CN110552039A - secondary oxidation sealing process - Google Patents
secondary oxidation sealing process Download PDFInfo
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- CN110552039A CN110552039A CN201910062033.1A CN201910062033A CN110552039A CN 110552039 A CN110552039 A CN 110552039A CN 201910062033 A CN201910062033 A CN 201910062033A CN 110552039 A CN110552039 A CN 110552039A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/12—Anodising more than once, e.g. in different baths
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/16—Pretreatment, e.g. desmutting
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/20—Electrolytic after-treatment
- C25D11/22—Electrolytic after-treatment for colouring layers
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
the invention relates to a secondary oxidation sealing process, which comprises the production procedures of oil removal, primary water washing, alkaline etching, secondary water washing, acid etching, tertiary water washing, primary oxidation, quartic water washing, sealing, quintic water washing, secondary oxidation, sextuplet water washing, coloring, hot water washing, pure water washing, electrophoresis, heptad water washing, draining, curing and packaging. The secondary oxidation sealing process can improve the adhesive force of the oxide film, improve the attractive effect and improve the product.
Description
Technical Field
the invention relates to a secondary oxidation sealing process, and belongs to the technical field of hardware production.
Background
because the aluminum product has the advantages of small density, light weight, strong plasticity and the like, the aluminum product is applied to various fields of national economy. At present, most of aluminum products on the market are directly subjected to subsequent process processing only after primary oxidation and highlight treatment, and the oxidation film of the product is easily damaged only after the product is subjected to primary oxidation, so that the oxidation film on the surface of the product is easy to fall off, the quality problems such as insufficient adhesive force and the like are caused, and the appearance and the service performance of the product are influenced due to the fact that the product surface subjected to highlight treatment is easily subjected to undesirable phenomena such as white fog, knife lines, corrosion and the like.
Disclosure of Invention
The invention aims to overcome the defects and provide a secondary oxidation sealing process for improving the adhesive force of an oxide film, improving the attractive effect and improving the service performance of a product.
The purpose of the invention is realized as follows: a secondary oxidation sealing process comprises the following steps:
Step one, removing oil
putting the aluminum product into an oil removing tank for oil removing treatment, and standing at normal temperature for 2-8 min;
step two, primary water washing
placing the deoiled aluminum product into a first washing tank for standing for 15-25 s;
Step three, alkaline etching
Placing the aluminum product subjected to primary water washing into an alkaline washing tank for alkaline washing treatment, and standing at the temperature of 40-70 ℃ for 6-12 min;
Step four, secondary water washing
placing the aluminum product subjected to alkali washing in a second water washing tank for standing for 15-25 s;
Step five, acid etching
Placing the aluminum product subjected to secondary water washing into a pickling tank, and standing for 4-10min at the temperature of 32-48 ℃ for pickling treatment;
Step six, washing for three times
Placing the pickled aluminum product into a third water washing tank for standing for 20-35 s;
Step seven, primary oxidation
Placing the washed aluminum product into a first oxidation tank for electrolytic oxidation, and placing the aluminum product for a corresponding time according to the thickness of a generated oxide film at the temperature of 16-22 ℃;
Eight and four times of water washing
Placing the aluminum product subjected to primary oxidation into a fourth rinsing bath and standing for 25-30 s;
Ninth step, sealing
Placing the washed aluminum product into a hole sealing groove for sealing treatment, and placing the aluminum product for corresponding time according to the thickness of a generated oxide film at the temperature of 35-40 ℃;
Ten and five times of water washing
Placing the sealed aluminum product into a fifth washing tank for standing for 15-25 s;
Step eleven, secondary oxidation
Placing the washed aluminum product into a second oxidation tank for electrolytic oxidation, and standing at 16-22 deg.C for 10-30 min;
Twelve and six times of water washing
Placing the aluminum product subjected to secondary oxidation into a sixth water washing tank for 20-30 s;
Thirteen step of coloring
placing the washed aluminum product into a coloring tank for electrolytic coloring treatment, and placing the aluminum product for a corresponding time according to the actual required color depth at the temperature of 18-22 ℃;
Washing with water for fourteen or seven times
placing the colored aluminum product in a seventh water washing tank for 30-40 s;
Fifteen step of draining
Step sixteen, curing
Seventeen, packaging.
preferably, the oil removing agent in the first step is free sulfuric acid with the concentration of 160-200 g/l.
Preferably, in the step one, a proper amount of nitric acid is added according to the actual production requirement.
preferably, the alkali wash in the second step adopts free alkali with the concentration of 20-60g/l and Al 3+ with the concentration of 20-60 g/l.
preferably, in the fifth step, the pickling agent is ammonium hydrogen fluoride, and the concentration of the ammonium hydrogen fluoride is 30-50 g/l.
Preferably, the aluminum product after being washed with water in the seventh step is put into a first oxidation tank to be subjected to electrolytic oxidation by applying a low-voltage current with a voltage of 16-20v and a voltage of 1.2-1.5A/dm 2.
Preferably, the oxidizing agent in the seventh step adopts free sulfuric acid with the concentration of 150-200g/l and Al 3+ with the concentration of 5-15 g/l.
Preferably, in the ninth step, the hole sealing agent adopts nickel ions with the concentration of 0.5-1.2g/l and fluorine ions with the concentration of 0.2-0.6g/l, and the pH value is 4.5-7.0.
preferably, in the thirteen step, the aluminum product after being washed by water is put into a coloring tank, and low-voltage current with the voltage of 18-24v and the voltage of 0.6-1.0A/dm 2 is applied for electrolytic coloring treatment.
preferably, in the thirteen-step coloring agent, stannous sulfate with the concentration of 5-10g/l, nickel sulfate with the concentration of 12-24g/l and free sulfuric acid with the concentration of 12-24g/l are adopted, and the pH value is 0.8-1.4.
compared with the prior art, the invention has the beneficial effects that:
The secondary oxidation sealing process has the advantages of improving the adhesive force of the oxide film, improving the attractive effect and improving the service performance of the product.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments of the present invention, 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 invention relates to a secondary oxidation sealing process, which comprises the main production procedures of oil removal, primary water washing, alkaline etching, secondary water washing, acid etching, tertiary water washing, primary oxidation, quaternary water washing, sealing, quintic water washing, secondary oxidation, sextuple water washing, coloring, seven-time water washing, draining, curing and packaging;
the specific production steps are as follows:
Step one, removing oil
Putting the aluminum product into an oil removing tank for oil removing treatment, standing at normal temperature for 2-8min, and adding a proper amount of nitric acid according to actual production requirements to prevent snowflake spots;
Preferably, the oil removing agent is free sulfuric acid with the concentration of 160-200 g/l;
step two, primary water washing
Placing the deoiled aluminum product into a first washing tank for standing for 15-25 s;
Step three, alkaline etching
Placing the aluminum product subjected to primary water washing into an alkaline washing tank for alkaline washing treatment, and standing at the temperature of 40-70 ℃ for 6-12 min;
Preferably, the alkali cleaning agent adopts free alkali with the concentration of 20-60g/l and Al 3+ with the concentration of 20-60 g/l;
step four, secondary water washing
placing the aluminum product subjected to alkali washing in a second water washing tank for standing for 15-25 s;
step five, acid etching
Placing the aluminum product subjected to secondary water washing into a pickling tank, standing at 32-48 ℃ for 4-10min for pickling treatment, and removing the hanging ash remained on the surface of the aluminum product subjected to alkaline etching to ensure that the surface of the aluminum product is bright;
preferably, the acid washing agent is ammonium hydrogen fluoride, and the concentration of the acid washing agent is 30-50 g/l;
Step six, washing for three times
Placing the pickled aluminum product into a third water washing tank for standing for 20-35 s;
Step seven, primary oxidation
Placing the washed aluminum product into a first oxidation tank for electrolytic oxidation to generate a layer of artificial oxidation film with pores on the surface of the aluminum product, and placing the aluminum product for a corresponding time according to the thickness of the generated oxidation film at the temperature of 16-22 ℃;
preferably, the oxidant adopts free sulfuric acid with the concentration of 150-200g/l and Al 3+ with the concentration of 5-15 g/l;
eight and four times of water washing
Placing the aluminum product subjected to primary oxidation into a fourth rinsing bath and standing for 25-30 s;
Ninth step, sealing
Placing the washed aluminum product into a hole sealing groove for sealing treatment, and placing the aluminum product for corresponding time according to the thickness of a generated oxide film at the temperature of 35-40 ℃;
Preferably, the hole sealing agent adopts nickel ions with the concentration of 0.5-1.2g/l and fluorine ions with the concentration of 0.2-0.6g/l, and the PH value is 4.5-7.0;
ten and five times of water washing
Placing the sealed aluminum product into a fifth washing tank for standing for 15-25 s;
step eleven, secondary oxidation
Placing the washed aluminum product into a second oxidation tank for electrolytic oxidation, and standing at 16-22 deg.C for 10-30 min;
twelve and six times of water washing
Placing the aluminum product subjected to secondary oxidation into a sixth water washing tank for 20-30 s;
Thirteen step of coloring
Putting the washed aluminum product into a coloring tank, applying low-voltage current with the voltage of 18-24v and the voltage of 0.6-1.0A/dm 2 to perform electrolytic coloring treatment, and standing for corresponding time according to the actual required color depth under the temperature condition of 18-22 ℃;
Preferably, the colorant adopts stannous sulfate with the concentration of 5-10g/l, nickel sulfate with the concentration of 12-24g/l and free sulfuric acid with the concentration of 12-24g/l, and the pH value is 0.8-1.4;
washing with water for fourteen or seven times
placing the colored aluminum product in a seventh water washing tank for 30-40 s;
fifteen step of draining
Step sixteen, curing
Seventeen, packaging.
Example one
a secondary oxidation sealing process is characterized in that: the production process comprises the following steps:
Step one, removing oil
Putting the aluminum product into an oil removing tank for oil removing treatment, and standing for 3min at normal temperature;
step two, primary water washing
placing the deoiled aluminum product into a first washing tank for standing for 15 s;
Step three, alkaline etching
Placing the aluminum product subjected to primary water washing into an alkaline washing tank for alkaline washing treatment, and placing for 6min at the temperature of 42 ℃;
Step four, secondary water washing
placing the aluminum product subjected to alkali washing in a second water washing tank for standing for 18 s;
step five, acid etching
placing the aluminum product subjected to secondary water washing into a pickling tank, and standing for 5min at the temperature of 33 ℃ for pickling treatment;
step six, washing for three times
Placing the pickled aluminum product into a third rinsing bath for standing for 25 s;
Step seven, primary oxidation
Placing the washed aluminum product into a first oxidation tank for electrolytic oxidation to generate an artificial oxidation film with the thickness of 5um on the surface of the aluminum product, and placing for 12min at the temperature of 18 ℃;
Eight and four times of water washing
Placing the aluminum product subjected to primary oxidation into a fourth rinsing bath for standing for 25 s;
ninth step, sealing
Placing the washed aluminum product into a hole sealing groove for sealing treatment, and placing the aluminum product for corresponding time according to the thickness of the generated oxide film at the temperature of 35 ℃;
ten and five times of water washing
Placing the sealed aluminum product into a fifth washing tank for standing for 18 s;
Step eleven, secondary oxidation
placing the washed aluminum product into a second oxidation tank for electrolytic oxidation, and placing for 15min at the temperature of 18 ℃;
Twelve and six times of water washing
Placing the aluminum product subjected to secondary oxidation in a sixth water washing tank for 22 s;
thirteen step of coloring
placing the washed aluminum product into a coloring tank for electrolytic coloring treatment, and standing at 18 deg.C for 4 min;
Washing with water for fourteen or seven times
placing the colored aluminum product in a seventh rinsing bath for 30 s;
fifteen step of draining
step sixteen, curing
Seventeen, packaging.
Example two
a secondary oxidation sealing process is characterized in that: the production process comprises the following steps:
step one, removing oil
Putting the aluminum product into an oil removing tank for oil removing treatment, and standing for 5min at normal temperature;
step two, primary water washing
placing the deoiled aluminum product into a first washing tank for standing for 18 s;
step three, alkaline etching
Placing the aluminum product subjected to primary water washing into an alkaline washing tank for alkaline washing treatment, and placing for 7min at the temperature of 45 ℃;
Step four, secondary water washing
Placing the aluminum product subjected to alkali washing in a second water washing tank for standing for 20 s;
Step five, acid etching
Placing the aluminum product subjected to secondary water washing into a pickling tank, and standing for 7min at the temperature of 40 ℃ for pickling treatment;
step six, washing for three times
Placing the pickled aluminum product into a third rinsing bath and standing for 20 s;
Step seven, primary oxidation
placing the washed aluminum product into a first oxidation tank for electrolytic oxidation to generate an artificial oxidation film with the thickness of 8um on the surface of the aluminum product, and placing for 18min at the temperature of 20 ℃;
Eight and four times of water washing
Placing the aluminum product subjected to primary oxidation into a fourth rinsing bath for standing for 28 s;
ninth step, sealing
Placing the washed aluminum product into a hole sealing groove for sealing treatment, and placing for a corresponding time according to the thickness of the generated oxide film at the temperature of 36 ℃;
Ten and five times of water washing
placing the sealed aluminum product into a fifth washing tank for standing for 20 s;
Step eleven, secondary oxidation
Placing the washed aluminum product into a second oxidation tank for electrolytic oxidation, and placing for 18min at the temperature of 20 ℃;
twelve and six times of water washing
Placing the aluminum product subjected to secondary oxidation into a sixth water washing tank for 25 s;
Thirteen step of coloring
Placing the washed aluminum product into a coloring tank for electrolytic coloring treatment, and standing at 20 deg.C for 5 min;
washing with water for fourteen or seven times
Placing the colored aluminum product in a seventh rinsing bath for 32 s;
Fifteen step of draining
Step sixteen, curing
seventeen, packaging.
EXAMPLE III
a secondary oxidation sealing process is characterized in that: the production process comprises the following steps:
Step one, removing oil
Putting the aluminum product into an oil removing tank for oil removing treatment, and standing at normal temperature for 8 min;
Step two, primary water washing
placing the deoiled aluminum product into a first washing tank for standing for 22 s;
Step three, alkaline etching
placing the aluminum product subjected to primary water washing into an alkaline washing tank for alkaline washing treatment, and placing for 10min at the temperature of 58 ℃;
Step four, secondary water washing
placing the aluminum product subjected to alkali washing in a second water washing tank for standing for 25 s;
Step five, acid etching
placing the aluminum product subjected to secondary water washing into a pickling tank, and standing at the temperature of 45 ℃ for 8min for pickling treatment;
step six, washing for three times
Placing the pickled aluminum product into a third rinsing bath and standing for 20 s;
step seven, primary oxidation
Placing the washed aluminum product into a first oxidation tank for electrolytic oxidation to generate an artificial oxidation film with the thickness of 14um on the surface of the aluminum product, and placing for 25min at the temperature of 21 ℃;
Eight and four times of water washing
placing the aluminum product subjected to primary oxidation into a fourth rinsing bath and standing for 30 s;
ninth step, sealing
Placing the washed aluminum product into a hole sealing groove for sealing treatment, and placing the aluminum product for corresponding time according to the thickness of the generated oxide film at the temperature of 40 ℃;
Ten and five times of water washing
Placing the sealed aluminum product into a fifth washing tank for standing for 25 s;
step eleven, secondary oxidation
Placing the washed aluminum product into a second oxidation tank for electrolytic oxidation, and placing for 24min at the temperature of 21 ℃;
twelve and six times of water washing
placing the aluminum product subjected to secondary oxidation into a sixth water washing tank for 28 s;
Thirteen step of coloring
placing the washed aluminum product into a coloring tank for electrolytic coloring treatment, and standing at 22 deg.C for 8 min;
Washing with water for fourteen or seven times
Placing the colored aluminum product into a seventh rinsing bath for 35 s;
Fifteen step of draining
step sixteen, curing
Seventeen, packaging.
the above is only a specific application example of the present invention, and the protection scope of the present invention is not limited in any way. All the technical solutions formed by equivalent transformation or equivalent replacement fall within the protection scope of the present invention.
Claims (10)
1. a secondary oxidation sealing process is characterized in that: the production process comprises the following steps:
step one, removing oil
Putting the aluminum product into an oil removing tank for oil removing treatment, and standing at normal temperature for 2-8 min;
step two, primary water washing
Placing the deoiled aluminum product into a first washing tank for standing for 15-25 s;
step three, alkaline etching
placing the aluminum product subjected to primary water washing into an alkaline washing tank for alkaline washing treatment, and standing at the temperature of 40-70 ℃ for 6-12 min;
step four, secondary water washing
Placing the aluminum product subjected to alkali washing in a second water washing tank for standing for 15-25 s;
Step five, acid etching
placing the aluminum product subjected to secondary water washing into a pickling tank, and standing for 4-10min at the temperature of 32-48 ℃ for pickling treatment;
Step six, washing for three times
placing the pickled aluminum product into a third water washing tank for standing for 20-35 s;
Step seven, primary oxidation
Placing the washed aluminum product into a first oxidation tank for electrolytic oxidation, and placing the aluminum product for a corresponding time according to the thickness of a generated oxide film at the temperature of 16-22 ℃;
Eight and four times of water washing
Placing the aluminum product subjected to primary oxidation into a fourth rinsing bath and standing for 25-30 s;
Ninth step, sealing
Placing the washed aluminum product into a hole sealing groove for sealing treatment, and placing the aluminum product for corresponding time according to the thickness of a generated oxide film at the temperature of 35-40 ℃;
Ten and five times of water washing
placing the sealed aluminum product into a fifth washing tank for standing for 15-25 s;
step eleven, secondary oxidation
Placing the washed aluminum product into a second oxidation tank for electrolytic oxidation, and standing at 16-22 deg.C for 10-30 min;
Twelve and six times of water washing
placing the aluminum product subjected to secondary oxidation into a sixth water washing tank for 20-30 s;
thirteen step of coloring
Placing the washed aluminum product into a coloring tank for electrolytic coloring treatment, and placing the aluminum product for a corresponding time according to the actual required color depth at the temperature of 18-22 ℃;
washing with water for fourteen or seven times
Placing the colored aluminum product in a seventh water washing tank for 30-40 s;
fifteen step of draining
step sixteen, curing
seventeen, packaging.
2. the secondary oxidation sealing process according to claim 1, wherein: preferably, the oil removing agent in the first step is free sulfuric acid with the concentration of 160-200 g/l.
3. The secondary oxidation sealing process according to claim 1, wherein: preferably, in the step one, a proper amount of nitric acid is added according to the actual production requirement.
4. The secondary oxidation sealing process according to claim 1, wherein the alkali wash in the second step is preferably free alkali with a concentration of 20-60g/l and Al 3+ with a concentration of 20-60 g/l.
5. The secondary oxidation sealing process according to claim 1, wherein: preferably, in the fifth step, the pickling agent is ammonium hydrogen fluoride, and the concentration of the ammonium hydrogen fluoride is 30-50 g/l.
6. the secondary oxidation sealing process according to claim 1, wherein the aluminum product washed with water in step seven is preferably subjected to electrolytic oxidation by applying a low-voltage current of 16-20v and 1.2-1.5A/dm 2 in the first oxidation tank.
7. The secondary oxidation blocking process according to claim 1, wherein the oxidizing agent used in step seven is preferably free sulfuric acid with a concentration of 150-200g/l and Al 3+ with a concentration of 5-15 g/l.
8. the secondary oxidation sealing process according to claim 1, wherein: preferably, in the ninth step, the hole sealing agent adopts nickel ions with the concentration of 0.5-1.2g/l and fluorine ions with the concentration of 0.2-0.6g/l, and the pH value is 4.5-7.0.
9. the secondary oxidation sealing process according to claim 1, wherein preferably, in step thirteen, the aluminum product after water washing is placed in a coloring tank, and low-voltage current with voltage of 18-24v and 0.6-1.0A/dm 2 is applied to perform electrolytic coloring treatment.
10. The secondary oxidation sealing process according to claim 1, wherein: preferably, in the thirteen-step coloring agent, stannous sulfate with the concentration of 5-10g/l, nickel sulfate with the concentration of 12-24g/l and free sulfuric acid with the concentration of 12-24g/l are adopted, and the pH value is 0.8-1.4.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112609219A (en) * | 2020-11-17 | 2021-04-06 | 中国航发西安动力控制科技有限公司 | Bath solution for red anodic oxidation of aluminum alloy material and process method |
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