CN112223099A - Surface cleaning method for sulfur-containing nickel beads of electroplating anode material - Google Patents
Surface cleaning method for sulfur-containing nickel beads of electroplating anode material Download PDFInfo
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- CN112223099A CN112223099A CN202011086666.5A CN202011086666A CN112223099A CN 112223099 A CN112223099 A CN 112223099A CN 202011086666 A CN202011086666 A CN 202011086666A CN 112223099 A CN112223099 A CN 112223099A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B31/00—Machines or devices designed for polishing or abrading surfaces on work by means of tumbling apparatus or other apparatus in which the work and/or the abrasive material is loose; Accessories therefor
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
- C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
- C23G5/032—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing oxygen-containing compounds
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Organic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention relates to a surface cleaning method of an electroplating anode material sulfur-containing nickel bead. The surface cleaning method combines chemical cleaning and mechanical grinding cleaning aiming at the surface smudging characteristic of the sulfur-containing nickel bead of the electroplating anode material, can effectively remove various metal or nonmetal ionic impurities and viscous oil stains with strong adhesive force on the surface of the sulfur-containing nickel bead, improves the surface quality of the sulfur-containing nickel bead of the electroplating anode material, and can also ensure the stability of the electroplating process and the performance of an electroplating nickel layer.
Description
Technical Field
The invention relates to the technical field of material cleaning, in particular to a surface cleaning method for a sulfur-containing nickel bead of an electroplating anode material.
Background
Printed Circuit Boards (PCBs), which are one of the important components of the electronics industry, are widely used for electrical interconnection between electronic components in integrated circuits. The printed circuit board consists of an insulating bottom plate, a connecting lead and a welding disc for assembling and welding electronic elements, and has double functions of a conductive circuit and the insulating bottom plate. The printed circuit board can replace complex wiring, realizes electrical connection among elements in a circuit, simplifies assembly and welding work of electronic products, reduces wiring workload in a traditional mode, greatly lightens labor intensity of workers, reduces the volume of the whole machine, reduces product cost and improves quality and reliability of electronic equipment.
In the process of preparing the printed circuit board, a gold immersion process is needed, in particular to a process for coating a solderability coating on the surface of bare copper of the printed circuit board, wherein nickel plating is usually carried out on the surface of the bare copper, and then gold immersion is carried out chemically. Since copper on the printed wiring board is mainly red copper, copper soldering points are very easily oxidized in air, thereby causing poor conductivity or poor contact and reducing the performance of the printed wiring board. Therefore, a gold immersion process is required to protect the surface of the copper solder joint, so as to effectively prevent the copper metal from contacting with air and prevent the copper solder joint from being oxidized in the air.
With the rapid development of artificial intelligence and 5G technology, the demand for semiconductor chips is increasing, so that the size of electronic equipment is smaller and smaller, the wiring density and difficulty of circuits are higher and higher, and the printed wiring board is required to be updated continuously. At present, the variety of the printed circuit board is developed from a single-sided board to a double-sided board, a multilayer board and a flexible board, the structure and the quality of the printed circuit board are also developed to the degree of ultrahigh density, miniaturization and high reliability, and a new design method, a design article, a board manufacturing material and a board manufacturing process are still on the rise, so that the requirement of a raw material nickel required by nickel plating in a gold immersion process is also promoted.
In order to improve the quality of the electroplated nickel layer, 200-300ppm of sulfur is usually intentionally added to the raw material nickel. At present, the sulfur-containing nickel beads with the diameter of 6-14mm are widely applied to the nickel plating industry of printed circuit boards because of the highest utilization efficiency. In the prior art, the carbonyl gas method is generally adopted to produce the sulfur-containing nickel beads, for example, CN101209494A discloses a method for preparing the sulfur-containing nickel beads, which is to introduce a mixed gas containing carbonyl nickel vapor, carbon monoxide gas, hydrogen sulfide or carbonyl sulfur gas into a decomposer to decompose and deposit on the surface of nickel bead seed crystals added into the decomposer, and the sulfur-containing nickel beads are prepared. The nickel metal particles prepared by the preparation method have the sulfur content of 0.02-0.03 percent, the impurity content of less than 0.01 percent, smooth surfaces of nickel beads, uniform granularity and controllable sulfur content, thereby effectively simplifying the process flow and reducing the production cost.
However, although the sulfur-containing nickel beads prepared by the carbonyl gas method have high purity and less residue, and the maintenance period of the nickel bath is greatly prolonged, the surfaces of the prepared sulfur-containing nickel beads are seriously polluted, and the surfaces of the sulfur-containing nickel beads not only contain various metallic or nonmetallic ionic impurities, such As Cu, Fe, P, Si, Pb, Bi, Zn, Co, Mn, As, Sb, Sn, C and the like, but also contain viscous oil stains with strong adhesion force, and cannot be directly used for electroplating, but no report is made on a surface cleaning method for the sulfur-containing nickel beads As an electroplating anode material at present.
In summary, in order to ensure the stability of the electroplated nickel layer, it is urgently needed to develop a surface cleaning method for the electroplated anode material containing sulfur nickel beads, which can effectively remove the stains on the surface of the sulfur nickel beads, improve the surface quality of the electroplated anode material containing sulfur nickel beads, and ensure the stability of the electroplating process.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a surface cleaning method for a sulfur-containing nickel bead of an electroplating anode material, which combines chemical cleaning and mechanical grinding cleaning aiming at the surface contamination characteristic of the sulfur-containing nickel bead of the electroplating anode material, and performs the chemical cleaning and then the mechanical grinding cleaning, so that various metal or nonmetal ionic impurities and viscous oil contamination with strong adhesive force on the surface of the sulfur-containing nickel bead can be effectively removed, the surface quality of the sulfur-containing nickel bead of the electroplating anode material is improved, and the stability of an electroplating process and the performance of an electroplated nickel layer can be ensured.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention aims to provide a surface cleaning method for a sulfur-containing nickel bead of an electroplating anode material, which comprises the following steps:
firstly, putting the electroplated anode material containing the sulfur nickel beads to be cleaned into a chemical cleaning agent for chemical cleaning, and then mechanically grinding and cleaning the sulfur nickel beads obtained by the chemical cleaning, thereby completing the surface cleaning of the electroplated anode material containing the sulfur nickel beads.
The surface cleaning method combines chemical cleaning and mechanical grinding cleaning aiming at the surface dirt characteristic of the sulfur-containing nickel bead of the electroplating anode material, converts a plurality of metal or nonmetal ionic impurities (such As Cu, Fe, P, Si, Pb, Bi, Zn, Co, Mn, As, Sb, Sn, C and the like) and viscous oil dirt with strong adhesive force which are remained on the surface of the sulfur-containing nickel bead of the electroplating anode material into water-soluble compounds through chemical cleaning, further removes the remaining metal or nonmetal ionic impurities and the oil dirt through mechanical grinding cleaning, and ensures the surface smoothness of the sulfur-containing nickel bead of the electroplating anode material; the surface cleaning method of the invention not only can effectively remove a plurality of metal or nonmetal ionic impurities and viscous oil stains with strong adhesive force on the surface of the nickel-sulfur bead, improve the surface quality of the nickel-sulfur bead of the electroplating anode material, but also can ensure the stability of the electroplating process and the performance of the electroplated nickel layer.
The following technical solutions are preferred but not limited to the technical solutions provided by the present invention, and the technical objects and advantages of the present invention can be better achieved and realized by the following technical solutions.
In a preferred embodiment of the present invention, the chemical cleaning agent comprises concentrated nitric acid and water in a volume ratio of 1 (1-3), for example, 1:1, 1:1.5, 1:2, 1:2.5, or 1:3, but is not limited to the recited values, and other values not recited within the range of the values are also applicable.
Preferably, the concentrated nitric acid has a mass concentration of 60-68%, such as 60%, 61%, 62%, 63%, 64%, 65%, 66%, 67%, or 68%, but is not limited to the recited values, and other values not recited within this range are equally applicable.
The chemical cleaning agent is based on the surface smudging characteristic of the sulfur-containing nickel bead of the electroplating anode material, and is prepared by adopting concentrated nitric acid with the mass concentration of 60-68% and water according to the volume ratio of (1-3), so that various metal or nonmetal ionic impurities and viscous greasy dirt with strong adhesive force remained on the surface of the sulfur-containing nickel bead of the electroplating anode material can be effectively converted into water-soluble compounds, the chemical cleaning speed can be controlled at a proper level, and the raw material cost of the chemical cleaning agent can be saved as much as possible.
In a preferred embodiment of the present invention, the chemical cleaning time is 15 to 20min, for example, 15min, 16min, 17min, 18min, 19min, or 20min, but the chemical cleaning time is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the chemical cleaning is performed in an automatic rotary cleaning tank.
As a preferable embodiment of the present invention, the chemical cleaning further includes water washing after the chemical cleaning and before the mechanical polishing cleaning.
Preferably, the water washing comprises: and (3) putting the sulfur-containing nickel beads obtained by chemical cleaning into a water tank for cleaning.
Preferably, the washing time is 5-10min, such as 5min, 6min, 7min, 8min, 9min or 10min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
The water washing is arranged after the chemical cleaning and before the mechanical grinding cleaning, so that not only can the chemical cleaning agent attached to the surface of the sulfur-containing nickel bead and impurities converted into water-soluble compounds after the chemical cleaning be cleaned, but also the acidic chemical cleaning agent can be prevented from corroding equipment and the surface of the sulfur-containing nickel bead in the mechanical grinding cleaning process.
In a preferred embodiment of the present invention, the time for the mechanical polishing and cleaning is 20 to 30min, for example, 20min, 21min, 22min, 23min, 24min, 25min, 26min, 27min, 28min, 29min, or 30min, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
Preferably, the mechanical mill cleaning is performed in a centrifugal mill.
Preferably, water is added to the centrifugal grinder to prevent the surface of the sulfur-containing nickel beads from being damaged by dry grinding.
The mechanical grinding and cleaning device is arranged after the chemical cleaning, so that the residual ionic impurities of various metals or nonmetals and oil stains are further removed through the mechanical grinding and cleaning, the surface smoothness of the anode material containing the sulfur nickel bead is ensured, the ionic impurities of various metals or nonmetals and the oil stains which are viscous and have strong adhesive force on the surface of the sulfur nickel bead can be effectively removed, the surface quality of the anode material containing the sulfur nickel bead is improved, and the stability of an electroplating process and the performance of an electroplating nickel layer can be ensured.
As a preferred technical solution of the present invention, after the mechanical polishing cleaning, an isopropyl alcohol cleaning is further included.
As a preferred embodiment of the present invention, the isopropyl alcohol cleaning includes: and (3) putting the sulfur-containing nickel beads obtained by mechanical grinding and cleaning into an isopropanol tank for cleaning.
Preferably, the time for the isopropanol cleaning is 5-10min, such as 5min, 6min, 7min, 8min, 9min or 10min, but not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the isopropanol cleaning is carried out under the action of ultrasound.
The isopropanol cleaning device is arranged after mechanical grinding cleaning, and can effectively remove the ground oil stain through the isopropanol.
As a preferable technical scheme of the invention, the mechanical grinding and cleaning device further comprises drying and vacuum packaging which are sequentially carried out.
As a preferred embodiment of the present invention, the drying is performed in a vacuum drying oven.
Preferably, the degree of vacuum of the drying is below 0.01 Pa.
Preferably, the drying temperature is 60-80 deg.C, such as 60 deg.C, 63 deg.C, 65 deg.C, 67 deg.C, 70 deg.C, 73 deg.C, 75 deg.C, 78 deg.C or 80 deg.C, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the drying time is 60-80min, such as 60min, 63min, 65min, 67min, 70min, 73min, 75min, 78min or 80min, but not limited to the recited values, and other values not recited in the range of values are equally applicable.
As a preferable technical solution of the present invention, the surface cleaning method includes the steps of:
(1) putting the electroplated anode material to be cleaned containing the sulfur nickel beads into an automatic rotary cleaning tank filled with a chemical cleaning agent, carrying out chemical cleaning for 15-20min, and then putting the sulfur nickel beads obtained by the chemical cleaning into a water tank for washing for 5-10 min;
wherein the chemical cleaning agent comprises concentrated nitric acid and water with the volume ratio of 1 (1-3) and the mass concentration of 60-68%;
(2) putting the sulfur-containing nickel beads cleaned in the step (1) into a centrifugal grinder with water, and performing mechanical grinding and cleaning for 20-30 min;
(3) putting the sulfur-containing nickel beads cleaned in the step (2) into an isopropanol tank, and cleaning the isopropanol for 5-10min under the action of ultrasound;
(4) and (4) putting the sulfur-containing nickel balls cleaned in the step (3) into a vacuum drying oven, controlling the vacuum degree to be below 0.01Pa, drying at the temperature of 60-80 ℃ for 60-80min, and then carrying out vacuum packaging on the dried sulfur-containing nickel balls to further finish surface cleaning of the electroplated anode material sulfur-containing nickel beads.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the surface cleaning method combines chemical cleaning and mechanical grinding cleaning aiming at the surface dirt characteristic of the sulfur-containing nickel bead of the electroplating anode material, converts a plurality of metal or nonmetal ionic impurities (such As Cu, Fe, P, Si, Pb, Bi, Zn, Co, Mn, As, Sb, Sn, C and the like) and viscous oil dirt with strong adhesive force which are remained on the surface of the sulfur-containing nickel bead of the electroplating anode material into water-soluble compounds through chemical cleaning, further removes the remaining metal or nonmetal ionic impurities and the oil dirt through mechanical grinding cleaning, and ensures the surface smoothness of the sulfur-containing nickel bead of the electroplating anode material;
(2) the surface cleaning method of the invention not only can effectively remove a plurality of metal or nonmetal ionic impurities and viscous oil stains with strong adhesive force on the surface of the nickel-sulfur bead, improve the surface quality of the nickel-sulfur bead of the electroplating anode material, but also can ensure the stability of the electroplating process and the performance of the electroplated nickel layer.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Typical but non-limiting examples of the invention are as follows:
example 1
The embodiment provides a surface cleaning method for a sulfur-containing nickel bead of an electroplating anode material, which comprises the following steps:
(1) putting the electroplated anode material to be cleaned containing the sulfur nickel beads into an automatic rotary cleaning tank filled with a chemical cleaning agent, carrying out chemical cleaning for 18min, and then putting the sulfur nickel beads obtained by the chemical cleaning into a water tank for washing for 8 min;
wherein the chemical cleaning agent is concentrated nitric acid and water with the volume ratio of 1:1.5 and the mass concentration of 68%;
(2) putting the sulfur-containing nickel beads cleaned in the step (1) into a centrifugal grinder with water, and carrying out mechanical grinding and cleaning for 25 min;
(3) putting the sulfur-containing nickel beads cleaned in the step (2) into an isopropanol tank, and cleaning the isopropanol for 8min under the action of ultrasound;
(4) and (4) putting the sulfur-containing nickel balls cleaned in the step (3) into a vacuum drying oven, controlling the vacuum degree to be below 0.01Pa, drying at 70 ℃ for 70min, and then carrying out vacuum packaging on the dried sulfur-containing nickel balls to further finish the surface cleaning of the electroplated anode material sulfur-containing nickel beads.
Example 2
The embodiment provides a surface cleaning method for a sulfur-containing nickel bead of an electroplating anode material, which comprises the following steps:
(1) putting the electroplated anode material to be cleaned containing the sulfur nickel beads into an automatic rotary cleaning tank filled with a chemical cleaning agent, carrying out chemical cleaning for 15min, and then putting the sulfur nickel beads obtained by the chemical cleaning into a water tank for washing for 10 min;
wherein the chemical cleaning agent is concentrated nitric acid and water with the volume ratio of 1:1 and the mass concentration of 60%;
(2) putting the sulfur-containing nickel beads cleaned in the step (1) into a centrifugal grinder with water, and performing mechanical grinding and cleaning for 20 min;
(3) putting the sulfur-containing nickel beads cleaned in the step (2) into an isopropanol tank, and cleaning the isopropanol for 5min under the action of ultrasound;
(4) and (4) putting the sulfur-containing nickel balls cleaned in the step (3) into a vacuum drying oven, controlling the vacuum degree to be below 0.01Pa, drying at 60 ℃ for 80min, and then carrying out vacuum packaging on the dried sulfur-containing nickel balls to further finish the surface cleaning of the electroplated anode material sulfur-containing nickel beads.
Example 3
The embodiment provides a surface cleaning method for a sulfur-containing nickel bead of an electroplating anode material, which comprises the following steps:
(1) putting the electroplated anode material to be cleaned containing the sulfur nickel beads into an automatic rotary cleaning tank filled with a chemical cleaning agent, carrying out chemical cleaning for 20min, and then putting the sulfur nickel beads obtained by the chemical cleaning into a water tank for washing for 5 min;
wherein the chemical cleaning agent is 65% concentrated nitric acid and water with the volume ratio of 1: 3;
(2) putting the sulfur-containing nickel beads cleaned in the step (1) into a centrifugal grinder with water, and performing mechanical grinding and cleaning for 30 min;
(3) putting the sulfur-containing nickel beads cleaned in the step (2) into an isopropanol tank, and cleaning the isopropanol for 10min under the action of ultrasound;
(4) and (4) putting the sulfur-containing nickel balls cleaned in the step (3) into a vacuum drying oven, controlling the vacuum degree to be below 0.01Pa, drying at 80 ℃ for 60min, and then carrying out vacuum packaging on the dried sulfur-containing nickel balls to further finish the surface cleaning of the electroplated anode material sulfur-containing nickel beads.
Example 4
This example provides a surface cleaning method for sulfur-containing nickel beads of an electroplating anode material, which is exactly the same as example 1 except that the chemical cleaning agent in step (1) is replaced by "1: 5" instead of "1: 1.5" in volume ratio.
Example 5
This example provides a surface cleaning method for sulfur-containing nickel beads of an electroplating anode material, which is exactly the same as example 1 except that the chemical cleaning agent in step (1) is replaced by 1:0.5 instead of 1:1.5 in volume ratio.
Example 6
This example provides a surface cleaning method for sulfur-containing nickel beads of an electroplating anode material, which is identical to example 1 except that the isopropanol cleaning in step (3) is completely omitted, that is, the sulfur-containing nickel beads cleaned in step (2) are directly placed into a vacuum drying oven for drying.
Comparative example 1
The comparative example provides a surface cleaning method of a sulfur-containing nickel bead of an electroplating anode material, which is completely the same as that of example 1 except that the mechanical grinding cleaning in the step (2) is completely omitted, namely, the sulfur-containing nickel bead cleaned in the step (1) is directly put into an isopropanol tank for isopropanol cleaning.
Comparative example 2
The present comparative example provides a surface cleaning method of sulfur-containing nickel beads of an electroplating anode material, except that the chemical cleaning described in the step (1) was completely omitted, that is, the sulfur-containing nickel beads of the electroplating anode material to be cleaned were directly put into a centrifugal grinder with water added for mechanical grinding cleaning, and the other conditions were completely the same as in example 1.
Comparative example 3
The comparative example provides a surface cleaning method of a sulfur-containing nickel bead of an electroplating anode material, except that the sequence of the step (1) and the step (2) is changed, the other conditions are completely the same as the example 1, and the specific contents are as follows:
(1) putting the electroplated anode material to be cleaned containing the sulfur nickel beads into a centrifugal grinder with water, and carrying out mechanical grinding cleaning for 25 min;
(2) putting the sulfur-containing nickel beads cleaned in the step (1) into an automatic rotary cleaning tank filled with a chemical cleaning agent, performing chemical cleaning for 18min, and then putting the sulfur-containing nickel beads obtained by the chemical cleaning into a water tank for water cleaning for 8 min;
wherein the chemical cleaning agent is concentrated nitric acid and water with the volume ratio of 1:1.5 and the mass concentration of 68%;
(3) putting the sulfur-containing nickel beads cleaned in the step (2) into an isopropanol tank, and cleaning the isopropanol for 8min under the action of ultrasound;
(4) and (4) putting the sulfur-containing nickel balls cleaned in the step (3) into a vacuum drying oven, controlling the vacuum degree to be below 0.01Pa, drying at 70 ℃ for 70min, and then carrying out vacuum packaging on the dried sulfur-containing nickel balls to further finish the surface cleaning of the electroplated anode material sulfur-containing nickel beads.
The sulfur-containing nickel beads obtained by cleaning the above examples and comparative examples were placed under light, and the surface smoothness of the sulfur-containing nickel beads was visually observed, as shown in table 1.
TABLE 1
| Group of | The surface smoothness of the sulfur-containing nickel beads |
| Example 1 | Smooth and glossy surface |
| Example 2 | Smooth and glossy surface |
| Example 3 | Smooth and glossy surface |
| Example 4 | Most of the surface of the product is smooth and glossy, and occasionally the surface is rough and dull |
| Example 5 | Smooth and glossy surface |
| Example 6 | Most of the surface of the product is smooth and glossy, and occasionally the surface is rough and dull |
| Comparative example 1 | Rough and dull surface with fine rust |
| Comparative example 2 | Rough and dull surface with greasy dirt attached |
| Comparative example 3 | Rough and dull surface, fine rust and little greasy dirt attached |
From table 1, the following points can be seen:
(1) the surface cleaning method of the invention combines chemical cleaning and mechanical grinding cleaning aiming at the surface dirt characteristics of the sulfur-containing nickel bead of the electroplating anode material, converts a plurality of metal or nonmetal ionic impurities (such As Cu, Fe, P, Si, Pb, Bi, Zn, Co, Mn, As, Sb, Sn, C and the like) and viscous oil dirt with strong adhesive force remained on the surface of the sulfur-containing nickel bead of the electroplating anode material into water-soluble compounds by the chemical cleaning, further removes the remaining metal or nonmetal ionic impurities and the oil dirt by the mechanical grinding cleaning, ensures the surface smoothness of the sulfur-containing nickel bead of the electroplating anode material, can effectively remove the metal or nonmetal ionic impurities and the viscous oil dirt with strong adhesive force on the surface of the sulfur-containing nickel bead, improves the surface quality of the sulfur-containing nickel bead of the electroplating anode material, the stability of the electroplating process and the performance of the electroplated nickel layer can be ensured;
(2) comparing the example 1 with the examples 4 and 5, because the proportion of the concentrated nitric acid in the chemical cleaning agent in the example 4 is less than the volume ratio 1 (1-3) of the invention, the cleaning of a plurality of metal or nonmetal ionic impurities and oil stains remained on the surface of the sulfur-containing nickel beads is not in place, most of the sulfur-containing nickel beads obtained by cleaning are smooth and glossy on the surface, and occasionally the surface is rough and dull, although the proportion of the concentrated nitric acid in the chemical cleaning agent in the example 5 is higher than the proportion of the volume ratio 1 (1-3) of the invention, the cleaning effect is basically consistent with the application, the concentrated nitric acid is wasted, and the raw material cost is increased;
(3) comparing example 1 with example 6, the isopropanol cleaning is omitted in example 6, so that the residual oil stain after mechanical grinding cleaning cannot be effectively removed, and most of the sulfur-containing nickel beads obtained by cleaning are smooth and glossy in surface, and occasionally rough and dull in surface;
(4) comparing the example 1 with the comparative examples 1 and 2, wherein the comparative example 1 omits mechanical grinding cleaning, so that ionic impurities and oil stains with strong adhesive force after chemical cleaning cannot be effectively removed, the surface of the cleaned sulfur-containing nickel beads is rough and dark, and fine rusty spots exist, and the comparative example 2 omits chemical cleaning, so that the ionic impurities and the viscous oil stains with strong adhesive force are not converted into water-soluble compounds, and the oil stains cannot be cleaned directly by mechanical grinding cleaning, so that the surface of the cleaned sulfur-containing nickel beads is rough and dark, and oil stains are adhered;
(5) comparing example 1 with comparative example 3, although comparative example 3 also combines chemical cleaning and mechanical grinding cleaning, the two are reversed in sequence, namely, mechanical grinding cleaning is carried out before chemical cleaning, resulting in unclean cleaning, rough and dull surface of the cleaned sulfur-containing nickel beads, fine rust and little oil stain adhesion.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A surface cleaning method for a sulfur-containing nickel bead of an electroplating anode material is characterized by comprising the following steps:
firstly, putting the electroplated anode material containing the sulfur nickel beads to be cleaned into a chemical cleaning agent for chemical cleaning, and then mechanically grinding and cleaning the sulfur nickel beads obtained by the chemical cleaning, thereby completing the surface cleaning of the electroplated anode material containing the sulfur nickel beads.
2. The surface cleaning method according to claim 1, wherein the chemical cleaning agent comprises concentrated nitric acid and water in a volume ratio of 1 (1-3);
preferably, the mass concentration of the concentrated nitric acid is 60-68%.
3. A surface cleaning method according to claim 1 or 2, characterized in that the chemical cleaning time is 15-20 min;
preferably, the chemical cleaning is performed in an automatic rotary cleaning tank.
4. The surface cleaning method according to any one of claims 1 to 3, further comprising a water washing after the chemical cleaning and before the mechanical polishing cleaning;
preferably, the water washing comprises: putting the sulfur-containing nickel beads obtained by chemical cleaning into a water tank for cleaning;
preferably, the time of the water washing is 5-10 min.
5. The surface cleaning method according to any one of claims 1 to 4, wherein the time for the mechanical polishing cleaning is 20 to 30 min;
preferably, the mechanical mill cleaning is performed in a centrifugal mill;
preferably, water is added to the centrifugal mill.
6. The surface cleaning method according to any one of claims 1 to 5, further comprising an isopropyl alcohol cleaning after the mechanical polishing cleaning.
7. The surface cleaning method according to claim 6, wherein the isopropyl alcohol cleaning comprises: putting the sulfur-containing nickel beads obtained by mechanical grinding and cleaning into an isopropanol tank for cleaning;
preferably, the time for cleaning the isopropanol is 5-10 min;
preferably, the isopropanol cleaning is carried out under the action of ultrasound.
8. The surface cleaning method according to any one of claims 1 to 7, further comprising drying and vacuum packaging in sequence after the mechanical abrasive cleaning.
9. The surface cleaning method according to claim 8, wherein the drying is performed in a vacuum drying oven;
preferably, the vacuum degree of the drying is below 0.01 Pa;
preferably, the temperature of the drying is 60-80 ℃;
preferably, the drying time is 60-80 min.
10. A surface cleaning method according to any one of claims 1-9, characterized in that the surface cleaning method comprises the steps of:
(1) putting the electroplated anode material to be cleaned containing the sulfur nickel beads into an automatic rotary cleaning tank filled with a chemical cleaning agent, carrying out chemical cleaning for 15-20min, and then putting the sulfur nickel beads obtained by the chemical cleaning into a water tank for washing for 5-10 min;
wherein the chemical cleaning agent comprises concentrated nitric acid and water with the volume ratio of 1 (1-3) and the mass concentration of 60-68%;
(2) putting the sulfur-containing nickel beads cleaned in the step (1) into a centrifugal grinder with water, and performing mechanical grinding and cleaning for 20-30 min;
(3) putting the sulfur-containing nickel beads cleaned in the step (2) into an isopropanol tank, and cleaning the isopropanol for 5-10min under the action of ultrasound;
(4) and (4) putting the sulfur-containing nickel balls cleaned in the step (3) into a vacuum drying oven, controlling the vacuum degree to be below 0.01Pa, drying at the temperature of 60-80 ℃ for 60-80min, and then carrying out vacuum packaging on the dried sulfur-containing nickel balls to further finish surface cleaning of the electroplated anode material sulfur-containing nickel beads.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011086666.5A CN112223099A (en) | 2020-10-12 | 2020-10-12 | Surface cleaning method for sulfur-containing nickel beads of electroplating anode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| CN108977770A (en) * | 2017-05-31 | 2018-12-11 | 宁波江丰电子材料股份有限公司 | The surface treatment method of copper evaporation material |
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| KR101908321B1 (en) * | 2017-12-20 | 2018-10-17 | 주식회사 이노메탈 | Method of surface treatment for roof rack |
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