WO2001098219A2 - Procede de fabrication d'une piece semi-finie en sio2, et piece obtenue suivant ce procede - Google Patents

Procede de fabrication d'une piece semi-finie en sio2, et piece obtenue suivant ce procede Download PDF

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Publication number
WO2001098219A2
WO2001098219A2 PCT/EP2001/006576 EP0106576W WO0198219A2 WO 2001098219 A2 WO2001098219 A2 WO 2001098219A2 EP 0106576 W EP0106576 W EP 0106576W WO 0198219 A2 WO0198219 A2 WO 0198219A2
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WO
WIPO (PCT)
Prior art keywords
blank
layer
core glass
deposition
layer sequence
Prior art date
Application number
PCT/EP2001/006576
Other languages
German (de)
English (en)
Other versions
WO2001098219A3 (fr
Inventor
Wolfgang Krock
Klaus Ruppert
Peter Kleinsorge
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 WO2001098219A2 publication Critical patent/WO2001098219A2/fr
Publication of WO2001098219A3 publication Critical patent/WO2001098219A3/fr

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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
    • 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
    • C03B37/01205—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
    • 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
    • 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
    • C03B2207/60—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 present invention relates to a process for the production of a SiO 2 blank in that the porous blank is formed by depositing successive layers of SiO 2 particles on the lateral surface of a support rotating about its longitudinal axis by means of at least one deposition burner and the support is removed.
  • the invention relates to a blank for the production of a preform for an optical fiber, which has a core glass region made of porous quartz glass which is formed from a plurality of successive layers and which is coaxially surrounded by at least one cladding glass region made of porous quartz glass.
  • a method and a blank of the type mentioned are known from US Pat. No. 4,362,545.
  • SiO 2 particles are deposited in layers on the cylindrical surface of a cylinder with both ends clamped in a lathe and rotating about its longitudinal axis, slightly conical dome.
  • a reciprocating movement of the deposition burner along the longitudinal axis of the dome forms an elongated, porous blank made of SiO 2 particles (soot body).
  • This process is known as the OVD process (Outside Vapor Deposition).
  • Aluminum oxide, quartz glass, graphite or silicon carbide are recommended as suitable materials for the manufacture of the dome.
  • the tubular, porous blank is used as a starting material for the production of a preform for optical fibers. It can be used to build the core and shell material of the preform.
  • the blank according to US Pat. No. 4,362,545 becomes a so-called core rod is produced by sintering and collapsing the inner bore.
  • This blank has a core glass layer made of SiO 2 , which is surrounded by a B 2 0 3 -doped SiO 2 layer.
  • the blank is usually subjected to a treatment in a chlorination process and then glazed in a sintering process.
  • This requires the inner bore to collapse if the blank is to form the central core area of the later preform. Otherwise, the porous or glazed blank is melted onto a further quartz glass cylinder arranged coaxially in the inner bore in the form of a rod or tube.
  • the mandrel must be removed from the inner bore beforehand. In the case of a stuck mandrel, however, this can lead to damage to the inner wall of the blank, which requires complex reworking of the inner bore and thereby increase the manufacturing costs.
  • the present invention is therefore based on the object of specifying a simple and inexpensive method which enables the production of a SiO 2 blank with an inner wall which is as defect-free as possible. Furthermore, the invention is based on the object of providing a blank for the production of a preform for an optical fiber which has an inner bore with an inner wall which is as defect-free as possible. With regard to the method, this object is achieved, based on the method mentioned at the outset, in that a hard layer sequence comprising the first layer is deposited, which has a higher density than layers following the hard layer sequence.
  • the higher density of the hard layer sequence results from a higher surface temperature during the deposition of the first layers of SiO 2 particles on the carrier.
  • the higher density can also be set by heating individual layers of the hard layer sequence or the hard layer sequence as a whole.
  • several comparatively harder layers are produced, which are referred to here as “hard layer sequence”.
  • the hard layer sequence comprises the first layer and at least one further layer.
  • the hard layer sequence is characterized by the fact that it is mechanically much more resistant than softer SiO 2 soot layers. However, this would also be associated with a comparatively stronger mechanical connection of the hard layer sequence with the carrier and, as a result, greater damage to the inner wall when removing the carrier. However, it has surprisingly been found that this effect does not occur if the hard layer sequence comprises at least the first layer and a further layer, and if softer SiO 2 soot layers follow the hard layer sequence. In this case, the effect of the higher mechanical resistance of the hard layer sequence predominates, so that injuries to the inner wall of the blank when pulling out the carrier are avoided; extensive post-processing of the inner wall is therefore not necessary.
  • the tubular, porous blank can consist of homogeneous material, such as doped or undoped SiO 2 ; it can also have areas of different doping. It is used as a starting material for the production of a preform for optical fibers, and it can be used to build up the core and cladding material of the preform.
  • the blank is used in the form of a porous or glazed tube or in the form of a rod.
  • the total thickness of the hard layer sequence must be so great that the required mechanical resistance is achieved.
  • a structure of the porous blank that is as open-pored as possible is to be maintained in order to ensure largely unimpeded access to treatment media in subsequent treatment steps. In view of this, it has proven to be advantageous if only the first to at most tenth layer, preferably the first to at most fifth layer, are deposited as the hard layer sequence.
  • a particularly simple procedure for producing the hard layer sequence results from the fact that a comparatively higher flame temperature of the deposition burner is set during its deposition. Accordingly, the surface temperature is reduced after the hard layer sequence has been deposited by lowering the flame temperature of the at least one deposition burner.
  • the surface temperature is the temperature on the blank surface at the point of impact of the flame.
  • the flame temperature is reduced by reducing the feed rate of burner gases to the at least one deposition burner relative to the feed rates of other gases supplied to the deposition burner.
  • the burner gases are understood to be those gases whose exothermic reaction with one another essentially feeds the burner flame.
  • a detonating gas burner is, for example, the burner gases oxygen and hydrogen.
  • a Lowering the flame temperature is achieved either by reducing the feed rate of oxygen and / or hydrogen to the deposition burner or by feeding or increasing the feed rate of other gases, such as, for example, inert gas or starting materials for the formation of the SiO 2 particles.
  • the surface temperature after the hard layer sequence has been deposited can also advantageously be reduced by increasing the distance between the at least one deposition burner and the surface of the blank being formed.
  • the distance can be increased or decreased. Reducing or increasing the distance can lower the surface temperature if the burner flame becomes colder at the point of impact. This can be the case in particular with so-called focusing deposition burners. The distance is measured between the mouth of the deposition burner and the blank surface.
  • the above-mentioned object is achieved according to the invention starting from the blank mentioned at the outset in that the core glass region has an inner core glass layer comprising the innermost layer and an outer core glass layer, the inner core glass layer being opposite the outer one Core glass layer has a higher density.
  • the blank according to the invention is used to produce a preform for optical fibers, the core glass area forming the central core of the later preform or the optical fiber after the inner bore of the blank has collapsed.
  • the main part of the light is guided.
  • the core glass region has an inner core glass layer which consists of a hard layer sequence comprising the innermost SiO 2 soot layer.
  • the hard layer sequence is formed in that the innermost SiO 2 soot layer and at least one further soot layer have a higher density than layers following the hard layer sequence outwards, so that an area of higher density is produced compared to the layers located further out.
  • the tubular, porous blank can consist of homogeneous material, such as doped or undoped SiO 2 ; it can also have areas of different doping. It is used as a starting material for the production of a preform for optical fibers, and it can be used to build up the core and cladding material of the preform.
  • the blank is used in the form of a porous or glazed tube or in the form of a rod.
  • the total thickness of the inner core glass layer must be so great that the required mechanical resistance is achieved.
  • a structure of the porous blank that is as open-pored as possible is to be maintained in order to ensure largely unimpeded access to treatment media in subsequent treatment steps.
  • the inner core glass layer comprises only the first to at most tenth layer, preferably the first to at most fifth layer.
  • the inner core glass layer has a total thickness of at most 500 ⁇ m; preferably has a maximum of 150 microns.
  • a blank with a hard layer sequence that has a density in the range from 20% to 35% of the density of quartz glass has proven particularly useful.
  • the invention is explained in more detail below on the basis of exemplary embodiments and a drawing. In the drawing, a schematic representation shows in detail:
  • FIG. 1 shows an embodiment of a blank according to the invention in a radial section
  • FIG. 2 shows an exemplary embodiment for producing a preform using a blank according to the invention on the basis of a flow diagram of the individual method steps
  • FIG. 3 shows a section of a typical density curve over the radius in the case of a blank produced by the method according to the invention.
  • Figure 1 shows a blank 1 in the form of a tubular, porous SiO 2 soot body.
  • the blank 1 has a core glass area, to which the overall reference number 2 is assigned and which is coaxially surrounded by a cladding glass area 3.
  • the core glass area 2 consists of SiO 2 soot, which is homogeneously doped with 5% by weight germanium dioxide, the cladding glass area 3 consists of undoped SiO 2 soot.
  • the diameter of the inner bore 4 is 5 mm; the outer diameter of the core glass area 2 is 50 mm and that of the cladding glass area 3 is 100 mm.
  • the core glass region 2 has a thin inner core glass layer 5 directly adjacent to the inner bore 4, which is surrounded by a thicker, outer core glass layer 6.
  • the thickness of the inner core glass layer 5 is only 0.15 mm; in Figure 1, the thickness is shown enlarged for clarity.
  • the remaining core glass area 2 is formed by the outer core glass layer 6.
  • Inner core glass layer 5 and outer core glass layer 6 nominally have the same chemical composition.
  • the main difference between these two layers is that the inner core glass layer 5 has a density of 28% of the density of quartz glass, while the density of the outer core glass layer 6 is only 20% of the density of quartz glass.
  • the density of the individual core glass layers 5, 6 is determined by means of mercury porosimetry. The method according to the invention for producing a tube made of synthetic quartz glass and its use for producing a preform for optical fibers is explained by way of example below with reference to FIG. 2.
  • a so-called core rod is first formed by means of a soot outer deposition method (OVD method) by flame hydrolysis of SiCI and / or GeCI, with corresponding oxide particles being deposited on the outer surface of a mandrel rotating about its longitudinal axis.
  • OTD method soot outer deposition method
  • An aluminum oxide tube with a diameter of 5 mm is used as the mandrel.
  • the inner core glass layer 5 is first deposited by means of a detonating gas deposition burner, in addition to SiCI 4 , GeCI 4 is also fed to the deposition burner in order to obtain the above-mentioned dopant concentration in the core glass region 2.
  • the deposition burner is moved back and forth along the dome longitudinal axis in a predetermined movement cycle, one layer of SiO 2 being produced one after the other on the mandrel or on the cylindrical surface of the blank being formed.
  • An essential method step of the method according to the invention is that a higher density is set in the inner core glass layer 5. This is achieved in that during the deposition of the inner core glass layer 5 a higher surface temperature is set in the area of the point of impact of the deposition burner than when the outer core glass layer 6 is deposited. The surface temperature is measured on the blank surface at the point of impact of the flame of the deposition burner. A commercially available thermal camera is used for this.
  • the inner core glass layer 5 is formed by the three first SiO 2 layers. When these layers are deposited, a surface temperature is set which brings about a specific density of the inner core glass layer 5 of 28% of the density of quartz glass. After the inner core glass layer 5 has been deposited, the outer core glass layer 6 is deposited, the surface temperature being reduced at the same time. There are several ways to do this.
  • the surface temperature after the core glass Layer 5 is reduced by lowering the flame temperature of the deposition burner. This is achieved by reducing the feed rates of the fuel gases hydrogen and oxygen to the separation burner by 15%.
  • the surface temperature after the deposition of the inner core glass layer 5 is reduced in that the distance between the deposition burner and the surface of the blank being formed is increased from 130 mm to 150 mm.
  • the surface temperature after the deposition of the inner core glass layer 5 is reduced in that the speed of the relative movement between the deposition burner and the surface of the blank being formed is increased by 100% by the feed speed of the deposition burner along the mandrel being increased accordingly.
  • the supply of GeCI 4 is stopped and the cladding glass region 3 is deposited in layers on the core glass region 2 using the same method.
  • the mandrel is then removed. Due to the high strength of the inner core glass layer 5, this can be done without damaging the wall of the inner bore.
  • the porous quartz glass tube thus obtained is dried in a chlorine-containing atmosphere and then sintered.
  • a so-called core rod is formed from it by collapsing the inner bore. In this way, a core rod with a diameter of 14 mm is obtained.
  • a flashing tube made of undoped quartz glass (a so-called "jacket tube”) is also produced by flame hydrolysis of SiCI 4 with the formation of SiO 2 particles and axial deposition of the SiO 2 particles on a rotating mandrel
  • the fiber obtained from the preform does not contribute significantly, the requirements for its purity and homogeneity are comparatively low.
  • the jacket tube can therefore be produced inexpensively using several separating burners.
  • the undoped, porous quartz glass is dried in a chlorine-containing atmosphere
  • the jacket tube has an inner diameter during sintering of about 15 mm and an outer diameter of about 60 mm.
  • the jacket tube is then melted onto the core rod by heating the arrangement in an electrically heated furnace to a temperature of 2150 ° C. (furnace temperature).
  • the ring gap is closed without problems by zone-by-zone heating of the vertically oriented arrangement.
  • the preform produced in this way then has an outer diameter of 100 mm.
  • the fiber drawn from it shows an attenuation of 0.6 dB / km at a wavelength of 1385 nm.
  • FIG. 3 shows a section of a typical density curve over the radius in the case of a porous SiO 2 blank produced by the method according to the invention.
  • the density " ⁇ " is plotted on the y-axis of the diagram and the radius "r" on the x-axis.
  • a region of higher density is provided, which is formed by the inner core glass layer 32.
  • the outer core glass layer 33 adjoins the inner core glass layer 32 on the outside and the cladding region 34 adjoins this.
  • the outer core glass layer 33 and the cladding region 34 do not differ in their density in this exemplary embodiment.
  • the density of the outer core glass layer 33 is clearly below the density in the inner core glass layer 32.
  • the interface between the inner core glass layer 32 and the outer core glass layer 33 is indicated by the dotted line 35.
  • the boundary surface is defined as the cylinder jacket surface running parallel to the longitudinal axis, at which the difference in density between the inner core glass layer 32 and the outer core glass layer 33 is half of its maximum value.
  • DE-A1 196 29 170 proposes to create an electrostatic field between the deposition burner and the soot body;
  • DE-A1 196 28 958 and DE-A1 198 27 945 specify measures for the homogenization of the soot separation when using an oscillating burner array.
  • Methods and devices for handling the soot body during and after the deposition process are known from DE-A1 197 51 919 and DE-A1 196 49 935; and US Pat. No. 5,665,132, US Pat. No. 5,738,702 and DE-A1 197 36 949 result in measures for holding the soot body during glazing.

Abstract

L'invention concerne un procédé de fabrication d'une pièce semi-finie en SiO2, selon lequel, et conformément à la technique connue, des couches superposées de particules de SiO2 sont déposées, au moyen d'un brûleur à précipitation, sur la surface latérale d'un support entraîné en rotation autour de son axe longitudinal, de manière à former la pièce semi-finie, le support étant ensuite retiré. L'invention a pour but de faciliter l'enlèvement du support et de permettre ainsi la fabrication d'une pièce semi-finie en SiO2 (1) dont les parois intérieures soient pratiquement exemptes de défauts. En conséquence, l'invention est caractérisée en ce qu'on dépose une succession de couches dures (5) entourant la première couche, présentant une densité supérieure aux couches (6) suivantes appliquées sur ladite succession de couches dures (5). La pièce semi-finie poreuse en SiO2 selon l'invention est caractérisée en ce qu'elle comprend une région formant une âme (2) en verre de quartz poreux, formée d'une pluralité de couches successives, région qui est entourée coaxialement par au moins une région enveloppante (3) en verre de quartz poreux, en ce que la région en verre formant l'âme (2) présente une couche de verre intérieure (5) et une couche de verre extérieure (6) entourant la couche la plus intérieure, et en ce que la couche de verre intérieure (5) de l'âme présente une densité plus élevée par rapport à la couche de verre extérieure (6) de l'âme.
PCT/EP2001/006576 2000-06-19 2001-06-11 Procede de fabrication d'une piece semi-finie en sio2, et piece obtenue suivant ce procede WO2001098219A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10029151.1 2000-06-19
DE2000129151 DE10029151C1 (de) 2000-06-19 2000-06-19 Verfahren für die Herstellung eines SiO¶2¶-Rohlings sowie SiO¶2¶-Rohling

Publications (2)

Publication Number Publication Date
WO2001098219A2 true WO2001098219A2 (fr) 2001-12-27
WO2001098219A3 WO2001098219A3 (fr) 2002-06-20

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DE (1) DE10029151C1 (fr)
WO (1) WO2001098219A2 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10157306C1 (de) * 2001-11-23 2003-06-05 Heraeus Tenevo Ag Verfahren zur Herstellung eines Bauteils aus dotiertem Quarzglas und rohrförmiges Halbzeug hierfür

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DE10029151C1 (de) 2001-08-16

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