Metal Oxide Synthesis from Acidic Solutions

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Solution Overview

Problem

The production of metal oxides, particularly transition metal oxides, is hindered by rapid or uncontrollable hydrolysis and polycondensation in aqueous solutions, leading to premature precipitation and non-uniform gel formation, which complicates the control of chemical composition and structural properties.

Innovation Solution

The method involves forming metal oxides from acidic solutions containing a metal and a strong acid, with a metal-stabilizing agent that decomposes at low temperatures, allowing for the formation of semi-liquid or solid materials without significant pH increase, incorporating oxyanions or polyoxyanions, and optionally adding chemicals to control structural and chemical properties.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional sol-gel processes are used to produce metal oxides, then gel formation can be achieved, but rapid or uncontrollable hydrolysis and polycondensation occur leading to premature precipitation and non-uniform gel formation

Engineering Contradiction:
Improvecontrol of chemical compositionVSAvoiduniformity of gel formation
Core Design Contradiction:
Manufacturing precisionVSStability of the object's composition

Solution Approach 1:

The patent applies preliminary action by adding a metal-stabilizing agent to the precursor solution before hydrolysis occurs. This agent prevents premature precipitation and controls the hydrolysis-polycondensation process, ensuring uniform gel formation throughout the solution. The stabilizing agent is removed later through decomposition or filtration, having served its protective function during the critical gel formation stage.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The metal-stabilizing agent acts as an intermediary substance that mediates between the metal ions and water during the sol-gel process. It temporarily complexes with metal ions to prevent uncontrolled hydrolysis, allowing gradual and uniform gel formation. The intermediary is then removed through decomposition at elevated temperatures or by filtration, leaving the desired metal oxide product.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Stability of the object's composition

If organic chelators are used to inhibit premature precipitation, then gel formation can be controlled, but the process becomes more complex and requires additional chemicals

Engineering Contradiction:
Improvecontrol of precipitationVSAvoidprocess complexity
Core Design Contradiction:
Stability of the object's compositionVSDevice complexity

Solution Approach 1:

The patent changes the chemical parameters of the system by using inorganic competing ions (such as fluoride, chloride, or sulfate ions) instead of organic chelators. These inorganic ions compete with the metal ions for coordination, slowing down the hydrolysis-polycondensation rate in a controllable manner. This parameter change simplifies the process by eliminating the need for organic chelating agents and their subsequent removal steps.

Inventive Principle:
Principle #35Parameter changes

3Manufacturing precision

If pH is increased to control gel formation, then hydrolysis and polycondensation can be managed, but significant pH increase leads to unwanted side reactions and complicates the process

Engineering Contradiction:
Improvecontrol of hydrolysisVSAvoidprocess simplicity
Core Design Contradiction:
Manufacturing precisionVSEase of operation

Solution Approach 1:

The patent uses inorganic competing ions as intermediaries to control the hydrolysis process without requiring significant pH adjustment. These ions compete with hydroxyl groups for coordination with metal ions, effectively slowing down hydrolysis and polycondensation rates. This intermediary approach maintains process simplicity by avoiding the need for complex pH control mechanisms and associated side reactions.

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 approach enables the production of metal oxides with controlled composition and structure, such as NaSICON-type frameworks, suitable for applications in batteries, catalysts, and ion conductors, while maintaining a stable pH and preventing premature precipitation.

Implementation Method 1

a metal-stabilizing agent that decomposes at low temperatures

Methodology Applied
Scientific EffectDecomposition: Decomposition (biological)

Implementation Method 2

Hydrolysis, condensation and complexation reactions of cations in aqueous solution are the phenomena involved in the formation of the solid by precipitation

Methodology Applied
Scientific EffectHydrolysis: Hydrolysis

Data Source

PatentUS10170759B2Metal oxides from acidic solutions
Publication Date: 2019.01.01 THE ARIZONA BOARD OF REGENTS ON BEHALF OF THE UNIV OF ARIZONA
  • US10170759B2 patent drawing
  • US10170759B2 patent drawing
  • US10170759B2 patent drawing

AI summary

Forming a metal oxide by treating an acidic solution containing a metal to yield a precursor in the form of a semi-liquid, semi-solid or solid, and treating the precursor to yield a product including the metal oxide. An organic or inorganic component may be combined with the precursor to yield a second semi-liquid, semi-solid or solid. The product may be treated to yield a new material. In some cases, the metal oxide has an empirical formula HxM2A1y-A2z, where M represents a transition metal or any combination of transition metals in Groups 3-12; A1 is a first oxyanion; A2 is a second oxyanion; 0≤x≤3; 0≤y≤3; 0≤z≤3; and y+z>0.