CN111472027B - Electrotinning additive and preparation method and use method thereof - Google Patents
Electrotinning additive and preparation method and use method thereof Download PDFInfo
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- CN111472027B CN111472027B CN202010385991.5A CN202010385991A CN111472027B CN 111472027 B CN111472027 B CN 111472027B CN 202010385991 A CN202010385991 A CN 202010385991A CN 111472027 B CN111472027 B CN 111472027B
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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
- C25D3/30—Electroplating: Baths therefor from solutions of tin
- C25D3/32—Electroplating: Baths therefor from solutions of tin characterised by the organic bath constituents used
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Abstract
The invention discloses an electrotinning additive, which takes water as a solvent and comprises the following components in concentration: 1-phenyl-2-pentanone: 0.2-20 g/L; 1- (3, 4-dihydroxyphenyl) -1-pentanone: 0.2-20 g/L; naphthol ethoxy sulfonic acid: 0.2-20 g/L; resorcinol: 1-20 g/L; antioxidant: 1-20 g/L; brightening agent: 1-30 g/L. The electrotinning additive can effectively reduce the generation of bubbles in the electroplating process, thereby reducing the dissolution of oxygen and ensuring the electroplating effect.
Description
Technical Field
The invention relates to the technical field of electroplating, in particular to an electrotinning additive and a preparation method and a use method thereof.
Background
Printed Circuit Boards (PCBs) are one of the important components in the electronics industry and are the supports for electronic components. Generally, a process of manufacturing a printed circuit board includes double-sided copper plating → machining → copper deposition → film (screen printing) → copper electroplating → tin electroplating → etching → tin stripping → processing. The conventional electrotinning additive is developed based on gantry line electroplating, however, gantry lines have low production efficiency, high cost and low safety compared with VCP lines, and the application of the conventional electrotinning additive to VCP lines has the following two problems: 1) in the electroplating process, a large amount of bubbles are produced on a VCP line, which easily causes phenomena of plating leakage, uneven plating and the like. 2) The generation of a large amount of bubbles leads to more dissolved oxygen, so that tetravalent tin is generated too fast, the frequency of tank replacement is high, and the cost is increased. Therefore, there is a need for an electrolytic tinning additive suitable for VCP lines that can solve the above two difficulties.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides the electrotinning additive which can effectively reduce the generation of bubbles in the electroplating process, thereby reducing the dissolution of oxygen and ensuring the electroplating effect.
The technical purpose of the invention is realized by the following technical scheme:
an electrolytic tinning additive, which takes water as a solvent and comprises the following components in concentration: 1-phenyl-2-pentanone: 0.2-20 g/L; 1- (3, 4-dihydroxyphenyl) -1-pentanone: 0.2-20 g/L; naphthol ethoxy sulfonic acid: 0.2-20 g/L; resorcinol: 1-20 g/L; antioxidant: 1-20 g/L; brightening agent: 1-30 g/L.
Preferably, the water is used as a solvent, and the following components are contained in the following concentrations: 1-phenyl-2-pentanone: 3-15 g/L; 1- (3, 4-dihydroxyphenyl) -1-pentanone: 1-15 g/L; naphthol ethoxy sulfonic acid: 1-15 g/L; resorcinol: 1-15 g/L; antioxidant: 5-20 g/L; brightening agent: 5-28 g/L.
Preferably, the antioxidant is at least one of diisobutyl ketone and methyl isobutyl ketone.
Further preferably, the antioxidant is methyl isobutyl ketone.
Preferably, the brightener is at least one of benzalacetone, 2-hydroxy-1-naphthaldehyde and sulfosalicylic acid.
Further preferably, the brightener is benzalacetone.
Preferably, the water is deionized water.
The invention also aims to provide a preparation method of the electrotinning additive, which comprises the following steps:
a preparation method of the electrotinning additive comprises the following steps:
(1) adding water to a container;
(2) under the condition of stirring, adding 1-phenyl-2-pentanone according to the proportion until the mixture is completely dissolved;
(3) adding the antioxidant in proportion under the condition of stirring until the antioxidant is completely dissolved;
(4) adding 1- (3, 4-dihydroxyphenyl) -1-pentanone in proportion while stirring until complete dissolution;
(5) under the condition of stirring, adding a brightener in proportion until the brightener is completely dissolved;
(6) under the condition of stirring, adding naphthol ethoxy sulfonic acid in proportion until the naphthol ethoxy sulfonic acid is completely dissolved;
(7) under the condition of stirring, adding resorcinol in proportion until resorcinol is completely dissolved;
(8) adding water to required amount, and stirring uniformly after completion.
The third purpose of the invention is to provide a using method of the electrotinning additive, which comprises the following steps:
a method of using the electrotinning additive as described above, comprising the steps of:
the above electrolytic tin plating additive was added to a tin plating solution in an amount of 10%, and then the plating was carried out at a temperature of 25 ℃.
The invention has the beneficial effects that:
(1) the electrotinning additive can effectively reduce the generation of bubbles in the electroplating process, thereby reducing the dissolution of oxygen;
(2) the electrotinning additive disclosed by the invention has a good anti-oxidation effect, can effectively prevent tetravalent tin from generating under a large current, and prolongs the service life of bath solution;
(3) the electrotinning additive has excellent electroplating performance, the dispersing capacity can reach more than 95 percent, the current efficiency can reach more than 96 percent, and the deep plating capacity can reach 100 percent.
Detailed Description
Examples 1 to 11:
a preparation method of the electrotinning additive comprises the following steps:
(1) adding water to a container;
(2) under the condition of stirring, adding 1-phenyl-2-pentanone according to the proportion until the mixture is completely dissolved;
(3) adding the antioxidant in proportion under the condition of stirring until the antioxidant is completely dissolved;
(4) adding 1- (3, 4-dihydroxyphenyl) -1-pentanone in proportion while stirring until complete dissolution;
(5) under the condition of stirring, adding a brightener in proportion until the brightener is completely dissolved;
(6) under the condition of stirring, adding naphthol ethoxy sulfonic acid in proportion until the naphthol ethoxy sulfonic acid is completely dissolved;
(7) under the condition of stirring, adding resorcinol in proportion until resorcinol is completely dissolved;
(8) adding water to required amount, and stirring uniformly after completion.
Wherein the water is deionized water, the antioxidant is one of diisobutyl ketone and methyl isobutyl ketone, and the brightener is one of benzalacetone, 2-hydroxy-1-naphthaldehyde and sulfosalicylic acid.
Wherein the concentrations of the components in examples 1-8 are shown in Table 1:
table 1: each component content amount in the electrolytic tin plating additive of examples 1 to 8 (g/L)
The concentrations of the components in example 9 are shown in table 2:
table 2: the content of each component in the electrolytic tin plating additive of example 9 (g/L)
The concentrations of the components in example 10 are shown in table 3:
table 3: the content of each component in the electrolytic tin plating additive of example 10 (g/L)
The concentrations of the components in example 11 are shown in table 4:
table 4: the content of each component in the electrolytic tin plating additive of example 11 (g/L)
The electrolytic tin plating additives obtained in examples 1 to 11 were used in the following manner by adding 10% of the above electrolytic tin plating additive to a tin plating solution, then performing plating at a temperature of 25 ℃ and testing the properties.
The dispersion property of the plating solution is tested according to the following method:
the dispersibility of the plating solution was measured by the Hull cell method at a current density of 1A, the area of the plated portion of the cathode, which was shifted by 1cm from the center line, was divided into 10 grids, the cathode thicknesses (1,5,8) at the center portions of the 1 st, 5 th and 8 th grids were measured by a micrometer screw, and the dispersibility of the plating solution was calculated by the calculation formula TP i/1X 100%.
The deep plating performance of the electroplating solution is tested according to the following method:
the deep plating performance of the plating solution is measured by an inner hole method. A copper tube with an opening at one end, a diameter (phi) of 10mm and a tube length (L) of 100mm is used as a cathode, the copper tube is cut longitudinally after plating is carried out under certain conditions, and the length (S) of an inner wall plating layer is measured, wherein the deep plating capacity of the plating solution is S/L multiplied by 100%.
The test results are shown in table 5:
table 5: results of testing the Performance of the plating solutions of examples 1 to 11
As can be seen from Table 5, the dispersion ability of the electroplating solution containing the electrotinning additive can reach more than 95%, and can reach 98.5% at most; the current efficiency can reach more than 96 percent and can reach 99.1 percent to the maximum; the deep plating capacity can reach 100 percent; and no bubble is generated in the electroplating and ultrasonic oscillation processes, no turbidity occurs after the electroplating and ultrasonic oscillation processes are continuously used for 30 days, the maximum continuous use time can be 56 days, and the cost is effectively reduced.
Meanwhile, comparing the examples 2, 9, 10 and 11, it can be seen that the electroplating solution has more excellent performance when the antioxidant is methyl isobutyl ketone and the brightener is benzalacetone, which indicates that the antioxidant and the brightener can play a synergistic role in the tin electroplating additive, and can effectively improve various performances of the electroplating solution.
Comparative examples 1 to 7:
comparative example 1 is a commercially available electrotinning additive of the same type.
The concentrations of the components of comparative examples 2 to 7 are shown in Table 6.
Table 6: the electrolytic tin plating additives of comparative examples 2 to 7 contain the respective components in the amounts (g/L)
The electrolytic tin plating additives prepared in comparative examples 2 to 7 and the electrolytic tin plating additive of comparative example 1 were used in such a manner that 10% of the above electrolytic tin plating additive was added to a tin plating solution, and then plating was performed at a temperature of 25 c, and the performance was tested.
The dispersion property of the plating solution is tested according to the following method:
the dispersibility of the plating solution was measured by the Hull cell method at a current density of 1A, the area of the plated portion of the cathode, which was shifted by 1cm from the center line, was divided into 10 grids, the cathode thicknesses (1,5,8) at the center portions of the 1 st, 5 th and 8 th grids were measured by a micrometer screw, and the dispersibility of the plating solution was calculated by the calculation formula TP i/1X 100%.
The deep plating performance of the electroplating solution is tested according to the following method:
the deep plating performance of the plating solution is measured by an inner hole method. A copper tube with an opening at one end, a diameter (phi) of 10mm and a tube length (L) of 100mm is used as a cathode, the copper tube is cut longitudinally after plating is carried out under certain conditions, and the length (S) of an inner wall plating layer is measured, wherein the deep plating capacity of the plating solution is S/L multiplied by 100%.
The test results are shown in table 7:
table 7: results of testing the Performance of the plating solutions of comparative examples 1 to 7
As can be seen from Table 7, it can be seen from the performance test of the plating solutions that the present electrolytic tinning additive is far superior to the commercial electrolytic tinning additives of the same type, as seen from comparative examples 1 to 11 and comparative example 1.
As can be seen from the comparison of example 2 and comparative examples 2-7, 1-phenyl-2-pentanone, 1- (3, 4-dihydroxyphenyl) -1-pentanone and naphthol ethoxy sulfonic acid in the electrotinning additive have a main synergistic effect on reducing the generation of bubbles in the electroplating solution, and when the electrotinning additive contains 1-phenyl-2-pentanone, 1- (3, 4-dihydroxyphenyl) -1-pentanone and naphthol ethoxy sulfonic acid, the generation of bubbles in the electroplating solution can be greatly reduced, and in addition, the absence of any component of the electrotinning additive has a great influence on the performances of the final electroplating solution.
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 (8)
1. An electrotinning additive, characterized in that: water is used as a solvent, and the components with the following concentrations are contained:
1-phenyl-2-pentanone: 0.2-20 g/L;
1- (3, 4-dihydroxyphenyl) -1-pentanone: 0.2-20 g/L;
naphthol ethoxy sulfonic acid: 0.2-20 g/L;
resorcinol: 1-20 g/L;
antioxidant: 1-20 g/L;
brightening agent: 1-30 g/L.
2. The electrolytic tinning additive according to claim 1, characterized in that: water is used as a solvent, and the components with the following concentrations are contained:
1-phenyl-2-pentanone: 3-15 g/L;
1- (3, 4-dihydroxyphenyl) -1-pentanone: 1-15 g/L;
naphthol ethoxy sulfonic acid: 1-15 g/L;
resorcinol: 1-15 g/L;
antioxidant: 5-20 g/L;
brightening agent: 5-28 g/L.
3. The electrolytic tinning additive according to claim 1, characterized in that: the antioxidant is at least one of diisobutyl ketone and methyl isobutyl ketone.
4. The electrolytic tinning additive according to claim 3, characterized in that: the antioxidant is methyl isobutyl ketone.
5. The electrolytic tinning additive according to claim 1, characterized in that: the brightener is at least one of benzalacetone, 2-hydroxy-1-naphthaldehyde and sulfosalicylic acid.
6. The electrolytic tinning additive according to claim 5, wherein: the brightener is benzalacetone.
7. A method for preparing the electrotinning additive of any one of claims 1 to 6 comprising the steps of:
(1) adding water to a container;
(2) under the condition of stirring, adding 1-phenyl-2-pentanone according to the proportion until the mixture is completely dissolved;
(3) adding the antioxidant in proportion under the condition of stirring until the antioxidant is completely dissolved;
(4) adding 1- (3, 4-dihydroxyphenyl) -1-pentanone in proportion while stirring until complete dissolution;
(5) under the condition of stirring, adding a brightener in proportion until the brightener is completely dissolved;
(6) under the condition of stirring, adding naphthol ethoxy sulfonic acid in proportion until the naphthol ethoxy sulfonic acid is completely dissolved;
(7) under the condition of stirring, adding resorcinol in proportion until resorcinol is completely dissolved;
(8) adding water to required amount, and stirring uniformly after completion.
8. The method of using the electrotinning additive of any one of claims 1 to 6, comprising the steps of: the above electrolytic tin plating additive was added to a tin plating solution in an amount of 10%, and then the plating was carried out at a temperature of 25 ℃.
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| CN114737228B (en) * | 2022-06-09 | 2022-08-26 | 深圳市板明科技股份有限公司 | Circuit board electrotinning brightener and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837415A (en) * | 2005-02-28 | 2006-09-27 | 罗门哈斯电子材料有限公司 | Acid electrolytes |
| CN103422130A (en) * | 2012-05-14 | 2013-12-04 | 中国科学院金属研究所 | Plating solution and method for electroplating bright tin plating layer |
| CN104562100A (en) * | 2014-12-31 | 2015-04-29 | 苏州禾川化学技术服务有限公司 | Multi-functional half-white brightness tin-plated additive |
| CN106835210A (en) * | 2017-03-09 | 2017-06-13 | 昆明理工大学 | A kind of sulfate bright tin plating solution and preparation method thereof |
| CN108866583A (en) * | 2018-08-28 | 2018-11-23 | 广州三孚新材料科技股份有限公司 | Tin or tin-lead alloy plating solution applied to leadless electronic component, and preparation method and plating method thereof |
| CN110205659A (en) * | 2019-07-17 | 2019-09-06 | 广州三孚新材料科技股份有限公司 | Electrotinning additive and preparation method thereof |
-
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837415A (en) * | 2005-02-28 | 2006-09-27 | 罗门哈斯电子材料有限公司 | Acid electrolytes |
| CN103422130A (en) * | 2012-05-14 | 2013-12-04 | 中国科学院金属研究所 | Plating solution and method for electroplating bright tin plating layer |
| CN104562100A (en) * | 2014-12-31 | 2015-04-29 | 苏州禾川化学技术服务有限公司 | Multi-functional half-white brightness tin-plated additive |
| CN106835210A (en) * | 2017-03-09 | 2017-06-13 | 昆明理工大学 | A kind of sulfate bright tin plating solution and preparation method thereof |
| CN108866583A (en) * | 2018-08-28 | 2018-11-23 | 广州三孚新材料科技股份有限公司 | Tin or tin-lead alloy plating solution applied to leadless electronic component, and preparation method and plating method thereof |
| CN110205659A (en) * | 2019-07-17 | 2019-09-06 | 广州三孚新材料科技股份有限公司 | Electrotinning additive and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Effects of Additive Agents on the Kinetics Of Tin Electrodeposition from An Acidic Solution of Tin(II) Sulfate;G.-S. Tzeng;《PLATING & SURFACE FINISHING》;19951130;第82卷(第11期);第67-71页 * |
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Address after: No. 8, Dongwei Avenue, Fusha Industrial Park, Fusha Town, Zhongshan City, Guangdong Province, 528400 Patentee after: Guangdong Hafu Technology Co.,Ltd. Address before: 528400, Fu Sha town, Guangdong City, Zhongshan province Fu Sha Industrial Park Patentee before: GUANGDONG HAFU SCIENCE & TECHNOLOGY Co.,Ltd. |