CN111058066A - Application of sodium polydithio-ethane sulfonate as accelerator and electroplating solution containing sodium polydithio-ethane sulfonate - Google Patents
Application of sodium polydithio-ethane sulfonate as accelerator and electroplating solution containing sodium polydithio-ethane sulfonate Download PDFInfo
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- CN111058066A CN111058066A CN201911378208.6A CN201911378208A CN111058066A CN 111058066 A CN111058066 A CN 111058066A CN 201911378208 A CN201911378208 A CN 201911378208A CN 111058066 A CN111058066 A CN 111058066A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/04—Tubes; Rings; Hollow bodies
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Abstract
The invention belongs to the technical field of copper electroplating, and particularly relates to application of sodium polydithio-ethane sulfonate as an accelerator and electroplating solution containing the same. The electroplating solution is prepared by taking sodium polydithio-ethane sulfonate as an accelerator and other raw materials, and a sample plated by hole filling of the electroplating solution has high hole filling rate and good flatness, so that the requirement of hole filling electroplating can be completely met; the accelerator has a wide use concentration range, is easy to control during electroplating hole filling, is suitable for high-current-density hole filling of 2-6 ASD, and can remarkably improve the production efficiency.
Description
Technical Field
The invention belongs to the technical field of electrolytic copper plating. More particularly, it relates to the use of sodium polydithioethane sulfonate as an accelerator and electroplating baths containing the same.
Background
In recent years, electronic product manufacturing and system manufacturing are rapidly developing, and gradually turning to miniaturization and multi-functionalization, Printed Circuit Boards (PCBs) are being developed toward high density, high precision, and high reliability. The printed circuit board is mainly manufactured by adopting acid sulfate copper plating solution to carry out hole metallization, has simple main components, is environment-friendly, is convenient to manage and maintain, has low production cost, can obtain a copper plating layer with better brightness, flatness and ductility by matching with a proper electroplating additive, and is widely applied to modern electronic products such as Integrated Circuits (ICs), high density interconnection boards (HDIs), PCBs and the like. In the acid sulfate copper plating system, an accelerator (also called brightener) needs to be added to cooperate with chloride ions to reduce cathode polarization and accelerate copper deposition.
Currently, the accelerators widely used are sodium polydithio-dipropanesulfonate (SPS) and sodium 3-mercapto-1-propanesulfonate (MPS). For example, Chinese patent application CN103060860A discloses an acid copper plating electroplating solution for a printed circuit board and a preparation and application method thereof. The brightener used in the electroplating solution is sulfur-containing organic sulfonate, including sodium polydithio-dipropyl sulfonate, sodium alcohol mercapto-propyl sulfonate and the like, and the prepared electroplating solution has good depth capability and dispersibility, can improve the uniform distribution of copper layers in through holes of a printed circuit board, and effectively reduces the ratio of the thickness of the surface copper layer to the thickness of the copper layer in the center of the through hole. On one hand, the concentration range of the brightener added into the electroplating solution is 1-100 mg/L, the adjustable range is narrow, and in actual production, in order to ensure that the concentration of the brightener is in the working range, frequent sampling is needed to analyze the content of the brightener, a high-price CVS analyzer is needed, the analysis and measurement errors are large, the addition amount of an accelerator is often insufficient or exceeds the limit, the blind hole filling effect is poor, and the difficulty is brought to actual production; on the other hand, although the current density of electroplating can be increased to accelerate the electroplating time and improve the working efficiency, the highest current density of electroplating in the prior art can only reach 4ASD, and the current density is increased to cause the consequences that blind holes cannot be filled, the hole filling rate is obviously reduced, and the flatness is poor.
Therefore, it is urgently needed to provide an electroplating copper accelerator with a wider concentration range and a larger current density suitable for electroplating and an electroplating solution containing the accelerator, and to achieve a better blind hole filling effect.
Disclosure of Invention
The invention aims to solve the technical problems of small using concentration range of an accelerator, high practical production control difficulty, small electroplating applicable current density and low electroplating efficiency in the prior art, and provides the application of the sodium polydithio-diethyl alkane sulfonate as the accelerator in the electroplating solution, which has wide using concentration range, high electroplating applicable current density and good blind hole filling effect.
It is another object of the present invention to provide such an accelerator.
It is another object of the present invention to provide an electroplating bath containing the accelerator.
The invention also aims to provide a using method of electroplating by using the electroplating solution.
The above purpose of the invention is realized by the following technical scheme:
use of sodium polydithio-diethyl alkane sulfonate as an accelerator in an electroplating bath, said sodium polydithio-diethyl alkane sulfonate having the structure of formula (I):
further, the addition amount of the accelerator in the plating solution is 4 to 800 mg/L.
Further, the current density of the plating solution during the hole-filling plating is 2 to 6 ASD.
In addition, the invention also provides the accelerator.
In addition, the invention also provides an electroplating solution containing the accelerator, which comprises the following raw materials: 200-250 g/L of blue vitriol, 30-50 g/L of sulfuric acid, 30-50 mg/L of chloride ions, 0.1-100 mg/L of leveling agent, 4-800 mg/L of accelerator and 10-1500 mg/L of inhibitor.
Preferably, the following raw materials are included: 220-250 g/L of blue vitriol, 40-50 g/L of sulfuric acid, 40-50 mg/L of chloride ions, 0.1-50 mg/L of leveling agent, 4-600 mg/L of accelerator and 80-700 mg/L of inhibitor.
More preferably, the following raw materials are included: 220g/L of blue vitriol, 40g/L of sulphuric acid, 40mg/L of chloride ion, 4mg/L of leveling agent, 300mg/L of accelerator and 300mg/L of inhibitor. In practice, the electroplating solution prepared under the condition has high hole filling rate and good electroplating effect.
Further, the leveling agent is a quaternary ammonium salt compound.
Preferably, the quaternary ammonium salt compound comprises Janus Green B.
Further, the inhibitor is a polyether compound.
Further, the inhibitor is selected from one or more of polyethylene glycol, polypropylene glycol, block copolymer PEO-PPO-PEO, and block copolymer PPO-PEO-PPO.
Preferably, the polyethylene glycol has the structural formula:
wherein n is an integer of 20 to 600.
Preferably, the polypropylene glycol has the structural formula:
wherein n is an integer of 20 to 600.
Preferably, the structural formula of the block copolymer PEO-PPO-PEO is as follows:
Preferably, the structural formula of the block copolymer PPO-PEO-PPO is as follows:
In addition, the invention also provides a using method of the electroplating solution, and the current density of the electroplating solution during hole filling electroplating is 2-6 ASD.
The added chloride ions can help the phosphorus-copper anode to dissolve, and can also reduce the cathode polarization, so that the plating layer is fine; quaternary ammonium salt compounds of the leveling agent are easily adsorbed in a high-density charge area in the electroplating hole filling process, so that the effects of inhibiting the reduction of copper ions and improving the leveling degree can be achieved; the inhibitor polyether compound can increase the cathode polarization and reduce the surface tension in the electroplating process; the accelerator sodium polydithio-ethane sulfonate can reduce cathode polarization and accelerate copper deposition under the synergistic action of the accelerator and chloride ions. The accelerator has a large use concentration range of 4-800 mg/L, so that the technical problem of difficulty in controlling the accelerator concentration in the prior art is greatly reduced, the accelerator is suitable for high-current density hole filling of 2-6 ASD, the electroplating time can be shortened, and the production efficiency is remarkably improved; the sample obtained by electroplating has high hole filling rate and can completely meet the requirement of hole filling electroplating.
The invention has the following beneficial effects:
the sample obtained by electroplating in the way of hole filling by using the electroplating solution prepared from sodium polydithio-ethane sulfonate as an accelerator and other raw materials is high in hole filling rate and good in flatness, and can completely meet the requirement of hole filling electroplating; the accelerator has a wide use concentration range, is easy to control during electroplating hole filling, is suitable for high-current-density hole filling of 2-6 ASD, and can remarkably improve the production efficiency.
Drawings
FIG. 1 is a sectional view showing a result of hole filling by plating using a plating solution according to example 1 of the present invention.
FIG. 2 is a sectional view showing a result of hole filling by plating using a plating solution according to example 2 of the present invention.
FIG. 3 is a sectional view showing a result of hole filling by plating using a plating solution according to example 3 of the present invention.
FIG. 4 is a sectional view showing a result of hole filling by plating using a plating solution in example 4 of the present invention.
FIG. 5 is a sectional view showing a result of hole filling by plating using a plating solution in example 5 of the present invention.
FIG. 6 is a sectional view showing a result of hole filling by plating using a plating solution in example 6 of the present invention.
FIG. 7 is a sectional view showing a result of hole filling by plating using a plating solution in example 7 of the present invention.
FIG. 8 is a sectional view showing a result of hole filling by plating using a plating solution in example 8 of the present invention.
FIG. 9 is a sectional view showing a result of hole filling by plating using a plating solution in example 9 of the present invention.
FIG. 10 is a sectional view showing the result of hole filling by plating with the plating solution of comparative example 1 of the present invention.
FIG. 11 is a sectional view showing a result of hole filling by plating with a plating solution according to comparative example 2 of the present invention.
FIG. 12 is a sectional view showing the result of hole filling by plating with a plating solution according to comparative example 3 of the present invention.
FIG. 13 is a sectional view showing a result of hole filling by plating with a plating solution according to comparative example 4 of the present invention.
FIG. 14 is a sectional view showing a result of hole filling by plating with a plating solution according to comparative example 5 of the present invention.
FIG. 15 is a sectional view showing a result of hole filling by plating with a plating solution according to comparative example 6 of the present invention.
FIG. 16 is a sectional view showing a result of hole filling by plating with a plating solution of comparative example 7 of the present invention.
FIG. 17 is a sectional view showing a result of hole filling by plating with a plating solution according to comparative example 8 of the present invention.
FIG. 18 is a sectional view showing a result of hole filling by plating with a plating solution of comparative example 9 of the present invention.
FIG. 19 is a sectional view showing a result of hole filling by plating with a plating solution according to comparative example 10 of the present invention.
FIG. 20 is a sectional view showing a result of hole filling by plating with a plating solution of comparative example 11 of the present invention.
Detailed Description
The invention is further described with reference to the drawings and the following detailed description, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
EXAMPLE 1 an electroplating solution
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 4mg/L of accelerator (sodium polydithio-ethane sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation method comprises the following steps: adding half volume of deionized water into a beaker, adding concentrated sulfuric acid under stirring, adding blue vitriol while hot, stirring for dissolving, cooling, adding chloride ions, leveling agent, accelerator and inhibitor, adding water to desired volume, and mixing well.
EXAMPLE 2 an electroplating solution
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 50mg/L of accelerator (sodium polydithio-diethyl-alkane sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
EXAMPLE 3 an electroplating solution
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 300mg/L of accelerator (sodium polydithio-ethane sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
EXAMPLE 4 an electroplating solution
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 600mg/L of accelerator (sodium polydithio-ethane sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
EXAMPLE 5 an electroplating solution
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 800mg/L of accelerator (sodium polydithio-ethane sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
EXAMPLE 6 an electroplating solution
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 50mg/L of accelerator (sodium polydithio-diethyl-alkane sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
EXAMPLE 7 an electroplating solution
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 800mg/L of accelerator (sodium polydithio-ethane sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
EXAMPLE 8 an electroplating solution
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 50mg/L of accelerator (sodium polydithio-diethyl-alkane sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
EXAMPLE 9 an electroplating solution
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 800mg/L of accelerator (sodium polydithio-ethane sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
Comparative example 1 an electroplating bath
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 0.1mg/L of accelerator (sodium polydithio-ethane sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
Comparative example 2 an electroplating bath
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 2mg/L of accelerator (sodium polydithio-ethane sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
Comparative example 3 an electroplating bath
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 1000mg/L of accelerator (sodium polydithio-ethane sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
Comparative example 4 an electroplating bath
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 4mg/L of accelerator (sodium polydithio dipropyl sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
Comparative example 5 an electroplating bath
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 4mg/L of accelerator (sodium polydithio dipropyl sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
Comparative example 6 an electroplating bath
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 4mg/L of accelerator (sodium polydithio dipropyl sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
Comparative example 7 an electroplating bath
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 50mg/L of accelerator (sodium polydithio dipropyl sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
Comparative example 8 an electroplating bath
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 50mg/L of accelerator (sodium polydithio dipropyl sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
Comparative example 9 an electroplating bath
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 800mg/L of accelerator (sodium polydithio dipropyl sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
Comparative example 10 an electroplating bath
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 800mg/L of accelerator (sodium polydithio dipropyl sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
Comparative example 11 an electroplating bath
The electroplating solution is prepared from the following raw materials:
220g/L of copper sulfate pentahydrate, 40g/L of sulfuric acid, 40mg/L of chloride ions, 4mg/L of leveling agent (Jianna green B), 50mg/L of accelerator (sodium polydithio dipropyl sulfonate) and 300mg/L of inhibitor (PEG 6000).
The preparation process is referred to example 1.
Experimental example 1 electroplating via filling application
Placing the electroplating solutions prepared in examples 1-9 and comparative examples 1-11 in an electroplating bath respectively, setting the electroplating temperature at 25 ℃, and electroplating current density as shown in Table 1, and electroplating a sample of a blind hole plate (the aperture of the blind hole is 70-75 μm, and the thickness is 50 μm) for 45 min; after the electroplating is finished, washing the sample by water, taking a hole in the middle as a slice, observing the distribution of copper layers in the hole, and calculating the hole filling rate by the following steps: (thickness-indentation value)/thickness X100%. And recording the pore filling rate data, and particularly, referring to the figures 1-20 and the table 1.
TABLE 1 plating Current Density and test data
As can be seen from the graphs of FIGS. 1 to 20 and Table 1, the electroplating solutions of examples 1 to 9 of the present invention can perform electroplating hole filling well under the current density of 2 to 6ASD, the hole filling rate is as high as 97 to 99%, and the hole filling flatness is good; compared with the comparative examples 1-3, the pore filling rate of the accelerator with different addition amounts is obviously reduced; in comparative examples 4-11, the hole filling rate of different accelerators (sodium polydithio-dipropyl sulfonate) is remarkably reduced, and the hole filling effect is poor due to the existence of a void phenomenon.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The application of sodium polydithio-diethyl alkane sulfonate as an accelerator in electroplating liquid is characterized in that the sodium polydithio-diethyl alkane sulfonate has a structure shown in a formula (I):
2. the use according to claim 1, wherein the accelerator is added to the plating solution in an amount of 4 to 800 mg/L.
3. The use according to claim 2, wherein the plating solution has a current density of 2 to 6ASD when the hole-filling plating is performed.
4. An accelerator according to any one of claims 1 to 3.
5. An electroplating bath comprising the accelerator of claim 4, wherein the electroplating bath comprises the following raw materials: 200-250 g/L of blue vitriol, 30-50 g/L of sulfuric acid, 30-50 mg/L of chloride ions, 0.1-100 mg/L of leveling agent, 4-800 mg/L of accelerator and 10-1500 mg/L of inhibitor.
6. The electroplating bath as set forth in claim 5 comprising the following raw materials: 220-250 g/L of blue vitriol, 40-50 g/L of sulfuric acid, 40-50 mg/L of chloride ions, 0.1-50 mg/L of leveling agent, 4-600 mg/L of accelerator and 80-700 mg/L of inhibitor.
7. The electroplating bath as set forth in claim 5 wherein the leveler is a quaternary ammonium salt compound.
8. The electroplating bath as set forth in claim 5 wherein said suppressor is a polyether compound.
9. The electroplating bath as set forth in claim 5, wherein the inhibitor is selected from one or more of polyethylene glycol, polypropylene glycol, block copolymer PEO-PPO-PEO, block copolymer PPO-PEO-PPO.
10. The method of using the plating solution as defined in any one of claims 5 to 9, wherein the current density of the plating solution at the time of the hole-filling plating is 2 to 6 ASD.
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Cited By (6)
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| CN115215776B (en) * | 2022-08-04 | 2023-10-03 | 江苏梦得新材料科技有限公司 | Preparation method and application of sodium polydithio-di-ethane sulfonate |
| CN116856022A (en) * | 2023-07-05 | 2023-10-10 | 诺博环保科技(中山)有限公司 | Alloy additive for electroplating and preparation method thereof |
| CN116856022B (en) * | 2023-07-05 | 2024-02-20 | 诺博环保科技(中山)有限公司 | Alloy additive for electroplating and preparation method thereof |
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Application publication date: 20200424 |