CN104342736A - Aluminum alloy oxide film nickel-free normal-temperature sealing process and sealing agent - Google Patents
Aluminum alloy oxide film nickel-free normal-temperature sealing process and sealing agent Download PDFInfo
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- CN104342736A CN104342736A CN201410604573.5A CN201410604573A CN104342736A CN 104342736 A CN104342736 A CN 104342736A CN 201410604573 A CN201410604573 A CN 201410604573A CN 104342736 A CN104342736 A CN 104342736A
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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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- 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
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Abstract
The invention provides a normal-temperature sealing agent which can obtain oxide film sealing performance and corrosion resistance equivalent or superior to that by using a nickel-containing oxide film sealing agent, is easy to use, does not contain heavy metal, is simple in wastewater treatment and does not cause environmental pollution. The aluminum alloy oxide film nickel-free normal-temperature sealing agent contains at least one of compound A selected from water-soluble titanium compound or water-soluble zirconium compound and an organic compound B which is used as a stabilizer and is provided with a plurality of functional groups, wherein the content of the compound A is 0.1-50mmol/L; the content of the organic compound B is 2.5-10 times of the content of the compound A. The sealing agent further comprises accelerant with content of 0.1-5.0g/L and PH buffering agent with content of 1.0-20.0g/L.
Description
Technical field
The invention belongs to aluminium alloy additive technical field, more specifically relate to a kind of Process on Aluminum Alloy Oxidation Film without nickel normal temperature closing process and encapsulant.
Background technology
The oxide film of aluminium alloy anode oxide process has a large amount of nanometer apertures, and they have very strong adsorptive power, and the resistance to corrosion exposing oxide film is in the environment more weak.
A large amount of heavy metal nickels is contained in the low temperature that current China mainly uses in a large number or middle temperature oxide film encapsulant, because long-time and human contact the lighter understand chafing, severe one may have carcinogenic danger, so a lot of country has limited the use of various nickel-and aluminum-containing goods in the world.Current China from the renovation dynamics having strengthened environmental pollution since 2008, for the requirement of nickel total in the serious regional waste water of present environmental pollution for being not more than 0.1mg/L.
Summary of the invention
The object of the invention is to the deficiency overcoming prior art existence, provide a kind of Process on Aluminum Alloy Oxidation Film without nickel normal temperature closing process.
Another object of the present invention is to provide a kind of closure and the good normal-temperature sealer of erosion resistance, and suitability for industrialized production can be applied on a large scale.
For achieving the above object, this invention takes following technical scheme:
A kind of Process on Aluminum Alloy Oxidation Film, without nickel normal temperature closing process, comprises following technological step:
One, pre-treatment
A. Al-alloy products is immersed in and soaks 1-5 minute containing in 130-180g/L sulphuric acid soln, remove surface and oil contaminant and various inorganic pollutant, tap water washing secondary;
B. by through A process Al-alloy products is placed in the sodium hydroxide solution of 50-80g/L containing additive, at 50-70 DEG C of temperature, react 2-5 minute, remove surperficial natural oxide film, tap water washing secondary;
C. the aluminium parts through B process being placed in massfraction is 15% sulfuric acid and 5% nitre aqueous acid, normal temperature ash disposal process 3 ~ 5 minutes, washes once again after tap water washing secondary with deionized water;
Two, anodic oxidation
To be 160-180g/L sulphuric acid soln through putting into content through the Al-alloy products of pre-treatment, at 20 ± 2 DEG C of temperature, determine DC anodizing 30-60 minutes, current density be 1.3A/dm
2, thickness is 10-20um.After Al-alloy products is taken out in power-off, secondary washed by tap water, and pure water washing once;
Three, electrolytic coloring or dyeing
A. electrolytic coloring: put into through the Al-alloy products after anodic oxidation containing SnSO
43-10g/L, single nickel salt 15-25g/L, sulfuric acid 15-25g/L, in the solution of stablizer 5-10g/L, use voltage of alternating current 16V, electrolytic coloring 2-10 minutes at 20-25 DEG C of temperature.After Al-alloy products is taken out in power-off, secondary washed by tap water, and pure water washing is once, to be closed;
B. dye: will put into the solution containing 1g/L alizarin red S dyestuff through the Al-alloy products after anodic oxidation, soak 2-5 minutes at 50-70 DEG C of temperature, after taking out Al-alloy products, secondary washed by tap water, and pure water washing is once, to be closed;
Four, close
Process on Aluminum Alloy Oxidation Film of the present invention is as follows without nickel normal-temperature sealer processing parameter:
Solution temperature: 15-35 DEG C, best: 25 ± 3 DEG C
Speed in a closed circuit: 0.5-3.0um/min
PH value: 3.5-6.5
Five, the evaluation of aluminium alloy anode oxide film seal quality
The present invention detects the seal quality of anode oxide film according to the phosphorus chromic acid method of the assessment method part 2-nitric acid preimpregnation of GB/T 8753.2-2005 Al and Alalloy anodic oxidation oxide film sealing quality;
Detection liquid consists of:
A, predip solution: move in 650ml nitric acid (p=1.4g/ml) 1000ml volumetric flask, be diluted with water to scale;
Temperature: 19 ± 1 DEG C
Soak time: 10min
B, phosphorus-chromic acid solution: dissolve 20g chromium trioxide (Cr0
3), 35ml phosphoric acid (p=1.7g/ml), in 500ml water, moves into 1000ml volumetric flask, is diluted to scale with water, mixing.
Temperature: 38 ± 1 DEG C.
Soak time: 15min.
Weigh the corrosion weight loss of closing membrane before and after A, B solution are soaked, weightlessness is not more than 30mg/dm
2for qualified.
The surface quality of the anode oxide film of inventive closure adopts appearance method inspection.Air-dry rear use 50 times of magnifying glasses from 45 degree of observations, close anode oxide film surface without obvious lime, macula lutea, water stain etc. be qualified.
A kind of Process on Aluminum Alloy Oxidation Film is closed without nickel normal temperature, it consists of: at least one compd A containing water-soluble titanium compound or water-soluble zirconium compound, the content of compd A is at 0.1mmol/L-50mmol/L, and as the organic compound B with multiple functional group of stablizer, the content of organic compound B is 2.5-10 times of compd A, and described the present invention also comprises promotor 0.1-5.0g/L, PH buffer reagent 1.0-20.0g/L.
Described Process on Aluminum Alloy Oxidation Film is the organism having a kind of functional group at least containing 1-3 hydroxyls, carboxyl, amino and phosphonate groups in 1 molecule without the stablizer organic compound B in nickel normal-temperature sealer; Such organism is at least one in glycolic acid, oxysuccinic acid, oxalic acid, lactic acid, L-glutamic acid, glycerine, HEDP and salt thereof etc.
Described Process on Aluminum Alloy Oxidation Film is its vitriol, fluoride salt, organic salt without the water-soluble titanium compound in nickel normal-temperature sealer or water-soluble zirconium compound, is specially at least one in titanium sulfate, titanium sulfate ammonium, titanium acetylacetone, titanium potassium oxalate(T.P.O.), potassium fluotitanate, titanium sodium fluoride, ammonium titanium fluoride, zirconium sulfate, titanium sulfate ammonium, zirconium acetate, zirconium lactate, potassium fluozirconate, sodium fluozirconate, ammonium fluozirconate etc.
Described Process on Aluminum Alloy Oxidation Film is fluorochemical without the promotor in nickel normal-temperature sealer, is specially at least one in hydrofluoric acid, Sodium Fluoride, Potassium monofluoride, Neutral ammonium fluoride, ammonium bifluoride, Sodium Silicofluoride, ammonium silicofluoride, fluoroboric acid, Sodium tetrafluoroborate, ammonium borofluoride etc.
Described Process on Aluminum Alloy Oxidation Film is phosphoric acid and salt, silicate, acetic acid and salt thereof, boric acid and salt, biphthalate, benzoate, thiocarbonyl compound without the PH buffer reagent in nickel normal-temperature sealer, is specially at least one in sodium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, acetic acid, sodium acetate, sodium Diacetate, boric acid, borax, phthalic acid, Potassium Hydrogen Phthalate, phenylformic acid, Sodium Benzoate, thiocarbamide, dimethyl thiourea etc.
Compared with prior art, the present invention has following beneficial effect:
The present invention can obtain the normal-temperature sealer being same as or surmounting nickeliferous oxide film closure and erosion resistance, and easily uses, and not containing heavy metal, wastewater treatment simply can not to environment; And suitability for industrialized production can be applied on a large scale.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
Process on Aluminum Alloy Oxidation Film forms without nickel normal-temperature sealer:
Titanium sulfate: 0.5mmol/L, glycolic acid: 1.5mmol/L,
Hydrofluoric acid: 0.2g/L, fluoroboric acid: 0.1g/L,
Boric acid: 1.0g/L, thiocarbamide: 1.0g/L, deionized water: surplus.
Processing condition: PH (regulating with acetic acid or ammoniacal liquor) 6.0, temperature 35 DEG C.
By the aluminum products of the thickness 10um of pre-treatment, anodic oxidation, put into above-mentioned confining liquid 10 minutes.After taking out Al-alloy products, secondary washed by tap water, and pure water washing is once, air-dry.
Check specimen surface water stain-free and pollen.According to according to the weightless 21.8mg/dm of GB/T 8753.2-2005 phosphorus-chromic acid method
2.
Embodiment 2
Process on Aluminum Alloy Oxidation Film forms without nickel normal-temperature sealer:
Zirconium acetate: 5mmol/L, oxalic acid: 15mmol/L,
Sodium Fluoride: 1.0g/L, Sodium tetrafluoroborate: 0.5g/L,
Water glass: 0.5g/L, potassium hydrogen phthalate: 2.0g/L, deionized water: surplus.
Processing condition: PH (regulating with acetic acid or ammoniacal liquor) 5.5, temperature 30 DEG C.
By the thickness 15um of pre-treatment, anodic oxidation aluminum products again electrolytic coloring be champagne, put into above-mentioned confining liquid 7 minutes.After taking out Al-alloy products, secondary washed by tap water, and pure water washing is once, air-dry.
Check specimen surface water stain-free and pollen.According to according to the weightless 15.6mg/dm of GB/T 8753.2-2005 phosphorus-chromic acid method
2.
Embodiment 3
Process on Aluminum Alloy Oxidation Film forms without nickel normal-temperature sealer:
Titanium potassium oxalate(T.P.O.): 15mmol/L, HEDP:40mmol/L,
Neutral ammonium fluoride: 2.5g/L, ammonium borofluoride: 0.5g/L, sodium acetate: 1.0g/L,
Dimethyl thiourea: 3.0g/L, deionized water: surplus.
Processing condition: PH (regulating with acetic acid or ammoniacal liquor) 4.5, temperature 20 DEG C.
Dye redness again by the aluminum products of the thickness 10um of pre-treatment, anodic oxidation, put into above-mentioned confining liquid 5 minutes.After taking out Al-alloy products, secondary washed by tap water, and pure water washing is once, air-dry.
Check specimen surface water stain-free and pollen.According to according to the weightless 11.2mg/dm of GB/T 8753.2-2005 phosphorus-chromic acid method
2.
Embodiment 4
Process on Aluminum Alloy Oxidation Film forms without nickel normal-temperature sealer:
Potassium fluozirconate: 30mmol/L, lactic acid: 100mmol/L, Sodium Fluoride: 0.5g/L,
Sodium Silicofluoride: 0.5g/L, sodium hydrogen phosphate: 1.0g/L,
Thiocarbamide: 5.0g/L, deionized water: surplus.
Processing condition: PH (regulating with acetic acid or ammoniacal liquor) 4.0, temperature 20 DEG C.
By the aluminum products of the thickness 20um of pre-treatment, anodic oxidation, put into above-mentioned confining liquid 10 minutes.After taking out Al-alloy products, secondary washed by tap water, and pure water washing is once, air-dry.
Check specimen surface water stain-free and pollen.According to according to the weightless 8.6mg/dm of GB/T 8753.2-2005 phosphorus-chromic acid method
2.
Embodiment 5
Process on Aluminum Alloy Oxidation Film forms without nickel normal-temperature sealer:
Ammonium titanium fluoride: 50mmol/L, L-glutamic acid: 150mmol/L,
Ammonium bifluoride: 0.5g/L, ammonium borofluoride: 0.2g/L,
Sodium Benzoate: 2.0g/L, thiocarbamide: 10.0g/L, deionized water: surplus.
Processing condition: PH (regulating with acetic acid or ammoniacal liquor) 3.5, temperature 15 DEG C.
Be black by the aluminum products electrolytic coloring of the thickness 20um of pre-treatment, anodic oxidation, put into above-mentioned confining liquid 7 minutes.After taking out Al-alloy products, secondary washed by tap water, and pure water washing is once, air-dry.
Check specimen surface water stain-free and pollen.According to according to the weightless 7.5mg/dm of GB/T 8753.2-2005 phosphorus-chromic acid method
2.
The present invention is not limited in embodiment described herein, can by adding, changes, deletion etc. shift gears performance action effect of the present invention, be also contained in scope of the present invention.
Claims (10)
1. Process on Aluminum Alloy Oxidation Film is without a nickel normal temperature closing process, it is characterized in that: comprise following technological step:
One, pre-treatment
A. Al-alloy products is immersed in and soaks 1-5 minute containing in 130-180g/L sulphuric acid soln, remove surface and oil contaminant and various inorganic pollutant, tap water washing secondary;
B. by through A process Al-alloy products is placed in the sodium hydroxide solution of 50-80g/L containing additive, at 50-70 DEG C of temperature, react 2-5 minute, remove surperficial natural oxide film, tap water washing secondary;
C. the aluminium parts through B process being placed in massfraction is 15% sulfuric acid and 5% nitre aqueous acid, normal temperature ash disposal process 3 ~ 5 minutes, washes once again after tap water washing secondary with deionized water;
Two, anodic oxidation
To be 160-180g/L sulphuric acid soln through putting into content through the Al-alloy products of pre-treatment, at 20 ± 2 DEG C of temperature, determine DC anodizing 30-60 minutes, current density be 1.3A/dm
2, thickness is 10-20um.After Al-alloy products is taken out in power-off, secondary washed by tap water, and pure water washing once;
Three, electrolytic coloring and dyeing
A. electrolytic coloring: put into through the Al-alloy products after anodic oxidation containing SnSO
43-10g/L, single nickel salt 15-25g/L, sulfuric acid 15-25g/L, in the solution of stablizer 5-10g/L, use voltage of alternating current 16V, electrolytic coloring 2-10 minutes at 20-25 DEG C of temperature; After Al-alloy products is taken out in power-off, secondary washed by tap water, and pure water washing is once, to be closed;
B. dye: will put into the solution containing 1g/L alizarin red S dyestuff through the Al-alloy products after anodic oxidation, soak 2-5 minutes at 50-70 DEG C of temperature, after taking out Al-alloy products, secondary washed by tap water, and pure water washing is once, to be closed;
Four, close
Process on Aluminum Alloy Oxidation Film of the present invention is as follows without nickel normal-temperature sealer processing parameter:
Solution temperature: 15-35 DEG C, best: 25 ± 3 DEG C
Speed in a closed circuit: 0.5-3.0um/min
PH value: 3.5-6.5
Five, the evaluation of aluminium alloy anode oxide film seal quality
The present invention detects the seal quality of anode oxide film according to the phosphorus chromic acid method of the assessment method part 2-nitric acid preimpregnation of GB/T 8753.2-2005 Al and Alalloy anodic oxidation oxide film sealing quality;
Detection liquid consists of:
A, predip solution: move in 650ml nitric acid (p=1.4g/ml) 1000ml volumetric flask, be diluted with water to scale;
Temperature: 19 ± 1 DEG C
Soak time: 10min
B, phosphorus-chromic acid solution: dissolve 20g chromium trioxide (Cr0
3), 35ml phosphoric acid (p=1.7g/ml), in 500ml water, moves into 1000ml volumetric flask, is diluted to scale with water, mixing;
Temperature: 38 ± 1 DEG C;
Soak time: 15min;
Weigh the corrosion weight loss of closing membrane before and after A, B solution are soaked, weightlessness is not more than 30mg/dm
2for qualified;
The surface quality of the anode oxide film of inventive closure adopts appearance method inspection; Air-dry rear use 50 times of magnifying glasses from 45 degree of observations, close anode oxide film surface without obvious lime, macula lutea, water stain etc. be qualified.
2. a Process on Aluminum Alloy Oxidation Film is without nickel normal-temperature sealer, it is characterized in that, it consists of: at least one compd A containing water-soluble titanium compound or water-soluble zirconium compound, the content of compd A is at 0.1mmol/L-50mmol/L, and as the organic compound B with multiple functional group of stablizer, the content of organic compound B is 2.5-10 times of compd A, also comprises promotor 0.1-5.0g/L, PH buffer reagent 1.0-20.0g/L.
3. a kind of Process on Aluminum Alloy Oxidation Film according to claim 2 is without nickel normal-temperature sealer, it is characterized in that, described Process on Aluminum Alloy Oxidation Film is the organism having a kind of functional group at least containing 1-3 hydroxyls, carboxyl, amino and phosphonate groups in 1 molecule without the stablizer organic compound B in nickel normal-temperature sealer.
4. a kind of Process on Aluminum Alloy Oxidation Film according to claim 3 is without nickel normal-temperature sealer, it is characterized in that, described stablizer organic compound B is at least one in glycolic acid, oxysuccinic acid, oxalic acid, lactic acid, L-glutamic acid, glycerine, HEDP and salt thereof.
5. a kind of Process on Aluminum Alloy Oxidation Film according to claim 2 is without nickel normal-temperature sealer, it is characterized in that, described water-soluble titanium compound or water-soluble zirconium compound are its vitriol, fluoride salt or organic salt.
6. a kind of Process on Aluminum Alloy Oxidation Film according to claim 5 is without nickel normal-temperature sealer, it is characterized in that, described water-soluble titanium compound or water-soluble zirconium compound are be specially at least one in titanium sulfate, titanium sulfate ammonium, titanium acetylacetone, titanium potassium oxalate(T.P.O.), potassium fluotitanate, titanium sodium fluoride, ammonium titanium fluoride, zirconium sulfate, titanium sulfate ammonium, zirconium acetate, zirconium lactate, potassium fluozirconate, sodium fluozirconate or ammonium fluozirconate.
7. a kind of Process on Aluminum Alloy Oxidation Film according to claim 2 is without nickel normal-temperature sealer, it is characterized in that, described Process on Aluminum Alloy Oxidation Film is fluorochemical without the promotor in nickel normal-temperature sealer.
8. a kind of Process on Aluminum Alloy Oxidation Film according to claim 7 is without nickel normal-temperature sealer, it is characterized in that, described Process on Aluminum Alloy Oxidation Film is specially at least one in hydrofluoric acid, Sodium Fluoride, Potassium monofluoride, Neutral ammonium fluoride, ammonium bifluoride, Sodium Silicofluoride, ammonium silicofluoride, fluoroboric acid, Sodium tetrafluoroborate or ammonium borofluoride without the promotor in nickel normal-temperature sealer.
9. a kind of Process on Aluminum Alloy Oxidation Film according to claim 2 is without nickel normal-temperature sealer, it is characterized in that, described Process on Aluminum Alloy Oxidation Film is phosphoric acid and salt, silicate, acetic acid and salt thereof, boric acid and salt, biphthalate, benzoate or thiocarbonyl compound without the PH buffer reagent in nickel normal-temperature sealer.
10. a kind of Process on Aluminum Alloy Oxidation Film according to claim 9 is without nickel normal-temperature sealer, it is characterized in that, described Process on Aluminum Alloy Oxidation Film is at least one in sodium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, acetic acid, sodium acetate, sodium Diacetate, boric acid, borax, phthalic acid, Potassium Hydrogen Phthalate, phenylformic acid, Sodium Benzoate, thiocarbamide or dimethyl thiourea without the PH buffer reagent in nickel normal-temperature sealer.
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| CN105386109A (en) * | 2015-11-28 | 2016-03-09 | 贵州凯星液力传动机械有限公司 | Special surface treatment process and system for improving aluminum alloy part abrasive resistance |
| CN105441922A (en) * | 2015-11-10 | 2016-03-30 | 铜陵市明诚铸造有限责任公司 | Method for processing exterior and interior of roller |
| CN105862104A (en) * | 2016-06-02 | 2016-08-17 | 哈尔滨工程大学 | Preparation method of wear-resistant anti-friction composite aluminum oxide film |
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Application publication date: 20150211 |