CN110607549A - Anti-static hard anodic oxidation process - Google Patents

Anti-static hard anodic oxidation process Download PDF

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Publication number
CN110607549A
CN110607549A CN201910767814.0A CN201910767814A CN110607549A CN 110607549 A CN110607549 A CN 110607549A CN 201910767814 A CN201910767814 A CN 201910767814A CN 110607549 A CN110607549 A CN 110607549A
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China
Prior art keywords
washing
water
temperature
acid
time
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Chinese (zh)
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黎纠
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Dijing Semiconductor Technology (suzhou) Co Ltd
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Dijing Semiconductor Technology (suzhou) Co Ltd
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Priority to CN201910767814.0A priority Critical patent/CN110607549A/en
Publication of CN110607549A publication Critical patent/CN110607549A/en
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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
    • C25D11/06Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/08Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic 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
    • C25D11/06Anodisation 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

Abstract

The invention discloses an anti-static hard anodizing process, and belongs to the field of part anodizing. An antistatic hard anodizing process comprises the following steps: hanging up; degreasing, namely putting the parts into degreasing liquid for degreasing, wherein the degreasing time is 5-10 min and the temperature is 48-52 ℃; the concentration of the solution is 5 percent; c, after the surfaces of the parts in the step B are free of grease, marks and scratches and surface water is not gathered, starting overflow, enabling the water quality resistivity to be larger than or equal to 200k omega, lifting the parts out of the liquid level of the washing tank in the step C, and carrying out fan-shaped spray washing on the parts from top to bottom, wherein the washing time is 60-90s, and the temperature is 20-30 ℃; the invention can realize the anti-static effect, improve the corrosion resistance and improve the breakdown voltage.

Description

Anti-static hard anodic oxidation process
Technical Field
The invention relates to the technical field of anodic oxidation of parts, in particular to an anti-static hard anodic oxidation process.
Background
Anodic oxidation, electrochemical oxidation of metal or alloy, and formation of an oxide film on the aluminum product anode under the action of an external current in a corresponding electrolyte and under specific process conditions.
Application No. 201310354018.7 in the prior art, and 2013-11-20 discloses an anodic oxidation process, which comprises the steps of: pretreatment, anodic oxidation, integral dyeing and post-treatment; further comprising the step between the step of anodizing and the step of post-treating: printing operation: and (3) single-color printing or multi-color printing, wherein the dyeing material is filled in the pores of the oxide film layer. According to the anodic oxidation process provided by the invention, an oxide film layer is formed on the surface of the metal product through an anodic oxidation procedure, and the oxide film layer has pores for generating adsorption force on the dye. Adding dyes with various colors to a specific position on the surface of the metal product in a printing mode, and adsorbing the dyes through pores to complete the addition of the various colors on the metal product; the anodic oxidation process provided by the invention has the advantages that various colors are added on the metal product, the metal product is prevented from being singly colored, the dye is added on the surface of the metal product by printing and is adsorbed for coloring, the processing method is simple and convenient, the production cost is greatly reduced, and the practicability is higher.
Application number 201611197261.2 in the prior art, and 2018-06-29 disclose an aluminum alloy anodic oxidation process, which comprises the following steps of degreasing, namely putting an aluminum alloy workpiece into a sulfuric acid tank for degreasing, carrying out alkali washing, namely putting the degreased aluminum alloy workpiece into a sodium hydroxide solution for alkali washing, carrying out first water washing, namely washing the aluminum alloy workpiece after alkali washing with tap water, carrying out chemical polishing, namely putting the washed aluminum alloy workpiece into a polishing solution for chemical polishing, carrying out second water washing, namely washing the polished aluminum alloy workpiece with tap water until the pH value of a washing solution is 5 ~ 6, putting the washed aluminum alloy workpiece into an anodic oxidation solution for direct-current anodic oxidation, coloring, namely putting the anodized aluminum alloy workpiece into a chemical dye solution for coloring, and sealing, namely putting the colored aluminum alloy workpiece into a sealing agent solution for sealing, wherein an oxide film is thicker, high in hardness, good in wear resistance, good in corrosion resistance, good in heat insulation performance, large in resistivity and good in insulating performance.
However, in the aluminum alloy anode oxide film prepared by the oxidation process in the prior art, 1, the surface of the oxide film has electrostatic action; 2. common sulfuric acid is adopted as electrolyte, and the corrosion resistance of an oxide film is poor; 3. the breakdown voltage is low.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides an anti-static hard anodizing process.
In order to achieve the purpose, the invention adopts the following technical scheme:
an antistatic hard anodizing process comprises the following steps:
A. hanging up;
B. degreasing
Degreasing the part in degreasing fluid for 5-10 min at 48-52 ℃; the concentration of the solution is 5 percent;
C. first washing with water
After the surfaces of the parts in the step B are free of grease, marks and scratches and surface water is not accumulated, starting overflow, enabling the water quality resistivity to be larger than or equal to 200k omega, lifting the parts out of the liquid level of the washing tank in the step C, and carrying out fan-shaped spray washing on the parts from top to bottom, wherein the washing time is 60-90s, and the temperature is 20-30 ℃;
D. alkali bite
Putting the part into a sodium hydroxide solution for alkali biting, wherein the alkali biting time is 15-30 s, the temperature is 40-50 ℃, hanging the part subjected to alkali biting out of the liquid surface of an alkali biting tank in the step D, spraying water to the part from top to bottom, and performing enhanced water spraying at blind holes, gaps and threads of the part;
E. second washing with water
E, starting overflow, lifting the parts out of the liquid level of the rinsing bath in the step E, and carrying out fan-shaped spray washing on the parts from top to bottom, wherein the water washing time is 60-90s, and the temperature is 20-30 ℃;
F. acid etching
Putting the part into an acid etching solution, wherein the acid etching time is 8-12 s, and the temperature is 15-25 ℃; when the part is discharged from the pickling tank, the part is sprayed in a fan shape from top to bottom, and water is sprayed at blind holes, gaps and threads of the part in an enhanced manner, so that the part is prevented from being corroded by acid to generate flow marks;
G. third time of water washing
Starting overflow, wherein the water quality is more than or equal to 200k omega, completely immersing the part into water, lifting twice through a crane to carry out enhanced washing, after the part is lifted out of the water level, carrying out fan-shaped spray washing on the part from top to bottom, wherein the washing time is 30-60 s, and the temperature is 20-30 ℃;
H. stripping film
Placing the part into a film stripping solution, wherein the film stripping time is 3-5 min, starting aeration, the temperature is 15-25 ℃, when the part is taken out of a film stripping groove, carrying out fan-shaped spray washing on the part from top to bottom, and carrying out enhanced water spraying at blind holes, gaps and threads of the part;
I. the fourth time of water washing
Starting overflow, wherein the water quality is more than or equal to 200k omega, completely immersing the part into water, lifting twice through a crane to carry out enhanced washing, after the part is lifted out of the water level, carrying out fan-shaped spray washing on the part from top to bottom, wherein the washing time is 60-90s, and the temperature is 15-25 ℃;
J. oxidation by oxygen
Placing the part into a tank containing sulfuric acid and oxalic acid tank liquor, shaking up and down and left and right to ensure that the part is fully contacted with the mixed acid tank liquor without accumulated gas, wherein the concentration of the sulfuric acid and oxalic acid tank liquor reaches 2g/L and 50g/L, the control voltage is 58V-60V, the peak current density is 2A/d square meter, the valley current density is 1A/d square meter, the peak value and valley value of the current are set according to the anode area S of the part, the boosting time is 5min-10min, the current value = current density multiplied by the anode area S of the part, the thickness of the film is 30-35um, the recording time is kept, and the temperature is 5 ℃;
K. fifth washing with water
Starting overflow, wherein the water quality is more than or equal to 200k omega, completely immersing the part into water, lifting twice through a crane to carry out enhanced washing, after the part is lifted out of the water level, carrying out fan-shaped spray washing on the part from top to bottom, wherein the washing time is 60-90s, and the temperature is 15-25 ℃;
l, acid washing
Immersing the part into a nitric acid solution with the concentration of 10 percent for 2-3min, and removing active wave electrons on an oxide film on the surface of the workpiece;
m, sixth washing
Starting overflow, wherein the water quality is more than or equal to 200k omega, completely immersing the part into water, lifting twice through a crane to carry out enhanced washing, after the part is lifted out of the water level, carrying out fan-shaped spray washing on the part from top to bottom, wherein the washing time is 60-90s, and the temperature is 15-25 ℃;
sealing holes by N and nickel acetate; the specific hole sealing method is to measure the film thickness by using an oxide film eddy current thickness meter, the hole sealing rate is calculated according to 2min/um, the water quality is more than or equal to 450k omega cm, the temperature is 80 ℃, the concentration of hole sealing liquid is 5g/L, and the PH value is 5.5-6.5;
o, seventh water washing
Completely immersing the part in water, lifting twice by a crane to carry out enhanced washing, after the part is lifted out of the water level, carrying out fan-shaped spray washing on the part from top to bottom, wherein the washing time is 60-90 s;
p, eighth water washing
Completely immersing the part in water, lifting twice by a crane to perform reinforced washing, after the part is lifted out of the water level, performing fan-shaped spray washing on the part from top to bottom, and spraying water at each blind hole, gap and thread for 3-5 s;
q, drying;
r, lower hanger
Placing the part on a lower hanging bracket;
s, washing with hot water;
t, drying by blowing again:
u, baking;
and V, packaging and adopting an anti-static PE bag for packaging.
Preferably, a titanium clip or a titanium screw is used for hanging in the step A.
Preferably, the degreasing fluid in the step B is a weak alkaline degreasing fluid, and the main component is sodium carbonate or sodium silicate or sodium dodecyl diphenyl ether disulfonate.
Preferably, the concentration of the sodium hydroxide in the step D is 50g/L, and 5g/L of analytically pure sodium gluconate is added in the preparation process of the sodium hydroxide.
Preferably, the acid etching is performed by a mixed acid solution of nitric acid and hydrofluoric acid in the step F, and the concentrations of the nitric acid and the hydrofluoric acid are 20% and 2%, respectively.
Preferably, in the step H, the main component of the stripping solution is ferric sulfate or phosphoric acid or sulfuric acid, and the concentration is 20%.
Preferably, in the fourth water washing, the fifth water washing and the sixth water washing, after the water washing, manual water spraying is preferably carried out at each blind hole, gap and thread, and the water spraying time is 3-5 s.
Preferably, the specific hole sealing method in the step N is to measure the film thickness by using an oxide film eddy current thickness meter, the hole sealing rate is calculated according to 2min/um, the water quality is more than or equal to 450k omega cm, the temperature is 80 ℃, the concentration of the hole sealing liquid is 5g/L, and the PH value is 5.5-6.5.
Preferably, the blow-drying method in the step Q is to blow-dry the part by using dry nitrogen air, and the blow-drying method in the step T is to blow-dry the part by using nitrogen after filtering by using a 0.01 μm filter, and then blow-dry the part by filling nitrogen, and increase the amount of air blown at the blind holes, gaps and threads.
Preferably, the baking method in the step U is that a baking oven is filled with nitrogen, the flow rate of the nitrogen in the baking oven is set to be 30-40L/min, the part is placed in the baking oven for 20-40 min, and the temperature in the baking oven is 75-85 ℃.
Compared with the prior art, the invention provides an anti-static hard anodizing process, which has the following beneficial effects:
1. according to the anti-static hard anodic oxidation process, 1, no electrostatic action exists on the surface of an oxide film, 2, sulfuric acid and oxalic acid are used as electrolytes, the corrosion resistance of the oxide film is enhanced, 3, the breakdown voltage is increased, 4, the sulfuric acid and oxalic acid tank liquor are used for oxidation in a tank body, the control voltage is 58V-60V, the peak current density is 2A/d square meter, the valley current density is 1A/d square meter, the peak value and the valley value of the current are set according to the anode area S of a part, the boosting time is 5min-10min, the current value = current density multiplied by the anode area S of the part, the film thickness is 30-35um, the wear resistance of the workpiece is increased, the corrosion resistance of the workpiece is increased, the decoration of the workpiece is increased, the insulation property and the hardness of the workpiece;
2. the anti-static hard anodizing process can realize the anti-static effect, improve the corrosion resistance and improve the breakdown voltage;
3. the anti-static hard anodizing process avoids the damage to equipment such as a finished product machine type and the like caused by static electricity generated at the use end after anodizing;
4. according to the anti-static hard anodic oxidation process, a titanium clamp and a titanium screw are adopted during hanging, so that good electric conduction of parts is ensured;
5. the main component of the anti-static hard anodic oxidation process is sodium carbonate or sodium silicate or sodium dodecyl diphenyl ether disulfonate, degreasing is carried out in the alkalescent degreasing solution, and oil stains and impurities on the surface of a workpiece are mainly removed;
6. according to the anti-static hard anodic oxidation process, a part is placed in a stripping solution, the main component of the solution is ferric sulfate, phosphoric acid or sulfuric acid, the volume of the solution is 20%, and residual iron ions and the like on the part are prevented from being brought into an oxidation tank to pollute oxidation tank liquid.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example (b):
an antistatic hard anodizing process comprises the following steps:
A. hanging up; when hanging, a titanium clamp and a titanium screw are adopted to ensure good electric conduction of the part;
B. degreasing
Degreasing the part in degreasing fluid for 5-10 min at 48-52 ℃; the concentration of the solution is 5 percent; the alkalescent degreasing fluid mainly comprises sodium carbonate or sodium silicate or sodium dodecyl diphenyl ether disulfonate, and is used for degreasing, so that oil stains and impurities on the surface of a workpiece are mainly removed.
C. First washing with water
After the surfaces of the parts in the step B are free of grease, marks and scratches and surface water is not accumulated, starting overflow, enabling the water quality resistivity to be larger than or equal to 200k omega, lifting the parts out of the liquid level of the washing tank in the step C, and carrying out fan-shaped spray washing on the parts from top to bottom, wherein the washing time is 60-90s, and the temperature is 20-30 ℃;
D. alkali bite
Putting the part into a sodium hydroxide solution for alkali biting, wherein the concentration of the sodium hydroxide is 50g/L, 5g/L of analytically pure sodium gluconate needs to be added in the preparation process of the sodium hydroxide, the alkali biting time is 15-30 s, the temperature is 40-50 ℃, the part subjected to alkali biting is lifted out of the liquid surface of an alkali biting groove in the step D, water is sprayed to the part from top to bottom, and the water is sprayed at blind holes, gaps and threads of the part in an enhanced manner;
E. second washing with water
E, starting overflow, lifting the parts out of the liquid level of the rinsing bath in the step E, and carrying out fan-shaped spray washing on the parts from top to bottom, wherein the water washing time is 60-90s, and the temperature is 20-30 ℃;
F. acid etching
Placing the part into an acid etching solution, and performing acid etching by using a mixed acid solution of nitric acid and hydrofluoric acid, wherein the concentration of the nitric acid and the hydrofluoric acid is 20%: 2 percent, the acid etching time is 8s-12s, and the temperature is 15-25 ℃; when the part is discharged from the pickling tank, the part is sprayed in a fan shape from top to bottom, and water is sprayed at blind holes, gaps and threads of the part in an enhanced manner, so that the part is prevented from being corroded by acid to generate flow marks;
G. third time of water washing
Starting overflow, wherein the water quality is more than or equal to 200k omega, completely immersing the part into water, lifting twice through a crane to carry out enhanced washing, after the part is lifted out of the water level, carrying out fan-shaped spray washing on the part from top to bottom, wherein the washing time is 30-60 s, and the temperature is 20-30 ℃;
H. stripping film
Placing the part into a stripping solution, wherein the main component of the solution is ferric sulfate, phosphoric acid or sulfuric acid, the volume of the solution is 20%, the stripping time is 3-5 min, and aerating; the temperature is 15-25 ℃; when the part is taken out of the film stripping groove, the part is sprayed in a fan shape from top to bottom, and the blind holes, the gaps and the threads of the part are sprayed with water in an enhanced manner, so that iron ions and the like remained on the part are prevented from being brought into the oxidation groove to pollute the oxidation groove liquid;
I. the fourth time of water washing
Starting overflow, wherein the water quality is more than or equal to 200k omega, completely immersing the part into water, lifting twice through a crane to carry out enhanced washing, after the part is lifted out of the water level, carrying out fan-shaped spray washing on the part from top to bottom, wherein the washing time is 60-90s, the temperature is 15-25 ℃, then manually spraying water, and the water spraying time at each blind hole, gap and thread reaches 3-5 s;
J. oxidation by oxygen
Placing the part into a tank containing sulfuric acid and oxalic acid tank liquor, shaking up and down and left and right to ensure that the part is fully contacted with the mixed acid tank liquor without accumulated gas, wherein the concentration of the sulfuric acid and the oxalic acid tank liquor reaches 2g/L and 50g/L, the sulfuric acid is of high-grade purity, the oxalic acid is of analytical purity, the control voltage is 58V-60V, the peak current density is 2A/d square meter, the valley current density is 1A/d square meter, the peak value and the valley value of the current are set according to the anode area S of the part, the boosting time is 5min-10min, the current value = current density multiplied by the anode area S of the part, the thickness of the film is 30-35um, the oxide film is aluminum oxide, and the main function of the film layer is as follows: 1. the wear resistance of the workpiece is increased; 2. the corrosion resistance of the workpiece is increased; 3. the decoration of the workpiece is increased; 4. the insulativity and the hardness of the workpiece are improved, the service life of the workpiece is prolonged, the time is recorded, and the temperature is 5 ℃;
K. fifth washing with water
Starting overflow, wherein the water quality is more than or equal to 200k omega, completely immersing the part into water, lifting twice through a crane to carry out enhanced washing, after the part is lifted out of the water level, carrying out fan-shaped spray washing on the part from top to bottom, wherein the washing time is 60-90s, the temperature is 15-25 ℃, and then manually spraying water at each blind hole, gap and thread for 3-5 s;
l, acid washing
Immersing the part into a nitric acid solution with the concentration of 10 percent for 2-3min, removing active wave electrons on an oxide film on the surface of the workpiece, and preparing for next hole sealing;
m, sixth washing
Starting overflow, wherein the water quality is more than or equal to 200k omega, completely immersing the part into water, lifting twice through a crane to carry out enhanced washing, after the part is lifted out of the water level, carrying out fan-shaped spray washing on the part from top to bottom, wherein the washing time is 60-90s, the temperature is 15-25 ℃, and then manually spraying water at each blind hole, gap and thread for 3-5 s;
sealing holes by N and nickel acetate; the specific hole sealing method is to measure the film thickness by using an oxide film eddy current thickness meter, the hole sealing rate is calculated according to 2min/um, the water quality is more than or equal to 450k omega cm, the temperature is 80 ℃, the concentration of hole sealing liquid is 5g/L, and the PH value is 5.5-6.5;
o, seventh water washing
Completely immersing the part in water, lifting twice by a crane to carry out enhanced washing, after the part is lifted out of the water level, carrying out fan-shaped spray washing on the part from top to bottom, wherein the washing time is 60-90 s;
p, eighth water washing
Completely immersing the part in water, lifting twice by a crane to perform reinforced washing, after the part is lifted out of the water level, performing fan-shaped spray washing on the part from top to bottom, and spraying water at each blind hole, gap and thread for 3-5 s; in the washing process, spraying and washing are adopted for small parts, and high-pressure washing is adopted for large parts;
q, drying; drying the part by dry nitrogen air;
r, hanging down: the parts are placed on the lower hanging bracket, so that scratching and corrosion are prevented in the process;
s, hot water washing: 1/3 is opened for overflow, the water quality is more than or equal to 4M omega, the common impregnation is carried out, the hot water washing time is 2min-5min, and the temperature is 38-46 ℃;
t, drying by blowing again: filtering with a 0.01-micron filter, then flushing nitrogen for drying, and increasing the air blowing amount at blind holes, gaps and threads;
u, baking; filling nitrogen into the oven, setting the flow of the nitrogen in the oven at 30-40L/min, placing the part in the oven for 20-40 min, and controlling the temperature in the oven at 75-85 ℃; the baking time can be prolonged for complex parts, and the temperature can be reduced for thin and easily deformed parts;
and V, packaging and adopting an anti-static PE bag for packaging.
Compared with the prior art, the invention provides an anti-static hard anodizing process, which has the following beneficial effects:
1. according to the anti-static hard anodic oxidation process, 1, no electrostatic action exists on the surface of an oxide film, 2, sulfuric acid and oxalic acid are used as electrolytes, the corrosion resistance of the oxide film is enhanced, 3, the breakdown voltage is increased, 4, the sulfuric acid and oxalic acid tank liquor are used for oxidation in a tank body, the control voltage is 58V-60V, the peak current density is 2A/d square meter, the valley current density is 1A/d square meter, the peak value and the valley value of the current are set according to the anode area S of a part, the boosting time is 5min-10min, the current value = current density multiplied by the anode area S of the part, the film thickness is 30-35um, the wear resistance of the workpiece is increased, the corrosion resistance of the workpiece is increased, the decoration of the workpiece is increased, the insulation property and the hardness of the workpiece;
2. the anti-static hard anodizing process can realize the anti-static effect, improve the corrosion resistance and improve the breakdown voltage;
3. the anti-static hard anodizing process avoids the damage to equipment such as a finished product machine type and the like caused by static electricity generated at the use end after anodizing;
4. according to the anti-static hard anodic oxidation process, a titanium clamp and a titanium screw are adopted during hanging, so that good electric conduction of parts is ensured;
5. the main component of the anti-static hard anodic oxidation process is sodium carbonate or sodium silicate or sodium dodecyl diphenyl ether disulfonate, degreasing is carried out in the alkalescent degreasing solution, and oil stains and impurities on the surface of a workpiece are mainly removed;
6. according to the anti-static hard anodic oxidation process, a part is placed in a stripping solution, the main component of the solution is ferric sulfate, phosphoric acid or sulfuric acid, the volume of the solution is 20%, and residual iron ions and the like on the part are prevented from being brought into an oxidation tank to pollute oxidation tank liquid.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (10)

1. An anti-static hard anodizing process is characterized by comprising the following steps:
A. hanging up;
B. degreasing
Degreasing the part in degreasing fluid for 5-10 min at 48-52 ℃; the concentration of the solution is 5 percent;
C. first washing with water
After the surfaces of the parts in the step B are free of grease, marks and scratches and surface water is not accumulated, starting overflow, enabling the water quality resistivity to be larger than or equal to 200k omega, lifting the parts out of the liquid level of the washing tank in the step C, and carrying out fan-shaped spray washing on the parts from top to bottom, wherein the washing time is 60-90s, and the temperature is 20-30 ℃;
D. alkali bite
Putting the part into a sodium hydroxide solution for alkali biting, wherein the alkali biting time is 15-30 s, the temperature is 40-50 ℃, hanging the part subjected to alkali biting out of the liquid surface of an alkali biting tank in the step D, spraying water to the part from top to bottom, and performing enhanced water spraying at blind holes, gaps and threads of the part;
E. second washing with water
E, starting overflow, lifting the parts out of the liquid level of the rinsing bath in the step E, and carrying out fan-shaped spray washing on the parts from top to bottom, wherein the water washing time is 60-90s, and the temperature is 20-30 ℃;
F. acid etching
Putting the part into an acid etching solution, wherein the acid etching time is 8-12 s, and the temperature is 15-25 ℃; when the part is discharged from the pickling tank, the part is sprayed in a fan shape from top to bottom, and water is sprayed at blind holes, gaps and threads of the part in an enhanced manner, so that the part is prevented from being corroded by acid to generate flow marks;
G. third time of water washing
Starting overflow, wherein the water quality is more than or equal to 200k omega, completely immersing the part into water, lifting twice through a crane to carry out enhanced washing, after the part is lifted out of the water level, carrying out fan-shaped spray washing on the part from top to bottom, wherein the washing time is 30-60 s, and the temperature is 20-30 ℃;
H. stripping film
Placing the part into a film stripping solution, wherein the film stripping time is 3-5 min, starting aeration, the temperature is 15-25 ℃, when the part is taken out of a film stripping groove, carrying out fan-shaped spray washing on the part from top to bottom, and carrying out enhanced water spraying at blind holes, gaps and threads of the part;
I. the fourth time of water washing
Starting overflow, wherein the water quality is more than or equal to 200k omega, completely immersing the part into water, lifting twice through a crane to carry out enhanced washing, after the part is lifted out of the water level, carrying out fan-shaped spray washing on the part from top to bottom, wherein the washing time is 60-90s, and the temperature is 15-25 ℃;
J. oxidation by oxygen
Placing the part into a tank containing sulfuric acid and oxalic acid tank liquor, shaking up and down and left and right to ensure that the part is fully contacted with the mixed acid tank liquor without accumulated gas, wherein the concentration of the sulfuric acid and oxalic acid tank liquor reaches 2g/L and 50g/L, the control voltage is 58V-60V, the peak current density is 2A/d square meter, the valley current density is 1A/d square meter, the peak value and valley value of the current are set according to the anode area S of the part, the boosting time is 5min-10min, the current value = current density multiplied by the anode area S of the part, the thickness of the film is 30-35um, the recording time is kept, and the temperature is 5 ℃;
K. fifth washing with water
Starting overflow, wherein the water quality is more than or equal to 200k omega, completely immersing the part into water, lifting twice through a crane to carry out enhanced washing, after the part is lifted out of the water level, carrying out fan-shaped spray washing on the part from top to bottom, wherein the washing time is 60-90s, and the temperature is 15-25 ℃;
l, acid washing
Immersing the part into a nitric acid solution with the concentration of 10 percent for 2-3min, and removing active wave electrons on an oxide film on the surface of the workpiece;
m, sixth washing
Starting overflow, wherein the water quality is more than or equal to 200k omega, completely immersing the part into water, lifting twice through a crane to carry out enhanced washing, after the part is lifted out of the water level, carrying out fan-shaped spray washing on the part from top to bottom, wherein the washing time is 60-90s, and the temperature is 15-25 ℃;
sealing holes by N and nickel acetate; the specific hole sealing method is to measure the film thickness by using an oxide film eddy current thickness meter, the hole sealing rate is calculated according to 2min/um, the water quality is more than or equal to 450k omega cm, the temperature is 80 ℃, the concentration of hole sealing liquid is 5g/L, and the PH value is 5.5-6.5;
o, seventh water washing
Completely immersing the part in water, lifting twice by a crane to carry out enhanced washing, after the part is lifted out of the water level, carrying out fan-shaped spray washing on the part from top to bottom, wherein the washing time is 60-90 s;
p, eighth water washing
Completely immersing the part in water, lifting twice by a crane to perform reinforced washing, after the part is lifted out of the water level, performing fan-shaped spray washing on the part from top to bottom, and spraying water at each blind hole, gap and thread for 3-5 s;
q, drying;
r, lower hanger
Placing the part on a lower hanging bracket;
s, washing with hot water;
t, drying by blowing again:
u, baking;
and V, packaging and adopting an anti-static PE bag for packaging.
2. The antistatic hard anodizing process of claim 1, wherein a titanium clip or a titanium screw is used for hanging in the step A.
3. The antistatic hard anodizing process of claim 2 wherein the degreasing fluid in step B is a weak alkaline degreasing fluid, the main component of which is sodium carbonate or sodium silicate or sodium dodecyl diphenyl ether disulfonate.
4. The process according to claim 1, wherein the concentration of sodium hydroxide in step D is 50g/L, and 5g/L of analytically pure sodium gluconate is added during the preparation of sodium hydroxide.
5. The antistatic hard anodizing process of claim 4, wherein the acid etching is performed by a mixed acid solution of nitric acid and hydrofluoric acid in the step F, and the concentrations of the nitric acid and the hydrofluoric acid are 20% and 2%, respectively.
6. The antistatic hard anodizing process of claim 1 wherein the stripping solution in step H is mainly ferric sulfate or phosphoric acid or sulfuric acid with a concentration of 20%.
7. The antistatic hard anodizing process of any one of claims 1-6, wherein in the fourth water washing, the fifth water washing and the sixth water washing, water is preferably manually sprayed at each blind hole, gap and thread after the water washing for 3-5 s.
8. The antistatic hard anodic oxidation process according to any one of claims 1 to 6, wherein in the step N, the specific hole sealing method is to measure the film thickness by using an oxide film eddy current thickness meter, the hole sealing rate is calculated according to 2min/um, the water quality is more than or equal to 450k Ω -cm, the temperature is 80 ℃, the concentration of the hole sealing liquid is 5g/L, and the PH value is 5.5-6.5.
9. The antistatic hard anodizing process of claim 1, wherein the drying method in the step Q is to dry the part by using dry nitrogen air, and the drying method in the step T is to blow the part by using nitrogen after filtering by using a 0.01 μm filter, and then blow the part by filling nitrogen, so that the air blowing amount is increased for blind holes, gaps and threads.
10. The anti-static hard anodic oxidation process according to claim 9, wherein the baking method in the step U is to fill nitrogen in the oven, set the flow rate of the nitrogen in the oven to be 30-40L/min, place the part in the oven for 20-40 min, and set the temperature in the oven to be 75-85 ℃.
CN201910767814.0A 2019-08-20 2019-08-20 Anti-static hard anodic oxidation process Pending CN110607549A (en)

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