CN102433578B - Agent for treatment before aluminum alloy secondary anode oxidation screen printing and aluminum alloy secondary anode oxidation technology - Google Patents
Agent for treatment before aluminum alloy secondary anode oxidation screen printing and aluminum alloy secondary anode oxidation technology Download PDFInfo
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- CN102433578B CN102433578B CN201110383966.4A CN201110383966A CN102433578B CN 102433578 B CN102433578 B CN 102433578B CN 201110383966 A CN201110383966 A CN 201110383966A CN 102433578 B CN102433578 B CN 102433578B
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Abstract
The invention discloses an agent for treatment before aluminum alloy secondary anode oxidation screen printing, which is characterized in that each kilo of treatment agent solution contains the following raw materials by weight: 0.02-0.08g of cobalt salt, 0.01-0.08g of titanium salt, 0.01-0.20g of accelerating agent, 0.01-0.20g of silane and remaining weight of water. The invention additionally discloses an aluminum alloy secondary anode oxidation technology, which comprises the steps of cleaning, primary alkali etching, primary neutralization, primary anode oxidation, primary organic salt closing, treatment by using the treatment agent and screen printing of anticorrosive ink; and secondary alkali etching, second neutralization, secondary anode oxidation and the like. The treatment agent disclosed by the invention can form a reactive conversion layer on an aluminum material, the conversion layer can effectively resist the penetration of water and oxides and provide excellent anticorrosive performance, the adhesiveness of a coating layer to ink, coating and the like can be improved, and the situation that the ink falls off or corrosion pits are generated in the subsequent treatment process is avoided.
Description
Technical field
The present invention relates to a kind ofly for the treatment agent before aluminium alloy two-step anodization silk-screen, the invention still further relates to the aluminium alloy secondary oxidation technique that this treatment agent of a kind of use is processed aluminium alloy.
Background technology
Along with widespread use and the development of aluminium alloy anode oxide technique, Al-alloy products is the decorative effect that increases its outward appearance, conventionally decoratively anodizing and silk-screen printing technique combination are carried out to comprehensive treating process to aluminum alloy surface, particularly repeatedly dye to process through two-step anodization and can form machicolated form pattern, is rich in stereoscopic sensation, decorative effect is fine, or application UV coating etc. again after anodic oxidation sealing.In the process of enforcement prior art scheme, applicant finds above-mentioned prior art, and there are the following problems: for ensureing the tack of ink or coating, after an anodic oxidation of aluminium alloy now, all adopt semiclosed mode, although the off-period of this mode is short, be generally 2-5min, can improve production rate, but the tack that the shortcoming of this treatment process is coating can not ensure in large production, and because sealing is incomplete, the over-all properties of product is also greatly affected.For this reason, be necessary the processing after an anodic oxidation to improve, improve overall performance.
Summary of the invention
An object of the present invention is to provide a kind of for the treatment agent before aluminium alloy two-step anodization silk-screen, to improve the silk-screen surface property after anodic oxidation one time.
Another object of the present invention is the aluminium alloy secondary oxidation technique that after will providing this treatment agent of a kind of use to an anodic oxidation, aluminium alloy is processed.
The technical solution adopted for the present invention to solve the technical problems is:
For the treatment agent before aluminium alloy two-step anodization silk-screen, it is characterized in that: the raw material that includes following weight in every kilogram for the treatment of agent solution: cobalt salt 0.02-0.08g, titanium salt 0.01-0.08g, promotor 0.01-0.20g, silane 0.01-0.20g, surplus are water.
Described cobalt salt can be rose vitriol, Cobaltous diacetate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES or cobaltous carbonate.
Described titanium salt can be fluotitanate, titanium tetrachloride, titanic acid ester, titanium sulfate or Titanium Nitrate.
Described promotor can be hydrofluoric acid, ammonium bifluoride, Neutral ammonium fluoride, Sodium Fluoride or silicofluoric acid.
Described silane can be epoxy radicals silicone hydride, amino silane compounds, fluoroalkyl silanes, vinyl silanes, alkyl silane or aromatic base silane.
Wherein, epoxy radicals silicone hydride can adopt 3-glycidyl ether oxygen propyl trimethoxy silicane or Polyetherfunctional group triethoxyl silane; Amino silane compounds can adopt N-aminoethyl-3-aminopropyl trimethoxysilane or 2-aminoethyl-3-aminopropyl methyl dimethoxysilane; Fluoroalkyl silanes can adopt ten trifluoro octyltri-ethoxysilane, fluoro alkyl-silane or modification fluoroalkyl siloxanes; Vinyl silanes is vinyl trichloro silane or vinyltriethoxysilane; Alkyl silane can adopt hexadecyl Trimethoxy silane, isobutyl triethoxy silane or octyltri-ethoxysilane; Aromatic base silane can adopt phenyltrimethoxysila,e etc.
A kind of aluminium alloy two-step anodization technique provided by the invention, is characterized in that: it comprises the steps: (1) cleaning, to remove the greasy dirt of aluminium material surface; (2) alkaline etching for the first time, to remove the natural oxide film of aluminium material surface, described alkaline etching tank liquor adopts the solution 40-60g/l of sodium hydroxide, inhibiter and complexing agent, at 40-60 DEG C, corrodes 30-120s; (3) neutralization for the first time, for removing aluminium material surface ash shape thing, spot and oxide film, puts into 10-30%HNO by aluminium
3solution, in 10-35 DEG C and 10-120s; (4) anodic oxidation for the first time, the cell liquid of employing is 150-250g/l sulphuric acid soln, temperature 18-22 DEG C, current density 1.0-2.5A/dm
2, oxidation 15-40min; (5) inorganic salt sealing is for the first time flooded 10-30min, pH value 5.3-5.8, temperature 75-85 DEG C in 5-10g/l nickelous acetate encapsulant solution; (6) treatment agent processing, at 10-35 DEG C, under pH value 2.5-3.3 condition, in treatment agent, flood 10-120s, wherein, in every kilogram for the treatment of agent solution, include the raw material of following weight: cobalt salt 0.02-0.08g, titanium salt 0.01-0.08g, promotor 0.01-0.20g, silane 0.01-0.20g, surplus are water; (7) the corrosion-resistant ink of silk-screen; (8) alkaline etching for the second time, to remove aluminium material surface oxide film, described alkaline etching tank liquor adopts the solution 40-60g/l of sodium hydroxide, inhibiter and complexing agent, at 40-60 DEG C, corrodes 30-120s; (9) neutralization for the second time, for removing aluminium material surface ash shape thing, spot and oxide film, puts into 10-30%HNO by aluminium
3solution, in 10-35 DEG C and 10-120s; (10) anodic oxidation for the second time, the cell liquid of employing is 150-250g/l sulphuric acid soln, temperature 18-22 DEG C, current density 1.0-2.5A/dm
2, oxidation 15-40min; (11) inorganic salt sealing for the second time, the Porosity anodic oxide film that anodic oxidation is generated seals with nickelous acetate, floods 10-30min, pH value 5.3-5.8 in 5-10g/l nickelous acetate encapsulant solution, temperature 75-85 DEG C, obtains the aluminium alloy through two-step anodization processing.
Above-mentioned alkaline etching tank liquor and electrolytic solution can adopt the proportioning in traditional technology.
In order to obtain best surface treatment effect, between each processing step, water cleans up.After the anodic oxidation of secondary, also can add painted processing.
The invention has the beneficial effects as follows: treatment agent of the present invention, can on aluminium, form reactive conversion coating, this conversion coating can effectively be resisted soaking into of water and oxide compound, excellent solidity to corrosion is provided, also can improve the tack of coating to ink, coating etc., prevent coming off or producing corrosion pit phenomenon through ink in subsequent processes simultaneously.
Brief description of the drawings
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the present invention's application production technological process.
Embodiment
Embodiment 1
The preparation for the treatment of agent: take following raw material:
Cobaltous diacetate 0.020g
Titanium tetrachloride 0.080g
Ammonium bifluoride 0.150g
Ten trifluoro octyltri-ethoxysilane 0.015g
Water 999.6g
Mentioned component is added to the water respectively in order, stir until all dissolving obtain the treatment agent of 1 ㎏ before for aluminium alloy two-step anodization silk-screen.
Embodiment 2
The preparation for the treatment of agent: take following raw material:
Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES 0.03g
Titanium sulfate 0.060g
Neutral ammonium fluoride 0.100g
Hexadecyl Trimethoxy silane 0.050g
Water 999.76g
Mentioned component is added to the water respectively in order, stir until all dissolving obtain the treatment agent of 1 ㎏ before for aluminium alloy two-step anodization silk-screen.
Embodiment 3
Cobaltous diacetate 0.06g
Titanic acid ester 0.03g
Ammonium bifluoride 0.15g
3-glycidyl ether oxygen propyl trimethoxy silicane 0.15g
Water 999.61g
Mentioned component is added to the water respectively in order, stir until all dissolving obtain the treatment agent of 1 ㎏ before for aluminium alloy two-step anodization silk-screen.
Embodiment 4
Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES 0.07g
Titanium Nitrate 0.04g
Sodium Fluoride 0.15g
Vinyl trichloro silane 0.20g
Water 999.54g
Mentioned component is added to the water respectively in order, stir until all dissolving obtain the treatment agent of 1 ㎏ before for aluminium alloy two-step anodization silk-screen.
Embodiment 5
(1) clean, to remove the greasy dirt of aluminium material surface, scavenging solution can adopt the conventional material in this area; (2) alkaline etching for the first time, to remove the natural oxide film of aluminium material surface, described alkaline etching tank liquor adopts the solution 40-60g/l of sodium hydroxide, inhibiter and complexing agent, at 40-60 DEG C, corrodes 30-120s; (3) neutralization for the first time, for removing aluminium material surface ash shape thing, spot and oxide film, puts into 10-30%HNO by aluminium
3solution, in 10-35 DEG C and 10-120s; (4) anodic oxidation for the first time, the cell liquid of employing is 150-250g/l sulphuric acid soln, temperature 18-22 DEG C, current density 1.0-2.5A/dm
2, oxidation 15-40min; (5) inorganic salt sealing is for the first time flooded 10-30min, pH value 5.3-5.8, temperature 75-85 DEG C in 5-10g/l nickelous acetate encapsulant solution; (6) treatment agent processing at 10-35 DEG C, is flooded 10-120s under pH value 2.5-3.3 condition in the treatment agent of preparing at embodiment 1; (7) the corrosion-resistant ink of silk-screen; (8) alkaline etching for the second time, to remove aluminium material surface oxide film, described alkaline etching tank liquor adopts the solution 40-60g/l of sodium hydroxide, inhibiter and complexing agent, at 40-60 DEG C, corrodes 30-120s; (9) neutralization for the second time, for removing aluminium material surface ash shape thing, spot and oxide film, puts into 10-30%HNO by aluminium
3solution, in 10-35 DEG C and 10-120s; (10) anodic oxidation for the second time, the cell liquid of employing is 150-250g/l sulphuric acid soln, temperature 18-22 DEG C, current density 1.0-2.5A/dm
2, oxidation 15-40min; (11) inorganic salt sealing for the second time, the Porosity anodic oxide film that anodic oxidation is generated seals with nickelous acetate, floods 10-30min, pH value 5.3-5.8 in 5-10g/l nickelous acetate encapsulant solution, temperature 75-85 DEG C, obtains the aluminium alloy through two-step anodization processing.
Embodiment 6
(1) clean, to remove the greasy dirt of aluminium material surface, scavenging solution can adopt the conventional material in this area; (2) alkaline etching for the first time, to remove the natural oxide film of aluminium material surface, described alkaline etching tank liquor adopts the solution 40-60g/l of sodium hydroxide, inhibiter and complexing agent, at 40-60 DEG C, corrodes 30-120s; (3) neutralization for the first time, for removing aluminium material surface ash shape thing, spot and oxide film, puts into 10-30%HNO by aluminium
3solution, in 10-35 DEG C and 10-120s; (4) anodic oxidation for the first time, the cell liquid of employing is 150-250g/l sulphuric acid soln, temperature 18-22 DEG C, current density 1.0-2.5A/dm
2, oxidation 15-40min; (5) inorganic salt sealing is for the first time flooded 10-30min, pH value 5.3-5.8, temperature 75-85 DEG C in 5-10g/l nickelous acetate encapsulant solution; (6) treatment agent processing at 10-35 DEG C, is flooded 10-120s under pH value 2.5-3.3 condition in the treatment agent of preparing at embodiment 3; (7) the corrosion-resistant ink of silk-screen; (8) alkaline etching for the second time, to remove aluminium material surface oxide film, described alkaline etching tank liquor adopts the solution 40-60g/l of sodium hydroxide, inhibiter and complexing agent, at 40-60 DEG C, corrodes 30-120s; (9) neutralization for the second time, for removing aluminium material surface ash shape thing, spot and oxide film, puts into 10-30%HNO by aluminium
3solution, in 10-35 DEG C and 10-120s; (10) anodic oxidation for the second time, the cell liquid of employing is 150-250g/l sulphuric acid soln, temperature 18-22 DEG C, current density 1.0-2.5A/dm
2, oxidation 15-40min; (11) inorganic salt sealing for the second time, the Porosity anodic oxide film that anodic oxidation is generated seals with nickelous acetate, floods 10-30min, pH value 5.3-5.8 in 5-10g/l nickelous acetate encapsulant solution, temperature 75-85 DEG C, obtains the aluminium alloy through two-step anodization processing.
Embodiment 7
(1) clean, taking sulfuric acid or nitric acid as base, add a small amount of wetting agent and emulsifying agent,
Temperature is controlled at 45-55 DEG C; (2) alkaline etching for the first time, the composition of alkali cleaning agent: sodium hydroxide 40-55g/l, alkali cleaning additive 10-15g/l; At 40-55 DEG C, process 30-60s; (3) chemical rightenning, the composition nitric acid 30-80g/l of polishing fluid, phosphoric acid 750-800g/l, sulfuric acid 50g/l processes 30-150s at 90-110 DEG C of temperature, and (4) neutralize for the first time, with 100-150ml/l nitric acid or the neutralization of potassium permanganate 5-10% solution; (5) anodic oxidation for the first time, using aluminium as anode oxidation groove liquid as anodic bonding to the positive pole that is oxidized power supply, under alive effect, make outside the oxide film of aluminium material surface formation multi-hole type, oxidizing condition: sulfuric acid 150-220 DEG C, temperature 18-22 DEG C, current density 1.2-1.4A/dm
2, oxidation 10-20min; (6) dyeing, is to carry out in the fenestra of aluminum anodized film, requires rete to have enough porositys on the one hand, requires on the other hand fenestra inwall to keep certain activity.The tone dullness that electrolytic coloring obtains, is used the method for dyeing can meet ornamental requirement; (7) inorganic salt sealing for the first time, the Porosity anodic oxide film that anodic oxidation is generated seals with nickelous acetate, floods 15-30min, pH value 5.3-5.8, temperature 80-85 DEG C in 5-7g/l nickelous acetate encapsulant solution; (8) treatment agent processing at 10-35 DEG C, is flooded 10-120s under pH value 2.5-3.3 condition in the treatment agent of preparing at embodiment 4; (9) the corrosion-resistant ink of silk-screen; (8) alkaline etching for the second time, the composition of alkali cleaning agent: sodium hydroxide 40-55g/l, alkali cleaning additive 10-15g/l; At 40-55 DEG C, process 30-60s; (9) chemical rightenning, the composition nitric acid 30-80g/l of polishing fluid, phosphoric acid 750-800g/l, sulfuric acid 50g/l processes 30-150s at 90-110 DEG C of temperature, and (10) neutralize for the second time, with 100-150ml/l nitric acid or the neutralization of potassium permanganate 5-10% solution; (11) anodic oxidation for the second time, using aluminium as anode oxidation groove liquid as anodic bonding to the positive pole that is oxidized power supply, under alive effect, make outside the oxide film of aluminium material surface formation multi-hole type, oxidizing condition: sulfuric acid 150-220 DEG C, temperature 18-22 DEG C, current density 1.2-1.4A/dm
2, oxidation 10-20min; (12) dyeing, is to carry out in the fenestra of aluminum anodized film, requires rete to have enough porositys on the one hand, requires on the other hand fenestra inwall to keep certain activity.The tone dullness that electrolytic coloring obtains, is used the method for dyeing can meet ornamental requirement; (13) inorganic salt sealing for the second time, the Porosity anodic oxide film that anodic oxidation is generated seals with nickelous acetate, floods 15-30min, pH value 5.3-5.8, temperature 80-85 DEG C in 5-7g/l nickelous acetate encapsulant solution; Last cleaning obtains the aluminium alloy through two-step anodization processing again.
Above-mentioned several embodiment that just the present invention enumerates; it is not the exhaustive of the specific embodiment of the invention; cobalt salt, titanium salt, promotor and the silane that the present invention adopts can also adopt other and the allied substances in technical scheme, enumerated to replace; as long as it reaches technique effect of the present invention with essentially identical means, all should belong to protection scope of the present invention.
Claims (6)
1. one kind for the treatment agent before aluminium alloy two-step anodization silk-screen, it is characterized in that: the raw material that includes following weight in every kilogram for the treatment of agent solution: cobalt salt 0.02-0.08g, titanium salt 0.01-0.08g, promotor 0.01-0.20g, silane 0.01-0.20g, surplus are water, described promotor is hydrofluoric acid, ammonium bifluoride, Neutral ammonium fluoride, Sodium Fluoride or silicofluoric acid.
2. according to claim 1 a kind of for the treatment agent before aluminium alloy two-step anodization silk-screen, it is characterized in that described cobalt salt is rose vitriol, Cobaltous diacetate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES or cobaltous carbonate.
3. according to claim 1 a kind of for the treatment agent before aluminium alloy two-step anodization silk-screen, it is characterized in that described titanium salt is fluotitanate, titanium tetrachloride, titanic acid ester, titanium sulfate or Titanium Nitrate.
4. according to claim 1 a kind of for the treatment agent before aluminium alloy two-step anodization silk-screen, it is characterized in that described silane is epoxy radicals silicone hydride, amino silane compounds, fluoroalkyl silanes, vinyl silanes, alkyl silane or aromatic base silane.
5. according to claim 4 a kind of for the treatment agent before aluminium alloy two-step anodization silk-screen, it is characterized in that epoxy radicals silicone hydride is 3-glycidyl ether oxygen propyl trimethoxy silicane or Polyetherfunctional group triethoxyl silane; Amino silane compounds is N-aminoethyl-3-aminopropyl trimethoxysilane or 2-aminoethyl-3-aminopropyl methyl dimethoxysilane; Fluoroalkyl silanes is ten trifluoro octyltri-ethoxysilane, fluoro alkyl-silane or modification fluoroalkyl siloxanes; Vinyl silanes is vinyl trichloro silane or vinyltriethoxysilane; Alkyl silane is hexadecyl Trimethoxy silane, isobutyl triethoxy silane or octyltri-ethoxysilane; Aromatic base silane is phenyltrimethoxysila,e.
6. an aluminium alloy two-step anodization technique, is characterized in that: it comprises the steps: (1) cleaning, to remove the greasy dirt of aluminium material surface; (2) alkaline etching for the first time, to remove the natural oxide film of aluminium material surface, described alkaline etching tank liquor adopts the solution 40-60g/l of sodium hydroxide, inhibiter and complexing agent, at 40-60 DEG C, corrodes 30-120s; (3) neutralization for the first time, for removing aluminium material surface ash shape thing, spot and oxide film, puts into 10-30%HNO by aluminium
3solution, in 10-35 DEG C and 10-120s; (4) anodic oxidation for the first time, the cell liquid of employing is 150-250g/l sulphuric acid soln, temperature 18-22 DEG C, current density 1.0-2.5A/dm
2, oxidation 15-40min; (5) inorganic salt sealing is for the first time flooded 10-30min, pH value 5.3-5.8, temperature 75-85 DEG C in 5-10g/l nickelous acetate encapsulant solution; (6) treatment agent processing, at 10-35 DEG C, under pH value 2.5-3.3 condition, in treatment agent, flood 10-120s, wherein, in every kilogram for the treatment of agent solution, include the raw material of following weight: cobalt salt 0.02-0.08g, titanium salt 0.01-0.08g, promotor 0.01-0.20g, silane 0.01-0.20g, surplus are water, described promotor is hydrofluoric acid, ammonium bifluoride, Neutral ammonium fluoride, Sodium Fluoride or silicofluoric acid; (7) the corrosion-resistant ink of silk-screen; (8) alkaline etching for the second time, to remove aluminium material surface oxide film, described alkaline etching tank liquor adopts the solution 40-60g/l of sodium hydroxide, inhibiter and complexing agent, at 40-60 DEG C, corrodes 30-120s; (9) neutralization for the second time, for removing aluminium material surface ash shape thing, spot and oxide film, puts into 10-30%HNO by aluminium
3solution, in 10-35 DEG C and 10-120s; (10) anodic oxidation for the second time, the cell liquid of employing is 150-250g/l sulphuric acid soln, temperature 18-22 DEG C, current density 1.0-2.5A/dm
2, oxidation 15-40min; (11) inorganic salt sealing for the second time, the Porosity anodic oxide film that anodic oxidation is generated seals with nickelous acetate, floods 10-30min, pH value 5.3-5.8 in 5-10g/l nickelous acetate encapsulant solution, temperature 75-85 DEG C, obtains the aluminium alloy through two-step anodization processing.
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