Zeolite Fine Particle Dispersion via Silane Maturation
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Solution Overview
Problem
Conventional methods for producing zeolite fine particles with uniform particle sizes of 100 nm or less for semiconductor applications face challenges in stability, aggregation, and filtration, leading to contamination and reduced mechanical strength of porous dielectric films.
Innovation Solution
A process involving the formation of zeolite seed crystals followed by the addition of an organic-group-containing hydrolyzable silane compound and a maturing reaction under elevated temperature and pressure conditions, which stabilizes the particles and prevents aggregation, allowing for filtration through filters with pore sizes of 0.2 μm or less without physical separation.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Manufacturing precision
If conventional hydrothermal synthesis is used to produce zeolite fine particles, then zeolite crystals can be formed, but the particle size becomes 100 nm or greater with poor uniformity, making it difficult to prevent mixing of large particles
Solution Approach 1:
The synthesis process is divided into two distinct stages: a first hydrothermal synthesis step that produces zeolite seed crystals with controlled small size (100 nm or less), followed by a second growth step that develops the final crystal structure. This segmentation allows precise control of particle size distribution while maintaining productivity, as the seed crystals serve as uniform nuclei for subsequent growth.
Solution Approach 2:
Zeolite seed crystals are prepared in advance through the first hydrothermal synthesis step before the main crystal growth process. These pre-formed seeds with uniform small size (100 nm or less) provide a controlled starting point that prevents formation of excessively large particles during subsequent synthesis, ensuring particle size uniformity in the final product.
2Manufacturing precision
If zeolite fine particles with particle size of 100 nm or less are produced, then uniform particle size is achieved, but the particles aggregate and show reduced stability
Solution Approach 1:
An organic group-containing hydrolyzable silane compound is introduced as an intermediary substance that adsorbs onto the surface of zeolite fine particles. This intermediary layer prevents direct interaction between particles, thereby suppressing aggregation while maintaining the small uniform particle size (100 nm or less) achieved through the two-stage synthesis process.
Solution Approach 2:
The surface properties of zeolite particles are modified by changing the chemical parameters through introduction of organic groups via hydrolyzable silane compounds. This parameter change in surface chemistry provides steric and electrostatic stabilization, preventing aggregation of the fine particles while preserving their small size and uniform distribution.
3Reliability
If porous dielectric films are made from fine zeolite particles, then low dielectric constant is achieved, but mechanical strength is reduced
Solution Approach 1:
The porous dielectric film is constructed as a composite material system where fine zeolite particles (providing low dielectric constant) are combined with an organic group-containing hydrolyzable silane compound (providing mechanical reinforcement). The silane compound forms a network structure that binds the zeolite particles together, creating a composite that simultaneously achieves low dielectric constant and adequate mechanical strength.
4Manufacturing precision
If physical separation methods are used to remove large particles, then particle size uniformity is improved, but the process becomes complex and filtration is difficult
Solution Approach 1:
The potential harm of particle aggregation and large particle formation is converted into a benefit by using the organic group-containing hydrolyzable silane compound to selectively stabilize small particles (100 nm or less). This chemical stabilization mechanism naturally prevents formation of filter-clogging large aggregates, allowing straightforward filtration through 0.2 μm pore size filters without complex physical separation equipment.
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 process achieves zeolite fine particles with uniform sizes, improved stability, and enhanced filtration capabilities, resulting in high-quality, low-dielectric-constant dielectric films with increased mechanical strength for semiconductor devices.
Implementation Method 1
zeolite crystals grow in equilibrium of aggregation and crystallization of a silicon oxide unit using a structure directing agent as a nucleus and re-dissolution
Implementation Method 2
aggregation and crystallization of a silicon oxide unit using a structure directing agent as a nucleus
Implementation Method 3
maturing reaction under elevated temperature and pressure conditions, which stabilizes the particles and prevents aggregation
Implementation Method 4
addition of an organic-group-containing hydrolyzable silane compound and a maturing reaction
Data Source
AI summary
The invention provides a preparation process of organic-group-modified zeolite fine particles excellent in stability of particle size and to be used for electronic materials or the like. The preparation process comprises a first step of obtaining a liquid containing zeolite seed crystals having a particle size of 80 nm or less which are formed in the presence of a structure directing agent, a second step of adding an organic-group-containing hydrolyzable silane compound to the liquid obtained by the first step, and a third step of maturing the liquid of the second step at temperature higher than that of the first step. A dispersion liquid of zeolite fine particles obtained by the process.