WO2013047834A1 - ガラス微粒子堆積体及びガラス母材の製造方法 - Google Patents

ガラス微粒子堆積体及びガラス母材の製造方法 Download PDF

Info

Publication number
WO2013047834A1
WO2013047834A1 PCT/JP2012/075240 JP2012075240W WO2013047834A1 WO 2013047834 A1 WO2013047834 A1 WO 2013047834A1 JP 2012075240 W JP2012075240 W JP 2012075240W WO 2013047834 A1 WO2013047834 A1 WO 2013047834A1
Authority
WO
WIPO (PCT)
Prior art keywords
glass
raw material
burner
gas
temperature
Prior art date
Application number
PCT/JP2012/075240
Other languages
English (en)
French (fr)
Japanese (ja)
Inventor
石原　朋浩
古川　将人
Original Assignee
住友電気工業株式会社
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from JP2012008158A external-priority patent/JP5682577B2/ja
Priority claimed from JP2012008303A external-priority patent/JP5720585B2/ja
Priority claimed from JP2012012384A external-priority patent/JP5953767B2/ja
Priority claimed from JP2012175012A external-priority patent/JP5737241B2/ja
Priority claimed from JP2012175011A external-priority patent/JP5737240B2/ja
Priority claimed from JP2012175010A external-priority patent/JP5737239B2/ja
Priority to US14/348,186 priority Critical patent/US9630872B2/en
Priority to CN201280048193.7A priority patent/CN103842303B/zh
Application filed by 住友電気工業株式会社 filed Critical 住友電気工業株式会社
Priority to EP12834881.0A priority patent/EP2762456B1/en
Priority to IN2480CHN2014 priority patent/IN2014CN02480A/en
Publication of WO2013047834A1 publication Critical patent/WO2013047834A1/ja
Priority to US15/495,334 priority patent/US10604439B2/en

Links

Images

Classifications

    • 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
    • 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
    • C03B2207/00—Glass deposition burners
    • C03B2207/04—Multi-nested ports
    • C03B2207/06—Concentric circular ports
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/04—Multi-nested ports
    • C03B2207/08—Recessed or protruding ports
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/20—Specific substances in specified ports, e.g. all gas flows specified
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/20—Specific substances in specified ports, e.g. all gas flows specified
    • C03B2207/22—Inert gas details
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/20—Specific substances in specified ports, e.g. all gas flows specified
    • C03B2207/24—Multiple flame type, e.g. double-concentric flame
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/80—Feeding the burner or the burner-heated deposition site
    • C03B2207/81—Constructional details of the feed line, e.g. heating, insulation, material, manifolds, filters
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57—Improving the yield, e-g- reduction of reject rates

Definitions

  • the present invention is a glass for producing a glass fine particle deposit by depositing glass fine particles on a starting rod by VAD method (vapor phase axis attaching method), OVD method (external attaching method), MMD method (multi-burner multilayer attaching method) or the like.
  • VAD method vapor phase axis attaching method
  • OVD method exitternal attaching method
  • MMD method multi-burner multilayer attaching method
  • the present invention relates to a method for producing a fine particle deposit and a method for producing a glass base material by heating the glass fine particle deposit to be transparent.
  • a deposition process for producing a glass fine particle deposit by the OVD method, the VAD method, or the like, and a transparent glass body (base material) for producing a transparent glass body by heating the glass fine particle deposit there is known a manufacturing method including a conversion step (see, for example, Patent Documents 1 to 3).
  • glass raw material gas is heated and vaporized, and the glass raw material gas is guided to a glass fine particle forming burner by piping under reduced pressure.
  • the temperature of the piping is 55 ° C.
  • the heat resistance temperature is about 70 ° C. This makes it possible to use piping made of a vinyl chloride material.
  • Patent Document 2 starts the deposition of glass fine particles after discarding the glass raw material gas for a predetermined time prior to the start of the deposition of the fine glass particles, and then discards the raw material gas, the volume of the piping, the pressure in the piping, and the piping. By satisfying the predetermined temperature, the occurrence of bubbles and cloudiness in the glass base material is avoided.
  • the piping temperature is 82 ° C. or 85 ° C.
  • a conduit from a source gas generator for supplying source gas to a burner is formed at 90 ° C. over the entire length using a heater and a heat insulating material.
  • Patent Document 4 describes a method for suppressing the spread of the flame by introducing gas into the inner periphery of the hood installed at the tip of the burner flame as a means for increasing the raw material yield.
  • a method for producing a glass fine particle deposit a method for producing a glass fine particle deposit by a gas phase synthesis method such as a VAD method, an OVD method, or an MMD method is generally known.
  • diameter for example, Patent Document 5, impregnated into dispersed mixture of additives particles was obtained by vapor phase synthesis porous soot body, in which heated transparent and the glass base material, SiO 2 system It is described that the particle size of the porous body is 500 to 1000 nm.
  • Patent Document 6 describes a production method in which pre-prepared glass fine particles are introduced into a burner flame, and the average particle size of the glass fine particles to be introduced is preferably 0.2 ⁇ m or less. Has been.
  • Patent Document 7 describes a production method in which a glass fine particle compact is sintered by microwave heating, and describes that the average particle size of the glass fine particles is 1 nm to 100 ⁇ m.
  • Japanese Unexamined Patent Publication No. 2004-161555 Japanese Unexamined Patent Publication No. 2006-342031 Japanese Unexamined Patent Publication No. 2003-165737 Japanese Laid-Open Patent Publication No. 7-144927 Japanese Unexamined Patent Publication No. 11-180719 Japanese Unexamined Patent Publication No. 2004-300006 Japanese Unexamined Patent Publication No. 2004-210548
  • An object of the present invention is to provide a method for producing a glass fine particle deposit and a glass base material, which can improve the adhesion efficiency of the produced glass fine particles to the starting rod and the glass fine particle deposit.
  • the method for producing a glass fine particle deposit according to the present invention capable of solving the above-mentioned problems is a method of heating and vaporizing a liquid glass raw material contained in a raw material container to form a glass raw material gas, and using the glass raw material gas as the raw material.
  • the glass raw material gas is burned from the vessel to the glass fine particle producing burner, and the glass raw material gas is ejected from the glass fine particle producing burner, and flame decomposition reaction (thermal decomposition reaction, flame hydrolysis reaction, thermal oxidation reaction, etc.) of the glass raw material gas.
  • the glass fine particle deposit is produced by depositing the glass fine particles produced by the step on the starting rod in the reaction vessel, and the glass fine particle producing burner from the raw material container in the deposition step. At least a part of the pipe up to 5 ° C / m or more is heated by the heating element on the burner side. It is characterized by controlling the temperature so as to slope.
  • the deposition step at least a part of the piping from the raw material container to the glass particulate generation burner is heated to 15 ° C. on the burner side by a heating element. It is characterized in that the temperature is controlled so as to have a temperature gradient of at least / m.
  • the deposition step at least a part of the piping from the raw material container to the glass particulate generation burner is heated to a temperature of 25 ° C. on the burner side by a heating element. It is characterized in that the temperature is controlled so as to have a temperature gradient of at least / m.
  • At least a part of the pipe from the raw material container to the glass particulate generation burner in the deposition step is controlled to a temperature of 100 ° C. or more by a heating element.
  • the Reynolds number of the glass raw material gas flowing in the pipe from the raw material container to the glass fine particle generating burner is 2000 or more.
  • the glass fine particles in the deposition step have a particle diameter of 10 (nm) or more, and the glass fine particles are placed between the particles in a flame of the glass fine particle producing burner.
  • the mass of the bonded particle group is 1.8 ⁇ 10 ⁇ 17 (g) or more.
  • the temperature of the glass raw material gas charged into the glass particulate generation burner in the deposition step is maintained at 100 ° C. or more, and the glass raw material gas of the glass particulate generation burner is maintained.
  • the glass raw material gas is chemically changed to silicon oxide gas (SiO 2 , SiO, etc.) within 700 mm from the nozzle.
  • the partial pressure of the chemically changed silicon oxide gas is set to be equal to or higher than the saturated vapor pressure of the silicon oxide gas (SiO 2 , SiO, etc.) at a position 20 mm from the glass raw material gas ejection port of the glass fine particle producing burner. It is characterized by.
  • silicon oxide described in the text is a generic term for silicon oxides such as SiO 2 and SiO.
  • the method for producing a glass fine particle deposit according to the present invention includes a partial pressure of the silicon oxide gas that has been chemically changed in the deposition step, preferably at a position 20 mm from the glass raw material gas jet of the glass fine particle producing burner. Is set to 1.5 times or more of the saturated vapor pressure of silicon oxide gas.
  • At least a part of the pipe from the raw material container to the glass particulate generation burner in the deposition step is controlled to a temperature of 100 ° C. or more by a heating element.
  • the Stokes number of the glass fine particles produced by the glass fine particle producing burner is 0.5 or more.
  • the deposition step in the deposition step, at least a part of the piping from the raw material container to the glass particulate generation burner is controlled to a temperature of 100 ° C. or more by a heating element. At the same time, it is characterized in that a region of 1/3 or less in the longitudinal direction from the end portion on the pipe side in the glass fine particle producing burner is controlled to a temperature of 100 ° C. or more by a heating element.
  • the method for producing a glass particulate deposit according to the present invention is characterized in that the heating element is a tape heater.
  • the method for producing a glass base material according to the present invention comprises producing a glass fine particle deposit by the method for producing a glass fine particle deposit, and heating the glass fine particle deposit produced in the deposition step to make it transparent. It is characterized by manufacturing a glass base material through a crystallization process.
  • the glass base material manufacturing method according to the present invention is characterized in that in the deposition step, a glass fine particle deposit is manufactured by an OVD method, a VAD method or an MMD method, and the glass base material is manufactured through the transparency step. It is said.
  • the method for producing a glass fine particle deposit and a glass base material according to the present invention, at least a part of the piping from the raw material container to the glass fine particle generating burner is heated to a temperature higher than 5 ° C./m by the heating element on the burner side. Since the temperature is controlled so as to be a gradient, the volume of the raw material gas in the pipe expands from the raw material container to the burner side, and the flow rate of the raw material gas is accelerated. As a result, the inertial force of the glass fine particles generated in the burner flame is increased, the straightness of the glass fine particles is promoted, and the glass fine particles are easily separated from the gas flow in the flame. Therefore, the adhesion efficiency of the glass fine particles to the starting rod and the glass fine particle deposit can be improved, and the raw material yield can be improved.
  • the method for producing a glass fine particle deposit and a glass base material according to the present invention, at least a part of the piping from the raw material container to the glass fine particle generating burner is controlled to a temperature of 100 ° C. or more by the heating element,
  • the Reynolds number of the glass raw material gas flowing in the pipe from the raw material container to the glass fine particle generating burner is 2000 or more, the flow of the glass raw material gas in the pipe is turbulent, and the raw material gas flowing in the pipe is piped.
  • the heating time of the source gas can be lengthened by following a longer path length than the length, and the temperature of the source gas can be easily increased.
  • the flame hydrolysis reaction is promoted in the burner flame, the number of glass fine particles generated in the flame is increased, and the outer diameter of the glass fine particles is also increased.
  • the increase in particle diameter promotes aggregation (bonding between particles) due to turbulent diffusion.
  • the particle size of the glass fine particles is set to 10 (nm) or more, and the glass fine particles are bonded to each other in the flame of the glass fine particle producing burner.
  • the mass of the bonded particles is set to 1.8 ⁇ 10 ⁇ 17 (g) or more.
  • the temperature of the glass raw material gas charged into the glass fine particle producing burner is maintained at 100 ° C. or higher, and the glass raw material for the glass fine particle producing burner is used.
  • the glass raw material gas is chemically changed to silicon oxide gas and the partial pressure of the chemically changed silicon oxide gas is 20 mm from the glass raw material gas outlet of the glass fine particle producing burner. Is equal to or higher than the saturated vapor pressure of silicon oxide gas.
  • the glass source gas when the glass source gas is chemically changed to silicon oxide gas at a position near the glass source gas outlet of the burner, the partial pressure of the silicon oxide gas increases, so that the silicon oxide gas is converted into silicon oxide particles (solid). It becomes easy to change, and the silicon oxide particles are also easily increased in diameter. Increasing the diameter of the particles facilitates the separation of the glass particles from the flow of the flame gas, improves the adhesion efficiency of the glass particles to the starting rod and the glass particle deposit, and improves the raw material yield. it can.
  • the method for producing a glass fine particle deposit and a glass base material according to the present invention, at least a part of the piping from the raw material container to the glass fine particle generating burner is controlled to a temperature of 100 ° C. or more by the heating element, By setting the Stokes number of the glass particles generated by the glass particle generating burner to 0.5 or more, the inertial force of the glass particles increases. Therefore, the glass fine particles are easily detached from the flow of the flame gas, the adhesion efficiency of the glass fine particles to the starting rod and the glass fine particle deposit can be improved, and the raw material yield can be improved.
  • At least a part of the piping from the raw material container to the glass fine particle producing burner is controlled to a temperature of 100 ° C. or higher by the heating element.
  • the raw material in the glass particle generation burner is controlled by a heating element to a temperature of 1/3 or less in the longitudinal direction from the end on the pipe side in the glass particle generation burner by a heating element. A decrease in gas temperature can be prevented.
  • the flame hydrolysis reaction of the raw material gas is promoted in the burner flame, and the number of glass fine particles generated in the flame is increased.
  • the outer diameter also increases.
  • the increase in particle diameter promotes aggregation (bonding between particles) due to turbulent diffusion.
  • FIG. 6A is a cross-sectional view showing a structural example of a burner
  • FIG. 6A is a structural example in which the tips of the burners are aligned
  • FIG. 6A is a cross-sectional view showing a structural example of a burner
  • 6B is a structural example in which the tips of the burners protrude on the outer peripheral side. It is a block diagram of an example of the manufacturing apparatus which enforces the manufacturing method of the glass fine particle deposit body concerning the 6th Embodiment of this invention. It is a graph which shows the temperature change of the raw material gas in a part of longitudinal direction in the gas supply piping and the burner for glass fine particle production
  • a manufacturing apparatus 10 that performs the method for manufacturing a glass fine particle deposit according to the present embodiment deposits glass fine particles by the VAD method.
  • the starting rod 13 is attached to the lower end of the support rod 12.
  • An exhaust pipe 21 is attached to the side surface of the reaction vessel 11.
  • the upper end of the support rod 12 is held by the lifting / lowering rotating device 15 and is lifted / lowered by the lifting / lowering rotating device 15 together with the rotation.
  • the raising / lowering rotation device 15 is controlled by the control device 16 so that the outer diameter of the glass fine particle deposit 14 is uniform.
  • Glass particulates 20 are deposited on the starting rod 13 to form a glass particulate deposit 14. Further, the glass fine particles 20 in the reaction vessel 11 that have not adhered to the starting rod 13 or the glass fine particle deposit 14 are exhausted through the exhaust pipe 21.
  • a clad burner 18 which is a glass fine particle producing burner is disposed below the inside of the reaction vessel 11, and a raw material gas and a flame forming gas are supplied to the clad burner 18 by a gas supply device.
  • the cladding burner 18 is a multi-tube burner such as an eight-fold tube. In FIG. 1, a gas supply device for supplying the flame forming gas is omitted.
  • the cladding burner 18 is charged with SiCl 4 as a source gas, H 2 and O 2 as a flame forming gas, and N 2 as a burner seal gas.
  • SiCl 4 as a source gas
  • H 2 and O 2 as a flame forming gas
  • N 2 as a burner seal gas.
  • glass fine particles 20 are generated by a flame hydrolysis reaction, and the glass fine particles 20 are deposited on the starting rod 13 to produce a glass fine particle deposit 14 having a predetermined outer diameter. To do.
  • the gas supply device 19 includes a raw material container 22 for storing the liquid raw material 28, an MFC 23 for controlling the supply flow rate of the raw material gas, a gas supply pipe 25 for guiding the raw material gas to the cladding burner 18, a raw material container 22, the MFC 23, and a gas supply pipe 25.
  • the temperature control booth 24 keeps a part of the temperature above a predetermined temperature.
  • the liquid raw material 28 in the raw material container 22 is controlled to a temperature not lower than the boiling point (for example, the normal boiling point in the case of SiCl 4 is 57.6 ° C.) in the temperature control booth 24, is vaporized in the raw material container 22, and is evaporated by the MFC 23.
  • the supply amount of the source gas supplied to the cladding burner 18 is controlled. Note that the control of the raw material gas supply amount by the MFC 23 is performed based on a command value from the control device 16.
  • the temperature on the burner side of at least a part of the gas supply pipe 25 from the raw material container 22 to the cladding burner 18 is increased to a temperature gradient of 5 ° C./m or more. To control the temperature.
  • At least a part of the gas supply pipe 25 from the raw material container 22 to the cladding burner 18 has a high temperature on the burner side so that the temperature gradient is preferably 15 ° C./m or more, more preferably 25 ° C./m or more. Control the temperature so that
  • the material of the gas supply pipe 25 when the gas supply pipe 25 is held at a temperature of less than 200 ° C., the material of the gas supply pipe 25 may be fluororesin (Teflon (registered trademark)), but it is 200 ° C. or more. In the case of holding at temperature, the material of the gas supply pipe 25 is preferably a metallic material such as SUS having excellent heat resistance.
  • a tape heater 26 as a heating element is wound around the outer periphery of the gas supply pipe 25 from the temperature control booth 24 to the cladding burner 18.
  • the tape heater 26 is a flexible heater in which an ultra fine stranded wire of a metal heating element or a carbon fibrous surface heating element is covered with a protective material. When the tape heater 26 is energized, the gas supply pipe 25 is heated.
  • a heat insulating tape 27 as a heat insulating material is wound around the outer periphery of the tape heater 26.
  • the power consumption of the tape heater 26 can be kept low.
  • FIG. 2 An example of temperature control of the gas supply pipe will be described.
  • three types of tape heaters 26 ⁇ / b> A, 26 ⁇ / b> B, and 26 ⁇ / b> C are wound around the outer periphery of the gas supply pipe 25 from the temperature control booth 24 to the cladding burner 18. That is, the first tape heater 26A is wound on the clad burner 18 side, the second tape heater 26B is wound so as to be adjacent to the side, and the third tape heater 26C is wound on the temperature control booth 24 side. ing.
  • the length of the gas supply pipe 25 between the temperature control booth 24 and the cladding burner 18 is 1 m.
  • thermocouples are installed at both ends of the gas supply pipe 25 and the outer periphery in the middle, and the respective temperatures are adjusted by the tape heaters 26A, 26B, and 26C.
  • the temperature of the thermocouple installed at one end of the pipe is set to 120 ° C. by the third tape heater 26C
  • the temperature of the thermocouple installed in the middle is set to 140 ° C. by the second tape heater 26B. If the temperature of the thermocouple installed at one end of the pipe (on the burner 18 side) is 160 ° C. by the first tape heater 26A, the temperature is controlled with a temperature gradient of 40 ° C./m.
  • the temperature of the gas supply pipe 25 from the temperature control booth 24 to the cladding burner 18 is controlled so that the temperature on the burner side is high and the temperature gradient is 5 ° C./m or more, the volume of the source gas in the gas supply pipe 25 is increased. Expands as it proceeds from the temperature control booth 24 to the cladding burner 18, and the flow velocity of the source gas is accelerated.
  • the above-described configuration of the three types of tape heaters 26A, 26B, and 26C is an example for realizing the present invention, and the present invention can be realized with another configuration. For example, even if a part of the tape heater 26B is controlled to be 140 ° C.
  • the effect can be obtained.
  • at least part of the gas supply pipe 25 may be controlled to 5 ° C./m or more, but the entire pipe may be controlled to 5 ° C./m or more.
  • the length of the gas supply pipe 25 between the temperature control booth 24 and the cladding burner 18 is 1 m, but the length of the gas supply pipe 25 can be adjusted as appropriate.
  • the inertial force of the glass fine particles 20 generated in the burner flame is increased, the straightness of the glass fine particles 20 is promoted, and the glass fine particles 20 are easily separated from the gas flow in the flame.
  • the adhesion efficiency of the glass fine particles 20 to the glass fine particle deposit 14 can be improved.
  • the pipe diameter is designed so that the Reynolds number (Re number) of the raw material gas flowing in the gas supply pipe 25 is 2000 or more, preferably 4000 or more, and more preferably 8000 or more.
  • the flow of the raw material gas in the gas supply pipe 25 is turbulent, and the raw material gas is efficiently heated in the gas supply pipe 25 to easily increase the temperature.
  • FIG. 4 shows the temperature of the raw material gas flowing in the gas supply pipe 25 when the entire length of the gas supply pipe 25 is heated to a constant value of 140 ° C. It can be seen from FIG. 4 that the higher the Re number, the easier the source gas flowing in the gas supply pipe 25 is heated.
  • the manufacturing procedure of the glass particulate deposit 14 and the glass base material will be described.
  • (Deposition process) As shown in FIG. 1, the support rod 12 is attached to the lifting / lowering rotation device 15, and the starting rod 13 attached to the lower end of the support rod 12 is placed in the reaction vessel 11. Next, while the starting rod 13 is rotated by the elevating and rotating device 15, the raw material gas is chemically changed into the glass fine particles 20 by the flame hydrolysis reaction in the oxyhydrogen flame formed by the clad burner 18. Deposit on starting rod 13.
  • the temperature of the gas supply pipe 25 is inclined at 5 ° C./m or more from the temperature control booth 24 toward the cladding burner 18. The temperature is controlled to be higher.
  • the obtained glass fine particle deposit 14 is heated to 1100 ° C. in a mixed atmosphere of an inert gas and a chlorine gas, and then heated to 1550 ° C. in a He atmosphere to perform transparent vitrification.
  • a glass base material is repeatedly manufactured.
  • the behavior of the glass fine particles 20 in the flame gas flow in the deposition process will be briefly described. As shown in FIG. 3, the flame gas flow G containing the source gas such as SiCl 4 formed by the cladding burner 18 hits the glass fine particle deposit 14 and the direction of the glass fine particle deposit 14 suddenly changes. It will bend in the outer circumferential direction.
  • the source gas such as SiCl 4 formed by the cladding burner 18
  • the glass particles flowing along the flame gas flow G have a higher Stokes number as the flow velocity increases, the inertial force of the glass particles increases and the straightness of the glass particles improves.
  • the glass fine particle 20A having a large inertial force has high straightness, so that the glass fine particle deposit 14 is intact. Collide with.
  • the glass fine particles 20B having a small inertia force flow along the flame gas flow G, they flow away in the outer peripheral direction of the glass fine particle deposit 14. Accordingly, it is important how to increase the inertial force of the glass fine particles 20.
  • the gas supply pipe 25 is given a temperature gradient, the flow rate of the raw material gas flowing in the gas supply pipe 25 is accelerated toward the downstream side of the gas supply pipe 25, and the glass particles in the burner flame Increase inertia force by 20.
  • the glass fine particles are easily separated from the flow of the flame gas, and the adhesion efficiency of the glass fine particles 20 to the starting rod 13 and the glass fine particle deposit 14 can be improved.
  • a glass base material is produced using the following materials.
  • -Starting rod quartz glass with a diameter of 25 mm and a length of 1000 mm-Input gas to the cladding burner: raw material gas ... SiCl 4 (1-7 SLM), flame forming gas ... H 2 (100-150 SLM), O 2 (100- 150 SLM), burner seal gas ... N 2 (20-30 SLM)
  • the obtained glass fine particle deposit is heated to 1100 ° C. in a mixed atmosphere of an inert gas and a chlorine gas, and then heated to 1550 ° C. in a He atmosphere to perform transparent vitrification.
  • the raw material yield X of the glass fine particles is the mass ratio of the glass fine particles actually deposited on the starting rod and the glass fine particle deposit body with respect to SiO 2 mass when the SiCl 4 gas to be input chemically reacts with 100% SiO 2.
  • the gas supply pipe from the temperature control booth to the cladding burner is heated to a high temperature on the burner side by a heating element, and the minimum temperature gradient T is gradually increased from 5 ° C./m to 40 ° C./m.
  • the minimum temperature gradient T is gradually increased from 5 ° C./m to 40 ° C./m.
  • the raw material yield is calculated when the temperature gradient is not managed and the minimum temperature gradient T is less than 5 ° C./m.
  • the raw material yield X is 32% or more.
  • the minimum temperature gradient T in Example A-5 is 40 ° C./m
  • the raw material gas temperature immediately before being introduced into the burner is 270 ° C., that is, the raw material gas temperature is higher than the standard boiling point of SiCl 4 as the raw material gas.
  • the raw material yield X is increased to 40%.
  • Comparative Examples A-1 and A-2 since the minimum temperature gradient T is less than 5 ° C./m, the raw material yield X is as low as 27% or less, and the minimum temperature gradient T in Comparative Example A-2 is low. Is 3 ° C./m, the raw material yield X is 24%, and it can be seen that only about one-fourth of the SiCl 4 gas to be introduced adheres as glass fine particles.
  • the glass base material manufacturing method of the present embodiment controls at least a part of the gas supply pipe 25 from the temperature control booth 24 to the cladding burner 18 to a temperature of 100 ° C. or more by a tape heater 26 as a heating element,
  • the Reynolds number Re of the source gas flowing in the gas supply pipe 25 from the source container 22 to the cladding burner 18 is set to 2000 or more.
  • the gas flow flowing in the pipe is laminar when the Reynolds number is less than 2000, is a transition region between 2000 and 4000, and becomes turbulent when 4000 or more.
  • at least a part of the gas supply pipe 25 may be controlled to 100 ° C. or higher, but the entire pipe is controlled to 100 ° C. or higher. May be.
  • the Reynolds number Re of the raw material gas flowing in the gas supply pipe 25 is expressed by the following equation, where D is the inner diameter of the pipe, V is the average gas flow velocity in the pipe, and v is the kinematic viscosity coefficient of the gas in the pipe.
  • Re DV / ⁇
  • the kinematic viscosity coefficient ⁇ of SiCl 4 at a temperature of 100 ° C. is about 3.1 ⁇ 10 ⁇ 6 (m 2 / s).
  • the Reynolds number Re is preferably 4000 or more, more preferably 8000 or more.
  • the raw material gas is sufficiently heated in the gas supply pipe 25 by the tape heater 26 and the temperature rises.
  • the raw material gas ejected from the burner is accelerated in the flame hydrolysis reaction in the burner flame.
  • the number of glass particles generated in the flame increases. Further, since the growth of the glass fine particles proceeds, the outer diameter of the glass fine particles also increases. Furthermore, when the particle diameter increases, aggregation (bonding between particles) due to turbulent diffusion is promoted. By these effects, the inertial force of the glass fine particles in the burner flame is increased, the glass fine particles are easily detached from the flow of the flame gas, and the adhesion efficiency of the glass fine particles 20 to the starting rod 13 and the glass fine particle deposit 14 is improved. Can be made.
  • the manufacturing procedure of the glass fine particle deposit body and the glass base material is the same as the deposition step and the transparentization step of the first embodiment, and thus detailed description thereof is omitted.
  • Glass fine particles 20 are deposited on the starting rod 13 shown in FIG. 1, and then heated in a mixed atmosphere of inert gas and chlorine gas, and heated in a He atmosphere to form a transparent glass.
  • the gas supply pipe 25 that supplies the raw material gas to the cladding burner 18 is designed with a pipe inner diameter D so as to obtain a desired Reynolds number Re. Further, the tape heater 26 wound around the outer periphery of the gas supply pipe 25 is energized to control at least a part of the gas supply pipe 25 to a temperature of 100 ° C. or higher. Thereby, the average flow velocity of the raw material gas flowing in the pipe is controlled so that a desired Reynolds number Re can be obtained.
  • the Reynolds number Re of the source gas flowing in the pipe is changed by changing the pipe inner diameter D of the gas supply pipe 25 and the temperature of the gas supply pipe 25. Can be controlled. Further, when the temperature of the source gas flowing through the gas supply pipe 25 changes, the kinematic viscosity coefficient of the source gas also changes.
  • the glass fine particle deposit 14 in which the glass fine particles 20 are deposited on the starting rod 13 is pulled up by the elevating and rotating device 15 according to the growth rate of the lower end portion of the glass fine particle deposit 14.
  • the gas supply pipe 25 from the temperature control booth 24 to the cladding burner 18 is controlled to a temperature of 100 ° C. or more by the tape heater 26 as a heating element, and from the raw material container 22 to the cladding burner 18.
  • the Reynolds number of the raw material gas flowing through the gas supply pipe 25 is 2000 or more, preferably 4000 or more, and more preferably 8000 or more.
  • the flow of the raw material gas in the gas supply pipe 25 becomes turbulent, and the raw material gas is sufficiently heated in the gas supply pipe 25 by the tape heater 26 and the temperature rises.
  • the raw material gas ejected from the burner is accelerated in the flame hydrolysis reaction in the burner flame.
  • the number of glass particles generated in the flame increases. Further, since the growth of the glass fine particles proceeds, the outer diameter of the glass fine particles also increases. Furthermore, the increase in particle diameter promotes aggregation (bonding between particles) due to turbulent diffusion. By these effects, the inertial force of the glass fine particles in the burner flame is increased, the glass fine particles are easily detached from the flow of the flame gas, and the adhesion efficiency of the glass fine particles 20 to the starting rod 13 and the glass fine particle deposit 14 is improved. Can be made.
  • a glass fine particle deposit is manufactured using the following materials.
  • ⁇ Starting rod quartz glass with a diameter of 20 mm and a length of 1000 mm
  • Input gas to a cladding burner raw material gas: SiCl 4 (1-3 SLM), flame forming gas: H 2 (40-70 SLM), O 2 (40- 70 SLM), burner seal gas ... N 2 (8-14 SLM)
  • ⁇ Gas supply pipe between raw material container and clad burner pipe temperature 100 ° C, 150 ° C, 260 ° C, 270 ° C, pipe inner diameter 2.7-19mm
  • the obtained glass fine particle deposit is heated to 1100 ° C. in a mixed atmosphere of an inert gas and a chlorine gas, and then heated to 1550 ° C. in a He atmosphere to perform transparent vitrification.
  • the pipe inner diameter D and pipe temperature of the gas supply pipe are appropriately selected, the Reynolds number Re is changed, and the Reynolds number Re of the source gas flowing in the pipe when the source gas flow rate becomes 3 SLM, and the glass
  • the raw material yield X (%) of the fine particles is evaluated.
  • the raw material yield X is the mass ratio of the glass fine particles actually deposited on the starting rod and the glass fine particle deposit to the SiO 2 mass in the case where the SiCl 4 gas to be added chemically reacts with 100% SiO 2 . As a result, the results shown in Table 2 are obtained.
  • Example B-4 is an example in which the gas supply pipe temperature is 150 ° C., that is, the gas supply pipe temperature is 92.4 ° C. higher than the standard boiling point of SiCl 4 which is the raw material gas. The rate X is improved to 32%.
  • Example B-5 is an example in which the gas supply pipe temperature is 260 ° C., that is, the pipe temperature is 202.4 ° C.
  • Example B-6 the temperature gradient of the gas supply pipe is increased from the raw material container toward the burner with a slope of 50 ° C./m, and the temperature of the gas supply pipe near the burner is increased to 270 ° C., that is, the gas supply pipe temperature is This is an example of 212.4 ° C. higher than the normal boiling point of SiCl 4 which is the source gas.
  • the Reynolds number Re is 11554, and the effect of providing a temperature gradient in the longitudinal direction of the gas supply pipe promotes the turbulent diffusion of the glass particles in the flame, and the raw material yield X jumps up to 37%.
  • Comparative Examples B-1 to B-3 in which the Reynolds number Re is less than 2000 the raw material yield X is as low as 25% or less, and in Comparative Example B-3 in which Re is less than 1500, in particular The yield X is 23%, and it can be seen that in Comparative Examples B-1 to B-3, only about a quarter of the SiCl 4 gas to be introduced adheres.
  • FIG. 4 shows the temperature of the raw material gas flowing in the gas supply pipe when the entire length of the gas supply pipe is heated to a constant value of 140 ° C. From this figure, in the laminar flow state where the Reynolds number Re is 1870 (broken line in the figure), the temperature rises gradually along the longitudinal direction of the pipe, but the Reynolds number Re is 2000 (dashed line in the figure) or 4000 (shown in the figure). In the turbulent state of the middle two-dot chain line), it can be seen that the temperature rises rapidly on the upstream side of the pipe. In Examples B-1 to B-6, the Reynolds number Re is 2000 or more, so in Examples B-1 to B-5, the temperature of the raw material gas charged into the burner is equal to the temperature of the gas supply pipe. In Example B-6, the temperature of the raw material gas charged into the burner is equal to the temperature of the gas supply pipe near the burner.
  • the pipe diameter is designed so that the Reynolds number (Re number) of the source gas flowing in the gas supply pipe 25 is 2000 or more, preferably 4000 or more, and more preferably 8000 or more.
  • the flow of the raw material gas in the gas supply pipe 25 is turbulent, and the raw material gas is efficiently heated in the gas supply pipe 25 to easily increase the temperature.
  • the deposition efficiency of the glass fine particles can be further improved by setting the temperature gradient of the gas supply pipe 25 to 5 ° C./m or more, preferably 15 ° C./m or more, and more preferably 25 ° C./m or more. It becomes possible.
  • Glass fine particles 20 are deposited on the starting rod 13 shown in FIG. 1, and then heated in a mixed atmosphere of inert gas and chlorine gas, and heated in a He atmosphere to form a transparent glass.
  • the particle size of the glass particles is set to 10 (nm) or more, preferably 50 (nm) or more, and the glass particles are aggregated between the particles in the flame of the glass particle generation burner.
  • the mass of the aggregated particles is 1.8 ⁇ 10 ⁇ 17 (g) or more, preferably 2.8 ⁇ 10 ⁇ 14 (g) or more.
  • the agglomeration rate due to turbulent diffusion depends on the particle number concentration and is promoted by increasing the particle number concentration.
  • the flame decomposition reaction of the source gas is preferably performed upstream of the flame where the source gas does not spread.
  • the number concentration of SiO 2 particles can be increased by changing 75% or more of the SiCl 4 gas into SiO 2 gas within 700 mm, preferably within 500 mm, more preferably within 300 mm from the tip of the burner.
  • the behavior of the glass particles in the flame gas flow will be briefly described. As shown in FIG. 5, the flame gas flow G containing the raw material gas such as SiCl 4 formed by the cladding burner 18 hits the glass fine particle deposit 14 and the direction of the glass fine particle deposit 14 rapidly changes. It will bend in the outer circumferential direction.
  • the raw material gas such as SiCl 4 formed by the cladding burner 18
  • the glass fine particle group 1020B having a small inertial force follows the flowing direction of the flame gas flow G.
  • the glass particle group 1020A having a large inertial force has improved straightness, it does not follow the flame gas flow G and easily separates from the flame gas flow G (see FIG. 5). Therefore, it is important how to increase the inertial force of the glass fine particle group.
  • the particle diameter of the glass fine particles is set to 10 (nm) or more, and the glass fine particles are aggregated between the particles in the flame of the glass fine particle generating burner.
  • the mass is set to 1.8 ⁇ 10 ⁇ 17 (g) or more. Aggregation is promoted by turbulent diffusion, and the aggregated particles are easily separated from the flow of the flame gas, and the adhesion efficiency of the glass fine particles to the starting rod and the glass fine particle deposit can be improved.
  • a glass base material is produced using the following materials.
  • -Starting rod quartz glass with a diameter of 25 mm and a length of 1000 mm-Input gas to the cladding burner: raw material gas ... SiCl 4 (1-7 SLM), flame forming gas ... H 2 (100-150 SLM), O 2 (100- 150 SLM), burner seal gas ... N 2 (20-30 SLM)
  • glass fine particles are deposited by the VAD method described above to produce a glass fine particle deposit.
  • the raw material gas temperature T (° C.) to be introduced into the burner, the particle diameter D (nm) of the glass fine particles, and the mass M (g) of the particle group were varied to evaluate the glass raw material yield A (%) of the glass fine particles. To do.
  • the particle diameter D of the glass fine particles can be changed by adjusting the raw material gas temperature T introduced into the burner and the flow rate of the flame forming gas. Further, as described above, the raw material gas (SiCl 4 ) is chemically changed to a SiO 2 gas in a region close to the raw material gas outlet of the glass fine particle generating burner (for example, a region 20 to 700 mm from the raw material gas outlet). it is, it is possible to promote the production and growth of the SiO 2 glass particles.
  • the particle diameter D is the minimum particle diameter confirmed by an electron microscope (SEM), and the raw material gas temperature is the raw material gas temperature immediately before being introduced into the burner.
  • the glass raw material yield A of the glass fine particles is the mass ratio of the glass fine particles actually deposited on the starting rod and the glass fine particle deposit body with respect to the SiO 2 mass when the SiCl 4 gas to be input chemically reacts with 100% SiO 2. To do.
  • the obtained glass fine particle deposit is heated to 1100 ° C. in a mixed atmosphere of an inert gas and a chlorine gas, and then heated to 1550 ° C. in a He atmosphere to form a transparent glass.
  • Table 3 the results shown in Table 3 are obtained.
  • the raw material gas temperature T is set to 100 ° C. or higher, that is, the raw material gas temperature is raised to 42.4 ° C. or higher from the normal boiling point of SiCl 4 as the raw material gas, and the particle diameter D of the glass fine particles is 10 nm or higher.
  • the raw material gas temperature T is lower than 100 ° C., and the particle diameter D of the glass fine particles is less than 10 nm.
  • the raw material yield A is increased.
  • Example C-5 in which the particle diameter D is 77 nm or more and the mass M of the particle group is 2.06 ⁇ 10 ⁇ 13 (g), the glass raw material yield A is 56.2%.
  • Example C-6 is an example in which the temperature gradient of the gas supply pipe is increased from the raw material container toward the burner with an inclination of 20 ° C./m, and the raw material gas temperature T charged into the burner is increased to 170 ° C.
  • Example C-5 Although the particle diameter D is smaller than that of Example C-5, the effect of providing a temperature gradient in the longitudinal direction of the gas supply pipe promotes turbulent diffusion of the glass fine particles in the flame, and the mass M of the particle group is equal to that of Example C.
  • the glass raw material yield A jumps to 58.6%.
  • the clad burner 18 is a multi-tube burner such as an eight-fold tube, for example, and is preferably a protruding multi-tube burner as shown in FIG.
  • the multi-tube burner having this protruding structure can form an inner flame on the burner central axis side, and can form an outer flame on the outer periphery of the inner flame.
  • the length of the outer multiple tube forming the outer flame is formed longer on the raw gas outlet side than the length of the inner multiple tube forming the inner flame.
  • the outer multiple tube protrudes from the inner multiple tube to the raw gas outlet side, so that it becomes difficult for the silicon oxide gas to diffuse in the limited volume inside the protruding portion. It becomes easy to raise pressure. Thereby, the reaction from silicon oxide gas to silicon oxide particles can be promoted. Note that it is sufficient that the partial pressure of the silicon oxide gas can be increased even with a normal multi-tube burner as shown in FIG. 6A and 6B are longitudinal sectional views showing only a part of the burner tip side, and only one side is shown with respect to the burner central axis.
  • the glass base material manufacturing method of the present embodiment is such that the temperature of the raw material gas (SiCl 4 ) charged into the cladding burner 18 is kept at 100 ° C. or more and within 700 mm from the source gas outlet of the cladding burner 18.
  • the gas is chemically changed to silicon oxide gas.
  • the partial pressure of the chemically changed silicon oxide gas is set to be equal to or higher than the saturated vapor pressure of the silicon oxide gas at a position 20 mm from the jet of the source gas of the cladding burner 18.
  • the reaction from the silicon oxide gas to the silicon oxide particles can be efficiently advanced. That is, since the source gas is not diffused in the radial direction at a position close to the cladding burner 18, if the source gas is chemically changed to a silicon oxide gas at a position close to the outlet of the source gas of the cladding burner 18, silicon oxide is obtained. The partial pressure of the gas increases, and a change from silicon oxide gas to silicon oxide particles that are solids easily occurs. At the same time, the growth of silicon oxide particles is promoted, so that the particle size is easily increased.
  • the partial pressure of the silicon oxide gas generated at a position away from the cladding burner 18 is difficult to increase. Therefore, even if silicon oxide gas is generated at a position away from the cladding burner 18, the partial pressure of the silicon oxide gas is low, so that it is difficult for the silicon oxide gas to change to silicon oxide particles, and the particle size is also difficult to grow.
  • the temperature of the raw material gas introduced into the cladding burner 18 is kept at 150 ° C. or more, and the raw material gas is chemically changed to silicon oxide gas within 670 mm from the raw material gas jet port of the cladding burner 18. preferable.
  • the temperature of the source gas is kept at 200 ° C. or higher, and the source gas is chemically changed to silicon oxide gas within 650 mm from the outlet of the source gas of the cladding burner 18.
  • the temperature of the raw material gas is kept at 300 ° C. or higher, and the raw material gas is preferably chemically changed to silicon oxide gas within 620 mm from the raw material gas outlet of the cladding burner 18.
  • the partial pressure of the chemically changed silicon oxide gas is preferably about 1.5 times or more, more preferably 2 times the saturated vapor pressure of the silicon oxide gas, in the vicinity of 20 mm from the raw material gas outlet of the cladding burner 18.
  • the above is preferable.
  • the temperature of the source gas is low, so that a chemical reaction from the source gas to the silicon oxide gas hardly occurs.
  • the position at which the raw material gas is changed to the silicon oxide gas and the partial pressure of the silicon oxide gas generated in the flame of the cladding burner 18 are not limited to the raw material gas temperature supplied to the cladding burner 18, It can also be controlled by the flow rate of (H 2 , O 2 ).
  • the partial pressure of the silicon oxide gas generated in the flame can also be increased by adopting a multiple flame structure for the cladding burner 18 and a protruding structure in which the inner flame close to the raw material gas injection port is surrounded by a multiple circular tube. it can.
  • the number of glass fine particles 20 generated by the cladding burner 18 can be increased, and the growth of the particle size can be promoted.
  • the particle diameter grows, the inertial force of the glass fine particles 20 increases, and the glass fine particles 20 are liable to leave the gas flow without following the flame gas flow.
  • the glass fine particles 20 are likely to adhere to the starting rod 13 and the glass fine particle deposit 14 and the adhesion efficiency can be improved.
  • Glass fine particles 20 are deposited on the starting rod 13 shown in FIG. 1, and then heated in a mixed atmosphere of inert gas and chlorine gas, and heated in a He atmosphere to form a transparent glass.
  • the gas supply pipe 25 is heated to 100 ° C. or more by energizing the tape heater 26 wound around the outer periphery of the gas supply pipe 25 that supplies the source gas to the cladding burner 18.
  • the temperature is controlled to an appropriate temperature, and the temperature of the raw material gas charged into the clad burner 18 is maintained at 100 ° C. or higher, preferably 150 ° C. or higher, more preferably 200 ° C. or higher, more preferably 300 ° C. or higher.
  • the source gas is chemically changed to silicon oxide gas within 700 mm, preferably within 670 mm, more preferably within 650 mm, and even more preferably within 620 mm from the jet of the source gas of the cladding burner 18.
  • the partial pressure of the chemically changed silicon oxide gas is higher than the saturated vapor pressure of the silicon oxide gas, preferably at least 1.5 times the saturated vapor pressure, in the vicinity of 20 mm from the source gas outlet of the cladding burner 18.
  • it is 2 times or more, more preferably 10 times or more.
  • the temperature of the raw material gas introduced into the cladding burner 18 is maintained at 100 ° C. or higher, and the raw material gas is chemically changed to silicon oxide gas within 700 mm from the raw material gas outlet of the cladding burner 18.
  • the partial pressure of the chemically changed silicon oxide gas is set to be equal to or higher than the saturated vapor pressure of the silicon oxide gas at a position 20 mm from the jet of the source gas of the cladding burner 18.
  • a glass base material is produced using the following materials.
  • -Starting rod quartz glass with a diameter of 25 mm and a length of 1000 mm-Input gas to the cladding burner: raw material gas ... SiCl 4 (1-7 SLM), flame forming gas ... H 2 (100-150 SLM), O 2 (100- 150 SLM), burner seal gas ... N 2 (20-30 SLM)
  • the obtained glass fine particle deposit is heated to 1100 ° C. in a mixed atmosphere of an inert gas and a chlorine gas, and then heated to 1550 ° C. in a He atmosphere to perform transparent vitrification.
  • the raw material gas temperature T (° C.) to be introduced into the burner the distance X (mm) from the raw material gas outlet of the burner to the chemical change of the raw material gas into 100% silicon oxide gas, the burner raw material gas injection
  • the raw material yield A (%) is evaluated by changing the pressure ratio Y of silicon oxide gas partial pressure / silicon oxide gas saturated vapor pressure at a position 20 mm from the outlet.
  • the raw material yield A is the mass ratio of the glass fine particles actually deposited on the starting rod and the glass fine particle deposit body with respect to the SiO 2 mass when the SiCl 4 gas to be added chemically reacts with 100% SiO 2 .
  • an ordinary multi-tube burner as shown in FIG. 6A is “1”
  • a multi-tube burner having a protruding structure as shown in FIG. 6B is “2”. The results are shown in Table 4.
  • the raw material gas temperature T is controlled to 100 ° C. or higher, that is, 42.4 ° C. or higher from the standard boiling point of SiCl 4 as the raw material gas, the reaction distance X is 700 mm or less, and the pressure ratio Y is In Examples D-1 to D-8, which are 1 or more, the raw material yield A is as high as 53.8% or more.
  • Example D-5 in which the raw material gas temperature T is 350 ° C., that is, the raw material gas temperature T is controlled to be 292.4 ° C. higher than the standard boiling point of the raw material gas SiCl 4 and the reaction distance X is 600 mm.
  • Example D-6 using a multi-tube burner having a protruding structure obtains the same high raw material yield as Example D-5 even when the raw material gas temperature T is 50 ° C. lower than that of Example D-5. be able to.
  • Example D-7 is an example in which the temperature gradient of the gas supply pipe is increased from the raw material container toward the burner with a slope of 50 ° C./m, and the raw material gas temperature T charged into the burner is set to 300 ° C.
  • Example D-8 is an example in which the temperature gradient of the gas supply pipe is increased from the raw material container toward the burner with a slope of 63 ° C./m, and the raw material gas temperature T charged into the burner is set to 350 ° C.
  • the reaction distance X is shortened to 570 mm, the pressure ratio Y is increased to 2, and the raw material yield A is improved to 73%.
  • Comparative Examples D-1 to D-3 in which the raw material gas temperature T (° C.) is controlled to a temperature of less than 100 (° C.), the reaction position X is greater than 700 mm, and the pressure ratio Y is less than 1. It can be seen that the raw material yield A is as low as less than 50%, and more than half of the SiCl 4 gas to be introduced does not adhere.
  • At least a part of the gas supply pipe 25 from the temperature control booth 24 to the cladding burner 18 is controlled to a temperature of 100 ° C. or more by a tape heater 26 as a heating element.
  • the Stokes number S of the glass fine particles 20 produced by the cladding burner 18 is set to 0.5 or more.
  • the Stokes number S of the glass fine particles 20 in the flame gas is expressed by the following equation, where the particle density ⁇ , the particle diameter d, the particle velocity u, the viscosity coefficient ⁇ of the flame gas, and the diameter L of the glass fine particle deposit.
  • S ⁇ d 2 u / 18 ⁇ L
  • the Stokes number S is preferably 1.0 or more, more preferably 1.5 or more.
  • the glass fine particles 20 When the inertial force of the glass fine particles 20 increases, the straight advanceability of the glass fine particles 20 is promoted, and the glass fine particles 20 do not follow the flame gas flow and are easily separated from the flame gas flow. As a result, the glass fine particles 20 are likely to adhere to the starting rod 13 and the glass fine particle deposit 14 and the adhesion efficiency can be improved.
  • the raw material gas is heated in the gas supply pipe 25 by controlling at least a part of the gas supply pipe 25 to a temperature of 100 ° C. or more by the tape heater 26 that is a heating element.
  • the particle velocity u of the glass fine particles 20 to be ejected increases.
  • at least part of the gas supply pipe 25 may be controlled to a temperature of 100 ° C. or higher, but the total length of the pipe may be controlled to 100 ° C. or higher.
  • the flame hydrolysis reaction of the source gas (SiCl 4 + 2H 2 O ⁇ SiO 2 + 4HCl) proceeds on the upstream side of the flame where the flame does not spread, so the SiO 2 gas partial pressure is increased on the upstream side of the flame. Can be raised.
  • generated within a burner flame increases, and since the growth of the glass fine particles 20 progresses simultaneously, the outer diameter of the glass fine particles 20 also becomes large.
  • the particle velocity u of the glass fine particles 20 can be increased, the particle diameter d can be increased, and the Stokes number S can be increased. it can.
  • the manufacturing procedure of the glass fine particle deposit body and the glass base material is the same as the deposition step and the transparentization step of the above-described embodiment, and thus detailed description thereof is omitted.
  • Glass fine particles 20 are deposited on the starting rod 13 shown in FIG. 1, and then heated in a mixed atmosphere of inert gas and chlorine gas, and heated in a He atmosphere to form a transparent glass.
  • At least a part of the gas supply pipe 25 is heated to 100 ° C. or more by energizing the tape heater 26 wound around the outer periphery of the gas supply pipe 25 that supplies the source gas to the cladding burner 18. Temperature control to an appropriate temperature.
  • the gas supply pipe 25 from the temperature control booth 24 to the cladding burner 18 is controlled to a temperature of 100 ° C. or more by the tape heater 26 which is a heating element, and the glass produced by the cladding burner 18.
  • the raw material gas flowing in the gas supply pipe 25 is heated by the tape heater 26 so that the Stokes number S of the fine particles 20 is 0.5 or more, preferably 1.0 or more, and more preferably 1.5 or more.
  • a glass base material is produced using the following materials.
  • ⁇ Starting rod Gas introduced into quartz glass / cladding burner with a diameter of 25 mm and a length of 1000 mm; source gas: SiCl 4 (1-7 SLM), flame forming gas: H 2 (100-150 SLM), O 2 (100- 150 SLM), burner seal gas ... N 2 (20-30 SLM)
  • the obtained glass fine particle deposit is heated to 1100 ° C. in a mixed atmosphere of an inert gas and a chlorine gas, and then heated to 1550 ° C. in a He atmosphere to perform transparent vitrification.
  • the particle velocity u of the glass fine particles generated in the burner flame is increased and the raw material reaction is promoted, so the particle diameter d of the glass fine particles. Can be enlarged. In this way, the Stokes number S can be changed.
  • the raw material yield X is the mass ratio of the glass fine particles actually deposited on the starting rod and the glass fine particle deposit to the SiO 2 mass in the case where the SiCl 4 gas to be added chemically reacts with 100% SiO 2 .
  • the average particle diameter is calculated from the surface area value of the particles measured by the BET surface area measurement method. The results are shown in Table 5.
  • the gas supply pipe temperature is the outer peripheral temperature of the gas supply pipe in the vicinity of the burner, and this temperature is equal to the temperature of the raw material gas charged into the burner.
  • the gas supply pipe temperature is set to 100 (° C.) or higher, that is, the gas supply pipe temperature is set to 42.4 ° C. or higher from the standard boiling point of SiCl 4 as the raw material gas, and the Stokes number S is set to 0.5 or higher.
  • the raw material yield X of the glass fine particles is 27% or more, and the higher the Stokes number S, the higher the raw material yield X.
  • the gas supply pipe temperature is 130 ° C., that is, when the gas supply pipe temperature is 72.4 ° C. higher than the normal boiling point of the raw material gas SiCl 4 and the Stokes number S is 1.06
  • the raw material yield X is 45%. It becomes.
  • the raw material yield X is 58. %.
  • Example E-8 is an example in which the temperature of the gas supply pipe is increased from the raw material container toward the burner with a slope of 44 ° C./m.
  • the flow rate of the glass microparticles generated in step 1 is further increased, and the raw material yield X is increased to 64%.
  • Example E-9 the temperature of the gas supply pipe is increased from the raw material container toward the burner at a slope of 50 ° C./m, the gas supply pipe temperature is 270 ° C., that is, the gas supply pipe temperature is SiCl 4 as the raw material gas.
  • the Stokes number S is 2.19, and the raw material yield X is improved to 66%.
  • Example E-10 the temperature of the gas supply pipe is increased from the raw material container toward the burner with a slope of 65 ° C./m, the gas supply pipe temperature is 300 ° C., that is, the gas supply pipe temperature is SiCl 4 as the raw material gas.
  • the Stokes number S is 2.84, and the raw material yield X jumps to 70%.
  • Examples E-1, E-3, E-4, E-5, E-6, E-7, E-8, E-9, E-10 having an average particle diameter of 85 nm or more are as follows: The raw material yield X becomes 29% or more, and the raw material yield X increases as the particle diameter increases. The higher the Stokes number S, the higher the raw material yield. However, when the Stokes number exceeds 100, the raw material yield tends to be saturated.
  • a manufacturing apparatus 2010 that performs the method for manufacturing a glass fine particle deposit according to the present embodiment deposits glass fine particles by the VAD method.
  • the starting rod 2013 is attached to the lower end of the support rod 2012.
  • the upper end of the support rod 2012 is gripped by the lifting / lowering rotation device 2015, and the rising speed is controlled by the control device 2016.
  • a clad burner 2018, which is a burner for generating glass particles, is disposed below the reaction vessel 2011, and the glass particles 2020 are ejected toward the starting rod 2013 to form a glass particle deposit 2014. Further, the glass particulates 2020 in the reaction vessel 2011 that did not adhere to the starting rod 2013 and the glass particulate deposit 2014 are exhausted through the exhaust pipe 2021.
  • the cladding burner 2018 is supplied with a raw material gas and a flame forming gas by a gas supply device 2019.
  • the gas supply device 2019 includes a raw material container 2022 for storing the liquid raw material 2028, an MFC 2023 for controlling the supply flow rate of the raw material gas, a gas supply pipe 2025 for guiding the raw material gas to the cladding burner 2018, a raw material container 2022, an MFC 2023, and a gas supply pipe 2025.
  • the temperature control booth 2024 maintains a part of the temperature above a predetermined temperature.
  • At least a part of the gas supply pipe 2025 from the temperature control booth 2024 to the cladding burner 2018 is controlled to a temperature of 100 ° C. or higher by a tape heater 2026 that is a heating element.
  • the region A of 1/3 or less in the longitudinal direction from the end on the gas supply pipe 2025 side in the cladding burner 2018 is controlled to a temperature of 100 ° C. or more by the heating element.
  • a tape heater is used as the heating element.
  • At least a part including the connection portion with the cladding burner 2018 in the gas supply pipe 2025 is controlled to be 100 ° C. or higher. Although good, you may control the whole piping so that it may become 100 degreeC or more.
  • the temperature control region of the gas supply pipe 2025 and the temperature in the region A that is 1/3 or less in the longitudinal direction from the end of the cladding burner 2018 on the gas supply pipe 2025 side should be controlled to be 150 ° C. or more. It is preferable that the temperature is controlled to be 260 ° C. or higher, more preferably 300 ° C. or higher.
  • the temperature of the raw material gas ejected from the raw material container 2022 through the cladding burner 2018 into the burner flame is increased, and the flame hydrolysis reaction of the raw material gas in the burner flame can be promoted.
  • the number of glass particles generated in the flame increases. Further, since the growth of the glass fine particles proceeds, the outer diameter of the glass fine particles also increases. Furthermore, when the particle diameter increases, aggregation (bonding between particles) due to turbulent diffusion is promoted. By these effects, the inertial force of the glass fine particles in the burner flame is increased, the glass fine particles are easily detached from the flow of the flame gas, and the adhesion efficiency of the glass fine particles 2020 to the starting rod 2013 and the glass fine particle deposit 2014 is improved. Can be made.
  • the material of the gas supply pipe 2025 when the gas supply pipe 2025 is held at a temperature of less than 200 ° C., the material of the gas supply pipe 2025 may be fluororesin (Teflon (registered trademark)) or the like. When the temperature is maintained, the material of the gas supply pipe 2025 is preferably made of metal such as SUS having excellent heat resistance. Further, the gas supply pipe 2025 from the temperature control booth 2024 to the clad burner 2018 and the outer periphery of the region A that is 1/3 or less in the longitudinal direction from the end of the clad burner 2018 on the gas supply pipe 2025 side are heating elements. A tape heater 2026 is wound around.
  • the tape heater 2026 is a flexible heater in which an ultra fine stranded wire of a metal heating element or a carbon fibrous surface heating element is covered with a protective material. When the tape heater 2026 is energized, the gas supply pipe 2025 and the cladding burner 2018 are heated.
  • the inner diameter of the gas supply pipe 2025 is set so that the Reynolds number (Re number) of the source gas flowing in the gas supply pipe 2025 and the cladding burner 2018 is 2000 or more, preferably 4000 or more, more preferably 8000 or more. design. Thereby, the flow of the raw material gas in the gas supply pipe 2025 is turbulent, and the raw material gas is efficiently heated in the gas supply pipe 2025 so that the temperature easily rises.
  • Re number Reynolds number
  • the heat insulation tape 2027 which is a heat insulating material is wound around the outer periphery of the portion where the tape heater 2026 is wound.
  • the power consumption of the tape heater 2060 can be kept low.
  • the temperature distribution in the longitudinal direction of the gas supply pipe 2025 and the cladding burner 2018 is preferably controlled so that the temperature increases from the raw material container 2022 toward the cladding burner 2018.
  • the deposition efficiency of the glass fine particles 2020 can be increased by setting the temperature gradient of the gas supply pipe 2025 to 5 ° C./m or more, preferably 15 ° C./m or more, and more preferably 25 ° C./m or more. it can.
  • the manufacturing procedure of the glass fine particle deposit and the glass base material will be described.
  • (Deposition process) As shown in FIG. 7, the support rod 2012 is attached to the lifting / lowering rotation device 2015, and the starting rod 2013 attached to the lower end of the support rod 2012 is placed in the reaction vessel 2011. Next, while the starting rod 2013 is rotated by the elevating and rotating device 2015, the raw material gas is chemically changed into the glass fine particles 2020 by the flame hydrolysis reaction in the oxyhydrogen flame formed by the cladding burner 2018, and the starting rod 2013 is made of glass. Fine particles 2020 are deposited.
  • the region A that is 1/3 or less of is controlled by the tape heater 2026 so that the temperature is 100 ° C. or higher.
  • the region A that is 1/3 or less in the longitudinal direction from the gas supply pipe 2025 and the end of the cladding burner 2018 on the gas supply pipe 2025 side is 150 ° C. or higher.
  • the temperature is preferably controlled to be 260 ° C. or higher, more preferably 300 ° C. or higher.
  • the glass fine particle deposit 2014 on which the glass fine particles 2020 are deposited on the starting rod 2013 is pulled up according to the growth rate of the lower end of the glass fine particle deposit 2014 by the elevating and rotating device 2015.
  • the obtained glass fine particle deposit 2014 is heated to 1100 ° C. in a mixed atmosphere of inert gas and chlorine gas, and then heated to 1550 ° C. in a He atmosphere to perform transparent vitrification.
  • a glass base material is repeatedly manufactured.
  • the temperature is controlled to 100 ° C. or higher by a tape heater 2026 which is a heating element.
  • the heating range of the clad burner 2018 may be heated from the end on the gas supply pipe 2025 side to a range of 1/3 or less in the longitudinal direction. Heating a range wider than 1/3 has no effect of further increasing the temperature of the raw material gas flowing in the burner. This is because the temperature is sufficiently increased in a range other than 1/3 from the end of the cladding burner 2018 on the gas supply pipe 2025 side due to radiant heat from the flame formed by the burner.
  • the optimum heating range is determined by the burner structure and the structure of the reaction vessel. However, if the region less than 1/3 from the end on the gas supply pipe 2025 side of the cladding burner 2018 is heated, almost any equipment structure Even so, there is an effect of keeping the temperature of the raw material gas flowing in the burner at a high temperature.
  • the raw material gas ejected from the cladding burner 2018 is promoted in the flame hydrolysis reaction in the burner flame.
  • the flame hydrolysis reaction is promoted in the burner flame, the number of glass fine particles 2020 generated in the flame increases. Further, since the growth of the glass fine particles proceeds, the outer diameter of the glass fine particles also increases. Furthermore, the increase in particle diameter promotes aggregation (bonding between particles) due to turbulent diffusion. By these effects, the inertial force of the glass fine particles 2020 in the burner flame increases, the glass fine particles 2020 are easily detached from the flow of the flame gas, and the adhesion efficiency of the glass fine particles 2020 to the starting rod 2013 and the glass fine particle deposit 2014 is increased. Can be improved.
  • a glass fine particle deposit is manufactured using the following materials.
  • ⁇ Starting rod Quartz glass with a diameter of 20 mm and a length of 1000 mm
  • the obtained glass fine particle deposit is heated to 1100 ° C. in a mixed atmosphere of an inert gas and a chlorine gas, and then heated to 1550 ° C. in a He atmosphere to perform transparent vitrification.
  • the piping temperature A (° C.) and the burner temperature B (° C.) are appropriately selected, and the raw material yield X (%) of the glass fine particles is evaluated.
  • the raw material yield X is the mass ratio of the glass fine particles actually deposited on the starting rod and the glass fine particle deposit to the SiO 2 mass in the case where the SiCl 4 gas to be added chemically reacts with 100% SiO 2 .
  • the pipe temperature A is the outer peripheral temperature of the gas supply pipe in the vicinity of the burner.
  • the burner temperature B is the outer peripheral temperature at a position 1/3 in the longitudinal direction from the end of the cladding burner on the gas supply pipe side.
  • Example F-6 the gas supply pipe in the cladding burner The region from the side edge to 1/8 in the longitudinal direction is heated. As a result, the results shown in Table 6 are obtained.
  • Example F-4 in which the piping temperature and the burner temperature are 300 ° C., that is, the piping temperature and the burner temperature are 242.4 ° C. higher than the standard boiling point of SiCl 4 as the raw material gas the raw material yield X is 67%.
  • Example F-5 the temperature gradient in the longitudinal direction of the gas supply pipe and the clad burner is increased from the raw material container side to the clad burner side with a 70 ° C./m slope, and the burner temperature is increased to 330 ° C., that is, In this example, the burner temperature is 272.4 ° C. higher than the normal boiling point of SiCl 4 which is a raw material gas.
  • the effect of imparting a temperature gradient in the longitudinal direction of the gas supply pipe and the cladding burner promotes turbulent diffusion of the glass particles in the flame, and the raw material yield X jumps up to 69%.
  • Example F-6 the pipe temperature was set to 300 ° C., the heating range of the burner was set to 1/8, and the outer peripheral temperature at the position 1/3 in the longitudinal direction from the end of the burner on the gas supply pipe side was set to 290 ° C. Yes.
  • the raw material yield X is slightly reduced by narrowing the heating range of the burner from 1/3 to 1/8.
  • the burner temperature B is less than 100 ° C., and the raw material yield X is reduced to 50% or less.
  • the burner temperature B is substantially equal to the temperature of the raw material gas flowing in the cladding burner.
  • FIG. 8 is a graph showing the temperature change of the raw material gas in a part of the longitudinal direction in the gas supply pipe and in the glass fine particle generating burner.
  • the data of the broken line is the case where the entire length of the gas supply pipe is heated to 200 ° C., but the burner is not heated. In this case, it can be seen that the raw material gas temperature is lowered in the burner.
  • the entire length of the gas supply pipe and the 1/3 region in the longitudinal direction from the end of the burner on the gas supply pipe side are heated to 200 ° C. In this case, it can be seen that the temperature of the raw material gas flowing in the burner does not decrease.
  • the manufacturing method of the glass fine particle deposit body and glass base material of this invention is not limited to embodiment mentioned above, A deformation
  • the case where the glass fine particle deposit is manufactured by the VAD method in the deposition step has been described as an example.
  • all other glass fine particle deposits and glasses using a flame decomposition reaction such as the OVD method and the MMD method are used. It is effective for the manufacturing method of the base material.
  • SiCl 4 is used as the source gas.
  • the core glass synthesis using SiCl 4 and GeCl 4 is also effective in improving the source yield.
  • a similar effect can be obtained with a source gas other than SiCl 4 (eg, siloxane).
  • 2012-008303 filed Jan. 18, 2012, 2012 Japanese Patent Application / Application No. 2012-012384 filed on January 24, Japanese Patent Application / Application No. 2012-175010 filed on August 7, 2012, Japanese Patent Application / Application No. 2012- filed on August 7, 2012 175011, based on Japanese Patent Application No. 2012-175012 filed on August 7, 2012, the contents of which are incorporated herein by reference.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Melting And Manufacturing (AREA)
  • Manufacture, Treatment Of Glass Fibers (AREA)
PCT/JP2012/075240 2011-09-29 2012-09-28 ガラス微粒子堆積体及びガラス母材の製造方法 WO2013047834A1 (ja)

Priority Applications (5)

Application Number Priority Date Filing Date Title
IN2480CHN2014 IN2014CN02480A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 2011-09-29 2012-09-28
EP12834881.0A EP2762456B1 (en) 2011-09-29 2012-09-28 Methods for manufacturing glass fine particle deposit and glass base material
US14/348,186 US9630872B2 (en) 2011-09-29 2012-09-28 Method for manufacturing glass-fine-particle-deposited body and method for manufacturing glass base material
CN201280048193.7A CN103842303B (zh) 2011-09-29 2012-09-28 玻璃微粒沉积体以及玻璃预制件的制造方法
US15/495,334 US10604439B2 (en) 2011-09-29 2017-04-24 Method for manufacturing glass-fine-particle-deposited body and method for manufacturing glass base material

Applications Claiming Priority (24)

Application Number Priority Date Filing Date Title
JP2011214780 2011-09-29
JP2011-214608 2011-09-29
JP2011214608 2011-09-29
JP2011-214780 2011-09-29
JP2012000827 2012-01-05
JP2012-000827 2012-01-05
JP2012008158A JP5682577B2 (ja) 2011-09-29 2012-01-18 ガラス微粒子堆積体及びガラス母材の製造方法
JP2012008218 2012-01-18
JP2012008303A JP5720585B2 (ja) 2012-01-18 2012-01-18 ガラス母材の製造方法
JP2012-008151 2012-01-18
JP2012-008158 2012-01-18
JP2012-008218 2012-01-18
JP2012008151 2012-01-18
JP2012-008153 2012-01-18
JP2012008153 2012-01-18
JP2012-008303 2012-01-18
JP2012012384A JP5953767B2 (ja) 2012-01-24 2012-01-24 ガラス微粒子堆積体の製造方法及びガラス母材の製造方法
JP2012-012384 2012-01-24
JP2012175010A JP5737239B2 (ja) 2012-01-18 2012-08-07 ガラス母材の製造方法
JP2012-175011 2012-08-07
JP2012175011A JP5737240B2 (ja) 2012-01-05 2012-08-07 ガラス微粒子堆積体及びガラス母材の製造方法
JP2012175012A JP5737241B2 (ja) 2011-09-29 2012-08-07 ガラス微粒子堆積体及びガラス母材の製造方法
JP2012-175012 2012-08-07
JP2012-175010 2012-08-07

Related Child Applications (2)

Application Number Title Priority Date Filing Date
US14/348,186 A-371-Of-International US9630872B2 (en) 2011-09-29 2012-09-28 Method for manufacturing glass-fine-particle-deposited body and method for manufacturing glass base material
US15/495,334 Continuation US10604439B2 (en) 2011-09-29 2017-04-24 Method for manufacturing glass-fine-particle-deposited body and method for manufacturing glass base material

Publications (1)

Publication Number Publication Date
WO2013047834A1 true WO2013047834A1 (ja) 2013-04-04

Family

ID=50804802

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2012/075240 WO2013047834A1 (ja) 2011-09-29 2012-09-28 ガラス微粒子堆積体及びガラス母材の製造方法

Country Status (5)

Country Link
US (2) US9630872B2 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
EP (1) EP2762456B1 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
CN (1) CN103842303B (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
IN (1) IN2014CN02480A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
WO (1) WO2013047834A1 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2019172527A (ja) * 2018-03-29 2019-10-10 古河電気工業株式会社 配管装置

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018203576A (ja) * 2017-06-06 2018-12-27 住友電気工業株式会社 ガラス微粒子堆積体の製造方法及びガラス母材の製造方法
JP6793676B2 (ja) * 2018-04-02 2020-12-02 信越化学工業株式会社 光ファイバ用多孔質ガラス母材の製造装置および製造方法
JP6694915B2 (ja) 2018-06-12 2020-05-20 株式会社フジクラ 多孔質ガラス微粒子体の製造方法および光ファイバ母材の製造方法
WO2020116523A1 (ja) * 2018-12-04 2020-06-11 住友電気工業株式会社 ガラス微粒子堆積体の製造装置及び製造方法
JP7170555B2 (ja) * 2019-02-12 2022-11-14 信越化学工業株式会社 光ファイバ用多孔質ガラス母材の製造方法
JP7487734B2 (ja) * 2019-04-03 2024-05-21 住友電気工業株式会社 ガラス母材の製造方法
US20220098084A1 (en) * 2020-05-20 2022-03-31 Corning Incorporated Methods for increasing deposition in a flame hydrolysis deposition process
WO2021235408A1 (ja) * 2020-05-20 2021-11-25 住友電気工業株式会社 ガラス母材製造装置、ガラス母材製造方法、および母材プロファイル予測方法
JP7428632B2 (ja) 2020-12-14 2024-02-06 信越化学工業株式会社 多孔質ガラス母材の製造方法及び製造装置
CN113354263B (zh) * 2021-07-03 2022-08-26 神光光学集团有限公司 一种生产合成石英玻璃的方法及设备

Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63222034A (ja) * 1987-03-11 1988-09-14 Furukawa Electric Co Ltd:The 煤状微粒子生成用バ−ナ
JPH07144927A (ja) 1993-11-24 1995-06-06 Furukawa Electric Co Ltd:The 光ファイバ母材合成用バーナ
JPH11180719A (ja) 1997-12-24 1999-07-06 Sumitomo Electric Ind Ltd 光ファイバ用ガラス母材の製造方法
JP2002160926A (ja) * 2000-09-14 2002-06-04 Sumitomo Electric Ind Ltd ガラス微粒子合成用バーナ及び多孔質ガラス体の製造方法
JP2003081644A (ja) * 2001-09-05 2003-03-19 Sumitomo Electric Ind Ltd ガラス母材の製造プロセスにおける原料供給方法
JP2003165737A (ja) 2001-11-27 2003-06-10 Furukawa Electric Co Ltd:The 光ファイバ用母材の製造方法
JP2003252635A (ja) * 2002-03-01 2003-09-10 Fujikura Ltd 多孔質母材の製造方法および製造装置
JP2004161555A (ja) 2002-11-14 2004-06-10 Sumitomo Electric Ind Ltd ガラス形成ガスの供給方法、ガラス微粒子堆積体の製造方法及びそれぞれの装置
JP2004210548A (ja) 2002-12-26 2004-07-29 Fujikura Ltd 石英ガラスの製造方法
JP2004300006A (ja) 2003-04-01 2004-10-28 Sumitomo Electric Ind Ltd 多孔質ガラス微粒子堆積体の製造法
JP2006342031A (ja) 2005-06-10 2006-12-21 Furukawa Electric Co Ltd:The 光ファイバ母材の製造方法
JP2007230813A (ja) * 2006-02-28 2007-09-13 Shin Etsu Chem Co Ltd 石英ガラス製バーナ

Family Cites Families (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS596819B2 (ja) * 1978-12-07 1984-02-14 小松電子金属株式会社 ド−プ石英ガラス棒の製造方法
US4220460A (en) * 1979-02-05 1980-09-02 Western Electric Company, Inc. Vapor delivery system and method
US4604118A (en) * 1985-08-13 1986-08-05 Corning Glass Works Method for synthesizing MgO--Al2 O3 --SiO2 glasses and ceramics
JPS63307137A (ja) * 1987-06-05 1988-12-14 Furukawa Electric Co Ltd:The 光フアイバ用ガラス母材の製造方法
JPH02102146A (ja) 1988-10-12 1990-04-13 Sumitomo Electric Ind Ltd ガラス微粒子堆積体の製造方法
JPH02133331A (ja) * 1988-11-15 1990-05-22 Sumitomo Electric Ind Ltd ガラス微粒子堆積体の製造方法
JPH0669898B2 (ja) * 1989-08-08 1994-09-07 矢崎総業株式会社 光ファイバ用多孔質母材合成用トーチ
US5043002A (en) 1990-08-16 1991-08-27 Corning Incorporated Method of making fused silica by decomposing siloxanes
JP3567574B2 (ja) 1995-12-26 2004-09-22 住友電気工業株式会社 多孔質ガラス母材合成用バーナ
JP3543537B2 (ja) 1996-05-09 2004-07-14 住友電気工業株式会社 ガラス微粒子合成方法及びそのための焦点型バーナ
AU743831B2 (en) * 1997-07-08 2002-02-07 Corning Incorporated Germanium chloride and siloxane feedstock for forming silica glass and method
JP3816268B2 (ja) 1999-06-14 2006-08-30 信越化学工業株式会社 多孔質ガラス母材の製造方法
JP4471445B2 (ja) 2000-04-06 2010-06-02 信越化学工業株式会社 多孔質ガラス母材の製造方法及びその装置
CN102421713A (zh) * 2009-05-13 2012-04-18 旭硝子株式会社 TiO2-SiO2玻璃体的制造方法及热处理方法、TiO2-SiO2玻璃体、EUVL用光学基材
JP5678467B2 (ja) 2010-04-30 2015-03-04 住友電気工業株式会社 ガラス母材製造方法
JP5533205B2 (ja) 2010-04-30 2014-06-25 住友電気工業株式会社 ガラス母材製造方法
JP2012006791A (ja) 2010-06-25 2012-01-12 Sumitomo Electric Ind Ltd 光ファイバ母材の製造方法
JP5640920B2 (ja) * 2011-08-18 2014-12-17 信越化学工業株式会社 チタニアドープ石英ガラス及びその製造方法

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63222034A (ja) * 1987-03-11 1988-09-14 Furukawa Electric Co Ltd:The 煤状微粒子生成用バ−ナ
JPH07144927A (ja) 1993-11-24 1995-06-06 Furukawa Electric Co Ltd:The 光ファイバ母材合成用バーナ
JPH11180719A (ja) 1997-12-24 1999-07-06 Sumitomo Electric Ind Ltd 光ファイバ用ガラス母材の製造方法
JP2002160926A (ja) * 2000-09-14 2002-06-04 Sumitomo Electric Ind Ltd ガラス微粒子合成用バーナ及び多孔質ガラス体の製造方法
JP2003081644A (ja) * 2001-09-05 2003-03-19 Sumitomo Electric Ind Ltd ガラス母材の製造プロセスにおける原料供給方法
JP2003165737A (ja) 2001-11-27 2003-06-10 Furukawa Electric Co Ltd:The 光ファイバ用母材の製造方法
JP2003252635A (ja) * 2002-03-01 2003-09-10 Fujikura Ltd 多孔質母材の製造方法および製造装置
JP2004161555A (ja) 2002-11-14 2004-06-10 Sumitomo Electric Ind Ltd ガラス形成ガスの供給方法、ガラス微粒子堆積体の製造方法及びそれぞれの装置
JP2004210548A (ja) 2002-12-26 2004-07-29 Fujikura Ltd 石英ガラスの製造方法
JP2004300006A (ja) 2003-04-01 2004-10-28 Sumitomo Electric Ind Ltd 多孔質ガラス微粒子堆積体の製造法
JP2006342031A (ja) 2005-06-10 2006-12-21 Furukawa Electric Co Ltd:The 光ファイバ母材の製造方法
JP2007230813A (ja) * 2006-02-28 2007-09-13 Shin Etsu Chem Co Ltd 石英ガラス製バーナ

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP2762456A4 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2019172527A (ja) * 2018-03-29 2019-10-10 古河電気工業株式会社 配管装置

Also Published As

Publication number Publication date
IN2014CN02480A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 2015-06-19
EP2762456B1 (en) 2020-08-05
US10604439B2 (en) 2020-03-31
US20170225998A1 (en) 2017-08-10
CN103842303B (zh) 2018-07-03
US9630872B2 (en) 2017-04-25
EP2762456A1 (en) 2014-08-06
CN103842303A (zh) 2014-06-04
US20140305168A1 (en) 2014-10-16
EP2762456A4 (en) 2015-06-03

Similar Documents

Publication Publication Date Title
WO2013047834A1 (ja) ガラス微粒子堆積体及びガラス母材の製造方法
JP6236866B2 (ja) ガラス微粒子堆積体の製造方法およびガラス微粒子堆積体製造用バーナー
JP2015113259A (ja) ガラス微粒子堆積体の製造方法およびガラス母材の製造方法
US20040187525A1 (en) Method and apparatus for making soot
JP4043768B2 (ja) 光ファイバ用母材の製造方法
JP5737241B2 (ja) ガラス微粒子堆積体及びガラス母材の製造方法
JP5720585B2 (ja) ガラス母材の製造方法
JP5737240B2 (ja) ガラス微粒子堆積体及びガラス母材の製造方法
JP5953767B2 (ja) ガラス微粒子堆積体の製造方法及びガラス母材の製造方法
JP5737239B2 (ja) ガラス母材の製造方法
JP5682577B2 (ja) ガラス微粒子堆積体及びガラス母材の製造方法
EP3608296B1 (en) Manufacturing device and manufacturing method for optical fiber porous preform
JP7115095B2 (ja) 光ファイバ用母材の製造方法
US7441416B2 (en) Method for manufacturing optical fibre preforms
CN111032587B (zh) 玻璃微粒沉积体的制造方法、玻璃母材的制造方法以及玻璃微粒沉积体
WO2012039227A1 (ja) ガラス母材の製造方法
JP4258612B2 (ja) 多重炎堆積バーナ及び光ファイバ予成形体の作製方法
JP5962382B2 (ja) ガラス微粒子堆積体の製造方法およびガラス母材の製造方法
JP2019172527A (ja) 配管装置
JP3417962B2 (ja) 合成石英ガラス部材の製造方法
JP3953855B2 (ja) 多孔質母材の製造方法
JP2006021978A (ja) ガラス体の加熱装置及びこれを用いた光ファイバ母材の製造方法
JP2004359519A (ja) 合成シリカガラス多孔体の製造方法及びその製造装置
JP2004522679A (ja) 光ファイバ予成形体を製造する方法及び堆積バーナ

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 12834881

Country of ref document: EP

Kind code of ref document: A1

WWE Wipo information: entry into national phase

Ref document number: 14348186

Country of ref document: US

Ref document number: 2012834881

Country of ref document: EP

NENP Non-entry into the national phase

Ref country code: DE