Inorganic gels and ceramic papers, films, fibers, boards, and coatings made therefrom

A method for preparing inorganic films and fibers containing crystals consisting essentially of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, hydroxyl hectorite, boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions among those and between those and other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, which consists in the steps of:

• (a) forming a fully or predominantly crystalline body containing crystals consisting essentially of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, hydroxyl hectorite, boron fluorphlogopite, hydroxy boron phlogopite, and solid solutions among those and between those and other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite;
• (b) contacting said body with a polar liquid for a time sufficient to cause swelling and disintegration thereof accompanied with the formation of a gel;
• (c) adjusting the solid:liquid ratio of said gel to a desired fluidity;
• (d) preparing a fiber or film of said gel;
• and then
• (e) drying said fiber or film.

A method for preparing inorganic films and fibers containing crystals consisting essentially of an exchanged lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, hydroxyl hectorite, boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions among those and between those and other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, which consists in the steps of:

• (a) forming a fully or predominantly crystalline body containing crystals consisting essentially of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, hydroxyl hectorite, boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions among those and between those and other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite;
• (b) contacting said body with a polar liquid for a time sufficient to cause swelling and disintegration thereof accompanied with the formation of a gel;
• (c) adjusting the solid:liquid ratio of said gel to a desired fluidity;
• (d) preparing a fiber or film of said gel;
• (e) contacting said fiber or film with a source of large cations for a time sufficient to cause an ion exchange reaction to occur between said large cations and the Li.sup.+ and/or Na.sup.+ ions from the interlayer of said lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, hydroxyl hectorite, boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions among those and between those and other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite;
• and then
• (f) drying said fiber or film.

A method for preparing inorganic films and fibers containing crystals consisting essentially of an exchanged lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, boron fluorphlogopite, and solid solutions between those and between those and other structurally-compatible species, selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, which consists in the steps of:

• (a) melting a batch for a glass consisting essentially, expressed in weight percent on the oxide basis, of 0.5-12% Li.sub.2 O, 0-10% Na.sub.2 O, 0.5-14% Li.sub.2 O+Na.sub.2 O, 0-30% B.sub.2 O.sub.3, 10-38% MgO, 0-10% Al.sub.2 O.sub.3, 35-70% SiO.sub.2, and 5-15% F;
• (b) simultaneously cooling said melt to a temperature at least within the transformation range thereof and forming a glass body therefrom;
• (c) heat treating said glass body at a temperature between 700.degree.-1200.degree. C. for a time sufficient to cause the development of crystals therein of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, boron fluorphlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of fluortalc, fluorpolylithionite, and fluorphlogopite, said body being fully or predominantly crystalline;
• (d) contacting said body with a polar liquid for a time sufficient to cause swelling and disintegration thereof accompanied with the formation of a gel;
• (e) adjusting the solid:liquid ratio of said gel to a desired fluidity;
• (f) preparing a fiber or film of said gel;
• and then
• (g) drying said fiber or film.

A method for preparing inorganic films and fibers containing crystals consisting essentially of an exchanged lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, boron fluorphlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, which consists in the steps of:

• (a) melting a batch for a glass consisting essentially, expressed in weight percent on the oxide basis, of 0.5-12% Li.sub.2 O, 0-10% Na.sub.2 O, 0.5-14% Li.sub.2 O+Na.sub.2 O, 0-30% B.sub.2 O.sub.3, 10-38% MgO, 0-10% Al.sub.2 O.sub.3, 35-70% SiO.sub.2, and 5-15% F;
• (b) simultaneously cooling said melt to a temperature at least within the transformation range thereof and forming a glass body therefrom;
• (c) heat treating said glass body at a temperature between 700.degree.-1200.degree. C. for a time sufficient to cause the development of crystals therein of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, born fluorphlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of fluortalc, fluorpolylithionite, phlogopite, and fluorphlogopite, said body being fully or predominantly crystalline;
• (d) contacting said body with a polar liquid for a time sufficient to cause swelling and disintegration thereof accompanied with the formation of a gel;
• (e) adjusting the solid:liquid ratio of said gel to a desired fluidity;
• (f) preparing a fiber or film of said gel;
• (g) contacting said fiber or film with a source of large cations for a time sufficient to cause an ion exchange reaction to occur between said large cations and the Li.sup.+ and or Na.sup.+ ions from the interlayer of said crystals;
• and then
• (h) drying said fiber or film.

A method for preparing inorganic films and fibers containing crystals consisting essentially of an exchanged lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, boron fluorphlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, which consists in the steps of:

• (a) melting a batch for a glass consisting essentially, expressed in weight percent on the oxide basis, of 0.5-12% Li.sub.2 O and/or 0-10% Na.sub.2 O, 0.5-14% Li.sub.2 O+Na.sub.2 O, 0-30% B.sub.2 O.sub.3, 10-38% MgO, 0-10% Al.sub.2 O.sub.3, 35-70% SiO.sub.2, and 5-15% F;
• (b) simultaneously cooling said melt to a temperature between about 900.degree.-1050.degree. C. to shape the melt into a body and cause phase separation and nucleation to take place therein;
• (c) further cooling said body to a temperature between about 700.degree.-900.degree. C. and maintaining that temperature for a time sufficient to effect the development of crystals therein of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, boron fluorphlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of fluortalc, fluorpolylithionite, and fluorphlogopite, said body being fully or predominantly crystalline;
• (d) contacting said body with a polar liquid for a time sufficient to cause swelling said disintegration thereof accompanied with the formation of a gel;
• (e) adjusting the solid:liquid ratio of said gel to a desired fluidity;
• (f) preparing a fiber or film of said gel;
• and then
• (g) drying said fiber or film,

A method for preparing inorganic films and fibers containing crystals consisting essentially of an exchanged lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, boron fluorphlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of fluortalc, fluorpolylithionite, and fluorphlogopite, which consists in the steps of:

• (a) melting a batch for a glass consisting essentially, expressed in weight percent on the oxide basis, of 0.5-12% Li.sub.2 O and/or 0-10% Na.sub.2 O, 0.5-14% Li.sub.2 O+Na.sub.2 O, 0-30% B.sub.2 O.sub.3, 10-38% MgO, 0-10% Al.sub.2 O.sub.3, 35-70% SiO.sub.2, and 5-15% F;
• (B) simultaneously cooling said melt to a temperature between about 900.degree.-1050.degree. C. to shape the melt into a body and cause phase separation and nucleation to take place therein;
• (c) further cooling said body to a temperature between about 700.degree.-900.degree. C. and maintaining that temperature for a time sufficient to effect the development of crystals therein of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, boron fluorphlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of fluortalc, fluorpolylithionite, and fluorphlogopite, said body being fully or predominantly crystalline;
• (d) contacting said body with a polar liquid for a time sufficient to cause swelling and disintergration thereof accompanied with the formation of a gel;
• (e) adjusting the solid-liquid ratio of said gel to a desired fluidity;
• (f) preparing a fiber or film of said gel;
• (g) contacting said fiber or film with a source of large cations for a time sufficient to cause an ion exchange reaction to occur between said large cations and the Li.sup.+ and/or Na.sup.+ ions from the interlayer of said crystals;
• and then
• (h) drying said fiber or film.

A method for preparing inorganic films and fibers containing crystals consisting essentially of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, hydroxyl hectorite, boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions among those and between those and other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, which consists in the steps of:

• (a) melting a batch for a glass consisting essentially, expressed in weight percent on the oxide basis, of 0-9% Li.sub.2 O and/or 2-10% Na.sub.2 O, 2-14% Li.sub.2 O+Na.sub.2 O, 0-20% B.sub.2 O.sub.3, 0-10% Al.sub.2 O.sub.3, 15-38% MgO, 50-70% SiO.sub.2, and 0-12% F;
• (b) simultaneously cooling said melt to a temperature below the transformation range thereof and shaping a glass body therefrom;
• (c) exposing said glass body to a water-containing gaseous atmosphere having a relative humidity of at least 50% at a temperature between about 200.degree.-400.degree. C. for a time sufficient to cause the development of crystals therein of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, hydroxyl hectorite, boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions among those and between those and other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, said body being fully or predominantly crystalline;
• (d) contacting said body with a polar liquid for a time sufficient to cause swelling and disintegration thereof accompanied with the formation of a gel;
• (e) adjusting the solid:liquid ratio of said gel to a desired fluidity;
• (f) preparing a fiber or film of said gel;
• and then
• (g) drying said fiber or film.

A method for preparing inorganic films and fibers containing crystals consisting essentially of an exchanged lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, hydroxyl hectorite, boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions among those and between those and other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, which consists in the steps of:

• (a) melting a batch for a glass consisting essentially, expressed in weight percent on the oxide basis, of 0-9% Li.sub.2 O and/or 2-10% Na.sub.2 O, 2-14% Li.sub.2 O+Na.sub.2 O, 0-20% B.sub.2 O.sub.3, 0-10% Al.sub.2 O.sub.3, 15-38% MgO, 50-70% SiO.sub.2, and 0-12% F;
• (b) simultaneously cooling said melt to a temperature below the transformation range thereof and shaping a glass body therefrom;
• (c) exposing said glass body to a water-containing gaseous atmosphere having a relative humidity of at least 50% at a temperature between about 200.degree.-400.degree. C. for a time sufficient to cause the development of crystals therein of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, hydroxyl hectorite, boron fluorphlogopite, hydroxyl boron phlogopite, and solid solution among those and between those and other structurally compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, said body being fully or predominantly crystalline;
• (d) contacting said body with a polar liquid for a time sufficient to cause swelling and disintegration thereof accompanied with the formation of a gel;
• (e) adjusting the solid:liquid ratio of said gel to a desired fluidity;
• (f) preparing a fiber or film of said gel;
• (g) contacting said fiber or film with a source of large cations for a time sufficient to cause an ion exchange reaction to occur between said large cations and the Li.sup.+ and/or Na.sup.+ ions from the interlayer of said crystals;
• and then
• (i) drying said fiber or film.

A method for preparing inorganic films and fibers containing crystals consisting essentially of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, hydroxyl hectorite, boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions among those and between those and other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, which consists in the steps of:

• (a) melting a batch for a glass consisting essentially, expressed in weight percent on the oxide basis, of 0-9% Li.sub.2 O and/or 2-10% Na.sub.2 O, 2-14% Li.sub.2 O+Na.sub.2 O, 0-20% B.sub.2 O.sub.3, 0-10% Al.sub.2 O.sub.3, 15-38% MgO, 50-70% SiO.sub.2, and 0-12% F;
• (b) simultaneously cooling said melt to a temperature at least within the transformation range thereof and forming a glass body therefrom;
• (c) heat treating said glass body to a temperature between 700.degree.-1200.degree. C. for a time sufficient to cause the development of crystals therein selected from the group of magnesium metasilicate, lithium disilicate, sodium magnesium silicate, and silica, where said composition is essentially free from fluoride, and/or of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, boron fluorphlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of fluortalc, fluorpolylithionite, and fluorphlogopite, where said composition contains significant fluoride, said body being fully or predominantly crystalline;
• (d) exposing said body to a water-containing gaseous atmosphere having a relative humidity of at least 50% at a temperature between about 200.degree.-400.degree. C. for a time sufficient to partially or totally convert the said crystals of magnesium metasilicate, lithium disilicate, sodium magnesium silicate, and silica into structures selected from the group of hydroxyl hectorite, hydroxyl boron phlogopite and solid solutions between those, and/or to partially or totally convert the said fluoride-containing crystals into the hydroxyl equivalents thereof;
• (e) contacting said body with a polar liquid for a time sufficient to cause swelling and disintegration thereof accompanied with the formation of a gel;
• (f) adjusting the solid:liquid ratio of said gel to a desired fluidity;
• (g) preparing a fiber or film of said gel;
• and then
• (h) drying said fiber of film.

A method for preparing inorganic films and fibers containing crystals consisting essentially of an exchanged lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, hydroxyl hectorite, boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions among those and between those and other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, which consists in the steps of:

• (a) melting a batch for a glass consisting essentially, expressed in weight percent on the oxide basis, of 0-9% Li.sub.2 O and/or 2-10% Na.sub.2 O, 2-14% Li.sub.2 O+Na.sub.2 O, 0-20% B.sub.2 O.sub.3, 0-10% Al.sub.2 O.sub.3, 15-38% MgO, 50-70% SiO.sub.2, and 0-12% F;
• (b) simultaneously cooling said melt to a temperature at least within the transformation range thereof and forming a glass body therefrom;
• (c) heat treating said glass body to a temperature between 700.degree.-1200.degree. C. for a time sufficient to cause the development of crystals therein selected from the group of magnesium metasilicate, lithium disilicate, sodium magnesium silicate, and silica, where said composition is essentially free from fluoride and/or of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, boron fluorphlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of fluortalc, fluorpolylithionite, and fluorphlogopite, where said composition contains significant fluoride, said body being fully or predominantly crystalline;
• (d) exposing said body to a water-containing gaseous atmosphere having a relative humidity of at least 50% at a temperature between about 200.degree.-400.degree. C. for a time sufficient to partially or totally convert the said crystals of magnesium metasilicate, lithium disilicate, sodium magnesium silicate, and silica into structures selected from the group of hydroxyl hectorite, hydroxyl boron phlogopite, and solid solutions between those, and/or to partially or totally convert the said fluoride-containing crystals into the hydroxyl equivalents thereof;
• (e) contacting said body with a polar liquid for a time sufficient to cause swelling and disintegration thereof accompanied with the formation of a gel;
• (f) adjusting the solid:liquid ratio of said gel to a desired fluidity;
• (g) preparing a fiber or film of said gel;
• (h) contacting said fiber or film with a source of large cations for a time sufficient to cause an ion exchange reaction to occur between said large cations and the Li.sup.+ and/or Na.sup.+ ions from the interlayer of said crystals;
• and then
• (i) drying said fiber of film.

A method for preparing inorganic films and fibers containing crystals consisting essentially of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, hydroxyl hectorite, boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions among those and between those and other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, which consists in the steps of:

• (a) melting a batch for a glass consisting essentially, expressed in weight percent on the oxide basis, of 0-9% Li.sub.2 O and/or 2-10% Na.sub.2 O, 2-14% Li.sub.2 O+Na.sub.2 O, 0-20% B.sub.2 O.sub.3, 0-10% Al.sub.2 O.sub.3, 15-38% MgO, 50-70% SiO.sub.2, and 0-12% F;
• (b) simultaneously cooling said melt to a temperature between about 900.degree.-1050.degree. C. to shape the melt into a body to cause phase separation and nucleation to take place therein;
• (c) further cooling said body to a temperature between about 700.degree.-900.degree. C. and maintaining that temperature for a time sufficient to effect the development of crystals therein selected from the group of magnesium metasilicate, lithium disilicate, sodium magnesium silicate, and silica, where said composition is essentially free from fluoride, and/or of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, boron fluorphlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of fluortalc, fluorpolylithionite, and fluorophlogopite, where said composition contains significant fluoride, said body being fully or predominantly crystalline;
• (d) exposing said body to a water-containing gaseous atmosphere having a relative humidity of at least 50% at a temperature between about 200.degree.-400.degree. C. for a time sufficient to either partially or totally convert the said crystals of magnesium metasilicate, lithium disilicate, sodium magnesium silicate, and silica into structures selected from the group of hydroxyl hectorite, hydroxyl boron phlogopite, and solid solutions between those, and/or to partially or totally convert the said fluoride-containing crystals into the hydroxyl equivalents thereof;
• (e) contacting said body with a polar liquid for a time sufficient to cause swelling and disintegration thereof accompanied with the formation of a gel;
• (f) adjusting the solid:liquid ratio of said gel to a desired fluidity;
• (g) preparing a fiber or film of said gel;
• and then
• (h) drying said fiber or film.

A method for preparing coatings containing crystals consisting essentially of an exchanged lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, hydroxyl hectorite, boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions among those and between those and other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, which consists in the steps of:

• (a) melting a batch for a glass consisting essentially, expressed in weight percent on the oxide basis, of 0-9% Li.sub.2 O and/or 2-10% Na.sub.2 O, 2-14% Li.sub.2 O+Na.sub.2 O, 0-20% B.sub.2 O.sub.3, 0-10% Al.sub.2 O.sub.3, 15-38% MgO, 50-70% SiO.sub.2, and 0-12% F;
• (b) simultaneously cooling said melt to a temperature below the transformation range thereof and shaping a glass body therefrom;
• (c) exposing said glass body to a water-containing gaseous atmosphere having a relative humidity of at least 50% at a temperature between about 200.degree.-400.degree. C. for a time sufficient to cause the development of crystals therein of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, hydroxyl hectorite, boron fluorphlogopite, hydroxyl boron hectorite, and solid solutions among those and between those and other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite;
• (d) contacting said body with a polar liquid for a time sufficient to cause swelling and disintegration thereof accompanied with the formation of a gel;
• (e) adjusting the solid:liquid ratio of said gel to a desired fluidity;
• (f) preparing a film of said gel;
• and then
• (g) contacting said film with a source of large cations for a time sufficient to cause an ion exchange reaction to occur between said large cations and the Li.sup.+ and/or Na.sup.+ ions from the interlayer of said crystals.

A method for preparing coatings containing crystals consisting essentially of an exchanged lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, hydroxyl hectorite, boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions among those and between those and other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, which consists in the steps of:

• (a) melting a batch for a glass consisting essentially, expressed in weight percent on the oxide basis, of 0-9% Li.sub.2 O and/or 2-10% Na.sub.2 O, 2-14% Li.sub.2 O+Na.sub.2 O, 0-20% B.sub.2 O.sub.3, 0-10% Al.sub.2 O.sub.3, 15-38% MgO, 50-70% SiO.sub.2, and 0-12% F;
• (b) simultaneously cooling said melt to a temperature below the transformation range thereof and shaping a glass body therefrom;
• (c) heat treating said glass body to a temperature between 700.degree.-1200.degree. C. for a time sufficient to cause the development of crystals therein selected from the group of magnesium silicate, lithium disilicate, and sodium magnesium silicate, and silica, where said glass is essentially free from fluoride, and/or of a lithium and/or sodium water-swelling mica selected from the group of fluorhectorite, boron fluorphlogopite, and solid solutions among those and between those and other structurally-compatible species selected from the group of fluortalc, fluorpolylithionite, and fluorphlogopite, where said glass contains significant fluoride, said body being fully or predominantly crystalline;
• (d) exposing said body to a water-containing gaseous atmosphere having a relative humidity of at least 50% at a temperature between about 200.degree.-400.degree. C. for a time sufficient to partially or totally convert the crystals of magnesium metasilicate, lithium disilicate, sodium magnesium silicate, and silica into structures selected from the group of hydroxyl hectorite, hydroxyl boron phlogopite, and solid solutions between those, and/or to partially or totally convert said fluoride-containing crystals into the hydroxyl equivalents thereof;
• (e) contacting said body with a polar liquid for a time sufficient to cause swelling and disintegration thereof accompanied with the formation of a gel;
• (f) adjusting the solid:liquid ratio of said gel to a desired fluidity;
• (g) preparing a film of said gel;
• and then
• (h) contacting said film with a source of large cations for a time sufficient to cause an ion exchange reaction to occur between said large cations and the Li.sup.+ and/or Na.sup.+ ions from the interlayer of said crystals.