CN101323965A - Middle temperature sealant and closing process for aluminum anodized film - Google Patents
Middle temperature sealant and closing process for aluminum anodized film Download PDFInfo
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- CN101323965A CN101323965A CNA2008100484930A CN200810048493A CN101323965A CN 101323965 A CN101323965 A CN 101323965A CN A2008100484930 A CNA2008100484930 A CN A2008100484930A CN 200810048493 A CN200810048493 A CN 200810048493A CN 101323965 A CN101323965 A CN 101323965A
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Abstract
The invention discloses a mesophilic sealing agent and a sealing technique of aluminum anodic oxide films and belongs to the technical field of the post sealing processing of the anodic oxide films of aluminum and aluminum alloys. The sealing agent of the invention is an aqueous solution that consists of alkali metals or salts of alkali earth metals, a complexing agent and a pH buffering agent; wherein, the concentration of the alkali metals or the salts of alkali earth metals is 5 to 15 g/L, the concentration of the complexing agent is 10 to 20 g/L,, the concentration of the pH buffering agent is 0 to 10 g/L, and the residual quantity is water; the pH value of the aqueous solution of the sealing agent is maintained between 5 and 6, the aluminum anodic oxide film is sealing processed by the sealing agent, the temperature of the aqueous solution of the sealing agent is 75 to 90 DEG C, and the soaking and sealing time lasts for 20 to 30 minutes. The sealing agent adopts the alkali earth metals or the salts of alkali metals with wide resource and low cost so as to replace heavy metal nickel salts or cobalt salts in the prior art and adopts the organic complexing agent that has biodegradability, low price and simple molecules so as to replace surface activating agents that contain giant molecules and benzene rings in the prior art, and consequently the aluminum anodic oxide film that is sealing processed by the sealing agent obtains excellent anti-pruina property, and the anti-corrosion and anti-pollution properties of the anodic oxide film of aluminum and aluminum alloys are generally improved.
Description
Technical field
The present invention is used for the warm encapsulant and the closing process of aluminum anodized film, belongs to the sealing post-processing technology field of aluminium and aluminium alloy anode oxide film, and is irrelevant with the sealing technique of aluminium hard anodized film or non-electrolytics conversion film.
Technical background
Aluminium and aluminium alloy are one of metals the most frequently used in the current industry, and aluminium and aluminium alloy are not only in light weight, the quality heavily fortified point, and have good ductility, electroconductibility, thermal conductivity, thermotolerance and anti-nuclear radiation, be the important foundation starting material of the national economic development.
Aluminium and aluminium alloy are very stable in the exsiccant atmosphere, but in humid atmosphere, particularly are easy to corrosion in the air of salt concentration.Industrially adopt anodic oxidation widely, generate layer oxide film at aluminium and articles made of aluminium alloy surface, usually adopting sulfuric acid or oxalic acid is electrolytic solution, carry out anode electrolysis with aluminium and aluminium alloy as anode and handle, the formed conversion film of anodic oxidation is cellular porous structure, has high porosity and adsorptivity, this high porosity and adsorptivity both be convenient to technology dyeing, but be easy to contaminatedly, especially in corrosive atmosphere, corrosive medium enters the rete hole easily and causes corrosion.Therefore, in the industrial production,, before dyeing or after the dyeing, generally all need the antianode oxidation film layer to carry out sealing treatment in order to improve the quality of aluminum anodized film.
The aluminum anodized film enclosure method of normal employing is boiling water sealing and nickel acetate closing process.And the drawback of these two kinds of closing process commonly used be oxide film behind sealing treatment, its surface is easy to generate disgusting white or grey meal, industry is referred to as sealing " pollen " or " sealing China ".When " pollen " was slight, available rag was wiped gently, then was difficult to wipe when serious, need move back film and handle again, caused oxide film to be scrapped.Studies show that the plurality of impurity ions of sealing treatment liquid can promote the generation of " pollen ", wherein Ca
2+, Mg
2+, Al
3+Isoionic existence effect is the most obvious.This shows for traditional boiling water closing process and nickel acetate closing process, alkaline-earth metal ions Ca
2+, Mg
2+Be deleterious, so let alone prepare sealing treatment liquid with them.
Should carry out sealing treatment after the oxide film dyeing, to increase the light permanency and the solidity to corrosion of color and luster.Sealing technique the earliest is to adopt pure water to boil to boil, its principle is that hydration reaction takes place in hot water the aluminium sesquioxide of oxide film surface and hole wall, generates hydrated aluminum oxide, and the volume of original oxide film is increased, the expansion of oxide film volume is significantly dwindled fenestra, thereby reaches the purpose of sealing of hole.Be difficult to control in the boiling water sealing actual production, the evaporation of sealing tank liquor is very fast, and impurity run-up in the tank liquor causes sealing quality deterioration, needs the frequent pure water of changing.
Interpolation nickel acetate or Cobaltous diacetate carry out sealing of hole to oxide film in pure water, and hydrolysis takes place in hot water for these nickel salts or cobalt salt, produces precipitation of hydroxide in the oxide film hole, plays sealing process equally.Such closing process can carry out under low slightly temperature condition, as 71-88 ℃.The tank liquor life-span is longer than the boiling water sealing; the sealing better quality; this closing process is so far industrial still very popular; nickel acetate or Cobaltous diacetate closing process have an environmental issue; just contain a large amount of heavy metal nickels and cobalt in the waste water of sealing treatment; heavy metal ion can cause serious harm to environment, in order to protect environmental safety, needs to use complicated and expensive wastewater treatment equipment.
Basic metal and alkaline-earth metal extensively are present in natural soil and the seawater, and be very little to the toxicity of biology, and the processing of its trade effluent is fairly simple and cheap.Proposed not contain the composition of heavy metal nickel (Ni) and cobalt (Co) encapsulant in the U.S. Pat 5362317, used alkaline earth salt: calcium acetate (Ca (OAc)
2), or magnesium acetate (Mg (OAc)
2), with anion surfactant: alkylbenzene ether sulfonate, pH value are 4.5-7.5.Temperature range at 71-82 ℃ is sealed, time 15min.The sealing quality is good, the no pollen in surface.
Proposed in the U.S. Pat 5411607 with the prescription of an alkali metal salt as encapsulant: Lithium Acetate (LiOAc), every liter contains (Li
+) ion 0.5g, anion surfactant: every liter contains alkylbenzene ether sulfonate 1g, and the pH value is 5.5-6.5, at 88 ℃ temperature range sealing, time 10min.The sealing quality is good, the no pollen in surface.
More than two patents all adopted macromole and contained the tensio-active agent of phenyl ring, this class organic compound is slow at natural degradation speed, life-time service is accumulated in environment easily, and ecology is damaged.
Summary of the invention
The purpose of this invention is to provide a kind of warm encapsulant and closing process that is used for aluminum anodized film; replace heavy metal nickel salt or the cobalt salt that costs an arm and a leg and environment is had pollution with wide an alkali metal salt with low cost of resource or alkaline earth salt; to be easy to the organism complexing agent of the low simple molecules of biological degradation price; replace the tensio-active agent that macromole contains phenyl ring; make aluminium and the aluminium alloy anode oxide film handled through this encapsulant; not only has good anti-pollen characteristic; improve the solidity to corrosion and the resistance to crocking of aluminium and aluminium alloy anode oxide film comprehensively; and help reducing cost, help ecology and environment protection.
The aqueous solution that encapsulant of the present invention is made up of salt, complexing agent, the pH buffer reagent of basic metal or alkaline-earth metal, wherein
The salt 5-15g/L of basic metal or alkaline-earth metal.
Complexing agent 10-20g/L
PH buffer reagent 0-10g/L
Excess water
PH value 5-6
An alkali metal salt that the present invention adopts or alkaline earth salt are alkali metal lithium or alkaline-earth metal magnesium, the acetate of calcium, formate, lactic acid salt, and wherein acetate, formate best results are considered cost factor, generally use their acetate.Under the condition of the acetate that is difficult for obtaining them, also can prepare with their oxyhydroxide or carbonate and corresponding acid-respons temporarily.Because the sealing of sulfate radical, nitrate radical, chlorion antianode oxide film is deleterious, do not adopt vitriol, nitrate, muriate so do not advocate;
The complexing agent that the present invention adopts is nitrogenous organic acid or organic bases, the organism that belongs to simple molecules, be easy to biological degradation, can not damage ecology, as trolamine, nitrilotriacetic acid(NTA), ethylenediamine tetraacetic acid (EDTA), acetic acid hydrazine, sulfamate, wherein trolamine, nitrilotriacetic acid(NTA) effect are best;
PH buffer reagent of the present invention is selected sodium-acetate and ammonium acetate for use, adds the rangeability that the pH buffer reagent can reduce encapsulant pH value of solution value, keeps the stable of encapsulant solution, makes the longer service life of encapsulant solution.According to the acid-basicity of institute's obtain solution, can adopt acetic acid or ammoniacal liquor, sodium hydroxide solution, adjust the regulation numerical value of pH value to 5-6.
Closing process by encapsulant of the present invention is:
75-90 ℃ of aqueous sealant solution temperature
Dipping 20-30min off-period
Adopt encapsulant sealing treatment aluminium of the present invention and aluminium alloy through the technology of anode oxide film to be: aluminium and aluminium alloy are after the anodic oxidation treatment film forming, through thoroughly washing, immerse immediately and carry out sealing treatment in the confining liquid of the present invention, the centre can not stop, the encapsulant solution temperature is 75-90 ℃, the dipping close process time depends on the thickness of oxide film, encapsulant antianode oxide film speed in a closed circuit of the present invention is about 0.5 μ m/min, so, be the oxide film of 10-15 μ m for thickness, its sealing dip treating time is 20-30min, after dip treating is finished, with the washing from the beginning of flowing, again through dry air, promptly obtain the oxide film of satisfied sealing effect, the no pollen in surface.
The present invention realizes that successfully substituting the hole sealing agent that nickel acetate, Cobaltous diacetate be used for aluminium and aluminium alloy anode oxide film with basic metal or alkaline earth salt carries out sealing treatment, and its key is that science selects complexing agent, on the one hand this complex compound should with Li
+, Ca
2+, Mg
2+Ion has enough complexation strengths, makes free Li
+, Ca
2+, Mg
2+The ionic concn appropriateness is low, is not enough in electrolytic solution or the generation precipitation of hydroxide of anode oxide film surface, thereby avoids basic metal Li
+Ion, alkaline-earth metal ions Ca
2+, Mg
2+Form the problem of " pollen " on the oxide film surface.This complex compound and Al on the other hand
3+The ionic complexation constant should greater than with Ca
2+, Mg
2+The ion complexation constant is reflected in the oxide film hole sealing of hole and is carried out.
It is as follows that capping takes place in the oxide film hole:
MY+Al(OH)
3＝AlY
++M
2++3OH
-
M
2++2OH
-＝M(OH)
2↓
M representation metal ion Ca in the top formula
2+, Mg
2+Ion or Li
+Ion is because free Li in the sealing treatment agent
+, Ca
2+, Mg
2+The ionic concn appropriateness is low, and its concentration is not enough in electrolytic solution or anode oxide film surface produces precipitation of hydroxide, and the Li of appropriate concentration in the oxide film hole only
+, Ca
2+, Mg
2+Ion is generated Ca, Mg or Li precipitation of hydroxide, and makes hole obtain filling, has reached the purpose of sealing.
The complexing agent that the present invention selects is nitrogenous organic acid or organic bases, is selected from trolamine, nitrilotriacetic acid(NTA), ethylenediamine tetraacetic acid (EDTA), and acetic acid hydrazine, sulfamate be as complex compound, and wherein trolamine, nitrilotriacetic acid(NTA) effect are best.Trolamine be alkalescence to its pH value be neutralized to 5-6 with acetic acid, the acetic acid hydrazine also is with in the acetic acid and the hydrazine hydrate acquisition.
Metal-salt can be selected their acetate, formate, lactic acid salt for use, and wherein acetate, formate best results are considered cost factor, generally use their acetate.Because the sealing of sulfate radical, nitrate radical, chlorion antianode oxide film is harmful, does not recommend to use vitriol, nitrate, muriate.Can't directly obtain under the condition of acetate, can prepare with corresponding acid-respons temporarily with their oxyhydroxide or carbonate.
The present invention selects for use sodium-acetate and ammonium acetate as the pH buffer reagent, can reduce the pH value rangeability of encapsulant solution, keeps the stable of encapsulant solution, prolongs the work-ing life of encapsulant solution.Under certain conditions, when after anodic oxidation, cleaning very thoroughly, also can not add buffer reagent as workpiece.
The present invention adopts CNS GB/T14952.1 evaluation sealing quality, and the anode oxide film after just will sealing is in the solution of following prescription and temperature:
CrO
3 20g/L
H
3PO
4(85％) 35mL/L
38 ℃ of temperature
Dipping 15min detects its corrosion weight loss, and is weightless less than 30mg/dm
2For the sealing qualified.
The present invention adopts an alkali metal salt or alkaline earth salt to replace heavy metal nickel salt or the cobalt salt that prior art is used, sealing treatment aluminium and aluminium alloy anode oxide film, obtained the anode oxide film of anti-pollen characteristic, improve the solidity to corrosion and the resistance to crocking of aluminium and aluminium alloy anode oxide film comprehensively, not only basic metal or alkaline-earth metal resource are wide with low cost, and avoided to handling the expensive treatment device that the contaminated wastewater institute that contains heavy metal nickel and cobalt must employing, in addition, the complexing agent that the present invention adopts is the organism of simple molecules, be easy to biological degradation, ecotope is had no adverse effects.These complexing agents all are industrial chemicals commonly used, are widely used in clean-out system industry as trolamine, and material obtains easily, and cost is low.
Embodiment
Now how to implement in conjunction with specific examples explanation the present invention:
One, aluminium and aluminium alloy anode oxide film forming are handled
Sample adopts 6063 aluminium alloys, and technical process is as follows:
1. acid degreasing: AC-98 acid degreasing agent 15g/L, sulfuric acid 150g/L, room temperature dipping 5min.
2. secondary flow is washed from the beginning.
3. caustic corrosion: ALC-2001 caustic corrosion agent 20g/L, sodium hydroxide 50g/L, 65 ℃ of dipping 5min.
4. secondary flow is washed from the beginning.
5. bright dipping: nitric acid 250g/L, room temperature dipping 3min.
6. secondary flow is washed from the beginning.
7. anodic oxidation: sulfuric acid 186g/L, Al
3+≤ 25g/L, 20 ℃, current density 1.2A/dm
2, electrolysis time 35min, thickness of oxidation film 15 μ m.
8. secondary flow is washed from the beginning.
Two, adopt encapsulant of the present invention and treatment process that above-mentioned anode oxide film is carried out sealing treatment.
Example 1
1, after 1.-8. aluminium and aluminum alloy specimen carry out the anode oxidation film-forming processing by above-mentioned steps, immediately oxide film is carried out following sealing treatment.
1, oxide film sealing treatment:
(1), encapsulant forms: four water acetic acid magnesium 6.7g/L, trolamine 10mL/L, ammonium acetate 0.5g/L transfers to 5.6 with acetic acid with the pH value.
(2), closing process: 80 ℃, flood 30min.
(3), secondary flow is washed from the beginning.
(4), dry in air at room temperature.
(5), check
Specimen surface is clean, does not have " pollen " the weightless 25.7mg/dm of phosphoric acid-chromic acid corrosion
2, it is qualified to seal.
Example 2
1, after 1.-8. aluminium and aluminum alloy specimen carry out the anode oxidation film-forming processing by above-mentioned steps, immediately oxide film is carried out following sealing treatment.
2, oxide film sealing treatment:
(1), encapsulant forms: four water acetic acid magnesium 6.7g/L, hydrazine hydrate (85%), ammonium acetate 1g/L transfers to 5.85 with acetic acid with the pH value.
(2), closing process: 80 ℃, flood 30min.
(3), secondary flow is washed from the beginning.
(4), dry in air at room temperature.
(5), check
Specimen surface does not totally have " pollen ", the weightless 24.1mg/dm of phosphoric acid-chromic acid corrosion
2, it is qualified to seal.
Example 3
1, after 1.-8. aluminium and aluminum alloy specimen carry out the anode oxidation film-forming processing by above-mentioned steps, immediately oxide film is carried out following sealing treatment.
2, oxide film sealing treatment:
(1), encapsulant forms: lithium hydroxide 10g/L, trolamine 10mL/L, sodium-acetate 0.5g/L transfers to 6.6 with acetic acid with the pH value.
(2), closing process: 85 ℃, flood 30min.
(3), secondary flow is washed from the beginning.
(4), dry in air at room temperature.
(5), check
Specimen surface is clean, does not have " pollen " the weightless 22.4mg/dm of phosphoric acid-chromic acid corrosion
2, it is qualified to seal.
Example 4
1, after 1.-8. aluminium and aluminum alloy specimen carry out the anode oxidation film-forming processing by above-mentioned steps, by following oxide film is carried out sealing treatment immediately.
2, oxide film sealing treatment:
(1), encapsulant forms: lithium hydroxide 10g/L, nitrilotriacetic acid(NTA) 10g/L, sodium-acetate 1g/L adds acetic acid and solids is dissolved fully and the pH value is transferred to 6.6.
(2), closing process: 85 ℃, flood 30min.
(3), secondary flow is washed from the beginning.
(4), dry in air at room temperature.
(5), check
Specimen surface is clean, does not have " pollen " the weightless 21.8mg/dm of phosphoric acid-chromic acid corrosion
2, it is qualified to seal.
Example 5
1, after 1.-8. aluminium and aluminum alloy specimen carry out the anode oxidation film-forming processing by above-mentioned steps, immediately oxide film is carried out following sealing treatment.
2, oxide film sealing treatment:
(1), encapsulant forms: lime carbonate 5.5g/L, nitrilotriacetic acid(NTA) 10g/L, sodium-acetate 0.5g/L adds acetic acid and solids is dissolved fully and the pH value is transferred to 6.8.
(2), closing process: 85 ℃, flood 30min.
(3), secondary flow is washed from the beginning.
(4), dry in air at room temperature.
(5), check
Specimen surface is clean, does not have " pollen " the weightless 26.4mg/dm of phosphoric acid-chromic acid corrosion
2, it is qualified to seal.
Example 6
1, after 1.-8. aluminium and aluminum alloy specimen carry out the anode oxidation film-forming processing by above-mentioned steps, immediately oxide film is carried out following sealing treatment.
2, oxide film sealing treatment:
(1), encapsulant forms: lime carbonate 10g/L, solids is dissolved fully and the pH value is transferred to 6.6 with thionamic acid.
(2), closing process: 85 ℃, flood 30min.
(3), secondary flow is washed from the beginning.
(4), dry in air at room temperature.
(5), check
Specimen surface does not totally have " pollen ", the weightless 25.9mg/dm of phosphoric acid-chromic acid corrosion
2, it is qualified to seal.
Remarks: AC-98 and ALC-2001 handle series additive for Wuhan Inst. of Material Protection's aluminum alloy surface.
Claims (7)
1, the warm encapsulant that is used for aluminum anodized film, the aqueous solution by salt, complexing agent, the pH buffer reagent of basic metal or alkaline-earth metal are formed is characterized in that
The salt 5-15g/L of basic metal or alkaline-earth metal.
Complexing agent 10-20g/L
PH buffer reagent 0-10g/L
Excess water
PH value 5-6
2, the warm encapsulant that is used for aluminum anodized film according to claim 1 is characterized in that an alkali metal salt is a lithium salts, and alkaline earth salt is magnesium salts or calcium salt.
3, the warm encapsulant that is used for aluminum anodized film according to claim 2 is characterized in that basic metal lithium salts, alkaline-earth metal magnesium salts or calcium salt are acetate, formate or the lactic acid salts that is selected from them.
4, the warm encapsulant that is used for aluminum anodized film according to claim 1 is characterized in that the complexing agent that adopts is nitrogenous organic acid or organic bases.
5, the warm encapsulant that is used for aluminum anodized film according to claim 4 is characterized in that nitrogenous organic acid or organic bases complexing agent are trolamine, nitrilotriacetic acid(NTA), ethylenediamine tetraacetic acid (EDTA), acetic acid hydrazine or sulfamate.
6, the warm encapsulant that is used for aluminum anodized film according to claim 1 is characterized in that the pH buffer reagent is selected from sodium-acetate or ammonium acetate.
7, the closing process that is used for the warm encapsulant of aluminum anodized film according to claim 1 is characterized in that the aqueous sealant solution temperature is 75-90 ℃, and dipping off-period is 20-30min.
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|---|---|---|---|
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| CN1003657B (en) * | 1987-03-29 | 1989-03-22 | 广东有色金属加工厂 | Method of pore sealing of anodic oxidation membrane on the aluminium and aluminium alloy anode |
| GB9422952D0 (en) * | 1994-11-14 | 1995-01-04 | Secr Defence | Corrosion inhibitor |
| CN101205617A (en) * | 2006-12-20 | 2008-06-25 | 深圳富泰宏精密工业有限公司 | Surface treating method for metal workpieces |
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