US2017362115A1PendingUtilityA1

Method of making halogen doped optical element

Assignee: CORNING INCPriority: Nov 26, 2014Filed: Nov 24, 2015Published: Dec 21, 2017
Est. expiryNov 26, 2034(~8.3 yrs left)· nominal 20-yr term from priority
C03C 3/06C03B 2201/12C03B 19/1453C03B 19/066C03B 19/1461C03B 2201/42C03B 2201/20C03B 2201/075C03B 37/01282C03B 37/01453C03B 25/02G02B 6/036C03B 37/014C03B 37/01853C03B 37/01446
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Claims

Abstract

A method of forming an optical element is provided. The method includes producing silica-based soot particles using chemical vapor deposition, the silica-based soot particles having an average particle size of between about 0.05 μm and about 0.25 μm. The method also includes forming a soot compact from the silica-based soot particles and doping the soot compact with a halogen in a closed system by contacting the silica-based soot compact with a halogencontaining gas in the closed system at a temperature of less than about 1200° C.

Claims

exact text as granted — not AI-modified
1 . A method of forming an optical element, the method comprising:
 producing silica-based soot particles using chemical vapor deposition, the silica-based soot particles having an average particle size of between about 0.05 μm and about 0.25 μm;   forming a soot compact from the silica-based soot particles; and   doping the soot compact with a halogen in a closed system by contacting the silica-based soot compact with a halogen-containing gas in the closed system at a temperature of less than about 1200° C.   
     
     
         2 . The method of  claim 1 , wherein forming a soot compact comprises depositing the silica-based soot particles onto a bait rod. 
     
     
         3 . The method of  claim 1 , wherein forming a soot compact comprises pressing the silica-based soot particles at a pressure of between about 100 psi and about 1000 psi. 
     
     
         4 . The method of  claim 3 , wherein pressing the silica-based soot particles comprises axially pressing the silica-based soot particles to form a disc shaped soot compact. 
     
     
         5 . The method of  claim 1 , further comprising maintaining a predetermined halogen-containing gas composition in the closed system. 
     
     
         6 . The method of  claim 5 , wherein maintaining a predetermined halogen-containing gas composition in the closed system comprises bleeding halogen-containing gas into the closed system. 
     
     
         7 . The method of  claim 1 , wherein doping the soot compact comprises maintaining a halogen composition in the closed system of greater than about 90% of the total gas composition of the closed system. 
     
     
         8 . The method of  claim 1 , further comprising maintaining a predetermined halogen-containing gas partial pressure in the closed system. 
     
     
         9 . The method of  claim 8 , wherein the predetermined halogen-containing gas partial pressure in the closed system is between about 0.10 atm and about 0.90 atm. 
     
     
         10 . The method of  claim 1 , wherein the halogen-containing gas is a fluorine-containing gas. 
     
     
         11 . The method of  claim 1 , wherein the halogen-containing gas is a chlorine-containing gas. 
     
     
         12 . The method of  claim 1 , further comprising consolidating the soot compact in the closed system to form a glass article. 
     
     
         13 . The method of  claim 12 , wherein consolidating the soot compact is sufficient to form a glass article comprising a variation of halogen concentration of less than about 0.20 wt. %. 
     
     
         14 . The method of  claim 1 , wherein the silica-based soot particles comprise silica and titania. 
     
     
         15 . The method of  claim 1 , wherein the silica-based soot particles have a surface area of greater than about 10 m 2 /gram. 
     
     
         16 . A method of forming an optical element, the method comprising:
 producing silica-based soot particles using chemical vapor deposition, the silica-based soot particles having an average particle size of between about 0.05 μm and about 0.25 μm;   forming a soot compact from the silica-based soot particles;   doping the soot compact with a halogen in a closed system by contacting the soot compact with a halogen-containing gas in the closed system at a temperature of less than about 1200° C.; and   consolidating the soot compact in the closed system to form a glass article by simultaneously increasing the temperature in the closed system and decreasing the concentration of the halogen-containing gas in the closed system.   
     
     
         17 . The method of  claim 16 , wherein forming a soot compact comprises depositing the silica-based soot particles onto a bait rod. 
     
     
         18 . The method of  claim 16 , wherein forming a soot compact comprises pressing the silica-based soot particles at a pressure of between about 100 psi and about 1000 psi. 
     
     
         19 . The method of  claim 18 , wherein pressing the silica-based soot particles comprises axially pressing the silica-based soot particles to form a disc shaped soot compact. 
     
     
         20 . The method of  claim 16 , wherein decreasing the concentration of the halogen-containing gas in the closed system comprises decreasing the concentration of the halogen-containing gas according to the following equation: 
       
         
           
             
               
                 
                   y 
                   II 
                 
                 = 
                 
                   
                     y 
                     
                       I 
                       , 
                       dop 
                     
                   
                    
                   
                     Exp 
                      
                     
                       [ 
                       
                         
                           - 
                           21741 
                         
                          
                         
                           ( 
                           
                             
                               ( 
                               
                                 1 
                                 
                                   T 
                                   
                                     I 
                                     , 
                                     dop 
                                   
                                 
                               
                               ) 
                             
                             - 
                             
                               ( 
                               
                                 1 
                                 
                                   T 
                                   II 
                                 
                               
                               ) 
                             
                           
                           ) 
                         
                       
                       ] 
                     
                   
                 
               
               , 
             
           
         
         wherein: T I,dop  is the temperature in the closed system when doping the soot compact with halogen; 
         T II  is the temperature in the closed system when consolidating the soot compact; 
         y I,dop  is the concentration in mole fraction of the halogen-containing gas in the closed system when doping the soot compact with halogen; and 
         y II  is the maximum concentration in mole fraction of the halogen-containing gas in the closed system when consolidating the soot compact at T II . 
       
     
     
         21 . The method of  claim 16 , further comprising annealing the glass article by cooling the glass article in the closed system at a temperature of between about 900° C. and about 1100° C. and maintaining the temperature between about 900° C. and about 1100° C. for less than about 10 hours. 
     
     
         22 . The method of  claim 21 , wherein annealing the glass article is sufficient to form a glass article having a fictive temperature of less than about 1100° C. 
     
     
         23 . The method of  claim 16 , further comprising decreasing the temperature of the closed system to between about 700° C. and about 850° C. at a rate of less than about 10° C. per hour. 
     
     
         24 . The method of  claim 16 , wherein doping the soot compact further comprises maintaining a predetermined halogen-containing gas composition in the closed system. 
     
     
         25 . The method of  claim 16 , wherein doping the soot compact comprises maintaining a halogen composition in the closed system of greater than about 90% of the total gas composition of the closed system. 
     
     
         26 . The method of  claim 16 , wherein doping the soot compact further comprises maintaining a predetermined halogen-containing gas partial pressure in the closed system. 
     
     
         27 . The method of  claim 26 , wherein the predetermined halogen-containing gas partial pressure in the closed system is between about 0.10 atm and about 0.90 atm. 
     
     
         28 . The method of  claim 16 , wherein the halogen-containing gas is a fluorine-containing gas. 
     
     
         29 . The method of  claim 16 , wherein the halogen-containing gas is a chlorine-containing gas. 
     
     
         30 . The method of  claim 16 , wherein consolidating the soot compact is sufficient to form a glass article comprising a variation of halogen concentration of less than about 0.20 wt. %. 
     
     
         31 . The method of  claim 16 , wherein the silica-based soot particles comprise silica and titania. 
     
     
         32 . The method of  claim 16 , wherein the silica-based soot particles have a surface area of greater than about 10 m 2 /gram.

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