EP0331483A2 — Process for the preparation of fluoride glass and…

Claim 1

Independent Claim 149 words

A process for preparing a fluoride glass comprising the step of introducing a gaseous mixture into a reaction system containing a substrate to react the ingredients of said gaseous mixture in a gaseous phase or on said substrate to deposite a metal fluoride to form a fluoride glass, an improvement characterized in that said gaseous mixture comprising: a barium β-diketonate complex serving as a first starting material and represented by the following general formula (1) of: wherein R is an alkyl group having 1 to 7 carbon atoms, R′ is a substituted alkyl group having fluorine atoms substituting hydrogen atoms and represented by C n F 2n+1 where n is an integer of from 1 to 3; a gaseous or vaporizable compound of the matallic element constituting said fluoride glass, the gaseous or vaporizable compound serving as a second starting material; and a fluorine-contained gas serving as fluorinating agent.

Claim 2

Dependent Claim 149 words

A process for preparing a fluoride glass comprising the step of introducing a gaseous mixture into a reaction system containing a substrate to react the ingredients of said gaseous mixture in a gaseous phase or on said substrate to deposite a metal fluoride to form a fluoride glass, an improvement characterized in that said gaseous mixture comprising: a barium β-diketonate complex serving as a first starting material and represented by the following general formula (1) of: wherein R is an alkyl group having 1 to 7 carbon atoms, R′ is a substituted alkyl group having fluorine atoms substituting hydrogen atoms and represented by C n F 2n+1 where n is an integer of from 1 to 3; a gaseous or vaporizable compound of the matallic element constituting said fluoride glass, the gaseous or vaporizable compound serving as a second starting material; and a fluorine-contained gas serving as fluorinating agent.

Claim 3

Dependent Claim 142 words

A process for preparing a fluoride glass comprising the step of introducing a gaseous mixture into a reaction system containing a substrate to react the ingredients of said gaseous mixture in a gaseous phase or on said substrate to deposite a metal fluoride to form a fluoride glass, an improvement characterized in that said gaseous mixture comprising: a barium β-diketonate complex serving as a first starting material and represented by the following general formula (1) of: wherein R is an alkyl group having 1 to 7 carbon atoms, R′ is a substituted alkyl group having fluorine atoms substituting hydrogen atoms and represented by C n F 2n+1 where n is an integer of from 1 to 3; and a gaseous or vaporizable compound of the matallic element constituting said fluoride glass, the gaseous or vaporizable compound serving as a second starting material.

Claim 4

Dependent Claim 142 words

A process for preparing a fluoride glass comprising the step of introducing a gaseous mixture into a reaction system containing a substrate to react the ingredients of said gaseous mixture in a gaseous phase or on said substrate to deposite a metal fluoride to form a fluoride glass, an improvement characterized in that said gaseous mixture comprising: a barium β-diketonate complex serving as a first starting material and represented by the following general formula (1) of: wherein R is an alkyl group having 1 to 7 carbon atoms, R′ is a substituted alkyl group having fluorine atoms substituting hydrogen atoms and represented by C n F 2n+1 where n is an integer of from 1 to 3; and a gaseous or vaporizable compound of the matallic element constituting said fluoride glass, the gaseous or vaporizable compound serving as a second starting material.

Claim 5

Dependent Claim 195 words

A process for preparing a fluoride glass comprising the step of introducing a gaseous mixture into a reaction system containing a cylindrical substrate to react the ingredients of said gaseous mixture in a gaseous phase or on the interior wall of said substrate to deposite coating or fine particles of a metal fluoride to form a fluoride glass, an improvement characterized in that said gaseous mixture comprising: a barium β-diketonate complex serving as a first starting material and represented by the following general formula (1) of: wherein R is an alkyl group having 1 to 7 carbon atoms, R′ is a substituted alkyl group having fluorine atoms substituting hydrogen atoms and represented by C n F 2n+1 where n is an integer of from 1 to 3; a gaseous or vaporizable compound of the matallic element constituting said fluoride glass, the gaseous or vaporizable compound serving as a second starting material; and; a fluorine-contained gas serving as a fluorinating agent; and the process being further characterized in that said cylindrical substrate containing therein deposited coating or fine particles of a fluoride glass is heated to solidify the same to form a preform for optical fibers.

Claim 6

Dependent Claim 195 words

A process for preparing a fluoride glass comprising the step of introducing a gaseous mixture into a reaction system containing a cylindrical substrate to react the ingredients of said gaseous mixture in a gaseous phase or on the interior wall of said substrate to deposite coating or fine particles of a metal fluoride to form a fluoride glass, an improvement characterized in that said gaseous mixture comprising: a barium β-diketonate complex serving as a first starting material and represented by the following general formula (1) of: wherein R is an alkyl group having 1 to 7 carbon atoms, R′ is a substituted alkyl group having fluorine atoms substituting hydrogen atoms and represented by C n F 2n+1 where n is an integer of from 1 to 3; a gaseous or vaporizable compound of the matallic element constituting said fluoride glass, the gaseous or vaporizable compound serving as a second starting material; and; a fluorine-contained gas serving as a fluorinating agent; and the process being further characterized in that said cylindrical substrate containing therein deposited coating or fine particles of a fluoride glass is heated to solidify the same to form a preform for optical fibers.

Claim 7

Dependent Claim 197 words

A process for preparing a fluoride glass comprising the step of introducing a gaseous mixture into a reaction system containing a rod-like glass substrate to react the ingredients of said gaseous mixture in a gaseous phase or on the surface of said substrate to deposite a layer or fine particles of fluoride glass on the surface of said substrate, an improvement characterized in that said gaseous mixture comprising: a barium β-diketonate complex serving as a first starting material and represented by the following formula (1) of: wherein R is an alkyl group having 1 to 7 carbon atoms, R′ is a substituted alkyl group having fluorine atoms substituting hydrogen atoms and represented by C n F 2n+1 where n is an integer of from 1 to 3; a gaseous or vaporizable compound of the matallic element constituting said fluoride glass, the gaseous or vaporizable compound serving as a second starting material, and; a fluorine-contained gas serving as a fluorinating agent; and the process being further characterized in that said rod-like glass substrate containing thereon a lyer or deposited fine particles of a fluoride glass is heated to solidify the same to form a preform for optical fibers.

Claim 8

Dependent Claim 197 words

A process for preparing a fluoride glass comprising the step of introducing a gaseous mixture into a reaction system containing a rod-like glass substrate to react the ingredients of said gaseous mixture in a gaseous phase or on the surface of said substrate to deposite a layer or fine particles of fluoride glass on the surface of said substrate, an improvement characterized in that said gaseous mixture comprising: a barium β-diketonate complex serving as a first starting material and represented by the following formula (1) of: wherein R is an alkyl group having 1 to 7 carbon atoms, R′ is a substituted alkyl group having fluorine atoms substituting hydrogen atoms and represented by C n F 2n+1 where n is an integer of from 1 to 3; a gaseous or vaporizable compound of the matallic element constituting said fluoride glass, the gaseous or vaporizable compound serving as a second starting material, and; a fluorine-contained gas serving as a fluorinating agent; and the process being further characterized in that said rod-like glass substrate containing thereon a lyer or deposited fine particles of a fluoride glass is heated to solidify the same to form a preform for optical fibers.

Claim 9

Dependent Claim 30 words

A process according to any of claims 1 to 4, wherein said gaseous or vaporizable compound is at least one of metal halides, organic metal compounds and metal β-diketonate complexes.

Claim 10

Dependent Claim 31 words

A process according to claim 5, wherein said metal halides are halides of metallic elements of Ia, IIa, IIIa, IVa, Va, Ib, IIb, IIIb, IVb, Vb, VIb, VIIb and VIIIb groups.

Claim 11

Dependent Claim 19 words

A process according to any of claims 1 to 4, wherein said organic metal compounds is Al(CH₃)₃ or Al(C₂H₅)₃.

Claim 12

Dependent Claim 24 words

A process according to any of claims 1 to 4, wherein said β-diketone are 3,5-pentadione, 2,2,6,6-tetramethyl 3,5-heptanedione, 2,2,-dimethyl 3,5-octanedione, 1,1,1,5,5,5-hexafluoro-2,4-heptanedione, 5,5,5-trifluoro-2,4-pentanedione, 2,2-dimethyl-6,6,6-trifluoro-3,5-hexanedione, 2.2.-dimethyl-6,6,7,7,7-pentafluoro-3,5-heptanedione, 2,2-dimethyl-6,6,7,7,8,8,8-heptafluoro-3,5-octanedione.

Claim 13

Dependent Claim 60 words

A process according to any of claims 1 to 4, wherein said metallic element constituting said fluoride glass is one or more of Ba, Zr, Ca, Al, Na, Li, Hf, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, In, Sn, Pb, Sb, Bi, Zn, Cd, Ti. Th, Nb, Ta, Mo or Mn.

Claim 14

Dependent Claim 38 words

A process according to any of claims 1, 3 and 4, wherein said fluorine-contained gas is fluorine gas or a gaseous compound of fluorine with any one or more of hydrogen, halogens, carbon, nitrogen, boron, silicon and sulfur.

Claim 15

Dependent Claim 24 words

A process according to any of claims 1 to 4, wherein said substrate is fluoride glass, CaF₂, metal, oxide glass, polymer or multi-layer thereof.

Claim 16

Dependent Claim 25 words

A process according to any of claims 1 to 4, wherein said fluoride glass is any of BaF₂-ZrF₄ system, BaF₂-HfF₄ system or BaF₂-AlF₃ system glasses.

Claim 17

Dependent Claim 35 words

A process according to claim 3 or 4, wherein hydrogen fluoride gas serving as a fluorinating agent is added to the gaseous flow in addition to said first starting material and said second starting material.

Claim 18

Dependent Claim 57 words

A process according to claim 3, wherein the fluoride glass deposited on the interior wall of said cyclidrical substrate is heated in an environment of fluorine or clorine, or gaseous compounds of fluorine or chlorine with any one or more of hydrogen, carbon, nitrogen, boron, sulfur and silicon, or mixture of at least two of said gases.

Claim 19

Dependent Claim 26 words

A Process according to claim 3 or 4, further comprising the step of drawing said preform for optical fiber to form an drawn optical fluoride fiber.

Process for the preparation of fluoride glass and process for the preparation of optical fiber preform using the fluoride glass

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