CN113046810B - Aluminum alloy hard anodizing pressurization method and aluminum alloy hard anodizing process - Google Patents
Aluminum alloy hard anodizing pressurization method and aluminum alloy hard anodizing process Download PDFInfo
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- CN113046810B CN113046810B CN202110285706.7A CN202110285706A CN113046810B CN 113046810 B CN113046810 B CN 113046810B CN 202110285706 A CN202110285706 A CN 202110285706A CN 113046810 B CN113046810 B CN 113046810B
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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
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
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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
- C25D11/12—Anodising more than once, e.g. in different baths
Abstract
The aviation aluminum alloy hard anodic oxidation process comprises the steps of pretreating an aluminum alloy part, placing the pretreated aluminum alloy into sulfuric acid electrolyte for hard anodic oxidation, wherein the pretreatment at least comprises oil removal and deoxidation; the hard anodizing step adopts a four-section power supply control mode; referring to the known comparative example, the current value required for the part to reach the target film thickness was derived from the feedback of the voltage at low current density of the aluminum alloy part. The invention provides a hard anodic oxidation method without calculating the anodic oxidation area, and improves the accuracy of controlling the thickness of an oxide film to a certain extent. The aluminum alloy part subjected to the hard anodizing process can stably reach the preset film thickness without the need of part oxidation area measurement work before setting the oxidation current, thereby avoiding finished product film thickness errors caused by oxidation area measurement errors and reducing repeated debugging experiments before measuring new products.
Description
Technical Field
The invention relates to an aluminum alloy hard anodizing process, in particular to an aluminum alloy hard anodizing pressurization method and an aluminum alloy hard anodizing process, which are suitable for aluminum alloy materials for aviation, such as 6061, 2024, 7075 and the like.
Background
The anodic oxidation of aluminum refers to a process of generating an oxide film on the surface of aluminum or aluminum alloy in an electrolyte under certain process conditions; the hard anodic oxidation is improved on the basis of the common anodic oxidation, so that the thickness and the hardness of a generated oxide film layer are increased, and excellent corrosion resistance and wear resistance are provided for products. The anodic oxidation and hard anodic oxidation processes are widely applied to the manufacturing process of aviation parts, and aviation aluminum alloy parts put high requirements on the thickness of an oxidation film layer.
The hard anodic oxidation generally adopts a direct current power supply to load current, so that an oxide film layer continuously grows under constant current density until the film thickness reaches the required range; to achieve a given current density, substitution is required to calculate an accurate oxidation area. The oxidation area needs to be calculated by professional drawing engineers according to a three-dimensional drawing, the aviation aluminum parts are various in variety, small in batch quantity and mostly in irregular complex structures, and the anodic oxidation area of part of the part is located at the inner hole, so that the anodic oxidation area of the part is difficult to calculate. If the three-dimensional drawing is lacked, the estimation can be carried out only according to the appearance, and the stable process is determined through multiple anodic oxidation tests, wherein one test usually requires more than one hour; part of the parts may also generate calculation errors due to their own dimensional differences. The estimated area is too large, so that the actual current density is increased, and parts are burned; the estimated area is too small, the film layer grows slowly and cannot reach the set thickness, and therefore the development speed and the cost of the aviation product hard anode are challenged.
When the anodic oxidation requirement of various complex parts is met in industrial production, the thickness of the stable and accurate oxide film layer cannot be achieved by using a conventional constant current method.
Disclosure of Invention
The invention aims to provide an aluminum alloy hard anodizing process, which can quickly and stably carry out hard anodizing on aviation aluminum parts, avoid the calculation of the oxidation area of complex parts, reduce the test process of parts with different specifications, accelerate the development speed, reduce the cost and improve the effect of hard anodizing as much as possible.
In order to achieve the aim of the invention, the invention provides an aluminum alloy hard anodic oxidation pressurizing method which comprises the following steps: putting the aluminum alloy part into sulfuric acid electrolyte, and adopting the following four-section power supply control mode:
first stage L1: slowly increasing the voltage for 5 minutes until reaching the target voltage U 1 Recording the target voltage U reached by hard anodic oxidation 1 Current of time I 1 ；
Second stage L2: applying a constant target voltage U 1 Keeping the time for 1 minute, setting the hard anodic oxidation current I 2 The current I 1 And current I 2 The ratio of (1);
third stage L3: slowly raising current to current I 2 The slow rising time is 10 minutes;
fourth stage L4: at a constant current I 2 Carrying out hard anodic oxidation, wherein the retention time is increased along with the thickness of the target film;
the target voltage U 1 The determination method comprises the following steps:
m1: selecting a reference product with the same material as the aluminum alloy part to be detected, and putting the reference product into the same electrolyte for hard anodic oxidation;
m2: calculating the current I to be reached by the electrolyte according to the sum of the oxidation areas of the reference substance and the hanger 4 ；
M3: the anodic oxidation pressurization process of the reference comprises two stages:
the first stage is as follows: slowly raising current to current I 4 Slow rising time of 15 minutes, set current I 3 Current I of 3 And current I 4 And recording the voltage value U at the time as 1 2 ；
And a second stage: maintaining a constant current I 4 The retention time increases with the required film thickness.
M4: repeating the above M1-M3 for multiple times to obtain multiple groups of voltage values U 2 Calculating a voltage value U 2 To obtain the target voltage U 1 。
In the above technical solution, the current density of the fourth stage L4 is 2.8-3.2A/dm 2 。
In the above technical solution, other parameters of the sulfuric acid electrolyte:
temperature of the electrolyte: -2 ℃ to 0 ℃; h 2 SO 4 220—230g/L；Al 3+ ＜20g/L。
In the above technical solution, the target voltage U of the first stage L1 and the second stage L2 1 Is 17-19V.
In the technical scheme, the parts are made of 6061 aluminum alloy and U 1 17.8-18.2V; the material of the parts is 2024 aluminum alloy, U 1 17.0-17.5V; the material of the part is 7075 aluminum alloy and U 1 Is 18.5-19V.
The invention also provides an aluminum alloy hard anodic oxidation process, which is used for pretreating aluminum alloy parts, wherein the pretreatment at least comprises oil removal and deoxidation;
and carrying out hard anodic oxidation on the pretreated aluminum alloy part according to any one of the aluminum alloy hard anodic oxidation pressurizing methods.
In the above technical solution, the pretreatment comprises the following steps:
s1, pre-cleaning: using isopropanol or butanone organic solution for pre-cleaning;
s2, clamping: putting the aluminum alloy part into a tool hanger made of a titanium alloy bar or an aluminum alloy bar;
s3, alkaline chemical oil removal: degreasing with weak alkaline cleaning agent at concentration of 30-50g/L and temperature of 50-65 deg.C for 5-10 min; carrying out two-pass overflow water washing on the deoiled part, wherein each pass lasts for 1-3 minutes;
s4, acid washing and deoxidation: removing an oxide film naturally generated in the air by using acid washing, wherein the acid washing solution comprises the following components:
HNO 3 75-160g/l，CrO 3 22.5-26.2g/l，HF 1％(V/V)；
and (3) carrying out three-pass overflow washing on the deoxidized part: each lane for 1-3 minutes.
In the technical scheme, the corrosion speed of the pickling solution in the S4 pickling and deoxidizing step is 10.16-15.24 mu m/h, and the deoxidizing time is 1-10 minutes.
In the above technical solution, the ratio of the anode area of the hanger to the aluminum alloy part is less than 10.
In the above technical solution, the aluminum alloy part is subjected to a sealing treatment after being subjected to a hard anodizing step, wherein the sealing treatment is double sealing, and the method comprises the following steps:
first blocking with nickel acetate:
the components: ni (AC) 2 5-10g/L; temperature: 80-95 ℃; sealing time: 20-30 minutes;
then, cleaning by two times of pure water for 1-3 minutes each time;
then using dichromate capping:
the components: k 2 Cr 2 O 7 45-55g/l; temperature: 92-100 ℃; sealing time: 15-20 minutes;
then, the mixture is washed by two times of pure water for 1-3 minutes each time.
In the field of aviation part anodization, irregular aluminum alloy parts without three-dimensional drawings are usually encountered by the inventor, the oxidation area of the part cannot be accurately calculated in the initial stage, and a great deal of effort is required for calibrating the anodization process of a new part. The inventor of the invention finds that under the action of approximate current density, the anodizing electrolyte has strong dispersing capacity, anodized virtual electric lines are uniform, the film forming rate of the aluminum alloy of the same material is almost equal, and the required oxidation voltage is also approximately equal.
The invention provides a hard anodic oxidation method without calculating the anodic oxidation area, and improves the accuracy of controlling the thickness of an oxide film to a certain extent. The invention improves the anodizing process and the voltage control process of electrolyte, and the aluminum alloy part subjected to the hard anodizing process can stably reach the preset film thickness without the need of part oxidation area measurement before setting the oxidation current, so that finished product film thickness errors caused by oxidation area measurement errors are avoided, and repeated debugging experiments before measuring new products are reduced.
Detailed Description
Example 1:
the material of the part to be measured: 6061.
after the pretreatment step, the parts are placed in sulfuric acid electrolyte for hard anodizing, and after the parts are dried, the parts are hung and inspected.
The pretreatment step comprises:
s1, pre-cleaning: the method has the advantages that the organic solvent such as isopropanol or butanone is used for pre-cleaning, the organic solvent has strong dissolving effect on the saponified oil and the unsaponifiable oil, and can remove oil stains remained on the surface of a part in the machining process, polishing paste remained in the polishing process, marks of a marker pen in the inspection process and the like, so that a more excellent oil removing effect can be obtained in the subsequent oil removing process of the weak alkaline cleaning agent;
s2, clamping: the tool clamp made of the titanium alloy bar or the aluminum alloy bar can clamp a part with an internal thread by screwing a specially-made titanium alloy thread into the internal thread of the part, and the design is very reliable for hard anodization and can obtain very stable current output;
s3, alkaline chemical oil removal: because the aluminum alloy has amphipathy and is different from other metals, the addition amount of the alkali is limited, and a weakly alkaline cleaning agent is used for removing oil; the concentration is 30-50g/L, the temperature is 50-65 ℃, and the time is 5-10 minutes; and (3) carrying out two times of overflow washing on the deoiled part: after washing for 1-3 minutes each time, carrying out water film inspection, and observing the water film continuity of the part within 30 seconds on the surface of the part, thereby proving that the part is fully cleaned;
s4, acid washing and deoxidation: the aluminum alloy can produce a natural oxide film in the air, and the natural oxide film is removed by acid washing, wherein the acid washing solution comprises the following components:
HNO 3 75-160g/l，CrO 3 22.5-26.2g/l，HF 1％(V/V)；
adjusting the corrosion rate to be 10.16-15.24 μm/h by adjusting the concentration of hydrofluoric acid, and deoxidizing for 1-10 min; and (3) carrying out three-pass overflow water washing on the acid-washed and deoxidized part, wherein each pass is 1-3 minutes, carrying out water film inspection after water washing, and observing the continuity of the water film of the part within 30 seconds on the surface of the part, thereby proving that the part is fully cleaned.
The hard anode oxidation step adopts a four-section power supply control mode:
the first stage is as follows: the voltage is slowly increased for 5 minutes until the target voltage U is reached 1 Recording the current I when the hard anode oxidation reaches the target voltage of 18V 1 ；
And a second stage: applying a constant target voltage U 1 Keeping the time for 1 minute, setting the hard anodic oxidation current I 2 Current I 1 And current I 2 The ratio of (A) to (B) is 1/3;
and a third stage: slowly increasing current to I 2 The slow rising time is 10 minutes;
a fourth stage: the hard anodizing is carried out at a constant current, and the holding time is increased according to the required film thickness.
Other parameters of the hard anodizing step:
temperature of the electrolyte: -2 ℃ to 0 ℃; h 2 SO 4 Concentration: 220-230 g/L; al (Al) 3+ Concentration: is less than 20g/L.
The following three groups of parts with 6061 materials are subjected to voltage and current changes in the hard anodizing process according to the steps and finally reach the film thickness of the parts.
Component 1
Component 2
Component 3
Target voltage U of the first stage in the hard anodizing step 1 The method is characterized by comprising the following steps of (1) determining by a parallel test before measuring a sample, wherein the parallel test adopts a reference substance which is the same as the sample to be measured in material, preferably selects a regular part with an easily-calculated oxidation area, and carries out hard anodic oxidation in the same electrolyte; the voltage control method is constant current method, and the current density is set to be 2.8A/dm 2 ～3.2A/dm 2 A step of,; calculating the current I to be reached by the electrolyte according to the sum of the oxidation areas of the reference substance and the hanger 4 . Controlling the area of the clamp: the area of the part is less than or equal to 10:1, the current error obtained increases when the clamp to part area ratio is too large.
The electrolytic pressing process of the reference comprises two stages: the first stage is as follows: slowly raising current to current I 4 Slow rising time of 15 minutes, set current I 3 Current I 3 And current I 4 The ratio of (A) to (B) is 1/3, so that the electrolyte is subjected to oxidation current I 3 The current density is kept at 0.9A/dm 2 ～1.1A/dm 2 And recording the voltage value at the moment, and taking the voltage value as the target voltage U of the sample to be tested 1 (ii) a And a second stage: maintaining a constant current I 4 The holding time is increased along with the required film thickness, and the film thickness curve of the same material can be obtained according to the data measured in the second stage, such as 6061 aluminum alloy parts with the constant current density of 2.8A/dm 2 ～3.2A/dm 2 Stage, the growth rate of the oxide film is 0.95-1.05 μm/min.
In order to reduce the target voltage U 1 Error, can carry on the multiple-unit repetition test to the reference article according to the above-mentioned step, and carry on the data processing to the voltage value obtained, make the target voltage U 1 More accurate.
Example 2:
the material of the part to be measured: 2024
The pretreatment procedure and the electrolyte composition of example 2 were the same as those of example 1. Parallel experiment according to 2024 measured target voltage U 1 Is 17.0-17.5V.
The hard anode oxidation step adopts a four-section power supply control mode:
the first stage is as follows: slowly increasing the voltage for 5 minutes until reaching the target voltage U 1 Recording the current I when the hard anode oxidation reaches the target voltage of 18V 1 ；
And a second stage: applying a constant target voltage U 1 Keeping the time for 1 minute, setting the hard anodizing current I 2 Current I of 1 And current I 2 The ratio of (A) to (B) is 1/3;
and a third stage: slowly increasing current to I 2 The slow rising time is 10 minutes;
a fourth stage: the hard anodizing is carried out at a constant current, and the holding time is increased according to the required film thickness.
The following is a group of 2024 parts, which are subjected to hard anodizing according to the above steps, and the final film thickness of the parts.
Details 4
Example 3:
the material of the part to be measured: 7075.
the pretreatment procedure and the electrolyte composition of example 2 were the same as those of example 1. The target voltage was measured to be 18.5-19V according to parallel experiments of 2024.
The hard anode oxidation step adopts a four-section power supply control mode:
the first stage is as follows: slowly increasing the voltage for 5 minutes until reaching the target voltage U 1 Recording the current I when the hard anodic oxidation reaches the target voltage of 18V 1 ；
And a second stage: applying a constant target voltage U 1 Keeping the time for 1 minute, setting the hard anodic oxidation current I 2 Current I 1 And current I 2 The ratio of (A) to (B) is 1/3;
and a third stage: slowly increasing current to I 2 The slow rising time is 10 minutes;
a fourth stage: the hard anodizing is carried out at a constant current, and the holding time is increased according to the required film thickness.
The following is a group of parts 7075 in accordance with the above procedure for hard anodizing process voltage, current change and final part film thickness.
Details 5
The five parts in the three embodiments are subjected to parallel tests for 10-20 times, and the difference between the test film thickness and the expected film thickness is 0.5-2 μm and is within the allowable error range of the expected film thickness.
Example 4:
the material of the part to be detected: 6061. 2025, 7075;
part of products with special purposes need to be subjected to hole sealing treatment after the hard anode is oxidized, and the parts are used for sealing air holes generated in the electrolytic process, so that an excellent corrosion resistant effect is obtained.
Embodiment 4, on the basis of embodiments 1 to 3, further includes a sealing step of the part subjected to the hard anodizing step according to the material of the part, where the sealing step is double sealing and includes the following two sealing processes:
first blocking with nickel acetate:
the components: ni (AC) 2 5-10g/L; temperature: 80-95 ℃; sealing time: 20-30 minutes;
then, cleaning by two times of pure water for 1-3 minutes each time;
then using dichromate capping:
the components: k is 2 Cr 2 O 7 45-55g/l; temperature: 92-100 ℃; sealing time: 15-20 minutes;
then, cleaning by two times of pure water for 1-3 minutes each time;
the aluminum alloy after double sealing treatment has excellent corrosion resistance.
Although an embodiment of the present invention has been shown and described above, it is understood that the above embodiment exemplifies three general aluminum materials for aerospace parts and is not to be construed as limiting the present invention, and those skilled in the art can make changes, modifications, substitutions and alterations to the above embodiment within the scope of the present invention.
Claims (6)
1. The aluminum alloy hard anodizing pressurization method is characterized by comprising the following steps: putting the aluminum alloy part into sulfuric acid electrolyte, and adopting the following four-section power supply control mode:
first stage L1: the voltage is slowly increased for 5 minutes until the target voltage U is reached 1 Recording the target voltage U reached by hard anodic oxidation 1 Current of time I 1 ；
Second stage L2: applying a constant target voltage U 1 Keeping the time for 1 minute, setting the hard anodizing current I 2 Said current I 1 And current I 2 The ratio of (1);
third stage L3: slowly raising current to current I 2 The slow rising time is 10 minutes;
fourth stage L4: at a constant current I 2 Carrying out hard anodic oxidation, wherein the retention time is increased along with the thickness of the target film;
the target voltage U 1 The determination method comprises the following steps:
m1: selecting a reference product with the same material as the aluminum alloy part to be detected, and putting the reference product into the same electrolyte for hard anodic oxidation;
m2: calculating the current I to be reached by the electrolyte according to the sum of the oxidation areas of the reference substance and the hanger 4 ；
M3: the anodic oxidation pressurization process of the reference comprises two stages:
the first stage is as follows: slowly raising current to current I 4 Slow rising time of 15 minutes, set current I 3 Current I of 3 And current I 4 And recording the voltage value U at the time as 1 2 ；
And a second stage: maintaining a constant current I 4 The holding time is increased along with the required film thickness;
m4: repeating the above M1-M3 for multiple times to obtain multiple groups of voltage values U 2 Calculating a voltage value U 2 To obtain the target voltage U 1 ；
Wherein the current density of the fourth stage L4 is 2.8-3.2A/dm 2 ；
Other parameters of the sulfuric acid electrolyte:
temperature of the electrolyte: -2 ℃ to 0 ℃; h 2 SO 4 220—230g/L；Al 3+ ＜20g/L；
The part material is 6061 aluminum alloy, and U1 is 17.8-18.2V; the material of the part is 2024 aluminum alloy, and U1 is 17.0-17.5V; the part material is 7075 aluminum alloy, and U1 is 18.5-19V.
2. The aluminum alloy hard anodizing process is characterized by comprising the following steps: pretreating the aluminum alloy part, wherein the pretreatment at least comprises oil removal and deoxidation;
hard anodizing the aluminum alloy member after the pretreatment according to the aluminum alloy hard anodizing pressure method as set forth in claim 1.
3. The aluminum alloy hard anodizing process of claim 2, wherein: the pretreatment comprises the following steps:
s1, pre-cleaning: using isopropanol or butanone organic solution for pre-cleaning;
s2, clamping: putting the aluminum alloy part into a tool hanger made of a titanium alloy bar or an aluminum alloy bar;
s3, alkaline chemical oil removal: degreasing with weak alkaline cleaning agent at concentration of 30-50g/L and temperature of 50-65 deg.C for 5-10 min; carrying out two-pass overflow water washing on the deoiled part, wherein each pass is 1-3 minutes;
s4, acid washing and deoxidation: removing an oxide film naturally generated in the air by using acid washing, wherein the acid washing solution comprises the following components:
HNO 3 75-160g/l，CrO 3 22.5-26.2g/l，HF 1Vol%；
and (3) carrying out three times of overflow washing on the deoxidized part: each lane for 1-3 minutes.
4. The aluminum alloy hard anodizing process of claim 3, wherein: and in the S4 acid pickling and deoxidizing step, the corrosion speed of the acid pickling solution is 10.16-15.24 mu m/h, and the deoxidizing time is 1-10 minutes.
5. The aluminum alloy hard anodizing process of claim 3, wherein: the ratio of the anode area of the hanger to the anode area of the aluminum alloy part is less than 10.
6. The aluminum alloy hard anodizing process of claim 3, wherein: after the aluminum alloy part is subjected to the hard anodizing step, the aluminum alloy part is also subjected to sealing treatment, wherein the sealing treatment is double sealing, and the method comprises the following steps:
first blocking with nickel acetate:
the components: ni (AC) 2 5-10g/L; temperature: 80-95 ℃; sealing time: 20-30 minutes; then passing through two times of pure water purificationWashing for 1-3 min;
then using dichromate capping:
the components: k 2 Cr 2 O 7 45-55g/l; temperature: 92-100 ℃; sealing time: 15-20 minutes;
then, the mixture is washed by two times of pure water, wherein each time lasts for 1-3 minutes.
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