Cobalt Ferrite Particle Synthesis With Citrate Size Control

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Solution Overview

Problem

Conventional methods for producing cobalt ferrite particles either result in nanometer-sized particles at low temperatures with wide size distribution or require high-energy hydrothermal processes to achieve larger particles, posing challenges in energy efficiency and facility costs.

Innovation Solution

A method involving the formation of a ferrite precursor from ferrous and cobalt salts, treated under high-temperature and high-pressure conditions with a complexing agent, allowing for the production of cobalt ferrite particles with larger diameters and narrow size distribution, using a hydrothermal method at lower temperatures (130°C to 190°C) and adjusting particle sizes through additives and pH control.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Temperature

If the co-precipitation method or wet oxidation method is used, then ferrite particles can be produced at relatively low temperatures, but only nanometer-order fine particles are obtained with wide size distribution

Engineering Contradiction:
Improveproduction temperatureVSAvoidparticle size distribution
Core Design Contradiction:
TemperatureVSManufacturing precision

Solution Approach 1:

The patent changes the chemical parameters by introducing a complexing agent (citrate) that forms stable complexes with metal ions, and adjusts the pH to 7-9 to control the precipitation process. This enables production of particles with 0.5-5 µm diameter and narrow size distribution at lower temperatures without requiring high-energy hydrothermal conditions

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If the hydrothermal method is used, then relatively large micrometer-order particles can be obtained, but high temperature and high pressure conditions are required which increase facility costs and energy consumption

Engineering Contradiction:
Improveparticle size controlVSAvoidenergy consumption
Core Design Contradiction:
Manufacturing precisionVSUse of energy by stationary object

Solution Approach 1:

The patent introduces a complexing agent (citrate) as an intermediary that mediates the precipitation process. The citrate forms complexes with Fe2+, Fe3+, and Co2+ ions, controlling their precipitation sequence and enabling particle growth to 0.5-5 µm at moderate temperatures (pH 7-9) without requiring high-pressure hydrothermal conditions, thus reducing energy consumption while maintaining particle size control

Inventive Principle:
Principle #24Intermediary (Mediator)

3Productivity

If conventional methods are used to produce cobalt ferrite particles, then particles can be formed, but they exhibit wide particle size distribution which limits application performance

Engineering Contradiction:
Improveproduction efficiencyVSAvoidparticle size uniformity
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent performs preliminary action by adjusting the pH to 7-9 before precipitation occurs and by pre-forming complexes with citrate. This preliminary pH adjustment and complex formation control the nucleation and growth processes, ensuring that particles grow uniformly to 0.5-5 µm with narrow size distribution, improving both productivity and particle size uniformity

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 enables the production of cobalt ferrite particles with average diameters of 5 to 50 µm and narrow size distribution, suitable for applications in copier toners, magnetic inks, and MR fluids, while reducing energy consumption and facility requirements.

Implementation Method 1

the ferrite precursor is thermally treated under a high-temperature and high-pressure condition in the presence of a complexing agent

Methodology Applied
Scientific EffectHydrothermal reaction:

Implementation Method 2

there is a need to perform a hydrothermal reaction (Schikorr reaction) at a high temperature and a high pressure

Methodology Applied
Scientific EffectSchikorr reaction:

Implementation Method 3

an alkali and a complexing agent are introduced into an aqueous solution including Fe3+

Methodology Applied
Scientific EffectComplexation:

Implementation Method 4

a solution of ferrous ions, cobalt ions and sodium citrate as complexing agent

Methodology Applied
Scientific EffectChelation:

Data Source

PatentEP3978443B1Cobalt ferrite particle production method and cobalt ferrite particles produced thereby
Publication Date: 2024.06.26 NITTETABU MINING CORP
  • EP3978443B1 patent drawingFigure 1~2
  • EP3978443B1 patent drawingFigure 3~4
  • EP3978443B1 patent drawingFigure 5

AI summary

Provided are cobalt ferrite particles having a micrometer-order average particle diameter and similar particle diameters. When a cobalt ferrite precursor is treated at a high temperature and a high pressure, an oxidation reaction is caused in the presence of a complexing agent, thereby obtaining intended cobalt ferrite magnetic particles.