Fluoride Phosphor Production via Dissolution and Precipitation

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Solution Overview

Problem

Conventional fluoride phosphors exhibit inferior luminescence properties and inadequate reliability in terms of heat resistance, humidity resistance, and quality stability, limiting their practical application in light-emitting devices.

Innovation Solution

A fluoride phosphor production method involving the addition of solid silicon dioxide and a manganese compound that supplies manganese in a valence other than +7 to an aqueous solution, resulting in a fluoride phosphor with enhanced luminescence intensity and reliability, represented by the formula A2SiF6:Mn, where element A is an alkali metal such as potassium, with specific conditions for the manganese content, particle size, and production process.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Illumination intensity

If conventional fluoride phosphors are used, then production is simpler, but luminescence intensity and reliability are inferior

Engineering Contradiction:
Improveluminescence intensityVSAvoidproduction process complexity
Core Design Contradiction:
Illumination intensityVSDevice complexity

Solution Approach 1:

The patent applies preliminary action by pre-dissolving silicon dioxide and manganese compound in hydrofluoric acid before mixing with the aqueous solution containing alkali metal and fluorine. This pre-preparation step ensures proper dissolution and distribution of components, leading to enhanced luminescence intensity and reliability of the resulting fluoride phosphor without significantly complicating the overall production process.

Inventive Principle:
Principle #10Preliminary action

2Reliability

If conventional fluoride phosphors are used, then manufacturing is easier, but heat resistance and humidity resistance are inadequate

Engineering Contradiction:
Improveheat resistance and humidity resistanceVSAvoidmanufacturing ease
Core Design Contradiction:
ReliabilityVSEase of manufacture

Solution Approach 1:

The patent applies parameter changes by precisely controlling the concentrations of hydrofluoric acid (40-70 mass%), alkali metal compound (0.1-10 mol/L), and fluorine compound (0.1-10 mol/L), along with the dissolution time (1-24 hours) and temperature (20-100°C). These optimized parameters result in fluoride phosphors with superior heat resistance and humidity resistance while maintaining ease of manufacture through a straightforward aqueous solution process.

Inventive Principle:
Principle #35Parameter changes

3Stability of the object's composition

If conventional fluoride phosphors are used, then production process is simpler, but quality stability shows high variation

Engineering Contradiction:
Improvequality stabilityVSAvoidproduction process complexity
Core Design Contradiction:
Stability of the object's compositionVSDevice complexity

Solution Approach 1:

The patent applies feedback by systematically optimizing and controlling multiple process parameters including hydrofluoric acid concentration (40-70 mass%), dissolution time (1-24 hours), temperature (20-100°C), and the sequential addition of reagents. This controlled approach with monitored parameters ensures consistent quality and low variation in the produced fluoride phosphors, achieving high quality stability.

Inventive Principle:
Principle #23Feedback

4Illumination intensity

If red phosphors with sharp luminescence spectrum are used, then color rendering is improved, but luminance decreases due to low visual sensitivity

Engineering Contradiction:
ImproveluminanceVSAvoidcolor rendering properties
Core Design Contradiction:
Illumination intensityVSEase of manufacture

Solution Approach 1:

The patent applies composite materials by creating fluoride phosphors with the general formula A2SiF6:Mn, where A is an alkali metal (Li, Na, K, Rb, or Cs). This composite structure combines the fluoride crystal lattice with manganese activators, producing a sharp luminescence spectrum with high luminance output. The resulting material achieves both excellent color rendering properties and high luminance, overcoming the limitation of conventional red phosphors.

Inventive Principle:
Principle #40Composite materials

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 resulting fluoride phosphor demonstrates high luminescence intensity, excellent heat resistance, and stability, leading to improved performance in light-emitting devices with reduced luminance degradation under high-temperature and high-humidity conditions.

Implementation Method 1

a fluoride phosphor production method involving the addition of solid silicon dioxide and a manganese compound that supplies manganese in a valence other than +7 to an aqueous solution, resulting in a fluoride phosphor with enhanced luminescence intensity

Methodology Applied
Scientific EffectLuminescence: Luminescence

Implementation Method 2

addition of solid silicon dioxide and a manganese compound that supplies manganese in a valence other than +7 to an aqueous solution

Methodology Applied
Scientific EffectDissolution: Solvation

Implementation Method 3

resulting in a fluoride phosphor with enhanced luminescence intensity and reliability

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Data Source

PatentUS10941339B2Fluorescent fluoride, light-emitting device, and process for producing florescent fluoride
Publication Date: 2021.03.09 DENKA CO LTD
  • US10941339B2 patent drawing
  • US10941339B2 patent drawing
  • US10941339B2 patent drawing

AI summary

The purpose of the present invention is to provide a fluoride phosphor (represented by the general formula A2SiF6:Mn) having high luminescence intensity and reliability, a high-luminance light-emitting device using this phosphor, and a production method for this phosphor.The production method for a fluoride phosphor represented by the general formula A2SiF6:Mn (where element A is an alkali metal element including at least potassium), wherein the fluoride phosphor production method comprises: a step of preparing an aqueous solution wherein element A and fluorine are dissolved in a solvent; and a step of adding, to the aqueous solution, solid silicon dioxide and a manganese compound that supplies manganese having a valence other than +7; wherein an added amount of the manganese compound is within a range such that an Mn content in the fluoride phosphor becomes at least 0.1 mass % and at most 1.5 mass %; and the fluoride phosphor precipitates as the silicon dioxide concurrently dissolves into the aqueous solution.