Metal Oxide Solid Solution via Supercritical Water Synthesis

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Solution Overview

Problem

Current methods for preparing metal oxide solid solutions in nano size face challenges such as long reaction times, high energy consumption, and post-process treatment of by-products, while also struggling to maintain high specific surface area and thermal resistance, especially when exposed to high temperatures.

Innovation Solution

A method involving the continuous reaction of a reactant mixture containing water and at least two water-soluble metal compounds under subcritical or supercritical conditions, between 200 to 700°C and 180 to 550 bar, without sintering, to produce metal oxide solid solutions with controlled crystallite size and high specific surface area.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If conventional methods (firing, mechanochemical synthesis, hydrothermal synthesis) are used to prepare metal oxide solid solutions, then metal oxide solid solutions can be produced, but the reaction time is long and energy consumption is high

Engineering Contradiction:
Improveproduction efficiencyVSAvoidreaction time
Core Design Contradiction:
ProductivityVSLoss of time

Solution Approach 1:

The invention utilizes the phase transition of water from liquid to supercritical state (above 374°C and 22.1 MPa) to enable rapid chemical reactions. The supercritical water environment allows metal salts to dissolve and react instantly, forming metal oxide solid solutions in seconds without prolonged heating or mechanical processing, thereby dramatically reducing reaction time and energy consumption.

Inventive Principle:
Principle #36Phase transitions

2Temperature

If metal oxide solid solutions are exposed to high temperature, then thermal resistance is improved, but crystallite size increases and specific surface area decreases

Engineering Contradiction:
Improvethermal resistanceVSAvoidspecific surface area
Core Design Contradiction:
TemperatureVSArea of stationary object

Solution Approach 1:

The invention changes the physical-chemical parameters of the reaction medium to supercritical state, enabling metal oxide solid solutions to be formed with controlled crystallite sizes (1-100 nm) directly in the supercritical water environment. This parameter change allows the material to maintain high specific surface area even after thermal treatment, as the supercritical formation process creates a stable nanostructure that resists sintering.

Inventive Principle:
Principle #35Parameter changes

3Ease of manufacture

If metal oxide solid solutions are prepared by conventional methods, then metal oxide solid solutions can be produced, but impurities are incorporated into the products

Engineering Contradiction:
Improvesimplicity of processVSAvoidpurity of product
Core Design Contradiction:
Ease of manufactureVSManufacturing precision

Solution Approach 1:

The invention uses supercritical water as an inert reaction medium that eliminates contamination from furnace atmospheres, mechanical milling media, and hydrothermal synthesis additives. The supercritical water environment is chemically inert toward the metal salts, allowing pure metal oxide solid solutions to form without incorporating impurities from the reaction environment, while maintaining process simplicity through direct injection of metal salt solutions into the supercritical water reactor.

Inventive Principle:
Principle #39Inert atmosphere (Inert environment)

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 metal oxide solid solutions with superior UV light shielding effects, reduced catalytic activity, and maintained specific surface area even at high temperatures, suitable for applications in UV light shielding and oxygen storage.

Implementation Method 1

reacting a reactant mixture containing water and at least two water-soluble metal compounds at 200 to 700°C under a pressure of 180 to 550 bar in a continuous manner

Methodology Applied
Scientific EffectSubcritical or supercritical water reaction: Supercritical Fluid

Data Source

PatentUS7700059B2Metal oxide solid solution and use as oxygen storage composition and UV light shielding agent
Publication Date: 2010.04.20 HANWHA CHEMICAL CORPORATION
  • US7700059B2 patent drawing

AI summary

Disclosed is a method for preparing a metal oxide solid solution in nano size. The metal oxide solid solution is prepared by reacting a reactant mixture containing water and at least two water-soluble metal compounds at 200 to 700° C. under a pressure of 180 to 550 bar in a continuous manner, wherein the reactant mixture contains the metal compounds at an amount of 0.01 to 30% by weight in total and the solid solution has a crystallite size of 1 to 1,000 nm. The metal oxide solid solution is, in particular suitable as a UV light shielding agent or as an oxygen storage component.