CN115787005A - Methanesulfonic acid tin plating solution in PCB production process and preparation method thereof - Google Patents
Methanesulfonic acid tin plating solution in PCB production process and preparation method thereof Download PDFInfo
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- CN115787005A CN115787005A CN202211579367.4A CN202211579367A CN115787005A CN 115787005 A CN115787005 A CN 115787005A CN 202211579367 A CN202211579367 A CN 202211579367A CN 115787005 A CN115787005 A CN 115787005A
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- methanesulfonic acid
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Abstract
The invention relates to a methanesulfonic acid tin plating solution in a PCB production process and a preparation method thereof. The mixed liquid obtained by uniformly mixing the methanesulfonic acid and the stannous methanesulfonate can effectively inhibit Sn 2+ Hydrolysis to Sn 4+ To obtain Sn with good stability 2+ The chemical stability of the tin plating solution is further improved; the stabilizer, the dispersant, the main brightener, the auxiliary brightener and the wetting agent are uniformly mixed to obtain a mixed solution II, so that the stabilizer, the dispersant, the main brightener, the auxiliary brightener and the wetting agent can play a good synergistic effect, a complexing system with good stability is formed, and Sn can be complexed more effectively 2+ More effective inhibition of Sn 2+ Oxidation or hydrolysis to Sn 4+ To a problem of (a). The invention mixes the first mixed solution and the second mixed solution to finally obtain the PCB production processThe methylsulfonic acid tin plating solution has good chemical stability, and can produce a coating with fine and soft crystals, small crystal grains, dense arrangement, uniform distribution, no whiskers or no dendrites, luster or brightness.
Description
Technical Field
The invention relates to the technical field of tin plating solution, in particular to methanesulfonic acid tin plating solution in a PCB production process and a preparation method thereof.
Background
The Printed circuit board is also called as a Printed circuit board, can be abbreviated as a Printed Circuit Board (PCB) or a Printed Wire Board (PWB), is a provider of electrical connection of electronic components, and is mainly applied to the fields of microelectronics, printed Circuit Boards (PCBs), automobiles, jewelry decoration, electrochemical energy storage batteries and the like. With the continuous progress of science, printed circuit boards are slowly developed from single-layer circuit boards to multi-layer circuit boards, and are continuously developed towards the trends of high precision, high density and high reliability so as to better adapt to the modern development trend.
At present, in the production process of the printed circuit board, the printed circuit board is usually required to be placed into tin plating solution for soaking operation, so that copper on the surface of the printed circuit board can perform a displacement reaction with tin ions in the tin plating solution, and a tin layer can be plated on the surface of the copper of the printed circuit board, therefore, the tin layer can not only effectively prevent the copper on the surface of the printed circuit board from performing an oxidation reaction with air, but also effectively avoid the occurrence of bad phenomena such as verdigris and the like on the surface of the printed circuit board, so that the corrosion resistance of the printed circuit board is improved, and the tin layer attached to the surface of the printed circuit board can also improve the solderability of the printed circuit board.
However, in the tin plating solution conventionally used for printed wiring boards, since tin ions in the tin plating solution are liable to undergo oxidation reaction, that is, sn in the tin plating solution 2+ Generation of Sn 4+ Thus, sn is produced 4+ Not only can lead the tin plating solution to become turbid, thereby reducing the stability of the tin plating solution, but also can generate Sn 4+ Will affect Sn in the tin plating solution 2+ The tin layer on the surface of the printed circuit board is easy to crystallize, tin whiskers are long, the surface of the tin layer is rough, blackening and poor in flatness and the like, so that the solderability of the printed circuit board is greatly reduced, and the problems of insufficient soldering, missing soldering and the like of the printed circuit board are easy to occur.
The Chinese patent with publication number CN110791784, the additive contains binary substituent on benzene ring in p-phenolsulfonic acid. The additive contains benzene rings, and when tin ions are deposited, additive molecules are adsorbed on the surface of a product and are not easy to desorb, and the additive molecules and the tin ions are deposited on the surface of the product together, so that the carbon content of a coating is high. And the porosity of the plating layer is increased along with the serious hydrogen evolution, and the plating layer is not corrosion-resistant.
The Chinese patent with publication number CN110791784, the additive contains binary substituent on benzene ring in p-phenolsulfonic acid. The additive contains benzene rings, and when tin ions are deposited, additive molecules are adsorbed on the surface of a product and are not easy to desorb, and the additive molecules and the tin ions are deposited on the surface of the product together, so that the carbon content of a coating is high. And the porosity of the plating layer is increased along with the serious hydrogen evolution, and the plating layer is not corrosion-resistant.
The Chinese patent with publication number CN108251869 adopts the compound additives thiourea, hydroquinone, 2-mercaptobenzimidazole and propylene glycol block polyether, and the proportion is strictly limited. The Chinese patent with publication number CN 103882484 adopts alkyl alcohol polyoxyethylene ether as a displacement agent, and is compounded with a fine grain agent to form an additive. In the electroplating process, the consumption of each substance in the compound additive is different, and the components in the compound additive can be out of proportion after being used for a period of time. Because the concentrations of each component cannot be analyzed and supplemented respectively, the compound additive loses effectiveness.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and develop a tin plating solution with better stability in the production process of a PCB and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
the tin plating solution comprises the following components:
the tin plating solution composed of the stannous methanesulfonate, the methanesulfonic acid, the dispersant, the stabilizer, the main brightener, the auxiliary brightener and the wetting agent has a good brightening effect, and the obtained plating layer is fine and bright in crystallization, difficult to peel and good in weldability.
As a further scheme of the invention: the source of tin ions is stannous methanesulfonate.
As a further scheme of the invention: the tin ions comprise Sn 2+ The concentration is 3-9 g/L.
As a further scheme of the invention: the concentration of the methanesulfonic acid is 80-125 mL/L.
As a further scheme of the invention: the dispersing agent is polyoxyethylene alkyl alcohol amide, and the concentration is 0.8-1.5 mL/L.
As a further scheme of the invention: the stabilizing agent is hydroquinone, and the concentration is 1-1.2 mL/L.
As a further scheme of the invention: the main brightening agent is benzalacetone with the concentration of 0.5-1 mL/L.
As a further scheme of the invention: the auxiliary brightening agent is glutaraldehyde with the concentration of 0.1-0.5 mL/L.
As a further scheme of the invention: the wetting agent is sodium dodecyl sulfate, and the concentration is 0.1-0.3 mL/L.
Stannous methanesulfonate and methanesulfonic acid are mixed according to the mass ratio of (3-8): (4-7) uniformly mixing to obtain a first mixed solution;
stabilizing agent, dispersing agent, main brightening agent, auxiliary brightening agent and wetting agent according to the mass ratio of (2-4): (3-5): (3-7): (2-5): (2-3) uniformly mixing to obtain a mixed solution II;
and mixing the mixed solution I and the mixed solution II to obtain the tinning liquid.
The invention has the following beneficial effects: the invention discloses a methanesulfonic acid tin plating solution in a PCB production process and a preparation method thereof, which can be applied to PCB tin plating. The methanesulfonic acid can provide an acid condition for the tin plating solution, and the mixed solution obtained by uniformly mixing the methanesulfonic acid and the stannous methanesulfonate can effectively inhibit Sn 2+ Hydrolysis to Sn 4+ To obtain Sn with good stability 2+ The chemical stability of the tin plating solution is further improved; the mixed solution II obtained by uniformly mixing the stabilizer, the dispersant, the main brightener, the auxiliary brightener and the wetting agent can play a good role in synergy, so that a complex system with good stability is formed, and Sn can be more effectively complexed 2+ More effective inhibition of Sn 2+ Oxidation or hydrolysis to Sn 4+ To a problem of (a). The methanesulfonic acid tin plating solution obtained by mixing the mixed solution I and the mixed solution II in the production process of the PCB has good chemical stability, and can produce a coating which is fine in crystal, soft, small in crystal grain, dense in arrangement, uniform in distribution, free of whiskers or dendrites, glossy or bright.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a flow chart of a method for preparing a tin plating solution of methanesulfonic acid in a PCB production process according to an embodiment of the disclosure.
Fig. 2 is a flow chart of a method for tinning a printed wiring board during PCB production in accordance with an embodiment of the present disclosure.
FIG. 3 is a graph comparing the test results of example 1, example 2 and comparative example 1 as disclosed herein.
Fig. 4 to 6 are SEM photographs of PCBs according to example 1, example 2 and comparative example 1 of the present disclosure.
Detailed Description
The invention is further illustrated by the following specific examples. But the content of the invention is not limited thereto.
Example 1
The embodiment provides a tin plating solution in a PCB production process, which comprises the following components in percentage by weight: 15% of stannous methanesulfonate, 19% of methanesulfonic acid, 12% of polyoxyethylene alkylolamide, 15% of hydroquinone, 15% of benzalacetone, 12% of glutaraldehyde and 12% of sodium dodecyl sulfate.
Uniformly mixing the stannous methanesulfonate and methanesulfonic acid to obtain a mixed solution I; uniformly mixing the stabilizer, the dispersing agent, the main brightener, the auxiliary brightener and the wetting agent to obtain a mixed solution II; and mixing the mixed solution I and the mixed solution II to obtain the methanesulfonic acid tin plating solution in the PCB production process.
In order to test the stability of the methanesulfonic acid tin plating solution, air is continuously blown into the methanesulfonic acid tin plating solution for 48 hours, and the methanesulfonic acid tin plating solution is always clear and transparent without turbidity, which indicates that the methanesulfonic acid tin plating solution has good stability.
With the methyl sulfonic acidAcid tinning solution is used as electroplating solution, 99.9% tin plate is used as an anode, a pretreated copper-plated PCB is used as a cathode, the temperature is 40 ℃, and the current density is 4A/dm 2 The plating is carried out for 6min under the condition of (1) to obtain a bright tin plating layer which is uniform, fine and high in density, the average thickness of the tin plating layer is measured to be 6.4 mu m, and the requirement of the thickness required by a pattern electroplating protection circuit is met. And continuously carrying out tin plating on multiple batches under the same conditions to obtain a batch of tin-plated PCB. After the tin plating is finished, analyzing Sn in the tin plating solution 2+ And the concentration of the main components is basically kept unchanged, and the weight of the anode tin plate is reduced by 390g.
Example 2
The embodiment provides a methanesulfonic acid tin plating solution in a PCB production process, which comprises the following components in parts by weight: 22% of stannous methanesulfonate, 18% of methanesulfonic acid, 9% of polyoxyethylene alkylolamide, 12% of hydroquinone, 18% of benzalacetone, 12% of glutaraldehyde and 9% of sodium dodecyl sulfate.
The preparation process and application method of this example are the same as those of example 1.
In order to test the stability of the methanesulfonic acid tin plating solution, air is continuously blown into the methanesulfonic acid tin plating solution for 48 hours, and the methanesulfonic acid tin plating solution is always clear and transparent without turbidity, which indicates that the methanesulfonic acid tin plating solution has good stability.
The methanesulfonic acid tin plating solution is used as electroplating solution, a 99.9% tin plate is used as an anode, a pretreated copper-plated PCB is used as a cathode, the temperature is 45 ℃, and the current density is 5A/dm 2 The plating is carried out for 5min under the condition of (1), a bright tin plating layer which is uniform, fine and high in density is obtained, the average thickness of the tin plating layer is measured to be 7.1 mu m, and the requirement of the thickness required by a pattern electroplating protection circuit is met. And continuously carrying out tin plating on multiple batches under the same conditions to obtain a batch of tin-plated PCB. After the tin plating is finished, analyzing Sn in the tin plating solution 2+ And the concentration of the main components is basically kept unchanged, and the weight of the anode tin plate is reduced by 420g.
Comparative example 1
The formulation of this comparative example is the same as example 1 except that: uniformly mixing stannous methanesulfonate, methanesulfonic acid, a dispersing agent, a stabilizing agent, a main brightener, an auxiliary brightener and a wetting agent together to obtain the methanesulfonic acid tin plating solution in the PCB production process.
In order to test the stability of the methanesulfonic acid tin plating solution, air was continuously blown into the methanesulfonic acid tin plating solution, and the methanesulfonic acid tin plating solution began to become turbid gradually after 30 hours of air blowing, and the stability of the methanesulfonic acid tin plating solution was found to be poor. The plating is carried out under the same condition, and the obtained tinning is uneven, loose and porous, and the plating layer is dark, thus the requirements of a pattern electroplating protection circuit can not be met.
The test results of the above examples 1, 2 and 1 are specifically shown in fig. 3, and the SEM photographs of the tinned PCBs of examples 1, 2 and 1 are shown in fig. 4 to 6.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. The tin plating solution of methanesulfonic acid in the PCB production process and the preparation method thereof are characterized in that the tin plating solution of methanesulfonic acid comprises stannous methanesulfonate, methanesulfonic acid, a dispersing agent, a stabilizing agent, a main brightener, an auxiliary brightener and a wetting agent in the PCB production process. The invention discloses a methanesulfonic acid tin plating solution, which is characterized in that: the mass ratio of the stannous methanesulfonate to the methanesulfonic acid to the dispersant to the stabilizer to the main brightener to the auxiliary brightener to the wetting agent is (2-9): (4-8): (1-5): (2-5): (2-8): (2-6): (2-4). The preparation method of the methanesulfonic acid tin plating solution in the PCB production process comprises the following steps: stannous methanesulfonate and methanesulfonic acid are mixed according to the mass ratio of (2-9): (4-8) uniformly mixing to obtain a first mixed solution; stabilizing agent, dispersing agent, main brightening agent, auxiliary brightening agent and wetting agent according to the mass ratio of (1-5): (2-5): (2-8): (2-6): (2-4) uniformly mixing to obtain a mixed solution II; and mixing the mixed solution I and the mixed solution II to prepare the methanesulfonic acid tin plating solution in the PCB production process, thereby obtaining the methanesulfonic acid tin plating solution in the PCB production process and the preparation method thereof.
2. The tin plating solution of methanesulfonic acid in the production process of PCB and the preparation method thereof are characterized in that Sn in the stannous methanesulfonate is 2+ The concentration of the ions is 3 to 9g/L.
3. A tin plating solution of methanesulfonic acid in the production process of PCB and a preparation method thereof are provided, wherein the concentration of the methanesulfonic acid is 80-125 mL/L.
4. A tin plating solution of methanesulfonic acid in the production process of PCB and a preparation method thereof are provided, wherein the dispersant is polyoxyethylene alkylolamide, and the concentration is 0.8-1.5 mL/L.
5. A tin plating solution of methanesulfonic acid in the production process of PCB and a preparation method thereof, wherein the stabilizer is hydroquinone with the concentration of 1-1.2 mL/L.
6. A tin plating solution of methanesulfonic acid in the production process of PCB and a preparation method thereof are provided, wherein the main brightening agent is benzalacetone, and the concentration is 0.5-1 mL/L.
7. A tin plating solution of methanesulfonic acid in the production process of PCB and a preparation method thereof are disclosed, wherein the auxiliary brightening agent is glutaraldehyde, and the concentration is 0.1-0.5 mL/L.
8. A tin plating solution of methanesulfonic acid in the production process of PCB and a preparation method thereof, wherein the wetting agent is sodium dodecyl sulfate, and the concentration is 0.1-0.3 mL/L.
9. A methanesulfonic acid tin plating solution in a PCB production process and a preparation method thereof are provided, wherein the preparation method of the methanesulfonic acid tin plating solution in the PCB production process comprises the following steps: stannous methanesulfonate and methanesulfonic acid are mixed according to the mass ratio of (3-8): (4-7) uniformly mixing to obtain a first mixed solution; stabilizing agent, dispersing agent, main brightening agent, auxiliary brightening agent and wetting agent according to the mass ratio of (2-4): (3-5): (3-7): (2-5): (2-3) uniformly mixing to obtain a mixed solution II; and mixing the mixed solution I and the mixed solution II to prepare the methanesulfonic acid tin plating solution in the PCB production process, thereby obtaining the methanesulfonic acid tin plating solution in the PCB production process and the preparation method thereof.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211579367.4A CN115787005A (en) | 2022-12-08 | 2022-12-08 | Methanesulfonic acid tin plating solution in PCB production process and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211579367.4A CN115787005A (en) | 2022-12-08 | 2022-12-08 | Methanesulfonic acid tin plating solution in PCB production process and preparation method thereof |
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| CN115787005A true CN115787005A (en) | 2023-03-14 |
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| CN202211579367.4A Pending CN115787005A (en) | 2022-12-08 | 2022-12-08 | Methanesulfonic acid tin plating solution in PCB production process and preparation method thereof |
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