CN109440162A - A kind of aluminium alloy anode oxide film is without nickel hole sealing agent and preparation method - Google Patents
A kind of aluminium alloy anode oxide film is without nickel hole sealing agent and preparation method Download PDFInfo
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- CN109440162A CN109440162A CN201811625408.2A CN201811625408A CN109440162A CN 109440162 A CN109440162 A CN 109440162A CN 201811625408 A CN201811625408 A CN 201811625408A CN 109440162 A CN109440162 A CN 109440162A
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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
- C25D11/24—Chemical after-treatment
- C25D11/246—Chemical after-treatment for sealing layers
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Abstract
The present invention provides a kind of aluminium alloy anode oxide films without nickel hole sealing agent and preparation method, by mass percentage, the aluminium alloy anode oxide film is made of following raw material without nickel hole sealing agent: 3.0~6.0% zinc owner salt compound, 2.0~4.0% complexing agent, 2.0~4.0% sealing of hole promotor, 4.0~10.0% stabilizer, 5.0~15.0% suppression ash brightener, surplus are water.Hole sealing agent operating temperature provided by the invention is low, pH range is wide, there is good sealing of hole effect at concentration 2~6%, pH 3~6,15~35 DEG C of temperature, and the hole sealing agent environmental protection is without nickel, avoid the harm to human body and environment, operating temperature is low, energy saving, process stabilizing only needs regular replenishment hole sealing agent that can keep the sealing of hole performance of sealing of hole slot.
Description
Technical field
The present invention relates to aluminium alloy anode oxide post-processing technology fields, more particularly to a kind of aluminium alloy anode oxide film
Without nickel hole sealing agent and preparation method.
Background technique
A kind of processing technique that anodic oxidation is most widely used as aluminium and aluminum alloy surface, can improve aluminium significantly
And its performance of alloy, it improves aluminium and its alloy surface hardness and wearability must since the surface of oxidation film is there are a large amount of micropores
Sealing pores must be carried out, common method for sealing mainly has boiling water (or steam) sealing of hole, nickel salt sealing of hole, macromolecule resin sealing of hole.
The common higher nickel salt hole sealing agent of sealing quality contains Ni2+To human body and the toxic effect of environment.
To solve Ni2+Exceeded problem, people have found the various metal ions that can be substituted, have described in the related technology
The medium temperature hole sealing agent of low nickel uses the metal salts such as zinc, copper, cerium, magnesium as supplement to reduce the demand to nickel, and this method can not accomplish
Entirely without nickel, and technique required temperature is higher, increases production cost.There are also no nickel hole sealing agents at present, mainly with magnesium and
Lithium cooperates zinc polysilicate or nano zine oxide and fluorine-containing surfactant etc. to obtain a kind of medium temperature hole sealing agent as main salt, but still deposits
The disadvantages of stability is poor, operating temperature is high, pH narrow range.
Summary of the invention
In view of the above situation, the present invention provides that a kind of stabilization, operating temperature is low, pH range is wide and can significantly improve aluminium and aluminium
The hole sealing agent of alloy surface performance.
A kind of aluminium alloy anode oxide film is made of following raw material without nickel hole sealing agent: zinc owner salt compound, complexing agent,
Sealing of hole promotor, stabilizer press down grey brightener, water.
Wherein, by mass percentage, the aluminium alloy anode oxide film is made of following raw material without nickel hole sealing agent: 3.0
~6.0% zinc owner salt compound, 2.0~4.0% complexing agent, 2.0~3.0% sealing of hole promotor, 4.0~10.0%
Stabilizer, 5.0~15.0% suppression ash brightener, surplus be water.
Wherein, the zinc owner salt compound is zinc nitrate, zinc acetate, zinc chloride, zinc lactate, at least one in zinc sulfate
Kind.
Wherein, the complexing agent be EDTA, sodium gluconate, sodium potassium tartrate tetrahydrate, sodium citrate, at least one in sodium oxalate
Kind.
Wherein, the sealing of hole promotor be potassium fluoride, ammonium acid fluoride, sodium thiosulfate, sodium metasilicate, in sodium phosphate at least
It is a kind of.
Wherein, the stabilizer is at least one of polyethylene glycol, glycerol, ethylene glycol, Tween 80, isoamyl alcohol.
Wherein, the grey brightener of the suppression is dimethyl silicone polymer, polyvinylpyrrolidone, saccharin sodium, thiocarbamide, hydroxyl second
Pitch at least one of diphosphonic acid, benzotriazole.
The aluminium alloy anode oxide film provided according to the present invention has the advantages that without nickel hole sealing agent
Compared to nickeliferous hole sealing agent, Zn (OH)2-Ksp be 7.1 × 10-18, than Ni (OH)2-Ksp 2.0 × 10-15It is low,
The numerical value is also below the solubility product of the alkali metal hydroxides such as calcium, magnesium, manganese, cobalt, i.e. main salt under the conditions of lower pH
Deposited in micropore, and the sealing of holes promotor such as sodium thiosulfate change porous membrane interface electrical property promote main salt metal ion into
Enter in fenestra, while improving pH in micropore, further decreases the work pH lower limit of pore-sealing liquid.Simultaneously in the help of stabilizer
Under, pore-sealing liquid is also able to maintain stabilization at higher pH and does not generate precipitating.In addition, Zn (OH)2-Lower Ksp value can make its compared with
It can be relatively easy within the scope of low concentration and wide in range temperature and be deposited in micropore.
Actual test the result shows that, hole sealing agent operating temperature provided by the invention is low, pH range is wide, concentration 2~6%,
PH 3~6, there is good sealing of hole effect at 15~35 DEG C of temperature, and the hole sealing agent environmental protection is avoided without nickel to human body and ring
The harm in border, operating temperature is low, energy saving, process stabilizing, only needs regular replenishment hole sealing agent that can keep the sealing of hole of sealing of hole slot
Performance.
All types of aluminium and its alloy press national standard (the phosphorus chromium of GB/T8753.2-2005 nitric acid preimpregnation after sealing pores
Acid system) weightlessness respectively less than 30mg/dm2, by national standard (GB/T8753.4-2005 acid treated dye speck method) crystal violet
Dyeing grade is 0, and anti-dye adsorption capacity is strong, and especially glossy surface workpiece brightness and resistance and fingerprint resistance antifouling capacity significantly mentions
It rises, aluminium and aluminum alloy surface performance can be significantly improved.The resistance to neutral salt spray time 72h or more of the hole sealing agent, stability are high.
Electron-microscope scanning is carried out to oxidation film surface, it is found that the micropore on the surface of oxidation film is nearly all closed, smooth surface,
Sealing of hole is more uniform.
In addition, the suppression ash brightener in hole sealing agent reduces surface tension on the one hand by means of surface-active action to have
It is entered in micropore conducive to the substance for participating in sealing of hole, on the other hand there is peptizaiton in metal surface, to effectively inhibit master
Salt is deposited in aluminium material surface, avoids the occurrence of sealing of hole phenomenon, and the significant increase flatness and brightness of aluminium material surface resists
Adsorption capacity enhancing.And zinc also greatly improves workpiece corrosion resistance the electrochemical protection of matrix.
Preparation method the present invention also provides above-mentioned aluminium alloy anode oxide film without nickel hole sealing agent, comprising:
Above-mentioned each raw material is sequentially added under stirring in order in water, under adding after a kind of raw material whole dissolved clarification
A kind of raw material, whole raw materials are stirred after adding, until solution clear.
Specific embodiment
To facilitate the understanding of the present invention, below with reference to each embodiment to invention is more fully described, still, this
Invention can be realized in many different forms, however it is not limited to embodiment described herein.On the contrary, providing these implementations
Example purpose be make it is more thorough and comprehensive to the disclosure.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term " and or " used herein includes one or more phases
Any and all combinations of the listed item of pass.
Embodiments of the present invention propose a kind of stabilization, operating temperature is low, pH range is wide and can significantly improve aluminium and aluminium closes
The aluminium alloy anode oxide film of gold surface performance is without nickel hole sealing agent.
The aluminium alloy anode oxide film is made of following raw material without nickel hole sealing agent: zinc owner salt compound, complexing agent, envelope
Hole promotor, stabilizer press down grey brightener, water.
Specifically, by mass percentage, the aluminium alloy anode oxide film is made of following raw material without nickel hole sealing agent:
3.0~6.0% zinc owner salt compound, 2.0~4.0% complexing agent, 2.0~4.0% sealing of hole promotor, 4.0~
10.0% stabilizer, 5.0~15.0% suppression ash brightener, surplus are water.
Wherein, the zinc owner salt compound is zinc nitrate, zinc acetate, zinc chloride, zinc lactate, at least one in zinc sulfate
Kind.
Wherein, the complexing agent be EDTA, sodium gluconate, sodium potassium tartrate tetrahydrate, sodium citrate, at least one in sodium oxalate
Kind.
Wherein, the sealing of hole promotor be potassium fluoride, ammonium acid fluoride, sodium thiosulfate, sodium metasilicate, in sodium phosphate at least
It is a kind of.
Wherein, the stabilizer is at least one of polyethylene glycol, glycerol, ethylene glycol, Tween 80, isoamyl alcohol.
Wherein, the grey brightener of the suppression is dimethyl silicone polymer, polyvinylpyrrolidone, saccharin sodium, thiocarbamide, hydroxyl second
Pitch at least one of diphosphonic acid, benzotriazole.
Divide multiple embodiments that the embodiment of the present invention is further detailed below.The embodiment of the present invention be not limited to
Under specific embodiment.Within the scope of the unchanged main rights, implementation can appropriate be changed.
Embodiment 1:
A kind of aluminium alloy anode oxide film by mass percentage, is made of following raw material without nickel hole sealing agent: 3.0%
Zinc owner salt compound, 3.0% complexing agent, 3.0% sealing of hole promotor, 10.0% stabilizer, 12.5% suppression ashen light
Bright dose, 68.5% water.
Above-mentioned aluminium alloy anode oxide film without nickel hole sealing agent the preparation method comprises the following steps:
Weigh zinc nitrate: 30 parts, sodium gluconate: 30 parts, ammonium acid fluoride: 30 parts, polyethylene respectively by weight percentage
Pyrrolidones: 25 parts, polyethylene glycol: 100 parts, dimethyl silicone polymer: 100 parts, water: 685 parts, in whole parts under stirring
Above-mentioned raw materials are sequentially added in order in amount water, a kind of lower raw material are added after a kind of raw material whole dissolved clarification, whole raw materials add
It is stirred after complete, until solution clear.
Embodiment 2:
A kind of aluminium alloy anode oxide film by mass percentage, is made of following raw material without nickel hole sealing agent: 3.0%
Zinc owner salt compound, 4.0% complexing agent, 4.0% sealing of hole promotor, 9.0% stabilizer, 11.0% suppression ash it is bright
Agent, 69.0% water.
Above-mentioned aluminium alloy anode oxide film without nickel hole sealing agent the preparation method comprises the following steps:
Weigh zinc nitrate: 30 parts, EDTA:40 parts, potassium fluoride: 40 parts, polyvinylpyrrolidone respectively by weight percentage:
20 parts, polyethylene glycol: 90 parts, dimethyl silicone polymer: 90 parts, water: 690 parts, by suitable in whole deal water under stirring
Sequence sequentially adds above-mentioned raw materials, and a kind of lower raw material is added after a kind of raw material whole dissolved clarification, and whole raw materials are stirred after adding
It mixes, until solution clear.
Embodiment 3:
A kind of aluminium alloy anode oxide film by mass percentage, is made of following raw material without nickel hole sealing agent: 6.0%
Zinc owner salt compound, 3.0% complexing agent, 3.0% sealing of hole promotor, 4.0% stabilizer, 5.0% suppression ash it is bright
Agent, 79.0% water.
Above-mentioned aluminium alloy anode oxide film without nickel hole sealing agent the preparation method comprises the following steps:
Weigh zinc lactate: 60 parts, sodium oxalate: 30 parts, sodium thiosulfate: 30 parts, polyethylene pyrrole respectively by weight percentage
Pyrrolidone: 20 parts, Tween 80: 40 parts, dimethyl silicone polymer: 30 parts, water: 790 parts, under stirring in whole deal water
Above-mentioned raw materials are sequentially added in order, a kind of lower raw material is added after a kind of raw material whole dissolved clarification, and whole raw materials add laggard
Row stirring, until solution clear.
Embodiment 4:
A kind of aluminium alloy anode oxide film by mass percentage, is made of following raw material without nickel hole sealing agent: 4.0%
Zinc owner salt compound, 3.0% complexing agent, 3.0% sealing of hole promotor, 6.0% stabilizer, 15.0% suppression ash it is bright
Agent, 69.0% water.
Above-mentioned aluminium alloy anode oxide film without nickel hole sealing agent the preparation method comprises the following steps:
Weigh zinc lactate: 40 parts, EDTA:30 parts, ammonium acid fluoride: 30 parts, polyvinylpyrrolidine respectively by weight percentage
Ketone: 10 parts, polyethylene glycol: 60 parts, dimethyl silicone polymer: 140 parts, water: 690 parts, under stirring in whole deal water
Above-mentioned raw materials are sequentially added in order, a kind of lower raw material is added after a kind of raw material whole dissolved clarification, and whole raw materials add laggard
Row stirring, until solution clear.
Embodiment 5:
A kind of aluminium alloy anode oxide film by mass percentage, is made of following raw material without nickel hole sealing agent: 3.0%
Zinc owner salt compound, 3.0% complexing agent, 2.0% sealing of hole promotor, 10.0% stabilizer, 11.5% suppression ashen light
Bright dose, 70.5% water.
Above-mentioned aluminium alloy anode oxide film without nickel hole sealing agent the preparation method comprises the following steps:
Weigh zinc nitrate: 30 parts, sodium gluconate: 30 parts, ammonium acid fluoride: 20 parts, polyethylene respectively by weight percentage
Pyrrolidones: 25 parts, polyethylene glycol: 100 parts, dimethyl silicone polymer: 90 parts, water: 705 parts, in whole parts under stirring
Above-mentioned raw materials are sequentially added in order in amount water, a kind of lower raw material are added after a kind of raw material whole dissolved clarification, whole raw materials add
It is stirred after complete, until solution clear.
Embodiment 6:
A kind of aluminium alloy anode oxide film by mass percentage, is made of following raw material without nickel hole sealing agent: 4.0%
Zinc owner salt compound, 2.0% complexing agent, 2.0% sealing of hole promotor, 8.0% stabilizer, 10.0% suppression ash it is bright
Agent, 74.0% water.
Above-mentioned aluminium alloy anode oxide film without nickel hole sealing agent the preparation method comprises the following steps:
Weigh zinc chloride: 40 parts, EDTA:20 parts, potassium fluoride: 20 parts, polyvinylpyrrolidone respectively by weight percentage:
20 parts, glycerol: 80 parts, dimethyl silicone polymer: 80 parts, water: 740 parts, under stirring in whole deal water in order according to
Secondary addition above-mentioned raw materials add a kind of lower raw material after a kind of raw material whole dissolved clarification, and whole raw materials are stirred after adding, directly
To solution clear.
Embodiment 7:
A kind of aluminium alloy anode oxide film by mass percentage, is made of following raw material without nickel hole sealing agent: 3.0%
Zinc owner salt compound, 3.0% complexing agent, 2.0% sealing of hole promotor, 5.0% stabilizer, 10.5% suppression ash it is bright
Agent, 76.5% water.
Above-mentioned aluminium alloy anode oxide film without nickel hole sealing agent the preparation method comprises the following steps:
Weigh zinc lactate: 30 parts, sodium oxalate: 30 parts, sodium thiosulfate: 20 parts, polyethylene pyrrole respectively by weight percentage
Pyrrolidone: 5 parts, Tween 80: 50 parts, dimethyl silicone polymer: 100 parts, water: 765 parts, under stirring in whole deal water
Above-mentioned raw materials are sequentially added in order, a kind of lower raw material is added after a kind of raw material whole dissolved clarification, and whole raw materials add laggard
Row stirring, until solution clear.
Embodiment 8:
A kind of aluminium alloy anode oxide film by mass percentage, is made of following raw material without nickel hole sealing agent: 4.0%
Zinc owner salt compound, 3.5% complexing agent, 2.0% sealing of hole promotor, 6.0% stabilizer, 10.5% suppression ash it is bright
Agent, 74.0% water.
Above-mentioned aluminium alloy anode oxide film without nickel hole sealing agent the preparation method comprises the following steps:
Weigh zinc lactate: 40 parts, EDTA:35 parts, ammonium acid fluoride: 20 parts, polyvinylpyrrolidine respectively by weight percentage
Ketone: it 5 parts, polyethylene glycol: 60 parts, dimethyl silicone polymer: 100 parts, water: 740 parts, is pressed in whole deal water under stirring
Sequence sequentially adds above-mentioned raw materials, a kind of lower raw material is added after a kind of raw material whole dissolved clarification, whole raw materials carry out after adding
Stirring, until solution clear.
In order to verify the effect of hole sealing agent provided by the invention, aluminium alloy anode oxide film prepared by Example 1 is without nickel
Hole sealing agent is compared with commercially available by the hole sealing agent of main salt of magnesium acetate, is tested under the conditions of 9 kinds respectively two kinds of hole sealing agents
Sealing of hole effect, test result please refer to table 1, wherein (GB/T8753.2-2005 nitric acid is pre- by national standard for following Weight loss data
The phosphorus chromic acid method of leaching) aluminum workpiece of sealing of hole is detected, coloration result presses national standard (GB/T8753.4-2005
Acid treated dye speck method) it is detected.
1 sealing of hole Contrast on effect of table
By above data comparison it can be seen that hole sealing agent stability, operating temperature, pH range and sealing of hole effect of the invention
It is superior to commercially available hole sealing agent.
The aluminium alloy anode oxide film provided according to the present invention is without nickel hole sealing agent, compared to nickeliferous hole sealing agent, Zn (OH)2-'s
Ksp is 7.1 × 10-18, than Ni (OH)2-Ksp 2.0 × 10-15Low, the numerical value is also below the alkali metal hydrogen-oxygen such as calcium, magnesium, manganese, cobalt
The solubility product of compound, i.e., main salt can deposit in micropore under the conditions of lower pH, in addition the sealing of holes such as sodium thiosulfate promote
Changing porous membrane interface electrical property into agent promotes main salt metal ion to enter in fenestra, while improving pH in micropore, makes pore-sealing liquid
Work pH lower limit further decrease.Simultaneously with the help of stabilizer, pore-sealing liquid is also able to maintain at higher pH to be stablized not
Generate precipitating.In addition, Zn (OH)2-Lower Ksp value can make it that can compare within the scope of lower concentration and wide in range temperature
Readily deposited in micropore.
Actual test the result shows that, hole sealing agent operating temperature provided by the invention is low, pH range is wide, concentration 2~6%,
There are good sealing of hole effect in pH3~6 at 15~35 DEG C of temperature, and the hole sealing agent environmental protection is avoided without nickel to human body and environment
Harm, operating temperature is low, and energy saving, process stabilizing only needs regular replenishment hole sealing agent that can keep the bridging of sealing of hole slot
Energy.
All types of aluminium and its alloy press national standard (the phosphorus chromium of GB/T8753.2-2005 nitric acid preimpregnation after sealing pores
Acid system) weightlessness respectively less than 30mg/dm2, by national standard (GB/T8753.4-2005 acid treated dye speck method) crystal violet
Dyeing grade is 0, and anti-dye adsorption capacity is strong, and especially glossy surface workpiece brightness and resistance and fingerprint resistance antifouling capacity significantly mentions
It rises, aluminium and aluminum alloy surface performance can be significantly improved.The resistance to neutral salt spray time 72h or more of the hole sealing agent, stability are high.
Electron-microscope scanning is carried out to oxidation film surface, it is found that the micropore on the surface of oxidation film is nearly all closed, smooth surface,
Sealing of hole is more uniform.
In addition, the suppression ash brightener in hole sealing agent reduces surface tension on the one hand by means of surface-active action to have
It is entered in micropore conducive to the substance for participating in sealing of hole, on the other hand there is peptizaiton in metal surface, to effectively inhibit master
Salt is deposited in aluminium material surface, avoids the occurrence of sealing of hole phenomenon, and the significant increase flatness and brightness of aluminium material surface resists
Adsorption capacity enhancing.And zinc also greatly improves workpiece corrosion resistance the electrochemical protection of matrix.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (8)
1. a kind of aluminium alloy anode oxide film is without nickel hole sealing agent, which is characterized in that be made of following raw material: zinc owner's salt chemical combination
Object, sealing of hole promotor, stabilizer, presses down grey brightener, water at complexing agent.
2. aluminium alloy anode oxide film according to claim 1 is without nickel hole sealing agent, which is characterized in that by mass percentage
Meter, the aluminium alloy anode oxide film are made of following raw material without nickel hole sealing agent: 3.0~6.0% zinc owner salt compound,
2.0~4.0% complexing agent, 2.0~4.0% sealing of hole promotor, 4.0~10.0% stabilizer, 5.0~15.0% suppression
Grey brightener, surplus are water.
3. aluminium alloy anode oxide film according to claim 1 is without nickel hole sealing agent, which is characterized in that the zinc owner salinization
Conjunction object is at least one of zinc nitrate, zinc acetate, zinc chloride, zinc lactate, zinc sulfate.
4. aluminium alloy anode oxide film according to claim 1 is without nickel hole sealing agent, which is characterized in that the complexing agent is
At least one of EDTA, sodium gluconate, sodium potassium tartrate tetrahydrate, sodium citrate, sodium oxalate.
5. aluminium alloy anode oxide film according to claim 1 is without nickel hole sealing agent, which is characterized in that the sealing of hole promotor
For at least one of potassium fluoride, ammonium acid fluoride, sodium thiosulfate, sodium metasilicate, sodium phosphate.
6. aluminium alloy anode oxide film according to claim 1 is without nickel hole sealing agent, which is characterized in that the stabilizer is poly-
At least one of ethylene glycol, glycerol, ethylene glycol, Tween 80, isoamyl alcohol.
7. aluminium alloy anode oxide film according to claim 1 is without nickel hole sealing agent, which is characterized in that the grey brightener of the suppression
For in dimethyl silicone polymer, polyvinylpyrrolidone, saccharin sodium, thiocarbamide, 1-hydroxy ethylidene-1,1-diphosphonic acid, benzotriazole at least
It is a kind of.
8. preparation method of the described in any item aluminium alloy anode oxide films of claim 1 to 7 without nickel hole sealing agent, feature exist
In, comprising:
It sequentially adds above-mentioned each raw material under stirring in order in water, adds lower one kind after a kind of raw material whole dissolved clarification
Raw material, whole raw materials are stirred after adding, until solution clear.
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| CN201811625408.2A CN109440162A (en) | 2018-12-28 | 2018-12-28 | A kind of aluminium alloy anode oxide film is without nickel hole sealing agent and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110230083A (en) * | 2019-07-09 | 2019-09-13 | 江苏飞拓界面工程科技有限公司 | A kind of aluminium and aluminium alloy anode oxide hole sealing agent and its application |
| CN111485269A (en) * | 2020-04-10 | 2020-08-04 | 高瑞安 | Chemical treatment liquid for sealing hole of aluminum profile electrolytic oxide film and hole sealing method |
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| CN111485269A (en) * | 2020-04-10 | 2020-08-04 | 高瑞安 | Chemical treatment liquid for sealing hole of aluminum profile electrolytic oxide film and hole sealing method |
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