Chalcogenide Glass Quenching Process for Refractive Index Control

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Solution Overview

Problem

Conventional methods for producing chalcogenide glasses, including rare-earth doped chalcogenide glasses, result in refractive index perturbations and low yield due to turbulent viscous flow and rapid quenching, leading to costly and low-quality optical fibers with limited optical performance.

Innovation Solution

A process involving heating glass components to a melt temperature, holding the melt in a vertical furnace for homogenization, slow cooling, and controlled sequential quenching from the top down, along with dynamic distillation to remove oxygen and hydrogen impurities, to produce stable and high-quality chalcogenide glasses.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Speed

If the ampoule is set from a 45 degree angle to a 90 degree angle for quenching, then the glass melt is cooled rapidly, but turbulent viscous flow occurs at the top of the glass melt near the meniscus causing refractive index perturbations

Engineering Contradiction:
Improvecooling rateVSAvoidrefractive index uniformity
Core Design Contradiction:
SpeedVSManufacturing precision

Solution Approach 1:

The quenching process is divided into multiple stages: first cooling the glass melt from 45 degrees to reduce surface area and minimize turbulent flow, then rotating to 90 degrees for final quenching. This segmented approach allows controlled cooling that prevents refractive index perturbations while achieving rapid quenching.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The glass melt is preliminarily cooled at a 45-degree angle before being rotated to 90 degrees for final quenching. This preliminary cooling action reduces the temperature and viscosity of the glass melt, preventing turbulent viscous flow and refractive index perturbations during the subsequent rapid quenching phase.

Inventive Principle:
Principle #10Preliminary action

2Speed

If conventional quenching is used, then the glass melt is cooled rapidly, but a large meniscus forms resulting in lower yield of usable glass

Engineering Contradiction:
Improvecooling rateVSAvoidglass yield
Core Design Contradiction:
SpeedVSProductivity

Solution Approach 1:

The quenching process is segmented into two phases: initial cooling at 45 degrees to minimize meniscus formation and maximize usable glass yield, followed by rotation to 90 degrees for rapid final quenching. This segmentation allows the glass to cool in a controlled manner that preserves volume while achieving rapid quenching.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The ampoule orientation angle is changed as a parameter during the quenching process. By dynamically adjusting the angle from 45 degrees to 90 degrees, the process optimizes both meniscus control (for high yield) and cooling rate (for rapid quenching), achieving over 80% usable glass yield.

Inventive Principle:
Principle #35Parameter changes

3Speed

If rapid quenching is used, then the glass is cooled quickly, but a powerful shock wave causes cracking of the chalcogenide glass

Engineering Contradiction:
Improvecooling rateVSAvoidglass integrity
Core Design Contradiction:
SpeedVSStrength

Solution Approach 1:

The glass is preliminarily cooled at a 45-degree angle before rapid quenching at 90 degrees. This preliminary cooling reduces thermal gradients and prevents the formation of powerful shock waves that cause cracking, while still achieving rapid final quenching to maintain glass structure.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The ampoule orientation angle is dynamically changed during quenching to control the cooling rate profile. By transitioning from 45 degrees to 90 degrees, the process achieves rapid quenching while controlling thermal stress distribution to prevent glass cracking and maintain integrity.

Inventive Principle:
Principle #35Parameter changes

4Speed

If conventional quenching is used, then the glass is cooled rapidly, but oxygen and hydrogen impurities remain in the glass affecting quality

Engineering Contradiction:
Improvecooling rateVSAvoidglass purity
Core Design Contradiction:
SpeedVSManufacturing precision

Solution Approach 1:

Dynamic distillation is performed as a preliminary action before quenching to remove oxygen and hydrogen impurities from the glass melt. This preliminary purification ensures high glass quality while the subsequent rapid quenching preserves the purified structure.

Inventive Principle:
Principle #10Preliminary 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 minimizes refractive index perturbations, increases the yield of usable glass to over 80%, and enables the production of high-quality optical fibers with improved optical properties, suitable for infrared applications, including fiber lasers and sensors.

Implementation Method 1

heating the glass components to a melt temperature to form a melt

Methodology Applied
Scientific EffectHeating: Heating

Implementation Method 2

slow cooling the melt at less than 10° C. per minute

Methodology Applied
Scientific EffectSlow cooling: Cooling

Implementation Method 3

sequentially quenching the melt from the top down in a controlled manner

Methodology Applied
Scientific EffectQuenching: Cooling

Implementation Method 4

process for removing oxygen and hydrogen impurities from chalcogenide glass components using dynamic distillation

Methodology Applied
Scientific EffectDistillation: Distillation

Data Source

PatentUS8726698B2Manufacturing process for chalcogenide glasses
Publication Date: 2014.05.20 THE UNITED STATES OF AMERICA AS REPRESENTED BY THE SECRETARY OF THE NAVY
  • US8726698B2 patent drawing
  • US8726698B2 patent drawing
  • US8726698B2 patent drawing

AI summary

The present invention is generally directed to a method of making chalcogenide glasses including holding the melt in a vertical furnace to promote homogenization and mixing; slow cooling the melt at less than 10° C. per minute; and sequentially quenching the melt from the top down in a controlled manner. Additionally, the present invention provides for the materials produced by such method. The present invention is also directed to a process for removing oxygen and hydrogen impurities from chalcogenide glass components using dynamic distillation.