Amorphous Silica Production via Iron-Free Vacuum Drying

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Solution Overview

Problem

Conventional methods for producing silica particles result in colorization due to iron contamination, leading to issues with purity and agglomeration, which are critical for applications in semiconductor sealing and LED materials where high purity and colorlessness are required.

Innovation Solution

The production of amorphous silica with a Fe content of 20 ppm or less is achieved through a process involving hydrolytic polycondensation of silicon alkoxide, followed by vacuum drying using a specifically configured heating tube and subsequent firing at 800° C. to 1200° C., which reduces iron contamination and agglomeration.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If a vacuum drying apparatus is used to dry silica particles, then productivity is improved and particles can be dried almost instantaneously without secondary agglomeration, but iron contamination occurs during the drying step causing colorization

Engineering Contradiction:
Improvedrying speedVSAvoidiron contamination
Core Design Contradiction:
ProductivityVSObject-generated harmful factors

Solution Approach 1:

The invention extracts and removes the harmful iron contamination from the system by replacing the iron-containing vacuum drying apparatus with an iron-free drying method, thereby eliminating the source of colorization while maintaining high productivity

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The invention introduces an intermediary substance (iron-free drying agent or modified drying environment) to transfer the drying function without introducing iron contamination, allowing instantaneous drying without contact with iron-containing components

Inventive Principle:
Principle #24Intermediary (Mediator)

2Manufacturing precision

If conventional drying methods are used to avoid iron contamination, then purity is improved, but secondary agglomeration occurs during drying

Engineering Contradiction:
Improveparticle purityVSAvoidparticle dispersion
Core Design Contradiction:
Manufacturing precisionVSStability of the object's composition

Solution Approach 1:

The invention changes the physical parameters of the drying process (temperature, pressure, humidity control) to achieve rapid drying that prevents secondary agglomeration while maintaining particle purity and monodispersity

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention performs preliminary surface treatment or stabilization of silica particles before drying to prevent agglomeration during the drying process, ensuring particles remain dispersed and maintain their individual characteristics

Inventive Principle:
Principle #10Preliminary action

3Manufacturing precision

If silica particles are dried slowly to prevent contamination, then purity is improved, but production time increases and productivity decreases

Engineering Contradiction:
Improveparticle purityVSAvoiddrying time
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The invention rushes through the drying process by implementing rapid drying conditions that complete evaporation quickly, skipping the prolonged drying period that would otherwise be needed to ensure complete moisture removal, thereby achieving both purity and speed

Inventive Principle:
Principle #21Skipping (Rushing through)

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 process produces silica particles with low iron content, low hygroscopicity, and a sharp particle size distribution, suitable for high-purity applications in semiconductor sealing and LED materials, ensuring minimal colorization and improved durability of the final products.

Implementation Method 1

drying a slurry of a hydrolysis-polycondensation product of a silicon alkoxide

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 2

vacuum drying apparatus having a heating tube which is externally heated and retained in reduced pressure

Methodology Applied
Scientific EffectVacuum: Vacuum

Implementation Method 3

firing the obtained dried particles at 800° C. to 1200° C.

Methodology Applied
Scientific EffectHeating: Heating

Data Source

PatentUS10173902B2Amorphous silica and process for producing same
Publication Date: 2019.01.08 NIPPON SHOKUBAI CO LTD
  • US10173902B2 patent drawing

AI summary

Provided are amorphous silica particles for application to industrial fields where there are increasing desires for high purity and colorlessness. The amorphous silica particles are produced through the steps of hydrolysis of an alkoxide, vacuum drying, and firing. The amorphous silica particles have been reduced in coloration and in Fe content, which is causative of coloration of the silica, and can meet the desires. The amorphous silica is characterized by having an Fe content of 20 ppm or less.