High purity electrolytic sulfonic acid solutions

a technology of sulfonic acid and high purity, applied in the field of high purity sulfonic acid, can solve the problems of poor corrosion resistance of deposited metal, etc., and achieve the effect of effective us

Inactive Publication Date: 2006-12-07
ARKEMA INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0022] It thus would be desirable to have new electrochemical compositions based on high purity sulfonic acids. It would be particularly desirable to have new sulfonic acid compositions that can be effectively used with metals of strong re...

Problems solved by technology

Sulfuric acid is not often used in the electrodeposition of silver or lead-based alloys due to the likelihood of metal precipitation in this acid.
However, even with the improvements in electroplating processes, circumstances may exist that can lead to plating defects due to inadequate coverage in recess areas such as in the vias or trenches or through-holes in electronic devices, poor corrosion resistance of the deposited metal, too high a residual stress leading to cracking in the metal coating or a rough, commercially unacceptable deposit.
These defects can occur as a result of an imbalance of the organic additives intended to obtain the desired metallic coating.
However, combinations of various low-valent sulfur compounds is typically unwanted due to competitive interactions at the surface of the work piece.
If the nickel electrolytes are made using impure sulfonic acids such as those containing reduced or easily reducible sulfur compounds, the likelihood of sulfur incorporation increases signific...

Method used

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  • High purity electrolytic sulfonic acid solutions
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  • High purity electrolytic sulfonic acid solutions

Examples

Experimental program
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Effect test

example 1

[0071] A. Commercially available 70% methanesulfonic acid (MSA) that contains a high concentration of methylmethanethiosulfonate, [MMTS, (CH3SO2SCH3)] was purified by the following procedure: [0072] (1) 250 ml of 70% methanesulfonic acid containing 12 parts-per-million (ppm) was placed into a 500 ml beaker. [0073] (2) 30% hydrogen peroxide solution, 1.125 grams, was added and the MSA was heated to 140 degrees Fahrenheit for three hours. [0074] (3) The methanesulfonic acid solution was cooled to room temperature and analyzed for MMTS.

[0075] The concentration of MMTS after the hydrogen peroxide treatment was non-detectable by gas chromatography methods. After purification the MSA was diluted to 15% by the addition of water.

[0076] B. A sample of 15% methanesulfonic acid (MSA) made according to Example 1A was electrolyted using a pure tin anode, an insoluble iridium oxide-coated titanium cathode. During electrolysis, tin dissolved into the 15% MSA. Trichloromethylmethylsulfone (TCMS) ...

example 2

[0077] A sample of 15% methanesulfonic acid (MSA) made as in Example 1(A) was electrolyted using a pure tin anode, an insoluble iridium oxide-coated titanium cathode.

[0078] During electrolysis, tin dissolved into the 15% MSA. Methylmethanethiosulfonate (MMTS) was incrementally added and the headspace gas above the electrochemical cell was smelled for detectable odor. After about 0.25 ppm of MMTS was added, an odor was noticeable. MMTS was seen to decompose using chromatographic techniques to primarily dimethyldisulfide (DMDS) in the electrolysis cell. Methylmercaptan (CH3SH) and dimethylsulfide (DMS) were also observed after electrolysis, both odorous impurities.

example 3

[0079] A sample of 15% methanesulfonic acid (MSA) made as in Example 1(A) was electrolytesdusing a pure tin anode, an insoluble iridium oxide-coated titanium cathode.

[0080] During electrolysis, tin dissolved into the 15% MSA. Methylmethanethiosulfonate (MMTS) was incrementally added up to 0.85 ppm. An odor was detectable. To this solution was added 1.0 ppm of Tricloromethylsulfone (TCMS). A very pungent odor was observed indicating a synergy between the two impurities in producing the undesirable odor.

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Abstract

Disclosed is a solution for an electrochemical process, the solution containing a sulfonic acid and having a low concentration of sulfur compounds, either low or high valence, that are susceptible to reduction and which is intended for use in electrodeposition, batteries, conductive polymers and descaling processes.

Description

BACKGROUND OF THE INVENTION [0001] 1. Field of the Invention [0002] The present invention relates to high purity sulfonic acids and their use in electrochemical processes, methods for preparing such high purity acids, methods for preparing high purity metal-sulfonate or sulfonic acid solutions, and products formed by using such methods and solutions. [0003] 2. Prior Art[0004] Electrochemical processes may contain acid electrolytes to impart conductivity and thus lower the required voltage, aid in the dissolution of metal (e.g. formation of metal salts) and metal oxides (e.g., descaling), aid in the deposition of metals from aqueous solutions (e.g., electrodeposition), and may be used in the synthesis of conductive polymers to provide proton conduction and in batteries to aid in the dissolution and salvation of metals such as zinc and lead. [0005] There are many acids that may be used in the above applications such as sulfuric, nitric, phosphoric, sulfamic, and hydrochloric acid as w...

Claims

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Application Information

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IPC IPC(8): C25D3/00C25D5/00C07C303/44C07C309/04C25D3/02C25D5/18C25D21/16C25F1/04H01M10/08H01M10/26
CPCC07C303/44C25D3/02C25D5/18C25F1/02C25F1/04H01M10/08H01M10/26Y02E60/126H01M12/085H01M2300/0005H01M2300/0011Y02E60/124C07C309/04Y02E60/10C25D5/627C25D21/18C25B1/02
Inventor MARTYAK, NICHOLAS MICHAELNOSOWITZ, MARTINSMITH, GARY S.JANNEY, PATRICK KENDALLOLLIVIER, JEAN-MARIE
Owner ARKEMA INC
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