A kind of corrosion inhibitor and its application in copper metal pickling solution and chemical polishing solution

A chemical polishing and corrosion inhibitor technology, which is applied in the field of printed circuits, can solve the problems of high toxicity of nitrogen oxide gas, high cost of benzotriazole, and short service life of polishing agent, and achieves low cost and corrosion inhibition performance. Stable, low toxicity effect

Active Publication Date: 2022-03-15
UNIV OF ELECTRONICS SCI & TECH OF CHINA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are three types of chemical polishing solutions used in production: (1) nitric acid and its salt series, which will produce nitrogen oxides during chemical polishing, commonly known as "yellow smoke". Nitrogen oxide gas is very toxic and harmful to the human body and environment will cause serious harm; (2) chromate series, there is Cr in this polishing method 6+ (3) Hydrogen peroxide series, this method has the problems of unstable hydrogen peroxide, generally short service life of polishing agent, and high production cost
As disclosed in Chinese patent CN 103757636 B, a kind of chemical polishing solution is provided, and the polishing solution includes sulfuric acid, hydrogen peroxide, acetic acid, corrosion inhibitor, auxiliary oxidant, brightener and regulator, and the corrosion inhibitor is diethanolamine oleate, One or more of sodium silicate, imidazole, sodium alkylbenzenesulfonate, triethanolamine, and benzotriazole; it is well known that benzotriazole has problems of high cost, poor biodegradability and toxicity

Method used

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  • A kind of corrosion inhibitor and its application in copper metal pickling solution and chemical polishing solution
  • A kind of corrosion inhibitor and its application in copper metal pickling solution and chemical polishing solution
  • A kind of corrosion inhibitor and its application in copper metal pickling solution and chemical polishing solution

Examples

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Comparison scheme
Effect test

Embodiment 1

[0034] The present embodiment provides a copper metal pickling solution: the acid solution is dilute sulfuric acid: the concentration is 0.5mol / L, the acid solution consumption is 1L, and prothioconazole 10 -4 mol / L, the electrochemical test was carried out after immersing the cleaned and dried red copper in the acid treatment solution for 40 minutes at 25°C.

[0035] The results of electrochemical impedance spectroscopy test show that the corrosion inhibition efficiency is 96.1%, such as figure 1 Shown; Potentiodynamic polarization curve test results show that the corrosion inhibition efficiency is 98.7%, such as figure 2 Shown; The corrosion inhibitor in the acid treatment solution is shown to be an efficient corrosion inhibitor.

Embodiment 2

[0037] This embodiment provides a copper metal pickling solution: the acid solution is dilute sulfuric acid: the concentration is 0.5mol / L, the acid solution consumption is 1L, and 5-mercapto-1-methyltetrazole 10 -5mol / L, the electrochemical test was carried out after immersing the cleaned and dried red copper in the acid treatment solution for 40 minutes at 35°C.

[0038] Electrochemical impedance spectroscopy test results show that the corrosion inhibition efficiency is 83.5%, such as image 3 Shown; Potentiodynamic polarization curve test results show that the corrosion inhibition efficiency is 84.7%, as Figure 4 Shown; The corrosion inhibitor in the acid treatment solution is shown to be an efficient corrosion inhibitor.

Embodiment 3

[0040] This embodiment provides a copper metal pickling solution: the acid solution is dilute sulfuric acid: the concentration is 0.5mol / L, dilute nitric acid: 0.3mol / L, the amount of pickling solution is 2L, and prothioconazole 10 -4 mol / L, 5-mercapto-1-methyltetrazole 10 -4 mol / L, the electrochemical test was carried out after immersing the cleaned and dried red copper electrode in the acid treatment solution for 30 minutes at 45°C.

[0041] The highest corrosion inhibition efficiency obtained by the weight loss test is 91.4%, and the electrochemical impedance spectroscopy test results show that the corrosion inhibition efficiency is 89.9%, such as Figure 5 Shown; Potentiodynamic polarization curve test results show that the corrosion inhibition efficiency is 97.4%, such as Figure 6 Shown; The corrosion inhibitor in the pickling solution is shown to be an efficient corrosion inhibitor.

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Abstract

The invention relates to the field of printed circuits, and relates to pickling technology and chemical polishing technology in printed circuit technology, in particular to a corrosion inhibitor and its application in copper metal pickling solution and chemical polishing solution. The present invention adopts prothioconazole and / or 5-mercapto-1-methyltetrazole as a corrosion inhibitor, 5-mercapto-1-methyltetrazole as a pharmaceutical intermediate, is environmentally friendly, and has low toxicity of prothioconazole , and both corrosion inhibitors have the characteristics of good water solubility and low cost. The corrosion inhibitor of the present invention is applied in copper metal pickling solution, the consumption of corrosion inhibitor is small, the water solubility is good and the corrosion inhibition efficiency is high, can reach 80-99%, and the corrosion inhibition performance is stable; The corrosion inhibitor of the present invention is applied to In the copper metal chemical polishing solution, sulfuric acid is used as the main corrosion system to avoid the NO produced during the polishing process. x , SO 2 and other harmful gases, using the chemical polishing solution of the present invention to chemically polish the metal surface, the chemically polished surface has high brightness and smooth surface, and can achieve the effect of mirror polishing.

Description

technical field [0001] The invention relates to the field of printed circuits, and relates to pickling technology and chemical polishing technology in printed circuit technology, in particular to a corrosion inhibitor and its application in copper metal pickling solution and chemical polishing solution. Background technique [0002] Copper material is one of the most widely used metal materials in non-ferrous metals. It is widely used in the field of electronic technology such as printed circuits, integrated circuit packaging substrates and integrated circuits, and its application range is still expanding. middle. Pickling, electroplating, polishing and other processes are also common processes in electronic circuits and their packaging processes, such as the TSV (Through silicon via) technology in three-dimensional packaging. The TSV process is to make vertical through holes on the wafer, and then stack the wafers or chips with TSV, and realize the interconnection between ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23F11/16C23F11/14C23G1/06C23G1/10C23F3/06
CPCC23F11/16C23F11/149C23G1/068C23G1/065C23G1/103C23F3/06
Inventor 陶志华刘冠廷李元勋苏桦彭睿韩莉坤
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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