Producing capillaries from cylinders

The method of continuous drawing and inverse collapse of large quartz glass cylinders with controlled diameter ratios addresses the inefficiencies of existing capillary production, achieving high-quality capillaries without thermal pretreatment and intermediate steps, enhancing productivity and reducing costs.

WO2026093466A1PCT designated stage Publication Date: 2026-05-07HERAEUS QUARZGLAS GMBH & CO KG
View PDF 11 Cites 0 Cited by

Patent Information

Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
HERAEUS QUARZGLAS GMBH & CO KG
Filing Date
2025-10-30
Publication Date
2026-05-07

AI Technical Summary

Technical Problem

Existing methods for producing capillaries or antiresonance element preforms require additional drawing steps and special pretreatments, leading to low productivity and high costs, and often result in inconsistent quality.

Method used

A method involving the continuous drawing of large hollow quartz glass cylinders through a heating zone with inverse collapse and elongation, maintaining a specific outer-to-inner diameter ratio of 1.2 to 6.0, allowing direct production of capillaries without thermal pretreatment, and using internal blowing pressure to stabilize the shape.

Benefits of technology

This method enables high-quality capillaries to be produced efficiently and consistently, eliminating the need for intermediate steps and reducing production costs, while maintaining precise diameter ratios.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure EP2025081426_07052026_PF_FP_ABST
    Figure EP2025081426_07052026_PF_FP_ABST
Patent Text Reader

Abstract

The present invention relates to a method for producing capillaries from large, mechanically processed quartz glass hollow cylinders, and to the capillaries produced according to the invention. The method comprises: continuously supplying a quartz glass hollow cylinder having an outer diameter Za and an inner diameter Zi into a heating zone until part of the quartz glass hollow cylinder is softened therein; and inversely collapsing and simultaneously elongating the quartz glass hollow cylinder from the softened part in order to obtain a capillary strand having an outer diameter Ca and an inner diameter Ci such that (Za∕Zi)∕(Ca∕Ci) = 1.2 to 6.0.
Need to check novelty before this filing date? Find Prior Art

Description

[0001] 2023PF00181

[0002] 1

[0003] Production of capillaries from cylinders

[0004] INTRODUCTION

[0005] The present invention relates to a method for producing capillaries or antiresonance element preforms, comprising a process step in which a hollow cylinder with an outer diameter Z is a and an inner diameter Zj, is continuously drawn through a heating zone to form a capillary strand.

[0006] BACKGROUND OF THE INVENTION AND STATE OF THE ART

[0007] The present invention relates to a method for producing capillaries or antiresonance element preforms, comprising a process step in which a hollow cylinder with an outer diameter Z is aand an inner diameter Zj, is continuously drawn through a heating zone to form a capillary strand. An internal blowing pressure is applied within the capillary strand to stabilize a round cross-section or, if necessary, to change the inner diameter relative to the outer diameter. In particular, the outer diameter is reduced. The capillary strand is defined by an outer diameter C. a and characterized by an inner diameter Ci.

[0008] By cutting the capillary strand to the desired length, capillaries of the required length are obtained. These serve as semi-finished products in the production of preforms for optical fibers, specifically as antiresonance element preforms. When these preforms are further processed into antiresonance hollow core fibers, the antiresonance element preforms incorporated within them become antiresonance elements.

[0009] In principle, methods for manufacturing such capillaries or antiresonance element preforms are already known in the prior art.

[0010] EP 4 011 840 A relates to a method for manufacturing a preform for an antiresonant hollow-core fiber. The preform consists of at least one sheath tube and at least one antiresonant element preform, which is fixed to the inside of the sheath tube by means of thermal input. A contact element between the sheath tube and the at least one antiresonant element preform is necessary to avoid the risk of damaging the antiresonant preform through thermal input.

[0011] JP 2004 123461 A relates to a process for manufacturing glass bodies that can serve as capillaries or antiresonance element preforms. In a first step, a glass hollow cylinder is polished until it has a mean surface roughness of 0.05 pm or less. The glass hollow cylinder is then elongated using a hot forming process. 2023PF00181

[0012] 2

[0013] EP 0 598 349 A relates to quartz glass hollow cylinders with a large diameter and capillaries or antiresonance element preforms which are processed into such products by means of the claimed method for the production of antiresonance hollow core fibers.

[0014] CN 116715447 A relates to a process for producing an F-doped glass hollow cylinder, which can be used to manufacture antiresonance element preforms. The doped hollow cylinder is elongated into an antiresonance element preform in a hot forming step using a process also described in CN 116715447 A. During this process, a gas stream is passed through the cylinder to stabilize its internal geometry.

[0015] WO 2008 / 138744 A concerns a process for manufacturing glass bodies that can serve as capillaries or antiresonance elements or preforms. For this purpose, a hollow cylinder made of quartz glass is elongated by drawing it along a drawing axis through a hot forming zone using a suitable roller drawer.

[0016] WO 2006 / 122904 A also addresses a process for manufacturing glass bodies that can serve as capillaries or antiresonance element preforms. For this purpose, a hollow cylinder made of quartz glass is elongated, which has a well-defined outer and inner radius. A radius ratio of 1.02 to 1.7 is targeted. This radius ratio ensures that the dimensional relationship between the outer and inner radii of the hollow cylinder is maintained even after the hot forming process in the capillary or antiresonance element preform.

[0017] WO 2004 / 083141 A concerns a process for manufacturing capillaries or antiresonance element preforms. A hollow cylinder made of synthetic quartz glass is fed from above into a furnace with an annular graphite heating element, oriented vertically along the cylinder's longitudinal axis. The desired ratio of the outer to inner diameters of the hollow cylinder is approximately 2.14. After elongation, the ratio of the outer to inner diameters in the capillary or antiresonance element preform is approximately 1.27.

[0018] DE 102 28 599 A relates to a further process for the production of glass bodies that can serve as capillaries or preforms for antiresonance elements. In this process, a hollow cylinder made of quartz glass is elongated into a tapered glass shape using hot forming processes. During the process, a gas stream is passed through the elongated body. This gas stream is a mixture of inert gas and oxygen, and the oxygen concentration can be varied.

[0019] CN 113651527 A relates to a process for the production of capillaries or antiresonance element preforms in which glass cylinders produced by vapor deposition are elongated. 2023PF00181

[0020] 3

[0021] EP 3 112 323 A relates to a process for manufacturing glass bodies that can serve as preforms for antiresonance elements. In this process, a hollow cylinder made of quartz glass with a specific inner and outer diameter is elongated under heat to form a new, tapered shape. To prevent the formed hollow cylinder from undergoing undesirable geometric deformations or even damage during the forming process, a counter-pressure is generated on the inside of the cylinder during the hot forming process, which promotes the formation of the undamaged and desired shape.

[0022] TASK OF INVENTION

[0023] A first object of the present invention is to avoid the use of a "small" semi-finished product or the need for an additional drawing step to create a small semi-finished product from a large one. Both approaches would lead to low productivity and high costs in the provision of the semi-finished products.

[0024] A further object of the present invention is to provide a method in which hollow cylinders can be processed into capillaries or antiresonance element preforms without the need for any special pretreatment of the hollow cylinders. The method should be scalable to an industrial scale and provide capillaries or antiresonance element preforms of consistent quality.

[0025] The inventors of the present invention have surprisingly succeeded in solving the problem by carrying out the process starting with large hollow cylinders whose inner and outer diameter ratio lies within a specific range according to the invention. Starting with hollow cylinders possessing such properties, the inventors have succeeded in continuously producing high-quality capillaries through collapse and elongation steps of the hollow cylinder. The ratio of the outer and inner diameters of both the hollow cylinder and the capillary strand lies within a size range according to the invention, which ensures the stability and quality of the separated capillaries.

[0026] BRIEF DESCRIPTION OF THE INVENTION

[0027] The present invention relates to a method for producing antiresonance element preforms according to the following points:

[0028] [1] Method for the production of capillaries or antiresonance element preforms, comprising the steps: 2023PF00181

[0029] 4 i) Providing a hollow quartz glass cylinder with a large outer diameter Z a , a small inner diameter Zi; ii) Continuous feeding of the quartz glass hollow cylinder into a heating zone until the quartz glass hollow cylinder is softened in certain areas; iii) Inverse collapse and simultaneous elongation of the quartz glass hollow cylinder from the softened area to form a capillary strand with an outer diameter C a and to obtain an inner diameter Cj, characterized in that the outer and inner diameter ratio of the cylinder changes during inverse collapse and simultaneous elongation to the capillary such that: 1.2 to 6.0;

[0030] Preferably 2.9 to 4.2 iv) Cutting off the capillary strand to the desired length while obtaining capillaries with an outer diameter C a and an inner diameter Cj, for which the following applies:

[0031] 1.05 to 1.50, preferably 1.08 to 1.30.

[0032] [2] Method for the production of capillaries or antiresonance element preforms, comprising the steps of: i) providing a hollow quartz glass cylinder with a large outer diameter Z a , a small inner diameter Zi; ii) Continuous feeding of the quartz glass hollow cylinder into a heating zone until the quartz glass hollow cylinder is softened in certain areas; iii) Inverse collapse and simultaneous elongation of the quartz glass hollow cylinder from the softened area to form a capillary strand with an outer diameter C aand to obtain an inner diameter Cj, characterized in that the outer and inner diameter ratio of the cylinder changes during inverse collapse and simultaneous elongation to the capillary such that: 1.2 to 6.0; preferably 2.9 to 4.2 iv) Cutting off the capillary strand to the desired length while obtaining capillaries with an outer diameter C a and an inner diameter Cj, for which the following applies:

[0033] — = greater than 1.00 to 1.30, preferably 1.02 to 1.30, further preferred 1.05 to 1.28, even more preferred 1.05 to 1.25. 2023PF00181

[0034] 5

[0035] [3] Method according to [1] or [2], characterized in that the quartz glass hollow cylinder is a mechanically machined quartz glass hollow cylinder,

[0036] [4] Method according to [1] to [3], characterized in that the quartz glass hollow cylinder does not require thermal pretreatment.

[0037] [5] Method according to [1] to [4], characterized in that the quartz glass hollow cylinder has a large outer diameter of 120 mm to 250 mm, preferably an outer diameter of 150 mm to 200 mm.

[0038] [6] Method according to [1] to [5], characterized in that the quartz glass hollow cylinder has a small inner diameter of 20 mm to 140 mm, preferably an inner diameter of 35 mm to 90 mm.

[0039] [7] Method according to [1] to [6], characterized in that the following applies to the ratio of the outer and inner diameter of the mechanically machined hollow quartz glass cylinder:

[0040] 1.8 to 5.0, room

[0041] Preferably, the quartz glass hollow cylinder has a ratio of outer to inner diameter of 1.8 to 3.0.

[0042] [8] Method according to [1] to [7], characterized in that the capillaries formed from the mechanically machined hollow quartz glass cylinder have an outer diameter of 2 mm to 20 mm, preferably an outer diameter of 2.6 mm to 17 mm.

[0043] [9] Method according to [1] to [8], characterized in that the capillaries formed from the mechanically machined hollow quartz glass cylinder have an inner diameter of 1 mm to 17 mm, preferably an inner diameter of 2 mm to 15.5 mm.

[0044]

[0010] Method according to [1] to [9], characterized in that the drawing speed of the capillary strand during the drawing process is 1 m / min to 6 m / min.

[0045]

[0011] Method according to [1] to

[0010] , characterized in that the tracking rate of the quartz glass hollow cylinder is 0.3 mm / min to 3 mm / min, preferably 1.1 mm / min to 1.5 mm / min.

[0046]

[0012] Method according to [1] to

[0011] , characterized in that the feed rate of the quartz glass hollow cylinder is 3.5 kg / h to 6.0 kg / h, preferably 3.9 to 5.3 kg / h. 2023PF00181

[0047] 6

[0048]

[0013] Method according to [1] to

[0012] , characterized in that quartz glass hollow cylinders with a volume flow rate between 29 cm 3 / min and 40 cm 3 / min are formed into a capillary strand.

[0049]

[0014] Method according to [1] to

[0013] , characterized in that a hollow quartz glass cylinder with a cross-sectional area of ​​10000 mm² is used to produce 2 up to 31000 mm 2 capillaries with a cross-sectional area of ​​2 mm 2 up to 40 mm 2 will be obtained.

[0050]

[0015] Method according to [1] to

[0014] , characterized in that the train section behind the heating zone to section position 1 is 0.0 m to 8.0 m long, preferably 1.5 m to 6.0 m long.

[0051]

[0016] Method according to [1] to

[0015] , characterized in that the capillary strand is protected against vibrations during the pulling process on the pulling path by means of suitable stabilizers.

[0052]

[0017] Method according to [1] to

[0016] , characterized in that during the drawing process of the capillary strand from the softened quartz glass hollow cylinder a blowing pressure p + is generated in the inner bore of the quartz glass hollow cylinder or the resulting capillary strand.

[0053]

[0018] Method according to

[0017] , characterized in that the blowing pressure p + between the equilibrium pressure of the quartz glass hollow cylinder pz and the equilibrium pressure of the capillary strand pc.

[0054]

[0019] Method according to

[0017] or

[0018] , characterized in that the blowing pressure is generated with a gas or gas mixture comprising dry air, nitrogen, argon and / or helium, preferably with dry air.

[0055]

[0020] Method according to [1] to

[0019] , characterized in that the separation of the capillaries to the desired length from a capillary strand comprises cutting, sawing, breaking and mixtures thereof.

[0056]

[0021] Method according to [1] to

[0020] , comprising the following steps: i) Providing a hollow quartz glass cylinder with an outer diameter Z a , from 120 mm to 250 mm and an inner diameter Zj from 20 mm to 140 mm; ii) Continuous feeding of the quartz glass hollow cylinder into a heating zone at a feed rate of 0.3 mm / min to 3 mm / min until the quartz glass hollow cylinder is softened in certain areas; iii) Inverse collapse and simultaneous elongation of the quartz glass hollow cylinder made of 2023PF00181

[0057] 7. The softened area is drawn at a speed of 1 m / min to 6 m / min while an internal blowing pressure p is applied. + is created to form a capillary strand with an outer diameter C a and to obtain an inner diameter Ci, characterized in that the outer and inner diameter ratio of the cylinder changes during inverse collapse and simultaneous elongation to the capillary such that: 2.9 to 4.2; iv) Cutting the capillary strand to the desired length while retaining capillaries with an outer diameter C a and an inner diameter Ci, for which the following applies:

[0058] 1.05 to 1.50, 'preferably 1.08 to 1.30.

[0059]

[0022] Method according to [1] to

[0020] , comprising the following steps: i) Providing a hollow quartz glass cylinder with an outer diameter Z a, from 120 mm to 250 mm and an inner diameter Zi of 20 mm to 140 mm; ii) Continuous feeding of the quartz glass hollow cylinder into a heating zone at a feed rate of 0.3 mm / min to 3 mm / min until the quartz glass hollow cylinder is softened in certain areas; iii) Inverse collapse and simultaneous elongation of the quartz glass hollow cylinder from the softened area at a drawing speed of 1 m / min to 6 m / min while an internal blowing pressure p + is created to form a capillary strand with an outer diameter C a and to obtain an inner diameter Ci, characterized in that the outer and inner diameter ratio of the cylinder changes during inverse collapse and simultaneous elongation to the capillary such that: 2.9 to 4.2; iv) Cutting the capillary strand to the desired length while retaining capillaries with an outer diameter C aand an inner diameter Ci, for which the following applies: 1.00 to 1.30, 2023PF00181

[0060] 8 preferably 1.02 to 1.30, further preferably 1.05 to 1.28, even more preferably 1.07 to 1.25.

[0061]

[0023] Method comprising the following steps: i) Providing a hollow quartz glass cylinder with an outer diameter Z a , from 120 mm to 250 mm and an inner diameter Zj from 20 mm to 140 mm; ii) Continuous feeding of the quartz glass hollow cylinder into a heating zone at a feed rate of 0.3 mm / min to 3 mm / min until the quartz glass hollow cylinder is softened in certain areas; iii) Inverse collapse and simultaneous elongation of the quartz glass hollow cylinder from the softened area at a drawing speed of 1 m / min to 6 m / min while an internal blowing pressure p + is created to form a capillary strand with an outer diameter C aand to obtain an inner diameter Cj, characterized in that the outer and inner diameter ratio of the cylinder changes during inverse collapse and simultaneous elongation to the capillary such that: 2.9 to 4.2; iv) Cutting the capillary strand to the desired length while retaining capillaries with an outer diameter C a and an inner diameter Cj, for which a ratio of outer diameter C applies a to have an inner diameter Cj of less than 1.30, preferably less than 1.28, even more preferably less than 1.25.

[0062]

[0024] Method according to

[0023] , wherein the produced capillaries have a ratio of outer diameter C a to have an inner diameter Cj of greater than 1.00, preferably greater than 1.02, more preferably greater than 1.05, and even more preferably greater than 1.07.

[0063]

[0025] Method according to

[0023] or

[0024] , wherein the produced capillaries have a ratio of outer diameter C a to have an inner diameter Cj of greater than 1.0 to 1.30, preferably 1.02 to 1.30, more preferably 1.05 to 1.28, and even more preferably 1.07 to 1.25.

[0064]

[0026] Method according to

[0023] to

[0025] , wherein the produced capillaries have an inner diameter Cj of less than 20 mm, preferably less than 19 mm, more preferably less than 18 mm, more preferably less than 17 mm, more preferably less than 16.5 mm.

[0065]

[0027] Method according to

[0023] to

[0026] , wherein the produced capillaries have an inner diameter Cj of greater than 1 mm, preferably greater than 1.5 mm, and even more preferably greater than 2 2023PF00181

[0066] 9 mm.

[0067]

[0028] Method according to

[0023] to

[0027] , wherein the produced capillaries have an inner diameter Ci of 1 to 20 mm, preferably 1 to 19 mm, more preferably 1.5 to 18 mm, more preferably 1.5 to 17 mm, more preferably 2.0 to 16.5 mm.

[0068]

[0029] Method according to

[0023] to

[0028] , wherein the produced capillaries have a ratio of outer diameter C a for inner diameter Ci of greater than 1.0 to 1.30, preferably 1.02 to

[0069] 1.30, more preferably 1.05 to 1.28, even more preferably 1.07 to 1.25, and have an inner diameter Ci of 1 to 20 mm, preferably 1 to 19 mm, more preferably 1.5 to 18 mm, more preferably 1.5 to 17 mm, even more preferably 2 to 16.5.

[0070]

[0030] Capillary, characterized in that it has a ratio of outer diameter C ato have an inner diameter Ci of less than 1.30, preferably less than 1.28, and even more preferably less than 1.25.

[0071]

[0031] Capillary according to

[0030] , characterized in that it has a ratio of outer diameter C a to have an inner diameter Ci of greater than 1.00, preferably greater than 1.02, more preferably greater than 1.05, and even more preferably greater than 1.07.

[0072]

[0032] Capillary according to

[0030] or

[0031] , characterized in that it has a ratio of outer diameter C a for inner diameter Ci of greater than 1.0 to 1.30, preferably 1.02 to

[0073] 1.30, more preferably 1.05 to 1.28, and even more preferably 1.07 to 1.25.

[0074]

[0033] Capillaries according to

[0030] to

[0032] , characterized in that they have an inner diameter Ci of less than 20 mm, preferably less than 19 mm, more preferably less than 18 mm, more preferably less than 17 mm, and still more preferably less than 16.5 mm.

[0075]

[0034] Capillaries according to

[0030] to

[0033] , characterized in that they have an inner diameter Ci of greater than 1 mm, preferably greater than 1.5 mm, more preferably greater than 2 mm.

[0076]

[0035] Capillaries according to

[0030] to

[0034] , characterized in that they have an inner diameter Ci of 1 to 20 mm, preferably 1 to 19 mm, more preferably 1.5 to 18 mm, more preferably 1.5 to 17 mm, and even more preferably 2 to 16.5 mm.

[0077]

[0036] Capillary according to

[0030] to

[0035] , characterized in that it has a ratio of outer diameter C afor inner diameter Ci of greater than 1.0 to 1.30, preferably 1.02 to

[0078] 1.30, more preferably 1.05 to 1.28, even more preferably 1.07 to 1.25, and an In- 2023PF00181

[0079] 10. The nominal diameter Ci ranges from 1 to 20 mm, preferably 1 to 19 mm, more preferably 1.5 to 18 mm, more preferably 1.5 to 17 mm, and even more preferably 2 to 16 mm.

[0080]

[0037] Capillary, characterized in that it has an outer diameter C a and has an inner diameter Ci for which the following applies:

[0081] 1.05 to 1.50,

[0082] Ci' prefers 1.08 to 1.30.

[0083]

[0038] Capillary according to

[0037] , characterized in that it has an equilibrium pressure PEQ of 50 Pa to 800 Pa.

[0084]

[0039] Capillary according to

[0037] or

[0038] , characterized in that the ratio of a longer axis to a shorter axis in the cross-section is 1.00 to 1.02, preferably less than 1.01, measured by means of an optical microscope.

[0085]

[0040] Capillary according to

[0037] to

[0039] , characterized in that it has an outer diameter C a and has an inner diameter Ci for which the following applies:

[0086] 1.05 to 1.50, preferably 1.08 to 1.30 and has an equilibrium pressure pc between 50 Pa and 800 Pa, and that the ratio of a longer axis to a shorter axis in the cross-section is 1.00 to 1.02.

[0087]

[0041] Capillaries according to

[0030] to

[0040] , obtainable by a process of [1] to

[0029] ,

[0088] DETAILED DESCRIPTION OF THE INVENTION

[0089] I. Definitions

[0090] For the purposes of the present invention, the term collapse refers to a process in which the geometry of a semi-finished product is altered such that the ratio of its outer to inner diameters increases. For example, a tubular semi-finished product collapses in a controlled manner, the inner diameter decreases faster than the outer diameter, and it undergoes controlled collapse. Typically—but not necessarily—collapse steps are carried out together with elongation steps under the influence of temperature. 2023PF00181

[0091] 11 leads.

[0092] For the purposes of the present invention, the term elongation refers to a process in which the geometry of a semi-finished product is altered to such an extent that its length is increased. Elongation steps are carried out under the influence of temperature and, optionally, pressure.

[0093] In the context of the present invention, the term "ratio drawing" refers to a process in which the ratio between the outer and inner diameters of a semi-finished product remains constant during its processing into a capillary strand or capillary. Ratio drawing typically occurs in the range of relatively large outer and inner diameters, as defined by the invention. If the outer and inner diameters fall below a certain threshold during processing, it becomes necessary to apply an internal pressure corresponding to the equilibrium pressure of the semi-finished product in order to perform the ratio drawing.

[0094] In the context of the present invention, the term "inverse collapse" refers to a process in which the geometry of a semi-finished product is altered such that the ratio of its outer to inner diameters decreases. This means that the outer diameter decreases faster than the inner diameter, which typically requires the application of an internal pressure that is higher than the equilibrium pressure of the semi-finished product.

[0095] For the purposes of the present invention, the term semi-finished product is a collective term which includes any intermediate product according to the invention which can be further processed into a capillary or an antiresonance element preform within a process step according to the invention.

[0096] For the purposes of the present invention, the term quartz glass hollow cylinder refers to a semi-finished product from which capillary strands are produced by means of the inventive method through collapse-inverse collapse and elongation steps or in a proportional process. Quartz glass hollow cylinders within the meaning of the present invention are usually manufactured mechanically and are characterized by large outer and inner diameters Z. a and Zj compared to quartz glass hollow cylinders, which are commonly used in the prior art to manufacture capillaries. Mechanically manufactured quartz glass hollow cylinders are preferred.

[0097] For the purposes of the present invention, the term capillary strand refers to the result of carrying out the inventive ratio steps or inverse collapse and elongation steps performed on quartz glass hollow cylinders. Capillary strands within the meaning of the present invention are characterized by an outer 2023PF00181

[0098] 12 diameter C a and an inner diameter Ci, and they can be further processed into capillaries in accordance with the invention by cutting them to a target length.

[0099] In the context of the present invention, the term capillaries refers to tubular bodies, usually made of glass. The capillaries according to the invention have an inner capillary bore and a longitudinal axis along which a capillary wall extends, bounded by an inner capillary surface and an outer capillary surface. The capillaries according to the invention have an inner capillary diameter Ci and an outer capillary diameter C. a The term capillaries, as used in this invention, refers exclusively to individual capillary units that have been cut from a capillary strand. According to the invention, capillaries are further processed into an antiresonance element within an antiresonance hollow-core fiber. In this context, the capillaries according to the invention are also referred to as antiresonance element preforms. The capillaries according to the invention are, as indicated by the inner capillary diameters Ci and C,a recognizably, all are very thin-walled and therefore have a low C ratio. a / Cj on.

[0100] When, within the meaning of the present invention, reference is made to explicitly designated numerical values ​​in a range from X to Y, or from at least X to at least Y, or from greater than X to greater than Y, etc., this includes, in particular, all implicitly intervening values ​​suggested by the indication of the zeros. Thus, if a value lies between 1 and 10, this includes, in particular, 2, 3, 4, 5, 6, 7, 8, and 9. If a value lies between 1.0 and 2.0, this includes, in particular, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, and 1.9. If a value lies between 1.00 and 1.10, this includes, in particular, 1.01, 1.02, 1.03,

[0101] I ,04, 1 ,05, 1 ,06, 1 ,07, 1 ,08 and 1 ,09 are included.

[0102] II. Procedure

[0103] The inventive method for producing capillaries or antiresonance element preforms preferably works for mechanically provided fused silica hollow cylinders characterized by relatively large dimensions. The method particularly comprises the following steps: i) Providing a fused silica hollow cylinder with a large outer diameter Z a , a small inner diameter Zi; ii) Continuous feeding of the quartz glass hollow cylinder into a heating zone until the quartz glass hollow cylinder is softened in certain areas; iii) Inverse collapse and simultaneous elongation of the quartz glass hollow cylinder from the softened area to form a capillary strand with an outer diameter C a and to obtain an inner diameter Cj, characterized in that the outer and inner diameter ratio of the cylinder changes during inverse collapse and is equal- 2023PF00181

[0104] 13. The elongation to the capillary changes in such a way that: 1.2 to 6.0 applies. preferably 2.9 to 4.2; iv) Cutting the capillary strand to the desired length while obtaining capillaries with an outer diameter C a and an inner diameter Ci, for which the following applies:

[0105] 1.05 to 1.5, preferably 1.08 to 1.30.

[0106] The procedure also includes, in particular, the following alternative steps: i) Providing a hollow quartz glass cylinder with a large outer diameter Z a , a small inner diameter Zi; ii) Continuous feeding of the quartz glass hollow cylinder into a heating zone until the quartz glass hollow cylinder is softened in certain areas; iii) Inverse collapse and simultaneous elongation of the quartz glass hollow cylinder from the softened area to form a capillary strand with an outer diameter C aand to obtain an inner diameter Ci, characterized in that the outer and inner diameter ratio of the cylinder changes during inverse collapse and simultaneous elongation to the capillary such that: 1.2 to 6.0, preferably 2.9 to 4.2; iv) Cutting the capillary strand to the desired length while obtaining capillaries with an outer diameter C a and an inner diameter Ci, for which the following applies: v) 1.00 to 1.30, preferably 1.02 to 1.30, further preferably 1.05 to 1.28, even more preferably 1.05 to 1.25.

[0107] It is not necessary to first thermally stretch the quartz glass hollow cylinder and process it further in a separate step, as is usually done in the prior art, thus performing a stepwise processing into capillaries. Instead, according to the invention, the mechanically produced cylinder can be processed directly and without an intermediate step. 2023PF00181

[0108] 14. By continuously heating, pushing and pulling out, to pull out the capillary strand.

[0109] The inventors of the present invention have surprisingly discovered that direct processing of a hollow quartz glass cylinder into a capillary strand is possible for a specific dimensional range of both the cylinder and the capillary strand, without additional thermal treatment steps. This means that the inventive method is preferably carried out with hollow quartz glass cylinders having specific outer and inner diameters and results in capillary strands, or, after cutting to the desired length, in capillaries that also have specific outer and inner diameters.According to the invention, the ratio between the outer and inner diameter of the hollow quartz glass cylinder, in relation to the ratio between the outer and inner diameter of the capillary strand, lies between 1.2 and 6.0, for example between 1.2 and 6.0, or between 1.5 and 5.5, or between 1.8 and 5.0, or between 2.0 and 4.8, or between 2.5 and 4.5, or between 2.0 and 4.2, preferably between 2.9 and 4.2. Therefore, the ratio is 1.2 to 6.

[0110] The capillaries or capillary strands according to the invention, which can be obtained with the method according to the invention, are characterized in a first embodiment by a ratio of the outer and inner diameter in which the outer diameter is 1.05 to 1.5 times larger than the inner diameter, i.e. it is greater than 1.05, 1.10, 1.15, 1.20, 1.25, or up to 1.30, 1.35, 1.40, 1.45 or up to 1.50, so that finally the following applies:

[0111] 1.05 to 1.5.

[0112] Finally, a value between 1.08 and 1.30 is preferred for the outer and inner diameter ratio of the capillaries or capillary strands.

[0113] In a second embodiment, the capillaries or capillary strands according to the invention, which can be obtained with the method according to the invention, are characterized by a ratio of the outer and inner diameter in which the outer diameter is 1.05 to 1.5 times larger than the inner diameter, i.e., it is greater than 1.05, 1.10, 1.15, 1.20, 1.25 and up to 1.30, so that finally: 1.0 to 1.3. 2023PF00181

[0114] 15

[0115] Preferably, the ratio of the outer to the inner diameter of the capillaries or capillary strands is between 1.02 and 1.30, more preferably 1.5 and 1.28, and even more preferably 1.07 and 1.25.

[0116] In accordance with the invention, these dimensions are preferably achieved using mechanically manufactured hollow quartz glass cylinders that have relatively large outer and inner diameters compared to semi-finished products typically used in the prior art.

[0117] The outer diameter Z a The outer diameter of quartz glass hollow cylinders, which are particularly well suited for the method according to the invention, is between 120 mm and 250 mm, i.e., for example, greater than 120 mm, 125 mm, 130 mm, 135 mm, 140 mm, 145 mm or greater than 150 mm, 155 mm, 160 mm, 165 mm, 170 mm, 175 mm or greater than 180 mm, 185 mm, 190 mm, 195 mm, 200 mm or up to 205 mm, 210 mm, 215 mm, 220 mm, 225 mm or up to 230 mm, 235 mm, 240 mm, 245 mm or up to 250 mm, preferably the outer diameter is between 150 and 200 mm.

[0118] The inner diameter Zj of quartz glass hollow cylinders, which are particularly well suited for the method according to the invention, is between 20 mm and 140 mm, i.e. e.g. greater than 20 mm, 25 mm, 30 mm, 35 mm, 40 mm, 45 mm or greater than 50 mm, 55 mm, 60 mm, 65 mm, 70 mm, 75 mm, 80 mm, 85 mm, 90 mm or up to 95 mm, 100 mm, 105 mm, 110 mm, 115 mm, 120 mm or up to 125 mm, 130 mm, 135 mm, or 140 mm, preferably the outer diameter is between 35 and 90 mm.

[0119] According to the invention, the inner and outer diameters of the hollow quartz glass cylinders are selected such that the ratio between the outer diameter and the inner diameter is between 1.8 and 5.0, i.e., for example, greater than 1.8, 1.9, 2.0 or greater than 2.1, 2.2, 2.3, 2.4 or greater than 2.5, 2.6, 2.7, 2.8, 2.9 or up to 3.0, 3.1, 3.2, 3.3, 3.4 or up to 3.5, 3.6, 3.7, 3.8, 3.9 or up to 4.0, 4.1, 4.2, 4.3, 4.4 or up to 4.5, 4.6, 4.7, 4.8, 4.9 or up to 5.0, which is the case where:

[0120] 1.8 to 5.0.

[0121] Preferably, the ratio between the outer diameter and inner diameter of the quartz glass hollow cylinders processed into capillaries using the inventive method is between 1.8 and 3.0.

[0122] The method according to the invention enables the previously exclusively mechanically treated hollow quartz glass cylinder with the described dimensions to be formed into capillary strands, respectively. 2023PF00181

[0123] 16. After cutting to the target length, the material is further processed into capillaries, which also have characteristic dimensions.

[0124] The outer diameter C a The diameters of capillaries, which can be obtained particularly by the method according to the invention, are between 2.0 mm and 20.0 mm, i.e., for example, greater than 2.0 mm, 2.5 mm, 3.0 mm, 3.5 mm, 4.0 mm, 4.5 mm or greater than 5.0 mm, 5.5 mm, 6.0 mm, 6.5 mm, 7.0 mm or greater than 7.5 mm, 8.0 mm, 8.5 mm, 9.0 mm, 9.5 mm or greater than 10.0 mm, 10.5 mm, 11.0 mm, 11.5 mm, 12.0 mm or greater than 12.5 mm, 13.0 mm, 13.5 mm, 14.0 mm, 14.5 mm or greater than 15.0 mm, 15.5 mm, 16.0 mm.

[0125] 16.5 mm or up to 17.0 mm, 17.5 mm, 18.0 mm, 18.5 mm, 19.0 mm, 19.5 mm or up to 20.0 mm, preferably between 2.5 and 17.0 mm.

[0126] The inner diameter Ci of capillaries, which can be obtained particularly by the method according to the invention, in a first embodiment lies between 1.0 mm and 17.0 mm, i.e., for example, greater than 1.0 mm, 1.5 mm, 2.0 mm or greater than 2.5 mm, 3.0 mm, 3.5 mm, 4.0 mm, 4.5 mm or greater than 5.0 mm, 5.5 mm, 6.0 mm, 6.5 mm, 7.0 mm or greater than 7.5 mm, 8.0 mm, 8.5 mm, 9.0 mm, 9.5 mm or greater than 10.0 mm.

[0127] 10.5 mm, 11.0 mm, 11.5 mm, 12.0 mm or, for dimensions greater than 12.5 mm, 13.0 mm, 13.5 mm, 14.0 mm, 14.5 mm, 15.0 mm or, for dimensions up to 15.5 mm, 16.0 mm, 16.5 mm or, for dimensions up to 17.0 mm, preferably between 1.0 mm and 15.5 mm.

[0128] In a second embodiment, the inner diameter Ci of capillaries, which can be obtained particularly by the method according to the invention, is preferably 1 mm to 20 mm, more preferably 1 mm to 19 mm, more preferably 1.50 mm to 18 mm, more preferably 1.50 mm to 17 mm, and even more preferably 2 mm to 16.50 mm.

[0129] The inventors of the present invention have surprisingly discovered that undesirable collapse behavior of capillaries is less related to their outer diameter and more strongly to their inner diameter. In particular, it has been shown that capillary strands and / or capillaries with an inner diameter of less than 20 mm tend to collapse undesirably, such that the OD / ID ratio increases when they are to be further tapered. If the ratio of outer to inner diameters is to remain constant or be reduced in such systems, an internal blowing pressure must be applied that is at least equal to the equilibrium pressure of the capillary strand.

[0130] The inventors of the inventive method have thus surprisingly succeeded in providing a process that can produce a wide range of differently dimensioned capillaries from hollow quartz glass cylinders. It is not necessary to perform an intermediate step involving thermal treatment of the hollow quartz glass cylinder; instead, the mechanically produced cylinder is directly processed into capillaries. Inventory 2023PF00181

[0131] 17 of them were surprisingly able to find that this simplification compared to the state of the art is possible when semi-finished products with the dimensions described above are processed.

[0132] In accordance with the inventive method, a hollow quartz glass cylinder is fed to a heating zone at a certain speed, the tracking rate, and is collapsed, elongated, or pulled out at a certain speed, the drawing speed.

[0133] According to the invention, the tracking rate and the drawing speed are related to the dimensions of the quartz glass hollow cylinder and the target dimensions of the capillary strand.

[0134] In accordance with the invention, the drawing speed of the quartz glass hollow cylinder to the capillary strand is between 1.0 m / min and 6.0 m / min, i.e., for example, at speeds greater than 1.0 m / min, 1.1 m / min, 1.2 m / min, 1.3 m / min, 1.4 m / min or at speeds greater than 1.5 m / min, 1.6 m / min, 1.7 m / min, 1.8 m / min, 1.9 m / min or at speeds greater than 2.0 m / min, 2.1 m / min, 2.2 m / min, 2.3 m / min.

[0135] 2.4 m / min or at greater than 2.5 m / min, 2.6 m / min, 2.7 m / min, 2.8 m / min, 2.9 m / min or at up to 3.0 m / min, 3.1 m / min, 3.2 m / min, 3.3 m / min, 3.4 m / min or at up to 3.5 m / min, 3.6 m / min, 3.7 m / min, 3.8 m / min, 3.9 m / min or at up to 4.0 m / min, 4.1 m / min, 4.2 m / min, 4.3 m / min, 4.4 m / min or at up to 4.5 m / min, 4.6 m / min, 4.7 m / min, 4.8 m / min, 4.9 m / min or at up to 5.0 m / min, 5.1 m / min, 5.2 m / min, 5.3 m / min, 5.4 m / min or up to 5.5 m / min, 5.6 m / min, 5.7 m / min, 5.8 m / min, 5.9 m / min or up to 6.0 m / min.

[0136] In this process, hollow quartz glass cylinder material is continuously fed into the heating zone, making the method according to the invention industrially applicable. The feed rate at which the hollow quartz glass cylinder is fed into the heating zone is, according to the invention, 1.1 mm / min up to...

[0137] 1.5 mm / min, for example, at greater than 1.1 mm / min, 1.2 mm / min, 1.3 mm / min or up to 1.4 mm / min or up to 1.5 mm / min.

[0138] The method according to the invention thus makes it possible to feed the quartz glass hollow cylinder with the dimensions preferred according to the invention to a heating zone at a certain speed and then to withdraw a capillary strand of constant high quality with constant target dimensions from softened cylinder material at a relatively high speed.

[0139] In accordance with the present invention, when drawing the quartz glass hollow cylinder into a capillary strand, 3.5 kg / h to 6.0 kg / h of the cylinder material is consumed, meaning that, for example, at consumption rates greater than 3.5 kg / h, 3.6 kg / h, 3.7 kg / h, 3.8 kg / h, 3.9 kg / h or greater than 4.0 kg / h, 4.1 kg / h, 4.2 kg / h, 4.3 kg / h, 4.4 kg / h or greater than 4.5 kg / h, 4.6 kg / h, 4.7 kg / h, 4.8 kg / h, 4.9 kg / h or greater than 5.0 kg / h, 5.1 kg / h, 5.2 kg / h or up to 5.3 kg / h, the material is consumed. 2023PF00181

[0140] 18 kg / h, 5.4 kg / h or up to 5.5 kg / h, 5.6 kg / h, 5.7 kg / h, 5.8 kg / h, 5.9 kg / h or up to 6.0 kg / h of the cylinder material is drawn into a capillary strand, preferably 3.9 to 5.3 kg / h of the quartz glass hollow cylinder is drawn into a capillary strand.

[0141] Furthermore, the inventive method enables the production of quartz glass hollow cylinders with a cross-sectional area of ​​10000 mm². 2 up to 31000 mm 2 to further process into capillaries or capillary strands with a cross-sectional area of ​​2 mm 2 up to 40 mm 2 exhibit.

[0142] This means that hollow quartz glass cylinders with a cross-sectional area greater than 10000 mm² can be used. 2 , 11000 mm 2 , 12000 mm 2 , 13000 mm 2 , 14000 mm 2 or greater than 15000 mm 2 , 16000 mm 2 , 17000 mm 2 , 18000 mm 2 , 19000 mm 2 or greater than 20000 mm 2 , 21000 mm 2, 22000 mm 2 , 23000 mm 2 or up to 24000 mm 2 , 25000 mm 2 , 26000 mm 2 , 27000 mm 2 , 28000 mm 2 , 29000 mm 2 , 30000 mm 2 or up to 31000 mm 2 are processed using the inventive method, wherein capillaries or capillary strands have a cross-sectional area greater than 2 mm 2 , 3 mm 2 , 4 mm 2 or larger than 5 mm 2 , 6 mm 2 , 7 mm 2 , 8 mm 2 , 9 mm 2 or larger than 10 mm 2 , 11 mm 2 , 12 mm 2 , 13 mm 2 , 14 mm 2 or larger than 15 mm 2 , 16 mm 2 , 17 mm 2 , 18 mm 2 , 19 mm 2 or larger than 20 mm 2 , 21 mm 2 , 22 mm 2 , 23 mm 2 , 24 mm 2 or larger than 25 mm 2 , 26 mm 2 , 27 mm2 , 28 mm 2 , 29 mm 2 or up to 30 mm 2 , 31 mm 2 , 32 mm 2 , 33 mm 2 , 34 mm 2 or up to 35 mm 2 , 36 mm 2 , 37 mm 2 , 38 mm 2 , 39 mm 2 or up to 40 mm 2 will be obtained.

[0143] A major advantage of the inventive method is that large quantities of capillaries can be produced from a relatively small proportion of the comparatively large hollow quartz glass cylinders. The particularly large hollow quartz glass cylinders, compared to the prior art, enable a high capillary yield, resulting in consistently high-quality capillaries. This is due, in part, to the fact that the size of the semi-finished product leads to more constant pressure conditions during the process. When capillaries are cut to the desired length, only a small percentage of the potentially pressurized system is lost, since both the semi-finished product itself and the section over which it is drawn are significantly longer than the desired length of the capillaries. For example, the pressure in a 5 m long system fluctuates by 20% when a 1 m long capillary section is cut off.However, in a 10 m long system, the pressure fluctuates by only 10% when a 1 m long capillary section is cut. Thanks to the particularly long semi-finished products and draw-out sections according to the invention, production is more stable, and the quality of the capillaries does not fluctuate due to pressure variations during drawing. Furthermore, vibrations that may occur when cutting the capillary to the desired length are not transmitted over the length of the system. This prevents damage to the material to be drawn further.

[0144] The method according to the invention provides an industrially attractive throughput rate and thus 2023PF00181

[0145] 19. The relatively high drawing speeds described above are required. The capillary strand, which is drawn off at such speeds, is preferably drawn off along a relatively long drawing section using the method according to the invention. According to the invention, the drawing section, which lies behind the heating zone, has a length between 1.0 m and 8.0 m, i.e., for example, longer than 1.0 m, 2.0 m, 3.0 m, or longer than 4.0 m, 5.0 m, or up to 6.0 m, up to 7.0 m, or up to 8.0 m. A drawing section of 1.5 m to 6.0 m is preferred.

[0146] In accordance with the invention, it is preferred if the capillary strand is stabilized against mechanical vibrations or other potentially damaging influences during the extension process. Therefore, in accordance with the invention, it is preferred if the capillary strand is mechanically stabilized. This can be achieved, for example, by means of additional wheels over which the extended capillary strand is guided in a horizontal or vertical position during the extension process.

[0147] A particularly preferred step according to the invention is to change the outer and inner diameter ratio between the quartz glass hollow cylinder and the capillary during the process according to the invention. In conventional methods known in the prior art, the ratio of the outer diameter to the inner diameter does not change, or does not change significantly, when a glass cylinder is processed into a capillary. The method according to the invention provides that the ratio of the inner and outer diameters changes during the processing of the quartz glass hollow cylinder. In principle, it is possible to influence the internal pressure conditions within the hollow cylinder and the capillary strand to achieve inverse collapse during elongation or drawing out.

[0148] It is therefore possible, for example, in accordance with the invention, to apply an internal blowing pressure p during the application of the method according to the invention. +to be applied to the hollow quartz glass cylinder. This counteracts the collapse pressure of the capillary strand and stabilizes a desirable, round geometry of the capillary strand, and thus also of the capillaries cut from it to the desired length. Collapse pressure describes the tendency of the capillary strand to collapse uncontrollably in on itself when guided through the heating zone according to the invention and thus elongated. For example, according to the invention, it is possible to melt the end face of the elongated capillary strand or seal it with a suitable material and then apply pressure using a suitable gas. On the other hand, a desired geometry of the capillaries can also be achieved by means of the applied pressure, for example by expanding the antiresonance element preforms from the inside with the applied pressure, preferably to stabilize a round geometry.Furthermore, according to the invention, the ratio between the outer and inner diameters can be changed by controlling the pressure conditions. 2023PF00181.

[0149] 20

[0150] Is a blowing pressure p + When applied, its value lies between the equilibrium pressure of the hollow quartz glass cylinder p z and the equilibrium pressure of the capillary strand p c The equilibrium pressure, referred to here generally as PEQ, is illustrated by the following relationship: where TA denotes the outer radius of the tubular element, n the inner radius of the tubular element and r| the surface tension of the tubular element.

[0151] If, in accordance with the inventive method, a blowing pressure p +If the process is to be carried out, this is preferably done using a suitable gas or gas mixture, which is guided inside the hollow quartz glass cylinder. Such gases or gas mixtures include, for example, dry air, nitrogen, argon and / or helium, with dry air being preferred.

[0152] Overpressure can be particularly advantageous when small inner diameters of less than 20 mm are desired in the capillaries according to the invention. As already mentioned, the inventors of the method were able to determine that the collapse pressure of the capillaries depends primarily on the inner diameter. For larger inner diameters above 30 mm, a ratio pull, i.e., an elongation, can easily be achieved in which the ratio between the outer and inner diameters of the quartz glass hollow cylinder and the capillary strand remains approximately constant. Smaller inner diameters, on the other hand, can be stabilized by the overpressure.

[0153] Once a capillary strand of the desired dimensions has been drawn from a hollow quartz glass cylinder by carrying out these optionally preferred process steps according to the inventive method, it is cut into capillaries of a target length. According to the invention, the cutting can be carried out in any conceivable way that results in a cut surface having the desired or required surface properties for the capillary. This includes, in particular, cutting, sawing, snapping, and combinations thereof, such as circumferential sawing followed by snapping.

[0154] The method according to the invention thus makes it possible to produce capillaries of consistent quality from large, mechanically machined hollow quartz glass cylinders on a continuous and industrially attractive scale. The method is characterized by a range of ratios between the outer and inner diameters of the hollow quartz glass cylinder and the capillaries. This ratio can be adjusted according to the invention by applying 2023PF00181

[0155] 21. The pressure of a blowing or vacuum can be varied more extensively than is usual in the prior art. Because it is carried out continuously with large semi-finished products, the method according to the invention produces only a few wt.% of the quartz glass hollow cylinder as rejects before an equilibrium is reached at which a capillary strand with continuous dimensions can be drawn off.

[0156] A particularly preferred variant of the method according to the invention comprises the following steps: i) Providing a hollow quartz glass cylinder with an outer diameter Z a , from 120 mm to 250 mm and an inner diameter Zj from 20 mm to 140 mm; ii) Continuous feeding of the quartz glass hollow cylinder into a heating zone at a feed rate of 0.3 mm / min to 3 mm / min until the quartz glass hollow cylinder is softened in certain areas; iii) Inverse collapse and simultaneous elongation of the quartz glass hollow cylinder from the softened area at a drawing speed of 1 m / min to 6 m / min while an internal blowing pressure p + is created to form a capillary strand with an outer diameter C aand to obtain an inner diameter Cj, characterized in that the outer and inner diameter ratio of the cylinder changes during inverse collapse and simultaneous elongation to the capillary such that: 2.9 to 4.2; iv) Cutting the capillary strand to the desired length while obtaining capillaries with an outer diameter Ca and an inner diameter Ci, for which the following applies:

[0157] 1.05 to 1.5.

[0158] Another particularly preferred variant of the method according to the invention comprises the following steps: i) Providing a hollow quartz glass cylinder with an outer diameter Z a, from 120 mm to 250 mm and an inner diameter Zj from 20 mm to 140 mm; ii) Continuous feeding of the quartz glass hollow cylinder into a heating zone at a feed rate of 0.3 mm / min to 3 mm / min until the quartz glass hollow cylinder is softened in certain areas; iii) Inverse collapse and simultaneous elongation of the quartz glass hollow cylinder from the softened area at a drawing speed of 1 m / min to 6 m / min while an internal blowing pressure p + is created to form a capillary strand with an outer 2023PF00181

[0159] 22 diameter C a and to obtain an inner diameter C>, characterized in that the outer and inner diameter ratio of the cylinder changes during inverse collapse and simultaneous elongation to the capillary such that: 2.9 to 4.2; iv) Cutting the capillary strand to the desired length while retaining capillaries with an outer diameter C aand an inner diameter Ci, for which the following applies: 1.00 to 1.3.

[0160] Another particularly preferred variant of the method according to the invention comprises the following steps: i) Providing a hollow quartz glass cylinder with an outer diameter Z a , from 120 mm to 250 mm and an inner diameter Zj from 20 mm to 140 mm; ii) Continuous feeding of the quartz glass hollow cylinder into a heating zone at a feed rate of 0.3 mm / min to 3 mm / min until the quartz glass hollow cylinder is softened in certain areas; iii) Inverse collapse and simultaneous elongation of the quartz glass hollow cylinder from the softened area at a drawing speed of 1 m / min to 6 m / min while an internal blowing pressure p + is created to form a capillary strand with an outer diameter C aand to obtain an inner diameter C>, characterized in that the outer and inner diameter ratio of the cylinder changes during inverse collapse and simultaneous elongation to the capillary such that: 2.9 to 4.2; iv) Cutting the capillary strand to the desired length while retaining capillaries with an outer diameter C a and an inner diameter Ci, for which the following applies:

[0161] 1.02 to 1.3.

[0162] Another particularly preferred variant of the method according to the invention comprises the following steps: i) Providing a hollow quartz glass cylinder with an outer diameter Z a , of 120 2023PF00181

[0163] 23 mm to 250 mm and an inner diameter Zj of 20 mm to 140 mm; ii) Continuous feeding of the quartz glass hollow cylinder into a heating zone at a feed rate of 0.3 mm / min to 3 mm / min until the quartz glass hollow cylinder is softened in certain areas; iii) Inverse collapse and simultaneous elongation of the quartz glass hollow cylinder from the softened area at a drawing speed of 1 m / min to 6 m / min while an internal blowing pressure p + is created to form a capillary strand with an outer diameter C a and to obtain an inner diameter Cj, characterized in that the outer and inner diameter ratio of the cylinder changes during inverse collapse and simultaneous elongation to the capillary such that: 2.9 to 4.2; iv) Cutting the capillary strand to the desired length while obtaining capillaries with an outer diameter Ca and an inner diameter Ci, for which the following applies:

[0164] 1.05 to 1.28.

[0165] Another particularly preferred variant of the method according to the invention comprises the following steps: i) Providing a hollow quartz glass cylinder with an outer diameter Z a , from 120 mm to 250 mm and an inner diameter Zj from 20 mm to 140 mm; ii) Continuous feeding of the quartz glass hollow cylinder into a heating zone at a feed rate of 0.3 mm / min to 3 mm / min until the quartz glass hollow cylinder is softened in certain areas; iii) Inverse collapse and simultaneous elongation of the quartz glass hollow cylinder from the softened area at a drawing speed of 1 m / min to 6 m / min while an internal blowing pressure p + is created to form a capillary strand with an outer diameter C aand to obtain an inner diameter C>, characterized in that the outer and inner diameter ratio of the cylinder changes during inverse collapse and simultaneous elongation to the capillary such that:

[0166] 2.9 to 4.2; iv) Cutting the capillary strand to the desired length while retaining capillaries with an outer diameter C a and an inner diameter Ci, for which the following applies: 2023PF00181

[0167] 24

[0168] 1.07 to 1.25.

[0169] III. Products

[0170] The present invention further relates to capillaries, which can be produced, for example, using the method according to the invention. For the purposes of the invention, the capillaries can be characterized by the ratio of their outer diameter to their inner diameter:

[0171] 1.05 to 1.5,

[0172] In accordance with the invention, these capillaries continue to exhibit an equilibrium pressure p con, which lies between 50 Pa and 800 Pa, for example, greater than 50 Pa, 51 Pa, 52 Pa, 53 Pa, 54 Pa or greater than 55 Pa, 56 Pa, 57 Pa, 58 Pa, 59 Pa or greater than 60 Pa, 61 Pa, 62 Pa, 63 Pa, 64 Pa or greater than 65 Pa, 66 Pa, 67 Pa, 68 Pa, 69 Pa or greater than 70 Pa, 71 Pa, 72 Pa, 73 Pa, 74 Pa or greater than 75 Pa, 76 Pa, 77 Pa, 78 Pa, 79 Pa or greater than 80 Pa, 81 Pa, 82 Pa, 83 Pa, 84 Pa or greater than 85 Pa, 86 Pa, 87 Pa, 88 Pa, 89 Pa or greater than 90 Pa, 91 Pa, 92 Pa, 93 Pa, 94 Pa or greater than 95 Pa, 96 Pa, 97 Pa, 98 Pa, 99 Pa or up to 100 Pa, 110 Pa, 120 Pa, 130 Pa, 140 Pa or up to 150 Pa, 160 Pa, 170 Pa, 180 Pa, 190 Pa or up to 200 Pa, 210 Pa, 220 Pa, 230 Pa, 240 Pa or up to 250 Pa, 260 Pa, 270 Pa, 280 Pa, 290 Pa or up to 300 Pa, 310 Pa, 320 Pa, 330 Pa, 340 Pa or up to 350 Pa, 360 Pa, 370 Pa, 380 Pa, 390 Pa or up to 400 Pa, 410 Pa, 420 Pa, 430 Pa,440 Pa or up to 450 Pa, 460 Pa, 470 Pa, 480 Pa, 490 Pa or up to 500 Pa, 510 Pa, 520 Pa, 530 Pa, 540 Pa or up to 550 Pa, 560 Pa, 570 Pa, 580 Pa, 590 Pa or up to 600 Pa, 610 Pa, 620 Pa, 630 Pa, 640 Pa or up to 650 Pa, 660 Pa, 670 Pa, 680 Pa, 690 Pa or up to 700 Pa, 710 Pa, 720 Pa, 730 Pa, 740 Pa or up to 750 Pa, 760 Pa, 770 Pa, 780 Pa, 790 Pa or up to 800 Pa.,

[0173] The products according to the invention are typically used in the range between 1800 °C and 2200 °C, i.e., at temperatures greater than 1800 °C, 1810 °C, 1820 °C, 1830 °C, 1840 °C or greater than 1850 °C, 1860 °C, 1870 °C, 1880 °C, 1890 °C or greater than 1900 °C, 1910 °C, 1920 °C, 1930 °C, 1940 °C or greater than 1950 °C, 1960 °C, 1970 °C, 1980 °C, 1990 °C or up to 2000 °C, 2010 °C, 2020 °C, 2030 °C, 2040 °C or up to Drawn from semi-finished products at temperatures of 2050 °C, 2060 °C, 2070 °C, 2080 °C, 2090 °C or up to 2100 °C, 2110 °C, 2120 °C, 2130 °C, 2140 °C or up to 2150 °C, 2160 °C, 2170 °C, 2180 °C, 2190 °C or up to 2200 °C, preferably between 1950 °C and 2100 °C.

[0174] The equilibrium pressure of the capillary p c This results from the relationship 2023PF00181

[0175] 25 in which r Ac the outer radius of the capillary, n c the inner radius of the capillary and r| cThe surface tension of the capillary is described. According to the invention, capillaries exhibit characteristic equilibrium pressures, since their dimensions with respect to the outer and inner diameters, and thus also the corresponding radii, depend on the hollow cylinders being processed, as the dimensional relationship between the semi-finished product and the finished product is of great importance for the applicability of the process according to the invention.

[0176] Capillaries produced using the inventive method are characterized by very low ovality, and are therefore at least almost circular, since the inventive method provides excellent control over the geometry, which is due on the one hand to the large-dimensioned semi-finished products (quartz glass hollow cylinders) and on the other hand to the possibility of pressure control.

[0177] In principle, mechanically manufactured hollow quartz glass cylinders are initially circular before processing. However, during elongation and collapse, or inverse collapse, through the heating zone, where capillaries are formed, the circular cross-section can assume an oval shape, characterized by a long axis and a short axis. The mean outer diameter of such a more oval capillary is then calculated according to the following formula:

[0178] The following applies to the ratio between the long and short axes, i.e., the question of whether the cross-section is round or rather oval:

[0179] Values ​​closer to 1 are characteristic of round geometries, while larger values ​​indicate greater deformations. Capillaries produced using the inventive method are characterized by achieving particularly round geometries; the axis ratio lies between 1.00 and 1.02, i.e., greater than or equal to 1.00 up to 1.02.

[0180] According to the invention, the ratio between the axis sizes can be determined, for example, by examining the cross-sectional area of ​​the capillaries with an optical microscope and evaluating the images using suitable software. Electro-optical distance measurements with suitable laser devices are also conceivable. 2023PF00181

[0181] 26

[0182] The capillaries according to the invention are therefore characterized by at least one of the dimensional parameters that are customary for production using the inventive method. Particularly preferred capillaries according to the invention are characterized by an outer diameter C. a and an inner diameter Ci for which the following applies:

[0183] 1.05 to 1.5, A diameter ratio between 1.08 and 1.30 is preferred, and an equilibrium pressure p c , which lies between 50 Pa and 800 Pa and has a particularly round geometry, characterized by a ratio of the axes examined in the cross-section of 1.00 to 1.02.

[0184] The capillaries according to the invention are further characterized by at least one of the dimensional parameters that are customary for production using the inventive method. Particularly preferred capillaries according to the invention are characterized by an outer diameter C. aand an inner diameter Ci, for which the following applies: 1.00 to 1.3, Preferably a diameter ratio between 1.02 and 1.30, more preferably 1.05 and 1.28, and even more preferably 1.05 and 1.25, and an equilibrium pressure p c , which lies between 50 Pa and 800 Pa, and a particularly round geometry, characterized by a ratio of the axes examined in the cross-section of 1.00 to 1.02.

[0185] The drawing process according to the invention could have the disadvantage, due to the small target geometry, that the throughput (mass per time) is relatively small, so that the person skilled in the art would not consider such a process.

[0186] However, within the scope of the present invention, as described above, this disadvantage due to the stable drawing process has been compensated for by increasing the throughput.

[0187] The advantage of the process according to the invention is therefore a high dimensional stability and yield, as already explained above:

[0188] Process stability through high taper ratio: Due to the higher taper ratio, the capillaries can be drawn off more quickly from a large semi-finished product (cylinder) used according to the invention, which increases process stability. 2023PF00181

[0189] Process stability through larger semi-finished product mass or long process runtime: According to the invention, a long process runtime in thermal equilibrium is achieved after a short start-up phase.

[0190] Geometric accuracy through mechanically machined semi-finished products and drawing in one step: In the drawing process according to the invention, which involves several steps (cylinder to tube to capillary), errors from the process steps can accumulate. The mechanically machined cylinder is more precise than the drawn tube.

[0191] EXAMPLES

[0192] I. Proportional pull and inverse collapse

[0193] The study investigated at which capillary dimensions the application of internal pressure was necessary to ensure a round geometry of the capillary strand or capillaries.

[0194] Table 1. Outer diameter (OD), inner diameter (ID), outer and inner diameter ratio (OD / ID) and equilibrium pressures (PEQ) at temperatures from approx. 1800 °C to approx. 2200 °C for various quartz glass hollow cylinders.

[0195] Table 2. Outer and inner diameters and corresponding equilibrium pressures at temperatures from approximately 1800 °C to approximately 2200 °C for various capillary systems. 2023PF00181

[0196] 28

[0197] The inventors of the present invention have observed that equilibrium pressures increase abruptly at inner diameters less than 20 mm. To maintain the proportional tension or to induce inverse collapse of the capillaries, it is necessary to apply internal pressure (see Figure 1).

[0198] II. Capillary yield of the inventive method It was further investigated what capillary yield can be achieved with the large quartz glass hollow cylinders according to the inventive method. For this purpose, capillaries of different dimensions were produced from a defined quartz glass hollow cylinder.

[0199] Table 3. Overview of the capillary yield of 1 m of a quartz glass hollow cylinder with an outer diameter of 200.00 mm and an inner diameter of 70.00 mm for three different capillary dimensions. 2023PF00181

[0200] 29

[0201] In addition to increased process stability, a large quantity of capillary material can also be produced by using large quartz glass hollow cylinders according to the invention.

[0202] DESCRIPTION OF THE FIGURES

[0203] FIGURE 1 Relationship between the equilibrium pressure at operating temperature and the inner diameter of the capillary strand(s). The figure shows a sharp increase in equilibrium pressure for inner diameters below approximately 20 mm, but an almost constant pressure behavior at higher values.

[0204] FIGURE 2 Schematic representation of the processes a) collapse, b) ratio pull, and c) inverse collapse. The illustrations demonstrate how the ratio between outer and inner diameters can change due to these processes.

Claims

1. 2023PF00181 30 REQUIREMENTS 1. Method for manufacturing capillaries or antiresonance element preforms, comprising the steps of: i) providing a hollow quartz glass cylinder with a large outer diameter Z a , a small inner diameter Zi; ii) Continuous feeding of the quartz glass hollow cylinder into a heating zone until the quartz glass hollow cylinder is softened in certain areas; iii) Inverse collapse and simultaneous elongation of the quartz glass hollow cylinder from the softened area to form a capillary strand with an outer diameter C a and to obtain an inner diameter Cj, characterized in that the outer and inner diameter ratio of the cylinder changes during inverse collapse and simultaneous elongation to the capillary such that: 1.2 to 6.0 preferably 2.9 to 4.2; iv) Cutting the capillary strand to the desired length while obtaining capillaries with an outer diameter C a and an inner diameter Cj, for which the following applies: 1.50 preferably 1.05 to 1.28, even more preferably 1.07 to 1.

25.

2. Method according to claim 1, characterized in that the quartz glass hollow cylinder is a mechanically machined quartz glass hollow cylinder.

3. Method according to claims 1 to 2, characterized in that the quartz glass hollow cylinder was not thermally pretreated.

4. Method according to claims 1 to 3, characterized in that the quartz glass hollow cylinder has a large outer diameter of 120 mm to 250 mm, preferably an outer diameter of 150 mm to 200 mm.

5. Method according to claims 1 to 4, characterized in that the quartz glass hollow cylinder has a small inner diameter of 20 mm to 140 mm, preferably an inner diameter of 35 mm to 90 mm. 2023PF00181 31 6. Method according to claims 1 to 5, characterized in that the following applies to the ratio of the outer and inner diameter of the mechanically machined hollow quartz glass cylinder: 7 1.8 to 5.0, Zi Preferably, the quartz glass hollow cylinder has a ratio of outer to inner diameter of 1.8 to 3.

0.

7. Method according to claims 1 to 6, characterized in that the drawing speed of the capillary strand during the drawing process is 1 m / min to 6 m / min.

8. Method according to claims 1 to 7, characterized in that the tracking rate of the quartz glass hollow cylinder is 0.3 mm / min to 3 mm / min, preferably 1.1 mm / min to 1.5 mm / min.

9. Method according to claims 1 to 8, characterized in that during the drawing process of the capillary strand from the softened quartz glass hollow cylinder a blowing pressure p is applied + is generated in the inner bore of the quartz glass hollow cylinder or the resulting capillary strand.

10. Method according to claims 1 to 9, characterized in that the blowing pressure is generated with a gas or gas mixture comprising dry air, nitrogen, argon and / or helium, preferably with dry air.

11. Method according to claims 1 to 10, characterized in that the blowing pressure lies between the equilibrium pressure of the quartz glass hollow cylinder pz and the equilibrium pressure of the capillary strand pc.

12. Method according to claims 1 to 11, characterized in that the heating zone has temperatures of 1800 °C to 2200 °C, preferably temperatures of 1950 °C to 2100 °C.

13. A method according to claims 1 to 12, comprising the following steps: i) providing a hollow quartz glass cylinder with an outer diameter Z a , from 120 mm to 250 mm and an inner diameter Zj from 20 mm to 140 mm; ii) Continuous feeding of the quartz glass hollow cylinder at a feed rate of 0.3 mm / min to 3 mm / min into a heating zone until the quartz glass hollow cylinder is inside 2023PF00181 32. is softened in certain areas; iii) Inverse collapse and simultaneous elongation of the quartz glass hollow cylinder from the softened area at a drawing speed of 1 m / min to 6 m / min while an internal blowing pressure p is applied. + is created to form a capillary strand with an outer diameter C aand to obtain an inner diameter Ci, characterized in that the outer and inner diameter ratio of the cylinder changes during inverse collapse and simultaneous elongation to the capillary such that: 2.9 to 4.2; iv) Cutting the capillary strand to the desired length while retaining capillaries with an outer diameter C a and an inner diameter Ci, for which the following applies: 1.08 to 1.

30. Cl 14. A capillary characterized in that it has an outer diameter C a and has an inner diameter Ci for which the following applies: 1.05 to 1.50, 'preferably 1.08 to 1.30, and that it has an equilibrium pressure pc between 50 Pa and 800 Pa, and that the ratio of a longer axis to a shorter axis in the cross-section is 1.00 to 1.

02.

15. The capillary according to claim 14, obtainable by a method according to claims 1 to 13.

Citation Information

Patent Citations

  • Full-fluorine-doped mother tube, full-fluorine-doped capillary tube and preparation method of full-fluorine-doped mother tube

    CN116715447A

  • Production of a glass tube in a hot drawing process comprises feeding a hollow cylinder having an inner bore into which an inert gas stream mixed with oxygen is fed, softening and removing the glass tube from the softened region

    DE10228599A1

  • Large sized quartz glass tube, large scale quartz glass preform, process for manufacturing the same and quartz glass optical fiber

    EP0598349A2

  • Process of making a hollow core anti resonant fiber preform

    EP4011840A1

  • Method for drawing glass member

    JP2004123461A