Method for monitoring concentration of sodium 3, 3 '-dithiodipropane sulfonate in copper foil plating solution

A plating solution and concentration technology, used in the measurement of color/spectral properties, material analysis by observing the effect on chemical indicators, and analysis by causing chemical reactions to occur in materials, etc. The interference effect of other additives, etc., to ensure reliability and accuracy, improve controllability and stability, and improve the effect of SPS concentration

Pending Publication Date: 2022-07-12
浙江花园新能源股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] However, since the plating solution often contains more than one additive, in addition to SPS, other additives also have an impact on the electrochemical process, which makes it impossible to rule out the interference of other additives through the analysis method of the conventional cyclic voltammetry curve.
The concentration obtained is actually the comprehensive effect of various additives, and it is difficult to accurately reflect the content of a specific additive

Method used

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  • Method for monitoring concentration of sodium 3, 3 '-dithiodipropane sulfonate in copper foil plating solution

Examples

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Effect test

Embodiment 1

[0038] In the copper foil electrolysis process, in a certain period of time, the monitoring method of the present invention is used to monitor the SPS concentration in real time, and the details are as follows:

[0039] (1) Use acetonitrile to dissolve SPS, and configure 5 to 9 SPS standard solutions with calibration concentrations in the concentration range of 0.5~50 ppm. In this example, 9 SPS standard solutions with calibration concentrations are configured, and the calibration concentrations are: 1, 2, 3, 4, 5, 6, 7, 8, 9 ppm. Then mix the standard solution with H 2 PO 4 - -HPO 4 2- The buffer solution and the chromogenic reagent are mixed and reacted to develop color, and then the absorbance test is carried out, and the standard curve of SPS concentration and absorbance is drawn. The developer used in this example is sodium borohydride. 1, 2, 3, 4, 5, 6, 7, 8, and 9 ppm of the SPS standard solution of each calibration concentration of the measured absorbance: 0.066,...

Embodiment 2

[0046] The electrolysis process of another copper foil adopts the following steps to monitor the SPS concentration:

[0047] The chromogenic agent used in steps (1) and (2) is TCEP, and the remaining steps are the same as in Example 1, and the monitoring data of specific steps will not be listed one by one.

[0048] Finally, the monitoring results of the whole electrolytic process of the copper foil in this example show that the SPS concentration is stable in the range of 3.1-3.5 ppm during the production process of the whole copper foil, and the gloss, tensile strength, roughness, etc. The key indicators remained stable, and the fluctuation range was less than 5%, indicating that the above technical methods can indeed achieve effective monitoring and regulation of SPS concentration and ensure the quality stability of copper foil products.

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Abstract

The invention discloses a method for monitoring the SPS concentration of a copper foil plating solution additive. The method comprises the following steps: 1) formulating a standard curve of SPS calibration concentration and absorbance; (2) carrying out solid-phase extraction on SPS in the plating solution, and testing the absorbance of eluent; and 3) preparing an SPS reference solution with known concentration, performing solid-phase extraction on the reference solution, and testing the absorbance to obtain the SPS solid-phase extraction elution ratio. And 4) obtaining the SPS concentration of the plating solution according to the standard curve, the absorbance of the plating solution eluent and the elution ratio. According to the method, the SPS is separated from the plating solution, the absorbance test is realized, the SPS concentration of the plating solution is obtained, and the technical difficulty that direct test cannot be realized due to serious interference of high-concentration copper ions and acid content in the plating solution on spectrophotometric test is overcome. And through selection of the extraction column and the eluent, an effective elution effect is obtained, so that SPS separation and monitoring and regulation of the concentration of the SPS additive are realized, and the controllability and stability of the quality of the copper foil are improved.

Description

technical field [0001] The invention relates to a method for testing additives, in particular to a method for monitoring the concentration of a sodium polydithiodipropane sulfonate additive in an electroplating solution during the preparation of electrolytic copper foil. [0002] technical background [0003] Electrolytic copper foil is an important material for copper clad laminates, printed circuit boards, and lithium-ion batteries. In the rapid development of today's electronic information industry, electrolytic copper foil is known as the "neural network" for signal and power transmission and communication of electronic products. Since 2002, the production value of printed circuit boards in my country has become the third largest in the world. As the substrate material of printed circuit boards, CCL has also become the third largest producer in the world. [0004] In the electrolytic production process of copper foil, except for common copper (divalent copper ions), acid...

Claims

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Application Information

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IPC IPC(8): G01N21/31G01N21/78
CPCG01N21/31G01N21/78Y02E60/10
Inventor 潘建锋刘嘉斌
Owner 浙江花园新能源股份有限公司
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