Metal Oxalate Hydrate Shape Control via Surfactant Mediation

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

Existing methods for synthesizing porous metal oxide particles struggle with controlling the shape and size of particles, particularly when using metal oxalate materials reacted with oxalic acid, which limits uniformity and precision in particle formation.

Innovation Solution

A hydrothermal reaction method involving a mixture of a metal hydrate salt, a surfactant, a saccharide as both a carbon source and shape-controlling agent, and water is used to form a metal oxalate hydrate body with controlled shape, followed by high-temperature calcination to retain carbon and create a metal oxide/carbon composite body with maintained shape and small metal oxide particles.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If metal oxalate materials are synthesized by reacting metal precursors with oxalic acid, then metal oxalate materials can be obtained, but the shape and size of particles cannot be controlled uniformly

Engineering Contradiction:
Improveparticle shape controlVSAvoidsynthesis process complexity
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The patent introduces a polymer surfactant as an intermediary substance that mediates between the metal precursor and oxalic acid during synthesis. The surfactant molecules adsorb onto the forming particle surfaces and direct their growth, enabling uniform shape control (cubes, rods, spheres) while maintaining the simplicity of the chemical reaction method. This resolves the contradiction by adding a controlling intermediary without fundamentally changing the synthesis approach.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent utilizes parameter changes by controlling the type and concentration of polymer surfactant, as well as reaction conditions (temperature, pH, mixing rate), to precisely control particle morphology. By adjusting these parameters, uniform particles with specific shapes and size distributions can be obtained, achieving manufacturing precision while keeping the synthesis process relatively simple through parameter optimization rather than procedural complexity.

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If polymer materials or silica materials are used as templates to form porous metal oxide bodies, then porous structures can be obtained, but the shape of particles cannot be uniformly controlled

Engineering Contradiction:
Improveparticle shape uniformityVSAvoidtemplate removal process
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent extracts and eliminates the complex template removal process by directly synthesizing particles with desired shapes using polymer surfactants as structure-directing agents during formation. The surfactants remain as surface modifiers rather than bulk templates, so no extensive thermal or chemical treatment is needed to remove templates. This achieves uniform particle shape control without the device complexity of template removal procedures.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent applies preliminary action by pre-organizing the polymer surfactant structures before metal oxide formation occurs. The surfactants self-assemble into specific configurations that template the particle shape during synthesis, so the shape control is built-in from the beginning rather than requiring post-synthesis template removal. This preliminary structuring achieves uniform shapes while avoiding complex removal processes.

Inventive Principle:
Principle #10Preliminary action

3Reliability

If high-temperature calcination is performed to decompose metal oxalate, then metal oxide particles are formed, but all carbon is eliminated

Engineering Contradiction:
Improvemetal oxide formationVSAvoidcarbon elimination
Core Design Contradiction:
ReliabilityVSLoss of substance

Solution Approach 1:

The patent applies partial action by performing calcination at controlled temperatures and for controlled durations that are sufficient to decompose the metal oxalate and form metal oxide particles, but not so extreme as to completely eliminate all carbon. This partial calcination achieves reliable metal oxide formation while retaining some carbon, resolving the contradiction between complete decomposition and carbon preservation.

Inventive Principle:
Principle #16Partial or excessive action

Solution Approach 2:

The patent achieves local quality by creating a core-shell structure where the interior retains carbon while the exterior forms metal oxide. The calcination process is controlled to allow oxygen diffusion from the exterior inward, forming metal oxide at the surface while preserving carbon in the core. This local differentiation resolves the contradiction by having different regions with different compositions.

Inventive Principle:
Principle #3Local quality

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 allows for the precise control of metal oxalate hydrate particle shape and size, forming metal oxide/carbon composite bodies with uniformity and retention of carbon, enhancing their applications in catalysts, adsorbents, and electrode materials.

Implementation Method 1

heating the mixture of step 1 to decompose the metal hydrate salt via a hydrothermal reaction, thereby forming a metal oxalate hydrate body having a controlled shape

Methodology Applied
Scientific EffectHydrothermal reaction:

Implementation Method 2

When metal oxalate hydrates are heated to a high temperature of 300° C. or greater, the carbon atoms that formed the crystals in the metal oxalate are eliminated as either carbon monoxide or carbon dioxide

Methodology Applied
Scientific EffectThermal decomposition: Thermolysis

Implementation Method 3

a hydrothermal reaction of a mixture including a metal hydrate salt, a surfactant, a saccharide, and water

Methodology Applied
Scientific EffectSurfactant action: Surfactant

Implementation Method 4

precise control of metal oxalate hydrate particle shape and size

Methodology Applied
Scientific EffectShape control:

Implementation Method 5

carry out a high-temperature calcination of the metal oxalate hydrate body having a certain shape under the air atmosphere or an inert gas atmosphere to retain carbons without eliminating all thereof

Methodology Applied
Scientific EffectCarbon retention:

Data Source

PatentUS10358457B2Metal oxalate hydrate body having a certain shape, preparation method thereof, and metal oxide/carbon composite body prepared from the same
Publication Date: 2019.07.23 KOREA INST OF ENERGY RES
  • US10358457B2 patent drawing
  • US10358457B2 patent drawing
  • US10358457B2 patent drawing

AI summary

The present invention relates to a metal oxalate hydrate body having a certain shape, a preparation method thereof, and a metal oxide/carbon composite body prepared by using the metal oxalate hydrate body. In the present invention, the metal oxalate body, whose shape is diversely controlled, and the metal oxide/carbon composite body therefrom are provided.