EP1135345A1 - Methods of manufacturing soot for optical fiber preforms and preforms made by the methods - Google Patents
Methods of manufacturing soot for optical fiber preforms and preforms made by the methodsInfo
- Publication number
- EP1135345A1 EP1135345A1 EP99956587A EP99956587A EP1135345A1 EP 1135345 A1 EP1135345 A1 EP 1135345A1 EP 99956587 A EP99956587 A EP 99956587A EP 99956587 A EP99956587 A EP 99956587A EP 1135345 A1 EP1135345 A1 EP 1135345A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- nitrate
- burner assembly
- chloride
- aqueous solution
- acetate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 239000004071 soot Substances 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 59
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 32
- 239000013307 optical fiber Substances 0.000 title claims description 10
- 239000007788 liquid Substances 0.000 claims abstract description 93
- 239000000376 reactant Substances 0.000 claims abstract description 67
- 239000007864 aqueous solution Substances 0.000 claims abstract description 58
- 239000000443 aerosol Substances 0.000 claims abstract description 23
- 150000003839 salts Chemical class 0.000 claims abstract description 19
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 16
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 6
- -1 alkali metal acetate Chemical class 0.000 claims description 23
- 238000002485 combustion reaction Methods 0.000 claims description 22
- 239000011521 glass Substances 0.000 claims description 20
- 239000002019 doping agent Substances 0.000 claims description 18
- 230000008569 process Effects 0.000 claims description 14
- 238000000151 deposition Methods 0.000 claims description 13
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 10
- NLSCHDZTHVNDCP-UHFFFAOYSA-N caesium nitrate Chemical compound [Cs+].[O-][N+]([O-])=O NLSCHDZTHVNDCP-UHFFFAOYSA-N 0.000 claims description 10
- FLJPGEWQYJVDPF-UHFFFAOYSA-L caesium sulfate Chemical compound [Cs+].[Cs+].[O-]S([O-])(=O)=O FLJPGEWQYJVDPF-UHFFFAOYSA-L 0.000 claims description 10
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 10
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 10
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 10
- 238000000429 assembly Methods 0.000 claims description 8
- 230000000712 assembly Effects 0.000 claims description 8
- MFEVGQHCNVXMER-UHFFFAOYSA-L 1,3,2$l^{2}-dioxaplumbetan-4-one Chemical compound [Pb+2].[O-]C([O-])=O MFEVGQHCNVXMER-UHFFFAOYSA-L 0.000 claims description 5
- MFGOFGRYDNHJTA-UHFFFAOYSA-N 2-amino-1-(2-fluorophenyl)ethanol Chemical compound NCC(O)C1=CC=CC=C1F MFGOFGRYDNHJTA-UHFFFAOYSA-N 0.000 claims description 5
- 229910017569 La2(CO3)3 Inorganic materials 0.000 claims description 5
- 229910000003 Lead carbonate Inorganic materials 0.000 claims description 5
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims description 5
- 150000008041 alkali metal carbonates Chemical class 0.000 claims description 5
- 229910001963 alkali metal nitrate Inorganic materials 0.000 claims description 5
- 229910052936 alkali metal sulfate Inorganic materials 0.000 claims description 5
- 229910001964 alkaline earth metal nitrate Inorganic materials 0.000 claims description 5
- JRLDUDBQNVFTCA-UHFFFAOYSA-N antimony(3+);trinitrate Chemical compound [Sb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JRLDUDBQNVFTCA-UHFFFAOYSA-N 0.000 claims description 5
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 claims description 5
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 5
- 229910001626 barium chloride Inorganic materials 0.000 claims description 5
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 claims description 5
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Inorganic materials [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 claims description 5
- 229940011182 cobalt acetate Drugs 0.000 claims description 5
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 5
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 5
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 5
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 5
- JVLRYPRBKSMEBF-UHFFFAOYSA-K diacetyloxystibanyl acetate Chemical compound [Sb+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JVLRYPRBKSMEBF-UHFFFAOYSA-K 0.000 claims description 5
- SYDXSHCNMKOQFW-UHFFFAOYSA-H erbium(3+);trisulfate Chemical compound [Er+3].[Er+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O SYDXSHCNMKOQFW-UHFFFAOYSA-H 0.000 claims description 5
- HDGGAKOVUDZYES-UHFFFAOYSA-K erbium(iii) chloride Chemical compound Cl[Er](Cl)Cl HDGGAKOVUDZYES-UHFFFAOYSA-K 0.000 claims description 5
- NZPIUJUFIFZSPW-UHFFFAOYSA-H lanthanum carbonate Chemical compound [La+3].[La+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NZPIUJUFIFZSPW-UHFFFAOYSA-H 0.000 claims description 5
- 229960001633 lanthanum carbonate Drugs 0.000 claims description 5
- JLRJWBUSTKIQQH-UHFFFAOYSA-K lanthanum(3+);triacetate Chemical compound [La+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JLRJWBUSTKIQQH-UHFFFAOYSA-K 0.000 claims description 5
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 5
- VQEHIYWBGOJJDM-UHFFFAOYSA-H lanthanum(3+);trisulfate Chemical compound [La+3].[La+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VQEHIYWBGOJJDM-UHFFFAOYSA-H 0.000 claims description 5
- 229940046892 lead acetate Drugs 0.000 claims description 5
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 claims description 5
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 claims description 5
- CFYGEIAZMVFFDE-UHFFFAOYSA-N neodymium(3+);trinitrate Chemical compound [Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CFYGEIAZMVFFDE-UHFFFAOYSA-N 0.000 claims description 5
- 239000001103 potassium chloride Substances 0.000 claims description 5
- 235000011164 potassium chloride Nutrition 0.000 claims description 5
- 235000010333 potassium nitrate Nutrition 0.000 claims description 5
- 239000004323 potassium nitrate Substances 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 235000010344 sodium nitrate Nutrition 0.000 claims description 5
- 239000004317 sodium nitrate Substances 0.000 claims description 5
- 229910001631 strontium chloride Inorganic materials 0.000 claims description 5
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 claims description 5
- RXSHXLOMRZJCLB-UHFFFAOYSA-L strontium;diacetate Chemical compound [Sr+2].CC([O-])=O.CC([O-])=O RXSHXLOMRZJCLB-UHFFFAOYSA-L 0.000 claims description 5
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 4
- 239000001110 calcium chloride Substances 0.000 claims description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 4
- 150000004820 halides Chemical class 0.000 claims description 4
- ATINCSYRHURBSP-UHFFFAOYSA-K neodymium(iii) chloride Chemical compound Cl[Nd](Cl)Cl ATINCSYRHURBSP-UHFFFAOYSA-K 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims 6
- 238000007599 discharging Methods 0.000 claims 2
- 239000002210 silicon-based material Substances 0.000 claims 2
- 230000008016 vaporization Effects 0.000 claims 1
- 230000003287 optical effect Effects 0.000 abstract description 31
- 239000000835 fiber Substances 0.000 abstract description 16
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 3
- 229910052691 Erbium Inorganic materials 0.000 abstract description 2
- 229910052779 Neodymium Inorganic materials 0.000 abstract description 2
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 abstract description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 abstract 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract 1
- 150000001340 alkali metals Chemical class 0.000 abstract 1
- 150000001342 alkaline earth metals Chemical class 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 abstract 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract 1
- 229910052787 antimony Inorganic materials 0.000 abstract 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 abstract 1
- 229910017052 cobalt Inorganic materials 0.000 abstract 1
- 239000010941 cobalt Substances 0.000 abstract 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract 1
- 238000007796 conventional method Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract 1
- 229910052746 lanthanum Inorganic materials 0.000 abstract 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 18
- 230000008021 deposition Effects 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000005350 fused silica glass Substances 0.000 description 3
- 239000008240 homogeneous mixture Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 239000005049 silicon tetrachloride Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 150000002902 organometallic compounds Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- SGQZOVOWSCLZRF-UHFFFAOYSA-M aluminum;calcium;chloride;nitrate Chemical compound [Al+3].[Cl-].[Ca+2].[O-][N+]([O-])=O SGQZOVOWSCLZRF-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000002716 delivery method Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 239000013628 high molecular weight specie Substances 0.000 description 1
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000012705 liquid precursor Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/01413—Reactant delivery systems
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
- C03B19/1415—Reactant delivery systems
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
- C03B19/1415—Reactant delivery systems
- C03B19/1423—Reactant deposition burners
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/01413—Reactant delivery systems
- C03B37/0142—Reactant deposition burners
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/32—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with aluminium
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/34—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with rare earth metals, i.e. with Sc, Y or lanthanides, e.g. for laser-amplifiers
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/34—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with rare earth metals, i.e. with Sc, Y or lanthanides, e.g. for laser-amplifiers
- C03B2201/36—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with rare earth metals, i.e. with Sc, Y or lanthanides, e.g. for laser-amplifiers doped with rare earth metals and aluminium, e.g. Er-Al co-doped
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/40—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with transition metals other than rare earth metals, e.g. Zr, Nb, Ta or Zn
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/50—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with alkali metals
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/54—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with beryllium, magnesium or alkaline earth metals
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/30—For glass precursor of non-standard type, e.g. solid SiH3F
- C03B2207/32—Non-halide
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/30—For glass precursor of non-standard type, e.g. solid SiH3F
- C03B2207/34—Liquid, e.g. mist or aerosol
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/50—Multiple burner arrangements
- C03B2207/52—Linear array of like burners
Definitions
- Non-aqueous liquid reactant 18 is preferably a liquid organometallic compound such as octamethylcyclotetrasiloxane, but can be a silicon alkoxide, a metal alkoxide, or other siliceous matrix material made soluble with a suitable organic solvent, such as ethyiene glycol monomethylether.
- Dopant 22, if used, can be ketonates, alkoxides, acetates, ⁇ -diketonates, or fluoro- ⁇ -diketonates of praeseodymium, holmium, and thulium dissolved in a suitable organic solvent such as ethyiene glycol monomethylether.
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- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- General Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
- Glass Compositions (AREA)
Abstract
The present invention is directed to methods of producing soot used in the manufacture of optical waveguides. Both non-aqueous liquid reactants and aqueous solutions containing one or more salts are delivered through an atomizing burner assembly to form a homogenous soot stream containing the oxides of the selected elements contained within the non-aqueous liquid reactant and the aqueous solution. The resulting multi-component soot is collected by conventional methods to form preforms used in the manufacture of optical waveguide fibers. Alternatively, an aqueous solution may be atomized with a gas at a first burner assembly to form an aerosol and a reactant vaporized for delivery to a second burner assembly. Preforms produced by the methods are also disclosed. The aqueous solution is preferably one comprising a metal salt, e.g. acetate, nitrate, sulfate, carbonate, chloride, hydroxide. The metal of the metal salt is preferably an alkali metal, an alkaline earth metal, lead, lanthanum, cobalt, antimony, erbium, aluminum, neodymium, praeseodymium.
Description
METHODS OF MANUFACTURING SOOT
FOR OPTICAL FIBER PREFORMS AND PREFORMS
MADE BY THE METHODS
FIELD OF THE INVENTION
The present invention relates to the formation of soot used in the manufacture of glass and, more particularly, to a method of delivering liquid precursors and other reactants into a flame to create soot for use in the manufacture of optical waveguides, and optical waveguides made by the method.
While the invention is subject to a wide range of glass soot applications, it is particularly well suited for the deposition of soot on a target to form preforms used in the manufacture of optical fibers, and will be particularly described in that connection.
BACKGROUND OF THE INVENTION
Various processes are known in the art that involve the production of oxides, and particularly, metal oxides from vaporous reactants. Such processes require a feedstock solution or precursor, a means of generating and transporting vapors of the feedstock solution (hereafter called vaporous reactants) and an oxidant to a conversion reaction site (also known as a soot reaction zone or combustion zone to those skilled in the art), and a means of catalyzing oxidation and combustion coincidentally to produce finely divided, spherical aggregates, called soot. This soot can be collected in any
number of ways, ranging from capture in a collection chamber to deposition on a rotating mandrel. The collected soot may be simultaneously or subsequently heat treated to form a non-porous, transparent, high purity glass article. This process is usually carried out with specialized equipment having a unique arrangement of nozzles, injectors, burners and/or burner assemblies.
Much of the initial research that led to the development of such processes focused on the production of bulk silica. Selection of the appropriate feedstock was an important aspect of that work. Consequently, it was at that time determined that a material capable of generating a vapor pressure of between 200-300 millimeters of mercury (mm Hg) at temperatures below approximately 100°C would be useful for making such bulk silica. The high vapor pressure of silicon tetrachloride (SiCI4) suggested its usefulness as a convenient vapor source for soot generation and launched the discovery and use of a series of similar chloride-based feedstocks. This factor, more than any other is responsible for the presently accepted use of SiCI4, GeCI4, POCI3, and BCI3 as feedstock vapor sources.
Use of these and other halide-based feedstocks as vapor sources, however, does have its drawbacks. The predominate drawback being the formation of hydrochloric acid (HCI) as a by-product of oxidation. HCI is not only detrimental to the deposition substrates and the reaction equipment, but to the environment as well. Overcoming this drawback, amongst others, led to the use of halide-free compounds as precursors or feedstocks for the production of soot for optical waveguides.
Although use of halide-free silicon compounds as feedstocks for fused silica glass production, as described in U.S. Patent Nos. 5,043,002 and
5,152,819, for example, avoids the formation of HCI, other problems remain, particularly when the soot is intended for the formation of optical waveguides. It has been found that, in the course of delivering a vaporized polyalkylsiloxane to the burner, high molecular weight species can be deposited as gels in the lines carrying the vaporous reactants to the burner, or within the burner itself.
This leads to a reduction in the deposition rate of the soot that is subsequently consolidated to a blank from which an optical waveguide fiber is drawn. It also
leads to imperfections in the blank that often produce defective and/or unusable optical waveguide fiber from the effected portions of the blank. An additional problem encountered while forming silica soot using siloxane feedstocks is the deposition of particulates having high molecular weights and high boiling points on the optical waveguide fiber blank. The build-up of these particulates results in "defect" or "clustered defect" imperfections that adversely affect the optical and structural quality of optical waveguides formed using the silica soot.
Other feedstocks, some of which are, and others of which may be useful in forming soot for the manufacture of optical waveguides are not currently acceptable alternatives to the halide-based and halide-free feedstocks for delivery via vapor deposition. Materials such as salts and those known as rare- earth elements, for example, are extremely unstable as vapors and often decompose before they can be delivered in their vapor phase. Rather than being delivered from the burner as a vapor, these elements tend to form solids that plane out of the solution.
Although it is often possible to deliver at least a percentage of these elements to the combustion zone as a vapor, it is technically very difficult. Elaborate systems incorporating expensive equipment are necessary to convert these elements to the vapor phase, and further, to deliver them to the combustion zone without leaving behind deposits of solids in the lines leading to the burners and in the burners themselves. Moreover, if multiple elements are being delivered as vapors and a specific percentage of each is necessary for the desired composition, it is difficult to control the delivery to provide that percentage since different elements have different vapor pressures.
U.S. Patent Application Serial Number 08/767,653, discloses that these and other limitations can be overcome by delivering a feedstock to an injector or burner in liquid form, atomizing the feedstock to form an aerosol containing fine droplets of the liquid feedstock, and converting the atomized liquid feedstock into soot at the combustion zone. The injectors, burners, and burner assemblies disclosed in U.S. Patent Application Serial Number 08/767,653 rely on very small orifices to deliver the liquid in a fine stream for proper
atomization. Because the feedstocks are delivered directly into the burner flame as liquids rather than vapors, the vapor pressures of the feedstocks are no longer limiting factors for delivery. Accordingly, many additional elements can now be delivered as feedstocks or dopants to form soot for use in the manufacture of optical waveguides.
A number of elements however, particularly those which are typically categorized as salts, are not easily delivered to a flame in liquid form as an organometallic compound. The purity requirements are often extremely high, as are the costs associated with attempting to obtain compounds of the required purity.
There is a need therefore, for a method of manufacturing soot for use in making optical waveguides, and particularly preforms for optical waveguide fibers that enables a user to precisely control the quantity of elements being delivered, and at the same time, eliminates gelling in the delivery lines. Further, what is needed is a liquid delivery method that produces glass soot containing metal oxides, traditional dopants, and salts in the required stoichiometry without requiring expensive and elaborate equipment.
SUMMARY OF THE INVENTION The present invention is directed to a method for delivering liquids and other reactants to a combustion zone adjacent a burner assembly to produce soot for use in the manufacture of glass. In a liquid delivery system, a liquid reactant, capable of being converted by thermal oxidative decomposition to glass, is provided and introduced directly into the combustion zone of a combustion burner, thereby forming finely divided amorphous soot. Examples of such liquid delivery systems are disclosed in U.S. Patent Application Serial No. 08/767,653, filed December 17, 1996, and entitled "Method and Apparatus for Forming Fused Silica by Combustion of Liquid Reactants"; U.S. Patent Application Serial No. 08/903,501 , filed July 30, 1997, and entitled "Method for Forming Silica by Combustion of Liquid Reactants Using Oxygen"; U.S. Patent
Application Serial No. 09/089,869, filed June 3, 1998, and entitled "Method and Apparatus for Forming Silica by Combustion of Liquid Reactants Using a
Heater"; U.S. Provisional Application Serial No. 60/068,255, filed December 19, 1997, entitled "Burner and Method for Producing Metal Oxide Soot"; and U.S. Provisional Application, filed July 31 , 1998, and entitled "Method and Apparatus for Forming Soot for the Manufacture of Glass," the specifications of which are hereby incorporated by reference. The amorphous soot can be captured in any number of ways, but is typically deposited on a receptor surface where, either substantially simultaneously with or subsequent to its deposition, the soot is consolidated into a body of fused glass. The body of glass may then be either used to make products directly from the fused body, or the fused body may be further treated, e.g., by forming an optical waveguide such as by drawing to make optical waveguide fiber as further described in, for example, U.S. Patent Application No. 08/574,961 entitled, "Method for Purifying polyalkylsiloxane and the Resulting Products", the specification of which is hereby incorporated by reference. The method of the present invention provides a number of advantages over other glass soot production methods known in the art. The present invention provides the capability of precisely varying and controlling the composition of the soot produced, which in turn provides for optical waveguide fibers having well defined and highly accurate index profiles, and other characteristics. The present invention further affords the industry with a method of concurrently delivering the greatest number of elements to a flame, to produce a multi-component glass soot. Any of a number of the organometallics, the rare earth elements, and now salts can all be concurrently delivered to a flame to produce homogenous soot. Similarly, these elements can be concurrently, or selectively delivered during the same soot production run to produce a preform meeting specific layering requirements. Accordingly, an optical fiber preform made by the method of the present invention has the advantage of containing precise quantities of elements, some of which have never been combined within a single optical waveguide fiber preform. To achieve these and other advantages, a non-aqueous liquid reactant and an aqueous solution are atomized to form an aerosol made up of numerous liquid droplets. The aerosol is delivered into a combustion zone and
reacted in the flame of the combustion zone to form finely divided glass soot particles.
In another aspect of the invention, a non-aqueous liquid reactant and an aqueous solution are delivered to a burner assembly. The non-aqueous liquid reactant and the aqueous solution are discharged from the burner assembly into a flame where they are reacted to form soot. The soot is deposited onto a target to form a preform.
In yet another aspect of the invention, an optical fiber preform is formed by the process of delivering a non-aqueous liquid reactant and an aqueous solution to a burner assembly. The non-aqueous liquid reactant and the aqueous solution are discharged from the burner assembly into a flame as an aerosol formed of a plurality of non-aqueous liquid reactant droplets and a plurality of liquid aqueous solution droplets. The droplets are reacted in the flame to produce soot and the soot is deposited on a target to form the preform.
In a further aspect of the invention, the delivery of an aqueous solution is combined with conventional vapor delivery. The aqueous solution is atomized with a gas at a burner assembly to form an aerosol made up of numerous liquid droplets, and another reactant is vaporized for delivery to the burner assembly. The vaporous reactant and the aerosol are reacted in a combustion zone adjacent the burner assembly to form finely divided glass soot.
Additional features and advantages of the invention will be set forth in the detailed description, which follows, and in part will be apparent from the description, or may be learned by practice of the invention. It will be understood by those skilled in the art that both the foregoing general description and the following detailed description are exemplary and explanatory in nature and are intended to provide further explanation of the invention as claimed. The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification. The drawings illustrate several embodiments of the
invention, and together with the description serve to explain the principles of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS FIG.1 schematically depicts a first preferred embodiment of a liquid delivery system used in the method of the present invention.
FIG. 2 schematically depicts a second preferred embodiment of a liquid delivery system used in the method of the present invention.
FIG. 3 schematically depicts a preferred embodiment of a combined vapor and liquid delivery system used in the method of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
A number of soot collection and soot deposition techniques are employed in the manufacture of glass products. While the present invention is capable of being employed in a number of these techniques, it is particularly well suited for those techniques used to deposit soot on a target to form glass preforms used in the manufacture of optical waveguides, and specifically optical waveguide fibers. It will be understood by those skilled in the art, however, that the method of the present invention can be used in the manufacture of planar waveguides as well.
During the manufacture of optical waveguide fibers, soot typically is uniformly deposited on or within a target. The collected soot is consolidated into a high purity glass preform and thereafter subjected to further processing steps such as drawing to form a thin fiber capable for carrying and directing light. Accordingly, the present invention will be described in this regard. It will be understood by those skilled in the optical waveguide fiber art, however, that there are other systems and variations of the depicted systems in which the present invention can be incorporated to perform the functions described and claimed herein. Reference will now be made in detail to the present preferred embodiments of the invention, examples of which are schematically illustrated in the accompanying drawings.
A first preferred embodiment of the system for delivering liquids into a combustion zone to form multi-component soots for use in the manufacture of glass is schematically depicted in FIG. 1. Liquid delivery system 10 includes an aqueous solution reservoir 12 containing aqueous solution 14, a non- aqueous liquid reactant reservoir 16 containing a non-aqueous liquid reactant
18, and optionally, a dopant reservoir 20 containing a dopant 22. In addition, liquid delivery system 10 includes an atomizing burner assembly 26 such as an atomizing burner assembly and the associated delivery mechanisms (hereinafter, "burner assembly") disclosed in U.S. Patent Application Serial No. 08/767,653, filed December 17, 1996, and entitled "Method and Apparatus for
Forming Fused Silica by Combustion of Liquid Reactants"; U.S. Patent Application Serial No. 08/903,501 , filed July 30, 1997, and entitled "Method for Forming Silica by Combustion of Liquid Reactants Using Oxygen"; U.S. Patent Application Serial No. 09/089,869, filed June 3, 1998, and entitled "Method and Apparatus for Forming Silica by Combustion of Liquid Reactants Using a
Heater"; U.S. Provisional Application Serial No. 60/068,255, filed December 19, 1997, entitled "Burner and Method for Producing Metal Oxide Soot"; and U.S. Provisional Application, filed July 31 , 1998, and entitled "Method and Apparatus for Forming Soot for the Manufacture of Glass", the specifications of which are hereby incorporated by reference.
In operation, aqueous solution 14, non-aqueous liquid reactant 18, and dopant 22 are mixed according to the desired stoichiometry and stored within their respective reservoirs 12, 16, and 20. Aqueous solution 14 preferably contains a water soluble salt such as an alkali metal nitrate, alkali metal carbonate, alkali metal sulfate, alkali metal acetate, alkaline earth metal nitrate, alkaline earth metal carbonate, alkaline earth metal sulfate, or alkaline earth metal acetate. More specifically, aqueous solution 14 contains one or more water soluble salts such as barium nitrate, barium acetate, barium chloride, strontium nitrate, strontium acetate, strontium chloride, antimony nitrate, antimony acetate, lead nitrate, lead carbonate, lead sulfate, lead acetate, lanthanum nitrate, lanthanum carbonate, lanthanum sulfate, lanthanum acetate, cobalt nitrate, cobalt acetate, cobalt chloride, neodymium nitrate,
neodymium praeseodymium chloride, potassium nitrate, potassium chloride, nitrate, cesium nitrate, cesium chloride, cesium sulfate, cesium hydroxide, calcium chloride aluminum nitrate, sodium nitrate, sodium chloride, erbium chloride, and erbium sulfate, but can contain other salts and/or other elements capable of being mixed in and delivered as an aqueous solution.
Non-aqueous liquid reactant 18 is preferably a liquid organometallic compound such as octamethylcyclotetrasiloxane, but can be a silicon alkoxide, a metal alkoxide, or other siliceous matrix material made soluble with a suitable organic solvent, such as ethyiene glycol monomethylether. Dopant 22, if used, can be ketonates, alkoxides, acetates, β-diketonates, or fluoro-β-diketonates of praeseodymium, holmium, and thulium dissolved in a suitable organic solvent such as ethyiene glycol monomethylether. Typically, the preferred dopants 22 are erbium, germanium, and other rare earth elements having properties beneficial for use in optical waveguide fibers. Aqueous solution 14, non-aqueous liquid reactant 18, and if desired, dopant 22 are delivered via liquid delivery lines 24 to burner assembly 26 in the desired quantities. Liquids 14, 18, and 22 are discharged from burner assembly 26 into flame 28 as atomized liquid droplets 30. Liquid droplets 30 are uniformly mixed in the atomization process and are reacted in the flame 28 to produce a soot stream 32. Soot stream 32 is preferably directed toward a target, such as rotating mandrel 34 as burner assembly 26 traverses along the length of rotating mandrel 34, resulting in the deposition of soot on rotating mandrel 34, which in turn forms a homogenous soot body 36 containing the desired quantities of oxides of the elements contained in aqueous solution 14, non-aqueous liquid reactant 18, and dopant 22.
A second preferred embodiment of the system for delivering liquids into a combustion zone to form multi-component soots for use in the manufacture of glass is schematically depicted in FIG. 2. Like the first preferred embodiment, liquid delivery system 40 includes an aqueous solution reservoir 42 for storing aqueous solution 44, a non-aqueous liquid reactant reservoir 46 for storing a non-aqueous liquid reactant 48, and optionally, a dopant reservoir 50 for storing a dopant 52. However, unlike the first preferred embodiment of
the invention, liquid delivery system 40 includes a first burner assembly 56 in selective fluid communication with non-aqueous liquid reactant reservoir 46 and dopant reservoir 50, and a second burner assembly 66 in fluid communication with aqueous solution reservoir 42. As described below, it will be understood by those skilled in the art that aqueous solution 44 and non- aqueous liquid reactant 48 can include one or more of the compounds described above with respect to the first preferred embodiment of the present invention.
In operation, aqueous solution 44 is selectively delivered to second burner assembly 66 and non-aqueous liquid reactant 48, and dopant 52, if desired, are selectively delivered to first burner assembly 56. First burner assembly 56 discharges atomized liquid droplets 60 into a flame 58 where the liquid droplets 60 are combusted to form a soot stream 62 containing a homogeneous mixture of oxides produced from the oxidization of the selected elements contained within non-aqueous liquid reactant 48 and dopant 52.
Second burner assembly 66 can be activated concurrently with or independently of first burner assembly 56 to discharge atomized liquid droplets 70 into a flame 68 to form a homogeneous soot stream 72 containing oxides of the element resulting from the oxidation of elements contained in aqueous solution 44. Soot stream 62 and 72 are preferably directed toward a target such as rotating mandrel 74, and soot from the soot streams 62 and 72 is deposited on rotating mandrel 74 in uniform layers as first burner assembly 56 and second burner assembly 66 traverse along the length of rotating mandrel 74. The resulting soot body 76 contains all of the oxides from soot streams 62 and 72 according to the rate at which they are delivered.
The multiple burner assemblies of this embodiment of the present invention generally facilitate a greater soot deposition rate than the first embodiment of the present invention. In addition, the spaced arrangement of the burner assemblies 56 and 66 enable the soot to be deposited in discrete layers which provides a controlled and cost effective way of making an optical waveguide having well defined index profiles and other optical characteristics.
FIG. 3 schematically depicts a preferred embodiment of a combined vapor and liquid delivery system 80 used in practicing the method of the present invention. The combined vapor and liquid delivery system 80 includes an aqueous solution reservoir 82 for storing aqueous solution 84 and a liquid delivery line 90 for placing a first burner assembly 94 in communication with aqueous solution 84. In addition, combined vapor and liquid delivery system 80 includes a vapor delivery system 86 for delivering a vaporous reactant 88 through liquid delivery line 92 to a second burner assembly 96. Vapor delivery system 86 can be any vapor delivery system known in the art such as, but not limited to, vapor delivery systems disclosed in US Patent No. 5,043,002, and
US Patent No. 3,698,936, the specifications of which are hereby incorporated by reference. Vaporized reactant 88 is preferably a halide-based feedstock such as, but not limited to, SiCI , or a halide-free based feedstock such as, but not limited to, octamethylcyclotetrasiloxane. Aqueous solution 14 preferably contains a water soluble salt such as an alkali metal nitrate, alkali metal carbonate, alkali metal sulfate, alkali metal acetate, alkaline earth metal nitrate, alkaline earth metal carbonate, alkaline earth metal sulfate, or an alkaline earth metal acetate. More specifically, aqueous solution 84 contains one or more water soluble salts such as barium nitrate, barium acetate, barium chloride, strontium nitrate, strontium acetate, strontium chloride, antimony nitrate, antimony acetate, lead nitrate, lead carbonate, lead sulfate, lead acetate, lanthanum nitrate, lanthanum carbonate, lanthanum sulfate, lanthanum acetate, cobalt nitrate, cobalt acetate, cobalt chloride, neodymium nitrate, neodymium chloride, potassium nitrate, potassium chloride, praeseodymium nitrate, cesium nitrate, cesium chloride, cesium sulfate, cesium hydroxide, calcium chloride, aluminum nitrate, sodium nitrate, sodium chloride, erbium chloride, and erbium sulfate, but can contain other salts and/or other elements capable of being mixed in and delivered as an aqueous solution.
In operation, aqueous solution 84 is selectively delivered to burner assembly 94, and vaporized reactant 88 is delivered to second burner assembly 96. Aqueous solution 84 is atomized with a gas such as air, but preferably oxygen, or oxygen together with an inert gas such as nitrogen, at
first burner assembly 94 to form an aerosol formed of a plurality of liquid droplets ranging generally in size from about 10 microns to 200 microns. The majority of droplets will typically be about 20 microns in size. Atomized liquid droplets 98 are discharged into a first flame 100 formed adjacent first burner assembly 94 where atomized liquid droplets 98 are combusted to form a first soot stream 102 containing a homogenous mixture of oxides produced from the oxidation of the selected elements contained within aqueous solution 84. Vaporous reactant 88 is delivered through vapor delivery line 92 and second burner assembly 96 as vapors 104 which are discharged into second flame 106 formed adjacent second burner assembly 96. Vapors 104 are combusted in second flame 106 to form a second soot stream 108 containing a homogenous mixture of oxides produced from the oxidation of the selected elements contained within vaporous reactant 88. First and second soot streams 102, 108, respectively, are directed toward a target, such as rotating mandrel 110, and the soot within soot streams 102 and 108 is deposited on rotating mandrel 110 in uniform layers as first burner assembly 94 and second burner assembly 96 traverse along the length of rotating mandrel 110. The resulting soot body 112 contains all the oxides from first and second soot streams 102 and 108, respectively, according to the rate at which they are delivered.
Although not shown in FIG. 3, an additional burner assembly and associated delivery mechanisms can be incorporated into the system shown in FIG. 3 to deliver additional dopants commonly used in the manufacture of soot for optical waveguide fibers. This embodiment of the present invention combines the higher soot deposition rate of vapor deposition with the unique optical characteristics provided by salts delivered in an aqueous solution. It will be understood by those skilled in the art that vaporous reactant 88 and aqueous solution 84 can be delivered into a common flame to produce a homogenous soot stream which can be collected in any manner commonly known in the art and thereafter further processed to form optical waveguides, and particularly preforms for optical waveguide fibers.
Although not shown in the drawing figures, it will be understood by those skilled in the art that the systems schematically depicted in FIGS. 1 , 2 and 3, are not limited to the number of burner assemblies and associated delivery mechanisms shown in the drawings. Each system can incorporate additional burner assemblies and associated delivery mechanisms to practice the methods of the present invention. Generally speaking, the greater the number of burner assemblies, the greater the soot deposition rate. Moreover, the present invention can be used in conjunction with other vapor delivery systems commonly known in the art to provide even greater flexibility in the manufacture of soot for optical waveguide fibers.
It will be apparent to those skilled in the art that various modifications and variations can be made in the methods of manufacturing soot for optical fiber preforms of the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents. In addition, the corresponding structures, materials, acts and equivalents of all means or step plus function elements in the claims below are intended to include any structure, material, or acts for performing the function in combination with other claimed elements as specifically claimed herein.
Claims
1. A method of making soot from which an optical fiber preform is made, said method comprising the steps of: a) atomizing a non-aqueous liquid reactant and an aqueous solution to form an aerosol comprising numerous liquid droplets, b) delivering said aerosol into a combustion zone; and c) reacting said aerosol in a flame provided at said combustion zone to form finely divided glass soot particles.
2. The method as claimed in claim 1 wherein said non-aqueous liquid reactant comprises a non-aqueous solution.
3. The method as claimed in claim 1 further comprising the step of delivering said non-aqueous liquid reactant and said aqueous solution to a single burner assembly prior to atomizing said non-aqueous liquid reactant and said aqueous solution.
4. The method as claimed in claim 1 , wherein prior to step a), the method further comprises the steps of: delivering said non-aqueous liquid reactant to a first burner assembly; and delivering said aqueous solution to a second burner assembly spaced from said first burner assembly.
5. The method as claimed in claim 4 further comprising the steps of: atomizing said non-aqueous liquid reactant at said first burner assembly to form a first aerosol; and atomizing said aqueous at said second burner assembly, to form a second aerosol.
6. The method as claimed in claim 5 further comprising the steps of: reacting said first aerosol in a first flame produced adjacent said first burner assembly; and reacting said second aerosol in a second flame produced adjacent said second burner assembly.
7. The method as claimed in claim 1 wherein said non-aqueous liquid reactant comprises at least one precursor and at least one dopant.
8. The method as claimed in claim 1 wherein said non-aqueous liquid reactant comprises a siloxane, and wherein said aqueous solution comprises a salt.
9. The method as claimed in claim 8 wherein said salt is selected from the group consisting of alkali metal nitrate, alkali metal carbonate, alkali metal sulfate, alkali metal acetate, alkaline earth metal nitrate, alkaline earth metal carbonate, alkaline earth metal sulfate, alkaline earth metal acetate, barium nitrate, barium acetate, barium chloride, strontium nitrate, strontium acetate, strontium chloride, antimony nitrate, antimony acetate, lead nitrate, lead carbonate, lead sulfate, lead acetate, lanthanum nitrate, lanthanum carbonate, lanthanum sulfate, lanthanum acetate, cobalt nitrate, cobalt acetate, cobalt chloride, neodymium nitrate, neodymium chloride, potassium nitrate, potassium chloride, praeseodymium nitrate, cesium nitrate, cesium chloride, cesium sulfate, cesium hydroxide, calcium nitrate, calcium chloride, aluminum nitrate, sodium nitrate, sodium chloride, erbium chloride, and erbium sulfate.
10. The method as claimed in claim 9 wherein said non-aqueous liquid reactant further comprises a dopant.
11. A process for making an optical fiber preform, said process comprising the steps of: a) delivering a non-aqueous liquid reactant and an aqueous solution to a burner assembly; b) discharging said non-aqueous liquid reactant and said aqueous solution from said burner assembly into a flame; c) reacting said non-aqueous liquid reactant and said aqueous solution in said flame to produce soot; and d) depositing said soot onto a rotating mandrel.
12. The process of claim 11 wherein step b) includes the step of atomizing said non-aqueous liquid reactant and said aqueous solution to form an aerosol comprising a plurality of non-aqueous liquid reactant droplets mixed with a plurality of liquid aqueous solution droplets.
13. The process of claim 12 wherein the step of atomizing occurs as said non-aqueous liquid reactant and said aqueous solution are discharged from said burner assembly.
14. The process of claim 11 wherein said burner assembly comprises a first burner assembly and a second burner assembly spaced from said first burner assembly, and wherein said non-aqueous liquid reactant is discharged from said first burner assembly as a first aerosol comprising a plurality of non- aqueous liquid reactant droplets, and wherein said aqueous solution is discharged from said second burner assembly as a second aerosol comprising a plurality of liquid aqueous solution droplets.
15. The process of claim 14 wherein said flame comprises a first flame adjacent said first burner assembly and a second flame adjacent said second burner assembly, and wherein said first aerosol is reacted in said first flame, and wherein said second aerosol is reacted in said second flame.
16. The process as claimed in claim 11 wherein said non-aqueous liquid reactant comprises at least one precursor and at least one dopant.
17. The method as claimed in claim 11 wherein said non-aqueous liquid reactant comprises a siloxane, and wherein said aqueous solution comprises a salt.
18. The method as claimed in claim 17 wherein said salt is selected from the group consisting of alkali metal nitrate, alkali metal carbonate, alkali metal sulfate, alkali metal acetate, alkaline earth metal nitrate, alkaline earth metal carbonate, alkaline earth metal sulfate, alkaline earth metal acetate, barium nitrate, barium acetate, barium chloride, strontium nitrate, strontium acetate, strontium chloride, antimony nitrate, antimony acetate, lead nitrate, lead carbonate, lead sulfate, lead acetate, lanthanum nitrate, lanthanum carbonate, lanthanum sulfate, lanthanum acetate, cobalt nitrate, cobalt acetate, cobalt chloride, neodymium nitrate, neodymium chloride, potassium nitrate, potassium chloride, praeseodymium nitrate, cesium nitrate, cesium chloride, cesium sulfate, cesium hydroxide, calcium nitrate, calcium chloride, aluminum nitrate, sodium nitrate, sodium chloride, erbium chloride, and erbium sulfate.
19. An optical fiber preform formed by the process of : a) delivering a non-aqueous liquid reactant and an aqueous solution to a burner assembly; b) discharging said non-aqueous liquid reactant and said aqueous solution from said burner assembly into a flame as an aerosol comprising a plurality of non-aqueous liquid reactant droplets and a plurality of liquid aqueous solution droplets; c) reacting said plurality of non-aqueous liquid reactant droplets and said plurality of liquid aqueous solution droplets in said flame to produce soot; and d) depositing said soot onto a target.
20. A method of making soot from which an optical fiber preform is made, said method comprising the steps of: a) atomizing an aqueous solution with a gas at a first burner assembly to form an aerosol comprising a plurality of droplets ranging in size from about 10 microns to 200 microns; b) vaporizing a reactant for delivery to a second burner assembly; and c) reacting the vaporous reactant and the aerosol within a combustion zone adjacent the first and second burner assemblies to form at least one soot stream.
21. The method as claimed in claim 20 wherein said reactant is selected from the group consisting of a halide-based silicon containing compound and a halide-free silicon-containing compound.
22. The method as claimed in claim 20 wherein said aqueous solution comprises a salt selected from the group consisting of alkali metal nitrate, alkali metal carbonate, alkali metal sulfate, alkali metal acetate, alkaline earth metal nitrate, alkaline earth metal carbonate, alkaline earth metal sulfate, alkaline earth metal acetate, barium nitrate, barium acetate, barium chloride, strontium nitrate, strontium acetate, strontium chloride, antimony nitrate, antimony acetate, lead nitrate, lead carbonate, lead sulfate, lead acetate, lanthanum nitrate, lanthanum carbonate, lanthanum sulfate, lanthanum acetate, cobalt nitrate, cobalt acetate, cobalt chloride, neodymium nitrate, neodymium chloride, potassium nitrate, potassium chloride, praeseodymium nitrate, cesium nitrate, cesium chloride, cesium sulfate, cesium hydroxide, calcium nitrate, calcium chloride, aluminum nitrate, sodium nitrate, sodium chloride, erbium chloride, and erbium sulfate.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US10651398P | 1998-10-30 | 1998-10-30 | |
US106513P | 1998-10-30 | ||
PCT/US1999/024304 WO2000026151A1 (en) | 1998-10-30 | 1999-10-18 | Methods of manufacturing soot for optical fiber preforms and preforms made by the methods |
Publications (1)
Publication Number | Publication Date |
---|---|
EP1135345A1 true EP1135345A1 (en) | 2001-09-26 |
Family
ID=22311815
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP99956587A Withdrawn EP1135345A1 (en) | 1998-10-30 | 1999-10-18 | Methods of manufacturing soot for optical fiber preforms and preforms made by the methods |
Country Status (10)
Country | Link |
---|---|
EP (1) | EP1135345A1 (en) |
JP (1) | JP2002528379A (en) |
KR (1) | KR20010089372A (en) |
CN (1) | CN1318038A (en) |
AU (1) | AU1316700A (en) |
BR (1) | BR9914871A (en) |
CA (1) | CA2344806A1 (en) |
ID (1) | ID28395A (en) |
WO (1) | WO2000026151A1 (en) |
ZA (1) | ZA200100713B (en) |
Families Citing this family (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6849334B2 (en) * | 2001-08-17 | 2005-02-01 | Neophotonics Corporation | Optical materials and optical devices |
US7575784B1 (en) | 2000-10-17 | 2009-08-18 | Nanogram Corporation | Coating formation by reactive deposition |
KR20040012671A (en) | 2000-10-17 | 2004-02-11 | 네오포토닉스 코포레이션 | Coating formation by reactive deposition |
US7491431B2 (en) | 2004-12-20 | 2009-02-17 | Nanogram Corporation | Dense coating formation by reactive deposition |
US20060130530A1 (en) * | 2004-12-21 | 2006-06-22 | Anderson James G | Method of doping silica glass with an alkali metal, and optical fiber precursor formed therefrom |
US8069690B2 (en) | 2005-12-16 | 2011-12-06 | Ofs Fitel, Llc | Apparatus and method for fabricating glass bodies using an aerosol delivery system |
GB2478307A (en) * | 2010-03-02 | 2011-09-07 | Heraeus Quartz Uk Ltd | Manufacture of silica glass |
JP5656469B2 (en) | 2010-06-23 | 2015-01-21 | 株式会社フジクラ | Glass base material manufacturing apparatus and manufacturing method |
CN106053705B (en) * | 2016-07-22 | 2018-01-16 | 黄石科森色谱科技有限公司 | A kind of preparation method of reverse-phase chromatography plate |
EP3950610A1 (en) * | 2020-08-06 | 2022-02-09 | Heraeus Quarzglas GmbH & Co. KG | Alternative fluorinating agent ii: fluid and soot accumulation |
Family Cites Families (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3883336A (en) * | 1974-01-11 | 1975-05-13 | Corning Glass Works | Method of producing glass in a flame |
CA1166527A (en) * | 1979-09-26 | 1984-05-01 | Shiro Takahashi | Method and apparatus for producing multi-component glass fiber preform |
JPS56155035A (en) * | 1980-04-25 | 1981-12-01 | Nippon Telegr & Teleph Corp <Ntt> | Light transmitting fiber and its preparation |
JPS57183089A (en) * | 1981-05-06 | 1982-11-11 | Nec Corp | Manufacture of quartz glass rod |
US5110335A (en) * | 1990-06-25 | 1992-05-05 | At&T Bell Laboratories | Method of glass soot deposition using ultrasonic nozzle |
US5212757A (en) * | 1991-10-03 | 1993-05-18 | At&T Bell Laboratories | Fatigue resistant optical fiber |
AU718737B2 (en) * | 1995-12-19 | 2000-04-20 | Corning Incorporated | Method and apparatus for forming fused silica by combustion of liquid reactants |
US6312656B1 (en) * | 1995-12-19 | 2001-11-06 | Corning Incorporated | Method for forming silica by combustion of liquid reactants using oxygen |
US5979185A (en) * | 1997-07-16 | 1999-11-09 | Corning Incorporated | Method and apparatus for forming silica by combustion of liquid reactants using a heater |
-
1999
- 1999-10-18 BR BR9914871-4A patent/BR9914871A/en not_active Application Discontinuation
- 1999-10-18 CN CN99810253A patent/CN1318038A/en active Pending
- 1999-10-18 KR KR1020017005329A patent/KR20010089372A/en active IP Right Grant
- 1999-10-18 AU AU13167/00A patent/AU1316700A/en not_active Abandoned
- 1999-10-18 JP JP2000579542A patent/JP2002528379A/en not_active Withdrawn
- 1999-10-18 EP EP99956587A patent/EP1135345A1/en not_active Withdrawn
- 1999-10-18 CA CA002344806A patent/CA2344806A1/en not_active Abandoned
- 1999-10-18 WO PCT/US1999/024304 patent/WO2000026151A1/en active IP Right Grant
- 1999-10-18 ID IDW00200101010A patent/ID28395A/en unknown
-
2001
- 2001-01-25 ZA ZA200100713A patent/ZA200100713B/en unknown
Non-Patent Citations (1)
Title |
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See references of WO0026151A1 * |
Also Published As
Publication number | Publication date |
---|---|
KR20010089372A (en) | 2001-10-06 |
CA2344806A1 (en) | 2000-05-11 |
AU1316700A (en) | 2000-05-22 |
BR9914871A (en) | 2001-07-03 |
JP2002528379A (en) | 2002-09-03 |
CN1318038A (en) | 2001-10-17 |
WO2000026151A1 (en) | 2000-05-11 |
ID28395A (en) | 2001-05-17 |
ZA200100713B (en) | 2001-07-17 |
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