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Potassium hydrogen peroxymonosulfate solutions

A potassium hydrogen peroxymonosulfate, solution technology, applied in peroxy hydrate/peroxy acid, improvement of metal adhesion of insulating substrates, printed circuit manufacturing, etc. Problems such as increased salt concentration

Active Publication Date: 2006-05-03
EI DU PONT DE NEMOURS & CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Meanwhile, as active oxygen is consumed, KHSO 5 Sulfate formation, resulting in an increased concentration of sulfate formed due to the presence of potassium sulfate in potassium peroxymonosulfate
Therefore, the concentration of copper sulfate in the bath increases, and finally the bath must be replaced, otherwise, the board will be stained and the quality will decrease
Although additional potassium persulfate can be added to replace the reduced active oxygen, the sulfate builds up, limiting the life of the bath

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] OXONE trademark potassium peroxymonosulfate (104 g, 4.52% active oxygen, solids) was slurried with 52 g deionized water (equivalent to 200 g OXONE per 100 g water). The slurry was stirred overnight at room temperature (22°C + / - 2°C), then filtered through a coarse glass filter funnel to remove undissolved potassium sulfate and bisulfate. The clear filtrate was analyzed and characterized as follows:

[0049] % active oxygen 2.98% KHSO 5 28.4

[0050] %KHSO 4 13.5 pH 0.9

[0051] Total Dissolved Solids (TDS), % 49.4

[0052] weight ratio, SO 5 / total SO 4 1.5:1

[0053] KHSO 5 The recovery of the active ingredient was a total of 99.0% in this example. As shown in Table 2, the resulting solutions were stable for many weeks upon storage with only a small loss of active oxygen content relative to conventional complete solutions of the prior art.

[0054] Active oxygen % content remaining after a period of time (based on initial conte...

Embodiment 2-11

[0059] The foregoing examples illustrate the preparation of the high-concentration potassium monopersulfate solution of the present invention in available concentration ranges and wider temperature ranges. The amount of OXONE trademark potassium peroxymonosulfate (4.52% active oxygen, solids) as specified in Table 3 was slurried with 100 grams of deionized water. The slurry was stirred at room temperature (water bath) as described in Table 3. Each slurry was equilibrated at the specified temperature for at least 3 hours but not more than 24 hours. Each slurry was filtered as described in Example 1 to obtain a clear filtrate. The characteristics of the high-concentration solution obtained in this way are shown in Table 3 after analysis.

Embodiment 12

[0075] This example illustrates how the highly concentrated solutions of the present invention can be used to prepare copper microetch baths with lower inert sulfate content and higher copper loading capacity. A high concentration potassium monopersulfate solution was prepared as described in Example 1. Prepare 50 grams of microetching baths by diluting 15.3 g of the high concentration solution with 34.7 g of deionized water to obtain a solution containing 0.91% active oxygen and 4.1% sulfate (such as SO 4 )The solution. The microetching solution was equilibrated to 30°C by stirring. Pre-weighed 2.5 in2 (40.3cm 3 ) copper-covered substrates were placed in the bath and microetched for a total of 40 minutes until copper sulfate was observed to begin to precipitate. At this point, the matrix was removed, rinsed, dried and reweighed. A total of 1.216 g of Cu was removed, implying a copper loading capacity of 24.3 g per 1000 g of starting microetching solution. The average etc...

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PUM

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Abstract

The invention discloses a solution comprising potassium peroxymonosulfate with a high concentration of KHSO5 and a weight ratio of SO5 / SO4 greater than 1.0:1, and its use in microetching metal substrates.

Description

field of invention [0001] The present invention relates to a high-concentration solution of potassium monopersulfate with low inert salt content, its preparation method and its use in the preparation of printed circuit boards and semiconductors. Background of the invention [0002] Trademarks are shown in capital letters herein. [0003] The term "potassium peroxymonosulfate", as it is commonly used in the industry, is used herein to refer to the mixed triple salt 2KHSO 5 ·KHSO 4 ·K 2 SO 4 . Potassium peroxymonosulfate has a theoretical active oxygen content of 5.2%. All references herein to potassium peroxymonosulfate refer to commercially available mixed triple salts typically having an active oxygen content of about 4.7%. It should be understood that commercially available potassium peroxymonosulfate has a purity of about 95% to about 98% due to the presence of minor impurities, minor additives such as anti-caking agents, and variants during processing. [0004] Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B15/08C23F1/18H01L21/321H01L21/3213H05K3/38
CPCC01B15/08C23F1/18H01L21/3212H05K3/383H05K2203/0796H01L21/3213H05K3/38
Inventor T·P·塔法诺M·B·科克西
Owner EI DU PONT DE NEMOURS & CO
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