Moisture Measurement in Battery Separators Using Gas Chromatography

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Solution Overview

Problem

Conventional methods, such as Karl-Fisher titration, fail to accurately measure moisture content in secondary battery separators, particularly when inorganic substances are present in the form of hydrates, affecting battery performance and lifespan.

Innovation Solution

A method utilizing a gas chromatograph equipped with a headspace sampler, where an internal standard solution is prepared with tetrahydrofuran and dimethylformamide, and the samples are analyzed at temperatures between 140°C and 160°C using a thermal conductivity detector, allowing for accurate measurement of moisture content in both free and hydrate forms.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If Karl-Fisher titration method is used to measure moisture content in separator, then the measurement process is simple and commonly available, but the measured value is not accurate especially when inorganic substances are present

Engineering Contradiction:
Improvemoisture content measurement accuracyVSAvoidmeasurement device complexity
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The patent replaces the chemical titration system (Karl-Fisher method) with a physical analysis system (gas chromatography). The GC system uses thermal conductivity detection to measure moisture content, avoiding the chemical reactions and assumptions that limit the accuracy of Karl-Fisher titration, especially in the presence of inorganic substances.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

The patent changes the measurement parameter from chemical equivalence (Karl-Fisher reagent consumption) to physical property detection (thermal conductivity of gas phase moisture). This parameter change enables accurate measurement of moisture in complex matrices containing inorganic substances without the interference that plagues chemical titration methods.

Inventive Principle:
Principle #35Parameter changes

2Measurement precision

If headspace sampling method is used with gas chromatograph, then moisture content measurement accuracy is improved, but the measurement process becomes more complex

Engineering Contradiction:
Improvemoisture content measurement accuracyVSAvoidmeasurement operation simplicity
Core Design Contradiction:
Measurement precisionVSEase of operation

Solution Approach 1:

The patent introduces a headspace sampler as an intermediary device between the sample and the gas chromatograph. This automated intermediary handles the complex tasks of sample preparation, heating, and gas phase extraction, transforming a complex manual process into an automated sequence that improves accuracy while reducing operational complexity.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The headspace sampling method performs preliminary actions of sample heating and moisture extraction into the gas phase before the actual GC analysis. This preliminary preparation separates the complex sample matrix from the moisture analyte, simplifying the subsequent measurement process and improving accuracy by eliminating interference from inorganic substances.

Inventive Principle:
Principle #10Preliminary action

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 method provides more accurate moisture content measurements in secondary battery separators, improving battery performance and lifespan by identifying internal states and moisture sources effectively.

Implementation Method 1

measuring a moisture content in the standard sample and a moisture content in the test sample with a gas chromatograph equipped with a headspace sampler

Methodology Applied
Scientific EffectThermal conductivity detection:

Implementation Method 2

temperature of the vessel is from 140 to 160° C.

Methodology Applied
Scientific EffectHeating: Heating

Implementation Method 3

mixing the solvent with water and then introducing the internal standard solution hereto to prepare a standard sample

Methodology Applied
Scientific EffectPhase change: Phase Change

Data Source

PatentUS11480552B2Method for measuring content of moisture in secondary battery separator
Publication Date: 2022.10.25 LG ENERGY SOLUTION LTD
  • US11480552B2 patent drawing
  • US11480552B2 patent drawing

AI summary

The present invention provides a method for measuring moisture content in a separator of secondary battery by using a gas chromatograph equipped with a headspace sampler. The separator of secondary battery may be a safety reinforced separator (SRS) in which inorganic substance particles and a binder polymer are coated on a polyolefin substrate.