Corning Incorporated

Carlos Alberto Duran

Kenneth Edward Hrdina

Sezhian Annamalai

William Rogers Rosch

Steven Bruce Dawes

Lisa Anne Moore

Richard Michael Fiacco

Jesse Kohl

Daniel Raymond Sempolinski

Bryan Ray Wheaton

John Edward Maxon

Ulrich Wilhelm Heinz Neukirch

Michael A Mueller

William Robert Angell, Iv

Seshian Annamalai

William R Iv Angell

Annealing treatments for modified titania-silica glasses and the glasses produced by the annealing treatments. The annealing treatments include an isothermal hold that facilitates equalization of non-uniformities in fictive temperature caused by non-uniformities in modifier concentration in the glasses. The annealing treatments may also include heating the glass to a higher temperature following the isothermal hold and holding the glass at that temperature for several hours. Glasses produced by the annealing treatments exhibit high spatial uniformity of CTE, CTE slope, and fictive temperature, including in the presence of a spatially non-uniform concentration of modifier.

Ultralow expansion titania-silica glass

Near-infrared shielding includes a glass material. The shielding provides transmittance at wavelengths between 390 to 700 nm, but near infrared absorbing species are distributed throughout the glass material and the shielding blocks light in the near infrared range. Further, the glass material has a near zero or negative coefficient of thermal expansion, allowing the glass material to heat up when the shielding is blocking a near infrared laser, without expanding much.

Near infrared shielding and laser-resistant window

An improved method and apparatus for determination of the absolute coefficient of thermal expansion of materials, including ultralow expansion materials, utilizes a metrology frame that is regulated within a first narrow temperature range that varies by only a small fraction of a degree Celsius from a set point temperature (e.g., less than about 0.01&#xb0; C. from the set point temperature), while the temperature of the sample is varied to determine the coefficient of thermal expansion over a larger temperature range (e.g., 30, 40 or 50&#xb0; C.). The method and apparatus permit determination of the coefficient of thermal expansion of a material to levels approaching 10/&#xb0; C.

Apparatus and method for the determination of the absolute coefficient of thermal expansion in ultralow expansion materials

A method of forming a doped silica-titania glass is provided. The method includes blending batch materials comprising silica, titania, and at least one dopant. The method also includes heating the batch materials to form a glass melt. The method further includes consolidating the glass melt to form a glass article, and annealing the glass article.

Doped silica-titania glass having low expansivity and methods of making the same

A doped silica-titania ('DST') glass article that includes a glass article having a glass composition comprising a silica-titania base glass containing titania at 7 to 14 wt. % and a balance of silica, and a dopant selected from the group consisting of (a) F at 0.7 to 1.5 wt. %, (b) BOat 1.5 to 5 wt. %, (c) OH at 1000 to 3000 ppm, and (d) BOat 0.5 to 2.5 wt. % and OH at 100 to 1400 ppm. The glass article has an expansivity slope of less than about 1.3 ppb/Kat 20&#xb0; C. For DST glass articles doped with F or BO, the OH level can be held to less than 10 ppm, or less than 100 ppm, respectively. In many aspects, the DST glass articles are substantially free of titania in crystalline form.

Doped ultra-low expansion glass and methods for annealing the same

Silica-titania glasses with small temperature variations in coefficient of thermal expansion over a wide range of zero-crossover temperatures and methods for making the glasses. The method includes a cooling protocol with controlled anneals over two different temperature regimes. A higher temperature controlled anneal may occur over a temperature interval from 750&#xb0; C.-950&#xb0; C. or a sub-interval thereof. A lower temperature controlled anneal may occur over a temperature interval from 650&#xb0; C.-875&#xb0; C. or a sub-interval thereof. The controlled anneals permit independent control over CTE slope and Tzc of silica-titania glasses. The independent control provides CTE slope and Tzc values for silica-titania glasses of fixed composition over ranges heretofore possible only through variations in composition.

Ultralow expansion glass

A doped silica-titania glass article is provided that includes a glass article having a glass composition comprising (i) a silica-titania base glass, (ii) a fluorine dopant, and (iii) a second dopant. The fluorine dopant has a concentration of fluorine of up to 5 wt. % and the second dopant comprises one or more oxides selected from the group consisting of Al, Nb, Ta, B, Na, K, Mg, Ca and Li oxides at a total oxide concentration from 50 ppm to 6 wt. %. Further, the glass article has an expansivity slope of less than 0.5 ppb/Kat 20&#xb0; C. The second dopant can be optional. The composition of the glass article may also contain an OH concentration of less than 100 ppm.

Doped ultra-low expansion glass and methods for making the same

Ultralow expansion titania-silica glass. The glass has high hydroxyl content and optionally include one or more dopants. Representative optional dopants include boron, alkali elements, alkaline earth elements or metals such as Nb, Ta, Al, Mn, Sn Cu and Sn. The glass is prepared by a process that includes steam consolidation to increase the hydroxyl content. The high hydroxyl content or combination of dopant(s) and high hydroxyl content lowers the fictive temperature of the glass to provide a glass having a very low coefficient of thermal expansion (CTE), low fictive temperature (T), and low expansivity slope.

[object Object]

A boron-doped titania-silica glass containing 0.1 wt % to 8.0 wt % boron, 9.0 wt % to 16.0 wt % TiO, and 76.0 wt % to 90.9 wt % SiO. The glass may further include F, Nb, Ta, Al, Li, Na, K, Ca, and Mg, individually or in combinations of two or more, at levels up to 4 wt %. The glass may have an OH concentration of more than 10 ppm. The glass features a CTE slope at 20&#xb0; C. of less than 1 ppb/K. The fictive temperature of the glass is less than 825&#xb0; C. and the peak CTE of the glass is less than 30 ppb/K. The glass has two crossover temperatures and a wide temperature interval over which CTE is close to zero. The uniformity of each crossover temperature relative to its average over a volume of at least 50 cmis within &#xb1;5&#xb0; C.

Boron-doped titania-silica glass having very low CTE slope

A glass article for use in Extreme Ultra-Violet Lithography (EUVL) is provided. The glass article includes a silica-titania glass having a compositional gradient through the glass article, the compositional gradient being defined by the functions:[TiO]=(()), and[SiO]=(100&#x2212;{()}&#x2212;&#x3b4;())wherein [TiO] is the concentration of titania in wt. %, [SiO] is the concentration of silica in wt. %, c is the titania concentration in wt. % for a predetermined zero crossover temperature (T), f(x, y, z) is a function in three-dimensional space that defines the difference in average composition of a volume element centered at the coordinates (x, y, z) with respect to c, and &#x3b4;(x, y, z) is a function in three-dimensional space that defines the sum of all other components of a volume element centered at the coordinates (x, y, z).

The present disclosure is directed to a doped silica-titania glass, DST glass, consisting essentially of 0.1 wt. % to 5 wt. % halogen, 50 ppm-wt. to 6 wt. % one or more oxides of Al, Ta and Nb, 3 wt. % to 10 wt. % TiOand the remainder SiO. In an embodiment the halogen content can be in the range of 0.2 wt. % to 3 wt. % along with 50 ppm-wt. to 6 wt. % one or more oxides of Al, Ta and Nb, 3 wt. % to 10 wt. % TiOand the remainder SiO. In an embodiment the DST glass has an OH concentration of less than 100 ppm. In another embodiment the OH concentration is less than 50 ppm. The DST glass has a fictive temperature Tof less than 875&#xb0; C. In an embodiment Tis less than 825&#xb0; C. In another embodiment Tis less than 775&#xb0; C.

Very low CTE slope doped silica-titania glass

The disclosure describes a method by which the Tzc of a silica-titania glass article, for example, a EUVL mirror substrate, can be tuned to within a specification range by means of a selected final anneal that shifts Tzc of the article or substrate to the desired Tzc value. In addition, since different mirrors in a set can be specified at different values of Tzc, this process can be on used glass samples or pieces from a single glass boule to make parts with different Tzc values, thus reducing the number of separate boules required to fill an order.

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Ottawa, Canada

Carlos Alberto Duran