Mn4+ Doped Phosphor Particle Size Control via Semi-Continuous Flow

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Solution Overview

Problem

Existing processes for producing Mn4+ doped red-emitting phosphors result in a wide range of particle sizes, leading to clogging issues in manufacturing and non-homogeneous distributions, which affect the performance and consistency of LED packages and display applications.

Innovation Solution

A semi-continuous flow process involving gradual addition of solutions containing sources of M and Mn in the presence of A, with periodic discharge of the product liquor from the reactor, to control particle size and distribution, resulting in a more homogeneous and efficient production of Mn4+ doped phosphors.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If batch processes are used to prepare Mn4+ doped phosphors, then the production process is simple, but the particle size distribution is broad and includes large particles that cause manufacturing problems

Engineering Contradiction:
Improveprocess simplicityVSAvoidparticle size distribution
Core Design Contradiction:
Ease of manufactureVSManufacturing precision

Solution Approach 1:

The batch process is segmented into multiple controlled addition steps where reagents are added incrementally rather than all at once. This segmentation of the addition process allows better control over nucleation and growth rates, resulting in narrower particle size distribution while maintaining process simplicity.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The process transitions from static batch mixing to dynamic controlled addition with varying rates. By adjusting the addition rate and timing of reagents during the reaction, the system dynamically controls particle formation to achieve uniform size distribution while keeping the overall process straightforward.

Inventive Principle:
Principle #15Dynamics

2Ease of manufacture

If batch processes are used to prepare Mn4+ doped phosphors, then the process is easy to implement, but large particles are produced that clog dispensing equipment

Engineering Contradiction:
Improveprocess implementationVSAvoidequipment clogging
Core Design Contradiction:
Ease of manufactureVSObject-affected harmful factors

Solution Approach 1:

The process performs preliminary control of particle formation through controlled reagent addition rates and sequences before the main reaction completes. By pre-establishing optimal addition conditions, the system prevents formation of oversized particles that would clog equipment, while keeping the overall implementation simple.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The process changes key parameters such as addition rate, temperature, and concentration during different stages of the reaction. By dynamically adjusting these parameters, the system maintains particle sizes within acceptable ranges to prevent equipment clogging without complicating the manufacturing implementation.

Inventive Principle:
Principle #35Parameter changes

3Ease of manufacture

If batch processes are used to prepare Mn4+ doped phosphors, then the production method is straightforward, but the product shows batch to batch variation in properties

Engineering Contradiction:
Improveproduction method simplicityVSAvoidproduct property consistency
Core Design Contradiction:
Ease of manufactureVSStability of the object's composition

Solution Approach 1:

The process incorporates feedback mechanisms where the addition rate and timing are adjusted based on observed reaction progress and particle formation. This feedback control ensures consistent product properties across batches while maintaining a straightforward production methodology through standardized control protocols.

Inventive Principle:
Principle #23Feedback

Solution Approach 2:

The process ensures continuous and consistent reaction conditions through controlled continuous addition of reagents throughout the reaction period. This continuity of useful action eliminates the variability inherent in manual batch operations, achieving consistent product properties without complicating the production method.

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 process yields Mn4+ doped phosphors with a narrower particle size distribution, improving manufacturing efficiency and maintaining performance in lighting and display applications by reducing large particles and ensuring better control over final product properties.

Implementation Method 1

Processes for preparing the materials described in the patent andscientific literature typically involve mixing the raw materials and precipitating the product

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Data Source

PatentEP3303516A1Color stable red-emitting phosphors
Publication Date: 2018.04.11 GE LIGHTING SOLUTIONS LLC

AI summary

A process for preparing a Mn+4 doped phosphor of formula: Ax [MFy]:Mn+4, includes gradually adding a first solution to a second solution and periodically discharging the product liquor from the reactor while volume of the product liquor in the reactor remains constant; 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. The first solution includes a source of M and HF and the second solution includes a source of Mn to a reactor in the presence of a source of A.