Flame Spray Synthesis of Monoclinic Lu2O3 Nanoparticles

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Solution Overview

Problem

Existing methods for producing lutetium oxide powders result in large particle sizes and agglomeration, leading to low mechanical strength and optical transparency issues in ceramics, particularly in high-energy laser applications where high thermal shock resistance and minimal scattering are required.

Innovation Solution

The method involves dispersing a lutetium salt solution in a stream of oxygen gas to form droplets, which are then combusted at a sufficient temperature to produce monoclinic lutetium oxide nanoparticles with controlled grain size and phase, using flame spray pyrolysis to achieve uniform nano-sized powders suitable for hot pressing and sintering at lower temperatures and pressures.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional methods (co-precipitation, oxalate precipitation, molten salts) are used to synthesize Lu2O3 powders, then the synthesis can be achieved, but the resulting powders have large particle sizes and agglomeration

Engineering Contradiction:
Improveparticle size controlVSAvoidpowder quality (agglomeration)
Core Design Contradiction:
Manufacturing precisionVSDifficulty of detecting and measuring

Solution Approach 1:

The invention changes the synthesis parameters by using flame spray pyrolysis instead of conventional wet chemistry methods. This involves changing the physical state of the reaction (from liquid-phase precipitation to gas-phase combustion), controlling oxygen flow rate and fuel composition to achieve rapid nucleation and growth of fine particles, and quenching the particles in the flame to prevent agglomeration. These parameter changes result in narrow particle size distribution and minimal agglomeration.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention utilizes phase transitions in the flame spray process: the precursor solution is sprayed as liquid droplets, which evaporate to form aerosol, then undergo combustion to form solid oxide particles, and are finally quenched to freeze the particle size. This sequence of phase transitions (liquid→aerosol→solid→quenched particles) enables precise control over particle size and morphology, producing fine, non-agglomerated powders.

Inventive Principle:
Principle #36Phase transitions

2Ease of manufacture

If larger grained materials are used in ceramics, then the material can be easier to process, but the mechanical strength and thermal shock resistance decrease

Engineering Contradiction:
Improveprocessing easeVSAvoidmechanical strength and thermal shock resistance
Core Design Contradiction:
Ease of manufactureVSStrength

Solution Approach 1:

The invention performs preliminary action by synthesizing ultra-fine nanoparticles with controlled size distribution before ceramic processing. These pre-synthesized fine particles serve as the starting material for ceramic fabrication, enabling the final ceramic to achieve fine grain structure after sintering. This preliminary preparation of fine particles ensures both ease of processing (due to high reactivity and surface area) and high mechanical strength (due to fine final grain size).

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The invention applies segmentation by producing monodisperse nanoparticles with uniform size distribution through controlled nucleation in the flame. This segmentation of the material into uniformly fine particles prevents agglomeration and ensures consistent grain size in the final ceramic, leading to improved mechanical properties and thermal shock resistance while maintaining processability.

Inventive Principle:
Principle #1Segmentation

3Productivity

If conventional synthesis methods are used, then the process can be completed, but the process is complicated and time consuming

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

Solution Approach 1:

The invention replaces mechanical and chemical processing steps with a thermal field-based flame spray process. Instead of multiple steps involving filtration, washing, drying, and calcination required in conventional methods, the flame spray process uses combustion and rapid quenching to directly produce the final oxide particles in a single step. This substitution dramatically reduces process complexity and time while maintaining high productivity.

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

Solution Approach 2:

The invention implements continuous synthesis where the flame spray process operates continuously, with precursor solution continuously sprayed and particles continuously formed and collected. This eliminates the batch-to-batch processing and intermediate steps required in conventional methods, achieving both high productivity and simplified continuous operation without complex batch processing equipment.

Inventive Principle:
Principle #20Continuity of useful action

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 approach yields high-purity, nano-sized lutetium oxide powders with narrow size distribution and low agglomeration, enabling the production of transparent ceramics with smaller grain sizes and enhanced mechanical strength, suitable for solid-state laser materials and other optical applications.

Implementation Method 1

combusting the droplets to form nanoparticles comprising lutetium oxide. The combustion occurs at a temperature sufficient to form monoclinic lutetium oxide in the nanoparticles

Methodology Applied
Scientific EffectCombustion: Combustion

Implementation Method 2

Flame spray pyrolysis (FSP) techniques are gas phase processes that are very effective in producing high purity oxide nanoparticles

Methodology Applied
Scientific EffectPyrolysis: Pyrolysis

Data Source

PatentUS11130675B2Flame spray synthesis of nanoparticles of monoclinic Lu203 and dopant
Publication Date: 2021.09.28 THE UNITED STATES OF AMERICA AS REPRESENTED BY THE SECRETARY OF THE NAVY
  • US11130675B2 patent drawing
  • US11130675B2 patent drawing
  • US11130675B2 patent drawing

AI summary

A nanoparticle containing monoclinic lutetium oxide. A method of: dispersing a lutetium salt solution in a stream of oxygen gas to form droplets, and combusting the droplets to form nanoparticles containing lutetium oxide. The combustion occurs at a temperature sufficient to form monoclinic lutetium oxide in the nanoparticles. An article containing lutetium oxide and having an average grain size of at most 10 microns.