In-situ Particle Characterization via Transparent Reactor Wall

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Solution Overview

Problem

Existing methods for characterizing nanoparticles in a liquid medium during synthesis are hindered by the need for sample extraction, which leads to volume loss, disturbance of reaction conditions, and lag in measurement due to the empirical nature of external analysis, and are further complicated by movement artifacts in stirred reactors.

Innovation Solution

A characterization device with a fiber-optic light source and detector, featuring a confinement tube that allows for in-situ analysis through a transparent wall of the reactor, minimizing sample volume and maintaining a sealed environment to compensate for solvent movement, using quasi-elastic or inelastic light scattering for size and molecular composition analysis.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If a sample is extracted from the reactor for external analysis, then particle characterization can be performed, but volume loss and disturbance of reaction conditions occur

Engineering Contradiction:
Improveparticle characterization accuracyVSAvoidreaction medium volume loss
Core Design Contradiction:
Measurement precisionVSLoss of substance

Solution Approach 1:

A transparent wall is introduced as an intermediary between the reactor interior and the external optical measurement system. This allows light to pass through for particle characterization without requiring physical extraction of the reaction medium, thereby eliminating volume loss while maintaining measurement capability

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The mechanical sampling process (extraction, transport, injection) is replaced by an optical measurement system that operates through the transparent wall. This substitution eliminates the need for physical sample extraction while maintaining particle characterization functionality

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

2Measurement precision

If a sample is extracted and transported to an external analysis instrument, then particle characterization is possible, but lag between measured characteristics and actual reactor conditions occurs

Engineering Contradiction:
Improveparticle characterization accuracyVSAvoidmeasurement lag time
Core Design Contradiction:
Measurement precisionVSLoss of time

Solution Approach 1:

The optical measurement system operates continuously through the transparent wall, allowing real-time particle characterization without interruption of the reaction process. This eliminates the time lag inherent in discrete sampling and transport operations

Inventive Principle:
Principle #20Continuity of useful action

Solution Approach 2:

The mechanical sampling and transport system is replaced by a stationary optical measurement system that remains positioned at the reactor wall throughout the reaction, enabling continuous monitoring without time delays

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

3Measurement precision

If multiple DLS probes are implemented to compensate for Doppler contribution from solvent movement, then measurement accuracy in stirred reactors improves, but device complexity and cost increase

Engineering Contradiction:
Improvemeasurement accuracy in stirred reactorsVSAvoidnumber of probes required
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The optical measurement system is extracted from the stirred reaction medium and positioned outside the reactor through the transparent wall. This removes the measurement system from the harmful moving environment, allowing accurate particle characterization without needing multiple probes to compensate for Doppler effects

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The transparent wall serves as an intermediary that isolates the optical measurement system from the stirred reaction medium. This physical separation eliminates the Doppler contribution from solvent movement while maintaining optical access for particle characterization

Inventive Principle:
Principle #24Intermediary (Mediator)

4Measurement precision

If the optical measuring head is placed in direct contact with the liquid sample, then in-situ measurement is achieved, but cleaning requirements and pollution risks increase

Engineering Contradiction:
Improvein-situ measurement capabilityVSAvoidcleaning and maintenance requirements
Core Design Contradiction:
Measurement precisionVSEase of manufacture

Solution Approach 1:

The transparent wall acts as an intermediary barrier between the optical measuring head and the liquid sample. This allows in-situ measurement through the wall while preventing direct contact, thereby eliminating cleaning requirements and pollution risks for the optical components

Inventive Principle:
Principle #24Intermediary (Mediator)

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

Enables reliable, real-time characterization of nanoparticles within the reactor, reducing volume loss and reaction disturbance, while maintaining a sealed optical head and minimizing the need for complex multi-probe setups, thus providing accurate and continuous monitoring of particle size and composition.

Implementation Method 1

Device for characterizing particles dispersed in a liquid medium by light scattering

Methodology Applied
Scientific EffectLight scattering: Scattering

Implementation Method 2

using quasi-elastic or inelastic light scattering for size and molecular composition analysis

Methodology Applied
Scientific EffectQuasi-elastic light scattering:

Implementation Method 3

inelastic scattering for example of Raman type

Methodology Applied
Scientific EffectInelastic scattering:

Implementation Method 4

inelastic scattering for example of Raman type, or else fluorescence, scattering of Raman type and fluorescence being adapted to the analysis of the molecular composition and of the external structure

Methodology Applied
Scientific EffectRaman scattering:

Implementation Method 5

inelastic scattering for example of Raman type, or else fluorescence, scattering of Raman type and fluorescence being adapted to the analysis of the molecular composition and of the external structure

Methodology Applied
Scientific EffectFluorescence: Fluorescence

Implementation Method 6

focusing optics for focusing in the confinement tube of an illuminating light beam coming from the light emission source

Methodology Applied
Scientific EffectOptical focusing: Focusing

Implementation Method 7

collection optics for the collection towards the optical detector of a beam of light backscattered by the particles dispersed in the confinement tube

Methodology Applied
Scientific EffectOptical collection:

Implementation Method 8

fiber-optic detector... The optical detector allows the detection at a given angle of the light backscattered by the particles in solution

Methodology Applied
Scientific EffectPhotodetection: Photoelectric Effect

Data Source

PatentEP3210938B1Device for characterising particles which are dispersed in a liquid medium
Publication Date: 2018.11.14 CORDOUAN TECH
  • EP3210938B1 patent drawingFigure 1
  • EP3210938B1 patent drawingFigure 2A~2C
  • EP3210938B1 patent drawingFigure 3A~3B

AI summary

This description relates to a device for characterizing particles dispersed in a liquid medium (30) comprising a fiber optic light source (200), a fiber optic detector (300), and a measuring probe (100) intended to be hermetically immersed in the liquid medium (30). The measuring probe (100) comprises: a containment tube designed to pass hermetically through at least one wall of the probe and adapted to receive a sample of the liquid medium, and an optical measuring head comprising a focusing optic for focusing a light beam into the containment tube, and a collection optic for collecting a beam of light backscattered by the dispersed particles towards the optical detector (300). The characterization device also includes a processing unit (400) adapted for characterizing the particles from the backscattered light beam.