CN113981500B - Oxalic acid anodizing process method for hard aluminum alloy shell part - Google Patents

Oxalic acid anodizing process method for hard aluminum alloy shell part Download PDF

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CN113981500B
CN113981500B CN202111496601.2A CN202111496601A CN113981500B CN 113981500 B CN113981500 B CN 113981500B CN 202111496601 A CN202111496601 A CN 202111496601A CN 113981500 B CN113981500 B CN 113981500B
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oxalic acid
oxidation
film layer
parts
oxide film
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CN113981500A (en
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史海峰
左文莉
茹怡
贺彪
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Shaanxi Baocheng Aviation Instrument Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/06Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/10Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/16Pretreatment, e.g. desmutting
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    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract

The oxalic acid anodizing process method of the hard aluminum alloy shell part is characterized in that a step boosting method is introduced to adjust and match the oxidation voltage, the oxidation time, the boosting speed and the frequency of an electrolytic cell, so that the three technical indexes of the appearance of an oxalic acid anodizing film layer formed on the surface of the shell part, the thickness of the film layer and the insulation resistance reach the standard acceptance requirements, the qualification rate is high, the problem of low oxalic acid anodizing qualification rate of the hard aluminum material shell is thoroughly solved, the problems of ablation of the film layer and part scrapping caused by black spots are greatly reduced, the consistency of the insulation resistance of different parts of the shell part is ensured, and the quality of the oxalic acid anodizing film layer of the shell part is greatly improved.

Description

Oxalic acid anodizing process method for hard aluminum alloy shell part
Technical Field
The invention belongs to the technical field of surface treatment, and particularly designs an oxalic acid anodizing process method for a hard aluminum alloy shell part.
Background
An oxalic acid anodizing process for aluminium and aluminium alloy features that the aluminium alloy part is put in the anode of oxalic acid type electrolyte and a certain current and voltage are applied to form an aluminium oxide film layer in a certain time, which is called oxalic acid anodizing; the parts materials suitable for oxalic acid anodization are mainly aluminum-magnesium series antirust aluminum alloys (5A 02, 5A 05), pure aluminum (1060, 1035) and the like, two series aluminum-copper series hard aluminum alloys (2A 12, 2A 11) are generally not suitable to be adopted, and as the hard aluminum alloy materials contain higher copper elements, the following problems exist in the oxalic acid anodization electrochemical reaction process: (1) the problems of black spots and film ablation easily occur on the surface of the part: according to the oxalic acid anodic oxidation process of pure aluminum and antirust aluminum alloy, the oxidation end point voltage of the oxalic acid anodic oxidation process needs to reach 110V-120V, the shell part is made of hard aluminum alloy and contains a large amount of copper elements, the copper elements are dissolved and separated out under high voltage, no film layer is locally formed on the separated part, the appearance of the shell part presents small and dense black spots, the black spot part is reduced in insulation resistance due to the fact that no film layer exists along with the continuous oxidation, and under the action of continuously increased voltage, an oxidation film cannot tolerate the passing of larger current, and the film layer is ablated; (2) the thickness and insulation resistance of the oxide film do not meet the technical requirements: the hard aluminum alloy is subjected to oxalic acid anodic oxidation, the film forming speed is low, a film layer caused by copper ion precipitation is discontinuous, the thickness of the film layer can only reach 10 mu M, the film layer is less than 200M omega under the condition of 500V when the insulation resistance of the film layer is tested, and meanwhile, the problem of poor stability of the insulation resistance exists at different parts of a shell part; the above defects will seriously affect the reliability of the fiber-optic gyroscope of the military products, so that improvement is necessary to improve the qualification rate and reliability of the products.
Disclosure of Invention
The technical problems solved by the invention are as follows: the oxalic acid anodic oxidation process method of the hard aluminum alloy shell part is characterized in that a step boosting method is introduced to adjust and match the oxidation voltage, the oxidation time, the boosting speed and the frequency of an electrolytic cell, so that three technical indexes of the appearance, the film thickness and the insulation resistance of an oxalic acid anodic oxidation film layer formed on the surface of the shell part meet the standard acceptance requirements, the qualification rate is high, the problems of low oxalic acid anodic oxidation qualification rate of the hard aluminum material shell are thoroughly solved, the problems of part scrapping caused by film ablation and black spots are greatly reduced, the consistency of the insulation resistances of different parts of the shell part is ensured, and the quality of the oxalic acid anodic oxidation film layer of the shell part is greatly improved.
The technical scheme adopted by the invention is as follows: the oxalic acid anodizing process method of the hard aluminum alloy shell part comprises the following steps:
1) And cleaning parts: in order to remove oil stains and emulsion on the surface of the part, the part is placed in a cleaning tank filled with clean aviation washing gasoline, the part is soaked for 20-30 min, all the surfaces of the part are scrubbed one by using a soft hairbrush, oil is removed by using the gasoline for 2-3 times according to the severity and the cleaning quantity of the oil stains on the part, the cleaned part is wiped by absorbent cotton, and the absorbent cotton has no black marks or the excess sundries are qualified for oil removal;
2) And drying in the air: placing the deoiled part indoors for natural drying until gasoline on the surface of the part is completely volatilized;
3) Selecting a clamp matched with the part according to the shape and size of the part, and clamping the parts on the clamp one by one with the hole openings facing upwards;
4) Anodic oxidation of oxalic acid: the prepared electrolyte is filled into an electrolytic cell, the part is placed into the electrolyte, and after the electrolytic cell is electrified, the applied oxidation voltage, the temperature of the electrolyte, the oxidation time, the boosting speed and the frequency are controlled by adopting a step boosting method, so that an oxalic acid anodic oxide film layer is formed on the surface of the part;
5) And sealing treatment: placing the part subjected to the anodic oxidation treatment of the oxalic acid into a tank filled with the solution, and standing for 25-30 min at the temperature of 85-100 ℃;
6) And (3) drying treatment: taking out the parts after the sealing treatment, standing for 25-30 min at 85-100 ℃ and drying;
7) And (3) checking: and (4) inspecting the appearance, the thickness and the insulation resistance of the oxalic acid anodic oxide film layer formed on the surface of the dried part.
In the step 4), the electrolyte is a solution prepared by mixing pure water and oxalic acid, wherein the oxalic acid concentration is 62-72 g/L.
In the step 4), the temperature of the electrolyte in the electrolytic cell is always kept at 12-18 ℃, and the oxalic acid anodizing time of the part in the electrolytic cell is 90 +/-5 min.
In the step 4), the step boosting method is a four-stage step boosting method, and includes the following specific steps:
boosting the pressure in the first stage: in the process from T1 to T3, the oxidation voltage of the electrolytic bath is increased from 0V to 10 +/-0.5V; wherein, the T1-T2 is the soft start process of the oxidation voltage of the electrolytic bath from 0V to 10 +/-0.5V, the soft start time is 1min, and the T2-T3 is the constant voltage maintaining process of the oxidation voltage of the electrolytic bath from 10 +/-0.5V, and the constant voltage maintaining time is 4 +/-1 min;
and a second stage of boosting: in the process of T3-T5, the oxidation voltage of the electrolytic bath is increased from 10 +/-0.5V to 30 +/-0.5V; wherein, the T3-T4 is the soft start process of the oxidation voltage of the electrolytic bath from 10 +/-0.5V to 30 +/-0.5V, the soft start time is 10min, the T4-T5 is the constant voltage maintaining process of the oxidation voltage of the electrolytic bath from 30 +/-0.5V, and the constant voltage maintaining time is 5 +/-1 min;
and (3) third stage boosting: in the process of T5-T7, the oxidation voltage of the electrolytic bath is increased from 30 +/-0.5V to 50 +/-0.5V; wherein, T5-T6 is a soft start process of the oxidation voltage of the electrolytic bath rising from 30 +/-0.5V to 50 +/-0.5V, the soft start time is 10min, T6-T7 is a constant voltage maintaining process of the oxidation voltage of the electrolytic bath rising to 50 +/-0.5V, and the constant voltage maintaining time is 15 +/-1 min;
and a fourth step of boosting: in the process from T7 to T9, the oxidation voltage of the electrolytic bath is increased from 50 plus or minus 0.5V to 70 plus or minus 0.5V; wherein, the soft start process from T7 to T8 when the oxidation voltage of the electrolytic cell rises from 50 +/-0.5V to 70 +/-0.5V is carried out, the soft start time is 10min, the constant voltage maintaining process from T8 to T9 when the oxidation voltage of the electrolytic cell rises to 70 +/-0.5V is carried out, and the constant voltage maintaining time is 35 +/-1 min.
In the step 5), the solution in the tank body is pure water.
In the step 7), the step of inspecting the oxalic acid anodic oxide film layer is as follows:
a) And appearance inspection of the oxalic acid anodic oxide film layer: under a daylight lamp, 100 percent of parts are visually checked at a position 450-500 mm away from naked eyes, the oxalic acid anode oxidation film layer is from milky white to grey white from semi-gloss to gloss, and is uniform and continuous without ablation, black spots, looseness, patches, obvious watermarks and local film layers;
b) And checking the thickness of the oxalic acid anodic oxide film layer: randomly extracting 3 parts per tank to measure the thickness of the oxalic acid anodic oxide film layer, and testing the thickness of the oxalic acid anodic oxide film layer to reach 10-20 mu m by using an eddy current method;
c) And checking the insulation resistance of the oxalic acid anodic oxidation film layer: and (3) randomly extracting parts in each tank to measure the film insulation resistance, and testing the film insulation resistance by using a digital megohmmeter, wherein the resistance value of the oxalic acid anodic oxide film insulation resistance is not less than 200M omega under the condition of 500V.
Compared with the prior art, the invention has the advantages that:
1. the technical scheme introduces a step boosting method to adjust and match the oxidation voltage, the oxidation time, the boosting speed and the frequency of the electrolytic cell, so that three technical indexes of the appearance, the film thickness and the insulation resistance of the oxalic acid anodic oxide film formed on the surface of the shell part reach the standard acceptance requirements, the qualification rate is high, and the problem of low oxalic acid anodic oxidation qualification rate of the shell made of the hard aluminum material is thoroughly solved;
2. the technical scheme optimizes the concentration of oxalic acid in the electrolyte and provides conditions for forming an oxalic acid anodic oxide film layer with the thickness meeting the requirements on the surface of the shell part;
3. according to the four-stage step boosting method, under the optimal oxidation voltage boosting speed, the problem of scrapping of parts caused by film ablation and black spots is greatly reduced, the consistency of insulation resistance at different parts of the shell part is ensured, the quality of the oxalic acid anode oxidation film of the shell part is greatly improved, and the stability of the insulation resistance of the oxalic acid anode oxidation film is good.
Drawings
FIG. 1 is a pressure-increasing step diagram of the oxalic acid anodizing process of the present invention.
Detailed Description
In the following, an embodiment of the present invention is described with reference to fig. 1, so as to clearly and completely describe the technical solution, it is obvious that the described embodiment is only a part of the embodiment of the present invention, and not a whole embodiment.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
The oxalic acid anodizing process method of the hard aluminum alloy shell part comprises the following steps:
1) And cleaning parts: in order to remove oil stains and emulsion on the surface of the part, the part is placed in a cleaning tank filled with clean aviation washing gasoline, the part is soaked for 20-30 min, all the surfaces of the part are scrubbed one by using a soft hairbrush, oil is removed by using the gasoline for 2-3 times according to the severity and the cleaning quantity of the oil stains on the part, the cleaned part is wiped by absorbent cotton, and the absorbent cotton has no black marks or the excess sundries are qualified for oil removal;
2) And drying in the air: placing the deoiled part indoors for natural drying until gasoline on the surface of the part is completely volatilized;
3) Selecting a clamp matched with the part according to the shape and size of the part, and clamping the part on the clamp one by one with the hole openings facing upwards;
4) Anodic oxidation of oxalic acid: the prepared electrolyte is filled into an electrolytic cell, the part is placed into the electrolyte, and after the electrolytic cell is electrified, the applied oxidation voltage, the temperature of the electrolyte, the oxidation time, the boosting speed and the frequency are controlled by adopting a step boosting method, so that an oxalic acid anodic oxide film layer is formed on the surface of the part; specifically, the electrolyte is a solution prepared by mixing pure water and oxalic acid, wherein the oxalic acid concentration is 62-72 g/L; specifically, the temperature of the electrolyte in the electrolytic cell is always kept at 12-18 ℃, and the oxalic acid anodizing time of parts in the electrolytic cell is 90 +/-5 min; in the technical characteristics, the thickness and the insulativity of the oxalic acid anodic oxide film layer are directly influenced by the concentration of oxalic acid, and the thick bottom of the oxalic acid anodic oxide film layer is low due to the excessively low concentration of oxalic acid, so that the insulativity (the electric resistance) of the oxalic acid anodic oxide film layer cannot meet the requirement, therefore, the solution with the concentration of oxalic acid of 62-72 g/L is preferred in the scheme; optimizing the concentration of oxalic acid in the electrolyte, and providing conditions for forming an oxalic acid anodic oxide film layer with the thickness meeting the requirements on the surface of the shell part;
specifically, the step boost method is a four-stage step boost method, as shown in fig. 1, and includes the following specific steps:
boosting the pressure in the first stage: in the process from T1 to T3, the oxidation voltage of the electrolytic bath is increased from 0V to 10V; wherein, T1-T2 is a soft start process of increasing the oxidation voltage of the electrolytic cell from 0V to 10V, the soft start time is 1min, T2-T3 is a constant voltage maintaining process of increasing the oxidation voltage of the electrolytic cell to 10V, and the constant voltage maintaining time is 4min;
and a second stage of boosting: in the process from T3 to T5, the oxidation voltage of the electrolytic bath is increased from 10V to 30V; wherein, T3-T4 is a soft start process of the oxidation voltage of the electrolytic cell rising from 10V to 30V, the soft start time is 10min, T4-T5 is a constant voltage maintaining process of the oxidation voltage of the electrolytic cell rising to 30V, and the constant voltage maintaining time is 5min;
and (3) third stage boosting: in the process from T5 to T7, the oxidation voltage of the electrolytic bath is increased from 30V to 50; wherein, T5-T6 is a soft start process of the oxidation voltage of the electrolytic cell rising from 30V to 50V, the soft start time is 10min, T6-T7 is a constant voltage maintaining process of the oxidation voltage of the electrolytic cell rising to 50V, and the constant voltage maintaining time is 15min;
and a fourth step of boosting: in the process from T7 to T9, the oxidation voltage of the electrolytic bath is increased from 50V to 70V; wherein, T7-T8 is a soft start process of increasing the oxidation voltage of the electrolytic cell from 50V to 70V, the soft start time is 10min, T8-T9 is a constant voltage maintaining process of increasing the oxidation voltage of the electrolytic cell to 70 +/-0.5V, and the constant voltage maintaining time is 35min;
the introduction of the four-stage step boosting method effectively reduces the oxidation end point voltage in the traditional process to 110V-120V to 70V, thereby effectively solving the problem of copper element dissolution and precipitation under high voltage, and the copper element can not be dissolved and precipitated, so that the quality of the oxalic acid anodic oxide film layer is ensured, the appearance of the oxalic acid anodic oxide film layer can not have dense black spots, the insulation resistance of the oxalic acid anodic oxide film layer is improved, and the oxalic acid anodic oxide film layer is prevented from being ablated; moreover, in the process of carrying out oxalic acid anodic oxidation, if the oxidation voltage rises too fast, the surface of the initially formed oxalic acid anodic oxide film layer can be ablated and broken down, and parts are scrapped; if the oxidation voltage is too low, the oxidation speed is slow, and the film forming speed is reduced, the thickness of the oxalic acid anodic oxidation film layer and the corrosion resistance of the surface of the film layer can not meet the requirements;
5) And sealing treatment: placing the part subjected to the anodic oxidation treatment of the oxalic acid into a tank filled with the solution, and standing for 25-30 min at the temperature of 85-100 ℃; specifically, the solution in the tank body is pure water;
6) And (3) drying treatment: taking out the parts after the sealing treatment, standing for 25-30 min at 85-100 ℃ and drying;
7) And (3) checking: inspecting the appearance, the thickness and the insulation resistance of an oxalic acid anodic oxide film layer formed on the surface of the dried part; specifically, the detection steps of the oxalic acid anodic oxide film layer are as follows:
a) And appearance inspection of the oxalic acid anodic oxide film layer: under a 40W fluorescent lamp or natural scattered light, 100 percent of parts are visually inspected at a position 450-500 mm away from naked eyes, the oxalic acid anode oxidation film layer is from milky white to grey white with semi-gloss to gloss, is uniform and continuous, and has no ablation, black spots, looseness, patches, obvious watermarks or no film layer locally;
b) And checking the thickness of the oxalic acid anodic oxide film layer: randomly extracting 3 parts per tank to measure the thickness of the oxalic acid anodic oxide film layer, and testing the thickness of the oxalic acid anodic oxide film layer to reach 10-20 mu m by using an eddy current method;
c) And checking the insulation resistance of the oxalic acid anodic oxidation film layer: and (3) parts are arbitrarily extracted from each tank to measure the film insulation resistance, the film insulation resistance is measured by using a digital megohmmeter, and the resistance value of the oxalic acid anodic oxide film insulation resistance is not less than 200M omega under the condition of 500V.
Taking a hard aluminum 2A12T4 shell part as an example, the thickness of an oxalic acid anodic oxide film layer is required to be 10-20 mu M, and the insulation resistance is not less than 200 MOmega under the condition of 500V;
by adopting the oxalic acid anodizing process method of the duralumin alloy shell part with the optimal technical parameters, the production and delivery of 20 batches of 5795 shell parts in oxalic acid anodizing are completed in sequence, the three technical indexes of the appearance, the thickness and the insulation resistance of the oxalic acid anodizing film layer are checked and accepted according to the customer standard, and the qualification rate reaches 99.84%. The method thoroughly solves the problems of low oxalic acid anodic oxidation yield of the shell made of the duralumin material and part scrap caused by ablation of the film and black spots.
TABLE 1 casing oxalic acid anodic oxidation test record table
Figure BDA0003400947550000081
Figure BDA0003400947550000091
The technical scheme introduces a step boosting method to adjust and match the oxidation voltage, the oxidation time, the boosting speed and the frequency of the electrolytic cell, so that three technical indexes of the appearance, the film thickness and the insulation resistance of the oxalic acid anodic oxide film formed on the surface of the shell part reach the standard acceptance requirements, the qualification rate is high, and the problem of low oxalic acid anodic oxidation qualification rate of the shell made of the hard aluminum material is thoroughly solved; the four-stage step boosting method has the advantages that under the optimal oxidation voltage boosting speed, the problem of part scrapping caused by film ablation and black spots is greatly reduced, the consistency of insulation resistance of different parts of a shell part is guaranteed, the quality of an oxalic acid anode oxidation film layer of the shell part is greatly improved, and the stability of the insulation resistance of the oxalic acid anode oxidation film layer is good.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (5)

1. The oxalic acid anodic oxidation process method of the hard aluminum alloy shell part is characterized by comprising the following steps of:
1) And cleaning parts: in order to remove oil stains and emulsion on the surfaces of parts, the parts are placed in a cleaning tank filled with clean aviation washing gasoline, the parts are soaked for 20-30 min, a soft brush is used for scrubbing all the surfaces of the parts one by one, oil is removed for 2-3 times by the gasoline according to the severity and cleaning quantity of the oil stains on the parts, the cleaned parts are wiped by absorbent cotton, and the absorbent cotton has no black marks or redundant sundries and is qualified for oil removal;
2) And drying in the air: placing the deoiled part indoors for natural drying until gasoline on the surface of the part is completely volatilized;
3) Selecting a clamp matched with the part according to the shape and size of the part, and clamping the parts on the clamp one by one with the hole openings facing upwards;
4) Anodic oxidation of oxalic acid: the prepared electrolyte is filled into an electrolytic cell, the part is placed into the electrolyte, and after the electrolytic cell is electrified, the applied oxidation voltage, the temperature of the electrolyte, the oxidation time, the boosting speed and the frequency are controlled by adopting a step boosting method, so that an oxalic acid anodic oxide film layer is formed on the surface of the part;
the step boosting method is a four-section step boosting method and comprises the following specific steps:
boosting the pressure in the first stage: in the process from T1 to T3, the oxidation voltage of the electrolytic bath is increased from 0V to 10 +/-0.5V; wherein, the process from T1 to T2 is the soft start process of the oxidation voltage of the electrolytic cell which is increased from 0V to 10 +/-0.5V, the soft start time is 1min, and the process from T2 to T3 is the constant voltage maintaining process of the oxidation voltage of the electrolytic cell which is increased to 10 +/-0.5V, and the constant voltage maintaining time is 4 +/-1 min;
and a second stage of boosting: in the process of T3-T5, the oxidation voltage of the electrolytic bath is increased from 10 +/-0.5V to 30 +/-0.5V; wherein, the process from T3 to T4 is the soft start process of the oxidation voltage of the electrolytic bath from 10 plus or minus 0.5V to 30 plus or minus 0.5V, the soft start time is 10min, the process from T4 to T5 is the constant voltage maintaining process of the oxidation voltage of the electrolytic bath after the oxidation voltage of the electrolytic bath rises to 30 plus or minus 0.5V, and the constant voltage maintaining time is 5 plus or minus 1min;
and a third stage of pressure boosting: in the process from T5 to T7, the oxidation voltage of the electrolytic bath is increased from 30 plus or minus 0.5V to 50 plus or minus 0.5V; wherein, T5-T6 is a soft start process of the oxidation voltage of the electrolytic bath rising from 30 +/-0.5V to 50 +/-0.5V, the soft start time is 10min, T6-T7 is a constant voltage maintaining process of the oxidation voltage of the electrolytic bath rising to 50 +/-0.5V, and the constant voltage maintaining time is 15 +/-1 min;
and a fourth step of boosting: in the process from T7 to T9, the oxidation voltage of the electrolytic bath is increased from 50 +/-0.5V to 70 +/-0.5V; wherein, the process from T7 to T8 is the soft start process of the oxidation voltage of the electrolytic bath from 50 +/-0.5V to 70 +/-0.5V, the soft start time is 10min, the process from T8 to T9 is the constant voltage maintaining process of the oxidation voltage of the electrolytic bath from 70 +/-0.5V, and the constant voltage maintaining time is 35 +/-1 min;
5) And sealing treatment: placing the part subjected to the anodic oxidation treatment of the oxalic acid into a tank filled with the solution, and standing for 25-30 min at the temperature of 85-100 ℃;
6) And (3) drying treatment: taking out the parts after the sealing treatment, standing for 25-30 min at 85-100 ℃ and drying;
7) And (3) checking: and (4) inspecting the appearance, the thickness and the insulation resistance of the oxalic acid anodic oxide film layer formed on the surface of the dried part.
2. The oxalic acid anodizing process method of the duralumin alloy case part as claimed in claim 1, wherein: in the step 4), the electrolyte is a solution prepared by mixing pure water and oxalic acid, wherein the oxalic acid concentration is 62-72 g/L.
3. The oxalic acid anodizing process method of the duralumin alloy case part as claimed in claim 1, wherein: in the step 4), the temperature of the electrolyte in the electrolytic cell is always kept at 12-18 ℃, and the oxalic acid anodizing time of the part in the electrolytic cell is 90 +/-5 min.
4. An oxalic acid anodizing process for a duralumin alloy case part according to claim 1, 2 or 3, wherein: in the step 5), the solution in the tank body is pure water.
5. The oxalic acid anodizing process of a duralumin alloy case part as claimed in claim 1, wherein: in the step 7), the inspection step of the oxalic acid anodic oxide film layer is as follows:
a) And appearance inspection of the oxalic acid anodic oxide film layer: under a daylight lamp, 100 percent of parts are visually checked at a position 450-500 mm away from naked eyes, the oxalic acid anode oxidation film layer is from milky white to grey white from semi-gloss to gloss, and is uniform and continuous without ablation, black spots, looseness, patches, obvious watermarks and local film layers;
b) And checking the thickness of the oxalic acid anodic oxide film layer: randomly extracting 3 parts per tank to measure the thickness of the oxalic acid anodic oxide film layer, and testing the thickness of the oxalic acid anodic oxide film layer to reach 10-20 mu m by using an eddy current method;
c) And checking the insulation resistance of the oxalic acid anodic oxidation film layer: and (3) randomly extracting parts in each tank to measure the film insulation resistance, and testing the film insulation resistance by using a digital megohmmeter, wherein the resistance value of the oxalic acid anodic oxide film insulation resistance is not less than 200M omega under the condition of 500V.
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