WO2003059808A1 - Method of preparing very pure silicon chloride and/or germanium chloride - Google Patents
Method of preparing very pure silicon chloride and/or germanium chloride Download PDFInfo
- Publication number
- WO2003059808A1 WO2003059808A1 PCT/NL2002/000716 NL0200716W WO03059808A1 WO 2003059808 A1 WO2003059808 A1 WO 2003059808A1 NL 0200716 W NL0200716 W NL 0200716W WO 03059808 A1 WO03059808 A1 WO 03059808A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- chloride
- substrate tube
- germanium
- interior
- preparing
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10778—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B9/00—General methods of preparing halides
- C01B9/02—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G17/00—Compounds of germanium
- C01G17/04—Halides of germanium
-
- 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]
- C03B37/018—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] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
- C03B37/01807—Reactant delivery systems, e.g. reactant deposition burners
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
- C03C1/022—Purification of silica sand or other minerals
-
- 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
- C03B2201/08—Doped silica-based glasses doped with boron or fluorine or other refractive index decreasing dopant
- C03B2201/12—Doped silica-based glasses doped with boron or fluorine or other refractive index decreasing dopant doped with fluorine
-
- 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
- C03B2201/31—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with germanium
-
- 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
Definitions
- the present invention relates to a method of preparing very pure silicon chloride and/or germanium chloride.
- the present invention furthermore relates to a method of depositing one or more glass layers on the interior of a substrate tube of quartz glass, in which one or more reactive gases and an oxygen-containing gas are supplied to said substrate tube, as well as to a method of manufacturing optical fibres, in which the substrate tube is contracted into a massive rod followi g the deposition of one or more glass layers on the interior of a substrate tube, from which rod optical fibres are drawn.
- a substrate tube of quartz glass in which one or more reactive gases and an oxygen-containing gas are supplied to the substrate tube, is known per se, for example from US patent No 6,260,510 to the present applicant.
- a substrate tube consisting of quartz glass for example, is coated on its inside surface with layers of doped silica (e.g. germanium-doped silica).
- doped silica e.g. germanium-doped silica
- Such a deposition reaction can be carried out by positioning the substrate tube along the cylindrical axis of the resonant cavity and subsequently flushing the inside of the tube with a gaseous mixture comprising, for example, oxygen, silicon chloride and germanium chloride.
- a localised plasma is generated within the resonant caviity so as to obtain direct deposition of germanium-doped silica on the inside surface of the substrate tube. Because such a deposition only takes place in the vicinity of the localised plasma, the resonant cavity (and thus the plasma) must be moved along the cylindrical axis of the substrate tube in order to achieve a uniform coating of the substrate tube along the entire length thereof.
- the substrate tube is thermally treated in such a manner that it will contract into a rod, which rod is also called an optical preform. If an end of the optical preform is heated so that it will become molten, an optical fibre can be drawn from the optical preform and be wound on a reel.
- Such an optical fibre thus has a core and a cladding portion corresponding to those of the optical preform. Because a germanium-doped core has a higher refractive index than, for example, the undoped cladding, the fibre can act as a waveguide, e.g. for use in propagating optical telecommunications signals. It should be noted, however, that the gaseous mixture flushed through the interior of the substrate tube may also contain other components; e.g. the addition of a fluorine-containing compound causes a reduction in the refractive index of the doped silica.
- the use of such an optical fibre for telecommunication purposes requires that the fibre is essentially free from impurities, because such impurities can cause serious attenuation of the signal being propagated if such an optical fibre is used in great lengths. Consequently it is desirable not only that the aforesaid PCVD process is very uniform, but that also the reactive gases used for the deposition process do not contain any undesirable impurities.
- the chloride compounds, in particular silicon chloride and germanium chloride, which are used as starting materials in the manufacture of glass fibres are generally slightly contaminated with small amounts of si lanes, such as trichloromethyl silane (SiCl 3 )CH 3 ), SiHCl 3 and the like.
- the hydrogen atoms can thus form -OH compounds or -bindings in the glass layers deposited on the interior of the substrate tube, which -OH compounds have a strong adverse effect on the transmission spectre of a fibre drawn from an optical preform, in particular due to the high absorption level thereof at 1240 nm and 1385 nm.
- Such absorption losses resulting from the minor presence of impurities in the gaseous starting materials can amount to 10 - 20 dB/km at a wavelength of 1385 nm.
- the object of the present invention is to provide a method which leads to a reduction of the number of -OH compounds in an optical fibre without resulting in increased Rayleigh scattering.
- Another object of the present invention is to provide a method of preparing a very pure starting material, which starting material in particular comprises silicon chloride and/or germanium chloride and which is used as a reactive gas in a deposition process, in particular a PCVD process.
- Yet another object is to provide a massive rod from which optical fibres can be obtained, which fibres exhibit a lower attenuation loss than the optical fibres that are known from the prior art.
- the invention as referred to in the introduction is characterized in that silicon chloride and/or germanium chloride is reacted with a fluorinating agent, which may or may not take place in the presence of a suitable catalyst.
- the impurities present in the starting material such as for example si lane compounds, are converted into CF compounds and Si-F compounds.
- the hydrogen atoms present in the starting material will be substituted for fluorine atoms, as a result of which the glass layers to be deposited during the deposition process will not contain any undesirable -OH compounds.
- the fluorinating agent from the group consisting of F 2 , SiF, SF 6a BF 3 and freons, such as CF 2 C1 2 , CF 4 and C 2 F 5 .
- freons such as CF 2 C1 2 , CF 4 and C 2 F 5 .
- the selection of a fluorinating agent is in particular dictated by the high reactivity, which creativity is in particular desirable with a view to reducing the number of impurities present in the starting materials, usually at ppm level, to practically zero.
- the thus fluorinated germanium chloride and/or silicon chloride and an oxygen-containing gas are supplied to the interior of the substrate tube, so that any impurities present in the starting materials, in particular silanes, hydrocarbon compounds and hydrogen-containing compounds, are converted into the less harmful fluorocarbon compounds and/or Si-F compounds.
- the present invention furthermore relates to a method of depositing one or more glass layers on the interior of a substrate tube, in which one or more reactive gases and an oxygen-containing gas are supplied to the substrate tube, which method is characterized in that silicon chloride and/or germanium chloride obtained in accordance with the present method are supplied to the substrate tube as the reactive gas.
- Undesirable incorporation of OH compounds in the optical fibre which OH compounds have a strong adverse effect on the transmission spectre of an optical glass fibre due to a high absorption level at 1240 nm and 1385 nm, is prevented by supplying such a reactive gas treated with a fluorinating agent to the interior of the substrate tube.
- the present invention furthermore relates to a method of manufacturing optical fibres from an optical preform as referred to in the introduction, which method is characterized in that the optical preform has been obtained by contracting the substrate tube formed in accordance with the present invention into a massive rod, from which massive rod the optical fibre is drawn.
- a preform for a single mode fibre was obtained.
- Said preform was manufactured by depositing a number of layers of undoped silica on the interior of a quartz tube, using fluorinated silicon tetrachloride obtained in accordance with the present method as the reactive gas. This treatment was followed by the deposition of layers of silica doped with germanium dioxide on the previously deposited layers for forming the light conducting core of the optical fibre. Also in this case fluorinated silicon tetrachloride and fluorinated germanium tetrachloride obtained in accordance with the present method were used as reactive gases for the deposition process.
- the attenuation losses due to the absorption of OH groups at 1385 nm in the present optical fibre amounted to less than 1 dB/km, which result means a significant improvement in comparison with attenuation losses of 10 - 20 dB/km measured on prior art optical fibres.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Geochemistry & Mineralogy (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
Abstract
The present invention relates to a method of preparing very pure silicon chloride and/or germanium chloride by reaction with a fluorinating agent. The present invention furthermore relates to a method of depositing one or more glass layers on the interior of a substrate tube of quartz glass, in which one or more reactive gases and an oxygen-containing gas are supplied to said substrate tube, as well as to a method of manufacturing optical fibres.
Description
Method of preparing very pure silicon chloride and/or germanium chloride.
The present invention relates to a method of preparing very pure silicon chloride and/or germanium chloride. The present invention furthermore relates to a method of depositing one or more glass layers on the interior of a substrate tube of quartz glass, in which one or more reactive gases and an oxygen-containing gas are supplied to said substrate tube, as well as to a method of manufacturing optical fibres, in which the substrate tube is contracted into a massive rod followi g the deposition of one or more glass layers on the interior of a substrate tube, from which rod optical fibres are drawn.
From European patent application No 0 488 765 there is known a method of purifying silicon tetrachloride contaminated with methylchlorosi lanes, wherein said purification is carried out by first exposing the silicon tetrachloride to light in the presence of chlorine, thereby chlorinating the methyl groups, and finally removing the chlorinated methylchlorosi lanes through distillation.
From US patent No 4,310,341 there is known a method for the removal of -OH impurities from precursor materials from which optical fibres are made, which method comprises the step of contacting a mixture of a first reactant, consisting of PC13 and/or PBr3, and a second reactant, consisting of chlorine and bromine, with silicon chloride or germanium chloride, for example.
From German Offenlegungsschrift No 2805824 there is known a method of purifying silicon tetrachloride, wherein silicon tetrachloride is exposed to light in the presence of at least one halogen, with only chlorine, bromine and iodine beeing mentioned as suitable halogens. The necessity of said exposure to light in this reaction is demonstrated in the experimental results, the comparative example was carried out without exposure to light.
From European patent application No 0 189 224 there is known a process for the removal of hydrogen from hydrogen compounds dissolved in silicon tetrachloride or germanium tetrachloride by chlorinating said hydrogen compounds, wherein said chlorination is carried out at a very high temperature of more than 1000 'C.
From US patent No 3,188,168 there is known a method of purifying silicon compounds, in which a silicon-containing material is brought into contact with a halogen selected from the group consisting of iodine, bromine and chlorine. It is explicitly mentioned in said document that fluorine cannot be considered to be a suitable candidate for carrying out the purification reaction, because such a compound would be highly reactive.
The deposition of glass layers on the interior of a substrate tube of quartz glass, in which one or more reactive gases and an oxygen-containing gas are supplied to the substrate tube, is known per se, for example from US patent No 6,260,510 to the present applicant. According to the method that is known therefrom, a substrate tube consisting of quartz glass, for example, is coated on its inside surface with layers of doped silica (e.g. germanium-doped silica). Such a deposition reaction can be carried out by positioning the substrate tube along the cylindrical axis of the resonant cavity and subsequently flushing the inside of the tube with a gaseous mixture comprising, for example, oxygen, silicon chloride and germanium chloride. Subsequently, a localised plasma is generated within the resonant caviity so as to obtain direct deposition of germanium-doped silica on the inside surface of the substrate tube. Because such a deposition only takes place in the vicinity of the localised plasma, the resonant cavity (and thus the plasma) must be moved along the cylindrical axis of the substrate tube in order to achieve a uniform coating of the substrate tube along the entire length thereof. Once the deposition of layers is complete, the substrate tube is thermally treated in such a manner that it will contract into a
rod, which rod is also called an optical preform. If an end of the optical preform is heated so that it will become molten, an optical fibre can be drawn from the optical preform and be wound on a reel. Such an optical fibre thus has a core and a cladding portion corresponding to those of the optical preform. Because a germanium-doped core has a higher refractive index than, for example, the undoped cladding, the fibre can act as a waveguide, e.g. for use in propagating optical telecommunications signals. It should be noted, however, that the gaseous mixture flushed through the interior of the substrate tube may also contain other components; e.g. the addition of a fluorine-containing compound causes a reduction in the refractive index of the doped silica.
The use of such an optical fibre for telecommunication purposes requires that the fibre is essentially free from impurities, because such impurities can cause serious attenuation of the signal being propagated if such an optical fibre is used in great lengths. Consequently it is desirable not only that the aforesaid PCVD process is very uniform, but that also the reactive gases used for the deposition process do not contain any undesirable impurities. The chloride compounds, in particular silicon chloride and germanium chloride, which are used as starting materials in the manufacture of glass fibres, are generally slightly contaminated with small amounts of si lanes, such as trichloromethyl silane (SiCl3)CH3), SiHCl3 and the like. During the above- discussed chemical vapour deposition, the hydrogen atoms can thus form -OH compounds or -bindings in the glass layers deposited on the interior of the substrate tube, which -OH compounds have a strong adverse effect on the transmission spectre of a fibre drawn from an optical preform, in particular due to the high absorption level thereof at 1240 nm and 1385 nm. Such absorption losses resulting from the minor presence of impurities in the gaseous starting materials can amount to 10 - 20 dB/km at a wavelength of 1385 nm.
Although a few methods for preventing the incorporation of
such -OH groups in the optical glass fibre are known from the prior art, for example comprising the carrying out of a chlorine treatment after the deposition process in the case of porous glass structures, as known from US patent No 4, 675,038, or the addition of fluorine during the chemical vapour deposition reaction, as known from European patent application No 0 127 227, said two prior art methods have this drawback that an additional amount of, respectively, chlorine or fluorine finds its way into the final glass structure, as a result of which the attenuation losses due to ayleigh scattering will increase.
The object of the present invention is to provide a method which leads to a reduction of the number of -OH compounds in an optical fibre without resulting in increased Rayleigh scattering.
Another object of the present invention is to provide a method of preparing a very pure starting material, which starting material in particular comprises silicon chloride and/or germanium chloride and which is used as a reactive gas in a deposition process, in particular a PCVD process.
Yet another object is to provide a massive rod from which optical fibres can be obtained, which fibres exhibit a lower attenuation loss than the optical fibres that are known from the prior art.
The invention as referred to in the introduction is characterized in that silicon chloride and/or germanium chloride is reacted with a fluorinating agent, which may or may not take place in the presence of a suitable catalyst.
As a result of the treatment of the chloride-containing starting materials, in particular silicon chloride and/or germanium chloride, with a fluorinating agent, the impurities present in the starting material, such as for example si lane compounds, are converted into CF compounds and Si-F compounds. Thus the hydrogen atoms present in the starting material will be substituted for fluorine atoms, as a result of which the glass layers to be deposited during the deposition process
will not contain any undesirable -OH compounds.
It is in particular preferable to select the fluorinating agent from the group consisting of F2, SiF, SF6a BF3 and freons, such as CF2C12, CF4 and C2F5. It should be understood that the aforesaid freons are merely mentioned by way of example and should not be considered as being limitative. The selection of a fluorinating agent is in particular dictated by the high reactivity, which creativity is in particular desirable with a view to reducing the number of impurities present in the starting materials, usually at ppm level, to practically zero. In addition to that it is desirable in specific embodiments to incorporate fluorine as a dopant in the glass layers to be deposited, so that the presence of the fluorinated component in the precursor material will not be a drawback in such a situation and that the hydrogen will escape in the form of HF or H2.
Although a thermally initiated deposition process for the preparation of fluorine-doped silica for an optical fibre, in which silicon tetrachloride is supplied to the interior of the substrate tube together with a fluorinating agent, is known from US patent No 4,735,648, it is not known from said US patent to have the gaseous starting material, in particular germanium chloride and/or silicon chloride, react with a fluorinating agent first, viz. prior to the introduction thereof to the substrate tube, after which the thus fluorinated germanium chloride and/or silicon chloride and an oxygen-containing gas are supplied to the interior of the substrate tube, so that any impurities present in the starting materials, in particular silanes, hydrocarbon compounds and hydrogen-containing compounds, are converted into the less harmful fluorocarbon compounds and/or Si-F compounds.
The present invention furthermore relates to a method of depositing one or more glass layers on the interior of a substrate tube, in which one or more reactive gases and an oxygen-containing gas are supplied to the substrate tube, which method is characterized in that
silicon chloride and/or germanium chloride obtained in accordance with the present method are supplied to the substrate tube as the reactive gas.
Undesirable incorporation of OH compounds in the optical fibre, which OH compounds have a strong adverse effect on the transmission spectre of an optical glass fibre due to a high absorption level at 1240 nm and 1385 nm, is prevented by supplying such a reactive gas treated with a fluorinating agent to the interior of the substrate tube.
The present invention furthermore relates to a method of manufacturing optical fibres from an optical preform as referred to in the introduction, which method is characterized in that the optical preform has been obtained by contracting the substrate tube formed in accordance with the present invention into a massive rod, from which massive rod the optical fibre is drawn.
The present invention will be explained hereinafter by means of an example; it should be noted, however, that the example is merely given by way of illustration and should not be construed as constituting a limitation of the invention.
Example.
Using the method described in US patent No 6,260,510, a preform for a single mode fibre was obtained. Said preform was manufactured by depositing a number of layers of undoped silica on the interior of a quartz tube, using fluorinated silicon tetrachloride obtained in accordance with the present method as the reactive gas. This treatment was followed by the deposition of layers of silica doped with germanium dioxide on the previously deposited layers for forming the light conducting core of the optical fibre. Also in this case fluorinated silicon tetrachloride and fluorinated germanium tetrachloride obtained in accordance with the present method were used as reactive gases for the deposition process. The tube thus formed, with deposited layers present
on the interior thereof, was contracted into a massive rod in a manner known to those skilled in the art, from which rod an optical fibre was drawn. The attenuation losses due to the absorption of OH groups at 1385 nm in the present optical fibre amounted to less than 1 dB/km, which result means a significant improvement in comparison with attenuation losses of 10 - 20 dB/km measured on prior art optical fibres.
Claims
1. A method of preparing very pure silicon chloride and/or germanium chloride, characterized in that silicon chloride and/or germanium chloride is reacted with a fluorinating agent, which may or may not take place in the presence of a suitable catalyst.
2. A method according to claim 1, characterized in that the fluorinating agent is selected from the group consisting of F2, SiF4, SF6, BF3 and freons, such as CF2C12, CF4 and C2F6.
3. A method of depositing one or more glass layers on the interior of a substrate tube of quartz glass, in which one or more reactive gases and an oxygen-containing gas are supplied to said substrate tube, characterized in that a reactive gas containing silicon chloride and/or germanium chlori e obtained in accordance with the method defined in any one or more of the preceding claims 1-2 is supplied to the substrate tube.
4. A method of manufacturing optical fibres, in which the substrate tube is contracted into a massive rod following the deposition of one or more glass layers on the interior of a substrate tube, from which rod optical fibres are drawn, characterized in that said substrate tube has been obtained in accordance with the method defined in claim 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2002343844A AU2002343844A1 (en) | 2001-11-15 | 2002-11-08 | Method of preparing very pure silicon chloride and/or germanium chloride |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| NL1019371A NL1019371C2 (en) | 2001-11-15 | 2001-11-15 | Process for the preparation of highly pure silicon chloride and / or germanium chloride. |
| NL1019371 | 2001-11-15 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2003059808A1 true WO2003059808A1 (en) | 2003-07-24 |
Family
ID=19774314
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/NL2002/000716 WO2003059808A1 (en) | 2001-11-15 | 2002-11-08 | Method of preparing very pure silicon chloride and/or germanium chloride |
Country Status (3)
| Country | Link |
|---|---|
| AU (1) | AU2002343844A1 (en) |
| NL (1) | NL1019371C2 (en) |
| WO (1) | WO2003059808A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106730964A (en) * | 2015-11-25 | 2017-05-31 | 衡阳恒荣高纯半导体材料有限公司 | A kind of distilling apparatus for producing high-purity germanium tetrachloride |
| TWI822886B (en) * | 2018-11-14 | 2023-11-21 | 德商贏創運營有限公司 | Tris(trichlorosilyl)dichlorogallylgermane, process for the preparation thereof and use thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3188168A (en) * | 1962-06-04 | 1965-06-08 | Union Carbide Corp | Purification of silicon compounds |
| DE2805824A1 (en) * | 1977-02-14 | 1978-08-17 | Shinetsu Chemical Co | Silicon tetra:chloride purificn. to remove silane cpds. - esp. where silane cpds. cause attenuation in quartz optical fibre mfr., by irradiation with light in presence of halogen |
| US4310341A (en) * | 1980-09-12 | 1982-01-12 | Bell Telephone Laboratories, Incorporated | Removal of --OH impurities from fiber optic precursor materials |
| EP0189224A2 (en) * | 1985-01-25 | 1986-07-30 | Philips Patentverwaltung GmbH | Process for removing hydrogen from hydrogenated compounds dissolved in silicon tetrachloride or germanium tetrachloride |
| US4735648A (en) * | 1984-07-25 | 1988-04-05 | Stc Plc | Optical fibre manufacture |
| EP0488765A1 (en) * | 1990-11-29 | 1992-06-03 | Shin-Etsu Chemical Co., Ltd. | Purification of silicon tetrachloride |
| US6260510B1 (en) * | 1997-12-31 | 2001-07-17 | Plasma Optical Fibre B.V. | PCVD apparatus and method of manufacturing an optical fiber, a preform rod and a jacket tube as well as the optical fiber manufactured therewith |
-
2001
- 2001-11-15 NL NL1019371A patent/NL1019371C2/en not_active IP Right Cessation
-
2002
- 2002-11-08 WO PCT/NL2002/000716 patent/WO2003059808A1/en not_active Application Discontinuation
- 2002-11-08 AU AU2002343844A patent/AU2002343844A1/en not_active Abandoned
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3188168A (en) * | 1962-06-04 | 1965-06-08 | Union Carbide Corp | Purification of silicon compounds |
| DE2805824A1 (en) * | 1977-02-14 | 1978-08-17 | Shinetsu Chemical Co | Silicon tetra:chloride purificn. to remove silane cpds. - esp. where silane cpds. cause attenuation in quartz optical fibre mfr., by irradiation with light in presence of halogen |
| US4310341A (en) * | 1980-09-12 | 1982-01-12 | Bell Telephone Laboratories, Incorporated | Removal of --OH impurities from fiber optic precursor materials |
| US4735648A (en) * | 1984-07-25 | 1988-04-05 | Stc Plc | Optical fibre manufacture |
| EP0189224A2 (en) * | 1985-01-25 | 1986-07-30 | Philips Patentverwaltung GmbH | Process for removing hydrogen from hydrogenated compounds dissolved in silicon tetrachloride or germanium tetrachloride |
| EP0488765A1 (en) * | 1990-11-29 | 1992-06-03 | Shin-Etsu Chemical Co., Ltd. | Purification of silicon tetrachloride |
| US6260510B1 (en) * | 1997-12-31 | 2001-07-17 | Plasma Optical Fibre B.V. | PCVD apparatus and method of manufacturing an optical fiber, a preform rod and a jacket tube as well as the optical fiber manufactured therewith |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106730964A (en) * | 2015-11-25 | 2017-05-31 | 衡阳恒荣高纯半导体材料有限公司 | A kind of distilling apparatus for producing high-purity germanium tetrachloride |
| TWI822886B (en) * | 2018-11-14 | 2023-11-21 | 德商贏創運營有限公司 | Tris(trichlorosilyl)dichlorogallylgermane, process for the preparation thereof and use thereof |
| US11851342B2 (en) | 2018-11-14 | 2023-12-26 | Evonik Operations Gmbh | Tris(trichlorosily1)dichlorogallylgermane, process for the preparation thereof and use thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| AU2002343844A1 (en) | 2003-07-30 |
| NL1019371C2 (en) | 2003-05-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP0547335B1 (en) | Method of making fluorine/boron doped silica tubes | |
| EP0249230B1 (en) | Glass preform for dispersion shifted single mode optical fiber and method for the production of the same | |
| EP0161680B1 (en) | Method for producing glass preform for optical fiber | |
| EP0198510B1 (en) | Method of producing glass preform for optical fiber | |
| EP0182250A1 (en) | Method for producing glass preform for optical fiber | |
| EP2294021B1 (en) | Process for preparing an optical preform | |
| EP0196671A1 (en) | Method of producing glass preform for optical fiber | |
| EP0177040B1 (en) | Method for producing glass preform for optical fiber | |
| CN103864290A (en) | Method for activating an inner surface of a hollow glass substrate tube for the manufacturing of an optical fiber preform | |
| US20080028799A1 (en) | Optical fiber preform manufacturing method | |
| WO2003059808A1 (en) | Method of preparing very pure silicon chloride and/or germanium chloride | |
| EP1270522B1 (en) | Method for fabricating optical fiber from preforms, using control of the partial pressure of oxygen during preform dehydration | |
| EP0164127B1 (en) | Method for producing glass preform for optical fibers | |
| US20020108404A1 (en) | Drying agent and improved process for drying soot preforms | |
| US6813907B2 (en) | Fluorine doping a soot preform | |
| KR100545813B1 (en) | Optical fiber preform manufacturing method using crystal chemical vapor deposition including dehydration and dechlorination process and optical fiber manufactured by this method | |
| JP2003300744A (en) | Method for manufacturing optical fiber, and optical fiber | |
| KR20050065398A (en) | Method of manufacturing fluorine doped silica glass article, and method of manufacturing optical fiber preform and optical fiber using the method, and optical fiber made by such method | |
| NL2004874C2 (en) | METHOD FOR MANUFACTURING A PRIMARY FORM | |
| JPH0476936B2 (en) | ||
| EP2660212A1 (en) | Optical fiber preform manufacturing method | |
| EP0135126B1 (en) | Preparation of glass for optical fibers | |
| JPH0479981B2 (en) | ||
| EP3118172B1 (en) | Method for activating an inner surface of a substrate tube for the manufacturing of an optical fiber preform | |
| NL1022140C2 (en) | Deposition of glass layers inside tube using reactive gases, useful for preparing optical fibres, comprises treating glass forming compounds with deuterium before deposition |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| AK | Designated states |
Kind code of ref document: A1 Designated state(s): AE AG AL AM AT AU AZ BA BB BG BR BY BZ CA CH CN CO CR CU CZ DE DK DM DZ EC EE ES FI GB GD GE GH GM HR HU ID IL IN IS JP KE KG KP KR KZ LC LK LR LS LT LU LV MA MD MG MK MN MW MX MZ NO NZ OM PH PL PT RO RU SC SD SE SG SI SK SL TJ TM TN TR TT TZ UA UG US UZ VC VN YU ZA ZM ZW |
|
| AL | Designated countries for regional patents |
Kind code of ref document: A1 Designated state(s): GH GM KE LS MW MZ SD SL SZ TZ UG ZM ZW AM AZ BY KG KZ MD RU TJ TM AT BE BG CH CY CZ DE DK EE ES FI FR GB GR IE IT LU MC NL PT SE SK TR BF BJ CF CG CI CM GA GN GQ GW ML MR NE SN TD TG |
|
| DFPE | Request for preliminary examination filed prior to expiration of 19th month from priority date (pct application filed before 20040101) | ||
| 121 | Ep: the epo has been informed by wipo that ep was designated in this application | ||
| 122 | Ep: pct application non-entry in european phase | ||
| NENP | Non-entry into the national phase |
Ref country code: JP |
|
| WWW | Wipo information: withdrawn in national office |
Country of ref document: JP |