ammonium hydroxide or sodium hydroxide.
The present invention also provides a kind of users of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid
Method, for forming framework film on marine aluminium alloy surface, specific preparation process is as follows：
(1) by aluminum alloy surface silicon carbide liquid honing to surface roughness at 10 μm hereinafter, being placed in acid deoiling
It is rinsed well with clear water after being impregnated 2-6 minutes in degreasing aqueous solution, naturally dry or air-dried after repetitive operation twice；
(2) aluminium alloy is subjected to chemical conversion treatment, processing time 60s-8min with treatment fluid；
(3) naturally dry or drying after washing with water the aluminium alloy in step (2) after chemical conversion treatment totally.
Further, chemical conversion treatment is that aluminium alloy is impregnated 3-8min in treatment fluid in step (2).
Further, chemical conversion treatment is that treatment fluid is directly sprayed in aluminum alloy surface 1-4min in step (2), is sprayed
Leaching pressure is 0.01-0.12KPa.
Further, chemical conversion treatment is that treatment fluid is coated on aluminum alloy surface 60-90s in step (2).
Further, cleaning process in step (3) carries out chemically treated aluminium alloy, place using spray or immersion way
Clear water once flushing is first used to aluminum alloy surface after reason, then is cleaned less than 200 μ s/cm clear water with conductivity；Using coating method
Chemically treated aluminium alloy is carried out, is directly rinsed well with cleaning after processing.
Further, drying temperature is 30-100 DEG C in step (3), drying time 8-12min.
The improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid and its application method of the present invention, has
Following advantageous effect：
(1) metal-organic framework film process liquid of the invention provides metal ion with fluorine zirconic acid, fluotitanic acid, and glucose carries
It for organic unsaturated bond, is combined to form skeleton with metal ion, is precipitated convenient for the attachment of aluminum oxide, be easy to form a film, be conducive to
The corrosion resistance and adhesion of framework film are improved, while the treatment fluid that is added to of manganese difluoride and sodium sulphate provides free fluorine
Ion plasma is conducive to treatment fluid and controls reaction when aluminum alloy surface is reacted to the progress of film forming direction, accelerates film forming procedure
With optimization film-formation result
(2) between 3 and 6, effective processing range is wide, fully avoids for metal-organic framework film process liquid pH value of the invention
The defect that existing chromium-free passivation liquid causes mass production limited because processing range is narrow, treatment fluid of the invention can be extensive
Applied in the surface treatment to metal materials such as aluminium alloys.
(3) application method of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid of the invention uses
Chromium free raw material forms framework film in aluminum alloy surface, environment friendly and pollution-free, and framework film obtained has higher anti-corrosion effects,
Be conducive to ship and resist the erosion of seawater and the influence of wet environment, while application method through the invention under marine climate
The framework film of formation has good adhesion to paint, coating etc., is conducive to the aesthetic measure for improving ship.
Specific implementation mode
Below in conjunction with specific embodiment, clear, complete description is carried out to technical scheme of the present invention, it is clear that retouched
The embodiment stated is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, originally
All other embodiment that field those skilled in the art are obtained without making creative work belongs to this
The protection domain of invention.
Metal material used in the following example：
Thickness is the domestic aluminium-magnesium alloy proximate matter 5083 of 1mm, main component Fe：0.35%, Mg：0.8~0.9%,
Si：0.65~0.75%, Cu：0.85~0.95%, Mn：0.15~0.25%, remaining is Al.
According to the acid deoiling degreasing aqueous solution of patent CN201010206660.7 or CN201010543878.1, to above-mentioned
Metal material surface is cleaned, and the surface treatment of the following example is subsequently used for.
Embodiment 1
A kind of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid, the treatment fluid are matched by following components
It makes：A concentration of 45% fluorine zirconic acid 1000ppm, a concentration of 50% fluotitanic acid 600ppm, manganese difluoride 30ppm, grape
Sugared 400ppm, a concentration of 50% sodium sulphate 10ppm, surplus is water.It is 4 to adjust treatment fluid pH value.
The application method of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid, is used in the present embodiment
Framework film is formed on marine aluminium alloy surface, specific preparation process is as follows：
(1) by aluminum alloy surface silicon carbide liquid honing to surface roughness at 10 μm hereinafter, being placed in acid deoiling
It is rinsed well with clear water after being impregnated 6 minutes in degreasing aqueous solution, naturally dry or air-dried after repetitive operation twice；
(2) aluminium alloy is subjected to chemical conversion treatment with treatment fluid, i.e., aluminium alloy is impregnated into 3min in treatment fluid；
(3) aluminium alloy in step (2) after chemical conversion treatment is first used into clear water once flushing, then is less than with conductivity
200 μ s/cm clear water are cleaned；It is dried later, drying temperature is 30 DEG C, drying time 12min.
Embodiment 2
A kind of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid, the treatment fluid are matched by following components
It makes：A concentration of 45% fluorine zirconic acid 100ppm, a concentration of 50% fluotitanic acid 800ppm, manganese difluoride 90ppm, glucose
100ppm, a concentration of 50% sodium sulphate 10ppm, surplus is water.It is 3 to adjust treatment fluid pH value.
The application method of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid, is used in the present embodiment
Framework film is formed on marine aluminium alloy surface, specific preparation process is as follows：
(1) by aluminum alloy surface silicon carbide liquid honing to surface roughness at 10 μm hereinafter, being placed in acid deoiling
It is rinsed well with clear water after being impregnated 3 minutes in degreasing aqueous solution, naturally dry or air-dried after repetitive operation twice；
(2) aluminium alloy is subjected to chemical conversion treatment with treatment fluid, i.e., treatment fluid is directly sprayed in into aluminum alloy surface
1min, spray pressure 0.12KPa；
(3) aluminum alloy surface in step (2) after chemical conversion treatment is first used into clear water once flushing, then uses conductivity
It is cleaned less than 200 μ s/cm clear water；Naturally dry later.
Embodiment 3
A kind of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid, the treatment fluid are matched by following components
It makes：A concentration of 45% fluorine zirconic acid 1200ppm, a concentration of 50% fluotitanic acid 200ppm, manganese difluoride 100ppm, grape
Sugared 500ppm, a concentration of 50% sodium sulphate 20ppm, surplus is water.It is 6 to adjust treatment fluid pH value.
The application method of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid, is used in the present embodiment
Framework film is formed on marine aluminium alloy surface, specific preparation process is as follows：
(1) by aluminum alloy surface silicon carbide liquid honing to surface roughness at 10 μm hereinafter, being placed in acid deoiling
It is rinsed well with clear water after being impregnated 2 minutes in degreasing aqueous solution, naturally dry or air-dried after repetitive operation twice；
(2) aluminium alloy is subjected to chemical conversion treatment with treatment fluid, i.e., treatment fluid is coated on aluminum alloy surface 60s；
(3) aluminium alloy in step (2) after chemical conversion treatment is directly rinsed well with cleaning；It dries in the air naturally later
It is dry.
Embodiment 4
A kind of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid, the treatment fluid are matched by following components
It makes：A concentration of 45% fluorine zirconic acid 300ppm, a concentration of 50% fluotitanic acid 100ppm, manganese difluoride 40ppm, glucose
100ppm, a concentration of 50% sodium sulphate 30ppm, surplus is water.It is 5 to adjust treatment fluid pH value.
The application method of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid, is used in the present embodiment
Framework film is formed on marine aluminium alloy surface, specific preparation process is as follows：
(1) by aluminum alloy surface silicon carbide liquid honing to surface roughness at 10 μm hereinafter, being placed in acid deoiling
It is rinsed well with clear water after being impregnated 6 minutes in degreasing aqueous solution, naturally dry or air-dried after repetitive operation twice；
(2) aluminium alloy is subjected to chemical conversion treatment with treatment fluid, i.e., treatment fluid is directly sprayed in into aluminum alloy surface
4min, spray pressure 0.01KPa；
(3) aluminum alloy surface in step (2) after chemical conversion treatment is first used into clear water once flushing, then uses conductivity
It is cleaned less than 200 μ s/cm clear water；It is dried later, drying temperature is 60 DEG C, drying time 10min.
Embodiment 5
A kind of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid, the treatment fluid are matched by following components
It makes：A concentration of 45% fluorine zirconic acid 125ppm, a concentration of 50% fluotitanic acid 300ppm, manganese difluoride 50ppm, glucose
70ppm, a concentration of 50% sodium sulphate 15ppm, surplus is water.It is 5.5 to adjust treatment fluid pH value.
The application method of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid, is used in the present embodiment
Framework film is formed on marine aluminium alloy surface, specific preparation process is as follows：
(1) by aluminum alloy surface silicon carbide liquid honing to surface roughness at 10 μm hereinafter, being placed in acid deoiling
It impregnates in degreasing aqueous solution and is rinsed well after five minutes with clear water, naturally dry or air-dried after repetitive operation twice；
(2) aluminium alloy is subjected to chemical conversion treatment with treatment fluid, i.e., treatment fluid is coated on aluminum alloy surface 90s.
(3) aluminium alloy in step (2) after chemical conversion treatment is washed with water totally, using spray or immersion way
Chemically treated aluminium alloy is carried out, clear water once flushing is first used to aluminum alloy surface after processing, then be less than 200 μ s/ with conductivity
Cm clear water is cleaned；Chemically treated aluminium alloy is carried out using coating method, is directly rinsed well with cleaning after processing；It carries out later
Drying, drying temperature are 100 DEG C, drying time 8min.
Embodiment 6
A kind of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid, the treatment fluid are matched by following components
It makes：A concentration of 45% fluorine zirconic acid 800ppm, a concentration of 50% fluotitanic acid 700ppm, manganese difluoride 80ppm, glucose
200ppm, a concentration of 50% sodium sulphate 30ppm, surplus is water.It is 3 to adjust treatment fluid pH value.
The application method of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid, is used in the present embodiment
Framework film is formed on marine aluminium alloy surface, specific preparation process is as follows：
(1) by aluminum alloy surface silicon carbide liquid honing to surface roughness at 10 μm hereinafter, being placed in acid deoiling
It is rinsed well with clear water after being impregnated 4 minutes in degreasing aqueous solution, naturally dry or air-dried after repetitive operation twice；
(2) aluminium alloy is subjected to chemical conversion treatment with treatment fluid, i.e., aluminium alloy is impregnated into 8min in treatment fluid；
(3) aluminum alloy surface in step (2) after chemical conversion treatment is first used into clear water once flushing, then uses conductivity
It is cleaned less than 200 μ s/cm clear water；Naturally dry later.
To treated in embodiment 1-6, aluminum alloy materials carry out electrostatic spraying three-level powdery paints, are cured later
Processing, solidification temperature are 210 DEG C, hardening time 15min.Material after solidification is carried out to acid salt spray test, constant temperature respectively
Condensed water test, resistance to SO2Test and filiform corrosion test, specific test condition are as follows：
(1) acid salt spray test
Test basis is ISO 9227：2012, test equipment Q-FOG/SSP1100, length of testing speech 2000 hours, technology
It is required that according to QUALICOAT 14 editions：Grade of blistering is according to ISO 4628-2：≤2(S2)；Along a stroke lattice infiltrating area：≤16mm2/
10cm；Draw lattice individually maximum penetration length in edge：≤4mm.
(2) constant-temperature condensation water is tested
Test foundation is ISO 6270-2：2005, test equipment LIEBISCH K300, length of testing speech 2000 hours, technology
It is required that according to QUALICOAT 14 editions：Grade of blistering is according to ISO 4628-2：≤2(S2)；Draw lattice individually maximum penetration length in edge：
≤1mm。
(3) resistance to SO2Test
Test foundation is DIN EN ISO 3231, test equipment A-SC KBG 400Co.Liebsche, length of testing speech
24cycles, technology are required according to QUALICOAT 14 editions：Without discoloration or blistering grade according to ISO4628-2：≤2(S2)；Edge
Draw lattice individually maximum penetration length：≤1mm.
(4) filiform corrosion is tested
Test foundation is DIN EN ISO 4623-2:2004, test equipment Climate Chamber Co Binder are surveyed
Try duration 1000 hours, technology is required according to QUALICOAT 14 editions：Filiform corrosion maximum length：≤ 4mm, filiform corrosion are average
Length：≤ 2mm, filiform corrosion number：≤20/10cm.
The test result that embodiment 1-6 is carried out is as shown in table 1.
1 the performance test results of table
It is attached：L- filiform corrosion maximum lengths；M- filiform corrosion length average values；N °-filiform corrosion number.
As shown in Table 1, using improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid of the present invention to aluminium
The framework film obtained after alloy surface processing so that the aluminum alloy materials have good corrosion resistance to three-level powdery paints
With the higher adhesion to powdery paints, shown under longer length of testing speech and a variety of test conditions good anti-
Corrosive nature, the quite even better than traditional hexavalent chromate film of corrosion resistance, but it is more environmentally-friendly pollution-free, the scope of application is more
It is wider greatly.
The present invention is further described by specific embodiment above, it should be understood that, here specifically
Description, should not be construed as the restriction to the spirit and scope of the invention, and one of ordinary skilled in the art is reading this explanation
The various modifications made to above-described embodiment after book belong to the range that the present invention is protected.
Claims (8)
1. a kind of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid, which is characterized in that the treatment fluid by
Following components is formulated：A concentration of 45% fluorine zirconic acid 25-1600ppm, a concentration of 50% fluotitanic acid 12.5-1000ppm,
Manganese difluoride 5-120ppm, glucose 25-600ppm, a concentration of 50% sodium sulphate 5-40ppm, surplus is water.
2. improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid according to claim 1, feature exist
In the pH value of the treatment fluid is 3-6, is adjusted by adding hydrofluoric acid, sulfuric acid, ammonium hydroxide or sodium hydroxide.
3. a kind of improved corrosion marine aluminium alloy surface metal-organic framework film according to any one of claim 1-2
The application method for the treatment of fluid, which is characterized in that for forming framework film on marine aluminium alloy surface, specific preparation process is as follows：
(1) by aluminum alloy surface silicon carbide liquid honing to surface roughness at 10 μm hereinafter, being placed in acid deoiling degreasing
It is rinsed well with clear water after being impregnated 2-6 minutes in aqueous solution, naturally dry or air-dried after repetitive operation twice；
(2) aluminium alloy is subjected to chemical conversion treatment, processing time 60s-8min with treatment fluid；
(3) naturally dry or drying after washing with water the aluminium alloy in step (2) after chemical conversion treatment totally.
4. the user of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid according to claim 3
Method, which is characterized in that chemical conversion treatment is that aluminium alloy is impregnated 3-8min in treatment fluid in step (2).
5. the user of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid according to claim 3
Method, which is characterized in that chemical conversion treatment is that treatment fluid is directly sprayed in aluminum alloy surface 1-4min in step (2), is sprayed
Pressure is 0.01-0.12KPa.
6. the user of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid according to claim 3
Method, which is characterized in that chemical conversion treatment is that treatment fluid is coated on aluminum alloy surface 60-90s in step (2).
7. the user of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid according to claim 3
Method, which is characterized in that cleaning process in step (3) carries out chemically treated aluminium alloy, after processing using spray or immersion way
Clear water once flushing is first used to aluminum alloy surface, then is cleaned less than 200 μ s/cm clear water with conductivity；It is carried out using coating method
Chemically treated aluminium alloy is directly rinsed well with cleaning after processing.
8. the user of improved corrosion marine aluminium alloy surface metal-organic framework film treatment fluid according to claim 3
Method, which is characterized in that drying temperature is 30-100 DEG C in step (3), drying time 8-12min.
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| CN111218172A (en) * | 2020-01-23 | 2020-06-02 | 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 |
| 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 |
| WO2023056725A1 (en) * | 2021-10-09 | 2023-04-13 | 南通海星电子股份有限公司 | Method for preparing corroded aluminum foil having high hole length consistency |
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