CN103388167A - Protective treatment method of aluminum alloy surface - Google Patents
Protective treatment method of aluminum alloy surface Download PDFInfo
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- CN103388167A CN103388167A CN2013103649531A CN201310364953A CN103388167A CN 103388167 A CN103388167 A CN 103388167A CN 2013103649531 A CN2013103649531 A CN 2013103649531A CN 201310364953 A CN201310364953 A CN 201310364953A CN 103388167 A CN103388167 A CN 103388167A
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Abstract
The invention discloses a protective treatment method of an aluminum alloy surface. The protective treatment method comprises the following steps of: carrying out pre-treatment and deoxidation treatment on a to-be-treated workpiece, so that a water film lasts for 30 seconds by a workpiece surface water film process test; and anodizing, wherein a boric acid-sulfuric acid solution is adopted, the anodizing temperature is 21 DEG C-29 DEG C, the direct-current voltage is 14V-16V, the anodizing time is 19 minutes-21 minutes, the voltage is increased to gradually reach 14V-16V at the velocity of 3V/minute from 0V, the boric acid-sulfuric acid is free of chromic acid and comprises 37.5g/L-52.0g/L (according to mass volume concentration) of sulfuric acid and 5.2g/L-10.7g/L of boric acid, the content of sodium benzoate additive is not bigger than 1000ppm, and the treated workpiece is obtained by washing in cold water and naturally drying. Compared with the chromic acid anodizing of the aluminum alloy, the anodizing solution is free of a chromic anhydride component, so that the use of chromic anhydride is reduced in an anodizing process, the environmental pollution is reduced, and the generated sewage treatment cost is lowered.
Description
Technical field
The invention belongs to material surface protection field, is a kind of aluminum alloy surface protection processing method specifically.
Background technology
Current in aircraft industry the application more aluminum alloy anode metallization processes be chromic acid anodizing and sulfur acid anodizing.Sulfur acid anodizing is larger because of its Influence of Fatigue Properties to material, and the use in the aluminium alloy protection of civilian aircraft is few; Chromic acid anodizing is because its erosion resistance is better, and is less and more be widely used in the protection of domestic and international civilian aircraft aluminium alloy to the Influence of Fatigue Properties of material.
Chromic acid is a kind of poisonous carcinogenic substance.Chromic acid in chromic acid anodizing solution can be dispersed in air in process of production, stimulate people's respiratory mucosa, make it produce inflammation, simultaneously chromic acid anodizing production also can produce a large amount of chromate waste waters, and annual aviation factory all needs a large amount of man power and material of chromate waste water cost who produces in the chromic acid anodizing production process for processing.Along with the development of society and the enhancing of people's environmental protection consciousness, the requirement meeting of industrial sewage discharging is more and more higher, as these, produces in process of production the technique of a large amount of chromate waste waters and obnoxious flavour, can more and more can not adapt to the development of modernization industry.
Summary of the invention
For above shortcomings part in prior art, the technical problem to be solved in the present invention is to provide a kind of eco-friendly aluminum alloy surface protection processing method.
The present invention adopts following technical scheme:
A kind of aluminum alloy surface protection processing method comprises following step:
Step 1: carry out to workpiece to be handled pre-treatment and deoxidation treatment, made the workpiece surface moisture film continuous 30 seconds;
Step 2: the workpiece through step 1 carries out anodizing, and technique is: adopt boric acid-sulphuric acid soln, 21～29 ℃ of temperature; Volts DS 14～16V; Time is 19～21min; Voltage from 0V, increases with 3V/min speed, progressively reaches 14～16V; Do not contain chromic acid in this boric acid-sulfuric acid,, according to the mass body volume concentrations, comprise 37.5～52.0g/L sulfuric acid, 5.2～10.7g/L boric acid, the content of Sodium Benzoate additive is not more than 1000ppm;
3) through workpiece seasoning under room temperature after cold wash of step 2.
Further, the pre-treatment of step 1 is:
1) adopt acetone to carry out solution and clean to workpiece to be handled, during workpiece surface visual inspection after cleaning, workpiece surface is answered free from dust, grease and external residue; The workpiece dress is hung;
2) adopting mass concentration is the basic solution alkali cleaning of 45-60g/L, and the dipping alkaline solution cleans 10min at least, and water temperature 30-50 ℃ is carried out Warm Wash, then the surface after cold wash should reach moisture film continuous 30 seconds;
3) deoxidation treatment, according to the mass body volume concentrations, the solution that deoxidation treatment adopts contains Cr
+ 6Concentration be 22.5～26g/L, HNO
3Concentration be 75～105g/l, by add hydrofluoric acid adjust erosion rate 20～25 μ m/ single faces/hour, at room temperature, reaction 1～3min, the surface after cold wash reached moisture film continuous 30 seconds.
Further, through the anodized workpiece of step 2, adopt rare chromatedsolution to carry out sealing treatment, described rare chromatedsolution contains according to the mass body volume concentrations Cr that concentration is 45～100mg/L
+ 6, the pH value is between 3.2～3.8, temperature is controlled at 90 ± 2 ℃, time 23～28min.
Further, the mixing solutions that rare chromatedsolution is comprised of Sodium chromate and chromic anhydride, preparation is according to chromic anhydride CrO
3The mass body volume concentrations is 70mg/L; Sodium chromate Na
2CrO
3The mass body volume concentrations is 49mg/L, and surplus is water.
The present invention has following advantage and beneficial effect:
1, the present invention compares with the sulfur acid anodizing of routine, and is less to the fatigue property shadow of part.
2, technique of the present invention is compared with the chromic acid anodizing of aluminium alloy, owing to there is no the chromic anhydride composition in its anodization solution, make the use that has effectively reduced chromic anhydride in anodizing process, environmental contamination reduction has also reduced consequent sewage disposal expense (expense how much depend on turnout), due to this mill solution temperature and voltage lower, treatment time is also shorter, can reduce heat energy consumption 20%-40%; Power consumption is more than 32%, and the 10%-20% that can enhance productivity.
3, the solidity to corrosion part of having relatively high expectations, can do sealing treatment; When bonding force is had relatively high expectations, can not carry out sealing treatment.
Embodiment
Below in conjunction with embodiment and experimental example, the present invention is described in detail:
Embodiment 1
The Aluminium Alloys in Common Use workpiece of taking on aircraft adopts 7075 naked aluminium alloys and 2024 alclad alloys, according to following steps, processes:
Pre-treatment:
1) adopt acetone to carry out solution and clean to workpiece to be handled, during workpiece surface visual inspection after cleaning, workpiece surface is answered free from dust, grease and external residue; The workpiece dress is hung;
2) adopt the 44# clean-out system to carry out alkali and clean, the surface after cold wash should reach moisture film continuous 30 seconds; Being specially and adopting mass concentration is that the Isoprep44 basic solution alkali of 45g/L cleans, and the dipping alkaline solution cleans 10min at least, and 50 ℃ of water temperatures are carried out Warm Wash, then the surface after cold wash should reach moisture film continuous 30 seconds;
Deoxidation treatment:
Deoxidation treatment, according to the mass body volume concentrations, the solution that deoxidation treatment adopts contains Cr
+ 6Concentration be 22.5g/L, HNO
3Concentration be 75g/l, by add hydrofluoric acid adjust erosion rate 20 μ m/ single faces/hour, at room temperature, reaction 3min, the surface after cold wash reached moisture film continuous 30 seconds through the test of moisture film method.
The workpiece of processing carries out anodizing, and technique is: adopt boric acid-sulphuric acid soln, 21 ℃ of temperature; Volts DS 14V; Time is 19min; Voltage from 0V, increases with 3V/min speed, progressively reaches 14V; Do not contain chromic acid in this boric acid-sulfuric acid,, according to the mass body volume concentrations, comprise 37.5g/L sulfuric acid, 5.2g/L boric acid, the content 500ppm of Sodium Benzoate additive;
Anodized workpiece is seasoning under room temperature after cold wash, obtains finished product.
Embodiment 2
Be with the difference of embodiment 1:
Adopt 2024 naked aluminium alloys and 2024 alclads.
In pre-treatment, adopting mass concentration is that the Isoprep44 basic solution alkali of 60g/L cleans, and the dipping alkaline solution cleans 10min at least, and 50 ℃ of water temperatures are carried out Warm Wash, then the surface after cold wash should reach moisture film continuous 30 seconds;
Deoxidation treatment:
According to the mass body volume concentrations, the solution that deoxidation treatment adopts contains Cr
+ 6Concentration be 23g/L, HNO
3Concentration be 80g/l, by add hydrofluoric acid adjust erosion rate 21 μ m/ single faces/hour, at room temperature, reaction 2min, the surface after cold wash reached moisture film continuous 30 seconds through the test of moisture film method.
Workpiece through deoxidation treatment carries out anodizing, and technique is: adopt boric acid-sulphuric acid soln, 23 ℃ of temperature; Volts DS 15V; Time is 20min; Voltage from 0V, increases with 3V/min speed, progressively reaches 15V; Do not contain chromic acid in this boric acid-sulfuric acid,, according to the mass body volume concentrations, comprise 40g/L sulfuric acid, 7g/L boric acid, the content 300ppm of Sodium Benzoate additive;
Embodiment 3
Be with the difference of embodiment 1:
Adopt respectively 2024 naked aluminium alloys and two kinds of samples of 2024 alclad alloys.
In pre-treatment:
Adopting mass concentration is that the Isoprep44 basic solution alkali of 50g/L cleans, and the dipping alkaline solution cleans 10min at least, and 40 ℃ of water temperatures are carried out Warm Wash, then the surface after cold wash should reach moisture film continuous 30 seconds;
Deoxidation treatment:
According to the mass body volume concentrations, the solution that deoxidation treatment adopts contains Cr
+ 6Concentration be 25g/L, HNO
3Concentration be 90g/l, by add hydrofluoric acid adjust erosion rate 23 μ m/ single faces/hour, at room temperature, reaction 3min, the surface after cold wash reached moisture film continuous 30 seconds.
Workpiece through deoxidation treatment carries out anodizing, and technique is: adopt boric acid-sulphuric acid soln, 25 ℃ of temperature; Volts DS 16V; Time is 21min; Voltage from 0V, increases with 3V/min speed, progressively reaches 16V; Do not contain chromic acid in this boric acid-sulfuric acid,, according to the mass body volume concentrations, comprise 45g/L sulfuric acid, 8g/L boric acid, the content 700ppm of Sodium Benzoate additive;
Workpiece after anodizing adopts rare chromatedsolution to carry out sealing treatment, and rare chromatedsolution contains the Cr of 45mg/L
+ 6, the pH value is 3.8, temperature is controlled at 90 ± 2 ℃, time 40min.
Embodiment 4
Be with the difference of embodiment 1:
Adopt respectively 2024 naked aluminium alloys and two kinds of samples of 2024 alclad alloys.
In pre-treatment: adopting mass concentration is that the Isoprep44 basic solution alkali of 48g/L cleans, and the dipping alkaline solution cleans 10min at least, and 45 ℃ of water temperatures are carried out Warm Wash, then the surface after cold wash should reach moisture film continuous 30 seconds;
Deoxidation treatment:
According to the mass body volume concentrations, the solution that deoxidation treatment adopts contains Cr
+ 6Concentration be 26g/L, HNO
3Concentration be 105g/l, by add hydrofluoric acid adjust erosion rate 25 μ m/ single faces/hour, at room temperature, reaction 1min, the surface after cold wash reached moisture film continuous 30 seconds through the test of moisture film method.
Workpiece through deoxidation treatment carries out anodizing, and technique is: adopt boric acid-sulphuric acid soln, 28 ℃ of temperature; Volts DS 15V; Time is 20min; Voltage from 0V, increases with 3V/min speed, progressively reaches 15V; Do not contain chromic acid in this boric acid-sulfuric acid,, according to the mass body volume concentrations, comprise 45g/L sulfuric acid, 9g/L boric acid, the content 1000ppm of Sodium Benzoate additive;
Adopt rare chromatedsolution to carry out sealing treatment through anodized workpiece, rare chromatedsolution contains the Cr of 52mg/L
+ 6, the pH value is 3.2, temperature is controlled at 90 ± 2 ℃, time 25min.
Embodiment 5
Be with the difference of embodiment 1:
Adopt respectively 2024 naked aluminium alloys and two kinds of samples of 2024 alclad alloys.
In pre-treatment: adopting mass concentration is that the Isoprep44 basic solution alkali of 55g/L cleans, and the dipping alkaline solution cleans 10min at least, and 38 ℃ of water temperatures are carried out Warm Wash, then the surface after cold wash should reach moisture film continuous 30 seconds;
Deoxidation treatment:
According to the mass body volume concentrations, the solution that deoxidation treatment adopts contains Cr
+ 6Concentration be 24g/L, HNO
3Concentration be 90g/l, by add hydrofluoric acid adjust erosion rate 24 μ m/ single faces/hour, at room temperature, reaction 1min, the surface after cold wash reached moisture film continuous 30 seconds through the test of moisture film method.
Workpiece carries out anodizing, and technique is: adopt boric acid-sulphuric acid soln, 27 ℃ of temperature; Volts DS 16V; Time is 21min; Voltage from 0V, increases with 3V/min speed, progressively reaches 16V; Do not contain chromic acid in this boric acid-sulfuric acid,, according to the mass body volume concentrations, comprise 48g/L sulfuric acid, 8g/L boric acid, the content 800ppm of Sodium Benzoate additive;
Adopt rare chromatedsolution to carry out sealing treatment through anodized workpiece, rare chromatedsolution contains the Cr of 49mg/L
+ 6, the pH value is 3.5, temperature is controlled at 90 ± 2 ℃, time 25min.
Adopt in the above-described embodiments the power supply model: Sorensen DCS40-30E.
Experimental example 1
The rete test
Rete after boric acid-sulfur acid anodizing in above-described embodiment is carried out the test of weight:
Untight anodizing rete weight 〉=21.5mg/dm on 2024 naked aluminium alloys
2
Untight anodizing rete weight≤75.3mg/dm on 7075 naked aluminium alloys
2This result is to guarantee certain thicknesses of layers, because rete after 2000 series aluminum material anodizing is thinner, for guaranteeing certain solidity to corrosion, so require rete weight 〉=21.5mg/dm
2Because rete after 7000 series material anodizing is thicker, but this material is used as bearing member often, and rete is thicker can affect fatigability, requires rete weight≤75.3mg/dm
2Result shows and all reaches requirement.
Experimental example 2
Boric acid-sulfur acid anodizing membranous layer corrosion resistance test
In embodiment 3,4,53 groups of aluminium test pieces through the boric acid-sulfur acid anodizing of sealing according to ASTM B117 carry out respectively 336,360, hour salt-fog test (testing surface is in vertical direction with 6 degree angles) after, in arbitrary test piece, no more than 5 of the independent spot that presents or spot corrosion, diameter is not more than 0.8mm; Amounting to 90 square inches of (5.8dm
2) test area on, no more than 9 of the independent spot that presents or spot corrosion, diameter is not more than 0.8mm; Except those zones in distance edge, sign seal or point of contact 1.6mm scope.Illustrate that the solidity to corrosion result is good, corrosion resisting property is to represent with the hours that neutral salt spray test can reach.Can be suitable with the chromic acid anodizing membranous layer corrosion resistance by the salt-fog test of 336 hours.The present invention, by 360 hours, has good solidity to corrosion.
Experimental example 3
Boric acid-sulfur acid anodizing membranous layer binding force experiment:
To the boric acid of the workpiece in embodiment 3,4,5 sealing-sulfur acid anodizing rete, pressing BAC5736 coating epoxy primer (the base-material trade mark: 515K011, the solidifying agent trade mark: 910-012, manufacturer: PRC-De-Soto International, Inc.) film thickness is after after (8-20 μ m) at room temperature dry 8 hours, press BSS7225, when 1 type 1 class was carried out dried tape test, coating was not peeled off.2024 alclad alloys after the inventive method is processed,, through combining power test, prove that the bonding force of rete is good, the rete difficult drop-off.
Experimental example 4
The bonding force test
To untight boric acid in embodiment 1 and 2-sulfur acid anodizing rete primer coating: after priming paint solidifies fully, adopt 250 adhesive tapes of 3M company to carry out cross cut test by the cross cut test standard of ISO2409 paint and varnish, film adhesion all reaches 0 grade of level.
Claims (4)
1. an aluminum alloy surface protection processing method, is characterized in that, comprises following step:
Step 1: carry out to workpiece to be handled pre-treatment and deoxidation treatment, make workpiece surface reach moisture film continuous 30 seconds;
Step 2: the workpiece through step 1 carries out anodizing, and technique is: adopt boric acid-sulphuric acid soln, 21～29 ℃ of temperature; Volts DS 14～16V; Time is 19～21 min; Voltage from 0V, increases with 3V/min speed, progressively reaches 14～16V; Do not contain chromic acid in this boric acid-sulfuric acid,, according to the mass body volume concentrations, comprise 37.5～52.0g/L sulfuric acid, 5.2～10.7g/L boric acid, the content of Sodium Benzoate additive is not more than 1000ppm;
3) through workpiece seasoning under room temperature after cold wash of step 2.
2., according to the aluminum alloy surface protection processing method of claim 1, it is characterized in that, the pre-treatment of step 1 is:
1) adopt acetone to carry out solution and clean to workpiece to be handled, during workpiece surface visual inspection after cleaning, workpiece surface is answered free from dust, grease and external residue; The workpiece dress is hung;
2) adopting mass concentration is the basic solution alkali cleaning of 45-60 g/L, and the dipping alkaline solution cleans at least 10 min, and water temperature 30-50 ℃ is carried out Warm Wash, then the surface after cold wash should reach moisture film continuous 30 seconds;
3) deoxidation treatment, according to the mass body volume concentrations, the solution that deoxidation treatment adopts contains Cr
+ 6Concentration be 22.5～26 g/L, HNO
3Concentration be 75～105g/l, by add hydrofluoric acid adjust erosion rate 20～25 μ m/ single faces/hour, at room temperature, reaction 1～3min, the surface after cold wash reached moisture film continuous 30 seconds.
3. according to the aluminum alloy surface protection processing method of claim 1, it is characterized in that, adopt rare chromatedsolution to carry out sealing treatment through the anodized workpiece of step 2, described rare chromatedsolution contains according to the mass body volume concentrations Cr that concentration is 45 ~ 100mg/L
+ 6, the pH value is between 3.2～3.8, temperature is controlled at 90 ± 2 ℃, time 23 ~ 28min.
4., according to the aluminum alloy surface protection processing method of claim 4, it is characterized in that, the mixing solutions that rare chromatedsolution is comprised of Sodium chromate and chromic anhydride, preparation is according to chromic anhydride CrO
3The mass body volume concentrations is 70mg/L; Sodium chromate Na
2CrO
3The mass body volume concentrations is 49mg/L, and surplus is water.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103774146A (en) * | 2014-01-09 | 2014-05-07 | 南昌航空大学 | Deoxidation treatment method for chemical milling pretreatment of aluminum alloy |
| CN105937046A (en) * | 2016-06-28 | 2016-09-14 | 苏州有色金属研究院有限公司 | Treatment method for improving corrosion resistance of aluminum alloy |
| CN106501480A (en) * | 2016-11-30 | 2017-03-15 | 江西洪都航空工业集团有限责任公司 | A kind of method for differentiating aluminium lithium alloy chromic acid anodizing deoxidation effect |
| CN112342587A (en) * | 2020-10-20 | 2021-02-09 | 天长市京发铝业有限公司 | Aluminum plate anodic oxidation method |
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| US3733291A (en) * | 1971-07-23 | 1973-05-15 | Sprague Electric Co | Formation process for producing dielectric aluminum oxide films |
| US6149795A (en) * | 1998-10-27 | 2000-11-21 | The Boeing Company | Fungus resistant boric acid-sulfuric acid anodizing |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103774146A (en) * | 2014-01-09 | 2014-05-07 | 南昌航空大学 | Deoxidation treatment method for chemical milling pretreatment of aluminum alloy |
| CN103774146B (en) * | 2014-01-09 | 2016-05-18 | 南昌航空大学 | A kind of deoxidation treatment method in Aluminium Alloy after Chemical Milling pre-treatment |
| CN105937046A (en) * | 2016-06-28 | 2016-09-14 | 苏州有色金属研究院有限公司 | Treatment method for improving corrosion resistance of aluminum alloy |
| CN106501480A (en) * | 2016-11-30 | 2017-03-15 | 江西洪都航空工业集团有限责任公司 | A kind of method for differentiating aluminium lithium alloy chromic acid anodizing deoxidation effect |
| CN112342587A (en) * | 2020-10-20 | 2021-02-09 | 天长市京发铝业有限公司 | Aluminum plate anodic oxidation method |
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Application publication date: 20131113 |