CN108677231A - Roll copper darkening ring piece preparation method and calendering copper darkening ring piece - Google Patents
Roll copper darkening ring piece preparation method and calendering copper darkening ring piece Download PDFInfo
- Publication number
- CN108677231A CN108677231A CN201810417823.2A CN201810417823A CN108677231A CN 108677231 A CN108677231 A CN 108677231A CN 201810417823 A CN201810417823 A CN 201810417823A CN 108677231 A CN108677231 A CN 108677231A
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- CN
- China
- Prior art keywords
- ring piece
- darkening ring
- darkening
- copper
- calendering copper
- Prior art date
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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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
Abstract
The present invention provides a kind of calendering copper darkening ring piece preparation method, and described method includes following steps：The molded darkening ring piece made of calendering copper product is provided；Oil removal treatment is carried out to darkening ring piece；Darkening ring piece is processed by shot blasting；Electroplating processes are carried out to darkening ring piece, one layer of copper wart layer of darkening ring piece electroplating surface is made to increase the roughness on darkening ring piece surface；Activation process is carried out to darkening ring piece；Darkening process is carried out to darkening ring piece, to change the color and luster on darkening ring piece surface；Processing is dried to darkening ring piece, obtains the finished product of calendering copper darkening ring piece.The present invention also provides a kind of calendering copper darkening ring pieces.Calendering copper darkening ring piece preparation method step provided by the invention is simple, exploitativeness is strong, mute black stable structure, calendering copper darkening ring piece preparation method not easily to fall off and of the invention and the calendering copper darkening ring piece of calendering copper darkening ring piece obtained also have the characteristics that easy melanism, simple for process, melanism back reflection rate is low.
Description
【Technical field】
The present invention relates to camera technology field more particularly to a kind of calendering copper darkening ring piece preparation method and calendering copper shadings
Enclose piece.
【Background technology】
With the fast development of science and technology, digital camera and the mobile phone rapid proliferation with digital camera, these light
Optical element used in instrument is learned gradually to be improved.Darkening ring piece is the optics member for regulating and controlling luminous flux in optical system
Part when ambient enters camera lens, can stop that unwanted light enters, to prevent via the darkening ring piece being arranged between the lenses
Solar flare or ghost image are only generated in photographed images.
In the related technology, darkening ring piece is made of Japan's SOMA light screening materials, this kind of material is double mute black gather to benzene
Naphthalate (Polyethylene terepHthalate, PET), and darkening ring piece presence made of the material is not easy
The defects of conduction, non-refractory, and the dumb light structure on darkening ring piece surface is easy aging and falls off, and influences shading performance.
Therefore, it is necessary to provide a kind of new calendering copper darkening ring piece preparation method and calendering copper darkening ring piece.
【Invention content】
A kind of that the purpose of the present invention is to provide steps is simple, exploitativeness is strong calendering copper darkening ring piece preparation method and
A kind of calendering copper darkening ring piece that performance is stablized.
In order to achieve the above object, the present invention provides a kind of calendering copper darkening ring piece preparation method, and the method includes such as
Lower step：
Molded darkening ring piece is provided, the darkening ring piece is made of calendering copper product；
Oil removal treatment is carried out to the darkening ring piece, to remove the rolling oil film of darkening ring piece surface attachment；
The darkening ring piece Jing Guo oil removal treatment is processed by shot blasting using polishing fluid, to remove the darkening ring piece
The concaveconvex structure on surface；
The darkening ring piece Jing Guo polishing treatment is placed in electroplate liquid and carries out electroplating processes, in the darkening ring piece
Surface adheres to one layer of copper wart layer and increases the roughness on darkening ring piece surface, wherein and the temperature of the electroplating processes is 20~
50 DEG C, the time is 30 seconds~5 minutes, and current density is 0.5~3.5A/dm2, the pH value 9~12 of the electroplate liquid, the plating
Liquid includes following component：The content of cupric sulfate pentahydrate, zinc sulfate, sodium potassium tartrate tetrahydrate and sodium citrate, the cupric sulfate pentahydrate is
2.5~25g/L, the zinc sulfate and the cupric sulfate pentahydrate and the ratio between mass concentration be (1~10)：1, the potassium tartrate
The content of sodium is 50~200g/L, and the content of the potassium citrate sodium is 10~30g/L；
Activation process is carried out to the darkening ring piece Jing Guo electroplating processes using activator, to increase the darkening ring piece
The activity on surface；
Darkening process is carried out to the darkening ring piece after activation using blackening liquid, to change darkening ring piece surface
Color and luster；
To processing is dried by the darkening ring piece of Darkening process under the vacuum condition less than 200 DEG C, obtain
The finished product of the calendering copper darkening ring piece.
Preferably, it needs to carry out air stirring to the electroplate liquid in the electroplating processes.
Preferably, it is needed after the electroplating processes darkening ring piece is dry under the vacuum condition less than 150 DEG C
10~30 minutes.
Preferably, further include alloy treatment after the electroplating processes, to remove the attachment of darkening ring piece surface
Metallic zinc or pltine, it is described that alloy treatment is gone to specifically include the following two kinds method：
(1) the darkening ring piece is placed in certain density sulfuric acid or hydrochloric acid solution and is corroded 1~48 hour；
(2) the darkening ring piece is placed in electrolyte and carries out electrochemical corrosion, wherein the temperature of the electrochemical corrosion
It it is 20~50 DEG C, the time is 30 seconds~5 minutes, and current density is 0.5~4A/dm2, the electrolyte is sodium chloride solution.
Preferably, the time of the Darkening process be 5 seconds~20 minutes, temperature be 50 DEG C~100 DEG C, the blackening liquid by
Black agent is formed with water by quality proportioning, the mass values ranging from 0.1~5 of black agent and water, wherein the black agent includes
Following component by percentage to the quality：85~95% sodium hydroxide, 5~8% potassium peroxydisulfate and 2~7% bicarbonate
Ammonium, by the black agent gross weight very in terms of.
Preferably, the oil removal treatment is specially：Using acetone ultrasonic cleaning 10~30 minutes, EtOH Sonicate ripple cleaning
20~60 minutes.
Preferably, the polishing fluid is copper polishing fluid.
Preferably, the activator by a concentration of 98% concentrated sulfuric acid and water according to 1：3 mass ratio configures, described
The time of activation process is 10 seconds~10 minutes.
Preferably, further include water-washing process between adjacent two step, the water-washing process continues 1~3 time.The present invention is also
A kind of calendering copper darkening ring piece is provided, the calendering copper darkening ring piece prepared using the calendering copper darkening ring piece preparation method and
At.
Compared with the relevant technologies, calendering copper darkening ring piece preparation method provided by the invention is made of calendering copper product
Darkening ring piece, and by flows such as oil removing, polishing, plating, activation, melanism, dryings, the finished product of calendering copper darkening ring piece is obtained,
The calendering copper darkening ring piece evaded in the related technology PET darkening rings piece not easy conductive, non-refractory the shortcomings that, have be easy to
The low advantage of melanism, reflectivity；Roll copper darkening ring piece surface simultaneously and increases the darkening ring piece table by adhering to copper wart layer
The roughness in face so that mute black stable structure, not easily to fall off.
【Description of the drawings】
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing, wherein：
Fig. 1 is the flow chart of calendering copper darkening ring piece preparation method provided by the invention；
Fig. 2 a amplify 10,000 times for obtained darkening ring piece surface after one electroplating processes of the embodiment of the present invention under Electronic Speculum
Micro-structure diagram；
Fig. 2 b are that 50,000 times microcosmic is amplified on the obtained calendering copper darkening ring piece surface of the embodiment of the present invention one under Electronic Speculum
Structure chart；
10,000 times micro- is amplified on obtained darkening ring piece surface under Electronic Speculum after two electroplating processes of Fig. 3 a embodiment of the present invention
See structure chart；
Fig. 3 b are that 50,000 times microcosmic is amplified on the obtained calendering copper darkening ring piece surface of the embodiment of the present invention two under Electronic Speculum
Structure chart；
Fig. 4 a amplify 10,000 times for obtained darkening ring piece surface after three electroplating processes of the embodiment of the present invention under Electronic Speculum
Micro-structure diagram；
Fig. 4 b are that 50,000 times microcosmic is amplified on the obtained calendering copper darkening ring piece surface of the embodiment of the present invention three under Electronic Speculum
Structure chart.
【Specific implementation mode】
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that the described embodiments are merely a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts all other
Embodiment shall fall within the protection scope of the present invention.
Referring to Fig. 1, the present invention provides a kind of calendering copper darkening ring piece preparation method comprising following steps：
S1：Molded darkening ring piece is provided, the darkening ring piece is made of calendering copper product.
Calendering copper is to be rolled with copper ingot, then be made through forging the processes such as fiery, anti-oxidant, roughening treatment, rolls copper thickness
It is generally completely embedded between 5um~135um, molecule, has flexible, intensity is high, bendability, ductility, plating resistance, conductive
The features such as property is good, and lustrous surface is excellent；Moreover, rolled copper foil have low surface oxygen characteristic, can adhere to various different substrate materials,
Such as metal, insulating materials etc. possesses wider temperature use scope.The darkening ring piece made of calendering copper product can evade phase
The shortcomings that PET material darkening ring piece is ageing-resistant in the technology of pass, yielding, non-refractory, at the same have dimensionally stable, be easy it is black
Change, feature simple for process, melanism back reflection rate is low.
The darkening ring piece is washed to remove dust, impurity or the particulate matter of surface attachment, the water
It washes Cheng Chixu 1~3 time, then carries out subsequent handling.
S2：Oil removal treatment is carried out to the darkening ring piece, to remove the rolling oil film of darkening ring piece surface attachment.
Due to calendering copper itself in the inherent characteristic of the production operation of rolling, determine that its double surface is rolled with larger amount of
Liquefaction film, the oil content on double surfaces is up to 5mg/m2More than, it has seriously affected its product export requirement and it is follow-up required
The progress of chemistry and electrochemical surface treatment process.The darkening ring piece made of calendering copper product needs the ROLLING OIL to its surface
Film carries out oil removal treatment, to facilitate the progress of subsequent handling.
The oil removal treatment is specially：Using acetone ultrasonic cleaning 10~30 minutes, EtOH Sonicate ripple cleaning 20~60
Minute.Acetone and ethyl alcohol are the organic solvent of environment-friendly type, can be reused, and oil removal efficiency is high, effect is good, is aided with super
Sound wave can be reinforced cleaning deoiling effect, so that oil removing cleaning efficiency is greatly improved, also make oil removing scavenging period significantly
Shorten.
It after the completion of oil removal treatment, needs to carry out washing 1~3 time to the darkening ring piece, to remove the darkening ring piece table
The acetone/ethanol solution of face attachment.
S3：The darkening ring piece Jing Guo oil removal treatment is processed by shot blasting using polishing fluid, to remove the shading
Enclose the concaveconvex structure on piece surface.
Polishing treatment can make the darkening ring surfacing, light.Preferably, the polishing fluid is copper polishing fluid,
Using existing commercially available copper polishing fluid.
It after the completion of polishing treatment, needs to carry out washing 1~3 time to the darkening ring piece, to remove the darkening ring piece table
The polishing fluid of face attachment.
S4：The darkening ring piece Jing Guo polishing treatment is placed in electroplate liquid and carries out electroplating processes, in the shading
The roughness that one layer of copper wart layer increases darkening ring piece surface is adhered on circle piece surface.
Specifically, the temperature of the electroplating processes be 20~50 DEG C, the time be 30 seconds~5 minutes, current density be 0.5~
3.5A/dm2, the pH value 9~12 of the electroplate liquid, the electroplate liquid includes following component：Cupric sulfate pentahydrate, zinc sulfate, winestone
Sour potassium sodium and sodium citrate, wherein the content of the cupric sulfate pentahydrate is 2.5~25g/L, the zinc sulfate and the five water sulphur
Sour copper and the ratio between mass concentration be (1~10)：1, the content of the sodium potassium tartrate tetrahydrate is 50~200g/L, the citric acid
The content of potassium sodium is 10~30g/L.
In electroplating processes, cupric sulfate pentahydrate is dissolved in hydrolytic dissociation and goes out copper ion (Cu2 as main salt+), copper ion is in the reaction
It is reduced into metallic copper (Cu2+(aq)+2e-→ Cu (s)), it is attached to darkening ring piece surface, copper wart layer is formed, reaches increase
The purpose of the darkening ring piece surface roughness, convenient for the attachment of dumb light structure in subsequent technique.It can be in the electroplate liquid
The pH value of the electroplate liquid is adjusted by the way that sodium hydroxide solution is added.
The zinc sulfate is used to increase the conductivity of the electroplate liquid；The sodium potassium tartrate tetrahydrate and the sodium citrate conduct
Additive can be used for stablizing the pH value in the electroplate liquid, promote the steady progress of reaction.
It is understood that according to actual needs, the ratio and electric current of each component in the electroplating processes process is adjusted
Size, different degrees of copper wart layer can be obtained.After the completion of electroplating processes, need to carry out washing 1~3 to the darkening ring piece
Time, to remove the electroplate liquid of darkening ring piece surface attachment.And to the darkening ring piece in 150 DEG C of vacuum environments below
It is 10~30 minutes dry.
In the electroplating processes, go out zinc ion since zinc sulfate is dissolved in hydrolytic dissociation, can also be reduced into metallic zinc or
Pltine is formed with the metallic copper, is attached to darkening ring piece surface, the metallic zinc and the pltine are easy
By oxidation corrosion, the quality of coating is influenced, alloy treatment can be used and remove, it is described that alloy treatment is gone to specifically include the following two kinds
Method：
(1) the darkening ring piece is placed in certain density sulfuric acid or hydrochloric acid solution and is corroded 1~48 hour；
(2) the darkening ring piece is placed in electrolyte and carries out electrochemical corrosion, wherein the temperature of the electrochemical corrosion
It it is 20~50 DEG C, the time is 30 seconds~5 minutes, and current density is 0.5~4A/dm2, the electrolyte is sodium chloride solution.
Further, after going alloy treatment, whether complete the metallic zinc in coating can be detected by elemental analysis
Full removal, if detecting the presence of Zn-ef ficiency, repeat it is described go alloy treatment process, until Zn-ef ficiency is not detected in coating
Presence.
S5：Activation process is being carried out to the darkening ring piece Jing Guo electroplating processes using activator, to increase the screening
The activity on iris diaphragm plate surface.
Activation process can increase the activity on darkening ring piece surface, prepare for subsequent handling.The activator by
A concentration of 98% concentrated sulfuric acid is with water according to 1：3 mass ratio configures, and the time of the activation process is 10 seconds~10 points
Clock.
It after the completion of activation process, needs to carry out washing 1~3 time to the darkening ring piece, to remove the darkening ring piece table
The activator of face attachment.
S6：Darkening process is carried out to the darkening ring piece after activation using blackening liquid, to change the darkening ring piece table
The color and luster in face.
Specifically, the time of the Darkening process is 5 seconds~20 minutes, temperature is 50 DEG C~100 DEG C.The blackening liquid by
Black agent is formed with water by quality proportioning, the mass values ranging from 0.1~5 of black agent and water, wherein the black agent includes
Following component by percentage to the quality：85~95% sodium hydroxide, 5~8% potassium peroxydisulfate and 2~7% bicarbonate
Ammonium, by the black agent gross weight very in terms of.The purpose of Darkening process be to ensure the darkening ring piece antistripping, it is corrosion-resistant,
The color and luster for changing the darkening ring piece on the basis of oxidation proof propertiess, achievees the purpose that shield lights.Specifically, at the melanism
The principle of reason is：In alkaline solution, copper is oxidized to copper oxide by potassium peroxydisulfate, and copper oxide is in black, it is extremely difficult to be dissolved in water, react
The copper oxide of generation forms one layer of fine and close film and is attached to darkening ring piece surface, makes the appearance of the darkening ring piece in mute black
Shape.
In blackening treatment process, it is observed that the color and luster variation of the darkening ring piece is by shallow brown → deep brown → blue → black.
It should be noted that needing that the darkening ring piece is shaken or moved in blackening treatment process, ensure the darkening ring
Piece and black agent come into full contact with, and are carried out with reacting fully.It preferably, can also be by the screening in blackening treatment process
Iris diaphragm plate takes out observation, and color and luster, which reaches requirement and takes out, carries out washing 1~3 time, is adhered to remove darkening ring piece surface
Black agent avoids the excessive of reaction from carrying out causing the thickness of film is excessive to cause to fall off or detach.Furthermore sodium hydroxide in blackening liquid
It is not consumed, it is only necessary to supplement the lasting progress that potassium peroxydisulfate ensures that reaction, economize on resources.
S7：To processing is dried by the darkening ring piece of Darkening process under the vacuum condition less than 200 DEG C, obtain
To the finished product of the calendering copper darkening ring piece.
The darkening ring piece after Darkening process is put into vacuum drying oven and is dried, flow terminates, and obtains institute
State the finished product of calendering copper darkening ring piece.
Embodiment one
The present invention provides a kind of calendering copper darkening ring piece preparation method comprising following steps：
(1) molded darkening ring piece is provided, the darkening ring piece is made of calendering copper product.
(2) after washing, acetone ultrasonic cleaning is used 10 minutes to the darkening ring piece, EtOH Sonicate ripple cleans 20 points
Clock, to remove the rolling oil film of darkening ring piece surface attachment.
(3) after washing, the darkening ring piece Jing Guo oil removal treatment is processed by shot blasting using copper polishing fluid, to go
Except the concaveconvex structure on darkening ring piece surface, the time of the polishing treatment is 5 minutes.
(4) after washing, the darkening ring piece Jing Guo polishing treatment is placed in electroplate liquid and carries out electroplating processes, in institute
It states darkening ring piece surface and adheres to the roughness that one layer of copper wart layer increases darkening ring piece surface, the temperature of the electroplating processes is
25 DEG C, the time is 5 minutes, and the pH value of the electroplate liquid is 9.0, current density 0.2A/dm2, each component in the electroplate liquid
Content be：Cupric sulfate pentahydrate 17.5g/L, zinc sulfate 11.3g/L, sodium potassium tartrate tetrahydrate 100g/L and potassium citrate sodium 18g/L.
(5) after washing, using activator to the darkening ring piece activation process Jing Guo electroplating processes, to increase the screening
The time of the activity on iris diaphragm plate surface, the activation process is 3 minutes, and the activator is by 98% concentrated sulfuric acid with water according to 1：
3 mass ratio configures.
(6) after washing, Darkening process is carried out to the darkening ring piece after activation using blackening liquid, to change the shading
The color and luster on piece surface is enclosed, the time of the Darkening process is 15 minutes, and temperature is 80 DEG C, and the blackening liquid is pressed by black agent and water
According to 1：1 mass ratio configures, and the black agent includes following component by percentage to the quality：90% sodium hydroxide,
8% potassium peroxydisulfate and 2% ammonium hydrogen carbonate.
(7) after washing, to processing is dried by the darkening ring piece of Darkening process in 150 DEG C of vacuum drying oven
5 minutes, obtain the finished product of the calendering copper darkening ring piece.
Please refer to Fig. 2 (a~b), one layer of " rubble " vesicular texture of the darkening ring piece Surface Creation after electroplating processes, warp
The dumb light structure that the calendering copper darkening ring piece surface obtained after subsequent processing is " needle " shape is crossed, the calendering copper is measured by experiment
0 ° of reflectivity of darkening ring piece is 1.14%, and scattering properties is relatively uniform, compared to double mute black PET material systems in the related technology
At darkening ring piece 0 ° of reflectivity have be greatly reduced；When carrying out vibrations processing with ultrasonic wave, the calendering copper darkening ring piece
The resistance to sonication times of dumb light structure on surface are longer, illustrate that the dumb light structure attachment on the calendering copper darkening ring piece surface is stablized,
It is not easily to fall off.
Embodiment two
The present invention provides a kind of calendering copper darkening ring piece preparation method comprising following steps：
(1) molded darkening ring piece is provided, the darkening ring piece is made of calendering copper product.
(2) after washing, acetone ultrasonic cleaning is used 20 minutes to the darkening ring piece, EtOH Sonicate ripple cleans 50 points
Clock, to remove the rolling oil film of darkening ring piece surface attachment.
(3) after washing, the darkening ring piece Jing Guo oil removal treatment is processed by shot blasting using copper polishing fluid, to go
Except the concaveconvex structure on darkening ring piece surface, the time of the polishing treatment is 1 minute.
(4) after washing, the darkening ring piece Jing Guo polishing treatment is placed in electroplate liquid and carries out electroplating processes, in institute
It states darkening ring piece surface and adheres to the roughness that one layer of copper wart layer increases darkening ring piece surface, the temperature of wherein electroplating processes is
35 DEG C, the time is 3 minutes, and the pH value of the electroplate liquid is 11.0, current density 1.5A/dm2, each component in the electroplate liquid
Content be：Cupric sulfate pentahydrate 17.5g/L, zinc sulfate 21.0g/L, sodium potassium tartrate tetrahydrate 180g/L and potassium citrate sodium 23g/L.
(5) after washing, using activator to the darkening ring piece activation process Jing Guo electroplating processes, to increase the screening
The time of the activity on iris diaphragm plate surface, the activation process is 5 minutes, and the activator is by 98% concentrated sulfuric acid with water according to 1：
3 mass ratio configures.
(6) after washing, Darkening process is carried out to the darkening ring piece after activation using blackening liquid, to change the shading
The color and luster on piece surface is enclosed, the time of the Darkening process is 5 minutes, and temperature is 50 DEG C, and the blackening liquid is pressed by black agent and water
According to 1：2 mass ratio configures, and the black agent includes following component by percentage to the quality：90% sodium hydroxide,
8% potassium peroxydisulfate and 2% ammonium hydrogen carbonate.
(7) after washing, to processing is dried by the darkening ring piece of Darkening process in 150 DEG C of vacuum drying oven
5 minutes, obtain the finished product of the calendering copper darkening ring piece.
Fig. 3 (a~b) is please referred to, one layer of the darkening ring piece Surface Creation is more concave-convex containing cavity after electroplating processes
Uneven vesicular texture, the calendering copper darkening ring piece surface obtained after subsequent processing are the dumb light structure of " needle " shape, are led to
It is 0.75% to cross experiment and measure 0 ° of reflectivity of the calendering copper darkening ring piece, and scattering properties is relatively uniform, compared to related skill
0 ° of reflectivity of darkening ring piece made of double mute black PET materials, which has, in art is greatly reduced；Vibrations processing is carried out with ultrasonic wave
When, the resistance to sonication times of dumb light structure on the calendering copper darkening ring piece surface are longer, illustrate the calendering copper darkening ring piece table
The dumb light structure attachment in face is stablized, not easily to fall off.
Embodiment three
The present invention provides a kind of calendering copper darkening ring piece preparation method comprising following steps：
(1) molded darkening ring piece is provided, the darkening ring piece is made of calendering copper product.
(2) after washing, acetone ultrasonic cleaning is used 30 minutes to the darkening ring piece, EtOH Sonicate ripple cleans 60 points
Clock, to remove the rolling oil film of darkening ring piece surface attachment.
(3) after washing, the darkening ring piece Jing Guo oil removal treatment is processed by shot blasting using copper polishing fluid, to go
Except the concaveconvex structure on darkening ring piece surface, the time of the polishing treatment is 5 seconds.
(4) after washing, the darkening ring piece Jing Guo polishing treatment is placed in electroplate liquid and carries out electroplating processes, in institute
It states darkening ring piece surface and adheres to the roughness that one layer of copper wart layer increases darkening ring piece surface, the temperature of the electroplating processes is
40 DEG C, the time is 1 minute, and the pH value of the electroplate liquid is 12.0, current density 3.0A/dm2, each component in the electroplate liquid
Content be：Cupric sulfate pentahydrate 17.5g/L, zinc sulfate 33.9g/L, sodium potassium tartrate tetrahydrate 80g/L and potassium citrate sodium 30g/L.
(5) after washing, using activator to the darkening ring piece activation process Jing Guo electroplating processes, to increase the screening
The activity on iris diaphragm plate surface, time of the activation process are 10 minutes, the activator by 98% the concentrated sulfuric acid and water according to
1：3 mass ratioes configure.
(6) after washing, Darkening process is carried out to the darkening ring piece after activation using blackening liquid, to change the shading
The color and luster on piece surface is enclosed, the time of the Darkening process is 30 seconds, and temperature is 100 DEG C, and the blackening liquid is pressed by black agent and water
According to 2：1 mass ratio configures, and the black agent includes following component by percentage to the quality：90% sodium hydroxide,
8% potassium peroxydisulfate and 2% ammonium hydrogen carbonate.
(7) after washing, to processing is dried by the darkening ring piece of Darkening process under 150 DEG C of vacuum condition
5 minutes, obtain the finished product of the calendering copper darkening ring piece.
Fig. 4 (a~b) is please referred to, one layer of the darkening ring piece Surface Creation contains empty and a small amount of bumps after electroplating processes
Uneven vesicular texture, the calendering copper darkening ring piece surface obtained after subsequent processing are the dumb light structure of " needle " shape, are led to
It is 0.90% to cross experiment and measure 0 ° of reflectivity of the calendering copper darkening ring piece, and scattering properties is relatively uniform, compared to related skill
0 ° of reflectivity of darkening ring piece made of double mute black PET materials, which has, in art is greatly reduced；Vibrations processing is carried out with ultrasonic wave
When, the resistance to sonication times of dumb light structure on the calendering copper darkening ring piece surface are longer, illustrate the calendering copper darkening ring piece table
The dumb light structure attachment in face is stablized, not easily to fall off.
Comprehensive analysis embodiment one to embodiment three experimental data, it can be seen that calendering copper shading provided by the invention
Circle piece preparation method flow is simple, and exploitativeness is strong, and the calendering copper darkening ring piece surface obtained is dumb light structure, and surface is black
Change uniform and stable structure, not easily to fall off, 0 ° of reflectivity of the calendering copper darkening ring piece maintains reduced levels, Neng Gouman
The shading demand of sufficient high-precision optical device.
The present invention also provides a kind of calendering copper darkening ring piece, the calendering copper darkening ring piece uses the calendering copper darkening ring
Piece preparation method forms, and it is dumb light structure to roll copper darkening ring piece surface described in the calendering copper darkening ring piece, and surface melanism is equal
Even and stable structure, not easily to fall off, 0 ° of reflectivity of the calendering copper darkening ring piece maintains reduced levels, disclosure satisfy that height
The shading demand of resolution optical device.
Compared with the relevant technologies, calendering copper darkening ring piece preparation method provided by the invention is made of calendering copper product
Darkening ring piece, and by flows such as oil removing, polishing, plating, activation, melanism, dryings, the finished product of calendering copper darkening ring piece is obtained,
The calendering copper darkening ring piece evaded in the related technology PET darkening rings piece not easy conductive, non-refractory the shortcomings that, have be easy to
The low advantage of melanism, reflectivity；Roll copper darkening ring piece surface simultaneously and increases the darkening ring piece table by adhering to copper wart layer
The roughness in face so that mute black stable structure, not easily to fall off.
Above-described is only embodiments of the present invention, it should be noted here that for those of ordinary skill in the art
For, without departing from the concept of the premise of the invention, improvement can also be made, but these belong to the protection model of the present invention
It encloses.
Claims (10)
1. a kind of calendering copper darkening ring piece preparation method, which is characterized in that described method includes following steps：
Molded darkening ring piece is provided, the darkening ring piece is made of calendering copper product；
Oil removal treatment is carried out to the darkening ring piece, to remove the rolling oil film of darkening ring piece surface attachment；
The darkening ring piece Jing Guo oil removal treatment is processed by shot blasting using polishing fluid, to remove darkening ring piece surface
Concaveconvex structure；
The darkening ring piece Jing Guo polishing treatment is placed in electroplate liquid and carries out electroplating processes, on darkening ring piece surface
One layer of copper wart layer of attachment increases the roughness on darkening ring piece surface, wherein and the temperature of the electroplating processes is 20~50 DEG C,
Time is 30 seconds~5 minutes, and current density is 0.5~3.5A/dm2, the pH value 9~12 of the electroplate liquid, the electroplate liquid packet
Include following component：Cupric sulfate pentahydrate, zinc sulfate, sodium potassium tartrate tetrahydrate and sodium citrate, the content of the cupric sulfate pentahydrate is 2.5~
25g/L, the zinc sulfate and the cupric sulfate pentahydrate and the ratio between mass concentration be (1~10)：1, the sodium potassium tartrate tetrahydrate
Content is 50~200g/L, and the content of the potassium citrate sodium is 10~30g/L；
Activation process is carried out to the darkening ring piece Jing Guo electroplating processes using activator, to increase darkening ring piece surface
Activity；
Darkening process is carried out to the darkening ring piece after activation using blackening liquid, to change the color on darkening ring piece surface
Pool；
To processing is dried by the darkening ring piece of Darkening process under the vacuum condition less than 200 DEG C, obtain described
Roll the finished product of copper darkening ring piece.
2. according to the method described in claim 1, it is characterized in that, needing to carry out the electroplate liquid in the electroplating processes empty
Gas agitating.
3. according to the method described in claim 1, it is characterized in that, needing to exist the darkening ring piece after the electroplating processes
It is 10~30 minutes dry under vacuum condition less than 150 DEG C.
4. according to the method described in claim 1, it is characterized in that, the electroplating processes after further include alloy treatment, with
The metallic zinc or pltine of the attachment of darkening ring piece surface are removed, it is described that alloy treatment is gone to specifically include the following two kinds side
Method：
(1) the darkening ring piece is placed in certain density sulfuric acid or hydrochloric acid solution and is corroded 1~48 hour；
(2) the darkening ring piece is placed in electrolyte and carries out electrochemical corrosion, wherein the temperature of the electrochemical corrosion is 20
~50 DEG C, the time is 30 seconds~5 minutes, and current density is 0.5~4A/dm2, the electrolyte is sodium chloride solution.
5. according to the method described in claim 1, it is characterized in that, the time of the Darkening process be 5 seconds~20 minutes, temperature
It it is 50 DEG C~100 DEG C, the blackening liquid is formed with water by quality proportioning by black agent, and the mass values of black agent and water are ranging from
0.1~5, wherein the black agent includes following component by percentage to the quality：85~95% sodium hydroxide, 5~8%
Potassium peroxydisulfate and 2~7% ammonium hydrogen carbonate, by the black agent gross weight very in terms of.
6. according to the method described in claim 1, it is characterized in that, the oil removal treatment is specially：It is clear using acetone ultrasonic wave
It washes 10~30 minutes, EtOH Sonicate ripple is cleaned 20~60 minutes.
7. according to the method described in claim 1, it is characterized in that, the polishing fluid is copper polishing fluid.
8. according to the method described in claim 1, it is characterized in that, the activator is pressed by a concentration of 98% concentrated sulfuric acid with water
According to 1：3 mass ratio configures, and the time of the activation process is 10 seconds~10 minutes.
9. described according to the method described in claim 1, it is characterized in that, further include water-washing process between adjacent two step
Water-washing process continues 1~3 time.
10. a kind of calendering copper darkening ring piece, which is characterized in that the calendering copper darkening ring piece is using any one of claim 1~9
The method is prepared.
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