US 11,731,896 B2
Manufacturing process for striae-free multicomponent chalcogenide glasses via multiple fining steps
Vinh Q. Nguyen, Fairfax, VA (US); Mikhail Kotov, Silver Spring, MD (US); Daniel J. Gibson, Falls Church, VA (US); Shyam S. Bayya, Ashburn, VA (US); Jasbinder S. Sanghera, Ashburn, VA (US); and Gryphon A. Drake, Potomac, MD (US)
Assigned to The Government of the United States of America, as represented by the Secretary of the Navy, Washington, DC (US)
Filed by The Government of the United States of America, as represented by the Secretary of the Navy, Arlington, VA (US)
Filed on Apr. 27, 2021, as Appl. No. 17/241,378.
Application 17/241,378 is a division of application No. 16/185,253, filed on Nov. 9, 2018, granted, now 10,988,407.
Application 16/185,253 is a division of application No. 15/059,637, filed on Mar. 3, 2016, granted, now 10,131,568.
Claims priority of provisional application 62/127,305, filed on Mar. 3, 2015.
Prior Publication US 2021/0246066 A1, Aug. 12, 2021
Int. Cl. C03C 3/32 (2006.01); C03B 5/06 (2006.01); C03B 1/00 (2006.01); C03B 5/16 (2006.01); C03B 5/187 (2006.01); C03B 25/00 (2006.01); C03B 27/02 (2006.01)
CPC C03C 3/321 (2013.01) [C03B 1/00 (2013.01); C03B 5/06 (2013.01); C03B 5/16 (2013.01); C03B 5/187 (2013.01); C03B 25/00 (2013.01); C03B 27/028 (2013.01); C03B 2201/86 (2013.01)] 1 Claim
 
1. A striae-free chalcogenide glass made by the method, comprising:
loading germanium, arsenic, selenium, and tellurium precursors into an ampoule, wherein the germanium, arsenic, selenium, and tellurium 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. tellurium, wherein 0.5≤x≤25, 30≤x+y≤55, and 0.5≤z≤20, 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 maintaining the Step 1 bottom zone temperature as the 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; and
removing the ampoule from the furnace and water quenching the glass.