Phosphor Aerogel Preparation via Integrated Sol-Gel and Supercritical Drying

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Solution Overview

Problem

Current methods for synthesizing phosphor aerogels with controlled particle sizes, monolithic, crack-free, and uniform luminescent properties are challenging due to time-consuming processes, multiple steps, solvent changes, and low probability of forming monolithic gels without cracks, and often involve hazardous or expensive materials.

Innovation Solution

A process involving the synthesis of phosphor aerogels using tetraethylorthosilicate (TEOS), transition metal salts, and rare-earth metals in varying ratios, with supercritical drying and annealing under controlled conditions to produce aerogels with uniform particle sizes, high porosity, and low density, achieving monolithic and crack-free gels with enhanced luminescence.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If conventional aerogel synthesis methods are used, then aerogels can be produced, but the process is enormously time consuming and involves multiple steps with solvent changes

Engineering Contradiction:
Improvesynthesis speedVSAvoidprocess steps
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The patent combines phosphor synthesis and aerogel formation into a single integrated sol-gel process. By using metal alkoxides that serve dual purposes as both phosphor precursors and aerogel building blocks, the method eliminates separate synthesis steps and reduces the overall process complexity while maintaining high productivity

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent modifies the sol-gel process parameters by using metal alkoxides with specific molecular structures and controlling hydrolysis conditions. This enables simultaneous phosphor particle formation and aerogel network development, reducing synthesis time from days to hours while maintaining material quality

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If conventional drying methods are used, then solvent removal is achieved, but cracks form during gel settling time and monolithic gels are difficult to form

Engineering Contradiction:
Improvegel uniformityVSAvoidcrack-free structure
Core Design Contradiction:
Manufacturing precisionVSReliability

Solution Approach 1:

The patent employs supercritical drying where the solvent is brought to supercritical conditions and then decompressed. This phase transition approach eliminates capillary forces that cause cracking during conventional drying, ensuring crack-free monolithic structures with uniform morphology

Inventive Principle:
Principle #36Phase transitions

Solution Approach 2:

The patent performs preliminary gel aging and solvent exchange before final drying. This preliminary action strengthens the gel network structure and replaces the solvent with a drying agent, preventing cracks during the subsequent drying process and ensuring monolithic formation

Inventive Principle:
Principle #10Preliminary action

3Manufacturing precision

If phosphor aerogels are synthesized with controlled particle sizes, then uniform luminescent properties are achieved, but the process becomes challenging and time consuming

Engineering Contradiction:
Improveparticle size controlVSAvoidsynthesis duration
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The patent controls particle size by adjusting sol-gel parameters including metal alkoxide concentration, water-to-alkoxide ratio, and pH. These parameter changes enable precise control over phosphor particle size (5-50 nm) and aerogel pore structure simultaneously, achieving uniform luminescence without excessive time investment

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses metal alkoxides as intermediaries that control both phosphor nucleation and aerogel network formation. The hydrolysis and condensation of metal alkoxides serve as intermediary reactions that synchronize particle size control with aerogel structure development, reducing overall synthesis time

Inventive Principle:
Principle #24Intermediary (Mediator)

4Ease of manufacture

If multiple solvents are used for solvent displacement, then aerogel formation is achieved, but the process involves change of multiple solvents from higher to lower critical conditions

Engineering Contradiction:
Improveaerogel formationVSAvoidsolvent exchange steps
Core Design Contradiction:
Ease of manufactureVSDevice complexity

Solution Approach 1:

The patent extracts the need for multiple solvent exchanges by directly using supercritical CO2 as the drying medium. This approach takes out the intermediate solvent displacement steps and directly achieves aerogel formation through supercritical drying, simplifying the manufacturing process

Inventive Principle:
Principle #2Taking out (Extraction)

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 results in phosphor aerogels with high porosity (>90%), low density (<100 kg/m³), and bright luminescence, suitable for various applications like lighting and display devices, with a high yield (>95%) and cost-effective production without the need for expensive equipment.

Implementation Method 1

the wet gel obtained in step (a) to supercritical drying in an autoclave for 5-6 hours at a temperature ranging from 250° C. to 300° C. at 60-120 bars pressure to obtain a dried aerogel

Methodology Applied
Scientific EffectSupercritical drying: Supercritical Drying

Implementation Method 2

subjecting the dried aerogel as obtained in step (b) to an annealing treatment in a controlled atmosphere of a high temperature furnace at a temperature in the range of 800° C. to 1500° C. for 1-5 hours so as to obtain the desired phosphor aerogel

Methodology Applied
Scientific EffectAnnealing: Annealing

Data Source

PatentUS10633257B2Process for the preparation of uniform sized phosphor aerogel
Publication Date: 2020.04.28 COUNCIL OF SCI & IND RES

AI summary

The present invention provides a process for the preparation of phosphor aerogel of uniform size having high porosity, low density; high thermal insulation and high luminescence, which is useful for various applications like lighting, display, sensing and other applications. More specifically, the present invention provides a simple and versatile process for the formation of monolithic gel, at room temperature, which on further drying at supercritical temperature and pressure result in dry aerogel.