Continuous Reactor Synthesis of Spherical Battery Precursors

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Solution Overview

Problem

Conventional methods for synthesizing transition metal precursors for battery electrode materials require lengthy maturation times, often resulting in nanometric aggregates rather than the desired micrometric size and homogeneous morphology, which is essential for high-performance electrochemical active materials.

Innovation Solution

A continuous reactor method involving a reaction tube supplied with two solutions, where transition metal sulfates and a hydroxide or carbonate are introduced at controlled flow rates to achieve a residence time of less than 10 seconds and a laminar flow regime, resulting in the precipitation of spherical, micrometric, and homogeneous precursor particles.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Stability of the object's composition

If conventional co-precipitation method is used with lengthy maturation times, then homogeneous composition is achieved, but production time is excessively long

Engineering Contradiction:
Improvehomogeneous compositionVSAvoidproduction time
Core Design Contradiction:
Stability of the object's compositionVSLoss of time

Solution Approach 1:

The patent replaces conventional mechanical stirring and lengthy maturation processes with a microfluidic system that uses controlled laminar flow and diffusion for mixing. The microfluidic reactor channels enable rapid homogeneous mixing through precise flow rate control, eliminating the need for hours-long maturation while maintaining composition uniformity

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

Solution Approach 2:

The patent changes critical process parameters by reducing residence time from hours to seconds, controlling flow rates at milliliter per minute levels, and maintaining specific pH ranges (7-12). These parameter changes enable rapid precipitation with homogeneous composition, resolving the time-composition contradiction

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If conventional synthesis methods are used, then nanometric aggregates are formed, but micrometric size particles are required for high-performance battery materials

Engineering Contradiction:
Improveparticle size controlVSAvoidaggregate size
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The patent changes the particle size outcome by adjusting process parameters including flow rates, residence time, and pH. By controlling these parameters in the microfluidic reactor, the precipitation process forms micrometric aggregates (1-100 micrometers) instead of nanometric particles, achieving the desired size for high-performance battery electrode materials

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses dynamic control of flow rates and residence time in the microfluidic system to control aggregate growth. The continuous flow regime allows real-time adjustment of mixing intensity and reaction time, enabling precise control over final particle size distribution in the micrometric range

Inventive Principle:
Principle #15Dynamics

3Productivity

If short residence time is used in continuous reactor, then production speed increases, but homogeneous micrometric spherical particles must be achieved

Engineering Contradiction:
Improveproduction speedVSAvoidparticle morphology and size uniformity
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent replaces traditional mechanical mixing systems with microfluidic flow-based mixing. The laminar flow regime in microfluidic channels, combined with diffusion and controlled injection, achieves homogeneous mixing in seconds without mechanical agitation, maintaining particle uniformity while enabling continuous high-speed production

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

Solution Approach 2:

The patent uses the microfluidic reactor channel itself as an intermediary mixing zone. The channel geometry and flow dynamics act as a mediator that ensures homogeneous contact between reactants during the brief residence time, enabling rapid production while maintaining precise control over particle morphology and size distribution

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

This method significantly reduces production time while achieving spherical particles of micrometric size and homogeneous composition, essential for high-performance battery electrode materials, with a residence time as short as 10 seconds and laminar flow ensuring efficient mixing and larger aggregate formation.

Implementation Method 1

delivering solutions A and B to the reaction tube of the continuous reactor at a flow rate of dA and dB respectively, resulting in the precipitation of the precursor in the reaction tube

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Implementation Method 2

the length L of the reaction tube and the delivery flow rates dA and dB are configured such that the residence time in the reaction tube is less than or equal to 10 seconds

Methodology Applied
Scientific EffectLaminar flow: Laminar Flow

Data Source

PatentUS20240262710A1Method for synthesising spherical material particles
Publication Date: 2024.08.08 CENT NAT DE LA RECH SCI (C N R S)
  • US20240262710A1 patent drawing
  • US20240262710A1 patent drawing
  • US20240262710A1 patent drawing

AI summary

A method for synthesising spherical material particles carried out in a continuous reactor. An intake tube is supplied with a solution A including at least one transition metal sulfate and the other intake tube being supplied with a solution B comprising hydroxide or a carbonate. The method includes delivering solutions A and B to a reaction tube at a flow rate dA and dB, and recovering the precipitated precursor at the outlet of the reaction tube. The length of the reaction tube and the delivery flow rates dA and dB are configured such that the residence time in the reaction tube is less than or equal to 10 seconds, wherein the pH in the reaction tube is 7 to 12 and wherein the regime in the reaction tube is a laminar regime.