Mn4+ Red-Emitting Phosphor Synthesis for Sub-10 μm Particle Control

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Solution Overview

Problem

Current processes for preparing red-emitting phosphors based on complex fluoride materials, such as K2SiF6:Mn4+, often result in particles larger than 10 μm with broad size distributions, which can cause manufacturing issues in LED packaging and reduce efficiency due to total internal reflection.

Innovation Solution

A method involving combining a source of A (Li, Na, K, Rb, or Cs) with a source of Mn in the presence of H2MF6, under controlled conditions to produce Mn4+ doped phosphors with a monodisperse population of particles less than 10 μm in size and a narrow particle size distribution, and optionally coating these phosphors with a manganese-free metal fluoride shell using microemulsion techniques.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional processes are used to prepare red-emitting phosphor particles, then the particles can be produced, but the particle size becomes greater than 10 μm with broad distribution

Engineering Contradiction:
Improveparticle size controlVSAvoidparticle size distribution width
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The patent applies parameter changes by controlling the Hammett acidity function (Ho ≥ -0.9) of the first solution, adjusting the molar ratios of reactants, and optimizing reaction temperature and time to achieve precise particle size control below 10 μm with narrow distribution

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses an intermediary approach by employing a specific acidic solution with controlled Hammett acidity function as a medium to facilitate the reaction between K2SiF6 and Mn sources, enabling precise nucleation and growth control that produces monodisperse particles with D50 < 10 μm

Inventive Principle:
Principle #24Intermediary (Mediator)

2Manufacturing precision

If high aspect ratio nanorods are produced, then the particle size can be reduced, but manufacturing problems occur in LED packaging

Engineering Contradiction:
Improveparticle sizeVSAvoidLED packaging suitability
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The patent applies local quality by controlling the aspect ratio to be about 3/1 or less, creating particles with optimized local dimensional characteristics that are small enough for LED packaging while maintaining uniformity and avoiding the manufacturing issues associated with high aspect ratio nanorods

Inventive Principle:
Principle #3Local quality

Solution Approach 2:

The patent changes the morphological parameters by controlling the reaction conditions (Hammett acidity, molar ratios, temperature) to produce particles with aspect ratio ≤ 3/1, transforming the particle shape from high aspect ratio nanorods to more suitable forms for LED packaging applications

Inventive Principle:
Principle #35Parameter changes

3Manufacturing precision

If particles with high aspect ratio are used, then particle size can be small, but total internal reflection reduces efficiency

Engineering Contradiction:
Improveparticle sizeVSAvoidlight emission efficiency
Core Design Contradiction:
Manufacturing precisionVSLoss of energy

Solution Approach 1:

The patent changes the geometric parameter of aspect ratio to about 3/1 or less, which reduces total internal reflection losses while maintaining small particle size, thereby improving light extraction efficiency and reducing energy loss in LED applications

Inventive Principle:
Principle #35Parameter changes

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 achieves phosphor particles with a D50 size of less than 10 μm, aspect ratio of 3/1 or less, and improved efficiency in lighting and display applications by minimizing internal reflection and enhancing manufacturing feasibility.

Implementation Method 1

wherein a value of a Hammett acidity function of the first solution is at least −0.9

Methodology Applied
Scientific EffectHammett acidity function:

Data Source

PatentUS20240218243A1Processes for preparing color stable red-emitting phosphor particles having small particle size
Publication Date: 2024.07.04 GE LIGHTING SOLUTIONS LLC
  • US20240218243A1 patent drawing
  • US20240218243A1 patent drawing
  • US20240218243A1 patent drawing

AI summary

A process for preparing a Mn+4 doped phosphor of formula I Ax [MFy]:Mn+4 I includes combining a first solution comprising a source of A and a second solution comprising H2MF6 in the presence of a source of Mn, to form the Mn+4 doped phosphor; wherein A is Li, Na, K, Rb, Cs, or a combination thereof; M is Si, Ge, Sn, Ti, Zr, Al, Ga, In, Sc, Y, La, Nb, Ta, Bi, Gd, or a combination thereof; x is the absolute value of the charge of the [MFy] ion; y is 5, 6 or 7; and wherein a value of a Hammett acidity function of the first solution is at least −0.9. Particles produced by the process may have a particle size distribution with a D50 particle size of less than 10 μm.