WO2002057193A2 - Procede de production d'une ebauche en sio¿2? - Google Patents

Procede de production d'une ebauche en sio¿2? Download PDF

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Publication number
WO2002057193A2
WO2002057193A2 PCT/EP2002/000478 EP0200478W WO02057193A2 WO 2002057193 A2 WO2002057193 A2 WO 2002057193A2 EP 0200478 W EP0200478 W EP 0200478W WO 02057193 A2 WO02057193 A2 WO 02057193A2
Authority
WO
WIPO (PCT)
Prior art keywords
burner
deposition
flame
range
value
Prior art date
Application number
PCT/EP2002/000478
Other languages
German (de)
English (en)
Other versions
WO2002057193A3 (fr
Inventor
Udo Peper
Jürgen Röper
Hans-Georg Fritsche
Original Assignee
Heraeus Tenevo Ag
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
Application filed by Heraeus Tenevo Ag filed Critical Heraeus Tenevo Ag
Publication of WO2002057193A2 publication Critical patent/WO2002057193A2/fr
Publication of WO2002057193A3 publication Critical patent/WO2002057193A3/fr

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
    • C03B19/1415—Reactant delivery systems
    • C03B19/1423—Reactant deposition burners
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/01413—Reactant delivery systems
    • C03B37/0142—Reactant deposition burners
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
    • 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
    • C03B2207/20—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
    • C03B2207/36—Fuel or oxidant details, e.g. flow rate, flow rate ratio, fuel additives
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/50—Multiple burner arrangements
    • C03B2207/52—Linear array of like burners
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/60—Relationship between burner and deposit, e.g. position
    • C03B2207/62—Distance
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/60—Relationship between burner and deposit, e.g. position
    • C03B2207/66—Relative motion
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/70—Control measures

Definitions

  • the invention relates to a method for producing an SiO 2 blank, in which SiO 2 particles are formed in a plurality of deposition burners arranged in a row, each of which is assigned a burner flame, and are deposited on a deposition surface of a carrier rotating about its longitudinal axis.
  • the row of separating burners in a predetermined movement sequence along the forming blank between turning points at which their direction of movement is reversed, and wherein the burner flame forms a projection surface in a projection onto a plane parallel to its main direction of propagation, the lateral surface of which Boundary lines with the main direction of propagation include an opening angle.
  • OTD method outside vapor deposition
  • SiO 2 particles are deposited on a carrier using one or more flame hydrolysis burners, so that a blank of porous quartz glass (hereinafter also referred to as “soot body”) is formed.
  • dopants are such as germanium, phosphorus, boron, titanium, aluminum, tantalum or fluorine into the quartz glass.
  • An OVD method of the type mentioned is known from EP-A 476 218. It describes the production of an elongated, porous blank from SiO 2 particles, with SiO 2 particles in the burner flames of
  • Flame hydrolysis burners are formed and deposited in layers on a horizontally oriented support rotating around its longitudinal axis.
  • the separation burners are mounted at an equidistant distance of 10 cm from each other on a burner block running parallel to the longitudinal axis of the carrier.
  • the burner block is moved back and forth along the forming porous, cylindrical blank between a left and a right turning point by means of an adjustable displacement device.
  • the amplitude of this Translational movement of the burner block is less than the length of the preform. It has been shown that inhomogeneities - predominantly in the form of bubbles - can occur in the area of the turning points after the blank has been vitrified.
  • DE-A 196 28 958 it is proposed in DE-A 196 28 958 to prevent the blank from overheating in the areas around the turning points by increasing the peripheral speed of the blank in the area of the turning points during the burner movement, reducing the flame temperature of the burner flame, or the distance of the Deposition burner from the blank surface is enlarged.
  • an increase in temperature of the blank surface in the area of the turning points can be compensated for in whole or in part, so that the blank is subjected to a heating power which is as high in terms of time and space as possible over its entire length, so that axial density fluctuations are avoided or reduced.
  • the burner flames are visible to the naked eye as essentially conical, luminous areas.
  • the burner flame In a projection onto a plane parallel to its main direction of propagation, the burner flame each has a projection surface, the lateral boundary lines of which include a certain opening angle with the main direction of propagation.
  • the present invention is therefore based on the object of specifying a simple method for producing a porous blank, from which a homogeneous quartz glass body is obtained.
  • this object is achieved according to the invention in that the opening angle of the burner flame is set to a value between 3 ° and 15 ° and the distance of the deposition burner from the deposition surface is in the range between 170 mm and 240 mm.
  • the burner flame is visible to the naked eye as an essentially conical, shining area.
  • the "opening angle" of the visible cone area is determined from the projection of the burner flame onto a plane parallel to the main direction of propagation.
  • the opening angle is the angle between the lateral boundary line of the burner flame and its main direction of propagation, the "lateral boundary line” of the burner flame in the projection as a tangent is defined on the cone area in the area of the exit of the burner flame from the burner mouth.
  • the deposition burner generally has several nozzles for the supply of glass raw materials, oxygen and fuel.
  • the opening angle of the burner flame is essentially dependent on the mass flow and the temperature of the media (usually gases) introduced into the burner flame and the
  • the desired opening angle can be set by changing these parameters.
  • a change in the temperature of the media is often undesirable, so that the opening angle is advantageously carried out by adjusting the mass flow (preferably the flow of the most important quantity of glass starting material) or by adjusting the nozzle cross sections.
  • the distance between the separating burner and the deposit surface is the shortest distance between the burner mouth and the surface of the blank being formed. Otherwise, this distance is defined as the shortest distance between the nozzle opening of the nozzle through which the most important quantity of glass starting material is passed. This is usually the central nozzle (middle nozzle).
  • the opening angle is set to a value between 5 ° and 10 ° and the distance of the deposition burner from the deposition surface is in the range between 180 mm and 220 mm.
  • the burner flame forms a cut surface with the deposition surface, the size of which lies in the range between 8 cm 2 to 20 cm 2 , preferably in the range between 10 cm 2 to 17 cm 2 . It has been shown that this cut surface can also be used as a measure of those particle properties and their local distribution in which a uniform application of mass is facilitated.
  • the temperature In addition to the geometric shape of the burner flame and the residence time of the SiO 2 particles in the flame, the temperature also has an effect on the properties of the SiO 2 particles that are relevant for the application of the mass. It has also proven to be advantageous to set the temperature of the burner flame in the region of the deposition area to a value between 1100 ° C. and 1300 ° C. If the distance between the deposition burner and the deposit surface is constant, the flame temperature can be adjusted accordingly by changing the flows of fuel, oxygen, glass raw materials or of inert gas flows.
  • the burner flame each has an impact point on the deposition surface defined by the point of intersection of the main direction of propagation with the deposition surface, and that the impingement points of adjacent burner flames from one another - seen in the direction of the longitudinal axis of the carrier - have an equidistant flame spacing from one another
  • the standard deviation of all flame distances is less than 5%.
  • the exact positioning and alignment of the separating burner ideally results in an exactly "equidistant" flame spacing. In practice, a deviation of 5% from the mean value of the spacings between neighboring impact points is tolerable in order to ensure sufficient uniformity of the mass application.
  • the movement sequence comprises a translation speed with which the deposition burner between the Reversal points are moved back and forth and an acceleration period during which the deposition burner accelerates from a turning point to the translation speed and a turning point approaching the translation speed are decelerated such that the translation speed is in a range between 350 mm / min and 550 mm / min and the acceleration duration is set to a value in the range between 70 ms and 700 ms.
  • Both the duration of the positive acceleration, at which the deposition burners are accelerated from a turning point to the translation speed, and the duration of the negative acceleration, during which the deposition burners are decelerated from the translation speed to a turning point, are set to a value in the range between 70 ms and set to 700 ms. It has been shown that this measure, in conjunction with a translation speed between 350 mm / min and 550 mm / min, makes it easier to maintain a uniform application of mass and a low waviness of the blank surface.
  • the translation speed is preferably set to a value in the range between 400 mm / min and 500 mm / min and the acceleration duration to a value in the range between 100 ms and 500 ms.
  • a procedure in which the deposition burners are accelerated and braked with exponential time dependence has proven particularly useful. Due to the exponential time dependency of the acceleration (positive and negative acceleration), a short acceleration duration and accordingly short distances are obtained with an exponent greater than 1, which facilitates the setting of a uniform particle distribution and a low waviness of the blank surface. In addition, it has been shown that this measure makes it possible to keep the dead time of the burner movement at the turning point, which affects a uniform application of mass, particularly short.
  • the distance between the turning points is set as an even multiple of the distance between adjacent burner flames. This facilitates the setting of a low ripple and a uniform particle distribution, whereas in in this regard, an odd multiple of the distance in question has surprisingly proven to be rather disadvantageous.
  • a method is preferred in which the deposition burners are supplied with a first silicon-containing starting component in a central region, a hydrogen stream and an oxygen stream in an outer region, and a separation gas stream between the central region and the outer region, the volume ratio of hydrogen stream and oxygen flow is set in the range of 0.2 to 0.4.
  • those deposition burners are advantageously used which each have a first, silicon-containing starting component in a central area, a hydrogen flow and an oxygen flow in an outer area, and between the central area and the outer area Separating gas stream are supplied. Separation burners of this type are known per se from DE-A1 195 27451. The invention is based on the additional finding that such
  • Separation burners are also particularly suitable for an application in which a homogeneous mass distribution on the deposit surface of a blank is important, the volume ratio of hydrogen flow and oxygen flow being set to a value in the range from 0.2 to 0.4.
  • the starting component can also contain dopant-forming substances, such as a hydrolyzable germanium compound for the formation of GeO 2 .
  • dopant-forming substances such as a hydrolyzable germanium compound for the formation of GeO 2 .
  • FIG. 1 an embodiment of a device for carrying out the method according to the invention in a side view
  • FIG. 2 shows a detail from FIG. 1 in an enlarged representation
  • Figure 3 a diagram with a speed profile of the burner movement as a function of the position of a separating burner in the area between two turning points A and B, and
  • Figure 4 a deposition burner suitable for performing the method according to the invention in a longitudinal section.
  • a support tube 1 made of aluminum oxide is provided, along which a plurality of flame hydrolysis burners 2 arranged in a row are arranged.
  • the flame hydrolysis burner 2 are mounted on a common burner block 3, which is parallel to the longitudinal axis 4 of the
  • Carrier tube 1 can be moved back and forth and displaced perpendicularly thereto, as indicated by the directional arrows 5 and 6.
  • the burner 2 consist of quartz glass; their distance from each other is 10 cm.
  • a control device 7 is provided, which is connected to the drive 8 for the burner block 3.
  • SiO 2 particles are deposited on the carrier tube 1 rotating about its longitudinal axis 4 by means of the burner 2, so that the blank 9 is built up in layers.
  • the burner block 3 is moved back and forth along the longitudinal axis 4 of the carrier tube 1 between two turning points which are stationary with respect to the longitudinal axis 4.
  • the amplitude of the back and forth movement is 20 cm and thus corresponds to twice the axial distance of the burners 2, which is characterized by the direction arrow 5.
  • the burners 2 are each supplied with oxygen and hydrogen as burner gases and gaseous SiCI as the starting material for the formation of the SiO 2 particles.
  • the volume ratio of hydrogen and oxygen is 0.3. In the case of one
  • the burners 2 are additionally supplied with a starting substance for the formation of the dopant, such as GeCl 4 for the formation of GeO 2) .
  • the temperature of the blank surface 10 is measured continuously.
  • a thermal camera 11 is on the blank surface 10 at the point of impact Brennerfla me 12 directed.
  • the thermal camera 11 is also connected to the burner block 3 and is moved back and forth with it. During the deposition process, a temperature of approximately 1200 ° C. is established on the blank surface 10.
  • the distance between the burner block 3 and the blank surface 11 is kept constant by displacing the burner block 3 in the direction of the arrow 6 accordingly.
  • the burner flames 12 of the deposition burner 2 each have a flame cone visible to the naked eye.
  • the main direction of propagation 13 of each burner flame 12 is perpendicular to the longitudinal axis 4 of the carrier.
  • the burner flame 12 and its distance from the blank surface 10 are explained in more detail below on the basis of the enlargement of the section “A” in FIG.
  • FIG. 2 schematically shows a projection of the visible flame cone of the burner flame 12 onto a plane parallel to the main direction of propagation 13.
  • the projection shows an axisymmetric to the main direction of propagation 13
  • Burner flame 12 In this illustration, the visible flame cone is clearly enclosed by lateral boundary lines 14. In contrast, in a photographic representation of the flame cone, the boundary lines 14 are blurred, but they are nevertheless easy to determine.
  • the point of incidence 17 of the burner flame 12 on the blank surface 10 is defined by the intersection of the main direction of propagation 13 with the blank surface 10.
  • the burner flame 12 cuts the blank surface 10 in an area which has an area of approximately 15 cm 2 .
  • the deposition burner 2 used is explained in more detail below with reference to FIG. 4. It has several nozzles for feeding glass raw materials, Oxygen and fuel, which end flush in the area of the burner mouth 16.
  • the distance "D" between the burner mouth 16 and the blank surface is set to 200 mm and is kept at this value during the deposition process.
  • the diagram according to FIG. 3 shows speed profile 30, on the basis of which burner block 3 is moved back and forth between turning points A and B.
  • the diagram shows the speed "v" of the translation movement in mm / s as a function of the location "r" between the turning points A and B.
  • the distance between A and B is 20 cm.
  • the separating burner is moved back and forth between the turning points A and B essentially at a constant speed of about 7 mm / sec (420 mm / min) (curve section 31).
  • the translation speed is reduced to zero with exponential time dependence or accelerated from zero to the constant speed of approximately 7 mm / sec (curve sections 32). Due to the exponential time dependency (exponent greater than 1), a short braking and acceleration duration is achieved, with the transition to the area of constant translation speed (when accelerating) or from this (during braking) taking place gradually on both sides of turning points A, B.
  • the separating burners run through the reverse
  • Velocity profile as when accelerating, so that the speed profile 30 when moving towards the turning point B is identical to the speed profile 30 when moving away from the turning point B; as this is symbolized by the block arrow 33. It has been shown that with such a speed profile, a uniform application of mass and thus a blank with low surface ripple is obtained.
  • the separating burner 41 consists of a total of four burner tubes 42, 43, 44, 45 made of quartz glass arranged coaxially to one another.
  • the central burner tube 42 surrounds the central nozzle 46, which is between the central burner tube 42 and the adjacent burner tube 43 Separating gas nozzle 47 formed, the burner tube 43 and the burner tube 44 enclose the annular gap nozzle 48 and the burner tube 44 and the outer tube 45 the outer nozzle 49.
  • the annular separating gas nozzle 47 bends in the direction of the central nozzle 46, the opening cross section simultaneously the separating gas nozzle 47 continuously tapers in this area.
  • the opening cross section of the annular gap nozzle 48 widens in the region of its nozzle opening 51.
  • the nozzle opening of the central nozzle is identified by the reference number 52.
  • the opening cross sections of the center nozzle 46, the separating gas nozzle 47, the annular gap nozzle 48 and the outer nozzle 49 are in the area of the line “L” in the order of their naming in a ratio of 1: 5: 15: 40 to one another.
  • an effective shielding of the fuel gas streams emerging from the nozzle openings 51 and 53 from the stream of the glass raw materials is achieved.
  • the shielding is further improved by the expansion of the annular gap nozzle 48 in the region of the nozzle opening 51.
  • the volume ratio of hydrogen flow and total oxygen flow is 0.3.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Glass Melting And Manufacturing (AREA)
  • Manufacture, Treatment Of Glass Fibers (AREA)

Abstract

Selon un procédé connu de production d'une ébauche en SiO2, des particules de SiO2 sont formées dans plusieurs brûleurs de dépôt disposés en série, une flamme étant associée à chaque brûleur, et ces particules sont déposées sur une surface de dépôt d'un support en rotation autour de son axe longitudinal. Selon ce procédé, la série de brûleurs de dépôt effectue un mouvement de va-et-vient, selon une séquence de déplacement prédéterminée le long de l'ébauche en formation, entre des points d'inversion au niveau desquels le sens de déplacement est inversé, la flamme des brûleurs formant, dans une projection sur un plan parallèle à son sens principal de propagation, une surface de projection dont les limites latérales forment un angle d'ouverture avec le sens principal de propagation. L'objectif de l'invention est de proposer, à partir de cela, un procédé simple de production d'une ébauche poreuse permettant d'obtenir un corps homogène en verre de quartz. A cet effet, l'angle d'ouverture (α) est défini sur une valeur comprise entre 3° et 15° et la distance (D) entre le brûleur de dépôt (2) et la surface de dépôt (10) est comprise entre 170 mm et 240 mm.
PCT/EP2002/000478 2001-01-21 2002-01-18 Procede de production d'une ebauche en sio¿2? WO2002057193A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10102611.0 2001-01-21
DE2001102611 DE10102611B4 (de) 2001-01-21 2001-01-21 Verfahren zur Herstellung eines SiO2-Rohlings

Publications (2)

Publication Number Publication Date
WO2002057193A2 true WO2002057193A2 (fr) 2002-07-25
WO2002057193A3 WO2002057193A3 (fr) 2002-10-31

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WO (1) WO2002057193A2 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104125933A (zh) * 2012-12-28 2014-10-29 住友电气工业株式会社 玻璃微粒沉积体的制造方法以及玻璃母材的制造方法
US20200262735A1 (en) * 2017-08-29 2020-08-20 Sumitomo Electric Industries, Ltd. Method for producing glass particulate deposit, method for producing glass preform, and glass preform
EP4428106A1 (fr) * 2023-03-07 2024-09-11 Heraeus Quarzglas GmbH & Co. KG Synchronisation d'entraînement pour machine de dépôt de suie pour éviter la formation de motif dans des processus de dépôt

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4015466A1 (fr) 2020-12-16 2022-06-22 Heraeus Quarzglas GmbH & Co. KG Procédé de fabrication de silice vitreuse synthétique
EP4015468A1 (fr) 2020-12-16 2022-06-22 Heraeus Quarzglas GmbH & Co. KG Procédé de fabrication de silice vitreuse synthétique

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0476218A1 (fr) * 1990-09-20 1992-03-25 Corning Incorporated Procédé et dispositif pour la fabrication d'un préforme de verre poreux
US6047564A (en) * 1996-07-18 2000-04-11 Heraeus Quarzglas Gmbh Method of producing quartz glass bodies
US6321573B1 (en) * 1998-06-25 2001-11-27 Heraeus Quarzglas Gmbh & Co. Kg Process and apparatus for manufacturing a porous SiO2 preform

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19527451C2 (de) * 1995-07-27 1998-06-04 Heraeus Quarzglas Verfahren zur Herstellung eines Quarzglasrohlings und dafür geeigneter Brenner

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0476218A1 (fr) * 1990-09-20 1992-03-25 Corning Incorporated Procédé et dispositif pour la fabrication d'un préforme de verre poreux
US6047564A (en) * 1996-07-18 2000-04-11 Heraeus Quarzglas Gmbh Method of producing quartz glass bodies
US6321573B1 (en) * 1998-06-25 2001-11-27 Heraeus Quarzglas Gmbh & Co. Kg Process and apparatus for manufacturing a porous SiO2 preform

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104125933A (zh) * 2012-12-28 2014-10-29 住友电气工业株式会社 玻璃微粒沉积体的制造方法以及玻璃母材的制造方法
US20200262735A1 (en) * 2017-08-29 2020-08-20 Sumitomo Electric Industries, Ltd. Method for producing glass particulate deposit, method for producing glass preform, and glass preform
EP4428106A1 (fr) * 2023-03-07 2024-09-11 Heraeus Quarzglas GmbH & Co. KG Synchronisation d'entraînement pour machine de dépôt de suie pour éviter la formation de motif dans des processus de dépôt

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Publication number Publication date
DE10102611B4 (de) 2004-07-15
DE10102611A1 (de) 2002-08-01
WO2002057193A3 (fr) 2002-10-31

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