CN109596681B - Method for detecting uniform plating capacity of tin methanesulfonate electroplating solution - Google Patents
Method for detecting uniform plating capacity of tin methanesulfonate electroplating solution Download PDFInfo
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- CN109596681B CN109596681B CN201710938511.1A CN201710938511A CN109596681B CN 109596681 B CN109596681 B CN 109596681B CN 201710938511 A CN201710938511 A CN 201710938511A CN 109596681 B CN109596681 B CN 109596681B
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
Abstract
The invention relates to a method for detecting the throwing power of tin methanesulfonate electroplating solution, which mainly solves the technical problem that the throwing power of the existing tin methanesulfonate electroplating solution cannot be directly detected. The invention discloses a method for detecting the uniform plating capacity of tin methanesulfonate electroplating solution, which comprises the following steps: 1) preparing a cathode sample; 2) heating the tin methane sulfonate electroplating solution; 3) installing a cathode and an anode for electroplating; 4) electroplating the sample, taking the sample out of the Harlin tank after the electroplating is finished, cleaning the sample and drying the sample; 5) detecting the tin plating amount of the sample; 6) and calculating the uniform plating capacity of the tin methane sulfonate electroplating solution. The method can visually reflect the uniform condition of the plating layer, and can be used for evaluating the uniform plating capacity of the tin methane sulfonate electroplating solution when electroplating the plating layer with low tin content.
Description
Technical Field
The invention relates to a method for detecting the performance of an electroplating solution, in particular to a method for detecting the uniform plating capacity of a tin methanesulfonate electroplating solution, and belongs to the technical field of electroplating solution performance detection.
Background
The tin electroplating process with methanesulfonic acid (MSA) is an environment-friendly tin electroplating technology appearing in recent years, and the technology is used by plum steel, first steel, sand steel and Zhongyue tin electroplating units at home. The core of the technology is the formula of the MSA electroplating solution, so a great deal of experimental research is carried out on the performance of the electroplating solution, and one important research content is the uniform plating capacity of the electroplating solution. The plating solution uniform plating capability refers to the capability of the plating solution to ensure uniform distribution of the thickness of a plating layer, and is one of necessary indexes for research, comparison and evaluation of a new process of the same plating solution or different plating solution systems. The better the throwing power of the plating solution, the more uniform the thickness distribution of the plating layer.
The detection of the uniform plating capacity of the tin methane sulfonate plating solution is commonly used in a universal 'far and near cathode method', the experimental device adopts a Harlin groove, and the detection method is thatTwo tin-plated substrates with the same size are placed in the tank to serve as cathodes, and anodes with the same size as the cathodes are placed between the two cathodes, so that the distance between the two cathodes is different. Pouring a certain volume of MSA electroplating solution to be tested into a Harlin tank, setting current and electroplating time, switching on a power supply, starting tin layer electroplating, and substituting the weight gain of two cathodes into a plating-equalizing capacity calculation formula pc ═ k-D after electroplating is finishedNear to/DFar away) (k-1) × 100% (pc — dispersing ability (expressed as a percentage); dNear to-weight gain (grams) after cathodic plating; dFar away-weight gain (grams) after telecast plating; k is the distance between the far cathode and the anode and the distance between the near cathode and the anode; ) And calculating to obtain the uniform plating capacity value of the MSA plating solution. The performance test is carried out on several MSA plating solutions under the same condition, and the larger the obtained uniform plating value is, the better the uniform plating capability of the plating solution is.
For the electrolytic tinning product, the tinning amount was 1.1g/m2～12.8g/m2In the meantime. The 'far and near cathode method' detects the following problems existing in the uniform plating capacity of the MSA plating solution: firstly, substituting a far and near cathode weight gain mode into a formula to calculate the uniform plating capacity of the MSA plating solution, wherein the uniform plating capacity cannot visually reflect the uniform plating condition; secondly, the method is used for detecting the uniform plating capacity of the MSA plating solution, the electrifying time is long, the target tin plating amount is high, and the general plating layer exceeds 15.6g/m2The tin plating amount of the target low tin is less than or equal to 5.6g/m2The plating area of the cathode is small due to the limitation of the solution volume of the bath body (for example, the plating area of a 1.5L Harlin bath is only 0.0055m2) Because the weight gain of the far and near cathodes is limited, the weighing error and other factors influence, the plating solution uniform plating capacity can not be calculated by substituting the formula, so that the method is not suitable for evaluating the uniform plating capacity of the MSA plating solution when plating a low-tin plating layer.
The chinese patent application publication No. CN1026866079A discloses a method for testing the throwing power of an electrolytic tinning solution, which applies a general method for testing the throwing power of a plating solution to an electrolytic tinning solution, and the method cannot visually reflect the condition of uniform plating and is not suitable for evaluating the throwing power of an MSA plating solution when a plating layer with a low tin content is electroplated.
The Chinese patent document with the grant publication number of CN204855503U discloses a device for testing the uniform plating capacity of electrotinning, which mainly solves the problem that the distance between an anode and a near-far cathode of an experimental device is accurately adjustable, and the method for testing the uniform plating capacity of the electrotinning solution is also a universal testing method.
Disclosure of Invention
The invention aims to provide a method for detecting the throwing power of tin methane sulfonate electroplating solution, which mainly solves the technical problem that the throwing power of the existing tin methane sulfonate electroplating solution cannot be directly detected.
The invention adopts the technical scheme that the method for detecting the uniform plating capacity of the tin methane sulfonate electroplating solution comprises the following steps:
1) preparing a cathode sample, continuously cutting two steel plates with the same size as the anode on a cold-rolled tin-plated substrate, and respectively carrying out oil removal and acid washing on the two steel plates to prepare the cathode sample;
2) heating the tin methane sulfonate electroplating solution, injecting a certain amount of the tin methane sulfonate electroplating solution into the Harlin bath, heating the electroplating solution in the Harlin bath in a water bath to the set temperature of the electroplating process, and keeping the temperature;
3) installing a cathode and an anode for electroplating, respectively placing two cathode samples at fixed positions of a Harlin tank, installing an anode with the same size as the cathode between the two cathodes, and enabling the distance between the anode and the two cathodes to be the same;
4) electroplating the sample, and electroplating the sample according to the set current density and time; after the electroplating is finished, taking out the sample from the Harlin groove, cleaning the sample and drying the sample;
5) detecting the tin plating amount of the samples, and respectively detecting the tin plating amount X of a circular area with the diameter of 2cm, which is formed by using an electrochemical workstation timing-potential method and has 3 points in the center line of the plating layer and the bilateral symmetry 2 points of the two samples along the length direction of the single cathodeiI 1,2, 3. cndot.6 in g/m2；
6) And calculating the uniform plating capacity of the tin methane sulfonate electroplating solution, wherein the uniform plating capacity of the tin methane sulfonate electroplating solution is the variance of the measured point tin plating amount of the electroplated sample.
The method for detecting the uniform plating capacity of the tin methanesulfonate electroplating solution is not a quantitative detection index, but a comparative detection index for judging the uniform plating performance of two or more electroplating solutions.
The mechanism of the method of the invention is as follows: the plating solution uniform plating capacity is defined as the capacity of the plating solution to enable the thickness of a plating layer to be uniformly distributed, and the uniformity of the thickness of the plating layer is represented by the variance of the tin plating amount of the plating layer after the tin methane sulfonate plating solution is electroplated according to a certain electroplating process, so that the uniform plating capacity of the tin methane sulfonate plating solution is obtained.
Compared with the prior art, the technical scheme has the following positive effects: 1. mainly solves the problem that the uniform condition of a plating layer can not be visually reflected in the existing detection method of a near-far cathode method. The method is used for evaluating the uniform plating capacity of the plating solution, and the evaluation result is more visual. 2. The detection method can be operated by common electroplating technicians, and can also be used for detecting the plating capacity of the plating solution for low-tin plating layers with short electroplating time.
Drawings
FIG. 1 is a schematic view of a single-cathode plating and tin plating amount detection area according to the present invention.
The notation in the figure is: 1-no coating area; 2-coating area; 3-tin plating amount detection zone.
Detailed Description
The invention is further described with reference to the following figures and specific embodiments.
Example 1 referring to FIG. 1, the throwing power of A-grade tin methanesulfonate-based electroplating solution was examined, and the cold-rolled annealed tin electroplated substrate used had a thickness of 0.2mm, a surface roughness Ra of 0.32um, a yield strength of 356MPa, a tensile strength of 402MPa, and a post-fracture elongation A50mmIs 31 percent;
the target coating thickness of the electroplating is 1.1g/m2For example, the volume of the Harlin groove is 1.5L, and the set current density is 2A/dm2Plating efficiency of 0.86 and plating area of 0.55dm2Calculating to obtain electroplating current of 1.1A and electroplating time of 20.8s according to Faraday's law;
a method for detecting the uniform plating capacity of tin methanesulfonate electroplating solution comprises the following steps:
1) preparing a cathode sample, continuously cutting two steel plates with the same size as the anode on a cold-rolled tin-plated substrate, and respectively carrying out oil removal and acid washing on the two steel plates to prepare the cathode sample;
2) heating the tin methane sulfonate electroplating solution, injecting the A-brand tin methane sulfonate electroplating solution into the Harlin groove to scale marks in the specification of 1.5, heating the electroplating solution in the Harlin groove to 45 ℃ in a water bath, and preserving heat;
3) installing a cathode and an anode for electroplating, respectively placing two cathode samples at fixed positions of a Harlin tank, installing an anode with the same size as the cathode between the two cathodes, and enabling the distance between the anode and the two cathodes to be the same;
4) electroplating the sample, wherein the electroplating current is 1.1A, the electroplating time is 20.8s, and after the electroplating is finished, taking the sample out of the Harlin tank, cleaning the sample and drying the sample;
5) detecting the tin plating amount of the samples, respectively detecting the tin plating amount of circular areas with the diameter of 2cm, which are formed by 3 points of the middle point of the plating layer center line and the bilateral symmetry 2 points of the two samples along the length direction of the single cathode by using an electrochemical workstation timing-potential method, and obtaining the tin plating amount of 1.15g/m2，1.11g/m2，1.15g/m2，1.16g/m2，1.10g/m2，1.16g/m2；
6) Calculating the uniform plating capacity of the A-grade tin methanesulfonate electroplating solution, wherein the uniform plating capacity of the tin methanesulfonate electroplating solution is the variance of the tin plating amount of the measurement point of the electroplated sample, and obtaining the uniform plating capacity S of the A-grade electroplating solutionA＝0.00059。
Example 2 referring to FIG. 1, the throwing power of a B-grade tin methanesulfonate-based electroplating solution was examined, and the cold-rolled annealed tin electroplated substrate used had a thickness of 0.2mm, a surface roughness Ra of 0.32um, a yield strength of 356MPa, a tensile strength of 402MPa, and a post-fracture elongation A50mmIs 31 percent;
the target coating thickness of the electroplating is 1.1g/m2For example, the volume of the Harlin groove is 1.5L, and the set current density is 2A/dm2Plating efficiency of 0.86 and plating area of 0.55dm2Calculating to obtain electroplating current of 1.1A and electroplating time of 20.8s according to Faraday's law;
a method for detecting the uniform plating capacity of tin methanesulfonate electroplating solution comprises the following steps:
1) preparing a cathode sample, continuously cutting two steel plates with the same size as the anode on a cold-rolled tin-plated substrate, and respectively carrying out oil removal and acid washing on the two steel plates to prepare the cathode sample;
2) heating the tin methane sulfonate electroplating solution, injecting the tin methane sulfonate electroplating solution of the brand B into the Harlin groove to scale marks in the specification of 1.5, heating the electroplating solution in the Harlin groove to 45 ℃ in a water bath, and preserving heat;
3) installing a cathode and an anode for electroplating, respectively placing two cathode samples at fixed positions of a Harlin tank, installing an anode with the same size as the cathode between the two cathodes, and enabling the distance between the anode and the two cathodes to be the same;
4) electroplating the sample, wherein the electroplating current is 1.1A, the electroplating time is 20.8s, and after the electroplating is finished, taking the sample out of the Harlin tank, cleaning the sample and drying the sample;
5) detecting the tin plating amount of the samples, respectively detecting the tin plating amount of a circular area with the diameter of 2cm, which is formed by the center point of the plating layer center line of the two samples along the length direction of the single cathode and the positions of the bilateral symmetry 2 points, by using an electrochemical workstation timing-potential method, and obtaining the following tin plating amounts: 0.95g/m2，1.03g/m2，0.86g/m2，0.93g/m2，0.91g/m2，0.86g/m2；
6) Calculating the uniform plating capacity of the B-brand tin methanesulfonate system electroplating solution, wherein the uniform plating capacity of the tin methanesulfonate system electroplating solution is the variance of the measured point tin plating amount of the electroplated sample, and obtaining the uniform plating capacity S of the B-brand plating solutionB＝0.0041。
In examples 1 and 2, SA<SBCompared with the A-grade tin methanesulfonate electroplating solution and the B-grade tin methanesulfonate electroplating solution, the variance of the tin plating amount of the detected point of the plating layer obtained under the same experimental conditions is small, namely the thickness distribution of the plating layer is relatively uniform. The plating ability of the A-grade tin methanesulfonate electroplating solution in example 1 was good.
In addition to the above embodiments, other embodiments are also possible in the present technical solution. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.
Claims (1)
1. A method for detecting the uniform plating capacity of tin methanesulfonate electroplating solution is characterized by comprising the following steps:
1) preparing a cathode sample, continuously cutting two steel plates with the same size as the anode on a cold-rolled tin-plated substrate, and respectively carrying out oil removal and acid washing on the two steel plates to prepare the cathode sample;
2) heating the tin methane sulfonate electroplating solution, injecting a certain amount of the tin methane sulfonate electroplating solution into the Harlin bath, heating the electroplating solution in the Harlin bath in a water bath to the set temperature of the electroplating process, and keeping the temperature;
3) installing a cathode and an anode for electroplating, respectively placing two cathode samples at fixed positions of a Harlin tank, installing an anode with the same size as the cathode between the two cathodes, and enabling the distance between the anode and the two cathodes to be the same;
4) electroplating the sample, and electroplating the sample according to the set current density and time; after the electroplating is finished, taking out the sample from the Harlin groove, cleaning the sample and drying the sample;
5) detecting the tin plating amount of the samples, and respectively detecting the tin plating amount X of a circular area with the diameter of 2cm, which is formed by using an electrochemical workstation timing-potential method and has 3 points in the center line of the plating layer and the bilateral symmetry 2 points of the two samples along the length direction of the single cathodeiI 1,2, 3. cndot.6 in g/m2；
6) And calculating the uniform plating capacity of the tin methane sulfonate electroplating solution, wherein the uniform plating capacity of the tin methane sulfonate electroplating solution is the variance of the measured point tin plating amount of the electroplated sample.
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Citations (5)
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|---|---|---|---|---|
| US4075065A (en) * | 1975-07-07 | 1978-02-21 | Handy & Harman | Gold plating bath and process |
| JPH03146689A (en) * | 1989-10-31 | 1991-06-21 | Nec Kansai Ltd | Solder and tin plating solution |
| CN102162110A (en) * | 2011-01-31 | 2011-08-24 | 张家港市新港星科技有限公司 | Methyl sulfonate tinning electrolyte and tinning method of steel strip or steel plate |
| CN102866079A (en) * | 2012-09-20 | 2013-01-09 | 信丰正天伟电子科技有限公司 | Testing method of electrotinning uniform plating capacity |
| CN204855503U (en) * | 2015-07-24 | 2015-12-09 | 信丰正天伟电子科技有限公司 | Electrotinplate all plates capability test device |
-
2017
- 2017-09-30 CN CN201710938511.1A patent/CN109596681B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4075065A (en) * | 1975-07-07 | 1978-02-21 | Handy & Harman | Gold plating bath and process |
| JPH03146689A (en) * | 1989-10-31 | 1991-06-21 | Nec Kansai Ltd | Solder and tin plating solution |
| CN102162110A (en) * | 2011-01-31 | 2011-08-24 | 张家港市新港星科技有限公司 | Methyl sulfonate tinning electrolyte and tinning method of steel strip or steel plate |
| CN102866079A (en) * | 2012-09-20 | 2013-01-09 | 信丰正天伟电子科技有限公司 | Testing method of electrotinning uniform plating capacity |
| CN204855503U (en) * | 2015-07-24 | 2015-12-09 | 信丰正天伟电子科技有限公司 | Electrotinplate all plates capability test device |
Non-Patent Citations (1)
| Title |
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| 碱性无氰镀锌工艺研究;高仙芝;《火箭推进》;20131031;第39卷(第5期);第75-81页 * |
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