Sol-Gel Oxide Film Nanoparticle Dispersion Control

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Solution Overview

Problem

Current methods for producing metallic-nanoparticle inorganic composites face challenges such as high production costs with electron beam lithography, difficulty in achieving even distribution and size reduction of nanoparticles in chemical synthesis, and poor crystallinity and aggregation issues in co-sputtering techniques.

Innovation Solution

A chemical synthesis method involving sol-gel oxide film formation, tin deposition, excess Sn2+ ion removal, metallic-nanoparticle deposition, and excess metal ion removal steps to create a composite with fine metallic nanoparticles evenly dispersed in a transparent oxide matrix, using a process that includes hydrolyzing metal alkoxide with an acid catalyst and using tin chloride and metal chelates to achieve nanoparticles of 20 nm or smaller.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If electron beam lithography is used to produce metallic-nanoparticle structures, then manufacturing precision and structure control are improved, but production cost and device complexity increase significantly

Engineering Contradiction:
Improvenanoparticle structure controlVSAvoidproduction cost
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The patent replaces the mechanical electron beam lithography system with a chemical synthesis system using sol-gel method and chemical reduction. The mechanical precision of electron beam writing is substituted by chemical self-assembly and controlled reduction reactions, achieving comparable nanoparticle uniformity through chemical pathways rather than physical writing processes.

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

Solution Approach 2:

The patent changes the fundamental parameters of the production method from physical (electron beam energy, writing speed) to chemical (pH, reducing agent concentration, temperature). By controlling chemical parameters such as pH adjustment during reduction and metal salt concentration, the patent achieves precise nanoparticle size and distribution control without the high cost of electron beam equipment.

Inventive Principle:
Principle #35Parameter changes

2Ease of manufacture

If chemical synthesis methods are used to produce metallic nanoparticles, then production cost decreases, but nanoparticle distribution evenness and size control worsen

Engineering Contradiction:
Improveproduction costVSAvoidnanoparticle size control
Core Design Contradiction:
Ease of manufactureVSManufacturing precision

Solution Approach 1:

The patent performs preliminary actions by first forming a sol-gel oxide matrix structure before introducing metal ions, then selectively reducing them. The oxide matrix is prepared in advance with controlled porosity and surface properties, which then guides the uniform distribution and size control of subsequent nanoparticle formation through the reduction process.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent introduces an intermediary oxide matrix (formed by sol-gel from metal alkoxides) that mediates between the metal salt precursor and the final metallic nanoparticle. This intermediary structure provides a controlled environment for nanoparticle formation, ensuring uniform size and distribution while maintaining low production costs through chemical synthesis.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Quantity of substance

If co-sputtering is used to incorporate gold nanoparticles into SiO2 film, then nanoparticle density increases, but heat treatment causes aggregation and poor crystallinity

Engineering Contradiction:
Improvenanoparticle densityVSAvoidparticle diameter uniformity
Core Design Contradiction:
Quantity of substanceVSManufacturing precision

Solution Approach 1:

The patent inverts the conventional sequence by first forming the oxide matrix through sol-gel method, then introducing and reducing metal ions within the already-formed matrix. This reverse approach allows nanoparticles to form in-situ within the oxide structure, preventing aggregation that occurs when heat treatment is applied to pre-formed nanoparticle composites in co-sputtering methods.

Inventive Principle:
Principle #13The other way round (Inversion)

Solution Approach 2:

The patent utilizes phase transitions in the sol-gel process, where metal alkoxides transition through hydrolysis and condensation to form the oxide matrix, followed by chemical reduction of metal ions to metallic nanoparticles. These controlled phase transitions occur at lower temperatures than co-sputtering heat treatment, preventing nanoparticle aggregation while achieving high density and uniform size distribution.

Inventive Principle:
Principle #36Phase transitions

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

The method produces a metallic-nanoparticle inorganic composite with nanoparticles of 20 nm or smaller, evenly distributed and high density, enabling clear plasmon absorption and potential use in optical devices like plasmon waveguides and nonlinear optical materials.

Implementation Method 1

an oxide film having micropores is formed on a substrate by a sol-gel method in which a metal alkoxide is partly hydrolyzed by the action of an acid catalyst

Methodology Applied
Scientific EffectHydrolysis: Hydrolysis

Implementation Method 2

a tin deposition step in which the oxide film is brought into contact with an acidic aqueous solution of tin chloride

Methodology Applied
Scientific EffectAdsorption: Adsorption

Implementation Method 3

a metallic-nanoparticle deposition step in which the oxide film is brought into contact with an aqueous solution of a metal chelate to deposit metallic nanoparticles in the micropores

Methodology Applied
Scientific EffectRedox Reactions: Redox Reactions

Data Source

PatentUS7972539B2Process for producing metallic-nanoparticle inorganic composite and metallic-nanoparticle inorganic composite
Publication Date: 2011.07.05 KK TOSHIBA
  • US7972539B2 patent drawing
  • US7972539B2 patent drawing
  • US7972539B2 patent drawing

AI summary

A process for producing a metallic-nanoparticle inorganic composite 10 includes an oxide film formation step in which an oxide film 14 having micropores is formed on a substrate by a sol-gel method in which a metal alkoxide is partly hydrolyzed by the action of an acid catalyst, a tin deposition step in which the oxide film 14 is brought into contact with an acidic aqueous solution of tin chloride, an excess Sn2+ ion removal step in which Sn2+ ions are removed from the micropores, a metallic-nanoparticle deposition step in which the oxide film 14 is brought into contact with an aqueous solution of a metal chelate to deposit metallic nanoparticles 12 in the micropores, and an excess metal ion removal step in which metal ions are removed from the micropores; and a metallic-nanoparticle inorganic composite 10 is produced by this process.