CN102732934B - The method in aluminium alloy anode oxide film hole closed by a kind of silicon sol - Google Patents
The method in aluminium alloy anode oxide film hole closed by a kind of silicon sol Download PDFInfo
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Abstract
The method in aluminium alloy anode oxide film hole closed by silicon sol, comprises following processing step: carry out suitable pre-treatment to aluminium or aluminium alloy, carry out anodic oxidation treatment with the technique of routine to it; Remove to process the aluminum or aluminum alloy of anodic oxidation treatment, electrophoretic deposition, oven dry, sintering with electrophoretic method with different processing condition, thus generate silicon oxide ceramics coating while closed Al and Alalloy anodic oxidation fenestra.Electrophoretic deposition method simple process provided by the present invention, easy to implement and without the need to higher conditional request, prepared ceramic coating is fine and close, functional, uniform composition.This technique can be used for closed aluminum or aluminum alloy anodic oxidation micropore, and in anodic oxidation fenestra, electrophoresis silicon sol technique cleanliness without any pollution easily realizes industrialization.
Description
Technical field
The present invention relates to a kind of for closed aluminum or aluminum alloy and the method containing micropore after aluminium parts anodic oxidation, the method in aluminium alloy anode oxide film hole is closed in particular to a kind of silicon sol, especially by carrying out repeatedly sealing of hole under the condition of low voltage, and then good sealing of hole effect can be realized.
Background technology
Specific tenacity is high owing to having for aluminium and aluminium alloy thereof, heat conduction and good conductivity, advantage that quality is light, be with a wide range of applications in the modern industries such as aerospace, building, automobile.But aluminium alloy matter soft, wear no resistance, be easily corroded.The Nature comparison of aluminium is active, and the oxide film that surface is formed in atmosphere has certain etch resistant properties, but the thickness of this oxide film only has a few nanometer to tens nanometers, and hardness is also very low, and the ability of opposing environmental attack is poor.Therefore usually first carry out necessary surface Hardening Treatment in use, Aluminum-aluminum alloy is placed in suitable electrolytic solution and carries out energising process as anode, under the effect of extra electric field, layer oxide film can be formed on the surface at aluminum products, thickness is between 10-200um, its solidity to corrosion, wear resistance, electrical insulating property improves greatly, this makes the range of application of Aluminum-aluminum alloy material 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, easily contaminated and corrosive medium corrodes, particularly aggressiveness negatively charged ion (as Cl-, S
2-, cation etc.) and water molecules etc. still can, through oxide film, cause solidity to corrosion (particularly pitting corrosion) and wear resistance to be deteriorated, therefore must carry out sealing pores, improve its solidity to corrosion, contamination resistance and fixed pigment ability of immigrants.
Summary of the invention
Object of the present invention, is to provide a kind of method that aluminium alloy anode oxide film hole closed by silicon sol, to improve erosion resistance and the resistance to crocking of film.
The technical scheme adopted is:
The method in aluminium alloy anode oxide film hole closed by silicon sol, comprises following processing step:
(1) pre-treatment: loose scale is carried out on aluminum or aluminum alloy surface, oil removing, descaling, bright dipping pre-treatment, polishing uses sand paper from coarse to fine, and the sand paper model of final choice is 2000
#; The salpeter solution that descaling is used: deionized water=0.5 ~ 2:1; Alkaline etching alkali concn used is 20 ~ 50g/L; After alkaline etching, workpiece surface often adheres to one deck dust, and carry out anodic oxidation treatment after removing dust by light-emitting solution, light-emitting solution adopts salpeter solution, and nitric acid: water=0.5 ~ 2:1 is stand-by;
(2) anodic oxidation: the aluminum or aluminum alloy after pre-treatment is carried out anodic oxidation, and direct supply is selected in anodic oxidation, the voltage of supply 8 ~ 22V of setting, current density 1.0 ~ 2.2A/dm
2, anodizing time is 10 ~ 60min, obtains the anode oxide film that thickness is 5 ~ 20 μm;
(3) electrophoretic deposition is closed: with 0.1 ~ 20A/dm
2current density under 0.1 ~ 100V voltage, electrophoresis silicon sol is deposited in aluminum or aluminum alloy anodic oxidation fenestra, by washed with de-ionized water, repeats 0 ~ 10 time;
(4) dry: dry 10 minutes ~ 24 hours at 50 ~ 120 DEG C, obtain dry rete;
(5) sinter: in retort furnace, sinter 0.5 ~ 5h at 50 ~ 1200 DEG C, obtain the good rete of sticking power;
Colloidal sol within the scope of above-mentioned electrophoresis silicon sol to be commercially available particle diameter be 10 ~ 20nm scope or 8 ~ 100nm, or under lab prepare voluntarily, be known technology.
First the present invention carries out suitable pre-treatment to aluminum or aluminum alloy and containing aluminium parts, with certain anode oxidation process, obtains the anode oxide film that thickness is 5 ~ 20 μm; According to method described in claims, obtain or buy required silicon sol, then with the method for electrophoresis, silicon sol " swimming " is arrived through the good aluminum or aluminum alloy of anodic oxidation treatment and containing aluminium parts, the laggard overbaking of electrophoresis is just at aluminum or aluminum alloy and containing aluminium parts with the addition of the good at least one deck coat of one deck sticking power after doing and sintering, and this coating can be thin ceramic coating also can be a kind of silica sol-gel (Sol-Gel) coating.
According to the embodiment of the present invention, the thin ceramic coating that different silicon sol obtains also can be a kind of thickness of silica sol-gel (Sol-Gel) coating is 0.5 ~ 25 μm.
The invention has the advantages that:
The present invention closes Al and Alalloy anode oxide film fenestra by electrophoretic method silicon sol, replace the dichromate sealing technique of aluminium alloy anode oxide film, alleviate the pollution to environment, electrophoretic deposition technique is a kind of surface coating process of gentleness, the phase transformation that pyroprocess can be avoided to cause and embrittlement; Technique easily realizes, and equipment is comparatively simple, and depositing operation is easy to control, and realize industrialization cost low, film is even.
Embodiment
Embodiment 1
The method in aluminium alloy anode oxide film hole closed by silicon sol, comprises following processing step:
(1) pre-treatment: loose scale is carried out on aluminum or aluminum alloy surface, oil removing, descaling, bright dipping pre-treatment, polishing uses sand paper from coarse to fine, and the sand paper model of final choice is 2000
#; The salpeter solution that descaling is used: deionized water=0.5:1; Alkaline etching alkali concn used is 20g/L; After alkaline etching, workpiece surface often adheres to one deck dust, and carry out anodic oxidation treatment after removing dust by light-emitting solution, light-emitting solution adopts salpeter solution, and nitric acid: water=0.5:1 is stand-by;
(2) anodic oxidation: the aluminum or aluminum alloy after pre-treatment is carried out anodic oxidation, and direct supply is selected in anodic oxidation, the voltage of supply 8V of setting, current density 1.0A/dm
2, anodizing time is 10min, obtains the anode oxide film that thickness is 5 μm;
(3) electrophoretic deposition is closed: use 0.1A/dm
2current density under 0.1V voltage, electrophoresis silicon sol is deposited in aluminum or aluminum alloy anodic oxidation fenestra, by washed with de-ionized water, repeats 1 time;
(4) dry: dry 24 hours at 50 DEG C, obtain dry rete;
(5) sinter: in retort furnace, sinter 0.5h at 1200 DEG C, obtain the good rete of sticking power;
Colloidal sol within the scope of above-mentioned electrophoresis silicon sol to be commercially available particle diameter be 10 ~ 20nm scope or 8 ~ 100nm, or under lab prepare voluntarily, be known technology.
Embodiment 2
The method in aluminium alloy anode oxide film hole closed by silicon sol, comprises following processing step:
(1) pre-treatment: loose scale is carried out on aluminum or aluminum alloy surface, oil removing, descaling, bright dipping pre-treatment, polishing uses sand paper from coarse to fine, and the sand paper model of final choice is 2000
#; The salpeter solution that descaling is used: deionized water=1:1; Alkaline etching alkali concn used is 30g/L; After alkaline etching, workpiece surface often adheres to one deck dust, and carry out anodic oxidation treatment after removing dust by light-emitting solution, light-emitting solution adopts salpeter solution, and nitric acid: water=1:1 is stand-by;
(2) anodic oxidation: the aluminum or aluminum alloy after pre-treatment is carried out anodic oxidation, and direct supply is selected in anodic oxidation, the voltage of supply 15V of setting, current density 1.6A/dm
2, anodizing time is 40min, obtains the anode oxide film that thickness is 12 μm;
(3) electrophoretic deposition is closed: use 10A/dm
2current density under 50V voltage, electrophoresis silicon sol is deposited in aluminum or aluminum alloy anodic oxidation fenestra, by washed with de-ionized water, repeats 5 times;
(4) dry: dry 10 hours at 80 DEG C, obtain dry rete;
(5) sinter: in retort furnace, sinter 3h at 600 DEG C, obtain the good rete of sticking power;
Colloidal sol within the scope of above-mentioned electrophoresis silicon sol to be commercially available particle diameter be 10 ~ 20nm scope or 8 ~ 100nm, or under lab prepare voluntarily, be known technology.
Embodiment 3
The method in aluminium alloy anode oxide film hole closed by silicon sol, comprises following processing step:
(1) pre-treatment: loose scale is carried out on aluminum or aluminum alloy surface, oil removing, descaling, bright dipping pre-treatment, polishing uses sand paper from coarse to fine, and the sand paper model of final choice is 2000
#; The salpeter solution that descaling is used: deionized water=2:1; Alkaline etching alkali concn used is 50g/L; After alkaline etching, workpiece surface often adheres to one deck dust, and carry out anodic oxidation treatment after removing dust by light-emitting solution, light-emitting solution adopts salpeter solution, and nitric acid: water=2:1 is stand-by;
(2) anodic oxidation: the aluminum or aluminum alloy after pre-treatment is carried out anodic oxidation, and direct supply is selected in anodic oxidation, the voltage of supply 22V of setting, current density 2.2A/dm
2, anodizing time is 60min, obtains the anode oxide film that thickness is 20 μm;
(3) electrophoretic deposition is closed: use 20A/dm
2current density under 100V voltage, electrophoresis silicon sol is deposited in aluminum or aluminum alloy anodic oxidation fenestra, by washed with de-ionized water, repeats 10 times;
(4) dry: dry 10 minutes at 120 DEG C, obtain dry rete;
(5) sinter: in retort furnace, sinter 5h at 50 DEG C, obtain the good rete of sticking power;
Colloidal sol within the scope of above-mentioned electrophoresis silicon sol to be commercially available particle diameter be 10 ~ 20nm scope or 8 ~ 100nm, or under lab prepare voluntarily, be known technology.
Claims (4)
1. close the method in aluminium alloy anode oxide film hole with silicon sol, it is characterized in that, comprise following processing step:
(1) pre-treatment: loose scale is carried out on aluminum or aluminum alloy surface, oil removing, descaling, bright dipping pre-treatment, polishing uses sand paper from coarse to fine, and the sand paper model of final choice is 2000
#; The salpeter solution that descaling is used: deionized water=0.5 ~ 2:1; Alkaline etching alkali concn used is 20 ~ 50g/L; After alkaline etching, workpiece surface often adheres to one deck dust, and carry out anodic oxidation treatment after removing dust by light-emitting solution, light-emitting solution adopts salpeter solution, and nitric acid: water=0.5 ~ 2:1 is stand-by;
(2) anodic oxidation: the aluminum or aluminum alloy after pre-treatment is carried out anodic oxidation, and direct supply is selected in anodic oxidation, the voltage of supply 8 ~ 22V of setting, current density 1.0 ~ 2.2A/dm
2, anodizing time is 10 ~ 60min, obtains the anode oxide film that thickness is 5 ~ 20 μm;
(3) electrophoretic deposition is closed: with 0.1 ~ 20A/dm
2current density under 0.1 ~ 100V voltage, electrophoresis silicon sol is deposited in aluminum or aluminum alloy anodic oxidation fenestra, by washed with de-ionized water, repeats 0 ~ 10 time;
(4) dry: dry 10 minutes ~ 24 hours at 50 ~ 120 DEG C, obtain dry rete;
(5) sinter: in retort furnace, sinter 0.5 ~ 5h at 50 ~ 1200 DEG C, obtain the good rete of sticking power.
2. the method in aluminium alloy anode oxide film hole closed by a kind of silicon sol according to claim 1, it is characterized in that, comprises following processing step:
(1) pre-treatment: loose scale is carried out on aluminum or aluminum alloy surface, oil removing, descaling, bright dipping pre-treatment, polishing uses sand paper from coarse to fine, and the sand paper model of final choice is 2000
#; The salpeter solution that descaling is used: deionized water=0.5:1; Alkaline etching alkali concn used is 20g/L; After alkaline etching, workpiece surface often adheres to one deck dust, and carry out anodic oxidation treatment after removing dust by light-emitting solution, light-emitting solution adopts salpeter solution, and nitric acid: water=0.5:1 is stand-by;
(2) anodic oxidation: the aluminum or aluminum alloy after pre-treatment is carried out anodic oxidation, and direct supply is selected in anodic oxidation, the voltage of supply 8V of setting, current density 1.0A/dm
2, anodizing time is 10min, obtains the anode oxide film that thickness is 5 μm;
(3) electrophoretic deposition is closed: use 0.1A/dm
2current density under 0.1V voltage, electrophoresis silicon sol is deposited in aluminum or aluminum alloy anodic oxidation fenestra, by washed with de-ionized water, repeats 1 time;
(4) dry: dry 24 hours at 50 DEG C, obtain dry rete;
(5) sinter: in retort furnace, sinter 0.5h at 1200 DEG C, obtain the good rete of sticking power.
3. the method in aluminium alloy anode oxide film hole closed by a kind of silicon sol according to claim 1, it is characterized in that, comprises following processing step:
(1) pre-treatment: loose scale is carried out on aluminum or aluminum alloy surface, oil removing, descaling, bright dipping pre-treatment, polishing uses sand paper from coarse to fine, and the sand paper model of final choice is 2000
#; The salpeter solution that descaling is used: deionized water=1:1; Alkaline etching alkali concn used is 30g/L; After alkaline etching, workpiece surface often adheres to one deck dust, and carry out anodic oxidation treatment after removing dust by light-emitting solution, light-emitting solution adopts salpeter solution, and nitric acid: water=1:1 is stand-by;
(2) anodic oxidation: the aluminum or aluminum alloy after pre-treatment is carried out anodic oxidation, and direct supply is selected in anodic oxidation, the voltage of supply 15V of setting, current density 1.6A/dm
2, anodizing time is 40min, obtains the anode oxide film that thickness is 12 μm;
(3) electrophoretic deposition is closed: use 10A/dm
2current density under 50V voltage, electrophoresis silicon sol is deposited in aluminum or aluminum alloy anodic oxidation fenestra, by washed with de-ionized water, repeats 5 times;
(4) dry: dry 10 hours at 80 DEG C, obtain dry rete;
(5) sinter: in retort furnace, sinter 3h at 600 DEG C, obtain the good rete of sticking power.
4. the method in aluminium alloy anode oxide film hole closed by a kind of silicon sol according to claim 1, it is characterized in that, comprises following processing step:
(1) pre-treatment: loose scale is carried out on aluminum or aluminum alloy surface, oil removing, descaling, bright dipping pre-treatment, polishing uses sand paper from coarse to fine, and the sand paper model of final choice is 2000
#; The salpeter solution that descaling is used: deionized water=2:1; Alkaline etching alkali concn used is 50g/L; After alkaline etching, workpiece surface often adheres to one deck dust, and carry out anodic oxidation treatment after removing dust by light-emitting solution, light-emitting solution adopts salpeter solution, and nitric acid: water=2:1 is stand-by;
(2) anodic oxidation: the aluminum or aluminum alloy after pre-treatment is carried out anodic oxidation, and direct supply is selected in anodic oxidation, the voltage of supply 22V of setting, current density 2.2A/dm
2, anodizing time is 60min, obtains the anode oxide film that thickness is 20 μm;
(3) electrophoretic deposition is closed: use 20A/dm
2current density under 100V voltage, electrophoresis silicon sol is deposited in aluminum or aluminum alloy anodic oxidation fenestra, by washed with de-ionized water, repeats 10 times;
(4) dry: dry 10 minutes at 120 DEG C, obtain dry rete;
(5) sinter: in retort furnace, sinter 5h at 50 DEG C, obtain the good rete of sticking power.
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| CN103215630B (en) * | 2013-04-23 | 2016-01-20 | 沈阳理工大学 | The method in aluminium alloy anode oxide film hole is closed with inorganic-organic composite silicon colloidal sol |
| CN106435685B (en) * | 2016-09-18 | 2018-09-07 | 佛山科学技术学院 | The method that aluminium surface electro-deposition prepares low absorptivity and high hemispherical emissivity oxidation film |
| CN106894071B (en) * | 2017-03-10 | 2019-07-26 | 国家开发投资公司 | A kind of aluminum alloy surface method for anticorrosion-treating |
| CN110257876A (en) * | 2018-03-12 | 2019-09-20 | 深圳市裕展精密科技有限公司 | The production method of anode oxide film |
| CN110257875A (en) * | 2018-03-12 | 2019-09-20 | 深圳市裕展精密科技有限公司 | Anode oxide film and preparation method thereof |
| CN110219031B (en) * | 2019-06-06 | 2020-12-08 | 北京航空航天大学 | Anodic oxidation electrolyte and method, and aluminum or aluminum alloy with anodic oxidation film |
| CN111996568A (en) * | 2020-07-21 | 2020-11-27 | 常熟恒富昱光电有限公司 | Processing method for improving surface appearance quality of aluminum structural member |
| CN112760692B (en) * | 2020-12-26 | 2021-10-26 | 佛山市三水凤铝铝业有限公司 | Aluminum alloy anodic oxidation sealing liquid and sealing method thereof |
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