US4239519A — Inorganic gels and ceramic papers, films, fibers,…

Claim 1

Independent Claim 420 words

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 2 O and/or 2-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 0-20% B 2 O 3 , 0-10% Al 2 O 3 , 15-38% MgO, 50-70% SiO 2 , and 0-12% F; (b) simultaneously cooling said melt to a temperature between about 900°-1050° 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°-900° 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 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°-400° 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; (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 + and/or Na + ions from the interlayer of said crystals; and then (i) drying said fiber or film.

Claim 2

Independent Claim 420 words

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 2 O and/or 2-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 0-20% B 2 O 3 , 0-10% Al 2 O 3 , 15-38% MgO, 50-70% SiO 2 , and 0-12% F; (b) simultaneously cooling said melt to a temperature between about 900°-1050° 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°-900° 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 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°-400° 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; (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 + and/or Na + ions from the interlayer of said crystals; and then (i) drying said fiber or film.

Claim 3

Dependent Claim 65 words

A method according to claim 1 wherein said glass also contains up to 20% by weight total of oxides selected from the group of 0-10% CaO, 0-10% CdO, 0-10% CoO, 0-10% CuO, 0-20% Fe 2 O 3 , 0-20% FeO, 0-10% MnO, 0-10% NiO, 0-20% PbO, 0-10% P 2 O 5 , 0-20% SrO, 0-10% TiO 2 , 0-20% ZnO, and 0-10% ZrO 2 .

Claim 4

Dependent Claim 26 words

A method according to claim 1 wherein said fully or predominantly crystalline body consists essentially of fluoride-containing crystals and said glass contains at least 5% F.

Claim 5

Dependent Claim 50 words

A method according to claim 1 wherein said glass consists essentially, expressed in weight percent on the oxide basis, of 0-6% Li 2 O and/or 2-8% Na 2 O, 2-14% Li 2 O+Na 2 O, 20-30% MgO, 0-15% B 2 O 3 , 60-70% SiO 2 , and 0-6% F.

Claim 6

Dependent Claim 24 words

A method according to claim 1 wherein said time sufficient to cause phase separation and nucleation ranges between a few seconds to a minute.

Claim 7

Dependent Claim 24 words

A method according to claim 1 wherein said time sufficient to effect the development of crystals ranges between about 2 minutes to several hours.

Claim 8

Dependent Claim 19 words

A method according to claim 1 wherein the time sufficient to convert said crystals ranges between about 0.5-48 hours.

Claim 9

Dependent Claim 12 words

A method according to claim 1 wherein said polar liquid is water.

Claim 10

Dependent Claim 21 words

A method according to claim 1 wherein said time sufficient to cause swelling, disintegration, and gelation ranges between about 1-48 hours.

Claim 11

Dependent Claim 22 words

A method according to claim 1 wherein the viscosity of said gel is adjusted by adding a deflocculating or peptizing agent thereto.

Claim 12

Dependent Claim 18 words

A method according to claim 1 wherein said solid: liquid ratio ranges between about 1-50% by weight solids.

Claim 13

Dependent Claim 17 words

A method according to claim 11 wherein said solid: liquid ratio ranges between about 2-25% by weight.

Claim 14

Dependent Claim 27 words

A method according to claim 1 wherein said solid: liquid ratio ranges up to 80% by weight solids and a fiber is prepared via high pressure extrusion.

Claim 15

Dependent Claim 23 words

A method according to claim 1 wherein said film is prepared by casting said gel onto the surface of an inert, impermeable substrate.

Claim 16

Dependent Claim 17 words

A method according to claim 1 wherein said source of large cations is an aqueous salt solution.

Claim 17

Dependent Claim 49 words

A method according to claim 1 wherein said large cations are selected from the group of K + , Rb + , Cs + , NH 4 + , H 3 O + , Ca +2 , Sr +2 , Ba +2 , Pb +2 , and organic polycations.

Claim 18

Dependent Claim 19 words

A method according to claim 1 wherein successive films are prepared and dried in superjacent relationship to form board.

Claim 19

Dependent Claim 36 words

A method according to claim 1 wherein inert fillers are included with said fully or predominantly crystalline body in the gelation step in an amount to constitute up to 75% by volume of the final product.

Claim 20

Dependent Claim 53 words

A method according to claim 1 wherein said fiber or film is prepared by contacting said gel having the desired fluidity with a flocculating agent to form a skin or membrane at the interface therebetween and thereafter drawing off said skin or membrane to renew the contact between said gel and flocculating agent.

Claim 21

Dependent Claim 28 words

A method according to claim 19 wherein said contact between said gel and flocculating agent is made by floating a liquid containing said flocculating agent over said gel.

Claim 22

Dependent Claim 32 words

A method according to claim 19 wherein said contact between said gel and flocculating agent is made by spraying a mist of a flocculating agent-containing liquid onto the surface of the gel.

Claim 23

Dependent Claim 26 words

A method according to claim 19 wherein said contact between said gel and flocculating agent is made by extruding said gel into a flocculating agent-containing liquid.

Claim 24

Dependent Claim 47 words

A method for forming a fiber according to claim 19 wherein said contact between said gel and flocculating agent is made by injecting said gel as a thin stream into a flocculating agent-containing liquid and, thereafter, pulling a continuous fiber or group of fibers from said liquid.

Claim 25

Dependent Claim 18 words

A method according to claim 1 wherein said flocculating agent is an aqueous salt solution of large cations.

Claim 26

Dependent Claim 49 words

A method according to claim 24 where said large cations are selected from the group of K + , Rb + , Cs + , NH 4 + , H 3 O + , Ca +2 , Sr +2 , Ba +2 , Pb +2 , and organic polycations.

Claim 27

Dependent Claim 69 words

A method according to claim 11 wherein said exchanged lithium and/or sodium water-swelling mica is a potassium mica which has a composition, expressed in weight percent on the oxide basis, of about 3-17% K 2 O, 0-8% Li 2 O, 0-5% Na 2 O, 15-38% MgO, 0-30% B 2 O 3 , 0-10% Al 2 O 3 , 50-70% SiO 2 , 0-12% F, 0-12% OH, and 4-12% F+OH.

Claim 28

Dependent Claim 111 words

A method according to claim 11 wherein said lithium and/or sodium water-swelling mica is basically a trisilicic mica selected from the group of boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of hydroxyl hectorite, fluorhectorite, talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite and wherein said exchanged lithium and/or sodium trisilicic mica is a potassium mica which has a composition of about 3-16% K 2 O, 0-4% Li 2 O, 0-5% Na 2 O, 20-38% MgO, 2-10% B 2 O 3 , 0-10% Al 2 O 3 , 35-56% SiO 2 , 0-12% F, 0-12% OH, and 4-12% F+OH.

Claim 29

Independent Claim 172 words

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.

Claim 30

Independent Claim 172 words

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.

Claim 31

Dependent Claim 12 words

A method according to claim 28 wherein said polar liquid is water.

Claim 32

Dependent Claim 21 words

A method according to claim 28 wherein said time sufficient to effect swelling, disintegration, and gelation ranges between about 1-48 hours.

Claim 33

Dependent Claim 22 words

A method according to claim 28 wherein the viscosity of said gel is adjusted by adding a deflocculating or peptizing agent thereto.

Claim 34

Dependent Claim 17 words

A method according to claim 28 wherein said solid:liquid ratio ranges between about 1-50% by weight solids.

Claim 35

Dependent Claim 17 words

A method according to claim 32 wherein said solid:liquid ratio ranges between about 2-25% by weight solids.

Claim 36

Dependent Claim 63 words

A method according to claim 28 wherein said fully or predominantly crystalline body consists essentially, expressed in weight percent on the oxide basis, of 0-12% Li 2 O, 0-10% Na 2 O, 0.5-14% Li 2 O+Na 2 O, 10-38% MgO, 0-30% B 2 O 3 , 0-10% Al 2 O 3 , 35-70% SiO 2 , 0-15% F, 0-15% OH, and 4-15% F+OH.

Claim 37

Dependent Claim 67 words

A method according to claim 34 wherein said fully or predominantly crystalline body also contains up to 30% by weight total of oxides selected from the group of 0-10% CaO, 0-10% CdO, 0-10% CoO, 0-20% FeO, 0-20% Fe 2 O 3 , 0-10% MnO, 0-10% NiO, 0-10% P 2 O 5 , 0-30% PbO, 0-20% SrO, 0-10% TiO 2 , 0-25% ZnO, and 0-10% ZrO 2 .

Claim 38

Dependent Claim 65 words

A method according to claim 34 wherein said fully or predominantly crystalline body consists essentially 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 hydroxyl hectorite, hydroxyl boron phlogopite, talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, and contains at least 5% F.

Claim 39

Dependent Claim 113 words

A method according to claim 28 wherein said lithium and/or sodium water-swelling mica is basically a trisilicic mica selected from the group of boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of fluorhectorite, hydroxyl hectorite, talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, consisting essentially, expressed in weight percent on the oxide basis, of 0-6% Li 2 O, 0-9% Na 2 O, 0.5-10% Li 2 O, 20-38% MgO, 2-10% B 2 O 3 , 0-10% Al 2 O 3 , 4-12% Al 2 O 3 +B 2 O 3 , 35-56% SiO 2 , 0-12% F, 0-12% OH, and 4-12% F+OH.

Claim 40

Independent Claim 63 words

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:

Claim 41

Independent Claim 63 words

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:

Claim 42

Dependent Claim 193 words

(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 + and/or Na + 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.

Claim 43

Dependent Claim 193 words

(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 + and/or Na + 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.

Claim 44

Dependent Claim 12 words

A method according to claim 38 wherein said polar liquid is water.

Claim 45

Dependent Claim 21 words

A method according to claim 38 wherein said time sufficient to effect swelling, disintegration, and gelation ranges between about 1-48 hours.

Claim 46

Dependent Claim 22 words

A method according to claim 38 wherein the viscosity of said gel is adjusted by adding a deflocculating or peptizing agent thereto.

Claim 47

Dependent Claim 17 words

A method according to claim 38 wherein said solid:liquid ratio ranges between about 1-50% by weight solids.

Claim 48

Dependent Claim 17 words

A method according to claim 42 wherein said solid:liquid ratio ranges between about 2-25% by weight solids.

Claim 49

Dependent Claim 27 words

A method according to claim 38 wherein said solid:liquid ratio ranges up to about 80% by weight solids and a fiber is prepared via high pressure extrusion.

Claim 50

Dependent Claim 23 words

A method according to claim 38 wherein said film is prepared by casting said gel onto the surface of an inert, impermeable substrate.

Claim 51

Dependent Claim 17 words

A method according to claim 38 wherein said source of large cations is an aqueous salt solution.

Claim 52

Dependent Claim 44 words

A method according to claim 38 wherein said large cations are selected from the group of K + , Rb + , Cs + , NH 4 + , Ca +2 , Sr +2 , Ba +2 , Pb +2 , and organic polycations.

Claim 53

Dependent Claim 63 words

A method according to claim 38 wherein said fully or predominantly crystalline body consists essentially, expressed in weight percent on the oxide basis, of 0-12% Li 2 O, 0-10% Na 2 O, 0.5-14% Li 2 O+Na 2 O, 10-38% MgO, 0-30% B 2 O 3 , 0-10% Al 2 O 3 , 35-70% SiO 2 , 0-15% F, 0-15% OH, and 4-15% F+OH.

Claim 54

Dependent Claim 69 words

A method according to claim 48 wherein said fully or predominantly crystalline body also contains up to 30% by weight total of oxides selected from the group of 0-10% CaO, 0-10% CdO, 0-10% CoO, 0-10% CuO, 0-20% FeO, 0-20% Fe 2 O 3 , 0-10% MnO, 0-10% NiO, 0-10% P 2 O 5 , 0-30% PbO, 0-20% SrO, 0-10% TiO 2 , 0-25% ZnO, and 0-10% ZrO 2 .

Claim 55

Dependent Claim 66 words

A method according to claim 38 wherein said fiber or film consists essentially of crystals 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 hydroxyl hectorite, hydroxyl boron phlogopite, talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, and contains at least 5% F.

Claim 56

Dependent Claim 69 words

A method according to claim 38 wherein said exchanged lithium and/or sodium water-swelling mica is a potassium mica which has a composition, expressed in weight percent on the oxide basis, of about 3-17% K 2 O, 0-8% Li 2 O, 0-5% Na 2 O, 10-38% MgO, 0-30% B 2 O 3 , 0-10% Al 2 O 3 , 35-70% SiO 2 , 0-15% F, 0-15% OH, and 4-15% F+OH.

Claim 57

Dependent Claim 119 words

A method according to claim 38 wherein said lithium and/or sodium water-swelling mica is basically a trisilicic mica selected from the group of boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of fluorhectorite, hydroxyl hectorite, talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite and wherein said exchanged lithium and/or sodium trisilicis mica is a potassium mica which has a composition, expressed in weight percent on the oxide basis, of about 3-16% K 2 O, 0-4% Li 2 O, 0-5% Na 2 O, 20-38% MgO, 2-10% B 2 O 3 , 0-10% Al 2 O 3 , 35-56% SiO 2 , 0-12% F, 0-12% OH, and 4-12% F+OH.

Claim 58

Dependent Claim 19 words

A method according to claim 38 wherein successive films are prepared and dried in superjacent relationship to form board.

Claim 59

Dependent Claim 36 words

A method according to claim 38 wherein inert fillers are included with said fully or predominantly crystalline body in the gelation step in an amount to constitute up to 75% by volume of the final product.

Claim 60

Dependent Claim 53 words

A method according to claim 38 wherein said fiber or film is prepared by contacting said gel having the desired fluidity with a flocculating agent to form a skin or membrane at the interface therebetween and thereafter drawing off said skin or membrane to renew the contact between said gel and flocculating agent.

Claim 61

Dependent Claim 28 words

A method according to claim 55 wherein said contact between said gel and flocculating agent is made by floating a liquid containing said flocculating agent over said gel.

Claim 62

Dependent Claim 32 words

A method according to claim 55 wherein said contact between said gel and flocculating agent is made by spraying a mist of a flocculating agent-containing liquid onto the surface of the gel.

Claim 63

Dependent Claim 25 words

A method according to claim 55 wherein said contact between said gel and flocculating agent is made by extruding said gel into a flocculating-containing liquid.

Claim 64

Dependent Claim 47 words

A method for forming a fiber according to claim 55 wherein said contact between said gel and flocculating agent is made by injecting said gel as a thin stream into a flocculating agent-containing liquid and, thereafter, pulling a continuous fiber or group of fibers from said liquid.

Claim 65

Dependent Claim 18 words

A method according to claim 55 wherein said flocculating agent is an aqueous salt solution of large cations.

Claim 66

Dependent Claim 49 words

A method according to claim 60 wherein said large cations are selected from the group of K + , Rb + , Cs + , NH 4 + , H 3 O + , Ca +2 , Sr +2 , Ba +2 , Pb +2 , and organic polycations.

Claim 67

Independent Claim 252 words

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 2 O, 0-10% Na 2 O, 0.5-14% Li 2 O+Na 2 O, 0-30% B 2 O 3 , 10-38% MgO, 0-10% Al 2 O 3 , 35-70% SiO 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°-1200° 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.

Claim 68

Independent Claim 252 words

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 2 O, 0-10% Na 2 O, 0.5-14% Li 2 O+Na 2 O, 0-30% B 2 O 3 , 10-38% MgO, 0-10% Al 2 O 3 , 35-70% SiO 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°-1200° 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.

Claim 69

Dependent Claim 62 words

A method according to claim 62 wherein said batch also contains up to 30% total of oxides selected from the group 0-10% CaO, 0-10% CdO, 0-10% CoO, 0-10% CuO, 0-20% FeO, 0-20% Fe 2 O 3 , 0-10% MnO, 0-10% NiO, 0-10% P 1 O 5 , 0-30% PbO, 0-20% SrO, 0-10% TiO 2 , 0-25% ZnO, and 0-10% ZrO 2 .

Claim 70

Dependent Claim 49 words

A method according to claim 62 wherein said batch consists essentially, expressed in weight percent on the oxide basis, of 2-10% Li 2 O, 0-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 18-32% MgO, 50-70% SiO 2 , 0-10% B 2 O 3 , and 7-12% F.

Claim 71

Dependent Claim 24 words

A method according to claim 62 wherein said time sufficient to cause the development of crystals ranges between about 3 minutes to 8 hours.

Claim 72

Dependent Claim 12 words

A method according to claim 62 wherein said polar liquid is water.

Claim 73

Dependent Claim 21 words

A method according to claim 62 wherein said time sufficient to effect swelling, disintegration, and gelation ranges between about 1-48 hours.

Claim 74

Dependent Claim 22 words

A method according to claim 62 wherein the viscosity of said gel is adjusted by adding a deflocculating or peptizing agent thereto.

Claim 75

Dependent Claim 17 words

A method according to claim 62 wherein said solid:liquid ratio ranges between about 1-50% by weight solids.

Claim 76

Dependent Claim 17 words

A method according to claim 69 wherein said solid:liquid ratio ranges between about 2-25% by weight solids.

Claim 77

Dependent Claim 96 words

A method according to claim 62 wherein said lithium and/or sodium water-swelling mica is basically a trisilicic mica, i.e., boron fluorphlogopite and solid solutions between that and other structurally-compatible species selected from the group of fluorhectorite, fluortalc, fluorpolylithionite, and fluorphlogopite, consisting essentially, expressed in weight percent on the oxide basis, of 0-6% Li 2 O, 0-9% Na 2 O, 0.5-10% Li 2 O+Na 2 O, 20-38% MgO, 2-10% B 2 O 3 , 0-10% Al 2 O 3 , 4-12% Al 2 O 3 +B 2 O 3 , 35-56% SiO 2 , and 4-12% F.

Claim 78

Independent Claim 290 words

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 2 O, 0-10% Na 2 O, 0.5-14% Li 2 O+Na 2 O, 0-30% B 2 O 3 , 10-38% MgO, 0-10% Al 2 O 3 , 35-70% SiO 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°-1200° 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 + and or Na + ions from the interlayer of said crystals; and then

Claim 79

Independent Claim 290 words

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 2 O, 0-10% Na 2 O, 0.5-14% Li 2 O+Na 2 O, 0-30% B 2 O 3 , 10-38% MgO, 0-10% Al 2 O 3 , 35-70% SiO 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°-1200° 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 + and or Na + ions from the interlayer of said crystals; and then

Claim 80

Dependent Claim 6 words

(h) drying said fiber or film.

Claim 81

Dependent Claim 6 words

(h) drying said fiber or film.

Claim 82

Dependent Claim 62 words

A method according to claim 72 wherein said batch also contains up to 30% total of oxides selected from the group 0-10% CaO, 0-10% CdO, 0-10% CoO, 0-10% CuO, 0-20% FeO, 0-20% Fe 2 O 3 , 0-10% MnO, 0-10% NiO, 0-10% P 2 O 5 , 0-30% PbO, 0-20% SrO, 0-10% TiO 2 , 0-25% ZnO, and 0-10% ZrO 2 .

Claim 83

Dependent Claim 49 words

A method according to claim 72 wherein said batch consists essentially, expressed in weight percent on the oxide basis, of 2-10% Li 2 O, 0-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 18-32% MgO, 50-70% SiO 2 , 0-10% B 2 O 3 , and 7-12% F.

Claim 84

Dependent Claim 24 words

A method according to claim 72 wherein said time sufficient to cause the development of crystals ranges between about 3 minutes to 8 hours.

Claim 85

Dependent Claim 12 words

A method according to claim 72 wherein said polar liquid is water.

Claim 86

Dependent Claim 21 words

A method according to claim 72 wherein said time sufficient to effect swelling, disintegration, and gelation ranges between about 1-48 hours.

Claim 87

Dependent Claim 22 words

A method according to claim 72 wherein the viscosity of said gel is adjusted by adding a deflocculating or peptizing agent thereto.

Claim 88

Dependent Claim 17 words

A method according to claim 72 wherein said solid:liquid ratio ranges between about 1-50% by weight solids.

Claim 89

Dependent Claim 17 words

A method according to claim 79 wherein said solid:liquid ratio ranges between about 2-25% by weight solids.

Claim 90

Dependent Claim 27 words

A method according to claim 72 wherein said solid:liquid ratio ranges up to about 80% by weight solids and a fiber is prepared via high pressure extrusion.

Claim 91

Dependent Claim 17 words

A method according to claim 72 wherein said source of large cations is an aqueous salt solution.

Claim 92

Dependent Claim 49 words

A method according to claim 72 wherein said large cations are selected from the group of K + , Rb + , Cs + , NH 4 + , H 3 O + , Ca +2 , Sr +2 , Ba +2 , Pb +2 , and organic polycations.

Claim 93

Dependent Claim 19 words

A method according to claim 72 wherein successive films are prepared and dried in superjacent relationship to form board.

Claim 94

Dependent Claim 36 words

A method according to claim 72 wherein inert fillers are included with said fully or predominantly crystalline body in the gelation step in an amount to constitute up to 75% by volume of the final product.

Claim 95

Dependent Claim 53 words

A method according to claim 72 wherein said fiber or film is prepared by contacting said gel having the desired fluidity with a flocculating agent to form a skin or membrane at the interface therebetween and thereafter drawing off said skin or membrane to renew the contact between said gel and flocculating agent.

Claim 96

Dependent Claim 27 words

A method according to claim 86 wherein said contact between said gel and flocculating agent is made by floating a liquid-containing said flocculating agent over said gel.

Claim 97

Dependent Claim 32 words

A method according to claim 86 wherein said contact between said gel and flocculating agent is made by spraying a mist of a flocculating agent-containing liquid onto the surface of the gel.

Claim 98

Dependent Claim 26 words

A method according to claim 86 wherein said contact between said gel and flocculating agent is made by extruding said gel into a flocculating agent-containing liquid.

Claim 99

Dependent Claim 47 words

A method for forming a fiber according to claim 86 wherein said contact between said gel and flocculating agent is made by injecting said gel as a thin stream into a flocculating agent-containing liquid and, thereafter, pulling a continuous fiber or group of fibers from said liquid.

Claim 100

Dependent Claim 18 words

A method according to claim 86 wherein said flocculating agent is an aqueous salt solution of large cations.

Claim 101

Dependent Claim 44 words

A method according to claim 91 wherein said large cations are selected from the group of K + , Rb + , Cs + , NH 4 + , H 3 O + , Ca =2 , Sr +2 , and Pb +2 .

Claim 102

Dependent Claim 65 words

A method according to claim 72 wherein said exchanged lithium and/or sodium water-swelling mica is a potassium mica which has a composition, expressed in weight percent on the oxide basis, of about 3-17%, K 2 O, 0-8% Li 2 O, 0-5% Na 2 O, 10-38% MgO, 0-30% B 2 O 3 , 0-10% Al 2 O 3 , 35-70% SiO 2 , and 5-15% F.

Claim 103

Dependent Claim 100 words

A method according to claim 72 wherein said lithium and/or sodium water-swelling mica is basically a trisilicic mica, i.e., boron fluorphlogopite and solid solutions between that and other structurally-compatible species selected from the group of fluorhectorite, fluortalc, fluorpolylithionite, and fluorphlogopite, and wherein said exchanged lithium and/or sodium trisilicic mica is a potassium mica which has a composition, expressed in weight percent on the oxide basis, of about 3-16% K 2 O, 0-4% Li 2 O, 0-5% Na 2 O, 20-38% MgO, 2-10% B 2 O 3 , 0-10% Al 2 O 3 , 35-56% SiO 2 , and 4-12% F.

Claim 104

Independent Claim 265 words

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 2 O and/or 0-10% Na 2 O, 0.5-14% Li 2 O+Na 2 O, 0-30% B 2 O 3 , 10-38% MgO, 0-10% Al 2 O 3 , 35-70% SiO 2 , and 5-15% F; (b) simultaneously cooling said melt to a temperature between about 900°-1050° 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°-900° 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,

Claim 105

Independent Claim 265 words

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 2 O and/or 0-10% Na 2 O, 0.5-14% Li 2 O+Na 2 O, 0-30% B 2 O 3 , 10-38% MgO, 0-10% Al 2 O 3 , 35-70% SiO 2 , and 5-15% F; (b) simultaneously cooling said melt to a temperature between about 900°-1050° 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°-900° 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,

Claim 106

Dependent Claim 62 words

A method according to claim 95 wherein said batch also contains up to 30% total of oxides selected from the group 0-10% CaO, 0-10% CdO, 0-10% CoO, 0-10% CuO, 0-20% FeO, 0-20% Fe 2 O 3 , 0-10% MnO, 0-10% NiO, 0-10% P 2 O 5 , 0-30% PbO, 0-20% SrO, 0-10% TiO 2 , 0-25% ZnO, and 0-10% ZrO 2 .

Claim 107

Dependent Claim 24 words

A method according to claim 95 wherein said time sufficient to cause phase separation and nucleation ranges between a few seconds to a minute.

Claim 108

Dependent Claim 24 words

A method according to claim 95 wherein said time sufficient to effect the development of crystals ranges between about 2 minutes to several hours.

Claim 109

Dependent Claim 12 words

A method according to claim 95 wherein said polar liquid is water.

Claim 110

Dependent Claim 21 words

A method according to claim 95 wherein said time sufficient to effect swelling, disintegration, and gelation ranges between about 1-48 hours.

Claim 111

Dependent Claim 22 words

A method according to claim 95 wherein the viscosity of said gel is adjusted by adding a deflocculating or peptizing agent thereto.

Claim 112

Dependent Claim 17 words

A method according to claim 95 wherein said solid:liquid ratio ranges between about 1-50% by weight solids.

Claim 113

Dependent Claim 17 words

A method according to claim 102 wherein said solid:liquid ratio ranges between about 2-25% by weight solids.

Claim 114

Dependent Claim 97 words

A method according to claim 95 wherein said lithium and/or sodium water-swelling mica is basically a trisilicic mica, i.e., boron fluorphlogopite and solid solutions between that and other structurally-compatible species selected from the group of fluorhectorite, fluortalc, fluorpolylithionite, and fluorphlogopite, consisting essentially, expressed in weight percent on the oxide basis, of 0-6% Li 2 O, 0-9% Na 2 O, 0.5-10% Li 2 O+Na 2 O, 20-38% MgO, 2-10% 2-10% B 2 O 3 , 0-10% Al 2 O 3 , 4-12% Al 2 O 3 +B 2 O 3 , 35-56% SiO 2 , and 4-12% F.

Claim 115

Independent Claim 304 words

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 2 O and/or 0-10% Na 2 O, 0.5-14% Li 2 O+Na 2 O, 0-30% B 2 O 3 , 10-38% MgO, 0-10% Al 2 O 3 , 35-70% SiO 2 , and 5-15% F; (B) simultaneously cooling said melt to a temperature between about 900°-1050° 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°-900° 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 + and/or Na + ions from the interlayer of said crystals; and then (h) drying said fiber or film.

Claim 116

Independent Claim 304 words

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 2 O and/or 0-10% Na 2 O, 0.5-14% Li 2 O+Na 2 O, 0-30% B 2 O 3 , 10-38% MgO, 0-10% Al 2 O 3 , 35-70% SiO 2 , and 5-15% F; (B) simultaneously cooling said melt to a temperature between about 900°-1050° 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°-900° 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 + and/or Na + ions from the interlayer of said crystals; and then (h) drying said fiber or film.

Claim 117

Dependent Claim 62 words

A method according to claim 105 wherein said batch also contains up to 30% total of oxides selected from the group 0-10% CaO, 0-10% CdO, 0-10% CoO, 0-10% CuO, 0-20% FeO, 0-20% Fe 2 O 3 , 0-10% MnO, 0-10% NiO, 0-10% P 2 O 5 , 0-30% PbO, 0-20% SrO, 0-10% TiO 2 , 0-25% ZnO, and 0-10% ZrO 2 .

Claim 118

Dependent Claim 24 words

A method according to claim 105 wherein said time sufficient to cause phase separation and nucleation ranges between a few seconds to a minute.

Claim 119

Dependent Claim 24 words

A method according to claim 105 wherein said time sufficient to effect the development of crystals ranges between about 2 minutes to several hours.

Claim 120

Dependent Claim 12 words

A method according to claim 105 wherein said polar liquid is water.

Claim 121

Dependent Claim 21 words

A method according to claim 105 wherein said time sufficient to effect swelling, disintegration, and gelation ranges between about 1-48 hours.

Claim 122

Dependent Claim 22 words

A method according to claim 105 wherein the viscosity of said gel is adjusted by adding a deflocculating or peptizing agent thereto.

Claim 123

Dependent Claim 17 words

A method according to claim 105 wherein said solid:liquid ratio ranges between about 1-50% by weight solids.

Claim 124

Dependent Claim 17 words

A method according to claim 112 wherein said solid:liquid ratio ranges between about 2-25% by weight solids.

Claim 125

Dependent Claim 27 words

A method according to claim 105 wherein said solid:liquid ratio ranges up to about 80% by weight solids and a fiber is prepared via high pressure extrusion.

Claim 126

Dependent Claim 23 words

A method according to claim 105 wherein said film is prepared by casting said gel onto the surface of an inert, impermeable substrate.

Claim 127

Dependent Claim 17 words

A method according to claim 105 wherein said source of large cations is an aqueous salt solution.

Claim 128

Dependent Claim 49 words

A method according to claim 105 wherein said large cations are selected from the group of K + , Rb + , Cs + , NH 4 + , H 3 O + , Ca +2 , Sr +2 , Ba +2 , Pb +2 , and organic polycations.

Claim 129

Dependent Claim 19 words

A method according to claim 105 wherein successive films are prepared and dried in superjacent relationship to form board.

Claim 130

Dependent Claim 36 words

A method according to claim 105 wherein inert fillers are included with said fully or predominantly crystalline body in the gelation step in an amount to constitute up to 75% by volume of the final product.

Claim 131

Dependent Claim 53 words

A method according to claim 105 wherein said fiber or film is prepared by contacting said gel having the desired fluidity with a flocculating agent to form a skin or membrane at the interface therebetween and therafter drawing off said skin or membrane to renew the contact between said gel and flocculating agent.

Claim 132

Dependent Claim 28 words

A method according to claim 120 wherein said contact between said gel and flocculating agent is made by floating a liquid containing said fluocculating agent over said gel.

Claim 133

Dependent Claim 32 words

A method according to claim 120 wherein said contact betwen said gel and flocculating agent is made by spraying a mist of a flocculating agent-containing liquid onto the surface of the gel.

Claim 134

Dependent Claim 26 words

A method according to claim 120 wherein said contact between said gel and flocculating agent is made by extruding said gel into a flocculating agent-containing liquid.

Claim 135

Dependent Claim 47 words

A method for forming a fiber according to claim 120 wherein said contact between said gel and flocculating agent is made by injecting said gel as a thin stream into a flocculating agent-containing liquid and, thereafter, pulling a continuous fiber or group of fibers from said liquid.

Claim 136

Dependent Claim 18 words

A method according to claim 120 wherein said flocculating agent is an aqueous salt solution of large cations.

Claim 137

Dependent Claim 49 words

A method according to claim 120 wherein said large cations are selected from the group of K + , Rb + , Cs + , NH 4 + , H 3 O + , Ca +2 , Sr +2 , Ba +2 , Pb +2 , and organic polycations.

Claim 138

Dependent Claim 65 words

A method according to claim 105 wherein said exchanged lithium and/or sodium water-swelling mica is a potassium mica which has a composition, expressed in weight percent on the oxide basis, of about 3-17% K 2 O, 0-8% Li 2 O, 0-5% Na 2 O, 10-38% MgO, 0-30% B 2 O 3 , 0-10% Al 2 O 3 , 35-70% SiO 2 , and 5-15% F.

Claim 139

Dependent Claim 91 words

A method according to claim 105 wherein said lithium and/or sodium water-swelling mica is basically a trisilicic mica, i.e., boron fluorphlogopite and solid solutions between that and other structurally-compatible species selected from the group of fluorhectorite, fluortalc, fluorpolylithionite, and fluorphlogopite, wherein said exchanged lithium and/or sodium trisilicic mica is a potassium mica which has a composition of about 3-16% K 2 O, 0-4% Li 2 O, 0-5% Na 2 O, 20-38% MgO, 2-10% B 2 O 3 , 0-10% Al 2 O 3 , 35-56% SiO 2 , and 4-12% F.

Claim 140

Independent Claim 276 words

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 2 O and/or 2-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 0-20% B 2 O 3 , 0-10% Al 2 O 3 , 15-38% MgO, 50-70% SiO 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°-400° 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.

Claim 141

Independent Claim 276 words

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 2 O and/or 2-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 0-20% B 2 O 3 , 0-10% Al 2 O 3 , 15-38% MgO, 50-70% SiO 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°-400° 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.

Claim 142

Dependent Claim 65 words

A method according to claim 129 wherein said glass also contains up to 20% by weight total of oxides selected from the group of 0-10% CaO, 0-10% CdO, 0-10% CoO, 0-10% CuO, 0-20% Fe 2 O 3 , 0-20% FeO, 0-10% MnO, 0-10% NiO, 0-20% PbO, 0-10% P 2 O 5 , 0-20% SrO, 0-10% TiO 2 , 0-20% ZnO, and 0-10% ZrO 2 .

Claim 143

Dependent Claim 70 words

A method according to claim 129 wherein the crystals of said fully or predominantly crystalline body consist essentially 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 hydroxyl hectorite, hydroxyl boron phlogopite, talc, fluortalc, polylithionite, fluoropolylithionite, phlogopite, and fluorphlogopite, and said glass contains at least 5% F.

Claim 144

Dependent Claim 50 words

A method according to claim 129 wherein said glass consists essentially, expressed in weight percent on the oxide basis, of 0-6% Li 2 O and/or 2-8% Na 2 O, 2-14% Li 2 O+Na 2 O, 20-30% MgO, 0-15% B 2 O 3 , 60-70% SiO 2 , and 0-6% F.

Claim 145

Dependent Claim 21 words

A method according to claim 129 wherein said time sufficient to cause the development of crystals ranges between about 0.5-48 hours.

Claim 146

Dependent Claim 12 words

A method according to claim 129 wherein said polar liquid is water.

Claim 147

Dependent Claim 21 words

A method according to claim 129 wherein said time sufficient to cause swelling, disintegration, and gelation ranges between about 1-48 hours.

Claim 148

Dependent Claim 22 words

A method according to claim 129 wherein the viscosity of said gel is adjusted by adding a deflocculating or peptizing agent thereto.

Claim 149

Dependent Claim 18 words

A method according to claim 129 wherein said solid: liquid ratio ranges between about 1-50% by weight solids.

Claim 150

Dependent Claim 18 words

A method according to claim 137 wherein said solid: liquid ratio ranges between about 2-25% by weight solids.

Claim 151

Dependent Claim 114 words

A method according to claim 129 wherein said lithium and/or sodium water-swelling mica is basically trisilicic mica selected from the group of boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of hydroxyl hectorite, fluorhectorite, talc, fluortalc, polylithionite, fluoropolylithionite, phlogopite, and fluorophlogopite, consisting essentially, expressed in weight percent on the oxide basis, of 0-6% Li 2 O, 0-9% Na 2 O, 0.5-10% Li 2 O+Na 2 O, 20-38% MgO, 2-10% B 2 O 3 , 0-10% Al 2 O 3 , 4-12% Al 2 O 3 +B 2 O 3 , 35-56% SiO 2 , 0-12% F, 0-12% OH, and 4-12% F+OH.

Claim 152

Independent Claim 320 words

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 2 O and/or 2-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 0-20% B 2 O 3 , 0-10% Al 2 O 3 , 15-38% MgO, 50-70% SiO 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°-400° 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 + and/or Na + ions from the interlayer of said crystals; and then (i) drying said fiber or film.

Claim 153

Independent Claim 320 words

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 2 O and/or 2-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 0-20% B 2 O 3 , 0-10% Al 2 O 3 , 15-38% MgO, 50-70% SiO 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°-400° 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 + and/or Na + ions from the interlayer of said crystals; and then (i) drying said fiber or film.

Claim 154

Dependent Claim 65 words

A method according to claim 140 wherein said glass also contains up to 20% by weight total of oxides selected from the group of 0-10% CaO, 0-10% CdO, 0-10% CoO, 0-10% CuO, 0-20% Fe 2 O 3 , 0-20% FeO, 0-10% MnO, 0-10% NiO, 0-20% PbO, 0-10% P 2 O 5 , 0-20% SrO, 0-10% TiO 2 , 0-20% ZnO, and 0-10% ZrO 2 .

Claim 155

Dependent Claim 71 words

A method according to claim 140 wherein the crystals of said fully or predominantly crystalline body consist essentially of an exchange 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 hydroxyl hectorite, hydroxyl boron hectorite, talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, and said glass contains at least 5% F.

Claim 156

Dependent Claim 50 words

A method according to claim 140 wherein said glass consists essentially, expressed in weight percent on the oxide basis, of 0-6% Li 2 O and/or 2-8% Na 2 O, 2-14% Li 2 O+Na 2 O, 20-30% MgO, 0-15% B 2 O 3 , 60-70% SiO 2 , and 0-6% F.

Claim 157

Dependent Claim 21 words

A method according to claim 140 wherein said time sufficient to cause the development of crystals ranges between about 0.5-48 hours.

Claim 158

Dependent Claim 12 words

A method according to claim 140 wherein said polar liquid is water.

Claim 159

Dependent Claim 21 words

A method according to claim 140 wherein said time sufficient to cause swellng, disintegration, and gelatin ranges between about 1-48 hours.

Claim 160

Dependent Claim 22 words

A method according to claim 140 wherein the viscosity of said gel is adjusted by adding a deflocculating or peptizing agent thereto.

Claim 161

Dependent Claim 18 words

A method according to claim 140 wherein said solid: liquid ratio ranges between about 1-50% by weight solids.

Claim 162

Dependent Claim 18 words

A method according to claim 148 wherein said solid: liquid ratio ranges between about 2-25% by weight solids.

Claim 163

Dependent Claim 28 words

A method according to claim 140 wherein said solid: liquid ratio ranges up to about 80% by weight solids and a fiber is prepared via high pressure extrusion.

Claim 164

Dependent Claim 23 words

A method according to claim 140 wherein said film is prepared by casting said gel onto the surface of an inert, impermeable substrate.

Claim 165

Dependent Claim 17 words

A method according to claim 140 wherein said source of large cations is an aqueous salt solution.

Claim 166

Dependent Claim 49 words

A method according to claim 140 wherein said large cations are selected from the group of K + , Rb + , Cs + , NH 4 + , H 3 O + , Ca +2 , Sr +2 , Ba +2 , Pb +2 , and organic polycations.

Claim 167

Dependent Claim 19 words

A method according to claim 140 wherein successive films are prepared and dried in superjacent relationship to form board.

Claim 168

Dependent Claim 36 words

A method according to claim 140 wherein inert fillers are included with said fully or predominantly crystalline body in the gelation step in an amount to constitute up to 75% by volume of the final product.

Claim 169

Dependent Claim 53 words

A method according to claim 140 wherein said fiber or film is prepared by contacting said gel having the desired fluidity with a flocculating agent to form a skin or membrane at the interface therebetween and thereafter drawing off said skin or membrane to renew the contact between said gel and flocculating agent.

Claim 170

Dependent Claim 28 words

A method according to claim 156 wherein said contact between said gel and flocculating agent is made by floating a liquid containing said flocculating agent over said gel.

Claim 171

Dependent Claim 32 words

A method according to claim 156 wherein said contact between said gel and flocculating agent is made by spraying a mist of a flocculating agent-containing liquid onto the surface of the gel.

Claim 172

Dependent Claim 26 words

A method according to claim 156 wherein said contact between said gel and flocculating agent is made by extruding said gel into a flocculating agent-containing liquid.

Claim 173

Dependent Claim 47 words

A method for forming a fiber according to claim 156 wherein said contact between said gel and flocculating agent is made by injecting said gel as a thin stream into a flocculating agent-containing liquid and, thereafter, pulling a continuous fiber or group of fibers from said liquid.

Claim 174

Dependent Claim 18 words

A method according to claim 156 wherein said flocculating agent is an aqueous salt solution of large cations.

Claim 175

Dependent Claim 49 words

A method according to claim 156 wherein said large cations are selected from the group of K + , Rb + , Cs + , NH 4 + , H 3 O + , Ca +2 , Sr +2 , Ba +2 , Pb +2 , and organic polycations.

Claim 176

Dependent Claim 69 words

A method according to claim 140 wherein said exchanged lithium and/or sodium water-swelling mica is a potassium mica which has a composition, expressed in weight percent on the oxide basis, of about 3-17% K 2 O, 0-8% Li 2 O, 0-5% Na 2 O, 18-38% MgO, 0-30% B 2 O 3 , 0-10% Al 2 O 3 , 50-70% SiO 2 , 0-12% F, 0-12% OH, and 4-12% F+OH.

Claim 177

Dependent Claim 129 words

A method according to claim 140 wherein said lithium and/or sodium water-swelling mica is basically a trisilicic mica selected from the group of boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of hydroxyl hectorite, fluorhectorite, talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, and wherein said exchanged lithium and/or sodium trisilicic mica is a potassium mica which has a composition, expressed in weight percent on the oxide basis, of about 3-16% K 2 O, 0-4% Li 2 O, 0-5% Na 2 O, 20-38% MgO, 2-10% B 2 O 3 , 0-10% Al 2 O 3 , 4-12% Al 2 O 3 +B 2 O 3 , 35-56% SiO 2 , 0-12% F, 0-12% OH, and 4-12% F+OH.

Claim 178

Independent Claim 364 words

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 2 O and/or 2-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 0-20% B 2 O 3 , 0-10% Al 2 O 3 , 15-38% MgO, 50-70% SiO 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°-1200° 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°-400° 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.

Claim 179

Independent Claim 364 words

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 2 O and/or 2-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 0-20% B 2 O 3 , 0-10% Al 2 O 3 , 15-38% MgO, 50-70% SiO 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°-1200° 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°-400° 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.

Claim 180

Dependent Claim 65 words

A method according to claim 165 wherein said glass also contains up to 20% by weight total of oxides selected from the group of 0-10% CaO, 0-10% CdO, 0-10% CoO, 0-10% CuO, 0-20% FE 2 O 3 , 0-20% FeO, 0-10% MnO, 0-10% NiO, 0-20% PbO, 0-10% P 2 O 5 , 0-20% SrO, 0-10% TiO 2 , 0-20% ZnO, and 0-10% ZrO 2 .

Claim 181

Dependent Claim 26 words

A method according to claim 165 wherein said fully or predominantly crystalline body consists essentially of fluoride-containing crystals and said glass contains at least 5% F.

Claim 182

Dependent Claim 56 words

A method according to claim 165 wherein said glass consists essentially, expressed in weight percent on the oxide basis, of 0-6% Li 2 O and/or 2-8% Na 2 O, 2-14% Li 2 O+Na 2 O, 20-30% MgO, 0-15% B 2 O 3 , 0-5% Al 2 O 3 , 60-70% SiO 2 , and 0-6% F.

Claim 183

Dependent Claim 24 words

A method according to claim 165 wherein the time sufficient to cause the development of crystals ranges between about 3 minutes to 8 hours.

Claim 184

Dependent Claim 19 words

A method according to claim 165 wherein the time sufficient to convert said crystals ranges between about 0.5-48 hours.

Claim 185

Dependent Claim 12 words

A method according to claim 165 wherein said polar liquid is water.

Claim 186

Dependent Claim 21 words

A method according to claim 165 wherein said time sufficient to cause swelling, disintegration, and gelation ranges between about 1-48 hours.

Claim 187

Dependent Claim 22 words

A method according to claim 165 wherein the viscosity of said gel is adjusted by adding a deflocculating or peptizing agent thereto.

Claim 188

Dependent Claim 18 words

A method according to claim 165 wherein said solid: liquid ratio ranges between about 1-50% by weight solids.

Claim 189

Dependent Claim 18 words

A method according to claim 174 wherein said solid: liquid ratio ranges between about 2-25% by weight solids.

Claim 190

Dependent Claim 118 words

A method according to claim 165 wherein said lithium and/or sodium water-swelling mica is basically a trisilicic mica selected from the group of boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of hydroxyl hectorite, fluorhectorite, talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, consisting essentially, expressed in weight percent on the oxide basis, of 0-6% Li 2 O, Li 2 O, 0-9% Na 2 O, 0.5-10% Li 2 O+Na 2 O, 20-38% MgO, 2-10% B 2 O 3 , 0-10% Al 2 O 3 , 4-12% Al 2 O 3 +B 2 O 3 , 35-56% SiO 2 , 0-12% F, 0-12% OH, and 4-12% F+OH.

Claim 191

Independent Claim 407 words

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 2 O and/or 2-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 0-20% B 2 O 3 , 0-10% Al 2 O 3 , 15-38% MgO, 50-70% SiO 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°-1200° 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°-400° 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 + and/or Na + ions from the interlayer of said crystals; and then (i) drying said fiber of film.

Claim 192

Independent Claim 407 words

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 2 O and/or 2-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 0-20% B 2 O 3 , 0-10% Al 2 O 3 , 15-38% MgO, 50-70% SiO 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°-1200° 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°-400° 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 + and/or Na + ions from the interlayer of said crystals; and then (i) drying said fiber of film.

Claim 193

Dependent Claim 65 words

A method according to claim 177 wherein said glass also contains up to 20% by weight total of oxides selected from the group of 0-10% CaO, 0-10% CdO, 0-10% CoO, 0-10% CuO, 0-20% Fe 2 O 3 , 0-20% FeO, 0-10% MnO, 0-10% NiO, 0-20% PbO, 0-10% P 2 O 5 , 0-20% SrO, 0-10% TiO 2 , 0-20% ZnO, and 0-10% ZrO 2 .

Claim 194

Dependent Claim 26 words

A method according to claim 177 wherein said fully or predominantly crystalline body consists essentially of fluoride-containing crystals and said glass contains at least 5% F.

Claim 195

Dependent Claim 56 words

A method according to claim 177 wherein said glass consists essentially, expressed in weight percent on the oxide basis, of 0-6% Li 2 O and/or 2-8% Na 2 O, 2-14% Li 2 O+Na 2 O, 20-30% MgO, 0-15% B 2 O 3 , 0-5% Al 2 O 3 , 60-70% SiO 2 , and 0-6% F.

Claim 196

Dependent Claim 24 words

A method according to claim 177 wherein the time sufficient to cause the development of crystals ranges between about 3 minutes to 8 hours.

Claim 197

Dependent Claim 19 words

A method according to claim 177 wherein the time sufficient to convert said crystals ranges between about 0.5-48 hours.

Claim 198

Dependent Claim 12 words

A method according to claim 177 wherein said polar liquid is water.

Claim 199

Dependent Claim 21 words

A method according to claim 177 wherein said time sufficient to cause swelling, disintegration, and gelation ranges between about 1-48 hours.

Claim 200

Dependent Claim 22 words

A method according to claim 177 wherein the viscosity of said gel is adjusted by adding a deflocculating or peptizing agent thereto.

Claim 201

Dependent Claim 17 words

A method according to claim 177 wherein said solid:liquid ratio ranges between about 1-50% by weight solids.

Claim 202

Dependent Claim 17 words

A method according to claim 186 wherein said solid:liquid ratio ranges between about 2-25% by weight solids.

Claim 203

Dependent Claim 27 words

A method according to claim 177 wherein said solid:liquid ratio ranges up to about 80% by weight solids and a fiber is prepared via high pressure extrusion.

Claim 204

Dependent Claim 23 words

A method according to claim 177 wherein said film is prepared by casting said gel onto the surface of an inert, impermeable substrate.

Claim 205

Dependent Claim 17 words

A method according to claim 177 wherein said source of large cations is an aqueous salt solution.

Claim 206

Dependent Claim 49 words

A method according to claim 177 wherein said large cations are selected from the group of K + , Rb + , Cs + , NH 4 + , H 3 O + , Ca +2 , Sr +2 , Ba +2 , Pb +2 , and organic polycations.

Claim 207

Dependent Claim 19 words

A method according to claim 177 wherein successive films are prepared and dried in superjacent relationship to form board.

Claim 208

Dependent Claim 36 words

A method according to claim 177 wherein inert fillers are included with said fully or predominantly crystalline body in the gelation step in an amount to constitute up to 75% by volume of the final product.

Claim 209

Dependent Claim 53 words

A method according to claim 177 wherein said fiber or film is prepared by contacting said gel having the desired fluidity with a flocculating agent to form a skin or membrane at the interface therebetween and thereafter drawing off said skin or membrane to renew the contact between said gel and flocculating agent.

Claim 210

Dependent Claim 28 words

A method according to claim 194 wherein said contact between said gel and flocculating agent is made by floating a liquid containing said flocculating agent over said gel.

Claim 211

Dependent Claim 32 words

A method according to claim 194 wherein said contact between said gel and flocculating agent is made by spraying a mist of a flocculating agent-containing liquid onto the surface of the gel.

Claim 212

Dependent Claim 26 words

A method according to claim 194 wherein said contact between said gel and flocculating agent is made by extruding said gel into a flocculating agent-containing liquid.

Claim 213

Dependent Claim 47 words

A method for forming a fiber according to claim 194 wherein said contact between said gel and flocculating agent is made by injecting said gel as a thin stream into a flocculating agent-containing liquid and, thereafter, pulling a continuous fiber or group of fibers from said liquid.

Claim 214

Dependent Claim 18 words

A method according to claim 177 wherein said flocculating agent is an aqueous salt solution of large cations.

Claim 215

Dependent Claim 49 words

A method according to claim 199 wherein said large cations are selected from the group of K + , Rb + , Cs + , NH 4 + , H 3 O + , Ca +2 , Sr +2 , Ba +2 , Pb +2 , and organic polycations.

Claim 216

Dependent Claim 69 words

A method according to claim 177 wherein said exchanged lithium and/or sodium water-swelling mica is a potassium mica which has a composition, expressed in weight percent on the oxide basis, of about 3-17% K 2 O, 0-8% Li 2 O, 0-5% Na 2 O, 15-38% MgO, 0-30% B 2 O 3 , 0-10% Al 2 O 3 , 50-70% SiO 2 , 0-12% F, 0-12% OH, and 4-12% F+OH.

Claim 217

Dependent Claim 119 words

A method according to claim 177 wherein said lithium and/or sodium water-swelling mica is basically a trisilicic mica selected from the group of boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of hydroxyl hectorite, fluorhectorite, talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite and wherein said exchanged lithium and/or sodium trisilicic mica is a potassium mica which has a composition, expressed in weight percent on the oxide basis, of aboout 3-16% K 2 O, 0-4% Li 2 O, 0-5% Na 2 O, 20-38% MgO, 2-10% B 2 O 3 , 0-10% Al 2 O 3 , 35-56% SiO 2 , 0-12% F, 0-12% OH, and 4-12% F+OH.

Claim 218

Independent Claim 377 words

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 2 O and/or 2-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 0-20% B 2 O 3 , 0-10% Al 2 O 3 , 15-38% MgO, 50-70% SiO 2 , and 0-12% F; (b) simultaneously cooling said melt to a temperature between about 900°-1050° 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°-900° 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°-400° 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.

Claim 219

Independent Claim 377 words

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 2 O and/or 2-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 0-20% B 2 O 3 , 0-10% Al 2 O 3 , 15-38% MgO, 50-70% SiO 2 , and 0-12% F; (b) simultaneously cooling said melt to a temperature between about 900°-1050° 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°-900° 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°-400° 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.

Claim 220

Dependent Claim 65 words

A method according to claim 203 wherein said glass also contains up to 20% by weight total of oxides selected from the group of 0-10% CaO, 0-10% CdO, 0-10% CoO, 0-10% CuO, 0-20% Fe 2 O 3 , 0-20% FeO, 0-10% MnO, 0-10% NiO, 0-20% PbO, 0-10% P 2 O 5 , 0-20% SrO, 0-10% TiO 2 , 0-20% ZnO, and 0-10% ZrO 2 .

Claim 221

Dependent Claim 26 words

The method according to claim 203 wherein said fully or predominantly crystalline body consists essentially of fluoride-containing crystals and said glass contains at least 5% F.

Claim 222

Dependent Claim 50 words

A method according to claim 203 wherein said glass consists essentially, expressed in weight percent on the oxide basis, of 0-6%, Li 2 O and/or 2-8% Na 2 O, 2-14% Li 2 O+Na 2 O, 20-30% MgO, 0-15% B 2 O 3 , 60-70% SiO 2 , and 0-6% F.

Claim 223

Dependent Claim 24 words

A method according to claim 203 wherein said time sufficient to cause phase separation and nucleation ranges between a few seconds to a minute.

Claim 224

Dependent Claim 24 words

A method according to claim 203 wherein said time sufficient to effect the development of crystals ranges between about 2 minutes to several hours.

Claim 225

Dependent Claim 19 words

A method according to claim 203 wherein the time sufficient to convert said crystals ranges between about 0.5-48 hours.

Claim 226

Dependent Claim 12 words

A method according to claim 203 wherein said polar liquid is water.

Claim 227

Dependent Claim 21 words

A method according to claim 203 wherein said time sufficient to cause swelling, disintegration, and gelation ranges between about 1-48 hours.

Claim 228

Dependent Claim 22 words

A method according to claim 203 wherein the viscosity of said gel is adjusted by adding a deflocculating or peptizing agent thereto.

Claim 229

Dependent Claim 17 words

A method according to claim 203 wherein said solid:liquid ratio ranges between about 1-50% by weight solids.

Claim 230

Dependent Claim 16 words

A method according to claim 213 wherein said solid:liquid ratio ranges between about 2-25% by weight.

Claim 231

Dependent Claim 115 words

A method according to claim 203 wherein said lithium and/or sodium water-swelling mica is basically a trisilicic mica selected from the group of boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions between those and between those and other structurally-compatible species selected from the group of hydroxyl hectorite, fluorhectorite, talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, consisting essentially, expressed in weight percent on the oxide basis, of 0-6% Li 2 O, 0-9% Na 2 O, 0.5-10% Li 2 O+Na 2 O, 20-38% MgO, 2-10% B 2 O 3 , 0-10% Al 2 O 3 , 4-12% Al 2 O 3 +B 2 O 3 , 35-56% SiO 2 , 0-12% F, 0-12% OH, and 4-12% F+OH.

Claim 232

Independent Claim 299 words

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 2 O and/or 2-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 0-20% B 2 O 3 , 0-10% Al 2 O 3 , 15-38% MgO, 50-70% SiO 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°-400° 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 + and/or Na + ions from the interlayer of said crystals.

Claim 233

Independent Claim 299 words

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 2 O and/or 2-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 0-20% B 2 O 3 , 0-10% Al 2 O 3 , 15-38% MgO, 50-70% SiO 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°-400° 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 + and/or Na + ions from the interlayer of said crystals.

Claim 234

Dependent Claim 65 words

A method according to claim 216 wherein said glass also contains up to 20% by weight total of oxides selected from the group of 0-10% CaO, 0-10% CdO, 0-10% CoO, 0-10% CuO, 0-20% Fe 2 O 3 , 0-20% FeO, 0-10% MnO, 0-10% NiO, 0-20% PbO, 0-10% P 2 O 5 , 0-20% SrO, 0-10% TiO 2 , 0-20% ZnO, and 10-10% ZrO 2 .

Claim 235

Dependent Claim 71 words

A method according to claim 216 wherein the crystals of said fully or predominantly crystalline body consist 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 hydroxyl hectorite, hydroxyl boron phlogopite, talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, and said glass contains at least 5% F.

Claim 236

Dependent Claim 56 words

A method according to claim 216 wherein said glass consists essentially, expressed in weight percent on the oxide basis, of 0-6% Li 2 O and/or 2-8% Na 2 O, 2-14% Li 2 O+Na 2 O, 20-30% MgO, 0-15% B 2 O 3 , 0-5% Al 2 O 3 , 60-70% SiO 2 , and 0-6% F.

Claim 237

Dependent Claim 21 words

A method according to claim 216 wherein said time sufficient to cause the development of crystals ranges between about 0.5-48 hours.

Claim 238

Dependent Claim 12 words

A method according to claim 216 wherein said polar liquid is water.

Claim 239

Dependent Claim 21 words

A method according to claim 216 wherein said time sufficient to cause swelling, disintegration, and gelation ranges between about 1-48 hours.

Claim 240

Dependent Claim 22 words

A method according to claim 216 wherein the viscosity of said gel is adjusted by adding a deflocculating or peptizing agent thereto.

Claim 241

Dependent Claim 17 words

A method according to claim 216 wherein said solid:liquid ratio ranges between about 1-50% by weight solids.

Claim 242

Dependent Claim 16 words

A method according to claim 224 wherein said solid:liquid ranges between about 2-25% by weight solids.

Claim 243

Dependent Claim 23 words

A method according to claim 216 wherein said film is prepared by casting said gel onto the surface of an inert, impermeable substrate.

Claim 244

Dependent Claim 17 words

A method according to claim 216 wherein said source of large cations is an aqueous salt solution.

Claim 245

Dependent Claim 49 words

A method according to claim 216 wherein said large cations are selected from the group of K + , Rb + , Cs + , NH 4 + , H 3 O + , Ca +2 , Sr +2 , Ba +2 , Pb +2 , and organic polycations.

Claim 246

Dependent Claim 36 words

A method according to claim 216 wherein inert fillers are included with said fully or predominantly crystalline body in the gelation step in an amount to constitute up to 75% by volume of the final product.

Claim 247

Dependent Claim 69 words

A method according to claim 216 wherein said exchanged lithium and/or sodium water-swelling mica is a potassium mica which has a composition, expressed in weight percent on the oxide basis, of about 3-17% K 2 O, 0-8% Li 2 O, 0-5% Na 2 O, 15-38% MgO, 0-30% B 2 O 3 , 0-10% Al 2 O 3 , 50-70% SiO 2 , 0-12% F, 0-12% OH, and 4-12% F+OH.

Claim 248

Dependent Claim 115 words

A method according to claim 216 wherein said lithium and/or sodium water-swelling mica is a trisilicic mica selected from the group of boron fluorphlogopite, hydroxyl boron phlogopite, 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 and wherein said exchanged lithium and/or sodium trisilicic mica is a potassium mica which has a composition, expressed in weight percent on the oxide basis, of about 3-16% K 2 O, 0-4% Li 2 O, 0-5% Na 2 O, 20-38% MgO, 2-10% B 2 O 3 , 0-10% Al 2 O 3 , 35-56% SiO 2 , 0-12% F, 0-12% OH, and 4-12% F+OH.

Claim 249

Independent Claim 391 words

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 2 O and/or 2-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 0-20% B 2 O 3 , 0-10% Al 2 O 3 , 15-38% MgO, 50-70% SiO 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°-1200° 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°-400° 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 + and/or Na + ions from the interlayer of said crystals.

Claim 250

Independent Claim 391 words

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 2 O and/or 2-10% Na 2 O, 2-14% Li 2 O+Na 2 O, 0-20% B 2 O 3 , 0-10% Al 2 O 3 , 15-38% MgO, 50-70% SiO 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°-1200° 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°-400° 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 + and/or Na + ions from the interlayer of said crystals.

Claim 251

Dependent Claim 64 words

A method according to claim 232 wherein said glass also contains up to 20% by weight total of oxides selected from the group of 0-10% CaO, 0-10% CdO, 0-10% CoO, 0-10% CuO, 0-20% Fe 2 O 3 , 0-20% FeO, 0-10% MnO, 0-10% NiO, 0-20% PbO, 0-10% P 2 O 5 , 0-20% SrO, 0-10% TiO 2 , 0-20% ZnO, 0-10% ZrO 2 .

Claim 252

Dependent Claim 71 words

A method according to claim 232 wherein the crystals of said fully or predominantly crystalline body consist 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 hydroxyl hectorite, hydroxyl boron phlogopite, talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite and said glass contains at least 5% F.

Claim 253

Dependent Claim 56 words

A method according to claim 232 wherein said glass consists essentially, expressed in weight percent on the oxide basis, of 0-6% Li 2 O and/or 2-8% Na 2 O, 2-14% Li 2 O+Na 2 O, 20-30% MgO, 0-15% B 2 O 3 , 0-5% Al 2 O 3 , 60-70% SiO 2 , and 0-6% F.

Claim 254

Dependent Claim 24 words

A method according to claim 232 wherein the time sufficient to cause the development of crystals ranges between about 3 minutes to 8 hours.

Claim 255

Dependent Claim 19 words

A method according to claim 232 wherein the time sufficient to convert said crystals ranges between about 0.5-48 hours.

Claim 256

Dependent Claim 12 words

A method according to claim 232 wherein said polar liquid is water.

Claim 257

Dependent Claim 21 words

A method according to claim 232 wherein said time sufficient to cause swelling, disintegration, and gelation ranges between about 1-48 hours.

Claim 258

Dependent Claim 22 words

A method according to claim 232 wherein the viscosity of said gel is adjusted by adding a deflocculating or peptizing agent thereto.

Claim 259

Dependent Claim 17 words

A method according to claim 232 wherein said solid:liquid ratio ranges between about 1-50% by weight solids.

Claim 260

Dependent Claim 17 words

A method according to claim 241 wherein said solid:liquid ratio ranges between about 2-25% by weight solids.

Claim 261

Dependent Claim 23 words

A method according to claim 232 wherein said film is prepared by casting said gel onto the surface of an inert, impermeable substrate.

Claim 262

Dependent Claim 17 words

A method according to claim 232 wherein said source of large cations is an aqueous salt solution.

Claim 263

Dependent Claim 49 words

A method according to claim 232 wherein said large cations are selected from the group of K + , Rb + , Cs + , NH 4 + , H 3 O + , Ca +2 , Sr +2 , Ba +2 , Pb +2 , and organic polycations.

Claim 264

Dependent Claim 36 words

A method according to claim 232 wherein inert fillers are included with said fully or predominantly crystalline body in the gelation step in an amount to constitute up to 75% by volume of the final product.

Claim 265

Dependent Claim 69 words

A method according to claim 232 wherein said exchanged lithium and/or sodium water-swelling mica is a potassium mica which has a composition, expressed in weight percent on the oxide basis, of about 3-17% K 2 O, 0-8% Li 2 O, 0-5% Na 2 O, 15-38% MgO, 0-30% B 2 O 3 , 0-10% Al 2 O 3 , 50-70% SiO 2 , 0-12% F, 0-12% OH, and 4-12% F+OH.

Claim 266

Dependent Claim 113 words

A method according to claim 232 wherein said lithium and/or sodium water-swelling mica is a trisilicic mica selected from the group of boron fluorphlogopite, hydroxyl boron phlogopite, and solid solutions between those and between those other structurally-compatible species selected from the group of talc, fluortalc, polylithionite, fluorpolylithionite, phlogopite, and fluorphlogopite, and wherein said exchanged lithium and/or sodium trisilicic mica is a potassium mica which has a composition, expressed in weight percent on the oxide basis, of about 3-16% K 2 O, 0-4% Li 2 O, 0-5% Na 2 O, 20-38MgO, 2-10% B 2 O 3 , 0-10% Al 2 O 3 , 35-56% SiO 2 , 0-12% F, 0-12% OH, and 4-12% F+OH.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1983-12-16	1984-06-16	1984-12-16	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1987-12-16	1988-06-16	1988-12-16	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1991-12-16	1992-06-16	1992-12-16	$7700.00	Window Closed / Lapsed

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

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