H-Form Cation Exchange Resin Purification for Aqueous Hydrogen Peroxide

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Solution Overview

Problem

Conventional methods for purifying aqueous hydrogen peroxide solutions using ion exchange resins suffer from instability and high TOC concentrations due to oxidative degradation and elution issues, leading to variations in purification quality and yield decreases in semiconductor manufacturing processes.

Innovation Solution

A purification method involving sequential treatment with a first H-form strong cation exchange resin, a salt-form strong anion exchange resin, and a second H-form strong cation exchange resin, specifically using H-form strong cation exchange resins with controlled crosslinking and production processes to inhibit TOC elution and achieve high-purity hydrogen peroxide solutions.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If conventional ion exchange resins are used for purification, then purification is achieved, but TOC elution occurs and purification stability deteriorates

Engineering Contradiction:
Improvepurification stabilityVSAvoidTOC elution
Core Design Contradiction:
ReliabilityVSObject-generated harmful factors

Solution Approach 1:

The patent applies parameter changes by controlling the degree of crosslinking of the cation exchange resin within 5-20% and managing the polymerization temperature during resin production. These parameter optimizations reduce TOC elution while maintaining purification effectiveness, directly resolving the contradiction between purification stability and TOC elution.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses a composite ion exchange system combining H-form cation exchange resin with salt-form anion exchange resin in sequential treatment. This composite approach enhances overall purification performance and stability while minimizing TOC elution through the synergistic effects of different resin types.

Inventive Principle:
Principle #40Composite materials

2Reliability

If strong oxidation resistance is required, then purification quality improves, but resin selection becomes more restricted

Engineering Contradiction:
Improveoxidation resistanceVSAvoidresin selection flexibility
Core Design Contradiction:
ReliabilityVSAdaptability or versatility

Solution Approach 1:

The patent optimizes the crosslinking degree parameter of the cation exchange resin to balance oxidation resistance and functional versatility. By controlling crosslinking within 5-20%, the resin achieves sufficient oxidation resistance for hydrogen peroxide treatment while maintaining adequate ion exchange capacity and adaptability.

Inventive Principle:
Principle #35Parameter changes

3Manufacturing precision

If metal concentration is reduced to less than 10 ng/L, then electronic component cleaning performance improves, but purification system complexity increases

Engineering Contradiction:
Improvemetal concentration controlVSAvoidpurification system structure
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent segments the purification process into distinct sequential stages: first H-form cation exchange treatment, then salt-form anion exchange treatment, and finally a second H-form cation exchange treatment. This segmentation achieves ultra-low metal concentrations through progressive removal at each stage while keeping individual treatment units relatively simple.

Inventive Principle:
Principle #1Segmentation

4Manufacturing precision

If TOC concentration in cleaning fluid is reduced to 1 μg/L or less, then semiconductor manufacturing yield improves, but purification difficulty increases

Engineering Contradiction:
ImproveTOC concentration controlVSAvoidpurification process simplicity
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The patent controls the crosslinking degree of the cation exchange resin within 5-20% to optimize TOC adsorption capacity. This parameter optimization enables the resin to achieve ultra-low TOC concentrations (1 μg/L or less) while maintaining reasonable process simplicity and avoiding excessive purification complexity.

Inventive Principle:
Principle #35Parameter changes

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This approach stabilizes the purification of aqueous hydrogen peroxide solutions by reducing TOC elution, ensuring consistent high-purity output with low metal and TOC concentrations, thereby enhancing the reliability and yield of semiconductor manufacturing processes.

Implementation Method 1

passing the aqueous hydrogen peroxide solution through an ion exchange resin column

Methodology Applied
Scientific EffectIon exchange: Ion Exchange

Implementation Method 2

treated, in the following order, with a cation exchange resin and an anion exchange resin

Methodology Applied
Scientific EffectIon exchange: Ion Exchange

Implementation Method 3

The concentrations of organic substances in ultrapure water used for cleaning have been controlled at the total organic carbon (TOC) of 1 μg/L or less

Methodology Applied
Scientific EffectAdsorption: Adsorption

Data Source

PatentUS11524896B2Aqueous hydrogen peroxide purification method and purification system
Publication Date: 2022.12.13 KURITA WATER INDUSTRIES LTD
  • US11524896B2 patent drawing
  • US11524896B2 patent drawing
  • US11524896B2 patent drawing

AI summary

A purification method for an aqueous hydrogen peroxide solution, includes passing the aqueous hydrogen peroxide solution through a first H-form strong cation exchange resin column 1, a salt-form strong anion exchange resin column 2 and a second H-form strong cation exchange resin column 3. An H-form strong cation exchange resin having crosslinking of 6% or less, an H-form strong cation exchange resin having crosslinking of 9% or more, or an H-form strong cation exchange resin produced by steps (a) and (b) is used as an H-form strong cation exchange resin packed in the second H-form strong cation exchange resin column 3: (a) copolymerizing a monovinyl aromatic monomer with a crosslinkable aromatic monomer having a non-polymerizable impurity content of 3% by weight or less therein using a predetermined amount of a specified radical polymerization initiator at a predetermined polymerization temperature to obtain a crosslinked copolymer; and (b) sulfonating the crosslinked copolymer.