CN110205659B - Electrotinning additive and preparation method thereof - Google Patents
Electrotinning additive and preparation method thereof Download PDFInfo
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- CN110205659B CN110205659B CN201910646655.9A CN201910646655A CN110205659B CN 110205659 B CN110205659 B CN 110205659B CN 201910646655 A CN201910646655 A CN 201910646655A CN 110205659 B CN110205659 B CN 110205659B
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- deionized water
- glucose
- naphthol
- stabilizer
- vinyl ketone
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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
Abstract
The invention discloses an electrotinning additive and a preparation method thereof, relating to the technical field of electroplating. The invention takes deionized water as a solvent and comprises the following components in concentration: 0.2-0.55g/L of naphthol ethoxy sulfonic acid, 0.05-0.2g/L of diphenyl vinyl ketone, 0.09-0.35g/L of sodium allyl sulfonate, 0.07-0.15g/L of glucose, 4-7g/L of stabilizer and 0.5-2g/L of dispersant. According to the invention, the brightening system takes naphthol ethoxy sulfonic acid and sodium allylsulfonate as main brightening agents and takes diphenyl vinyl ketone and glucose as auxiliary brightening agents, so that the deposition of organic impurities on the surface of a cathode is reduced on the premise of obtaining the brightening condition meeting the requirement, and the electroplated tin layer with more uniform surface and less impurity content can be obtained.
Description
Technical Field
The invention belongs to the technical field of electroplating, and particularly relates to an electrotinning additive and a preparation method thereof.
Background
In the electroplating field, the pure tin coating is nontoxic, easy to weld, good in ductility, conductivity and corrosion resistance, and widely applied to various industries. In the electroplating process, only a coarse or dendritic tin coating can be obtained by a simple common electroplating tin plating solution, so that the additive is selectively added. The additives generally comprise a stabilizer, a brightener and a dispersant, can influence the nucleation of crystal grains, and play roles in brightening a plating layer, refining the crystal grains, inhibiting oxidation, improving mechanical and physical properties and the like.
At present, according to the long-term research of people, after the stabilizer, the brightener and the dispersant are compounded, the tin-plated layer with the required functionality can be directionally formed. In recent decades, benzylidene acetone-sulfate electroplating systems have been studied successively to improve the quality of tin plating and obtain bright and uniform tin plating, but in practical applications, it is found that the organic content of the tin plating layer obtained by the benzylidene acetone-sulfate electroplating system is relatively high, and the inventor guesses that the benzylidene acetone can adsorb divalent tin and also can correspondingly adsorb organic impurities such as C, S, N and O, so that the deposition layer is easy to have an inclusion phenomenon, that is, the deposition layer contains organic impurities such as C, S, N and O, which affect the crystal particles and orientation, so that the content of the organic impurities in the tin plating layer is high, and finally the performance of the tin plating layer is affected.
Disclosure of Invention
The invention aims to provide an electrotinning additive and a preparation method thereof, which can reduce the deposition of organic impurities on the surface of a cathode and obtain an electrotinning layer with more uniform surface and less impurity content on the premise of obtaining the brightness meeting the requirement.
In order to achieve the purpose, the invention adopts the following technical scheme: the electrolytic tinning additive takes deionized water as a solvent and comprises the following components in concentration: 0.2-0.55g/L of naphthol ethoxy sulfonic acid, 0.05-0.2g/L of diphenyl vinyl ketone, 0.09-0.35g/L of sodium allyl sulfonate, 0.07-0.15g/L of glucose, 4-7g/L of stabilizer and 0.5-2g/L of dispersant.
Deionized water is used as a solvent, and the deionized water contains the following components in concentration: 0.2g/L of naphthol ethoxy sulfonic acid, 0.05g/L of diphenyl vinyl ketone, 0.09g/L of sodium allyl sulfonate, 0.07g/L of glucose, 4g/L of stabilizer and 0.5g/L of dispersant.
Deionized water is used as a solvent, and the deionized water contains the following components in concentration: 0.3g/L of naphthol ethoxy sulfonic acid, 0.1g/L of diphenyl vinyl ketone, 0.1g/L of sodium allyl sulfonate, 0.09g/L of glucose, 5g/L of stabilizer and 0.8g/L of dispersant.
Deionized water is used as a solvent, and the deionized water contains the following components in concentration: 0.55g/L of naphthol ethoxy sulfonic acid, 0.2g/L of diphenyl vinyl ketone, 0.35g/L of sodium allyl sulfonate, 0.15g/L of glucose, 7g/L of stabilizer and 2g/L of dispersant.
The stabilizer is at least one of citric acid, sodium sorbate and oxalic acid.
The dispersing agent comprises polyoxyethylene fatty alcohol ether and polyethylene glycol, wherein the mass ratio of the polyoxyethylene fatty alcohol ether to the polyethylene glycol is 1: (0.5-1).
Deionized water is used as a solvent, and the deionized water contains the following components in concentration: 0.2-0.55g/L of naphthol ethoxy sulfonic acid, 0.05-0.2g/L of diphenyl vinyl ketone, 0.09-0.35g/L of sodium allyl sulfonate, 0.07-0.15g/L of glucose, 4-7g/L of citric acid, 0.1-0.25g/L of polyoxyethylene fatty alcohol ether and 0.1-0.25g/L of polyethylene glycol.
The preparation method comprises the following steps:
s1: weighing naphthol ethoxy sulfonic acid, sodium allylsulfonate, glucose and deionized water according to a formula ratio, and mixing to obtain a mixture A;
s2: weighing a stabilizer, a dispersant and diphenyl vinyl ketone according to a formula ratio, and mixing to obtain a mixture B;
s3: and adding the mixture B in the step S2 into the mixture A in the step S1, exhausting for 4-5min, and continuing stirring for 20-25min under the inert gas to obtain the electroplating additive.
The mixing condition in the step S1 is that stirring is carried out for 10-15min at room temperature, and the stirring speed is 50-100 r/min;
the mixing condition of the step S2 is that the mixture is stirred for 10-15min at the temperature of 30-35 ℃, the stirring speed is 20-70r/min, and then the temperature is reduced to the room temperature.
The inert gas is argon or nitrogen.
The invention discloses a method for improving the brightness of an electroplated tin layer, which is characterized in that naphthols ethoxysulfonic acid and sodium allylsulfonate are used as main brightening agents to enable the electroplated tin layer to obtain an ideal brightness effect, but in the actual production process, the brightness system is easy to enable the content of organic impurities of the electroplated tin layer to be higher, and due to improvement of the condition, the inventor finds that the content of the organic impurities of the electroplated tin layer is reduced after adding diphenyl vinyl ketone through a large number of creative tests and screens, and the effect reaches the optimal level after adding glucose. The above mechanism is still under investigation, and it is presumed that the presence of benzophenone has an effect of inhibiting the adsorption of organic impurities on the surface of the electrode, and the addition of glucose has an effect of enhancing this inhibitory effect.
Compared with the prior art, the invention has the following beneficial effects:
the electrotinning additive is suitable for electrotinning process, and the bright and uniform electrotinning layer can be obtained by adding the diphenyl vinyl ketone and the glucose into the bright system, and the obtained electrotinning layer has low organic impurity content, so that the performance of the electrotinning layer is better.
Detailed Description
The present invention will be described in further detail with reference to the following examples. It should not be understood that the scope of the above-described subject matter of the present invention is limited to the following examples.
Example 1 electrotinning additive
Deionized water is used as a solvent, and the deionized water contains the following components in concentration: 0.2g/L of naphthol ethoxy sulfonic acid, 0.05g/L of diphenyl vinyl ketone, 0.09g/L of sodium allyl sulfonate, 0.07g/L of glucose, 4g/L of citric acid, 0.25g/L of polyoxyethylene fatty alcohol ether and 0.25g/L of polyethylene glycol.
The preparation method comprises the following steps: the preparation method comprises the following steps:
s1: measuring naphthol ethoxy sulfonic acid, sodium allylsulfonate, glucose and deionized water according to the formula ratio, and stirring at room temperature at a rotating speed of 75r/min for 10min to obtain a mixture A;
s2: measuring the stabilizer, the dispersant and the diphenyl vinyl ketone according to the formula amount, stirring for 10min at the temperature of 30 ℃ at the rotating speed of 50r/min, and cooling to room temperature to obtain a mixture B;
s3: and adding the mixture B in the step S2 into the mixture A in the step S1, exhausting for 5min, and continuing stirring for 20min under nitrogen to obtain the electroplating additive.
Example 2 electrotinning additive
Deionized water is used as a solvent, and the deionized water contains the following components in concentration: 0.3g/L of naphthol ethoxy sulfonic acid, 0.1g/L of diphenyl vinyl ketone, 0.1g/L of sodium allyl sulfonate, 0.09g/L of glucose, 2g/L of citric acid, 3g/L of oxalic acid, 0.5g/L of polyoxyethylene fatty alcohol ether and 0.3g/L of polyethylene glycol.
The preparation method comprises the following steps: similar to example 1.
Example 3 electrotinning additive
Deionized water is used as a solvent, and the deionized water contains the following components in concentration: 0.4g/L of naphthol ethoxy sulfonic acid, 0.15g/L of diphenyl vinyl ketone, 0.2g/L of sodium allyl sulfonate, 0.12g/L of glucose, 1.5g/L of sodium sorbate, 4g/L of oxalic acid, 0.6g/L of polyoxyethylene fatty alcohol ether and 0.6g/L of polyethylene glycol.
The preparation method comprises the following steps: similar to example 1.
Example 4 electrotinning additive
Deionized water is used as a solvent, and the deionized water contains the following components in concentration: 0.5g/L of naphthol ethoxy sulfonic acid, 0.18g/L of diphenyl vinyl ketone, 0.3g/L of sodium allyl sulfonate, 0.15g/L of glucose, 3g/L of citric acid, 2g/L of sodium sorbate, 1g/L of polyoxyethylene fatty alcohol ether and 0.65g/L of polyethylene glycol.
The preparation method comprises the following steps: similar to example 1.
Example 5 electrotinning additive
Deionized water is used as a solvent, and the deionized water contains the following components in concentration: 0.55g/L of naphthol ethoxy sulfonic acid, 0.2g/L of diphenyl vinyl ketone, 0.35g/L of sodium allyl sulfonate, 0.15g/L of glucose, 3g/L of citric acid, 1g/L of sodium sorbate, 3g/L of oxalic acid, 1g/L of polyoxyethylene fatty alcohol ether and 1g/L of polyethylene glycol.
The preparation method comprises the following steps: similar to example 1.
Comparative example 1 electrotinning additive
Similar to example 2, except that: glucose was not added and the remaining parameters were the same as in example 2.
Comparative example 2 electrotinning additive
Similar to example 2, except that: no benzophenone was added and the remaining parameters were the same as in example 2.
Test I, surface appearance test
Test materials: the electrotinning additive described in examples 1-5 and comparative examples 1-2.
The test method comprises the following steps: adopting a tin plate as an anode and a copper plate as a cathode, adding 100mL/L sulfuric acid, 30g/L stannous sulfate, 500mL/L electrotinning additive and the balance of deionized water into a plating bath, and then immersing the tin plate and the copper plate into the plating bath at the temperature of 25 ℃ and the cathode current density of 1A/dm2Electroplating for 20min under the condition to obtain a tinned copper plate. The obtained tin-plated copper plate was observed under an SEM electron microscope.
Test two, solderability test
The tin-plated copper plates obtained in the first test of examples 1 to 5 and comparative examples 1 to 2 were dipped in solder, and then immersed in molten tin at 250 ℃ for 5 seconds, and after taking out, defects such as no pin hole, no bubble, no black spot, no tin plating, etc. were observed to be acceptable.
TABLE I results of test one and test two
As can be seen from the first Table, the tin-plated copper sheets after plating in examples 1 to 5 were bright and uniform as compared with those in comparative examples 1 to 2.
Test III, Oxidation resistance test
The tin-plated copper plate obtained in the first test of examples 1 to 5 was left for 7 days and observed under an SEM electron microscope.
And (3) test results: the oxidation of the surface of the tin-plated copper plate was not significant under SEM electron microscope observation.
Experiment four, analysis of organic impurities
The tin-plated copper plate stripped coating obtained in the first test and a tin-plated copper plate stripped coating prepared from a commercially available tin-plating additive (containing benzylidene acetone) were subjected to elemental analysis and combustion analysis to determine the content of organic impurities.
Epi-di organic impurity content (%)
| Group of | Plating impurities (C) | Plating impurities (S) | Coating impurities (N) | Plating impurities (O) |
| Example 1 | 0.0043 | 0.0009 | 0.0010 | 0.0015 |
| Example 2 | 0.0035 | 0.0005 | 0.0005 | 0.0013 |
| Example 3 | 0.0040 | 0.0005 | 0.0007 | 0.0011 |
| Example 4 | 0.0037 | 0.0007 | 0.0009 | 0.0017 |
| Example 5 | 0.0037 | 0.0010 | 0.0010 | 0.0013 |
| Comparative example 1 | 0.0127 | 0.0119 | 0.0052 | 0.0144 |
| Comparative example 2 | 0.0093 | 0.0164 | 0.0081 | 0.0163 |
| Certain tin plating additives are commercially available Additive agent | 0.0093 | 0.0019 | 0.0018 | 0.0075 |
As can be seen from Table II, the plating layers of the tin-plated copper sheets obtained in examples 1 to 5 had a small content of organic impurities. The higher organic impurity content of the tin-electroplated layer in comparative example 1 (no glucose added) and the higher organic impurity content of the tin-electroplated layer in comparative example 2 (benzophenone) compared to example 2 show that benzophenone and glucose can reduce the organic impurity content of the tin-electroplated layer.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (8)
1. An electrotinning additive, characterized in that: deionized water is used as a solvent, and the deionized water contains the following components in concentration: 0.2-0.55g/L of naphthol ethoxy sulfonic acid, 0.05-0.2g/L of diphenyl vinyl ketone, 0.09-0.35g/L of sodium allyl sulfonate, 0.07-0.15g/L of glucose, 4-7g/L of stabilizer and 0.5-2g/L of dispersant;
the stabilizer is at least one of citric acid, sodium sorbate and oxalic acid;
the dispersing agent comprises polyoxyethylene fatty alcohol ether and polyethylene glycol, wherein the mass ratio of the polyoxyethylene fatty alcohol ether to the polyethylene glycol is 1: (0.5-1).
2. The electrotinning additive of claim 1 wherein: deionized water is used as a solvent, and the deionized water contains the following components in concentration: 0.2g/L of naphthol ethoxy sulfonic acid, 0.05g/L of diphenyl vinyl ketone, 0.09g/L of sodium allyl sulfonate, 0.07g/L of glucose, 4g/L of stabilizer and 0.5g/L of dispersant.
3. The electrotinning additive of claim 1 wherein: deionized water is used as a solvent, and the deionized water contains the following components in concentration: 0.3g/L of naphthol ethoxy sulfonic acid, 0.1g/L of diphenyl vinyl ketone, 0.1g/L of sodium allyl sulfonate, 0.09g/L of glucose, 5g/L of stabilizer and 0.8g/L of dispersant.
4. The electrotinning additive of claim 1 wherein: deionized water is used as a solvent, and the deionized water contains the following components in concentration: 0.55g/L of naphthol ethoxy sulfonic acid, 0.2g/L of diphenyl vinyl ketone, 0.35g/L of sodium allyl sulfonate, 0.15g/L of glucose, 7g/L of stabilizer and 2g/L of dispersant.
5. An electrotinning additive, characterized in that: deionized water is used as a solvent, and the deionized water contains the following components in concentration: 0.2-0.55g/L of naphthol ethoxy sulfonic acid, 0.05-0.2g/L of diphenyl vinyl ketone, 0.09-0.35g/L of sodium allyl sulfonate, 0.07-0.15g/L of glucose, 4-7g/L of citric acid, 0.1-0.25g/L of polyoxyethylene fatty alcohol ether and 0.1-0.25g/L of polyethylene glycol.
6. A preparation method of the electrotinning additive is characterized in that: the preparation method comprises the following steps:
s1: weighing naphthol ethoxy sulfonic acid, sodium allylsulfonate, glucose and deionized water according to a formula ratio, and mixing to obtain a mixture A;
s2: weighing a stabilizer, a dispersant and diphenyl vinyl ketone according to a formula ratio, and mixing to obtain a mixture B;
s3: adding the mixture B in the step S2 into the mixture A in the step S1, exhausting for 4-5min, and continuing stirring for 20-25min under inert gas to obtain an electroplating additive;
the stabilizer is at least one of citric acid, sodium sorbate and oxalic acid;
the dispersing agent comprises polyoxyethylene fatty alcohol ether and polyethylene glycol, wherein the mass ratio of the polyoxyethylene fatty alcohol ether to the polyethylene glycol is 1: (0.5-1).
7. The method for preparing an electrotinning additive according to claim 6 wherein: the mixing condition in the step S1 is that stirring is carried out for 10-15min at room temperature, and the stirring speed is 50-100 r/min;
the mixing condition of the step S2 is that the mixture is stirred for 10-15min at the temperature of 30-35 ℃, the stirring speed is 20-70r/min, and then the temperature is reduced to the room temperature.
8. The method for preparing an electrotinning additive according to claim 6 wherein: the inert gas is argon or nitrogen.
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| CN111472027B (en) * | 2020-05-09 | 2020-12-25 | 广东哈福科技有限公司 | Electrotinning additive and preparation method and use method thereof |
| CN111850644B (en) * | 2020-06-28 | 2022-08-26 | 南通松伟压铸有限公司 | Zipper coloring method |
| CN112538643B (en) * | 2020-11-17 | 2022-05-13 | 珠海松柏科技有限公司 | High-speed tin plating additive and tin plating solution |
| CN113684508A (en) * | 2021-09-02 | 2021-11-23 | 中山市康迪斯威科技有限公司 | Compacting agent for neutral electrotinning, electroplating solution containing compacting agent, preparation method and application thereof |
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