CN103215630A - Method for sealing aluminum alloy anode oxide film pore by adopting organic-inorganic composite silica sol - Google Patents
Method for sealing aluminum alloy anode oxide film pore by adopting organic-inorganic composite silica sol Download PDFInfo
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Abstract
The invention discloses a method for sealing an aluminum alloy anode oxide film pore by adopting organic-inorganic composite silica sol. The method comprises the following steps of: coating or depositing a layer or organic-inorganic composite silica sol layer on the anode surface of pre-treated aluminum or aluminum alloy; and then drying and sintering. The organic-inorganic composite silica sol is prepared from 0.5-30ml of silane reagent or tetraethoxysilane, 0.5-30ml of inorganic silicon solution, 1-40ml of water, 1-90ml of organic solvent, 0.05-100g of filler powder and 0.01-10g of surfactant. The aluminum and aluminum alloy anode oxide film pore is sealed by organic-inorganic composite silica sol by using coating, brushing, dipping, high-pressure spraying, electrostatic spraying, and cathode or anode electrophoresis method, the pollution to the environment is reduced; the method for sealing the aluminum alloy anode oxide film pore by adopting the organic-inorganic composite silica sol is an environment-friendly coating method; the phase change and brittle rupture caused high temperature process are avoided; the process is easy to carry out; equipment is simple; the processes of coating, brushing, dipping, spraying and electrophoresis are easy to control; the industrial product can be realized; the cost is low; and the film coating is uniform.
Description
Technical field
The present invention relates to a kind of be used to seal aluminum or aluminum alloy and contain the aluminium parts anodic oxidation after the method for micropore, be particularly related to a kind of method with inorganic-organic composite silicon colloidal sol sealing aluminium alloy anode oxide film hole, especially can by be coated with, brush, technology such as dipping, high-pressure air spraying, electrostatic spraying, electrophoretic painting carries out sealing of hole to aluminium and aluminium alloy anode oxide film, and then realizes sealing of hole effect preferably.
Background technology
Aluminium and aluminium alloy thereof are with a wide range of applications in modern industries such as aerospace, building, automobile owing to have the advantage of specific tenacity height, heat conduction and good conductivity, light weight.Yet aluminium alloy matter is soft, wear no resistance, easily be corroded.The character of aluminium is more active, and the oxide film that the surface forms in air has certain etch resistant properties, but the thickness of this oxide film has only several nanometers to tens nanometers, and hardness is also very low, and the ability of opposing environmental attack is relatively poor.So usually carry out necessary surface Hardening Treatment in use earlier, aluminium and alloy thereof are placed in the suitable electrolytic solution as the anode processing of switching on, under the effect of extra electric field, can on the aluminum products surface, form layer oxide film, thickness is between 5-20um, its solidity to corrosion, wear resistance, electrical insulating property improves greatly, this makes the range of application of aluminium and alloy material thereof significantly widen, but the oxide film that the porous-film that aluminium alloy anode oxide obtains-oxidising process produces has very high porosity and adsorptive power, and contaminated easily and corrosive medium corrodes, particularly the aggressiveness negatively charged ion (as Cl-, S
2-, cation etc.) and water molecules etc. still can see through oxide film, cause solidity to corrosion (particularly pitting corrosion) and wear resistance variation, therefore must carry out sealing of hole to handle, improve its solidity to corrosion, contamination resistance and fixed pigment physical efficiency power.
Summary of the invention
Purpose of the present invention provides a kind of method with inorganic-organic composite silicon colloidal sol sealing aluminium alloy anode oxide film hole, to improve the erosion resistance and the resistance to crocking of film.
The technical scheme that adopts is:
Method with inorganic-organic composite silicon colloidal sol sealing aluminium alloy anode oxide film hole comprises following processing step:
1, pre-treatment: the aluminum or aluminum alloy anode is carried out loose scale, oil removing, descaling and polished finish, be known technology.
2, the aluminum or aluminum alloy anode is carried out oxidation.Aluminum or aluminum alloy anode after the pre-treatment is carried out anodic oxidation, and direct supply is selected in anodic oxidation for use, the voltage of supply 8 ~ 22V of setting, current density 1.0 ~ 2.2A/dm
2, anodizing time is 5 ~ 60min, obtains the anode oxide film that thickness is 1 ~ 20 μ m, anodic oxidation is preferably incomplete oxidation, makes that the aluminum or aluminum alloy electrode surface is coarse to get final product.
3, at surface-coated or the deposition last layer or the two-layer above inorganic-organic composite silicon sol layer of the anode oxide film of aluminum or aluminum alloy.
4, oven dry:, obtain the exsiccant rete 50 ~ 120 ℃ of oven dry 10 minutes ~ 24 hours;
5, sintering: 50 ~ 1200 ℃ of following sintering 2 min ~ 5h in retort furnace, obtain sticking power rete preferably, thick 0.5 ~ 25 μ m of rete, promptly.
Apply or deposit organic-inorganic compounding silica sol layer, can adopt knownly be coated with, brush, dipping, high-pressure air spraying, electrostatic spraying or electrophoretic deposition preparation.
The preparation method of inorganic-organic composite silicon colloidal sol is: get 0.5 ~ 30ml silane reagent or tetraethoxy, 0.5 ~ 30ml inorganic silicon colloidal sol, 1 ~ 40ml water, 1 ~ 90ml organic solvent, 0.05 ~ 100g filler powder, 0.01 ~ 10g tensio-active agent stirs, and obtains inorganic-organic composite silicon colloidal sol.
Above-mentioned organic substance silane reagent or tetraethoxy, be commercially available various silane reagents, silane coupling agent or tetraethoxy, when experiment or production, at first carry out composite silane or tetraethoxy, stirred solution then allows the abundant hydrolysis of silane or tetraethoxy.
Inorganic silicon colloidal sol can also comprise water-soluble homodisperse nano silicon oxide with the preparation of technology such as ion exchange method, dispersion method, electrolytic electro-dialysis method, peptisation, elemental silicon dissolution method in the comprehensive silicon colloidal sol, and the dispersion agent of dispersing nanometer silicon oxide.
Above-mentioned organo silane coupling agent is: r-chloropropyl trimethoxyl silane (WD-30), vinyl trichloro silane, vinyltriethoxysilane (WD-20), vinyl three (β one methoxy ethoxy) silane (A-172), γ monomethyl acryloxy propyl trimethoxy silicane (KH570), vinyltrimethoxy silane, γ-glycidyl ether propyl trimethoxy silicane (KH-560), vinyltriacetoxy silane, β-(3,4 epoxy cyclohexanes) ethyl dimethoxy silane, γ-mercapto propyl group dimethoxy silane (KH-590), γ-mercaptopropyltriethoxysilane (KH-845-4), γ-An Bingjisanyiyangjiguiwan (KH-550, WD-50), N-β-(aminoethyl)-γ-nitrogen propyl trimethoxy silicane (KH-792, WD-51), γ-urea groups propyl-triethoxysilicane, anilinomethyl triethoxysilane (ND-42), anilinomethyl dimethoxy silane (ND-73), ɑ monomethyl acryloyl-oxy Union carbide A-162 (ND-NS), hexyl amino methyl triethoxyl silane (ND-24), dimethyldiethoxysilane (DDS), the KH-567 silane coupling agent, KH-460 silane coupling agent, KH-450 silane coupling agent, the KH-578 silane coupling agent, the KH-470 silane coupling agent, KH-5501 silane coupling agent, KH792, DL602, silane coupling agents such as DL171.
Above-mentioned filler powder is: glass fibre, silicon-dioxide, aluminum oxide, titanium oxide, zirconium white, magnesium oxide, calcium oxide, zinc oxide, ferric oxide, white carbon black, silicate, talcum powder, mica, potter's clay, aluminium hydroxide, iron powder, aluminium powder, silica flour, Fe
3Nanometers such as Al powder, asbestos, magnesium hydroxide, graphite, boron nitride, carbon black, lime carbonate, calcium sulfate, barium sulfate, carboxymethyl cellulose, Resins, epoxy, poly-ammonia are cruel, resol and melamine resin (0.1 ~ 100nm) or the powder of micron (0.1 ~ 100 μ m) material.
Above-mentioned tensio-active agent is organic surface active agent (dispersion agent), inorganic dispersant.Organic dispersing agent has vinylformic acid (ester), the polymethyl acid amide, polymethyl acrylic acid, the polyethylene quadrol, the N-N-dimethyl formamide, trolamine, the citric acid diamines, polyvinyl alcohol, polyvinyl butyral acetal, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, month water glass, polyoxyethylene glycol, Soxylat A 25-7, polyethenoxy ether, Polyvinylpyrolidone (PVP), oleic acid, citric acid, toxilic acid (ester) and they and derivative, the hydrophobic side monomer mostly is unsaturated hydro carbons, as vinylbenzene, ethene, divinyl, diisobutylene, ethylene methacrylic ether, vinyl acetate, a-vinyl toluene etc., poly-phosphate (as Sodium hexametaphosphate 99), silicate etc.Inorganic dispersant has: yellow soda ash, Sodium Tetraborate, Sodium hexametaphosphate 99, sodium polyphosphate, Potassium tripolyphosphate (KTPP) and tetrapotassium pyrophosphate (TKPP) etc.
Above-mentioned organic solvent is: organic solvents such as ethanol, ethylene glycol, methyl alcohol, butanols, benzene,toluene,xylene, chloroform.
Described silane coupling agent molecular formula is Y (CH
2) nSiX
3Herein, n=0～3; The hydrolyzable group of X-; Y one organo-functional group can react with resin.X is chloro, methoxyl group, oxyethyl group, methoxy ethoxy, acetoxyl group etc. normally, generates silanol during these group hydrolysis, and combines with inorganic substance, forms siloxanes.Y is vinyl, amino, epoxy group(ing), methacryloxy, sulfydryl or urea groups.These reactive groups can combine with the organic substance reaction.Therefore,, can between the interface of inorganic substance and organic substance, erect " molecule bridge ", the material of two kinds of character great disparities is linked together improve the effect of performance of composites and increase bonding strength by using silane coupling agent.
Above-mentioned inorganic-organic composite silicon colloidal sol also can be substituted by mixing solutions or the single inorganic silicon sol solution of single silane with alcohol, water.
The invention has the advantages that:
The present invention by be coated with, brush, dipping, high pressure painting, electrostatic spraying, negative electrode or anodic electrophoresis method, with inorganic-organic composite silicon colloidal sol sealing aluminium and aluminium alloy anode oxide film fenestra, the dichromate sealing technique that replaces aluminium alloy anode oxide film, alleviate pollution to environment, inorganic-organic composite silicon colloidal sol is a kind of surface coating process of environmental protection, phase transformation and the embrittlement that can avoid pyroprocess to cause; Technology realizes that easily equipment is simpler, is coated with, brushes, floods, spraying and electrophoresis process be easy to control, can realize suitability for industrialized production, and cost is low, films evenly.
Embodiment
Method with inorganic-organic composite silicon colloidal sol sealing aluminium alloy anode oxide film hole comprises following processing step:
(1) pre-treatment: loose scale is carried out on aluminum or aluminum alloy sun plate surface, and polishing uses sand paper from coarse to fine, and the sand paper model of finally selecting for use is 2000
#The salpeter solution that descaling is used: deionized water=0.5 ~ 2:1; The used alkali concn of alkaline etching is 30g/L; Workpiece surface often adheres to one deck dust after the alkaline etching, and with carrying out anodic oxidation treatment after the light-emitting solution removal dust, polishing fluid adopts salpeter solution, nitric acid: water=0.5 ~ 2:1, and stand-by;
(2) anodic oxidation: the aluminum or aluminum alloy anode after the pre-treatment is carried out anodic oxidation, and direct supply is selected in anodic oxidation for use, voltage of supply 12V, the current density 1.5A/dm of setting
2, anodizing time is 30min, obtains the anode oxide film that thickness is 15 μ m, anodic oxidation can not exclusively be carried out, surface irregularity gets final product, and is used to improve the bonding force of aluminium alloy and organic and inorganic silicon coating;
(3) inorganic-organic composite silicon colloidal sol is adopted be coated with, brush, dipping, high-pressure air spraying, electrostatic spraying, employing electrophoretic method prepare coating on the oxide film of aluminum or aluminum alloy sun plate.
The spraying of employing high-pressure air: along with the prolongation of spray time and the increasing of spray pressure, the thickness of coating increases.
Adopt electrophoretic deposition: use 10A/dm
2Current density under 50V voltage, the electrophoresis silicon sol is deposited in the aluminum or aluminum alloy anodic oxidation fenestra, uses washed with de-ionized water, repeats 5 times;
(4) oven dry:, obtain the exsiccant rete 50 ℃ of oven dry 24 hours;
(5) sintering: 800 ℃ of following sintering 2h in retort furnace obtain sticking power rete preferably, promptly.
Above-mentioned organic substance is silane reagent or tetraethoxy, be commercially available various silane reagents, silane coupling agent or tetraethoxy, when experiment or production, at first carry out composite silane or tetraethoxy, stirred solution then allows the abundant hydrolysis of silane or tetraethoxy.
Claims (9)
1. with the method in inorganic-organic composite silicon colloidal sol sealing aluminium alloy anode oxide film hole, it is characterized in that: comprise following processing step:
1. pre-treatment: the aluminum or aluminum alloy anode is carried out loose scale, oil removing, descaling and polished finish;
2. the aluminum or aluminum alloy anode is carried out oxidation, the aluminum or aluminum alloy anode after the pre-treatment is carried out anodic oxidation, direct supply is selected in anodic oxidation for use, the voltage of supply 8 ~ 22V of setting, current density 1.0 ~ 2.2A/dm
2, anodizing time is 5 ~ 60min, obtains the anode oxide film that thickness is 1 ~ 20 μ m, anodic oxidation is preferably incomplete oxidation, makes that the aluminum or aluminum alloy electrode surface is coarse to get final product;
3. adopt on the surface of the anode oxide film of aluminum or aluminum alloy be coated with, brush, dipping, high-pressure air spraying, electrostatic spraying, electrophoretic method prepare one or more layers inorganic-organic composite silicon collosol coating;
4. oven dry:, obtain the exsiccant rete 50 ~ 120 ℃ of oven dry 10 minutes ~ 24 hours;
5. sintering: 50 ~ 1200 ℃ of following sintering 2 min ~ 5h in retort furnace, obtain sticking power rete preferably, thick 0.5 ~ 25 μ m of rete, promptly.
2. the method with inorganic-organic composite silicon colloidal sol sealing aluminium alloy anode oxide film hole according to claim 1, it is characterized in that: the preparation method of inorganic-organic composite silicon colloidal sol is: get 0 ~ 30ml silane reagent or tetraethoxy, 0.5 ~ 30ml inorganic silicon colloidal sol, 1 ~ 40ml water, 0 ~ 90ml organic solvent, 0 ~ 100g filler powder, 0 ~ 10g tensio-active agent stirs, and obtains inorganic-organic composite silicon colloidal sol.
3. the method with inorganic-organic composite silicon colloidal sol sealing aluminium alloy anode oxide film hole according to claim 1, it is characterized in that: above-mentioned organic substance silane reagent or tetraethoxy are commercially available silane reagent, silane coupling agent or tetraethoxy.
4. the method with inorganic-organic composite silicon colloidal sol sealing aluminium alloy anode oxide film hole according to claim 1, it is characterized in that: silane coupling agent is: r-chloropropyl trimethoxyl silane WD-30, vinyl trichloro silane, vinyltriethoxysilane WD-20, vinyl three β one methoxy ethoxy silane A-172, γ monomethyl acryloxy propyl trimethoxy silicane KH570, vinyltrimethoxy silane, γ-glycidyl ether propyl trimethoxy silicane KH-560, vinyltriacetoxy silane, β-3,4 epoxy cyclohexane ethyl dimethoxy silane, γ-mercapto propyl group dimethoxy silane KH-590, γ-mercaptopropyltriethoxysilane KH-845-4, γ-An Bingjisanyiyangjiguiwan KH-550, WD-50, N-β-aminoethyl-γ-nitrogen propyl trimethoxy silicane KH-792, WD-51, γ-urea groups propyl-triethoxysilicane, anilinomethyl triethoxysilane ND-42, anilinomethyl dimethoxy silane ND-73, ɑ monomethyl acryloyl-oxy Union carbide A-162 ND-NS, hexyl amino methyl triethoxyl silane ND-24, dimethyldiethoxysilane DDS, the KH-567 silane coupling agent, the KH-460 silane coupling agent, the KH-450 silane coupling agent, KH-578 silane coupling agent, KH-470 silane coupling agent, the KH-5501 silane coupling agent, KH792, DL602, DL171 silane coupling agent.
5. the method with inorganic-organic composite silicon colloidal sol sealing aluminium alloy anode oxide film hole according to claim 1, it is characterized in that: above-mentioned filler powder is: glass fibre, silicon-dioxide, aluminum oxide, titanium oxide, zirconium white, magnesium oxide, calcium oxide, zinc oxide, ferric oxide, white carbon black, silicate, talcum powder, mica, potter's clay, aluminium hydroxide, iron powder, aluminium powder, silica flour, Fe
3Nanometers such as Al powder, asbestos, magnesium hydroxide, graphite, boron nitride, carbon black, lime carbonate, calcium sulfate, barium sulfate, carboxymethyl cellulose, Resins, epoxy, poly-ammonia are cruel, resol and melamine resin (0.1 ~ 100nm) or the powder of micron (0.1 ~ 100 μ m) material.
6. the method with inorganic-organic composite silicon colloidal sol sealing aluminium alloy anode oxide film hole according to claim 1, it is characterized in that: above-mentioned tensio-active agent is organic surface active agent (dispersion agent), inorganic dispersant, organic dispersing agent has vinylformic acid (ester), the polymethyl acid amide, polymethyl acrylic acid, the polyethylene quadrol, the N-N-dimethyl formamide, trolamine, the citric acid diamines, polyvinyl alcohol, polyvinyl butyral acetal, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, month water glass, polyoxyethylene glycol, Soxylat A 25-7, polyethenoxy ether, Polyvinylpyrolidone (PVP), oleic acid, citric acid, toxilic acid (ester) and they and derivative, the hydrophobic side monomer mostly is unsaturated hydro carbons, as vinylbenzene, ethene, divinyl, diisobutylene, ethylene methacrylic ether, vinyl acetate, a-vinyl toluene etc., poly-phosphate (as Sodium hexametaphosphate 99), silicate etc., inorganic dispersant has: yellow soda ash, Sodium Tetraborate, Sodium hexametaphosphate 99, sodium polyphosphate, Potassium tripolyphosphate (KTPP) and tetrapotassium pyrophosphate (TKPP) etc.
7. the method with inorganic-organic composite silicon colloidal sol sealing aluminium alloy anode oxide film hole according to claim 1, it is characterized in that: above-mentioned organic solvent is: organic solvents such as ethanol, ethylene glycol, methyl alcohol, butanols, benzene,toluene,xylene, chloroform.
8. the method with inorganic-organic composite silicon colloidal sol sealing aluminium alloy anode oxide film hole according to claim 1, it is characterized in that: above-mentioned comprehensive silicon colloidal sol can be replaced by the mixing solutions of single or two or more silane with alcohol, water, also can replace by the aqueous solution of single or two or more silane, also can by single inorganic silicon sol solution by be coated with, brush, the mode of the spraying of dipping, high-pressure air, electrostatic spraying prepares coating, more than replaces all can adding or not add in the liquid dispersion agent that powder that right item 5 carried and right item 6 are carried.
9. the method with inorganic-organic composite silicon colloidal sol sealing aluminium alloy anode oxide film hole according to claim 1, it is characterized in that: above-mentioned comprehensive silicon colloidal sol can not add powder and dispersion agent, is only mixed by one or more organosilanes and inorganic silicon colloidal sol.
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