# US 11,078,114 B2 · Method for treating vitreous materials by thermal poling > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 11,078,114 B2 - Document ID: US11078114B2 - Status: Granted - Kind: B2 - Application number: 15/774,814 - Filed: 2016-11-08 - Published: 2018-11-15 - Granted: 2021-08-03 - Earliest claimed: 2015-11-10 - Assignees: Centre National De La Recherche Scientifique - Applicants: Centre national de la recherche scientifique - Inventors: Maxime Paraillous; Thierry Cardinal; Angeline Poulon; Evelyne Fargin; Marc Dussauze - Web page: https://patentgrep.com/patent/US11078114B2 ## CPC - C03C 23/009: {Poling glass} - C03C 3/087: containing calcium oxide, e.g. common sheet or container glass - C03C 3/111: {containing nitrogen} - C03C 21/007: {in gaseous phase} - C03C: CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS ## Abstract The invention relates to a method for treating a silicate-type glass comprising alkali and alkaline-earth metal oxides or d10 or IIIA metal oxides, said method comprising at least the following steps: (a) incorporation of nitrogen into the surface of the glass; and (b) thermal poling treatment of the material obtained in (a), under a chemically inert controlled atmosphere. The invention also relates to the material produced by said method. ## Claims ### Claim 1 A method for treating a silicate-type glass comprising alkali and alkaline earth metal oxides or IIIA metal oxides, said method comprising: (a) incorporating nitrogen into a surface of the silicate-type glass whereby a material comprising nitrogen is obtained, and (b) thermal poling treatment of the material comprising nitrogen from (a) under a chemically inert controlled atmosphere, wherein the material comprising nitrogen is placed between an anode and a cathode without direct contact between the material comprising nitrogen and the anode. ### Claim 2 (depends on 1) The method according to claim 1, wherein (a) comprises a thermal treatment of the silicate-type glass at a temperature greater than or equal to 150° C. in a nitrogen-controlled atmosphere. ### Claim 3 (depends on 2) The method according to claim 2, wherein the temperature is 200° C. to 500° C. in (a). ### Claim 4 (depends on 2) The method according to claim 2, wherein in (a) the atmosphere comprises a gas selected from the group consisting of N2 and NH3. ### Claim 5 (depends on 2) The method according to claim 2, wherein in (a) the atmosphere comprises nitrogen N2, or a mixture of nitrogen and an inert gas selected from the group consisting of Ar and He. ### Claim 6 (depends on 1) The method according to claim 1, wherein in (b) the material comprising nitrogen is maintained at a temperature ranging from 150 to 500° C. and exposed to an electric field having a voltage of 0.1 to 10 kV. ### Claim 7 (depends on 1) The method according to claim 1, wherein in (b), the controlled atmosphere consists essentially of a gas selected from the group consisting of dry air, O2, N2, Ar, He, and a mixture of two or more of these gases. ### Claim 8 (depends on 7) The method according to claim 7, wherein in (b) the controlled atmosphere consists essentially of N2 nitrogen. ### Claim 9 (depends on 6) The method according to claim 6, wherein in (b) the material comprising nitrogen is maintained at a temperature of from 200 to 300° C. ### Claim 10 (depends on 1) The method according to claim 1, wherein the silicate-type glass has a mass composition of 0 to 40% Al2O3; 50 to 97% SiO2; 0 to 15% B2O3; 0 to 25% ZnO; 0% to 5% ZrO2; 0 to 10% TiO2; 0 to 40% Na2O; 0 to 40% Li2O; 0 to 40% K2O; 0 to 40% MgO; 0 to 50% CaO; 0 to 40% SrO; 0 to 40% BaO; 0 to 15% Ag2O; 0 to 15% Au2O3, Au2O; 0 to 15% Cu2O, and at least 95% by weight of the components, relative to the total mass of the glass, that are selected from the group consisting of Al2O3; SiO2; B2O3; ZnO; ZrO2; TiO2; Na2O; Li2O; K2O; MgO; CaO; SrO; BaO; Ag2O; Au2O3; Au2O; and Cu2O. ### Claim 11 (depends on 1) The method according to claim 1, wherein the silicate-type glass used is a glass of the composition, defined in % by mass, of from 60 to 74% of SiO2, 8.2 to 16.4% of Na2O, 3.2 to 7.40% CaO, 2.8 to 4.30% MgO, 0.3 to 1.20% Al2O3, 0.3 to 1.20% K2O and 0.1 to 0.30% SO3. ### Claim 12 A method for improving durability of glazing of a silicate-type glass comprising alkali and alkaline earth metal oxides or IIIA metal oxides; or improving scratch resistance of a digital/tactile screen comprising alkali and alkaline earth metal oxides or IIIA metal oxides; or increasing resistance to abrasion of a mirror comprising alkali and alkaline earth metal oxides or IIIA metal oxides; said method comprising: (a) incorporating nitrogen into a surface of the silicate-type glass whereby a material comprising nitrogen is obtained, and (b) thermal poling treatment of the material comprising nitrogen from (a) under a chemically inert controlled atmosphere, wherein the material comprising nitrogen is placed between an anode and a cathode without direct contact between the material comprising nitrogen and the anode. ### Claim 13 A method of manufacturing: a building glazing comprising a silicate-type glass comprising alkali and alkaline earth metal oxides or IIIA metal oxides; or a solar panel mirror comprising a silicate-type glass comprising alkali and alkaline earth metal oxides or IIIA metal oxides; or a screen for electronic devices comprising a silicate-type glass comprising alkali and alkaline earth metal oxides or IIIA metal oxides; or a fiberglass comprising a silicate: type glass comprising alkali and alkaline earth metal oxides or IIIA metal oxides; said method comprising: (a) incorporating nitrogen into a surface of the silicate-type glass whereby a material comprising nitrogen is obtained, and (b) thermal poling treatment of the material comprising nitrogen from (a) under a chemically inert controlled atmosphere, wherein the material comprising nitrogen is placed between an anode and a cathode without direct contact between the material comprising nitrogen and the anode.