Manufacturing process for striae-free multicomponent chalcogenide glasses via multiple fining steps

Patent metadata

Field	Value
Publication number	US-10988407-B2
Application number	US-201816185253-A
Country	US
Kind code	B2
Filing date	Nov 9, 2018
Priority date	Mar 3, 2015
Publication date	Apr 27, 2021
Grant date	Apr 27, 2021

Abstract

The present invention provides for synthesizing high optical quality multicomponent chalcogenide glasses without refractive index perturbations due to striae, phase separation or crystal formation using a two-zone furnace and multiple fining steps. The top and bottom zones are initially heated to the same temperature, and then a temperature gradient is created between the top zone and the bottom zone. The fining and cooling phase is divided into multiple steps with multiple temperature holds.

First claim

What is claimed as new and desired to be protected by Letters Patent of the United States is:

1. A striae-free chalcogenide glass made by the method, comprising:
loading germanium, arsenic, sulfur, and selenium precursors into an ampoule, wherein the germanium, arsenic, sulfur, and selenium precursors are sufficient to constitute a glass with the composition of x % at. germanium, y % at. arsenic, z % at. selenium, and (100-x-y-z) % at. sulfur, wherein 0.5≤x≤10, 30≤x+y≤45, and 0.5≤z≤10, sealing the ampoule, and placing the ampoule in a rocking furnace, wherein the rocking furnace comprises a top zone and a bottom zone, wherein the top and bottom zones are two independently controllable temperature zones;
heating both the top and bottom zones at a rate of 3° C. per minute to a Step 1 temperature, wherein the Step 1 temperature is the same for both the top and bottom zones;
maintaining the Step 1 temperature in the top and bottom zones while rocking the furnace at an inclination angle of +45° for 15 hours;
increasing the temperature of the top zone at a rate of 0.6° C. per minute to a Step 3 top zone temperature and decreasing the temperature of the bottom zone at a rate of 0.6° C. per minute to a Step 3 bottom zone temperature while rocking the furnace at an inclination angle of +45°, wherein there is a temperature gradient of 100° C. between the Step 3 top zone temperature and the Step 3 bottom zone temperature;
setting the furnace to a vertical position and maintaining the Step 3 top zone temperature and the Step 3 bottom zone temperature for 3 hours;
decreasing the temperature of the top zone at a rate of 10° C. per minute to a Step 5 top zone temperature, decreasing the temperature of the bottom zone at a rate of 10° C. per minute to a Step 5 bottom zone temperature, and maintaining the Step 5 top zone temperature and Step 5 bottom zone temperature for 3 hours, wherein the Step 5 top zone temperature is 100° C. lower than the Step 3 top zone temperature, and wherein the Step 5 bottom zone temperature is 100° C. lower than the Step 3 bottom zone temperature;
decreasing the temperature of the top zone at a rate of 10° C. per minute to a Step 6 top zone temperature, decreasing the temperature of the bottom zone at a rate of 10° C. per minute to a Step 6 bottom zone temperature, and maintaining the Step 6 top zone temperature and Step 6 bottom zone temperature for 3 hours, wherein the Step 6 top zone temperature is 100° C. lower than the Step 5 top zone temperature, and wherein the Step 6 bottom zone temperature is 100° C. lower than the Step 5 bottom zone temperature;
decreasing the temperature of the top zone at a rate of 10° C. per minute to a Step 7 top zone temperature, decreasing the temperature of the bottom zone at a rate of 10° C. per minute to a Step 7 bottom zone temperature, and maintaining the Step 7 top zone temperature and Step 7 bottom zone temperature for 30 minutes, wherein the Step 7 top zone temperature is at least 100° C. lower than the Step 6 top zone temperature, and wherein the Step 7 bottom zone temperature is at least 100° C. lower than the Step 6 bottom zone temperature; and
removing the ampoule from the furnace and water quenching the glass.

Assignees

• Us Gov Sec Navy

Inventors

• Nguyen Vinh Q
• Kotov Mikhail
• Gibson Daniel J
• Bayya Shyam S
• Sanghera Jasbinder S
• Drake Gryphon A

Classifications

• C03B2201/86

  Chalcogenide glasses, i.e. S, Se or Te glasses · CPC title

• C03B1/00

  Preparing the batches (chemical compositions C03C) · CPC title

• C03B5/16

  Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces · CPC title

• C03B27/028

  the liquid being water-based · CPC title

• C03B5/06

  in pot furnaces {(C03B5/02 takes precedence)} · CPC title