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US4528010A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for producing optical glass product

Assignee: Sumitomo Electric Industries Ltd
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Filing: 1984-02-29
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Granted: 1985-07-09
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Expires: 2004-02-29
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Abstract

Abstract A process for producing an optical glass product having a predetermined distribution of refractive index in the interior of the product is disclosed. The process comprises the steps of: (a) preparing an aqueous silicate solution containing from about 0.1 to about 0.6 mol/liter of Si (as SiO 2 ) comprising silicic acid and at least one element selected from the group consisting of rubidium, thallium and cesium; (b) mixing the silicate solution with an acidic aqueous solution, and letting the two solutions react with each other for a period of time sufficient for polymerization to produce a porous gelled product wherein the silica particles are agglomerated; (c) leaching the gelled product with a liquid selected from the group consisting of water, a weakly acidic aqueous solution, an aqueous solution having an alkali metal salt dissolved therein and an aqueous solution of organic matter capable of dissolving Rb 2 O, Cs 2 O, or Tl 2 O, unitl the center of the product starts to dissolve; and (d) drying the leached product in a predetermined atmosphere, and further heating the partially leached gelled product at a temperature sufficiently high to eliminate the particulate material but lower than the melting point of the silica.

Inventors

  • 👤 Takao Edahiro
  • 👤 Nobuo Inagaki
  • 👤 Shiro Kurosaki

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-24 03:11
CPC Classifications
C; C03; C03C; C03C23/00; C03C23/008; C03B; C03B37/00; C03B37/01; C03B37/012; C03B37/014; C03B37/016; C03C3/00; C03C3/04; C03C3/06; C03B2201/00; C03B2201/06; C03B2201/30; C03B2201/50; C03C2201/00; C03C2201/06; C03C2201/30; C03C2201/50; C03C2203/00; C03C2203/20; C03C2203/24; C03C2203/36; Y; Y10; Y10S; Y10S65/00; Y10S65/901

Claims Analysis

Total Claims: 9
Claim 1
Independent Claim 359 words
A process for producing an optical glass product having a predetermined distribution of refractive index in the interior of the product, said process comprising the steps of: (a) mixing together a silica compound with a silicate selected from the group consisting of rubidium silicate, thallium silicate and cesium silicate, and thereby preparing an aqueous silicate solution containing from about 0.1 to about 0.6 mol/liter of Si, as SiO 2 , said solution comprising silicic acid and at least one element selected from the group consisting of rubidium, thallium and cesium; (b) mixing the silicate solution with an acidic aqueous solution of dilute acetic acid, dilute H 2 SO 4 , H 3 BO 3 , H 3 PO 4 , Al 2 (SO 4 ) 3 or HCl to produce a reaction mixture having a pH of about 6.3 when HCl is used or a pH of about 4.4 when acetic acid, H 2 SO 4 , H 3 BO 3 , H 3 PO 4 or Al 2 (SO 4 ) is used, and allowing the reaction mixture to react for a period of time sufficient for polymerization to produce a completely gelled porous product wherein the silica particles of said product are agglomerated; (c) leaching the gelled product with a liquid capable of dissolving Rb 2 O, Cs 2 O or Tl 2 O, said liquid being selected from the group consisting of (i) water, (ii) a weakly acidic aqueous solution, (iii) an aqueous solution having an alkali metal salt dissolved therein, and (iv) an aqueous solution of organic matter or (v) a mixture of any two of (i) to (iv), said leaching being continued until the concentration of at least one compound selected from the group consisting of Tl 2 O, Rb 2 O and Cs 2 O parabolically decreases from the center of said gelled product outward; and (d) drying the leached product in a predetermined atmosphere, and further heating the partially leached gelled product at a temperature sufficiently high to eliminate the particulate material but lower than the melting point of the silica, whereby the micropores in the leached product are caused to collapse.
Claim 2
Dependent Claim 359 words
A process for producing an optical glass product having a predetermined distribution of refractive index in the interior of the product, said process comprising the steps of: (a) mixing together a silica compound with a silicate selected from the group consisting of rubidium silicate, thallium silicate and cesium silicate, and thereby preparing an aqueous silicate solution containing from about 0.1 to about 0.6 mol/liter of Si, as SiO 2 , said solution comprising silicic acid and at least one element selected from the group consisting of rubidium, thallium and cesium; (b) mixing the silicate solution with an acidic aqueous solution of dilute acetic acid, dilute H 2 SO 4 , H 3 BO 3 , H 3 PO 4 , Al 2 (SO 4 ) 3 or HCl to produce a reaction mixture having a pH of about 6.3 when HCl is used or a pH of about 4.4 when acetic acid, H 2 SO 4 , H 3 BO 3 , H 3 PO 4 or Al 2 (SO 4 ) is used, and allowing the reaction mixture to react for a period of time sufficient for polymerization to produce a completely gelled porous product wherein the silica particles of said product are agglomerated; (c) leaching the gelled product with a liquid capable of dissolving Rb 2 O, Cs 2 O or Tl 2 O, said liquid being selected from the group consisting of (i) water, (ii) a weakly acidic aqueous solution, (iii) an aqueous solution having an alkali metal salt dissolved therein, and (iv) an aqueous solution of organic matter or (v) a mixture of any two of (i) to (iv), said leaching being continued until the concentration of at least one compound selected from the group consisting of Tl 2 O, Rb 2 O and Cs 2 O parabolically decreases from the center of said gelled product outward; and (d) drying the leached product in a predetermined atmosphere, and further heating the partially leached gelled product at a temperature sufficiently high to eliminate the particulate material but lower than the melting point of the silica, whereby the micropores in the leached product are caused to collapse.
Claim 3
Dependent Claim 29 words
A process according to claim 1, wherein the aqueous silicate solution prepared in step (a) contains a member selected from the group consisting of ammonium, lithium, sodium, and potassium.
Claim 4
Dependent Claim 24 words
A process according to claim 1, wherein the acidic aqueous solution of step (b) contains a cation capable of being converted to an oxide.
Claim 5
Dependent Claim 22 words
A process according to claim 1, wherein prior to drying according to step (d), the product is soaked in an organic solvent.
Claim 6
Dependent Claim 14 words
A process according to claim 4, wherein the organic solvent is ethanol or propanol.
Claim 7
Dependent Claim 110 words
A process according to claim 1, 2, 3, 4, or 5, wherein in step (b) said mixing comprises pouring a stirred mixture of the silicate solution and the acidic aqueous solution into a cylindrical vessel where it is gelled, wherein the gelled product of step (b) is leached in step (c) until the concentration of said at least one compound begins to decrease from said center outward, and thereafter the leached product is dried and sintered in step (d), to provide a glass rod wherein the concentration of at least one compound selected from Tl 2 O, Rb 2 O, and Cs 2 O decreases parabolically from the center outward.
Claim 8
Dependent Claim 114 words
A process according to claim 1, 2, 3, 4, or 5, wherein in step (b) said mixing includes stirring the silicate solution and the acidic aqueous solution and said process includes cylindrically grinding the gelled product of step (b) to form a rod prior to step (c), and wherein in step (c) said leaching is until the concentration of said at least one compound begins to decrease from said center outward, and thereafter the leached product is dried and sintered in step (d), to provide a glass rod wherein the concentration of at least one compound selected from Tl 2 O, Rb 2 O, and Cs 2 O decreases parabolically from the center outward.
Claim 9
Dependent Claim 22 words
A process according to claim 1, wherein the acidic aqueous solution in step (b) is 3% aqueous H 2 SO 4 .

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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1988-07-08 1989-01-07 1989-07-09 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1992-07-08 1993-01-07 1993-07-09 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1996-07-08 1997-01-07 1997-07-09 $7700.00 Window Closed / Lapsed

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