CN117105519A - Preparation method of large-size quartz bushing - Google Patents
Preparation method of large-size quartz bushing Download PDFInfo
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- CN117105519A CN117105519A CN202311151139.1A CN202311151139A CN117105519A CN 117105519 A CN117105519 A CN 117105519A CN 202311151139 A CN202311151139 A CN 202311151139A CN 117105519 A CN117105519 A CN 117105519A
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- hollow glass
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- glass base
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 185
- 239000010453 quartz Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 71
- 238000000034 method Methods 0.000 claims abstract description 59
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 48
- 230000008569 process Effects 0.000 claims abstract description 37
- 239000007787 solid Substances 0.000 claims abstract description 24
- 230000008021 deposition Effects 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 238000000227 grinding Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 235000012239 silicon dioxide Nutrition 0.000 claims description 78
- 239000000758 substrate Substances 0.000 claims description 34
- 238000000151 deposition Methods 0.000 claims description 28
- 239000007789 gas Substances 0.000 claims description 24
- 239000013307 optical fiber Substances 0.000 claims description 24
- 239000012535 impurity Substances 0.000 claims description 23
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 230000007704 transition Effects 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 239000000460 chlorine Substances 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- 229910052731 fluorine Inorganic materials 0.000 claims description 6
- 239000011737 fluorine Substances 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 6
- 229910052734 helium Inorganic materials 0.000 claims description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000002912 waste gas Substances 0.000 claims description 6
- 238000005491 wire drawing Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 230000001276 controlling effect Effects 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 claims description 3
- 238000001089 thermophoresis Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- WMIYKQLTONQJES-UHFFFAOYSA-N hexafluoroethane Chemical compound FC(F)(F)C(F)(F)F WMIYKQLTONQJES-UHFFFAOYSA-N 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 claims description 2
- 238000012545 processing Methods 0.000 abstract description 12
- 230000005484 gravity Effects 0.000 abstract description 6
- 238000005253 cladding Methods 0.000 abstract description 4
- 238000010586 diagram Methods 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 230000009471 action Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000004017 vitrification Methods 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000004807 localization Effects 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
Abstract
The application relates to a preparation method of a large-size quartz bushing, wherein a target rod assembly is formed by a hollow glass base pipe and an internal solid carbon rod, so that when a silica loose body is formed by deposition outside the hollow glass base pipe, the hollow glass base pipe and the internal solid carbon rod are internally supported, the problem that the size of the silica loose body is limited due to gravity deformation can be solved, and a loose body with larger size can be prepared; in addition, in the pretreatment and vacuum sintering stages, the solid core rod, the hollow glass base tube and the silica loose body outside the hollow glass base tube form a structure, and complex processing such as center hole digging, diffraction grinding and the like is not needed in the follow-up process, so that the process is simplified. Furthermore, the finally formed quartz lining sleeve blank only needs simple grinding and processing to directly prepare the front end of the sleeve in the subsequent working procedure, and meanwhile, the central hole digging and the diffraction grinding are not needed, so that the raw material of the sleeve is utilized to the greatest extent; of course, it can also be used directly for the outer cladding of the RIC rod.
Description
Technical Field
The application relates to the technical field of manufacturing of optical fiber preforms and quartz products, in particular to a preparation method of a large-size quartz lining pipe.
Background
The quartz liner tube and the sleeve are important basic raw materials which are indispensable in the optical fiber preform industry, and are widely applied to manufacturing of single-mode optical fiber preforms, multimode optical fiber preforms and special optical fiber preforms. Wherein the quartz liner is used primarily as a starting deposition substrate tube for preparing optical fiber preforms in MCVD (Modified-Chemical Vapor Deposition) and PCVD (Plasma ChemicalVapor Deposition), etc., while the liner is used primarily as a relatively thicker overclad material for overcladding the core rod in RIC (Rod In Cylinder) rod making processes. Along with the development of the optical fiber preform industry towards a large size, a large-size quartz lining pipe plays a crucial role; on the other hand, the quality (such as purity, hydroxyl content, defects, etc.) of the quartz lining tube and the sleeve has important influence on the optical transmission loss, mechanical strength, etc. of the drawn optical fiber, and particularly, as the communication optical fiber evolves towards lower transmission loss and larger section length, higher requirements are also put on the quality of the quartz lining tube.
However, although China is the largest fiber optic cable manufacturing country worldwide, large-size quartz bushings for optical fibers still depend mainly on foreign importation. Patent CN103224326A describes a method for preparing a large-diameter optical fiber preform sleeve by using a high-frequency plasma solid-phase external deposition PSOD process by taking quartz sand as a raw material, but the problems of high impurity content, more defects, low deposition efficiency, complicated mechanical processing and the like exist. Patent CN103951182a describes a method for preparing a complex refractive index profile optical fiber preform sleeve based on MCVD and horizontal OVD processes, but cannot overcome the problem of small sleeve size due to the influence of transverse gravity. And the industrial technology of high-end quartz lining pipe products with large size and high purity is in need of solving the urgent need of autonomous localization.
Disclosure of Invention
The embodiment of the application provides a preparation method of a large-size quartz lining pipe, which aims to solve the problem that complicated machining processes are needed in the related art.
In a first aspect, a method for preparing a large-size quartz bushing is provided, which comprises:
depositing outside the target rod assembly to form a silica loose body; the target rod assembly comprises a hollow glass base tube and a solid carbon rod therein;
extracting a solid carbon rod, then placing the hollow glass substrate tube and the silica loose body thereon in a pretreatment furnace, and introducing impurity removal process gas to remove impurities at high temperature to obtain a pretreatment body;
and plugging the bottom of the hollow glass base pipe of the pretreatment body, and then placing the hollow glass base pipe in a vacuum sintering furnace to form a quartz lining pipe blank under set pressure and set temperature.
In some embodiments, after obtaining the quartz liner tube blank, the method further comprises the steps of:
and carrying out medium-frequency non-contact secondary tube drawing on the quartz lining tube blank according to different target requirements so as to obtain the quartz lining tube with corresponding size.
In some embodiments, after obtaining the quartz liner tube blank, the method further comprises the steps of:
inserting an optical fiber preform core rod into the center of the quartz lining pipe blank, and vacuumizing the interior of the optical fiber preform core rod; rod making and wire drawing are performed by using RIC technology after vacuumizing, so as to obtain the optical fiber preform.
In some embodiments, after obtaining the quartz liner tube blank, the method further comprises the steps of:
grinding a conical transition section at the lower part of the quartz lining pipe blank to form a pipe front end, and cutting off a transition section at the top of the quartz lining pipe blank and a glass base pipe tail pipe to obtain an effective pipe section; and finally, cleaning the effective pipe section.
In some embodiments, during the sintering process of placing the pre-treated body in the vacuum sintering furnace, the method further comprises the steps of:
and introducing inert process gas into the top of the hollow glass substrate tube, and controlling the pressure in the hollow glass substrate tube to be within a set pressure range through a pressure monitoring and pressure regulating device.
In some embodiments, the hollow glass substrate tube and the loose body of silica thereon are placed in a pretreatment furnace, and the method further comprises the following steps in addition to introducing the impurity removal process gas:
introducing fluorine-containing gas to prepare a fluorine-doped pretreatment body; the fluorine-containing gas includes carbon tetrafluoride, silicon tetrafluoride and hexafluoroethane.
In some embodiments, depositing the silica loose body outside of the target assembly comprises the steps of:
vertically arranging the target rod assembly;
a multi-blast lamp deposition system of the OVD deposition equipment is adopted, silicon-containing raw materials are chemically reacted to form silicon dioxide particles, and the silicon dioxide particles are deposited on a target rod assembly layer by layer according to a thermophoresis effect at an average deposition rate of 120-200g/min to form a silicon dioxide loose body with the diameter of 350-450mm and the length of 2000-3500 mm.
In some embodiments, the pretreatment furnace has an exhaust outlet at the top and an air inlet at the bottom;
the impurity removal process gas comprises 5-20SLM helium, 0.8-2SLM chlorine and 0.1-0.5SLM oxygen;
placing the hollow glass substrate tube and the silica loose body thereon in a pretreatment furnace, and introducing impurity removal process gas to remove impurities at high temperature to obtain a pretreatment body, wherein the pretreatment body comprises the following steps:
placing the hollow glass substrate tube and the silica loose body thereon in a pretreatment furnace;
then 5-20SLM helium, 0.8-2SLM chlorine and 0.1-0.5SLM oxygen are introduced from the gas inlet; simultaneously removing impurities on the inner wall of the silica loose body and the hollow glass substrate tube at the temperature of 1000-1200 ℃, and discharging waste gas generated by the reaction through a waste gas outlet;
wherein, the micro positive pressure of 0.5 to 3Torr in the pretreatment furnace is maintained in the whole pretreatment process.
In some embodiments, the specific steps of plugging the bottom of the hollow glass substrate tube of the pretreatment body are: and (3) burning and melting the lower end of the hollow glass base pipe through high-temperature oxyhydrogen flame to form a conical plug.
In some embodiments, the hollow glass substrate tube in the target rod assembly has a thickness of 10-20mm, and the single-sided gap between the hollow glass substrate tube and the solid carbon rod is between 0.5-1 mm.
The technical scheme provided by the application has the beneficial effects that:
the embodiment of the application provides a preparation method of a large-size quartz bushing, wherein a target rod assembly is formed by a hollow glass base pipe and an internal solid carbon rod, so that when a silica loose body is formed by deposition outside the hollow glass base pipe, the hollow glass base pipe and the internal solid carbon rod are internally supported, the problem that the size of the silica loose body is limited due to gravity deformation can be solved, and a loose body with larger size can be prepared; in addition, in the pretreatment and vacuum sintering stages, the solid core rod, the hollow glass base tube and the silica loose body outside the hollow glass base tube form a structure, and complex processing such as center hole digging, diffraction grinding and the like is not needed in the follow-up process, so that the process is simplified.
Furthermore, the finally formed quartz lining sleeve blank only needs simple grinding and processing to directly prepare the front end of the sleeve in the subsequent working procedure, and meanwhile, the central hole digging and the diffraction grinding are not needed, so that the raw material of the sleeve is utilized to the greatest extent; of course, it can also be used directly for the outer cladding of the RIC rod.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present application, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method for preparing a large-sized bushing pipe according to an embodiment of the present application;
FIG. 2 is a schematic diagram of a large-size silica loose body prepared by vertical OVD deposition provided by an embodiment of the present application;
FIG. 3 is a schematic diagram of pretreatment impurity removal of a large-size silica loose body provided by an embodiment of the application;
FIG. 4 is a schematic diagram of a blank of a large-size quartz bushing manufactured by vacuum sintering one-step molding according to an embodiment of the present application;
FIG. 5 is a schematic view of a large-size quartz bushing blank provided by an embodiment of the present application;
FIG. 6 is a schematic diagram of a large-sized quartz bushing machined from a large-sized quartz bushing blank according to an embodiment of the present application;
FIG. 7 is a schematic diagram of a large-size quartz bushing blank for intermediate frequency non-contact tube pulling to prepare a liner tube according to an embodiment of the application;
FIG. 8 is a schematic diagram of a large-size quartz bushing blank directly used as a cladding of an optical fiber preform according to an embodiment of the present application.
In the figure: 1. a solid carbon rod; 2. a hollow glass substrate tube; 3. a multiple lamp deposition system; 4. a loose body of silica; 5. a pretreatment furnace; 6. an air inlet; 7. an exhaust gas outlet; 8. conical plugging; 9. a vacuum sintering furnace; 10. a hollow glass substrate tube seal; 11. an air inlet pipe; 12. an exhaust tube; 13. quartz lining pipe blank; 14. a transition section at the upper part of the sleeve blank; 15. a lower transition section of the sleeve blank; 16. quartz lining pipe; 17. the front end of the sleeve; 18. intermediate frequency non-contact tube drawing equipment; 19. an optical fiber preform core rod.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments of the present application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
The quartz lining pipe can be used as a lining pipe and a sleeve pipe, and the quartz lining pipe obtained by the preparation method can be used as the lining pipe and the sleeve pipe, so that the following identification description is carried out by the quartz lining pipe.
The embodiment of the application provides a preparation method of a large-size quartz lining pipe, which aims to solve the problems of low deposition efficiency and complicated machining process in the related art.
Referring to fig. 1-8, a method for preparing a large-size quartz bushing comprises the following steps:
s01, depositing outside the target rod assembly to form a silica loose body 4; the target rod assembly comprises a hollow glass base tube 2 and a solid carbon rod 1 therein; the hollow glass substrate tube 2 is a high-purity quartz glass substrate tube;
step S02, extracting the solid carbon rod 1, then placing the hollow glass substrate tube 2 and the silica loose body 4 thereon in a pretreatment furnace 5, and introducing impurity removal process gas to remove impurities at high temperature to obtain a pretreatment body;
step S03, sealing the bottom of the hollow glass substrate tube 2 of the pretreatment body, vacuumizing the vacuum sintering furnace 9, and placing the hollow glass substrate tube 2 with the sealed bottom in the vacuum sintering furnace 9 to form a quartz lining tube blank 13 under set pressure and set temperature.
Because the hollow glass base tube 2 and the internal solid carbon rod 1 form a target rod assembly, when the silica loose body 4 is formed by deposition outside the hollow glass base tube 2, the hollow glass base tube 2 and the internal solid carbon rod 1 are internally supported, so that the problem that the size of the silica loose body is limited due to gravity deformation can be solved, and a loose body with larger size can be prepared; in addition, in the pretreatment and vacuum sintering stages, the solid core rod, the hollow glass base tube and the silica loose body outside the hollow glass base tube form a structure, and complex processing such as center hole digging, diffraction grinding and the like is not needed in the follow-up process, so that the process is simplified.
Furthermore, the finally formed quartz lining sleeve blank only needs simple grinding and processing to directly prepare the front end of the sleeve in the subsequent working procedure, and meanwhile, the central hole digging and the diffraction grinding are not needed, so that the raw material of the sleeve is utilized to the greatest extent; of course, it can also be used directly for the outer cladding of the RIC rod.
The problem that the size of a loose body is limited due to gravity deformation is overcome by vertical deposition, and the prepared quartz lining pipe blank 13 is large in size and high in manufacturing efficiency; the prepared quartz bushing blank 13 has extremely low hydroxyl and impurity element contents, has few defects such as bubbles in glass materials, and meets the requirement of the optical fiber industry on high-quality bushings.
Referring to fig. 2, in some preferred embodiments, the specific steps of step S01 are:
the large-size silica loose body deposition is carried out by preparing a large-size silica loose body 4 by using vertical OVD deposition equipment, namely, adopting a multi-blast lamp deposition system outside a starting target rod assembly arranged in the vertical direction, chemically reacting silicon-containing raw materials such as high-purity silicon tetrachloride (SiCl 4), octamethyl cyclotetrasiloxane (OMCTS) and the like to form silica particles, and gradually depositing the silica particles layer by layer according to thermophoresis effect at an average deposition rate of 120-200g/min on the outside of the target rod assembly to form the large-size silica loose body 4 with the diameter of 350-450mm and the length of 2000-3500 mm.
The high-purity solid carbon rod 1 is nested in a high-purity quartz glass base tube to form a target rod assembly, the thickness of the high-purity quartz glass base tube (namely the hollow glass base tube 2) is 10-20mm, and the unilateral clearance between the high-purity solid carbon rod 1 and the high-purity quartz glass base tube is controlled to be 0.5-1mm; the initial target rod assembly formed by the combination is arranged in the vertical direction and rotates at a certain speed, the multi-lamp deposition system 3 is also arranged in the vertical direction, and the torch flame is perpendicular to the target rod assembly. The target rod component is formed by nesting a high-purity solid carbon rod 1 in a high-purity quartz glass substrate tube (namely a hollow glass substrate tube 2).
Referring to fig. 3, in some preferred embodiments, the specific steps of step S02 are:
the pretreatment process comprises the steps of deeply removing impurities, extracting a high-purity solid carbon rod 1 from a target rod assembly of a large-size silica loose body 4, transferring the large-size silica loose body 4 carried by a high-purity quartz glass substrate tube into a pretreatment furnace 5, introducing 5-20SLM helium, 0.8-2SLM chlorine, 0.1-0.5SLM oxygen and other process gases from a process gas inlet 6, and removing hydroxyl, carbon, metal ions and other impurities on the inner wall of the large-size silica loose body 4 and the high-purity quartz glass substrate tube at a high temperature of 1000-1200 ℃; the waste gas generated by the reaction is discharged through a waste gas outlet 7, and the micro positive pressure of 0.5-3Torr in the pretreatment furnace 5 is maintained in the whole pretreatment process.
In some preferred embodiments, the specific steps of step S03 are:
the vacuum sintering process comprises the steps of forming in one step, burning and plugging the lower end of a hollow glass substrate tube 2 through high-temperature flames such as oxyhydrogen flames or propane flames to form a lower conical plug 8 and an upper opening structure, transferring the pretreated body after pretreatment into a vacuum sintering furnace 9, and pumping the interior to a complete vacuum state to enable a silica loose body 4 to be completely located in a vacuum environment; the silica loose body 4 is integrally sintered and molded under the vitrification temperature of 1400-1500 ℃ and vacuum condition, the upper part of a high-purity quartz glass base tube with the lower part blocked is blocked by a hollow glass base tube sealing piece 10, and inert process gases such as nitrogen or argon are introduced into the glass base tube through an air inlet pipe 11, and the air is extracted outwards from an exhaust pipe 12 to control the pressure in the tube; heating the vacuum sintering furnace 9 to 1400-1500 ℃ to vitrify the large-size silica loose body 4 into a whole, and sintering and forming to form a large-size quartz lining pipe blank 13 with uniform outer diameter of 180-220mm and hollow inside and length of 2000-3500mm, for example, as shown in fig. 4 and 5;
further, in order to avoid deformation or fusion shrinkage of the central through hole glass tube in the vitrification radial shrinkage process of the loose body, the pressure monitoring and automatic adjusting device is used for controlling the air inlet flow and the air exhaust flow so as to ensure that the pressure in the hollow glass substrate tube 2 is stabilized between 100 Pa and 500 Pa; finally, a large-size quartz bushing blank 13 with a uniform outer diameter of 180-220mm and a hollow interior and a length of 2000-3500mm is formed.
There are several subsequent embodiments for the quartz liner blank 13 formed, specific embodiments are given below:
example 1
Cutting off the upper transition section 14 of the sleeve blank and the tail pipe of the glass base pipe of the prepared large-size quartz lining sleeve blank 13, carrying out simple grinding processing on the lower transition section 15 of the sleeve blank to directly prepare a sleeve front end 17, and then carrying out cleaning processing to obtain a large-size quartz lining sleeve 16 with the effective weight of 100-275 Kg; reference is made to fig. 6.
Example two
The large-size quartz bushing blank 13 prepared in the third step is subjected to intermediate frequency non-contact secondary tube drawing on intermediate frequency non-contact tube drawing equipment 18 to prepare large-size liners with different specifications; the intermediate frequency furnace is used for heating, and the quartz bushing blank 13 is not contacted with the heater, so that the prepared large-size bushing tube is not polluted by secondary pollution and still keeps higher purity; the large-sized liner tube prepared as above can be used as a glass base tube on which the large-sized silica porous body 4 is deposited; reference is made to fig. 7.
Example III
The large-size quartz lining pipe blank 13 obtained in the third step can be inserted into a high-purity quartz glass base pipe of the large-size quartz lining pipe blank to be matched with an optical fiber preform core rod 19 designed, and the optical fiber preform core rod 19 can be obtained by directly performing rod making and wire drawing by using RIC (RIC) technology); wherein, through inside evacuation, can directly use RIC technology to carry out online wire drawing in the high temperature wire drawing stove, single jumbo size sleeve pipe can wire drawing length reaches more than 6000Km, and the reference is shown in FIG. 8.
Example IV
When the prepared large-size silica loose body 4 is transferred into a pretreatment furnace 5 for pretreatment, 1SLM CF4 is synchronously introduced from a process gas inlet 6 for fluorine doping, and then the large-size fluorine doped sleeve with the refractive index sinking of-0.12% can be obtained after vacuum sintering and simple processing.
Therefore, through the above description, the obtained quartz lining pipe blank has various subsequent construction modes, and different products can be obtained according to the needs.
Through the above description, the vertical OVD deposition technology is adopted to deposit the large-size silica loose body 4 at high speed outside the target rod assembly consisting of the solid carbon rod 1 and the hollow glass base tube 2, and the target rod assembly has a supporting function, so that the problems of low deposition efficiency and limited size of the loose body caused by gravity deformation are effectively solved;
then, extracting a solid carbon rod 1 from the target rod assembly, placing a silica loose body 4 carried by a hollow glass substrate tube 2 in a pretreatment furnace, introducing process gases such as helium, oxygen, chlorine and the like, removing hydroxyl groups and other impurity elements on the loose body and the glass tube at high temperature, plugging the bottom of the hollow glass substrate tube 2, placing the silica loose body 4 in a vacuum sintering furnace 9, maintaining a certain positive pressure in the hollow glass tube, and integrally forming glass of a large-size loose body at high temperature to form a large-size quartz sleeve blank with uniform outer diameter and hollow inside; the quartz glass with high purity and few defects can be obtained through pretreatment and vacuum sintering technology, and the prefabricated central through hole avoids the subsequent complicated drilling, grinding and other processing processes, and meanwhile, the waste of raw materials is effectively reduced.
The prepared quartz lining pipe has extremely low hydroxyl and impurity element contents, has few defects such as bubbles in glass materials, and meets the requirements of the optical fiber industry on high-quality lining pipes; the central through hole of the sleeve is prefabricated, complex processing such as central hole digging and grinding is not needed after the integrated molding is carried out, and the process is simplified; the lower conical surface of the sintering large-size quartz lining sleeve blank 13 is simply ground to directly prepare the sleeve front end, and meanwhile, the central hole drawing and the diffraction grinding are not needed, so that the sleeve raw material is utilized to the greatest extent.
In the description of the present application, it should be noted that the azimuth or positional relationship indicated by the terms "upper", "lower", etc. are based on the azimuth or positional relationship shown in the drawings, and are merely for convenience of describing the present application and simplifying the description, and are not indicative or implying that the apparatus or element in question must have a specific azimuth, be constructed and operated in a specific azimuth, and thus should not be construed as limiting the present application. Unless specifically stated or limited otherwise, the terms "mounted," "connected," and "coupled" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art according to the specific circumstances.
It should be noted that in the present application, relational terms such as "first" and "second" and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The foregoing is only a specific embodiment of the application to enable those skilled in the art to understand or practice the application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The preparation method of the large-size quartz bushing is characterized by comprising the following steps of:
depositing outside the target rod assembly to form a silica loose body (4); the target rod assembly comprises a hollow glass base tube (2) and a solid carbon rod (1) therein;
extracting a solid carbon rod (1), then placing the hollow glass substrate tube (2) and the silica loose body (4) thereon in a pretreatment furnace (5), and introducing impurity removal process gas to remove impurities at high temperature to obtain a pretreated body;
the bottom of the hollow glass base tube (2) of the pretreatment body is plugged, and then the hollow glass base tube is placed in a vacuum sintering furnace (9) to form a quartz lining tube blank (13) at a set pressure and a set temperature.
2. A method for producing a large-size quartz bushing according to claim 1, characterized in that after obtaining the quartz bushing blank (13), it further comprises the steps of:
and carrying out medium-frequency non-contact secondary tube drawing on the quartz lining tube blank (13) according to different target requirements so as to prepare the quartz lining tube with corresponding size.
3. A method for producing a large-size quartz bushing according to claim 1, characterized in that after obtaining the quartz bushing blank (13), it further comprises the steps of:
inserting an optical fiber preform core rod (19) into the center of the quartz lining pipe blank (13), and vacuumizing the interior of the optical fiber preform core rod; rod making and wire drawing are performed by using RIC technology after vacuumizing, so as to obtain the optical fiber preform.
4. A method for producing a large-size quartz bushing according to claim 1, characterized in that after obtaining the quartz bushing blank (13), it further comprises the steps of:
grinding a conical transition section at the lower part of the quartz lining pipe blank (13) to form a pipe front end (17), and cutting off a transition section at the top of the quartz lining pipe blank (13) and a glass base pipe tail pipe to obtain an effective pipe section; and finally, cleaning the effective pipe section.
5. The method for producing a large-sized quartz bushing according to claim 1, characterized by further comprising the steps of, during the sintering of the pre-treated body in the vacuum sintering furnace (9):
and introducing inert process gas into the top of the hollow glass substrate tube (2), and controlling the pressure in the hollow glass substrate tube (2) to be within a set pressure range through a pressure monitoring and pressure regulating device.
6. The method for manufacturing a large-sized quartz bushing according to claim 1, wherein:
placing the hollow glass substrate tube (2) and the silica loose body (4) on the hollow glass substrate tube in a pretreatment furnace (5), and introducing impurity removing process gas, wherein the method further comprises the following steps of:
introducing fluorine-containing gas to prepare a fluorine-doped pretreatment body; the fluorine-containing gas includes carbon tetrafluoride, silicon tetrafluoride and hexafluoroethane.
7. A method of preparing a large size quartz bushing according to claim 1, wherein depositing a loose body of silica (4) outside the target rod assembly comprises the steps of:
vertically arranging the target rod assembly;
a multi-torch deposition system of the OVD deposition equipment is adopted, silicon-containing raw materials are chemically reacted to form silicon dioxide particles, and the silicon dioxide particles are deposited on a target rod assembly layer by layer according to a thermophoresis effect at an average deposition rate of 120-200g/min to form a silicon dioxide loose body (4) with the diameter of 350-450mm and the length of 2000-3500 mm.
8. The method for manufacturing a large-sized quartz bushing according to claim 1, wherein:
the top of the pretreatment furnace (5) is provided with an exhaust gas outlet (7), and the bottom of the pretreatment furnace is provided with an air inlet (6);
the impurity removal process gas comprises 5-20SLM helium, 0.8-2SLM chlorine and 0.1-0.5SLM oxygen;
placing the hollow glass substrate tube (2) and the silica loose body (4) on the hollow glass substrate tube in a pretreatment furnace (5), and introducing impurity removal process gas to remove impurities at high temperature to obtain a pretreatment body, wherein the pretreatment body comprises the following steps of:
placing the hollow glass substrate tube (2) and the silica loose body (4) thereon in a pretreatment furnace (5);
then 5-20SLM helium, 0.8-2SLM chlorine and 0.1-0.5SLM oxygen are introduced from the gas inlet (6); simultaneously removing impurities on the inner walls of the silica loose body (4) and the hollow glass base tube (2) at the temperature of 1000-1200 ℃, and discharging waste gas generated by the reaction through a waste gas outlet (7);
wherein, the micro positive pressure of 0.5 to 3Torr in the pretreatment furnace (5) is maintained in the whole pretreatment process.
9. The method for manufacturing a large-sized quartz bushing according to claim 1, wherein:
the concrete steps of plugging the bottom of the hollow glass base tube (2) of the pretreatment body are as follows: the lower end of the hollow glass base tube (2) is burnt and melted by high-temperature oxyhydrogen flame to form a conical plug (8).
10. The method for manufacturing a large-sized quartz bushing according to claim 1, wherein:
the thickness of the hollow glass base tube (2) in the target rod assembly is 10-20mm, and the unilateral gap between the hollow glass base tube (2) and the solid carbon rod (1) is 0.5-1 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311151139.1A CN117105519A (en) | 2023-09-07 | 2023-09-07 | Preparation method of large-size quartz bushing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311151139.1A CN117105519A (en) | 2023-09-07 | 2023-09-07 | Preparation method of large-size quartz bushing |
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| Publication Number | Publication Date |
|---|---|
| CN117105519A true CN117105519A (en) | 2023-11-24 |
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| CN202311151139.1A Pending CN117105519A (en) | 2023-09-07 | 2023-09-07 | Preparation method of large-size quartz bushing |
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| Country | Link |
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| CN (1) | CN117105519A (en) |
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- 2023-09-07 CN CN202311151139.1A patent/CN117105519A/en active Pending
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