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
  • C03B37/01205—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
  • C03B37/01211—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments by inserting one or more rods or tubes into a tube
  • C03B37/0122—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments by inserting one or more rods or tubes into a tube for making preforms of photonic crystal, microstructured or holey optical fibres
• • 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
  • C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
  • C03B37/025—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from reheated softened tubes, rods, fibres or filaments, e.g. drawing fibres from preforms
  • C03B37/027—Fibres composed of different sorts of glass, e.g. glass optical fibres
  • C03B37/02781—Hollow fibres, e.g. holey fibres
• • 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
  • C03B37/01211—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments by inserting one or more rods or tubes into a tube
• • 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
  • C03B37/01225—Means for changing or stabilising the shape, e.g. diameter, of tubes or rods in general, e.g. collapsing
  • C03B37/0124—Means for reducing the diameter of rods or tubes by drawing, e.g. for preform draw-down
• • G—PHYSICS
  • G02—OPTICS
  • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
  • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
  • G02B6/02—Optical fibres with cladding with or without a coating
  • G02B6/02395—Glass optical fibre with a protective coating, e.g. two layer polymer coating deposited directly on a silica cladding surface during fibre manufacture
• • G—PHYSICS
  • G02—OPTICS
  • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
  • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
  • G02B6/02—Optical fibres with cladding with or without a coating
  • G02B6/032—Optical fibres with cladding with or without a coating with non solid core or cladding
• • C—CHEMISTRY; METALLURGY
  • C03—GLASS; MINERAL OR SLAG WOOL
  • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
  • C03B2201/00—Type of glass produced
  • C03B2201/06—Doped silica-based glasses
  • C03B2201/08—Doped silica-based glasses doped with boron or fluorine or other refractive index decreasing dopant
  • C03B2201/12—Doped silica-based glasses doped with boron or fluorine or other refractive index decreasing dopant doped with fluorine
• • C—CHEMISTRY; METALLURGY
  • C03—GLASS; MINERAL OR SLAG WOOL
  • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
  • C03B2201/00—Type of glass produced
  • C03B2201/06—Doped silica-based glasses
  • C03B2201/20—Doped silica-based glasses doped with non-metals other than boron or fluorine
  • C03B2201/24—Doped silica-based glasses doped with non-metals other than boron or fluorine doped with nitrogen, e.g. silicon oxy-nitride glasses
• • C—CHEMISTRY; METALLURGY
  • C03—GLASS; MINERAL OR SLAG WOOL
  • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
  • C03B2201/00—Type of glass produced
  • C03B2201/06—Doped silica-based glasses
  • C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
  • C03B2201/32—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with aluminium
• • C—CHEMISTRY; METALLURGY
  • C03—GLASS; MINERAL OR SLAG WOOL
  • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
  • C03B2203/00—Fibre product details, e.g. structure, shape
  • C03B2203/10—Internal structure or shape details
  • C03B2203/14—Non-solid, i.e. hollow products, e.g. hollow clad or with core-clad interface
• • C—CHEMISTRY; METALLURGY
  • C03—GLASS; MINERAL OR SLAG WOOL
  • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
  • C03B2203/00—Fibre product details, e.g. structure, shape
  • C03B2203/10—Internal structure or shape details
  • C03B2203/14—Non-solid, i.e. hollow products, e.g. hollow clad or with core-clad interface
  • C03B2203/16—Hollow core
• • C—CHEMISTRY; METALLURGY
  • C03—GLASS; MINERAL OR SLAG WOOL
  • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
  • C03B2203/00—Fibre product details, e.g. structure, shape
  • C03B2203/42—Photonic crystal fibres, e.g. fibres using the photonic bandgap PBG effect, microstructured or holey optical fibres

Definitions

• the invention relates to a method for producing an anti-resonant hollow core fiber which has a hollow core extending along a longitudinal axis of the fiber and a cladding area surrounding the hollow core which comprises a number of anti-resonant elements, with the method steps:
• a primary preform for the hollow core fiber which comprises at least one cladding tube which has an inner casing tube bore and a longitudinal axis of the cladding tube along which a cladding tube wall, delimited by an inner side and an outer side, extends,
• the invention also relates to a method for producing a preform for an anti-resonant hollow core fiber, which has a hollow core extending along a longitudinal axis of the fiber and surrounding the hollow core, which comprises several anti-resonant elements, with the method steps:
• Antiresonance elements at target positions of the cladding tube wall are Antiresonance elements at target positions of the cladding tube wall
• hollow core fibers in which the core comprises an evacuated, gas or liquid-filled cavity.
• the interaction of the light with the glass is less than in solid core fibers.
• the refractive index of the core is smaller than that of the cladding, so that light transmission through total reflection is not possible and the light would normally escape from the core into the cladding.
• hollow core fibers are divided into “photonic bandgap fibers” and “anti-resonance reflection fibers”.
• the hollow core area is surrounded by a cladding in which small hollow channels are periodically arranged.
• the periodic structure of the hollow channels in the cladding causes the effect known as the “photonic band gap” based on semiconductor technology, according to which light from certain wavelength ranges scattered on the cladding structures interferes constructively in the central cavity due to Bragg reflection and cannot propagate transversely in the cladding.
• the hollow core area is surrounded by an inner cladding area in which so-called “antiresonant elements” (or “antiresonant elements”; in short: “ AREs ”) are arranged.
• the walls of the anti-resonance elements evenly distributed around the hollow core can act as anti-resonance-operated Fabry-Perot cavities that reflect the incident light and guide it through the fiber core.
• This fiber technology promises low optical attenuation, a very broad transmission spectrum (also in the UV or IR wavelength range) and low latency in data transmission. '
• hollow core fibers are in the field of data transmission, high-performance beam guidance, for example for material processing, modal filtering, non-linear optics, in particular for supercontinuous generation, from the ultraviolet to the infrared wavelength range.
• high-performance beam guidance for example for material processing, modal filtering, non-linear optics, in particular for supercontinuous generation, from the ultraviolet to the infrared wavelength range.
• a disadvantage of antiresonant hollow core fibers is that higher order modes are not necessarily suppressed, so that they are often not purely single-mode over long transmission lengths and the quality of the output beam deteriorates.
• the effective mode suppression depends on the center wavelength of the transmitted light and on structural parameters of the fiber design, such as the radius of the hollow core and the difference in diameter between nested ring structures in the anti-resonance elements.
• An anti-resonant hollow core fiber is known from EP 3 136 143 A1 (referred to there as “hollow core fiber without band gap”), in which the core can conduct other modes in addition to the fundamental mode. For this purpose, it is surrounded by an inner jacket with “non-resonant elements”, which provide phase matching of anti-resonant modes with the higher modes.
• the hollow core fiber is manufactured using a so-called “stack-and-draw technique”, in which the starting elements are arranged in an axially parallel ensemble and fixed in a preform, and the preform is then elongated.
• a cladding tube with a hexagonal inner cross-section is used and six so-called “ARE preforms” (anti-resonance element preforms) are fixed in the inner edges of the cladding tube.
• This preform is drawn into a hollow core fiber in two stages.
• a method for producing a preform for anti-resonant hollow core fibers is known from WO 2018/169487 A1, in which a first cladding area comprises a large number of rods and a second cladding area comprises a multiplicity of tubes which are surrounded by an outer cladding tube. Rods, tubes and cladding are put together using the “stack and draw” technique to form a preform. Before the preform is elongated, the preform end is sealed, which is done by applying a sealing compound.
• a UV adhesive for example, is used as the sealing compound.
• Antiresonant hollow core fibers and especially those with nested structural elements have complex internal geometries, which makes their exact and reproducible manufacture difficult. This is all the more true because, in order to maintain the resonance or anti-resonance conditions, even small dimensional deviations in the order of magnitude of the working wavelength of the light to be conducted cannot be tolerated. Deviations from the target geometry can be caused by the configuration of the fiber preform, and they can also occur as a result of undesired, out-of-scale deformations during the fiber drawing process.
• Antiresonance element preforms each consisting of an antiresonance element outer tube (short: ARE outer tube) and an antiresonant element inner tube (short: ARE inner tube) welded on one side of the ARE outer tube inner surface, on the inside of a cladding tube be attached.
• the azimuthal position of the anti-resonance elements within the cladding tube is important in addition to a uniform wall thickness of the walls of the anti-resonance elements. This cannot be easily realized with the “stack-and-draw” technique.
• the aim of the invention is to provide a method for the cost-effective production of an anti-resonant hollow core fiber which avoids the limitations of conventional production processes.
• the aim of the invention is to provide a method for producing an anti-resonant hollow core fiber and a preform for anti-resonant hollow core fibers with which high precision of the structural elements and exact positioning of the anti-resonant elements in the fiber can be achieved in a sufficiently stable and reproducible manner can
• this object is achieved, based on a method of the type mentioned above, according to the invention in that when a process is carried out according to method step (c), components of the primary preform made of quartz glass and / or components of quartz glass surrounding the primary preform are common heated and softened who the, the quartz glass of at least one of the preform components and / or the quartz glass of at least one of the components surrounding the preform contains at least one dopant that lowers or increases the viscosity of quartz glass.
• Components of the preform include the cladding tube and antiresonance element preforms arranged on the inside of the cladding tube, as well as any additional jacket material produced on the outer jacket surface of the jacket tube.
• the components surrounding the preform are, for example, an overlay cylinder or several overlay cylinders which surround the preform during the hot forming process in order to be collapsed thereon in order to form additional jacket material.
• the components surrounding the preform are also subsumed below under the term “components” of the preform.
• At least one of the preform components contains at least one that reduces the viscosity of quartz glass or increases the viscosity of quartz glass Dopant.
• a type of doping that lowers the viscosity of quartz glass is also referred to below for short as “off-doping” and a type of doping that increases the viscosity of quartz glass is also referred to below for short as ““ on-doping ”.
• Fluorine, chlorine and / or flydroxyl groups are preferably used as dopants which lower the viscosity of quartz glass.
• Al 2 O 3 and / or nitrogen come into consideration as the dopant increasing the viscosity of quartz glass.
• the starting point for the manufacture of the anti-resonant hollow core fiber is a preform, which is also referred to here as a “primary preform”. It comprises a cladding tube in which or on which precursors or preforms for shaping anti-resonant elements in the hollow core fibers (here referred to as “anti-resonant elements” for short) are contained.
• the primary preform can be elongated into the hollow core fiber; As a rule, however, additional jacket material is added to the primary preform in order to create a preform, referred to here as a “secondary preform”.
• the hollow core fiber is created by elongating the secondary preform.
• the primary preform or the secondary preform are surrounded with the formation of a coaxial ensemble of components with a covering cylinder or with several covering cylinders and the coaxial ensemble is elongated directly to form the hollow core fiber.
• the general term “preform” is understood here to denote that component or that coaxial ensemble of components from which the hollow core fiber is ultimately drawn.
• the jacket material is added, for example, by collapsing an overlay cylinder onto the primary preform.
• the coaxial arrangement of the primary preform and the overshooting cylinder is elongated when the overshooting cylinder collapses, or it is not elongated.
• the shape or arrangement of the anti-resonance element preforms is changed, or their shape or arrangement is not changed
• thermal processing Carrying out one of the hot forming processes mentioned in process step (c) (hereinafter also referred to as “thermal processing”) can lead to deformation and structural deviations in the desired fiber geometry. This is particularly the case when both thick-walled and filigree Preform components which are made of the same material are close together or are adjacent to one another.
• the necessary processing temperature is usually determined by the component with the greatest surface area; this is typically the outer jacket area of the preform.
• Smaller components (such as the anti-resonance element preforms and their individual structural elements) are subject to greater deformation at the same temperature. Since during thermal processing the preform is heated from the outside inwards in the heating zone, a radial temperature profile with a minimum in the center of the preform is established over the preform volume. This can aggravate the deformation problem mentioned if filigree components are arranged on a preform radius that is closer to the heating zone than a less filigree component, which is regularly the case with preforms for anti-resonant hollow core fibers.
• the quartz glass contains at least one of the preform components at least one dopant that lowers or increases the viscosity of quartz glass.
• the doping enables the viscosities of neighboring preform components to be adjusted. In particular, it can be used to reduce the thermal stability of one component in favor of the stability of an adjacent component. In particular, by doping the preform component with the greatest surface area, the necessary processing temperature can be lowered and thus the relative stiffness and thermal stability of further internal components can be indirectly improved by exposing them to a lower temperature during the hot forming process.
• a component in the outer jacket area of the preform is provided with an off-doping.
• this is the outermost jacket of the preform. This enables the processing temperature to be lowered, as a result of which the deformation during the hot-forming process can be reduced.
• the optional further processing of the primary preform is the collapse of additional Comprises cladding material
• the additional cladding material consists of quartz glass, which contains a dopant lowering the viscosity of quartz glass, the dopant preferably being fluorine and in a concentration between 500 and 14,500 ppm by weight, preferably between 2,000 and 10,000 ppm by weight is included.
• Fluorine doping of the additional cladding material in this area made it possible to lower the viscosity compared to the quartz glass of the cladding tube, even if the quartz glass of the cladding tube itself does not contain any dopant. It has proven to be beneficial if the quartz glass of the cladding tube at a Messtem temperature of 1250 ° C has a viscosity at least 0.5 dPas higher, preferably at least 0.6 dPas higher viscosity than the quartz glass of the additional jacket material. The viscosity differences are stated here and below as logarithmic viscosity value in dPa s.
• all preform components of the preform consist of different quartz glass qualities, the viscosity of the components increasing as a first approximation from the outside inwards.
• other dopants such as Al 2 O 3 , nitrogen, chlorine and flydroxyl groups can be used to adjust the viscosity.
• Al 2 O 3 has a viscosity-increasing effect in quartz glass up to a concentration of about 15 ppm by weight. In the simplest case, however, it is sufficient if only the additional cladding material contains a dopant and consists of fluorine-containing quartz glass.
• the precursors for antiresonance elements are in the form of tubular antiresonance element preforms, which are preferably composed of several structural elements nested with one another, comprising an ARE outer tube and an ARE inner tube inserted therein, the antiresonance element preforms from Quartz glass be available, which at a measuring temperature of 1250 ° C compared to the quartz glass of the cladding tube has a viscosity at least 0.4 dPas higher, preferably at least 0.5 dPas higher viscosity.
• the quartz glass of the ARE outer tube can increase the viscosity and contain dopants such as Al 2 O 3 or nitrogen. It has however, it has been found to be particularly advantageous if the cladding tube is made of quartz glass which contains a dopant which lowers the viscosity of quartz glass.
• the ARE inner tubes are made of quartz glass, which is at a measuring temperature of 1250 ° C compared to the Quartz glass of the ARE outer tube has a viscosity that is at least 0.4 dPas higher, preferably a viscosity that is at least 0.5 dPas higher.
• the cladding tube is preferably produced in a vertical drawing process without a molding tool with a two-stage elongation process.
• a hollow cylinder made of glass is machined to set the final dimensions of the hollow cylinder.
• the starting cylinder is continuously fed to a heating zone with a first heating zone length, softened in some areas and an intermediate cylinder is withdrawn from the softened area.
• this is continuously fed to another heating zone with a second, shorter heating zone length, where it is softened in some areas and a pipe string is pulled from the softened area.
• the casing tube is obtained from the pipe string by cutting to length.
• the method according to the invention enables the use of comparatively large preforms for thermal processing.
• a secondary preform is preferably formed which has an outer diameter in the range from 30 to 90 mm, and / or that a primary preform is formed which has an outer diameter in the range from 20 mm to 70 mm, preferably in the range of 30 to 70 mm.
• the preform outside diameter in the range from 30 to 90 mm is large compared to the current state of the art. Since the absolute geometry error present during fiber drawing is scaled down with increasing outer diameter of the preform, a more precise production of the hollow core fiber is fundamentally made possible when using a large preform. With diameters larger than 90 mm, however, they form in the fiber drawing process Temperature gradients within the preform volume, which can result in deviations in the wall thickness of the anti-resonance elements in the hollow core fiber. With preform outside diameters of less than 30 mm, there is no longer any special contribution from scaling down the geometry error.
• the outer diameter of the primary preform is in the range from 20 to 70 mm, preferably in the range from 30 to 70 mm. This is a comparatively large outer diameter.
• the outer diameters of the primary preforms are typically 4 to 6 mm.
• the formation of preforms for antiresonance elements according to method step (b) comprises arranging the antiresonance element preforms at target positions on the inside of the cladding tube wall, a positioning template being used for arranging the holding elements for positioning the antiresonance element -Preforms at the target positions.
• the positioning template has, for example, a shaft which protrudes into the inner bore of the casing tube and is provided with holding elements in the form of a plurality of holding arms pointing radially outward.
• the structurally predetermined star-shaped arrangement of the holding elements facilitates the exact positioning of the anti-resonance element preforms at the respective target positions and their fixation.
• the positioning template is preferably used exclusively in the area of the cladding tube end faces, preferably in the area of both cladding tube end faces.
• the accuracy of the positioning of the preforms on the inner circumferential surface of the cladding tube is improved in that the cladding tube inside is produced by machining, in particular by drilling, milling, grinding, honing and / or polishing.
• the accuracy of the positioning of the preforms in the cladding tube is further improved by providing tubular structural elements, at least some of which have a wall thickness in the range of 0.2 and 2 mm, preferably a wall thickness in the range of 0.25 and 1 mm, and wherein a cladding tube with an outer diameter in the range of 90 and 250 mm and preferably with an outer diameter in the range of 120 to 200 mm.
• tubular structural elements at least some of which have a wall thickness in the range of 0.2 and 2 mm, preferably a wall thickness in the range of 0.25 and 1 mm, and wherein a cladding tube with an outer diameter in the range of 90 and 250 mm and preferably with an outer diameter in the range of 120 to 200 mm.
• These components each have a length of at least 1 m and are relatively large-volume structural elements for the formation of anti-resonance elements. This simplifies handling.
• the gravitational force supports the parallelism and vertical alignment of the structural element longitudinal axes when the structural elements are each positioned and fixed at their upper end at the target position, for example and preferably using the Sealing or connecting compound explained in more detail above and additionally or alternatively by means of the positioning template explained in more detail above.
• the technical problem given above is achieved according to the invention, based on a method of the type mentioned at the beginning, in that when carrying out a process according to method step (c) components of the primary preform made of quartz glass and / or the primary preform surrounding quartz glass components are jointly heated and softened, the quartz glass of at least one of the preform components and / or the quartz glass of at least one of the components surrounding the preform containing at least one dopant that lowers the viscosity of quartz glass.
• the preform is the starting point for the manufacture of the anti-resonant hollow core fibers.
• the anti-resonant hollow core fiber is drawn directly or a semi-finished product is first produced from which the anti-resonant hollow core fiber is then drawn.
• the production of the preform includes the formation of constituents of the primary preform from quartz glass, which contains a dopant which lowers the viscosity of quartz glass. This allows the processing temperature to be reduced during the hot forming process and enables comparatively large preforms to be used.
• the anti-resonance elements can be simple or nested structural elements of the hollow core fiber. They have at least two walls that, when viewed from the direction of the hollow core, have a negative curvature (convex) or have no curvature (flat, straight). They usually consist of a material that is transparent to the work light, for example glass, in particular doped or undoped S1O 2 , a plastic, in particular a polymer, a composite material or a crystalline material.
• anti-resonance element preforms Components or parts of the preform are referred to as anti-resonance element preforms, which essentially become anti-resonance elements in the hollow core fiber by simply elongating during the fiber drawing process.
• Antiresonance element precursors are components or parts of the preform that are only transformed into antiresonance element preforms or directly into antiresonance elements through reshaping.
• the anti-resonance element preforms can be simple or nested components on which positioning aids can also be fixed. They are originally in the primary preform.
• Nested antiresonance element preforms form nested antiresonance elements in the hollow core fiber. They are composed of an outer tube and at least one further structural element which is arranged in the inner bore of the outer tube.
• the further structural element can be a further tube which rests against the inner circumferential surface of the outer tube.
• the outer tube is known as the "anti-resonance element outer tube” or as “ARE outer tube” and the other tube as “anti-resonance element inner tube” or “ARE inner tube” for short or also as “nested ARE inner tube”.
• At least one further structural element can be arranged in the inner bore of the nested ARE inner tube, for example a third tube resting on the inner surface of the nested ARE inner tube.
• a distinction is made between “outer nested ARE inner tube” and “inner nested ARE inner tube”.
• cross-section in connection with cylindrical anti-resonance element preforms and their cylindrical structural elements always refers to the cross section perpendicular to the respective cylinder longitudinal axis, namely - unless otherwise stated - the cross section of the outer contour (not: the cross section of the inner contour) for tubular components.
• intermediate products can arise in which the original anti-resonance element preforms are present in a shape that is different from the original shape.
• the changed shape is also referred to here as an antiresonance element preform or as an antiresonance element precursor.
• Preform / primary preform / secondary preform / core preform (cane)
• the preform is the component from which the anti-resonant hollow core fiber is drawn. It is a primary preform or a secondary preform produced by further processing the primary preform.
• the primary preform can be present as an enmul of at least one jacket tube and preforms or precursors for anti-resonance elements loosely received or firmly fixed therein.
• the further processing of the primary preform into a secondary preform from which the hollow core fiber is drawn can include performing one or more of the following hot forming processes once or repeatedly: (i) elongation,
• a core preform is a preform obtained by collapsing and / or elongating a primary preform. Typically, it is covered with additional sheath material before or when the hollow core fiber is drawn.
• the primary preform When elongating, the primary preform is elongated.
• the elongation can take place without collapsing at the same time.
• the elongation can take place to scale so that, for example, the shape and arrangement of components or parts of the primary preform are reflected in the elongated end product.
• the primary preform can also be drawn out of scale and its geometry changed.
• the ensemble of at least one cladding tube and loosely received or firmly fixed preforms or precursors for anti-resonance elements is also referred to here as the “primary preform”.
• the primary preform includes the hollow core and a cladding area. This mantle area is also called the “inner Jacket area ”denotes if there is also an“ outer jacket area ”, which has been created, for example, by collapsing onto the ensemble, and if a distinction should be made between these jacket areas.
• the terms “inner cladding area” and “outer cladding area” are also used for the corresponding areas in the hollow core fiber or in intermediate products that are obtained through further processing of the primary preform.
• pipe inside is also used as a synonym for “pipe inner jacket surface” and the term “pipe outside” is also used as a synonym for “pipe outer jacket surface”.
• inner bore in connection with a pipe does not mean that the inner bore was created by a drilling process.
• This processing creates a longitudinal structure which extends in the direction of the longitudinal axis of the filler tube and which serves as a positioning aid for the anti-resonance element preforms.
• the longitudinal structure is accessible from the inside of the cladding tube; it can also extend to the outside through the entire cladding tube wall.
• Particle size and particle size distribution of the SiC particles are characterized on the basis of the Dso values. These values are taken from particle size distribution curves which show the cumulative volume of the SiC particles as a function of the particle size.
• the particle size distributions are often characterized on the basis of the respective D10, D50 and D90 values.
• the Dio value characterizes the particle size that is not achieved by 10% of the cumulative volume of the Si0 2 particles, and accordingly the Dso value and the D90 value those particle sizes that are 50% and 90% of the cumulative volume of the Si0 2 particles is not reached.
• the particle size distribution is determined by scattered light and laser diffraction spectroscopy according to ISO 13320.
• FIG. 1 shows a coaxial tube arrangement made up of an overlay cylinder and a primary preform, which is composed of a cladding tube and anti-resonance element preforms positioned and fixed therein, using a view of the cross section,
• Figure 2 is a diagram of the radial course of the fluorine concentration
• FIG. 3 shows a sketch to explain an ideal radial concentration or viscosity profile of a preform for a hollow core fiber.
• a sealing compound based on S1O2 is used, as is known from DE 10 2004 054 392 A1. Since an aqueous slip is produced by wet grinding of quartz glass grains, which contains amorphous Si0 2 particles with a particle size distribution which is characterized by a D 50 value of about 5 pm and a D90 value of about 23 pm. Further amorphous Si0 2 grains with an average grain size of about 5 ⁇ m are added to the base slip.
• the slip used as the bonding compound has a solids content of 90%, at least 99.9% by weight of which consists of S1O2.
• Figure 1 shows schematically the coaxial tube arrangement 1 with a Studentsfangzy cylinder 2, a cladding tube 3 with a cladding tube wall, on the inside at previously defined azimuthal positions at a uniform distance
• Antiresonance element preforms 4 are fixed; in the exemplary embodiment there are six preforms 4, in another preferred embodiment, not shown, it is an odd number of preforms.
• the cladding tube 3 has an outer diameter of 27 mm and an inner diameter of 20 mm.
• the anti-resonance element preforms 4 are present as an ensemble of interleaved structural elements made up of an ARE outer tube 4a and an ARE inner tube 4b.
• the ARE outer pipe 4a has an outer diameter of 6.2 mm and the ARE inner pipe 4b has an outer diameter of 2.5 mm.
• the wall thickness of both structural elements (4a; 4b) is the same and is 0.3 mm. All tubular components 2, 3, 4a, 4b have a length of 700 mm.
• the anti-resonance element preforms 4 are fixed to the inner wall of the cladding tube 3 by means of the connecting compound based on S1O2.
• the compound is applied locally to the cladding tube inner surface in the area of the front ends and the antiresonance element preforms 4 are placed on it using a positioning template with a structurally predetermined star-shaped arrangement of holding arms for the individual antiresonance element preforms 4.
• the action of the positioning template is limited to the area around the two cladding tube ends.
• the primary preform obtained in this way is covered with the covering cylinder 2 made of quartz glass.
• the overlapping cylinder 2 has an outside diameter of 63.4 mm and a wall thickness of 17 mm.
• the coaxial tube arrangement is elongated at the same time.
• the coaxial tube arrangement of cladding tube 3 and cover cylinder 2 is fed to a temperature-controlled heating zone coming from below with a vertically oriented longitudinal axis and is softened in zones beginning with the upper end of the tube arrangement.
• the heating zone is set to a target temperature of 1580 ° C held with a control accuracy of +/- 0.1 ° C. This allows temperature fluctuations in the hot forming process to be limited to less than +/- 0.5 ° C.
• the secondary preform formed in the collapsing and elongation process has an outer diameter of about 50 mm and a wall thickness of 16.6 mm, made up of the outer jacket and inner jacket. It is then drawn to the anti-resonant hollow core fiber. Before this, all anti-resistance element preforms are closed with the sealing or bonding compound. The sealing compound is only applied to that end face of the anti-resonance element preforms which faces upward during the fiber drawing process. This face is connected to a holding tube made of quartz glass, which also serves as a gas connection. The holder is fixed to the covering cylinder 2 and to the cladding tube 3 by means of the sealing or connecting compound.
• the secondary preform is fed from above with a vertically oriented longitudinal axis to a temperature-controlled heating zone, where it is softened zone by zone starting with the lower end.
• gas is supplied to the core area (hollow core) so that an internal pressure of 4 mbar is established in the core area.
• the heating zone is kept at a target temperature of around 2080 ° C with a control accuracy of +/- 0.1 ° C. This allows temperature fluctuations in the hot forming process to be limited to less than +/- 0.5 ° C.
• the existing absolute geometric error is scaled down, so that in the hollow core fiber the anti-resonance elements obtained from the anti-resonance element preforms have a maximum deviation of less than 3.5% in the wall thickness (based on an average wall thickness) .
• the small error in the wall thickness is attributed on the one hand to the use of the comparatively large secondary preform and the associated scaling down of the original absolute geometric deviations and on the other hand to the comparatively low processing temperatures in the hot forming processes (elongation and collapse, fiber drawing).
• the lower processing temperatures are in turn due to the fact that the cladding cylinder 2 and the cladding tube 3 consist of quartz glass, which with Fluorine is doped. In the coaxial arrangement 1, these components represent the components with the greatest surface area and decisively determine the processing temperature.
• the necessary processing temperature can be lowered and the relative stiffness and thermal stability of the tire resonance element preforms 4 further inside can be indirectly improved by exposing them to a lower temperature during the industrial molding process will.
• the following table 1 summarizes information on the materials of the components of the coaxial arrangement or of the secondary preform.
• the fluorine-doped quartz glass tubes (2; 3) have a fluorine concentration profile with a maximum of the fluorine concentration in the middle of the tube wall.
• the data on the fluorine concentration of the quartz glass given in the "Material" column of Table 1 are mean values.
• the diagram in FIG. 2 shows measured fluorine concentration profiles C (in ppm by weight) for a cladding tube C F (M) and for an overlay cylinder C F (Z) ”, as well as Vis calculated from the concentration profiles for a temperature of 1250 ° C viscosity profile h (in lg dPa-s) along the radial position coordinate (position P (in mm)).
• the fluorine concentration curve in quartz glass is determined by infrared spectroscopy.
• the viscosity scales with the fluorine concentration for a given temperature and is calculated based on a base value for undoped quartz glass (h 11.8 dPa-s (corresponds to 100%)) using the following formula: Decrease in viscosity at 1250 ° C: 12% ( ⁇ 2%) per wt% fluorine.
• Table 2 shows viscosity values for the fluorine content of commercially available quartz glass qualities (for a measuring temperature of 1250 ° C).
• the diagram of Figure 2 shows that the viscosity of the cover cylinder h (Z) is lower than that of the cladding tube h (M).
• the viscosity of both quartz glass tubes has a minimum in the middle of the tube, which is around 10 11 - 45 dPa-s for the cladding tube and around 10 10 - 65 dPa s for the overlay cylinder.
• the difference in viscosity between the minima (in lg dPa -s) is thus around 0.80 dPa-s.
• the difference between the viscosity of the cladding tube in the area of the outside of the cladding tube (approx. 10 11 ' 5 dPa-s) and the viscosity minimum in the casing cylinder is approx. 0.85 (in lg dPa-s.
• the difference in viscosity in the area of the contact surface is thus about 0.35 (in lg dPa-s).
• the structural elements (4a; 4b) of the antiresonance element preforms (4) consist of undoped quartz glass and have a viscosity of about 10 11 8 dPa s.
• the diagram of FIG. 3 shows the radial dopant concentration profile over the wall of the secondary preform in an idealized form.
• the fluorine concentration CF (in relative unit) is plotted against the position coordinate P (in relative unit) on the y-axis.
• the dopant concentration CF (Z) of the fluorine-doped quartz glass that comes from the cladding cylinder is ideally as high as the concentration CF (M) of the fluorine-doped quartz glass that comes from the cladding tube.
• the corresponding viscosity profile of the viscosities of the cladding tube and the cover cylinder accordingly shows the same viscosity on both sides at the contact surface K.

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• 2019
  • 2019-07-17 EP EP19186863.7A patent/EP3766850B1/de active Active
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