CN108677231B - Preparation method of rolled copper shading ring sheet and rolled copper shading ring sheet - Google Patents
Preparation method of rolled copper shading ring sheet and rolled copper shading ring sheet Download PDFInfo
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- CN108677231B CN108677231B CN201810417823.2A CN201810417823A CN108677231B CN 108677231 B CN108677231 B CN 108677231B CN 201810417823 A CN201810417823 A CN 201810417823A CN 108677231 B CN108677231 B CN 108677231B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- 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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- 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
- C23C22/63—Treatment of copper or alloys based thereon
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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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/78—Pretreatment of the material to be coated
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03B—APPARATUS OR ARRANGEMENTS FOR TAKING PHOTOGRAPHS OR FOR PROJECTING OR VIEWING THEM; APPARATUS OR ARRANGEMENTS EMPLOYING ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ACCESSORIES THEREFOR
- G03B11/00—Filters or other obturators specially adapted for photographic purposes
- G03B11/04—Hoods or caps for eliminating unwanted light from lenses, viewfinders or focusing aids
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Abstract
The invention provides a preparation method of a rolled copper shading ring sheet, which comprises the following steps: providing a formed shading ring sheet made of a rolled copper material; carrying out oil removal treatment on the shading ring sheet; polishing the shading ring sheet; electroplating the shading ring sheet to enable the surface of the shading ring sheet to be electroplated with a copper nodule layer so as to increase the roughness of the surface of the shading ring sheet; activating the shading ring sheet; blackening the shading ring sheet to change the color of the surface of the shading ring sheet; and drying the shading ring sheet to obtain a finished product of the rolled copper shading ring sheet. The invention also provides a rolled copper shading ring sheet. The preparation method of the rolled copper shading ring sheet provided by the invention has the advantages of simple steps and strong practicability, the matte black structure of the prepared rolled copper shading ring sheet is stable and is not easy to fall off, and the preparation method of the rolled copper shading ring sheet and the rolled copper shading ring sheet also have the characteristics of easy blackening, simple process and low reflectivity after blackening.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of camera shooting, in particular to a preparation method of a rolled copper shading ring sheet and the rolled copper shading ring sheet.
[ background of the invention ]
With the rapid development of scientific technology, digital cameras and mobile phones with digital cameras are rapidly popularized, and optical parts used in these optical instruments are gradually improved. The shading ring sheet is an optical element for regulating and controlling light flux in an optical system, and when external light enters a lens, the shading ring sheet arranged between lenses can block the entry of unwanted light so as to prevent flare or ghost images from being generated in a shot image.
In the related art, the shading ring sheet is made of japanese SOMA shading material, the material is Polyethylene terepHthalate (PET) with double matt black, and the shading ring sheet made of the material has the defects of difficult conduction, no high temperature resistance and the like, and a matte structure on the surface of the shading ring sheet is easy to age and fall off, so that the shading performance is influenced.
Therefore, it is necessary to provide a novel method for producing a rolled copper shade sheet and a rolled copper shade sheet.
[ summary of the invention ]
The invention aims to provide a preparation method of a rolled copper shading ring sheet with simple steps and strong practicability and the rolled copper shading ring sheet with stable performance.
In order to achieve the above object, the present invention provides a method for producing a rolled copper shading ring sheet, comprising the steps of:
providing a formed shading ring sheet, wherein the shading ring sheet is made of a rolled copper material;
carrying out oil removal treatment on the shading ring sheet to remove a rolling oil film attached to the surface of the shading ring sheet;
polishing the shading ring sheet subjected to oil removal treatment by using polishing liquid to remove the concave-convex structure on the surface of the shading ring sheet;
placing the polished shading ring sheet in an electroplating solution for electroplating treatment to attach a layer of copper nodule layer on the surface of the shading ring sheet so as to increase the roughness of the surface of the shading ring sheet, wherein the electroplating treatment is carried out at the temperature of 20-50 ℃ for 30 seconds-5 minutes, and the current density is 0.5-3.5A/dm2The pH value of the electroplating solution is 9-12, and the electroplating solution comprises the following components: the copper sulfate pentahydrate, the zinc sulfate, the potassium sodium tartrate and the sodium citrate, wherein the content of the copper sulfate pentahydrate is 2.5-25 g/L, and the mass concentration ratio of the zinc sulfate to the copper sulfate pentahydrate is (1-10): 1, the content of the potassium sodium tartrate is 50-200 g/L, and the content of the potassium sodium citrate is 10-30 g/L;
activating the shading ring sheet subjected to electroplating treatment by using an activating agent so as to increase the activity of the surface of the shading ring sheet;
carrying out blackening treatment on the activated shading ring sheet by using blackening liquid so as to change the color of the surface of the shading ring sheet;
and drying the shading ring sheet subjected to blackening treatment under the vacuum condition of less than 200 ℃ to obtain a finished product of the rolled copper shading ring sheet.
Preferably, the plating solution is stirred with air during the plating treatment.
Preferably, after the electroplating treatment, the shading ring sheet needs to be dried for 10-30 minutes under a vacuum condition of less than 150 ℃.
Preferably, the electroplating treatment further includes a dealloying treatment to remove the metal zinc attached to the surface of the light shielding ring sheet, and the dealloying treatment specifically includes the following two methods:
(1) placing the shading ring sheet in a sulfuric acid or hydrochloric acid solution with a certain concentration to corrode for 1-48 hours;
(2) placing the shading ring piece into electrolyte for electrochemical corrosion, wherein the electrochemical corrosion temperature is 20-50 ℃, the time is 30 seconds-5 minutes, and the current density is 0.5-4A/dm2And the electrolyte is a sodium chloride solution.
Preferably, the blackening treatment time is 5 seconds to 20 minutes, the temperature is 50 ℃ to 100 ℃, the blackening solution is prepared from a blackening agent and water according to a mass ratio of 0.1 to 5, and the blackening agent comprises the following components in percentage by mass: 85-95% of sodium hydroxide, 5-8% of potassium persulfate and 2-7% of ammonium bicarbonate, wherein the total weight of the blackening agent is calculated by weight percentage.
Preferably, the oil removal treatment specifically comprises: and ultrasonic cleaning is carried out for 10-30 minutes by adopting acetone, and ultrasonic cleaning is carried out for 20-60 minutes by adopting ethanol.
Preferably, the polishing solution is a copper polishing solution.
Preferably, the activating agent is prepared by mixing concentrated sulfuric acid with water at the concentration of 98% according to the weight ratio of 1: 3, and the activation treatment time is 10 seconds to 10 minutes.
Preferably, a water washing process is further included between the two adjacent steps, and the water washing process lasts for 1-3 times. The invention also provides a rolled copper shading ring sheet which is prepared by adopting the preparation method of the rolled copper shading ring sheet.
Compared with the prior art, the preparation method of the calendered copper shading ring sheet provided by the invention has the advantages that the calendered copper material is adopted to prepare the shading ring sheet, and the finished product of the calendered copper shading ring sheet is obtained through the processes of oil removal, polishing, electroplating, activation, blackening, drying and the like, and the calendered copper shading ring sheet avoids the defects that the PET shading ring sheet in the prior art is not easy to conduct electricity and does not resist high temperature, and has the advantages of easy blackening and low reflectivity; meanwhile, the roughness of the surface of the calendered copper shading ring sheet is increased by attaching a copper nodule layer, so that the matte black structure is stable and is not easy to fall off.
[ description of the drawings ]
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without inventive efforts, wherein:
FIG. 1 is a flow chart of a method for producing a rolled copper gobo sheet according to the present invention;
FIG. 2a is a microstructure diagram of a shading ring piece surface obtained after an electroplating process according to an embodiment of the present invention, which is magnified by 1 ten thousand times under an electron microscope;
FIG. 2b is a microstructure diagram of a surface of a rolled copper gobo sheet obtained in the first embodiment of the present invention, magnified 5 ten thousand times under an electron microscope;
FIG. 3a is a microstructure diagram of a shading ring piece obtained after electroplating treatment according to the second embodiment of the present invention, wherein the microstructure diagram is magnified by 1 ten thousand times under an electron microscope;
FIG. 3b is a microstructure diagram of the surface of a rolled copper gobo sheet obtained in example two of the present invention magnified 5 ten thousand times under an electron microscope;
FIG. 4a is a microstructure diagram of a shading ring piece surface obtained after electroplating treatment according to the third embodiment of the present invention, which is magnified by 1 ten thousand times under an electron microscope;
FIG. 4b is a microstructure diagram of the surface of the rolled copper gobo sheet obtained in the third example of the present invention magnified 5 ten thousand times under an electron microscope.
[ detailed description ] embodiments
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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. 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 invention.
Referring to fig. 1, the present invention provides a method for manufacturing a rolled copper shading ring sheet, which comprises the following steps:
s1: providing a molded shade ring sheet made of a calendered copper material.
The rolled copper is manufactured by rolling a copper ingot, and then performing forging fire, oxidation resistance, roughening treatment and other processes, the thickness of the rolled copper is generally 5-135 um, the molecules are tightly connected, and the rolled copper has the characteristics of good flexibility, high strength, good bending property, ductility, electroplating property, conductivity, excellent surface gloss and the like; furthermore, the rolled copper foil has low surface oxygen characteristics, can be adhered to various substrates such as metals, insulating materials and the like, and has a wide temperature use range. The shading ring sheet made of the calendered copper material can overcome the defects that a PET material shading ring sheet in the related technology is not aging-resistant, easy to deform and not high-temperature-resistant, and has the characteristics of stable size, easy blackening, simple process and low reflectivity after blackening.
The shading ring piece needs to be washed by water to remove dust, impurities or granular substances attached to the surface, the washing process lasts for 1-3 times, and then follow-up procedures are carried out.
S2: and carrying out oil removal treatment on the shading ring sheet to remove a rolling oil film attached to the surface of the shading ring sheet.
Because of the inherent characteristics of the rolled copper in the production and rolling process, a large amount of rolling oil films are attached to the double surfaces of the rolled copper, and the oil content of the double surfaces can reach 5mg/m2The requirements of product delivery and the subsequent chemical and electrochemical surface treatment procedures are seriously influenced. The shading ring sheet made of the rolled copper material needs to be subjected to oil removal treatment on a rolling oil film on the surface of the shading ring sheet so as to facilitate the subsequent processes.
The oil removing treatment specifically comprises the following steps: and ultrasonic cleaning is carried out for 10-30 minutes by adopting acetone, and ultrasonic cleaning is carried out for 20-60 minutes by adopting ethanol. Acetone and ethanol are environment-friendly organic solvents, can be repeatedly used, have high oil removal efficiency and good effect, and can enhance the cleaning and oil removal effect by being supplemented with ultrasonic waves, so that the oil removal cleaning efficiency is greatly improved, and the oil removal cleaning time is greatly shortened.
After the oil removal treatment is finished, the shading ring sheet needs to be washed for 1-3 times to remove the acetone/ethanol solution attached to the surface of the shading ring sheet.
S3: and polishing the shading ring sheet subjected to oil removal treatment by using polishing liquid to remove the concave-convex structure on the surface of the shading ring sheet.
The surface of the shading ring can be flat and bright by polishing treatment. Preferably, the polishing solution is a copper polishing solution, and any commercially available copper polishing solution can be used.
And after the polishing treatment is finished, the shading ring sheet needs to be washed for 1-3 times to remove polishing liquid attached to the surface of the shading ring sheet.
S4: and placing the polished shading ring sheet in electroplating solution for electroplating treatment so as to attach a layer of copper nodule layer on the surface of the shading ring sheet and increase the roughness of the surface of the shading ring sheet.
Specifically, the electroplating treatment temperature is 20-50 ℃, the time is 30 seconds-5 minutes, and the current density is 0.5-3.5A/dm2The pH value of the electroplating solution is 9-12, and the electroplating solution comprises the following components: copper sulfate pentahydrate, zinc sulfate, potassium sodium tartrate and sodium citrate, wherein the content of the copper sulfate pentahydrate is 2.5-25 g/L, and the mass concentration ratio of the zinc sulfate to the copper sulfate pentahydrate is (1-10): 1, the content of the potassium sodium tartrate is 50-200 g/L, and the content of the potassium sodium citrate is 10-30 g/L.
In the electroplating treatment, copper sulfate pentahydrate is used as main salt, and dissolved in water to dissociate copper ions (Cu 2)+) The copper ions are reduced to metallic copper (Cu) in the reaction2+(aq) + 2e-→ Cu (s)), adhered to the surface of the shading ring sheet to form copperAnd the nubby layer achieves the purpose of increasing the surface roughness of the shading ring sheet and is convenient for the adhesion of a matte structure in the subsequent process. The pH of the plating solution may also be adjusted by adding sodium hydroxide solution to the plating solution.
The zinc sulfate is used for increasing the conductivity of the electroplating solution; the potassium sodium tartrate and the sodium citrate are used as additives to stabilize the pH value of the plating solution and promote smooth reaction.
It can be understood that the proportion of each component and the current in the electroplating treatment process can be adjusted according to actual requirements, so that copper nodule layers with different degrees can be obtained. And after the electroplating treatment is finished, the shading ring sheet needs to be washed for 1-3 times to remove the electroplating solution attached to the surface of the shading ring sheet. And drying the shading ring sheet for 10-30 minutes in a vacuum environment below 150 ℃.
In the electroplating treatment, as zinc sulfate is dissolved in water to dissociate zinc ions, the zinc sulfate can also be reduced into metal zinc or form a zinc-copper alloy with the metal copper, the metal zinc is attached to the surface of the shading ring sheet, the metal zinc is easy to oxidize and corrode to influence the quality of a plating layer, and the zinc-copper alloy can be removed by adopting a dealloying treatment, wherein the dealloying treatment specifically comprises the following two methods:
(1) placing the shading ring sheet in a sulfuric acid or hydrochloric acid solution with a certain concentration to corrode for 1-48 hours;
(2) placing the shading ring piece into electrolyte for electrochemical corrosion, wherein the electrochemical corrosion temperature is 20-50 ℃, the time is 30 seconds-5 minutes, and the current density is 0.5-4A/dm2And the electrolyte is a sodium chloride solution.
Further, after the dealloying treatment is finished, whether the metal zinc in the coating is completely removed or not can be detected through element analysis, and if the existence of the zinc element is detected, the dealloying treatment process is repeated until the existence of the zinc element is not detected in the coating.
S5: and activating the shading ring sheet subjected to the electroplating treatment by using an activating agent so as to increase the activity of the surface of the shading ring sheet.
The activation treatment can increase the activity of the surface of the shading ring sheet and prepare for the subsequent process. The activating agent is prepared from 98% concentrated sulfuric acid and water according to the weight ratio of 1: 3, and the activation treatment time is 10 seconds to 10 minutes.
And after the activation treatment is finished, the shading ring sheet needs to be washed for 1-3 times to remove the activating agent attached to the surface of the shading ring sheet.
S6: and carrying out blackening treatment on the activated shading ring sheet by using blackening liquid so as to change the color of the surface of the shading ring sheet.
Specifically, the blackening treatment time is 5 seconds to 20 minutes, and the temperature is 50 ℃ to 100 ℃. The blackening solution is prepared from a blackening agent and water according to a mass ratio of 0.1-5, wherein the blackening agent comprises the following components in percentage by mass: 85-95% of sodium hydroxide, 5-8% of potassium persulfate and 2-7% of ammonium bicarbonate, wherein the total weight of the blackening agent is calculated by weight percentage. The purpose of blackening treatment is to change the color of the shading ring sheet on the basis of ensuring the anti-stripping, corrosion-resistant and anti-oxidation performances of the shading ring sheet, so as to achieve the purpose of shielding light. Specifically, the principle of the blackening treatment is as follows: in an alkaline solution, potassium persulfate oxidizes copper into copper oxide, the copper oxide is black and is extremely difficult to dissolve in water, and the copper oxide generated by the reaction forms a compact film to be attached to the surface of the shading ring piece, so that the appearance of the shading ring piece is matte black.
During the blackening treatment, the color change of the shading ring sheet is observed from light brown → dark brown → blue → black. In the blackening process, the shading ring sheet needs to be shaken or moved to ensure that the shading ring sheet is in sufficient contact with the blackening agent so as to fully perform the reaction. Preferably, in the blackening treatment process, the shading ring sheet can be taken out for observation, and the shading ring sheet is taken out to be washed for 1-3 times when the color meets the requirement so as to remove the blackening agent attached to the surface of the shading ring sheet and avoid falling or separation caused by overlarge thickness of the film due to excessive reaction. In addition, sodium hydroxide in the blackening solution is not consumed, and the continuous reaction can be ensured only by supplementing potassium persulfate, so that resources are saved.
S7: and drying the shading ring sheet subjected to blackening treatment under the vacuum condition of less than 200 ℃ to obtain a finished product of the rolled copper shading ring sheet.
And (3) putting the shading ring sheet subjected to blackening treatment into a vacuum oven for drying, and ending the process to obtain a finished product of the calendered copper shading ring sheet.
Example one
The invention provides a preparation method of a rolled copper shading ring sheet, which comprises the following steps:
(1) providing a molded shade ring sheet made of a calendered copper material.
(2) After water washing, the shading ring sheet is subjected to acetone ultrasonic cleaning for 10 minutes, and ethanol ultrasonic cleaning for 20 minutes, so that a rolling oil film attached to the surface of the shading ring sheet is removed.
(3) And after washing, polishing the shading ring sheet subjected to oil removal treatment by using copper polishing solution to remove the concave-convex structure on the surface of the shading ring sheet, wherein the polishing treatment time is 5 minutes.
(4) After washing, placing the polished shading ring sheet in electroplating solution for electroplating treatment to attach a layer of copper nodule layer on the surface of the shading ring sheet to increase the roughness of the surface of the shading ring sheet, wherein the electroplating treatment temperature is 25 ℃, the time is 5 minutes, the pH value of the electroplating solution is 9.0, and the current density is 0.2A/dm2The electroplating solution comprises the following components in percentage by weight: 17.5g/L of blue vitriol, 11.3g/L of zinc sulfate, 100g/L of potassium sodium tartrate and 18g/L of potassium sodium citrate.
(5) After washing, activating the electroplated shading ring sheet by using an activating agent to increase the activity of the surface of the shading ring sheet, wherein the activating treatment time is 3 minutes, and the activating agent is prepared by mixing 98% concentrated sulfuric acid and water according to the ratio of 1: 3, is arranged.
(6) After washing, carrying out blackening treatment on the activated shading ring sheet by using a blackening solution to change the surface color of the shading ring sheet, wherein the blackening treatment time is 15 minutes, the temperature is 80 ℃, and the blackening solution is prepared from a blackening agent and water according to the ratio of 1: 1, and the blackening agent comprises the following components in percentage by mass: 90% sodium hydroxide, 8% potassium persulfate and 2% ammonium bicarbonate.
(7) And after washing, drying the shading ring sheet subjected to blackening treatment in a vacuum oven at 150 ℃ for 5 minutes to obtain a finished product of the rolled copper shading ring sheet.
Referring to fig. 2 (a-b), after electroplating, a layer of porous structure with "residual walls" is formed on the surface of the shading ring sheet, and after subsequent processing, the surface of the rolled copper shading ring sheet is a "needle" -shaped matte structure, and through experimental tests, the 0 ° reflectivity of the rolled copper shading ring sheet is 1.14%, and the scattering characteristics are relatively uniform, and are greatly reduced compared with the 0 ° reflectivity of the shading ring sheet made of a double matte black PET material in the related art; when the ultrasonic wave is used for vibration treatment, the matte structure on the surface of the rolled copper shading ring sheet has longer ultrasonic wave resistant time, which shows that the matte structure on the surface of the rolled copper shading ring sheet is stable in adhesion and is not easy to fall off.
Example two
The invention provides a preparation method of a rolled copper shading ring sheet, which comprises the following steps:
(1) providing a molded shade ring sheet made of a calendered copper material.
(2) After water washing, the shading ring sheet is subjected to acetone ultrasonic cleaning for 20 minutes, and ethanol ultrasonic cleaning for 50 minutes, so that a rolling oil film attached to the surface of the shading ring sheet is removed.
(3) After washing, polishing the shading ring sheet subjected to oil removal treatment by using copper polishing solution to remove the concave-convex structure on the surface of the shading ring sheet, wherein the polishing time is 1 minute.
(4) After washing, placing the polished shading ring sheet in electroplating solution for electroplating treatment so as to attach a layer of copper nodule layer on the surface of the shading ring sheet and increase the surface of the shading ring sheetWherein the temperature of the plating treatment is 35 ℃ for 3 minutes, the pH of the plating solution is 11.0, and the current density is 1.5A/dm2The electroplating solution comprises the following components in percentage by weight: 17.5g/L of blue vitriol, 21.0g/L of zinc sulfate, 180g/L of potassium sodium tartrate and 23g/L of potassium sodium citrate.
(5) After washing, activating the electroplated shading ring sheet by using an activating agent to increase the activity of the surface of the shading ring sheet, wherein the activating treatment time is 5 minutes, and the activating agent is prepared by mixing 98% concentrated sulfuric acid and water according to the ratio of 1: 3, is arranged.
(6) After washing, carrying out blackening treatment on the activated shading ring sheet by using a blackening solution to change the surface color of the shading ring sheet, wherein the blackening treatment time is 5 minutes, the temperature is 50 ℃, and the blackening solution is prepared from a blackening agent and water according to the ratio of 1: 2, and the blackening agent comprises the following components in percentage by mass: 90% sodium hydroxide, 8% potassium persulfate and 2% ammonium bicarbonate.
(7) And after washing, drying the shading ring sheet subjected to blackening treatment in a vacuum oven at 150 ℃ for 5 minutes to obtain a finished product of the rolled copper shading ring sheet.
Referring to fig. 3 (a-b), after electroplating, a porous structure with many recesses and protrusions is formed on the surface of the shading ring sheet, and after subsequent processing, the surface of the calendered copper shading ring sheet is a "needle" -shaped matte structure, and through experiments, the 0 ° reflectivity of the calendered copper shading ring sheet is 0.75%, and the scattering property is relatively uniform, which is greatly reduced compared with the 0 ° reflectivity of the shading ring sheet made of a double matte black PET material in the related art; when the ultrasonic wave is used for vibration treatment, the matte structure on the surface of the rolled copper shading ring sheet has longer ultrasonic wave resistant time, which shows that the matte structure on the surface of the rolled copper shading ring sheet is stable in adhesion and is not easy to fall off.
EXAMPLE III
The invention provides a preparation method of a rolled copper shading ring sheet, which comprises the following steps:
(1) providing a molded shade ring sheet made of a calendered copper material.
(2) After water washing, the shading ring sheet is subjected to ultrasonic cleaning for 30 minutes by acetone and 60 minutes by ethanol so as to remove a rolling oil film attached to the surface of the shading ring sheet.
(3) And after washing, polishing the light shielding ring sheet subjected to oil removal treatment by using copper polishing solution to remove the concave-convex structure on the surface of the light shielding ring sheet, wherein the polishing treatment time is 5 seconds.
(4) After washing, placing the polished shading ring sheet in electroplating solution for electroplating treatment to attach a layer of copper nodule layer on the surface of the shading ring sheet to increase the roughness of the surface of the shading ring sheet, wherein the electroplating treatment temperature is 40 ℃, the time is 1 minute, the pH value of the electroplating solution is 12.0, and the current density is 3.0A/dm2The electroplating solution comprises the following components in percentage by weight: 17.5g/L of blue vitriol, 33.9g/L of zinc sulfate, 80g/L of potassium sodium tartrate and 30g/L of potassium sodium citrate.
(5) After washing, activating the electroplated shading ring sheet by using an activating agent to increase the activity of the surface of the shading ring sheet, wherein the activating treatment time is 10 minutes, and the activating agent is prepared by mixing 98% concentrated sulfuric acid and water according to the ratio of 1: 3 mass ratio.
(6) After washing, carrying out blackening treatment on the activated shading ring sheet by using a blackening solution to change the surface color of the shading ring sheet, wherein the blackening treatment time is 30 seconds, the temperature is 100 ℃, and the blackening solution is prepared from a blackening agent and water according to the ratio of 2: 1, and the blackening agent comprises the following components in percentage by mass: 90% sodium hydroxide, 8% potassium persulfate and 2% ammonium bicarbonate.
(7) And after washing, drying the shading ring sheet subjected to blackening treatment for 5 minutes under the vacuum condition of 150 ℃ to obtain a finished product of the rolled copper shading ring sheet.
Referring to fig. 4 (a-b), after electroplating, a porous structure with cavities and a small number of unevenness is generated on the surface of the shading ring sheet, and after subsequent processing, the surface of the calendered copper shading ring sheet is a "needle" -shaped matte structure, and through experiments, the 0 ° reflectivity of the calendered copper shading ring sheet is 0.90%, and the scattering property is relatively uniform, and is greatly reduced compared with the 0 ° reflectivity of the shading ring sheet made of the double matte black PET material in the related art; when the ultrasonic wave is used for vibration treatment, the matte structure on the surface of the rolled copper shading ring sheet has longer ultrasonic wave resistant time, which shows that the matte structure on the surface of the rolled copper shading ring sheet is stable in adhesion and is not easy to fall off.
By comprehensively analyzing the experimental data of the first to third embodiments, it can be seen that the method for preparing the calendered copper shading ring sheet provided by the invention has the advantages of simple process and strong feasibility, the surface of the prepared calendered copper shading ring sheet is of a matte structure, the surface is uniformly blackened, the structure is stable, the rolled copper shading ring sheet is not easy to fall off, and the 0-degree reflectivity of the calendered copper shading ring sheet is maintained at a lower level, so that the shading requirement of a high-precision optical device can be met.
The invention also provides a rolled copper shading ring sheet which is formed by adopting the preparation method of the rolled copper shading ring sheet, the surface of the rolled copper shading ring sheet is of a matte structure, the surface is uniformly blackened, the structure is stable, the rolled copper shading ring sheet is not easy to fall off, the 0-degree reflectivity of the rolled copper shading ring sheet is maintained at a lower level, and the shading requirement of a high-precision optical device can be met.
Compared with the prior art, the preparation method of the calendered copper shading ring sheet provided by the invention has the advantages that the calendered copper material is adopted to prepare the shading ring sheet, and the finished product of the calendered copper shading ring sheet is obtained through the processes of oil removal, polishing, electroplating, activation, blackening, drying and the like, and the calendered copper shading ring sheet avoids the defects that the PET shading ring sheet in the prior art is not easy to conduct electricity and does not resist high temperature, and has the advantages of easy blackening and low reflectivity; meanwhile, the roughness of the surface of the calendered copper shading ring sheet is increased by attaching a copper nodule layer, so that the matte black structure is stable and is not easy to fall off.
While the foregoing is directed to embodiments of the present invention, it will be understood by those skilled in the art that various changes may be made without departing from the spirit and scope of the invention.
Claims (6)
1. The preparation method of the rolled copper shading ring sheet is characterized by comprising the following steps:
providing a formed shading ring sheet, wherein the shading ring sheet is made of a rolled copper material;
carrying out oil removal treatment on the shading ring sheet to remove a rolling oil film attached to the surface of the shading ring sheet;
polishing the shading ring sheet subjected to oil removal treatment by using polishing liquid to remove the concave-convex structure on the surface of the shading ring sheet;
placing the polished shading ring sheet in an electroplating solution for electroplating treatment to attach a layer of copper nodule layer on the surface of the shading ring sheet so as to increase the roughness of the surface of the shading ring sheet, wherein the electroplating treatment is carried out at the temperature of 20-50 ℃ for 30 seconds-5 minutes, and the current density is 0.5-3.5A/dm2The pH value of the electroplating solution is 9-12, and the electroplating solution comprises the following components: the copper sulfate pentahydrate, the zinc sulfate, the potassium sodium tartrate and the sodium citrate, wherein the content of the copper sulfate pentahydrate is 2.5-25 g/L, and the mass concentration ratio of the zinc sulfate to the copper sulfate pentahydrate is (1-10): 1, the content of the potassium sodium tartrate is 50-200 g/L, and the content of the potassium sodium citrate is 10-30 g/L;
activating the shading ring sheet subjected to electroplating treatment by using an activating agent so as to increase the activity of the surface of the shading ring sheet;
carrying out blackening treatment on the activated shading ring sheet by using blackening liquid so as to change the color of the surface of the shading ring sheet;
drying the shading ring sheet subjected to blackening treatment under the vacuum condition of less than 200 ℃ to obtain a finished product of the calendered copper shading ring sheet;
the blackening treatment time is 5 seconds to 20 minutes, the temperature is 50 ℃ to 100 ℃, the blackening solution is prepared from a blackening agent and water according to a mass ratio of 0.1 to 5, and the blackening agent comprises the following components in percentage by mass: 85-95% of sodium hydroxide, 5-8% of potassium persulfate and 2-7% of ammonium bicarbonate, wherein the total weight of the blackening agent is calculated by hundred percent;
the oil removing treatment specifically comprises the following steps: ultrasonic cleaning is carried out for 10-30 minutes by adopting acetone, and ultrasonic cleaning is carried out for 20-60 minutes by adopting ethanol;
the polishing solution is copper polishing solution;
the activating agent is prepared from 98% concentrated sulfuric acid and water according to the weight ratio of 1: 3, and the activation treatment time is 10 seconds to 10 minutes.
2. The method as set forth in claim 1, wherein air agitation of the plating solution is required in the plating treatment.
3. The method as claimed in claim 1, wherein the shading ring sheet is dried under vacuum condition of less than 150 ℃ for 10-30 minutes after the electroplating process.
4. The method according to claim 1, further comprising a de-alloying treatment after the electroplating treatment to remove the zinc metal attached to the surface of the light-shielding ring sheet, wherein the de-alloying treatment specifically comprises the following two methods:
placing the shading ring sheet in a sulfuric acid or hydrochloric acid solution with a certain concentration to corrode for 1-48 hours;
placing the shading ring piece into electrolyte for electrochemical corrosion, wherein the electrochemical corrosion temperature is 20-50 ℃, the time is 30 seconds-5 minutes, and the current density is 0.5-4A/dm2And the electrolyte is a sodium chloride solution.
5. The method according to claim 1, further comprising a water washing process between two adjacent steps, wherein the water washing process lasts for 1-3 times.
6. A rolled copper shading ring sheet, characterized in that the rolled copper shading ring sheet is prepared by the method of any one of claims 1 to 5.
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