IP Library Granted Patent US 9,708,210
Granted Patent B2
US 9,708,210 · App. 14/712,338 · Granted Jul 18, 2017

Striae-free chalcogenide glasses

Inventors: Vinh Q. Nguyen (Fairfax, VA); Mikhail Kotov (Silver Spring, MD); Daniel J. Gibson (Cheverly, MD); Shyam S. Bayya (Ashburn, VA); Jasbinder S. Sanghera (Ashburn, VA)
Assignee: The United States of America, as represented by the Secretary of the Navy
C03C3/321C03B5/06C03B5/16C03B2201/86
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Quick Facts
Patent No.
US 9,708,210
App. No.
14/712,338
Granted
Jul 18, 2017
Kind
B2
Abstract

A method to synthesize striae-free chalcogenide glass using melt processing. A striae-free chalcogenide glass with uniform refractive index.

Claims (46)

1. A method to synthesize striae-free chalcogenide glass using melt processing, comprising the steps of:

melting chalcogenide glass inside a sealed silica ampoule;

providing a 2-zone furnace comprising an upper zone and a lower zone wherein the upper zone is at a higher temperature than the lower zone and wherein the zones are independently controllable temperature zones;

mixing by rocking the sealed silica ampoule inside the 2-zone furnace;

placing the sealed silica ampoule in a vertical position;

forming a glass melt as the upper zone is at a higher temperature than the lower zone;

positioning the glass melt such that the glass melt is within the lower zone; and

cooling slowly and quenching the temperature;

reducing the temperature of the upper zone at a rate of 0.6° C./min to 370° C.;

reducing the temperatures of the lower zone at a rate of 0.6° C./min to 260° C.;

holding these temperatures for 12 hours; and thereby

forming the striae-free chalcogenide glass.

2. The method to synthesize striae-free chalcogenide glass using melt processing of claim 1 , further comprising the step of preventing convection currents within the glass melt as the glass melt solidifies forming the chalcogenide glass.

3. The method to synthesize striae-free chalcogenide glass using melt processing of claim 2 , further comprising the step of preventing condensation of glass on the ampoule as the glass melt cools.

4. The method to synthesize striae-free chalcogenide glass using melt processing of claim 1 , further comprising the steps of:

allowing for an initial melting of the chalcogenide glass prior to the step of mixing by rocking; and

allowing for homogenization of the chalcogenide glass.

5. The method to synthesize striae-free chalcogenide glass using melt processing of claim 4 , further comprising the step of avoiding abrasion of the ampoule during the rocking step.

6. The method to synthesize striae-free chalcogenide glass using melt processing of claim 1 , further comprising the steps of:

maintaining the temperature of the lower zone at a temperature of about 700° C. for about 24 hours; and

maintaining the temperature of the upper zone at a temperature of about 100° C. greater than the temperature of the lower zone for about 24 hours.

7. A method to synthesize striae-free chalcogenide glass using melt processing, comprising the steps of:

loading arsenic and sulfur precursors sufficient to constitute a 120 gram batch of glass with the composition of 39% at. arsenic (As) and 61% at. sulphur (S) or about 71.88 grams As and 48.12 grams S into a silica ampoule under an inert gas atmosphere;

connecting the ampoule to a vacuum pump;

evacuating the ampoule for 4 hours at 1×10 −5 Torr;

sealing the ampoule;

placing the ampoule inside a rocking furnace with a ±45° angle of inclination wherein the furnace has a top zone and a bottom zone and wherein the zones are independently controllable temperature zones;

heating and rocking the ampoule;

heating the top zone and the bottom zone of the furnace at a rate of 3° C./min from room temperature;

heating the top zone to 850° C.;

heating the bottom zone to 750° C.;

holding constant the temperature of the top zone (850° C.) and bottom zone (750° C.) for 10 hours;

rocking the furnace at an inclination angle of ±45° to facilitate mixing and homogenization of the elemental components;

stopping the furnace motion;

setting the furnace to a vertical position or 90° fixed angle;

decreasing the temperature of the top zone at a rate of 1° C./min to 800° C.;

decreasing the temperature of the bottom zone at a rate of 1° C./min to 700° C.;

holding the furnace position and temperature profile for 24 hours to facilitate fining and settling of the glass melt;

reducing the temperature of the top zone at a rate of 0.6° C./min to 370° C.;

reducing the temperatures of the bottom zone at a rate of 0.6° C./min to 260° C.;

holding these temperatures for 12 hours;

forming a chalcogenide glass;

removing the ampoule from the furnace;

submerging the ampoule in a room temperature water bath for 10 seconds to quench the chalcogenide glass;

annealing the chalcogenide glass by placing the ampoule in another furnace at 180° C. for 10 hours; and

forming a striae-free chalcogenide glass.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 22, 2015
From: NGUYEN, VINH Q.; GIBSON, DANIEL J.; BAYYA, SHYAM S.; SANGHERA, JASBINDER S.; KOTOV, MIKHAIL
To: THE GOVERNMENT OF THE UNITED STATES OF AMERICA, AS REPRESENTED BY THE SECRETARY OF THE NAVY
Reel/Frame 036622/0129 →
Continuity (2)
Provisional Application 62007245 · Jun 3, 2014
Related Publication 20150344342A1 · Dec 3, 2015