CN117210892A - Cyanide-free copper plating process - Google Patents
Cyanide-free copper plating process Download PDFInfo
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- CN117210892A CN117210892A CN202311234825.5A CN202311234825A CN117210892A CN 117210892 A CN117210892 A CN 117210892A CN 202311234825 A CN202311234825 A CN 202311234825A CN 117210892 A CN117210892 A CN 117210892A
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- Prior art keywords
- copper plating
- cyanide
- workpiece
- anode
- plating process
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- 238000007747 plating Methods 0.000 title claims abstract description 59
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 43
- 239000010949 copper Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 39
- 230000008569 process Effects 0.000 title claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000009713 electroplating Methods 0.000 claims abstract description 21
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims abstract description 14
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000027 potassium carbonate Inorganic materials 0.000 claims abstract description 7
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 6
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 239000013527 degreasing agent Substances 0.000 claims description 4
- 238000005237 degreasing agent Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 abstract description 9
- 230000001788 irregular Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000005282 brightening Methods 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000011253 protective coating Substances 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 244000137852 Petrea volubilis Species 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- Electroplating And Plating Baths Therefor (AREA)
Abstract
The application relates to the technical field of electroplating, in particular to a cyanide-free copper plating process. The adopted copper plating solution comprises 38-42g/L of copper sulfate, 3-8-42g/L of hydroxyethylidene diphosphonic acid, 58-62g/L of potassium carbonate, 9-11g/L of potassium hydroxide, 0.2-0.3mL/L of main gloss agent, 0.25-0.35mL/L of leveling agent and 0.2-0.3mL/L of cylinder opening agent. The adopted copper plating solution does not contain cyanide, has simple components, and eliminates the harm of cyanide-containing substances to human bodies and the environment; the added trace brightening agent, leveling agent and cylinder opening agent can ensure that the copper plating solution has better dispersion capability, and the uniformity of the thickness of the surface plating layer of the irregular spherical workpiece is improved.
Description
Technical Field
The application relates to the technical field of electroplating, in particular to a cyanide-free copper plating process.
Background
The special metal special-shaped spherical shell workpiece is easy to deform in the processing process, and a protective coating with a mould pressing shaping function is required to be coated for repairing the workpiece, so that the special metal special-shaped spherical shell workpiece can protect a coated part and repair microscopic deformation of the coated part. However, the special-shaped spherical shell workpiece has irregular appearance, the current distribution on the surface of the matrix is uneven in the electroplating process, and a uniform, smooth and bright plating layer with a certain function is difficult to obtain. Meanwhile, the existing special-shaped spherical shell workpiece surface protection technology still adopts a cyanide-containing electroplating technology, and has adverse effects on human health and environment.
Therefore, it is necessary to develop a cyanide-free copper plating process for special metal special-shaped spherical shell workpieces so as to prepare a protective coating with uniform and smooth appearance and better performance, and meanwhile, the cyanide pollution and harm caused by the traditional cyanide-containing process are eliminated.
Disclosure of Invention
The application aims to provide a cyanide-free copper plating process, which can prepare a uniform and flat protective coating on the surface of a special-shaped spherical shell workpiece, and the copper plating solution used does not contain cyanide, so that the process is more environment-friendly and healthy.
The cyanide-free copper plating process provided by the application adopts copper plating solution comprising 38-42g/L of copper sulfate, 3-8-42g/L of hydroxyethylidene diphosphonic acid, 58-62g/L of potassium carbonate, 9-11g/L of potassium hydroxide, 0.2-0.3mL of main gloss agent, 0.25-0.35mL/L of leveling agent and 0.2-0.3mL/L of cylinder opening agent.
Preferably, the main gloss agent is HR-510A, the leveling agent is HR-510B, and the cylinder opener is HR-510Mu.
Preferably, the copper plating solution includes 40g/L copper sulfate, 40g/L hydroxyethylidene diphosphonic acid, 60g/L potassium carbonate, 10g/L, HR-510A 0.25mL/L, HR-510B 0.3mL/L, HR-510mu0.25mL/L potassium hydroxide.
Preferably, the copper plating solution has a pH of 9.3.
Preferably, the method comprises the following steps:
(1) Polishing the workpiece to be electroplated to remove rust spots on the surface of the workpiece;
(2) Placing the polished workpiece into an oil removing agent for ultrasonic treatment;
(3) And (3) cleaning the workpiece subjected to ultrasonic treatment in the step (2) by water and alcohol, airing, and then placing the workpiece into the copper plating solution for electroplating.
Preferably, the polishing in the step (1) is sequentially carried out by adopting 600-2400 mesh sand paper; the degreasing agent in the step (2) is FKD-835D, and the ultrasonic treatment time is 20 minutes.
Preferably, the electroplating temperature in the step (3) is 44-45 ℃ and the current density is 15-16mA/cm 2 The cathode rotation period is 8-10 minutes.
Preferably, the workpiece in the step (1) is used as a cathode when electroplating, and the workpiece is hemispherical in shape, wherein a hemispherical cavity is formed at the hemispherical plane end.
Preferably, in the step (3), a profiling anode is adopted for electroplating, the profiling anode comprises a first anode and a second anode, the shape of the bottom of the first anode is matched with the shape of the plane end of the workpiece, and the shape of the second anode is matched with the shape of the spherical outer surface of the workpiece to be electroplated.
Preferably, in the step (3), the first anode and the second anode are adopted for electroplating for 100 minutes, and then the first anode is adopted for plating for 20 minutes.
In summary, the application has the following advantages:
the copper plating solution adopted in the cyanide-free copper plating process provided by the application does not contain cyanide, has simple components, and eliminates the harm of cyanide-containing substances to human bodies and the environment; the added trace brightening agent, leveling agent and cylinder opening agent can ensure that the copper plating solution has better dispersion capability, and the uniformity of the thickness of the surface plating layer of the irregular spherical workpiece is improved.
Compared with the conventional plate type anode, the plating thickness deviation is reduced from 20% to 2%, the plating with the thickness uniformity of +/-2 mu m is prepared, and the preparation of the special-shaped spherical shell workpiece surface protection plating is realized.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present application, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic view showing the structure of a cathode and an anode in the electroplating process in example 1 of the present application.
Reference numerals illustrate: 1-a first anode, 2-a second anode and 3-a special-shaped spherical shell workpiece.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the application. 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.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present application. As used herein, the singular forms also include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
The technical solutions of the present application will be clearly and completely described in connection with the embodiments, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Example 1
A cyanide-free copper plating process comprises forming a workpiece with a special spherical shell to be electroplated into a hemispherical shape, wherein a hemispherical cavity is arranged at the planar end of the hemispherical cavity (as shown in figure 1)) The method comprises the steps of carrying out a first treatment on the surface of the The composition of copper plating solution used in electroplating and the concentration of each substance are as follows: cuSO 4 ·5H 2 O40 g/L, hydroxyethylidene diphosphonic acid 40g/L, potassium carbonate 60g/L, potassium hydroxide 10g/L, HR-510A 0.25mL/L, HR-510B 0.3mL/L, HR-510Mu0.25mL/L, and the pH value of the solution is 9.3; the specific process is as follows:
(1) Sequentially polishing rust spots on the surface of the workpiece by adopting 600-2400-mesh sand paper until the rust spots are bright and have no rust marks;
(2) Putting the polished workpiece into a solution with a degreasing agent (FKD-835D is adopted as the degreasing agent) for ultrasonic treatment for 20 minutes;
(3) Cleaning the ultrasonic treated workpiece with pure water and alcohol, air drying, electroplating at 45deg.C with current density of 15mA/cm 2 The cathode rotation period is 8 minutes; the anode is a profiling anode, the profiling anode comprises a first anode 1 and a second anode 2, the shape of the first anode 1 is similar to a pot cover, the profiling anode consists of a plane circle and a spherical bulge positioned at the bottom of the circle, the spherical bulge is matched with a cavity shape of the plane end of the special-shaped spherical shell workpiece 3, and the circular plane is matched with the plane end of the special-shaped spherical shell workpiece 3; the shape of the second anode 2 is a hollow hemispherical shape and is matched with the spherical surface of the special-shaped spherical shell workpiece 3; the second anode 2 in this embodiment consists of two hollow sphere quarter-shaped anodes; when electroplating is carried out, the first anode 1 is placed at a position 2 cm above the special-shaped spherical shell workpiece 3, and the second anode 2 is placed at a position 2 cm below the special-shaped spherical shell workpiece 3, as shown in fig. 1. The two-step electroplating method is adopted, wherein the first anode 1 and the second anode 2 are adopted for electroplating for 100 minutes, and then the first anode 1 is adopted for plating for 20 minutes.
The uniformity of the protective coating on the surface of the special-shaped spherical shell workpiece 3 is measured by a thickness meter to be +/-2 mu m, and the thickness deviation is 2%.
Example 2
The technical scheme of the cyanide-free copper plating process is basically the same as that of the embodiment 1, except that: in the step (3), the first anode and the second anode are only adopted for electroplating for 120 minutes, and the first anode is not adopted for plating.
The protective coating on the surface of the special-shaped spherical shell workpiece obtained by the process is flat and uniform, and the thickness of the coating on the planar end of the workpiece and the thickness of the coating of the hemispherical cavity are measured by a thickness meter to be 6 mu m smaller than those of the coating on the spherical outer surface of the workpiece.
Comparative example 1
The copper plating process is basically the same as the embodiment 1 of the application in the technical scheme, except that: (1) The copper plating solution consists of 40g/L copper sulfate, 160g/L hydroxyethylidene diphosphonic acid, 60g/L potassium carbonate and 10g/L potassium hydroxide; (2) The electroplating in step (3) is performed using an anode conventionally used in the art.
The plating layer on the surface of the special-shaped spherical shell workpiece prepared by the process is rough, the Ra is far more than 25 mu m as measured by a coarser instrument, and the protection effect is poor.
Comparative example 2
The copper plating process is basically the same as the embodiment 1 of the application in the technical scheme, except that: in the step (3), the second anode plating was used only for 120 minutes.
The protective coating prepared by the process is uniform and flat, but the thickness of the coating at the plane end and the hemispherical cavity of the workpiece is different from the spherical thickness of the outer surface of the workpiece by more than 20 mu m.
Comparative example 3
The copper plating process is basically the same as the embodiment 1 of the application in the technical scheme, except that: the anode employs a plate type anode conventionally used in the art.
The relative deviation of the thickness of the protective coating prepared by the process is 20%.
According to analysis of examples 1-2 and comparative examples 1-3, it can be seen that the copper plating process provided by the application can prepare a uniform and complete protective coating on the surface of the special-shaped spherical shell workpiece, and compared with a conventional plate type anode, the uniformity of the coating thickness is improved by adopting a profiling anode, the relative deviation of the coating thickness is reduced from 20% to 2%, and the uniformity of the spherical shell coating thickness is improved. The process provided in the embodiment 1 ensures that the prepared plating layer has thickness uniformity of +/-2 mu m, is more uniform and flat, and has better protective performance.
The copper plating solution adopted in the cyanide-free copper plating process provided by the application is added with a trace amount of additive (brightening agent, leveling agent and cylinder opening agent) to obtain a plating layer with better appearance, and compared with the traditional additive, the additive has simple components and obvious effects, and meanwhile, the dispersion capacity of the solution after the additive is added is reduced from 70% to 48%, so that the uniformity of the thickness of the plating layer on the surface of an irregular spherical shell workpiece is greatly improved, and the harm of cyanide-containing substances to human bodies and the environment is eliminated.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present application, and not for limiting the same; although the application has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the application.
Claims (10)
1. A cyanide-free copper plating process is characterized in that a copper plating solution is adopted, wherein the copper plating solution comprises 38-42g/L of copper sulfate, 3-8-42g/L of hydroxyethylidene diphosphonic acid, 58-62g/L of potassium carbonate, 9-11g/L of potassium hydroxide, 0.2-0.3mL/L of a main gloss agent, 0.25-0.35mL/L of a leveling agent and 0.2-0.3mL/L of a cylinder opening agent.
2. The cyanide-free copper plating process according to claim 1, wherein the main gloss agent is HR-510A, the leveling agent is HR-510B, and the cylinder opener is HR-510Mu.
3. The cyanide-free copper plating process according to claim 2, wherein the copper plating solution comprises 40g/L of copper sulfate, 40g/L of hydroxyethylidene diphosphonic acid, 60g/L of potassium carbonate, 10g/L, HR-510a 0.25ml/L, HR-510b 0.3ml/L, HR-510mu0.25ml/L of potassium hydroxide.
4. A cyanide-free copper plating process according to claim 3 wherein the copper plating solution has a pH of 9.3.
5. The cyanide-free copper plating process according to any one of claims 1 to 4, comprising the steps of:
(1) Polishing the workpiece to be electroplated to remove rust spots on the surface of the workpiece;
(2) Placing the polished workpiece into an oil removing agent for ultrasonic treatment;
(3) And (3) cleaning the workpiece subjected to ultrasonic treatment in the step (2) by water and alcohol, airing, and then placing the workpiece into the copper plating solution for electroplating.
6. The cyanide-free copper plating process according to claim 5, wherein the polishing in the step (1) is sequentially performed using 600 mesh to 2400 mesh sandpaper; the degreasing agent in the step (2) is FKD-835D, and the ultrasonic treatment time is 20 minutes.
7. The cyanide-free copper plating process according to claim 6, wherein the plating temperature in the step (3) is 44 to 45 ℃ and the current density is 15 to 16mA/cm 2 The cathode rotation period is 8-10 minutes.
8. The cyanide-free copper plating process according to claim 7, wherein the workpiece in step (1) is a hemispherical workpiece in shape when electroplating is performed, and wherein a hemispherical cavity is provided at a planar end of the hemispherical workpiece.
9. The cyanide-free copper plating process according to claim 8, wherein the step (3) is performed by using a profiling anode, the profiling anode comprises a first anode and a second anode, the shape of the bottom of the first anode is matched with the shape of the planar end of the workpiece, and the shape of the second anode is matched with the shape of the spherical outer surface of the workpiece to be plated.
10. The cyanide-free copper plating process according to claim 9, wherein the electroplating in step (3) is performed by first electroplating with a first anode and a second anode for 100 minutes and then plating with the first anode for 20 minutes.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN202311234825.5A CN117210892A (en) | 2023-09-22 | 2023-09-22 | Cyanide-free copper plating process |
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CN202311234825.5A CN117210892A (en) | 2023-09-22 | 2023-09-22 | Cyanide-free copper plating process |
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CN117210892A true CN117210892A (en) | 2023-12-12 |
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CN202311234825.5A Pending CN117210892A (en) | 2023-09-22 | 2023-09-22 | Cyanide-free copper plating process |
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- 2023-09-22 CN CN202311234825.5A patent/CN117210892A/en active Pending
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