CN113046808B - Electrolytic coloring method for optical metal structural member - Google Patents
Electrolytic coloring method for optical metal structural member Download PDFInfo
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- CN113046808B CN113046808B CN202110261586.7A CN202110261586A CN113046808B CN 113046808 B CN113046808 B CN 113046808B CN 202110261586 A CN202110261586 A CN 202110261586A CN 113046808 B CN113046808 B CN 113046808B
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- 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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
- C25D17/007—Current directing devices
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
- C25D17/06—Suspending or supporting devices for articles to be coated
- C25D17/08—Supporting racks, i.e. not for suspending
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- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/30—Electroplating: Baths therefor from solutions of tin
- C25D3/32—Electroplating: Baths therefor from solutions of tin characterised by the organic bath constituents used
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
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Abstract
The invention discloses an electrolytic coloring method of an optical metal structural member, which comprises the following steps: pretreatment: sequentially roughening, degreasing and deoiling the optical metal structural part; and (3) oxidation: placing the pretreated optical metal structural part in an oxidation bath solution for oxidation for 45 +/-1 min, wherein the oxidation voltage is 16-17V; electrolytic coloring: placing the oxidized optical metal structural part in an electrolysis device for electrolytic coloring for 300 +/-20S, wherein the electrolytic coloring voltage is 2-3V higher than the oxidation voltage, and obtaining a semi-finished product of the optical metal structural part; chemical color complementing: soaking the obtained semi-finished product of the optical metal structural part in a color supplementing liquid for 5 +/-1 min, wherein the color supplementing liquid is a solution which has the same color as the semi-finished product of the optical metal structural part and has the concentration of 5 +/-1 g/l; sealing holes; and (5) drying. The high-precision, heat-resistant and illumination-resistant performance of the optical metal structural part is met, the white edge of the sharp edge of the workpiece is avoided, the white spot formed by bubbles generated in the inner cavity of the workpiece is avoided, and the appearance consistency is good.
Description
Technical Field
The invention belongs to the technical field of metal surface treatment, and particularly relates to an electrolytic coloring method for an optical metal structural member.
Background
With the development of modern optical technology, laser light sources are widely applied in real life and are already in mass production in factory enterprises, but a great new problem is brought to optical metal structural members matched with the laser light sources, namely, the high irradiation temperature and illumination of the laser light sources have extremely high requirements on oxidation treatment film layers of the optical metal structural members. According to the conditions of the weatherometer (110 ℃, 4mm irradiation distance, 3500 lumen or more illuminance) required by the customers on the market. The film layer subjected to common anodic oxidation can change color and even turn white in 4-6 hours. For micro-arc oxidation, because the aluminum material is oxidized into ceramic during the process characteristic, the film layer is very temperature resistant and illumination resistant, but the thickness of the film layer is frequently floated in a range of more than ten um due to the process characteristic, and the tolerance of an optical metal structural member is usually only 15um, so the micro-arc oxidation process is not suitable for precise optical metal structural members. For electrolytic coloring, inorganic salt is generally used for electrolytic coloring, and the melting point and the boiling point of the inorganic salt are both more than 1000 ℃, so that the requirements of illumination can be met, and the control of film thickness can be met.
The existing electrolytic coloring technology is basically used for manufacturing large-scale materials on large-scale oxidation equipment, such as decorative parts of profiles, door frames, fences and the like. The pretreatment of the parts needs to be performed with strong alkali etching, such as alkali etching or chemical polishing for about two minutes, and the removed size is about 25 um, which has a considerable influence on the size of the parts. And if the procedures of alkaline etching or chemical polishing are not carried out, a circle of white edges can appear at the place with the sharp edges (the optical structural part basically has sharp chamfers and threads which are mutually connected and matched, and the inner walls of a plurality of parts are provided with structures of extinction threads for reducing stray light, and have the sharp edges), so that the requirement that the inner cavity of the optical metal structural part bearing the lens needs black extinction and the requirement that the appearance color is consistent cannot be met. In addition, during electrolytic coloring, because the main components of the bath solution are sulfuric acid and stannous sulfate, stannous sulfate in a free state is very easy to decompose, if the bath solution is stirred, the bath solution in the whole bath is scrapped, but if the bath solution is not stirred, bubbles generated in the electrolytic coloring process cannot be discharged from a workpiece with a cavity, the bubbles can be attached to an inner cavity of the optical metal structural member and cannot be discharged, and the optical metal structural member is isolated from the bath solution to generate white spots.
Disclosure of Invention
The invention aims to solve the problems, provides an electrolytic coloring method for an optical metal structural part, meets the performance requirements of high precision, heat resistance and illumination resistance of the optical metal structural part, can avoid white edges at sharp edges of workpieces and bubbles generated in an inner cavity from forming white spots, and has good appearance consistency.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides an electrolytic coloring method of an optical metal structural member, which comprises the following steps:
s1, pretreatment: sequentially carrying out coarsening, degreasing and deoiling treatment on the optical metal structural part;
s2, oxidation: the optical metal structural part pretreated in the step S1 is put into an oxidation bath solution to be oxidized for 45 +/-1 min, the oxidation bath solution is a sulfuric acid solution with the concentration of 200 +/-20 g/l, and the current density is 1.0 +/-0.1A/dm2The oxidation voltage is 16-17V, and the oxidation temperature is 20 +/-2 ℃;
s3, electrolytic coloring: placing the optical metal structural part oxidized in the step S2 in an electrolytic device for electrolytic coloring for 300 +/-20S, wherein the electrolytic device contains electrolyte, the electrolyte comprises a stannous sulfate solution with the concentration of 20 +/-2 g/l and an analytical pure sulfuric acid solution with the concentration of 12 +/-1 g/l, the pH value is 1-1.5, and the electrolytic coloring voltage is 2-3V higher than the oxidation voltage, so that a semi-finished product of the optical metal structural part is obtained;
s4, chemical complementary color: soaking the semi-finished product of the optical metal structural part obtained in the step S3 in a color supplementing liquid for 5 +/-1 min, wherein the color supplementing liquid is a solution which has the same color as the semi-finished product of the optical metal structural part and has the concentration of 5 +/-1 g/l, and the temperature is 55 +/-5 ℃;
s5, sealing holes;
and S6, drying.
Preferably, electrolytic device is including the cell body, the conducting rod, two conducting seats and a plurality of cylinder that are used for holding electrolyte, and two conducting seats are used for supporting the conducting rod to be located the both sides of cell body respectively, the last hanger that carries of conducting rod is used for placing the work piece, and the bottom and the piston rod that correspond the cylinder of conducting seat are connected, and the cylinder body of cylinder is fixed on cell body or subaerial, still overlaps on the piston rod of cylinder to be equipped with and is used for the absorbing spring.
Preferably, the groove body is provided with a guide device for guiding a piston rod of the air cylinder.
Preferably, the stroke of the cylinder is 50mm, and the frequency of up-and-down vibration is 3 times/min.
Preferably, the roughening treatment: the optical metal structural part is placed in a roughening solution to be soaked for 35 +/-5S, wherein the roughening solution is an ammonium bifluoride solution with the concentration of 100 +/-10 g/l, and the temperature is 55 +/-5 ℃.
Preferably, the optical metal structure after being roughened in step S1 is further subjected to water washing, ash removal and water washing in sequence.
Preferably, degreasing treatment: and (5) placing the optical metal structural part subjected to the roughening treatment in the step S1 into degreasing fluid, and soaking for 10 +/-1 min, wherein the degreasing fluid is 843-II degreaser solution with the concentration of 35 +/-5 g/l and the temperature is 55 +/-5 ℃.
Preferably, the optical metal structure after electrolytic coloring in step S3 is further immersed in an analytically pure sulfuric acid solution with a concentration of 50 + -5 g/l for 120 + -5S for deashing.
Preferably, in steps S1 to S5, each step is further washed with water two to three times after the completion of the execution.
Preferably, sealing the pores: and (5) soaking the optical metal structural part subjected to chemical color compensation in the step (S4) in a hole sealing liquid for 10 +/-1 min, wherein the hole sealing liquid is a DX-500 solution with the concentration of 7 +/-1 g/l, the temperature is 70 +/-5 ℃, and the PH value is 5.8-6.5.
Compared with the prior art, the invention has the beneficial effects that:
1) the burr sharp edge is not needed to be removed through long-time alkali washing or chemical polishing, the performance requirements of high precision, heat resistance and illumination resistance of the optical metal structural part are met, the optical metal structural part is guaranteed to obtain tolerance within 10-15 um, the processing time is shortened, and the production efficiency is improved.
2) The sharp edge of the workpiece can be prevented from generating a white edge through chemical color compensation, and good appearance consistency is kept;
3) the stroke and frequency of vertical vibration of the workpiece are controlled, so that white spots formed by bubbles in the inner cavity of the workpiece are avoided, poor conduction between the workpiece and the hanger is avoided through buffering and shock absorption, and the appearance consistency is good.
Drawings
FIG. 1 is a schematic view of the structure of an electrolytic apparatus of the present invention.
Description of reference numerals: 1. a trough body; 2. a conductive rod; 3. a conductive seat; 4. a cable; 5. a hanger; 6. a workpiece; 7. a spring; 8. a support; 9. and a cylinder.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It will be understood that when an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used in the description of the present application herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.
As shown in fig. 1, a method for electrolytic coloring of an optical metal structural member comprises the steps of:
s1, pretreatment: sequentially carrying out coarsening, degreasing and deoiling treatment on the optical metal structural part;
s2, oxidation: the optical metal structural part pretreated in the step S1 is put into an oxidation bath solution to be oxidized for 45 +/-1 min, the oxidation bath solution is a sulfuric acid solution with the concentration of 200 +/-20 g/l, and the current density is 1.0 +/-0.1A/dm2The oxidation voltage is 16-17V, and the oxidation temperature is 20 +/-2 ℃;
s3, electrolytic coloring: placing the optical metal structural part oxidized in the step S2 in an electrolytic device for electrolytic coloring for 300 +/-20S, wherein the electrolytic device contains electrolyte, the electrolyte comprises a stannous sulfate solution with the concentration of 20 +/-2 g/l and an analytical pure sulfuric acid solution with the concentration of 12 +/-1 g/l, the pH value is 1-1.5, and the electrolytic coloring voltage is 2-3V higher than the oxidation voltage, so that a semi-finished product of the optical metal structural part is obtained;
s4, chemical complementary color: soaking the semi-finished product of the optical metal structural part obtained in the step S3 in a color supplementing liquid for 5 +/-1 min, wherein the color supplementing liquid is a solution which has the same color as the semi-finished product of the optical metal structural part and has the concentration of 5 +/-1 g/l, and the temperature is 55 +/-5 ℃;
s5, sealing holes;
and S6, drying.
The workpiece 6 is an optical metal structural member, the electrolytic coloring voltage of the workpiece 6 is higher than the oxidation voltage by 2-3V, and if the workpiece 6 is 6061 material and the oxidation voltage is 16V, the electrolytic coloring voltage is 18-19V. Because the semiconductor characteristic of oxidation film layer, the alternating current is during electrolytic coloring, restores oxidation film layer bottom during the positive voltage, produces electrolysis during the negative voltage and sinks the tin salt to the oxidation film hole bottom and produces black, adopts the voltage higher than during the oxidation, can be better more thorough electrolyze electrolytic tin salt to the hole bottom of oxidation film for electrolytic colored work piece 6 obtains good outward appearance uniformity, can not appear bad phenomena such as reddening, bronze. In order to ensure the tolerance of the optical metal structural part to be within 10 um-15 um, the thickness range of the oxidized oxide film is ensured to be within 15.5 +/-1 um. It should be noted that, when the electrolytic coloring voltage is higher than the oxidation voltage, the specific differential pressure value can be adjusted according to actual requirements, for example, according to the characteristics of different materials.
The oxide film layer formed on the sharp edge part of the optical metal structural member is usually not connected or not connected sufficiently with the optical metal structural member, is approximately suspended in a bath solution, does not generate or does not generate electrolytic coloring reaction completely, and the semiconductor characteristic can not be completely embodied during electrolytic coloring, so that the sharp edge part has the phenomenon that part of the sharp edge part is not colored in place, and is visually shown as white edge or white spots of star points. Through chemical color compensation, the workpiece 6 is soaked in color compensation liquid for 5 +/-1 min, the color compensation liquid is a solution which has the same color with the semi-finished product of the optical metal structural member and has the concentration of 5 +/-1 g/l, and the temperature is 55 +/-5 ℃. And during chemical color compensation, the suspended oxide film formed by the sharp edge part is used for coloring by utilizing the adsorption force generated by the oxide film layer in the bath solution, so that the defect of white edge or white spot at the sharp edge part is compensated.
This application need not to wash with alkaline or change and throw away the burr sharp limit for a long time, satisfies the high accuracy of optics metallic structure spare, heat-resisting and resistant light performance requirement, guarantees that optics metallic structure spare obtains the tolerance in 10um ~ 15um, and helps shortening process time, improves production efficiency. The sharp edge of the workpiece can be prevented from generating white edges or white spots through chemical color complementing, and good appearance consistency is obtained.
In an embodiment, the electrolytic device includes a tank body 1 for containing electrolyte, a conducting rod 2, two conducting seats 3 and a plurality of cylinders 9, the two conducting seats 3 are used for supporting the conducting rod 2 and are respectively located on two opposite sides of the tank body 1, a hanger 5 for placing a workpiece 6 is carried on the conducting rod 2, the bottom of the conducting seat 3 is connected with a piston rod corresponding to the cylinder 9, a cylinder body of the cylinder 9 is fixed on the tank body 1 or the ground, and a spring 7 for damping is further sleeved on the piston rod of the cylinder 9.
The electrolysis device comprises a tank body 1, a conducting rod 2, two conducting seats 3 and a plurality of cylinders 9, wherein the two cylinders 9 are preferably selected, the cylinders 9 are connected with the conducting seats 3 in a one-to-one correspondence mode and are respectively located on two opposite sides of the tank body 1, supports 8 fixedly connected with the ground are further arranged on two opposite sides of the tank body 1, and the cylinders 9 move synchronously. Electrically conductive seat 3 is connected with cable 4, if be 100A's red copper cable, the cylinder 9 of being convenient for drives electrically conductive seat 3 up-and-down motion to drive the electrically conductive pole 2 up-and-down motion that supports on the electrically conductive seat 3, the last thing that carries of electrically conductive pole 2 is used for placing the hanger 5 of work piece 6, the bottom and the piston rod of cylinder 9 of electrically conductive seat 3 are connected, the cylinder body of cylinder 9 is fixed on support 8, still overlaps on the piston rod of cylinder 9 and is equipped with and is used for absorbing spring 7. It should be noted that the cylinder body of the cylinder 9 can also be fixed on the tank body 1, and the number of the cylinders 9 can also be set according to the type of the cylinder or the size of the load.
Because the workpiece 6 except the part connected with the hanger 5 is provided with the oxidation film during electrolytic coloring, the damping spring 7 is added, the condition that the workpiece 6 and the hanger 5 are not conductive due to too large vibration is avoided, the normal operation of the electrolytic coloring process is ensured, bubbles generated in the inner cavity of the workpiece 6 can swing up and down along with the movement of the air cylinder 9 during the electrolytic coloring, the bubbles are discharged from the inside of the workpiece 6 under the impact of water flow, white spots generated by the bubbles are eliminated, and high appearance quality is obtained.
In an embodiment, the groove body 1 is provided with a guiding device for guiding a piston rod of the air cylinder 9.
Wherein, for the stability of reinforcing cylinder 9 motion, improve life, avoid the slope card simultaneously to pause, lead to the piston rod of cylinder 9 through guider, can be guide rail slider mechanism if guider, the vertical two offsides of fixing at cell body 1 of guide rail, the piston rod end-to-end connection of slider and cylinder 9 still can directly adopt electrically conductive seat 3 and fix the guide arm on cell body 1 and slide fit from top to bottom leads, or adopt arbitrary guider among the prior art to lead.
In one embodiment, the stroke of the cylinder 9 is 50mm, and the frequency of up-and-down vibration is 3 times/min.
Wherein, the stroke of the air cylinder 9 is 50mm, and the frequency of up-down vibration is 3 times/min. Can avoid the bath solution decomposition failure caused by overlarge stroke or overlarge vibration frequency or poor conduction between the workpiece 6 and the hanger 5 caused by overlarge vibration. Is beneficial to eliminating white spots generated by bubbles and obtains higher appearance quality. And the stroke of the cylinder 9 can be adjusted according to the actual requirement.
In one embodiment, the coarsening process: the optical metal structural part is placed in a roughening solution to be soaked for 35 +/-5S, wherein the roughening solution is an ammonium bifluoride solution with the concentration of 100 +/-10 g/l, and the temperature is 55 +/-5 ℃.
Wherein, the coarsening treatment can make the surface of the optical metal structural component become rough and then make the adhesion of the plated substance strengthen and not easy to fall off, and helps to ensure that the optical metal structural component obtains the tolerance within 10 um-15 um, and then meets the high precision requirement of the optical metal structural component.
In one embodiment, the optical metal structure after being roughened in step S1 is further sequentially subjected to water washing, ash removal and water washing.
The optical metal structural part is sequentially washed twice, deashed and washed three times, the washing can be carried out by adopting a soaking or spraying mode, and during deashing, the optical metal structural part after twice washing is placed in 50% industrial nitric acid to be soaked for a preset time for neutralization. The washing times and the dedusting process can be adjusted according to actual requirements, and the surface purification treatment is carried out on the optical metal structural part, so that the product quality and the qualification rate are improved.
In one embodiment, degreasing treatment: and (5) placing the optical metal structural part subjected to the roughening treatment in the step S1 into degreasing fluid, and soaking for 10 +/-1 min, wherein the degreasing fluid is 843-II degreaser solution with the concentration of 35 +/-5 g/l and the temperature is 55 +/-5 ℃.
Wherein, the surface purification is carried out by degreasing and deoiling, which is beneficial to ensuring that the optical metal structural part has good adhesive force in the subsequent treatment. It should be noted that the degreasing liquid is 843-II degreaser, and other types of degreasers, such as ECH-35 organic degreasers, can be selected according to actual requirements.
In one embodiment, the electrolytically colored optical metal structure is also deashed by immersing the structure in an analytically pure sulfuric acid solution with a concentration of 50g/l + -5 for 120S + -5.
In one embodiment, the steps S1 to S5 are performed with water two to three times after the completion of the steps.
Wherein, the washing can adopt and soak or spray the mode and wash, through carrying out surface purification to optical metal structure spare, help improving product quality and qualification rate.
In one embodiment, sealing: and (5) soaking the optical metal structural part subjected to chemical color compensation in the step (S4) in a hole sealing liquid for 10 +/-1 min, wherein the hole sealing liquid is a DX-500 solution with the concentration of 7g +/-1 g/l, the temperature is 70 +/-5 ℃, and the PH value is 5.8-6.5.
Wherein, hole sealing treatment is carried out for protecting the film layer, further improving the corrosion resistance, the weather resistance and the pollution resistance, and preventing fading. It should be noted that the hole sealing liquid can be selected from other types according to actual requirements.
Example 1:
an electrolytic coloring method for an optical metal structural part, wherein the optical metal structural part is a lens cone made of 6061 materials, comprises the following steps:
s1, pretreatment: the method comprises the following steps of (1) carrying out coarsening and degreasing treatment on the optical metal structural part in sequence, wherein:
roughening treatment: the optical metal structural part is placed in a roughening solution to be soaked for 35S, wherein the roughening solution is an ammonium bifluoride solution with the concentration of 90g/l, and the temperature is 55 ℃. And (3) soaking and washing the coarsened optical metal structural part twice in a water tank, taking out and soaking in 50% industrial nitric acid for 2min for neutralization and deashing, and soaking and washing in the water tank for three times to purify the surface.
Degreasing: and (4) soaking the optical metal structural part subjected to the roughening treatment in the step S1 in degreasing liquid for 10min, wherein the degreasing liquid is 843-II degreaser solution with the concentration of 35g/l and the temperature is 55 ℃. Degreasing, soaking and washing twice in a water tank.
S2, oxidation: oxidizing the optical metal structural part pretreated in the step S1 in an oxidizing bath solution for 45min, wherein the oxidizing bath solution is a sulfuric acid solution with the concentration of 200g/l and the current density is 1.1A/dm2The oxidation voltage is 16V, the oxidation temperature is 20 ℃, and the thickness of the oxide film of the obtained optical metal structural part is 15.5 um. Then soaked in water in a water tank and washed three times.
S3, electrolytic coloring: and (5) placing the optical metal structural member oxidized in the step (S2) in an electrolysis device for electrolytic coloring for 300S, wherein the electrolysis device contains electrolyte, the electrolyte comprises stannous sulfate solution with the concentration of 20g/l and analytical pure sulfuric acid solution with the concentration of 12g/l, the pH value is 1.5, the electrolytic coloring voltage is 18V, the stroke of the air cylinder 9 is 50mm, and the frequency of vertical vibration is 3 times/min, so that the semi-finished product of the optical metal structural member is obtained. And (3) soaking the semi-finished product of the optical metal structural part in analytically pure sulfuric acid with the concentration of 50g/l for 120S for deashing, and then soaking and washing in a water tank for three times.
S4, chemical complementary color: and (4) soaking the semi-finished product of the optical metal structural part obtained in the step (S3) in a color supplementing liquid for 5min, wherein the color supplementing liquid is a solution with the concentration of 5g/l and the dye color number of 415, and the dye color number adopts the Japan Australian dye standard and is at the temperature of 55 ℃. Then soaked in water in a water tank and washed three times.
S5, sealing holes: and (5) soaking the optical metal structural part subjected to chemical color compensation in the step S4 in a hole sealing liquid for 10min, wherein the hole sealing liquid is a DX-500 solution with the concentration of 7g/l, the temperature is 70 ℃, and the PH value is 6.5. Then soaking and washing twice in a water tank, and washing once by pure water.
S6, drying: and (3) placing the optical metal structural part subjected to hole sealing in a dryer, drying at 90 ℃ for 20min, and thus obtaining the optical metal structural part with good appearance consistency. It should be noted that, the drying temperature can also be increased, the drying time is further shortened, and the drying efficiency is improved.
Example 2:
an electrolytic coloring method for an optical metal structural part, wherein the optical metal structural part is a lens cone made of 6061 materials, comprises the following steps:
s1, pretreatment: the method comprises the following steps of (1) carrying out coarsening and degreasing treatment on the optical metal structural part in sequence, wherein:
roughening treatment: the optical metal structural part is placed in a roughening solution to be soaked for 40S, wherein the roughening solution is an ammonium bifluoride solution with the concentration of 95g/l, and the temperature is 50 ℃. And (3) soaking and washing the coarsened optical metal structural part twice in a water tank, taking out and soaking in 50% industrial nitric acid for 2min for neutralization and deashing, and soaking and washing in the water tank for three times to purify the surface.
Degreasing: and (5) placing the optical metal structural part subjected to the roughening treatment in the step S1 into degreasing fluid, and soaking for 11min, wherein the degreasing fluid is 843-II degreaser solution with the concentration of 30g/l and the temperature is 50 ℃. Degreasing, soaking and washing twice in a water tank.
S2, oxidation: the optical metal structural part pretreated in the step S1 is put into an oxidation bath solution for oxidation for 45min, the oxidation bath solution is a sulfuric acid solution with the concentration of 180g/l, and the current density is 1.1A/dm2The oxidation voltage is 16V, the oxidation temperature is 18 ℃, and the thickness of the oxide film of the obtained optical metal structural part is 14.7 um. Then soaked in water in a water tank and washed three times.
S3, electrolytic coloring: and (5) placing the optical metal structural member oxidized in the step (S2) in an electrolysis device for electrolytic coloring for 300S, wherein the electrolysis device contains electrolyte, the electrolyte comprises stannous sulfate solution with the concentration of 20g/l and analytical pure sulfuric acid solution with the concentration of 12g/l, the pH value is 1.5, the electrolytic coloring voltage is 18V, the stroke of the air cylinder 9 is 50mm, and the frequency of vertical vibration is 3 times/min, so that the semi-finished product of the optical metal structural member is obtained. And (3) soaking the semi-finished product of the optical metal structural part in analytically pure sulfuric acid with the concentration of 50g/l for 120S for deashing, and then soaking and washing in a water tank for three times.
S4, chemical complementary color: and (4) soaking the semi-finished product of the optical metal structural part obtained in the step (S3) in a color supplementing liquid for 5min, wherein the color supplementing liquid is a solution with the concentration of 4g/l and the dye color number 415, and the dye color number adopts the Japan Australian dye standard and is 60 ℃. Then soaked in water in a water tank and washed three times.
S5, sealing holes: and (5) soaking the optical metal structural part subjected to chemical color compensation in the step S4 in a hole sealing liquid for 10min, wherein the hole sealing liquid is a DX-500 solution with the concentration of 7g/l, the temperature is 70 ℃, and the PH value is 6.5. Then soaking and washing twice in a water tank, and washing once by pure water.
S6, drying: and (3) placing the optical metal structural part subjected to hole sealing in a dryer, drying at 90 ℃ for 20min, and thus obtaining the optical metal structural part with good appearance consistency. It should be noted that, the drying temperature can also be increased, the drying time is further shortened, and the drying efficiency is improved.
Example 3:
an electrolytic coloring method for an optical metal structural part, wherein the optical metal structural part is a lens cone made of 6061 materials, comprises the following steps:
s1, pretreatment: the method comprises the following steps of (1) carrying out coarsening and degreasing treatment on the optical metal structural part in sequence, wherein:
roughening treatment: the optical metal structural part is placed in a roughening solution to be soaked for 30S, wherein the roughening solution is an ammonium bifluoride solution with the concentration of 110g/l, and the temperature is 60 ℃. And (3) soaking and washing the coarsened optical metal structural part twice in a water tank, taking out and soaking in 50% industrial nitric acid for 2min for neutralization and deashing, and soaking and washing in the water tank for three times to purify the surface.
Degreasing: and (4) soaking the optical metal structural part subjected to the roughening treatment in the step S1 in degreasing liquid for 10min, wherein the degreasing liquid is 843-II degreaser solution with the concentration of 40g/l and the temperature is 60 ℃. Degreasing, soaking and washing twice in a water tank.
S2, oxidation: placing the optical metal structure pretreated in the step S1 in oxygenOxidizing for 45min in the solution of the oxidation tank, wherein the solution of the oxidation tank is a sulfuric acid solution with the concentration of 220g/l, and the current density is 1.1A/dm2The oxidation voltage is 16V, the oxidation temperature is 22 ℃, and the thickness of the oxide film of the obtained optical metal structural part is 16.5 um. Then soaked in water in a water tank and washed three times.
S3, electrolytic coloring: and (5) placing the optical metal structural member oxidized in the step (S2) in an electrolysis device for electrolytic coloring for 300S, wherein the electrolysis device contains electrolyte, the electrolyte comprises stannous sulfate solution with the concentration of 20g/l and analytical pure sulfuric acid solution with the concentration of 12g/l, the pH value is 1.5, the electrolytic coloring voltage is 19V, the stroke of the air cylinder 9 is 50mm, and the frequency of vertical vibration is 3 times/min, so that the semi-finished product of the optical metal structural member is obtained. And (3) soaking the semi-finished product of the optical metal structural part in analytically pure sulfuric acid with the concentration of 50g/l for 120S for deashing, and then soaking and washing in a water tank for three times.
S4, chemical complementary color: and (4) soaking the semi-finished product of the optical metal structural part obtained in the step (S3) in a color supplementing liquid for 5min, wherein the color supplementing liquid is a solution with the concentration of 6g/l and the dye color number of 415, and the dye color number adopts the Japan Australian dye standard and is at 50 ℃. Then soaked in water in a water tank and washed three times.
S5, sealing holes: and (5) soaking the optical metal structural part subjected to chemical color compensation in the step S4 in a hole sealing liquid for 10min, wherein the hole sealing liquid is a DX-500 solution with the concentration of 7g/l, the temperature is 75 ℃, and the PH value is 5.8. Then soaking and washing twice in a water tank, and washing once by pure water.
S6, drying: and (3) placing the optical metal structural part subjected to hole sealing in a dryer, drying at 90 ℃ for 20min, and thus obtaining the optical metal structural part with good appearance consistency. It should be noted that, the drying temperature can also be increased, the drying time is further shortened, and the drying efficiency is improved.
In embodiment 1, embodiment 2, and embodiment 3, the lens barrel that satisfies the requirements of the optical metal structure for high precision, heat resistance, and illumination resistance can be obtained, the tolerance of the optical metal structure is controlled within 10um to 15um, the processing time is greatly shortened, the production efficiency is improved, the occurrence of white edges or white spots on the workpiece is avoided, the lens barrel can obtain good appearance consistency, and the lens barrel is helpful for eliminating stray light in practical use, so that the light path passes through according to the design requirements.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express the more specific and detailed embodiments described in the present application, but not should be understood as the limitation of the invention claims. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the concept of the present application, which falls within the scope of protection of the present application. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (9)
1. An electrolytic coloring method for an optical metal structural member, characterized in that: the electrolytic coloring method of the optical metal structural part comprises the following steps:
s1, pretreatment: the method comprises the following steps of (1) carrying out coarsening treatment and degreasing treatment on the optical metal structural part in sequence, wherein:
the coarsening treatment comprises the following steps: placing an optical metal structural part in a roughening solution to be soaked for 35 +/-5S, wherein the roughening solution is an ammonium bifluoride solution with the concentration of 100 +/-10 g/l, and the temperature is 55 +/-5 ℃;
and (3) degreasing treatment: placing the roughened optical metal structural part in degreasing liquid to be soaked for 10 +/-1 min at the temperature of 55 +/-5 ℃;
s2, oxidation: placing the optical metal structural part pretreated in the step S1 in an oxidation bath solution for oxidation for 45 +/-1 min, wherein the oxidation bath solution is a sulfuric acid solution with the concentration of 200 +/-20 g/l, and the current density is 1.0 +/-0.1A/dm2The oxidation voltage is 16-17V, and the oxidation temperature is 20 +/-2 ℃;
s3, electrolytic coloring: placing the optical metal structural member oxidized in the step S2 in an electrolytic device for electrolytic coloring for 300 +/-20S, wherein the electrolytic device contains electrolyte, the electrolyte comprises a stannous sulfate solution with the concentration of 20g +/-2 g/l and an analytical pure sulfuric acid solution with the concentration of 12g +/-1 g/l, the pH value is 1-1.5, and the electrolytic coloring voltage is 2-3V higher than the oxidation voltage, so that a semi-finished product of the optical metal structural member is obtained;
s4, chemical complementary color: soaking the optical metal structural part semi-finished product obtained in the step S3 in a color supplementing liquid for 5 +/-1 min, wherein the color supplementing liquid is a solution which has the same color as the optical metal structural part semi-finished product and has the concentration of 5 +/-1 g/l, the temperature is 55 +/-5 ℃, and the color supplementing liquid is a solution of a dye with the color number 415;
s5, sealing holes;
and S6, drying.
2. A method for electrolytic coloring of an optical metal structure according to claim 1, wherein: the electrolytic device comprises a tank body (1) for containing electrolyte, a conducting rod (2), two conducting seats (3) and a plurality of cylinders (9), wherein the conducting seats (3) are used for supporting the conducting rod (2) and are respectively located on two opposite sides of the tank body (1), hanging tools (5) for placing workpieces (6) are mounted on the conducting rod (2), the bottom of each conducting seat (3) corresponds to a piston rod of each cylinder (9) and is connected with the cylinder body of each cylinder (9), the cylinder body of each cylinder (9) is fixed to the tank body (1) or the ground, and each piston rod of each cylinder (9) is further sleeved with a spring (7) for damping.
3. A method for electrolytic coloring of an optical metal structure according to claim 2, wherein: the groove body (1) is provided with a guide device for guiding a piston rod of the air cylinder (9).
4. A method for electrolytic colouring of optical metallic structures according to claim 2 or 3, characterized in that: the stroke of the air cylinder (9) is 50mm, and the up-and-down vibration frequency is 3 times/min.
5. A method for electrolytic coloring of an optical metal structure according to claim 1, wherein: and the optical metal structural member subjected to the roughening treatment in the step S1 is further subjected to water washing, dust removal and water washing in sequence.
6. A method for electrolytic coloring of an optical metal structure according to claim 1, wherein: the degreasing solution is 843-II degreasing solution with the concentration of 35 +/-5 g/l.
7. A method for electrolytic coloring of an optical metal structure according to claim 1, wherein: and (3) soaking the semi-finished product of the optical metal structural part obtained in the step (S3) in an analytically pure sulfuric acid solution with the concentration of 50 +/-5 g/l for 120 +/-5S for deashing.
8. A method for electrolytic coloring of an optical metal structure according to claim 7, wherein: in steps S1 to S5, after the execution of each step is completed, the washing is performed two to three times.
9. A method for electrolytic coloring of an optical metal structure according to claim 1, wherein: and (3) hole sealing: and (3) soaking the optical metal structural part subjected to chemical color compensation in the step S4 in a hole sealing liquid for 10 +/-1 min, wherein the hole sealing liquid is a DX-500 solution with the concentration of 7 +/-1 g/l, the temperature is 70 +/-5 ℃, and the PH value is 5.8-6.5.
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