CN113046810A - 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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- CN113046810A CN113046810A CN202110285706.7A CN202110285706A CN113046810A CN 113046810 A CN113046810 A CN 113046810A CN 202110285706 A CN202110285706 A CN 202110285706A CN 113046810 A CN113046810 A CN 113046810A
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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 voltage control mode; referring to the known comparative example, the current value required for the part to reach the target film thickness was deduced 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 aviation aluminum alloy materials such as 6061, 2024 and 7075.
Background
The anodic oxidation of aluminum refers to a process of generating an oxide film on the surface of aluminum or aluminum alloy in 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 the oxide film layer continuously increases 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 given 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 voltage control mode:
first stage L1: the voltage is slowly increased for 5 minutes until the target voltage U is reached1Recording the target voltage U reached by hard anodic oxidation1Current of time I1；
Second stage L2: applying a constant target voltage U1Keeping the time for 1 minute, setting the hard anodic oxidation current I2Said current I1And current I2The ratio of (A) to (B) is 1: 3;
third stage L3: slowly raising current to current I2The slow rising time is 10 minutes;
fourth stage L4: at a constant current I2Carrying out hard anodic oxidation, wherein the retention time is increased along with the thickness of the target film;
the target voltage U1The 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 hanger4；
M3: the anodic oxidation pressurization process of the reference comprises two stages:
the first stage is as follows: slowly raising current to current I4The slow rising time is 15 minutes, and the current I is set3Current I of3And current I4Is 1:3, and records the voltage value U at the moment2；
And a second stage: maintaining a constant current I4The retention time increases with the required film thickness.
M4: repeating the above M1-M3 for multiple times to obtain multiple groups of voltage values U2Calculating a voltage value U2To obtain the target voltage U1。
In the above technical solution, the current density of the fourth stage L4 is 2.8-3.2A/dm2。
In the above technical solution, other parameters of the sulfuric acid electrolyte:
temperature of the electrolyte: -2 ℃ to 0 ℃; h2SO4 220—230g/L；Al3+＜20g/L。
In the above technical solution, the target voltage U of the first stage L1 and the second stage L21Is 17-19V.
In the technical scheme, the part is made of 6061 aluminum alloy and U117.8-18.2V; the material of the parts is 2024 aluminum alloy, U117.0-17.5V; the material of the part is 7075 aluminum alloy and U1Is 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;
hard anodizing the aluminum alloy member after the pretreatment according to the aluminum alloy hard anodizing pressure method as set forth in any one of claims 1 to 5.
In the above technical solution, the pretreatment comprises the following steps:
s1 precleaning: 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 degreasing: 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:
HNO3 75-160g/l，CrO3 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 technical scheme, the area ratio of the hanger to the anode of the aluminum alloy part is less than 10: 1.
In the technical scheme, 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)25-10 g/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: k2Cr2O745-55 g/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.
In the field of anodic oxidation of aviation parts, the inventors generally encounter irregular aluminum alloy parts without three-dimensional drawings, cannot accurately calculate the oxidation area of the part in the early stage, and need to spend a great deal of effort on calibration of the anodic oxidation process of new parts. 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, 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, the error of finished product film thickness caused by the error of oxidation area measurement is 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 the following steps:
s1 precleaning: 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 degreasing: because the aluminum alloy has amphipathy and is different from other metals, the addition amount of alkali is limited, and a weak 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:
HNO3 75-160g/l，CrO3 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 voltage control mode:
the first stage is as follows: the voltage is slowly increased for 5 minutes until the target voltage U is reached1Recording the current I when the hard anodic oxidation reaches the target voltage of 18V1；
And a second stage: applying a constant target voltage U1Keeping the time for 1 minute, setting the hard anodic oxidation current I2Current I of1And current I21/3;
and a third stage: slowly increasing current to I2The slow rising time is 10 minutes;
a fourth stage: the hard anodic oxidation is carried out at a constant current, and the retention time is increased according to the required film thickness.
Other parameters of the hard anodizing step:
temperature of the electrolyte: -2 ℃ to 0 ℃; h2SO4Concentration: 220-230 g/L; al (Al)3+Concentration: is less than 20 g/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 step1Is determined by parallel test before measuring sample, the parallel test adopts reference substance of the same material as the sample to be measured, and preferably adopts oxidized surfaceHard anodizing the regular part easy to calculate in the same electrolyte; the voltage control method is constant current method, and the current density is set to be 2.8A/dm2～3.2A/dm2B, carrying out the following steps 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 hanger4. 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 I4The slow rising time is 15 minutes, and the current I is set3Current I of3And current I4Is 1/3, so that the electrolyte is in the oxidation current I3The current density is kept at 0.9A/dm2～1.1A/dm2And recording the voltage value at the moment, and taking the voltage value as the target voltage U of the sample to be tested1(ii) a And a second stage: maintaining a constant current I4The 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/dm2～3.2A/dm2And in the stage, the growth rate of the oxide film is 0.95-1.05 μm/min.
In order to reduce the target voltage U1Error, 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 U1And is 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 U1Is 17.0-17.5V.
The hard anode oxidation step adopts a four-section voltage control mode:
the first stage is as follows: the voltage is slowly increased for 5 minutes until the target voltage U is reached1Recording the current I when the hard anodic oxidation reaches the target voltage of 18V1；
And a second stage: applying a constant target voltage U1Keeping the time for 1 minute, setting the hard anodic oxidation current I2Current I of1And current I21/3;
and a third stage: slowly increasing current to I2The slow rising time is 10 minutes;
a fourth stage: the hard anodic oxidation is carried out at a constant current, and the retention 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 voltage control mode:
the first stage is as follows: the voltage is slowly increased for 5 minutes until the target voltage U is reached1Recording the current I when the hard anodic oxidation reaches the target voltage of 18V1；
And a second stage: applying a constant target voltage U1Keeping the time for 1 minute, setting the hard anodic oxidation current I2Current I of1And current I21/3;
and a third stage: slowly increasing current to I2The slow rising time is 10 minutes;
a fourth stage: the hard anodic oxidation is carried out at a constant current, and the retention 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 measured: 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)25-10 g/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: k2Cr2O745-55 g/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 (10)
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 voltage control mode:
first stage L1: the voltage is slowly increased for 5 minutes until the target voltage U is reached1Recording the target voltage U reached by hard anodic oxidation1Current of time I1；
Second stage L2: applying a constant target voltage U1Keeping the time for 1 minute, setting the hard anodic oxidation current I2Said current I1And current I2The ratio of (A) to (B) is 1: 3;
third stage L3: slowly raising current to current I2The slow rising time is 10 minutes;
fourth stage L4: at a constant current I2Carrying out hard anodic oxidation, wherein the retention time is increased along with the thickness of the target film;
the target voltage U1The 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 hanger4；
M3: the anodic oxidation pressurization process of the reference comprises two stages:
the first stage is as follows: slowly raising current to current I4The slow rising time is 15 minutes, and the current I is set3Current I of3And current I4Is 1:3, and records the voltage value U at the moment2；
And a second stage: maintaining a constant current I4The retention time increases with the required film thickness.
M4: repeating the above M1-M3 for multiple times to obtain multiple groups of voltage values U2Calculating a voltage value U2To obtain the target voltage U1。
2. The aluminum alloy hard anodizing pressure method of claim 1,the method is characterized in that: the current density of the fourth stage L4 is 2.8-3.2A/dm2。
3. The aluminum alloy hard anodizing pressure process of claim 1, wherein: other parameters of the sulfuric acid electrolyte:
temperature of the electrolyte: -2 ℃ to 0 ℃; h2SO4 220—230g/L；Al3+＜20g/L。
4. The aluminum alloy hard anodizing pressure process of claim 3, wherein: target voltage U of the first stage L1 and the second stage L21Is 17-19V.
5. The aluminum alloy hard anodizing pressure process of claim 4, wherein: the part material is 6061 aluminum alloy, U117.8-18.2V; the material of the parts is 2024 aluminum alloy, U117.0-17.5V; the material of the part is 7075 aluminum alloy and U1Is 18.5-19V.
6. 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 any one of claims 1 to 5.
7. The aluminum alloy hard anodizing process of claim 6, wherein: the pretreatment comprises the following steps:
s1 precleaning: 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 degreasing: 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:
HNO3 75-160g/l，CrO3 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.
8. The aluminum alloy hard anodizing process of claim 7, wherein: the corrosion speed of the acid washing solution in the step of S4 acid washing and deoxidation is 10.16-15.24 μm/h, and the deoxidation time is 1-10 minutes.
9. The aluminum alloy hard anodizing process of claim 7, wherein: the ratio of the anode area of the hanger to the anode area of the aluminum alloy part is less than 10: 1.
10. The aluminum alloy hard anodizing process of claim 7, 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)25-10 g/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: k2Cr2O745-55 g/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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