CN109264985A - A kind of degassing method and device of preform - Google Patents
A kind of degassing method and device of preform Download PDFInfo
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- CN109264985A CN109264985A CN201811353111.5A CN201811353111A CN109264985A CN 109264985 A CN109264985 A CN 109264985A CN 201811353111 A CN201811353111 A CN 201811353111A CN 109264985 A CN109264985 A CN 109264985A
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- preform
- drying oven
- vacuum drying
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
- C03B37/01853—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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- Thermal Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
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- Organic Chemistry (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
Abstract
The embodiment of the invention discloses a kind of degassing method and devices of preform, the degassing method includes heating up first to quartz glass tube, preform is installed on quartz hanging bar later, and is inserted into quartz glass tube, is handled finally by vacuum evacuation device.In addition, present applicant proposes a kind of devices applied to above-mentioned preform degassing method.The embodiment of the invention provides a kind of degassing method and devices of preform, the application provides heat source using vacuum drying oven, calandria is made of multistage graphite heating pipe, there is graphite Thiele tube in simultaneously, equipped with multiple groups temperature sensor, conducive to the control of in-furnace temperature, due to remaining vacuum state in furnace, the service life for greatly improving furnace body, reduces maintenance cost.In addition, the degassing and annealing of preform are completed in quartz glass tube, and close to vacuum state in quartz glass tube, movable impurity is less in furnace, and preform surface contamination can be greatly reduced.
Description
Technical field
The present invention relates to preform technical fields, and in particular to a kind of degassing method and device of preform.
Background technique
Since the communications field is arrived in the invention and extensive application of silica fibre, the market demand increases year by year, current entire optical fiber
Up to hundred billion scales, each manufacturer also constantly expands production, and constantly pursues lower production cost, higher in market
Product quality.
Main production link is plug production and surrounding layer production in preform production process, all contains SiO2
Then the deposition of dust sinters glass into, during the sintering process, a certain amount of gas can be remained in vitreum, such as helium, nitrogen
Gas, chlorine etc., and remain a large amount of internal stress.The presence of residual gas and internal stress can seriously affect the wire drawing quality of optical fiber, packet
Include the disconnected fine probability increased in fiber drawing process, the intensity for reducing optical fiber, the pad value for increasing optical fiber etc., and plug and optical fiber
The degassing and annealing of prefabricated rods can well solve problem above.
Theoretically, the annealing of preform can continue to complete for several hours at 1100 DEG C or so, vitreum internal gas
Molecule can be dispersed into surface by warm-up movement；The atomic structure of internal SiO2 can also carry out warm-up movement at high temperature and arrange from new
Column, to discharge internal stress.Patent CN 106830651A discloses a kind of large-scale optical fiber prefabricating stick deshydroxy method for annealing and dress
It sets, the laterally disposed several preforms in a burner hearth, is disappeared by certain heating, heat preservation, cooling step realization
Except stick internal stress and residual gas.But its preform is due to laterally disposed, at high temperature due to gravity, radially
New internal stress can be generated；Preform outer surface is exposed in holding furnace, since calandria, insulation fibre are exposed to
Outside, the metal impurities largely evaporated are had under high temperature, in cavity be bonded to prefabricated rods surface and pollute, influence prefabricated rods
Quality.Patent CN105753311A discloses the degasser and method of a kind of preform, and multifiber prefabricated rods are put
Enter in quartz ampoule, quartz ampoule is vacuumized, be de-gassed after heating, improves production efficiency.But the device is to seal request
It is higher, especially size fibers prefabricated rods stick size is difficult be accurately obtained control, and the sealing of quartz ampoule and quartz plate
There are biggish difficulty.More prefabricated rods equally exist the non-uniform temperature of prefabricated rods in the radial direction in same quartzy furnace,
There can be portion of residual stress after completing degassing, and generate new thermal stress.
The condition of preform degassing annealing is very harsh, if temperature is too low, internal gas can be detached from, if being lower than
Specific 950 DEG C of temperature, then long time also can not be completed degassing and annealing function；If temperature is excessively high, be more than 1200 DEG C very
To higher, then preform surface can gradually crystallize, embrittlement, seriously affect drawing optical fibers quality.Accordingly, it is determined that one moderate
Degassing annealing process, it is most important to the production of preform.
Summary of the invention
A kind of degassing method and device for being designed to provide preform of the embodiment of the present invention, entire degasification process
It is to carry out under vacuum, can be speeded away prefabricated rods surface by the residual gas that warm-up movement reaches preform, it is more sharp
In the quick progress of degassing work.
To achieve the above object, the embodiment of the present invention provides a kind of degassing method of preform, comprising the following steps:
Step 1: the quartz glass tube internal temperature of Raise vacuum furnace is to 600~900 DEG C；
Step 2: opening the fire door of cooling chamber, preform is installed on quartz hanging bar, decline hanging compression bar
It arrives, realizes and seal until O-ring, close fire door；
Step 3: being vacuumized using vacuum evacuation device to cooling chamber, it is warming up to 10~300 DEG C/h of speed
It 1000~1300 DEG C, is kept for 3~20 hours, cools to 900 DEG C hereinafter, holding 0.5~3 is small with 10~300 DEG C/h of speed
When, compression bar is hung later and is risen, and preform is cooling in cooling chamber.
Among some embodiments, when deaerating heating, heating rate≤200 DEG C/h, when cooling, cooling rate≤
200℃/h。
Among some embodiments, the absolute pressure inside vacuum drying oven is controlled in 5~100Pa, and cooling chamber is in operation
Cheng Zhong, absolute pressure are controlled in 10~200Pa.
In addition, present applicant proposes a kind of device applied to above-mentioned preform degassing method, described device includes
Vacuum drying oven, the cooling chamber that vacuum furnace top is arranged in and hanging compression bar, are equipped with thermal insulation layer, institute between the vacuum drying oven and cooling chamber
The hanging compression bar stated sequentially passes through cooling chamber and thermal insulation layer enters in vacuum drying oven, and the bottom end of the hanging compression bar is equipped with predispersed fiber
Stick processed is respectively equipped with vacuum evacuation device in the vacuum drying oven and cooling chamber.
Among some embodiments, the thermal insulation layer includes quartzy heat shield and the stone that is arranged in above quartzy heat shield
Black heat shield.
Among some embodiments, the vacuum drying oven includes furnace shell, calandria, graphite Thiele tube, insulation quilt, Yi Jishe
The quartz glass tube that can accommodate preform in furnace shell is set, and sets gradually heat preservation from furnace shell to quartz glass tube direction
Felt, calandria and graphite Thiele tube.
Among some embodiments, calandria is made of 2~6 groups of heaters in the vacuum drying oven, adjacent heater it
Between gap be 20~50mm, there are two temperature sensors, a temperature sensor to be used for monitoring temperature for installation on every group of calandria,
Another temperature sensor is for controlling temperature.
Among some embodiments, graphite Thiele tube is spliced by 2~6 groups of graphite-pipes, graphite-pipe with a thickness of 4~
8mm。
Among some embodiments, metal pressure ring is equipped at the top of the thermal insulation layer, a screw sequentially passes through metal pressure ring
And vacuum furnace top, realization thermal insulation layer are fixedly connected with vacuum drying oven.
Among some embodiments, polytetrafluoroethylene (PTFE) pad is equipped between the thermal insulation layer and metal pressure ring, it is described heat-insulated
Perfluor O-ring is equipped between layer and vacuum drying oven, the diameter of section of perfluor O-ring is 6~12mm, and seal compression is diameter of section
1/4~1/2.
Compared with prior art, this have the advantage that: the embodiment of the invention provides a kind of optical fiber prefabricatings
The degassing method and device of stick, the application provide heat source using vacuum drying oven, and calandria is made of multistage graphite heating pipe, while interior
There is graphite Thiele tube, is furnished with multiple groups temperature sensor, conducive to the control of in-furnace temperature, due to remaining vacuum state in furnace,
The service life for greatly improving furnace body, reduces maintenance cost.In addition, the degassing and annealing of preform are in quartz glass
It is completed in pipe, and close to vacuum state in quartz glass tube, movable impurity is less in furnace, and preform can be greatly reduced
Surface contamination；Under vacuum conditions, also it is conducive to residual gas in prefabricated rods and degassing time and temperature is greatly reduced to external diffusion.
Preform vertically downward, conducive to the release of side internal stress, is conducive to pull out the higher optical fiber of qualification rate when deaerating simultaneously.
Detailed description of the invention
Fig. 1 is one of the structural schematic diagram of device described in an exemplary embodiments of the invention；
Fig. 2 is the structural schematic diagram of vacuum drying oven in an exemplary embodiments of the invention；
Description of symbols: 1, vacuum drying oven；2, cooling chamber；3, fire door；4, compression bar is hung；5, vacuum evacuation device；6, O-shaped
Circle；7, preform；8, graphite heat shield；9, quartzy heat shield；10, quartz hanging bar；101, quartz glass tube；102, add
Hot body；103, graphite Thiele tube；104, insulation quilt；105, furnace shell；106, perfluor O-ring；107, polytetrafluoroethylene (PTFE) pad；108, golden
Belong to pressure ring, 109, screw.
Specific embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book is understood other advantages and efficacy of the present invention easily.
Present embodiment discloses a kind of degassing methods of preform, comprising the following steps:
Step 1: the quartz glass tube internal temperature of Raise vacuum furnace is to 600~900 DEG C；
Step 2: opening the fire door of cooling chamber, preform is installed on quartz hanging bar, decline hanging compression bar
It arrives, realizes and seal until O-ring, close fire door；
Step 3: being vacuumized using vacuum evacuation device to cooling chamber, it is warming up to 10~300 DEG C/h of speed
It 1000~1300 DEG C, is kept for 3~20 hours, cools to 900 DEG C hereinafter, holding 0.5~3 is small with 10~300 DEG C/h of speed
When, compression bar is hung later and is risen, and preform is cooling in cooling chamber.
Further, when deaerating heating, heating rate≤200 DEG C/h, when cooling, cooling rate≤200 DEG C/h.Vacuum
The absolute pressure of furnace interior is controlled in 5~100Pa, and in operation process, absolute pressure is controlled in 10~200Pa cooling chamber.
In addition, present applicant proposes a kind of device applied to above-mentioned preform degassing method, described device includes
Vacuum drying oven, the cooling chamber that vacuum furnace top is arranged in and hanging compression bar, are equipped with thermal insulation layer, institute between the vacuum drying oven and cooling chamber
The hanging compression bar stated sequentially passes through cooling chamber and thermal insulation layer enters in vacuum drying oven, and the bottom end of the hanging compression bar is equipped with predispersed fiber
Stick processed is respectively equipped with vacuum evacuation device in the vacuum drying oven and cooling chamber.
Further, the thermal insulation layer includes quartzy heat shield and the graphite heat shield that is arranged in above quartzy heat shield.
Further, the vacuum drying oven includes furnace shell, calandria, graphite Thiele tube, insulation quilt and is arranged in furnace shell
Can accommodate the quartz glass tube of preform, and from furnace shell to quartz glass tube direction set gradually insulation quilt, calandria and
Graphite Thiele tube.
Further, calandria is made of 2~6 groups of heaters in the vacuum drying oven, and gap is 20 between adjacent heater
~50mm, there are two temperature sensors, a temperature sensor to be used for monitoring temperature, another temperature for installation on every group of calandria
Sensor is for controlling temperature.
Further, graphite Thiele tube is spliced by 2~6 groups of graphite-pipes, and graphite-pipe is with a thickness of 4~8mm.
Further, it is equipped with metal pressure ring at the top of the thermal insulation layer, a screw sequentially passes through metal pressure ring and vacuum furnace roof
Portion, realization thermal insulation layer are fixedly connected with vacuum drying oven.
Further, polytetrafluoroethylene (PTFE) pad, the thermal insulation layer and vacuum drying oven are equipped between the thermal insulation layer and metal pressure ring
Between be equipped with perfluor O-ring, the diameter of section of perfluor O-ring is 6~12mm, and seal compression is the 1/4~1/ of diameter of section
2。
The present invention is described in detail combined with specific embodiments below.
Preform degasification furnace as shown in Fig. 1, device include vacuum drying oven 1, cooling chamber 2, fire door 3, hanging pressure
Bar 4, vacuum evacuation device 5, O-ring 6, graphite heat shield 8, quartzy heat shield 9, quartz hanging bar 10.
Attached vacuum drying oven shown in Fig. 2, device include quartz glass tube 101, calandria 102, graphite Thiele tube 103, protect
Warm felt 104, furnace shell 105, perfluor O-ring 106, polytetrafluoroethylene (PTFE) pad 107, metal pressure ring 108, screw 109.
Target degassing object is preform, diameter≤180mm, Qualified Length≤2500mm；Quartz glass tube 101
Length is 4000mm, internal diameter 260mm, and with a thickness of 5mm, top flange is with a thickness of 10mm, flange outer diameter 500mm；Graphite is equal
Heat pipe 103 is spliced by 5 sections of graphite-pipes, and soaking bore is 290mm, outer diameter 302mm, total a height of 3600mm after splicing；
Calandria 102 is made of 5 groups of cylindrical graphite calandrias, and single common heater height is 600mm, internal diameter 360mm, two heating
Body part spacing is 650mm, total a height of 3200mm of calandria 102；The thickness of insulation quilt 104 takes 120mm, is distributed in burner hearth four
Week, the outer diameter of burner hearth are 920mm, total height 4300mm；Quartzy heat shield 11 is with a thickness of 10mm, outer diameter 300mm, inner hole
50mm；Graphite heat shield outer diameter is 300mm, and with a thickness of 20mm, internal diameter 60mm, material is graphite felt.
The cavity heights of cooling chamber 2 are 5000mm, diameter 800mm；Hanging compression bar diameter is 50mm, the following length of flange
For 4800mm, material is SUS 316L, surface polishing treatment；Quartz hanging pole length be 800mm, diameter 45mm, upper end with
Compression bar is hung to connect using pin hole；O-ring 6 uses fluorubber material, and diameter 8mm sets sealing volume under pressure as 3mm.
After furnace body is installed, furnace body 1 is vacuumized using vacuum evacuation device 5, when absolute pressure is shown as 10Pa,
Valve is closed, pressure maintaining test is carried out to burner hearth, pressure maintaining 48 hours, pressure changing is checked, if there is larger raising, checks leakage
Point.Under light condition, fire door 3, decline hanging compression bar, until the decrement of O-ring 6 reaches 3mm or so, the good hanging of record are closed
The travel position S of compression bar is closed fire door 3, is vacuumized using vacuum evacuation device 5 to cooling chamber 2, absolute pressure is shown as
When 10Pa, valve is closed, pressure maintaining test is carried out to burner hearth, pressure maintaining 48 hours, checks pressure changing, if there is larger raising,
Then check leak source.By carrying out equipment debugging, N2 being filled with into vacuum drying oven after the leakage test of the above vacuum drying oven and cooling chamber,
It is vacuumized again, when pressure is shown as 50Pa, closes valve, keep negative pressure value in furnace.Calandria 102 be powered and is added
Heat is risen with the upper end position of calandria 102 and is surveyed using the axial temperature of external temperature thermocouple measurement quartz glass tube hub,
Measurement total length is 3200mm, is spaced 50mm, takes a point, record the temperature value of 65 points, checks the temperature of intermediate 56 points
Undulating value, adjustment controls temperature by the corresponding each temperature transducer of calandria 102, until the temperature fluctuation value of 56 points exists
1100 ± 5 DEG C, keep the temperature 48 hours, after cool to 700 DEG C.Fire door 3 is opened, is 160mm by diameter, effective length is
The preform of 2500mm is installed to quartz hanging 10 lower end of bar, and hanging compression bar 4 is dropped to position S, fire door is closed, opens
Vacuum evacuation device, until absolute pressure value reaches 50Pa, closing valve in cooling chamber.It waits 1 hour, then presses 50 DEG C/h
Speed be warming up to 1200 DEG C, kept for 6 hours, then cool to 700 DEG C with 50 DEG C/h of speed, kept for 2 hours, upper hanging
Compression bar 4200mm is hung, is kept for 2 hours, fire door is opened, takes out preform.The prefabricated rods are subjected to drawing optical fibers, can be obtained
To the optical fiber low, intensity is good of decaying.
Although above having used general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention are fallen within the scope of the claimed invention.
Claims (10)
1. a kind of degassing method of preform, which comprises the following steps:
Step 1: the quartz glass tube internal temperature of Raise vacuum furnace is to 600~900 DEG C；
Step 2: opening the fire door of cooling chamber, preform is installed on quartz hanging bar, decline hanging compression bar arrives, directly
It realizes and seals to O-ring, close fire door；
Step 3: vacuumized using vacuum evacuation device to cooling chamber, 1000 are warming up to 10~300 DEG C/h of speed~
1300 DEG C, keep 3~20 hours, with 10~300 DEG C/h of speed cool to 900 DEG C hereinafter, keep 0.5~3 hour, later
It hangs compression bar to rise, preform is cooling in cooling chamber.
2. the degassing method of preform according to claim 1, it is characterised in that: when degassing heating, heating rate≤
200 DEG C/h, when cooling, cooling rate≤200 DEG C/h.
3. the degassing method of preform according to claim 1, it is characterised in that: the absolute pressure control inside vacuum drying oven
System is in 5~100Pa, and in operation process, absolute pressure is controlled in 10~200Pa cooling chamber.
4. the device that one kind is applied to the degassing method of preform described in any one of claim 1-3, it is characterised in that:
Described device includes vacuum drying oven, the cooling chamber that vacuum furnace top is arranged in and hanging compression bar, between the vacuum drying oven and cooling chamber
Equipped with thermal insulation layer, the hanging compression bar sequentially passes through cooling chamber and thermal insulation layer enters in vacuum drying oven, the bottom of the hanging compression bar
End is equipped with preform, is respectively equipped with vacuum evacuation device in the vacuum drying oven and cooling chamber.
5. device according to claim 4, it is characterised in that: the thermal insulation layer includes quartzy heat shield and is arranged in quartz
Graphite heat shield above heat shield.
6. device according to claim 4, it is characterised in that: the vacuum drying oven includes furnace shell, calandria, graphite soaking
Insulation quilt and the quartz glass tube that can accommodate preform is arranged in furnace shell in pipe, and from furnace shell to quartz glass tube side
To setting gradually insulation quilt, calandria and graphite Thiele tube.
7. device according to claim 6, it is characterised in that: calandria is by 2~6 groups of heater groups in the vacuum drying oven
At gap is 20~50mm between adjacent heater, and there are two temperature sensor, a temperature sensing for installation on every group of calandria
Device is used for monitoring temperature, another temperature sensor is for controlling temperature.
8. device according to claim 6, it is characterised in that: graphite Thiele tube is spliced by 2~6 groups of graphite-pipes, stone
Black tube thickness is 4~8mm.
9. device according to claim 4, it is characterised in that: be equipped with metal pressure ring at the top of the thermal insulation layer, a screw according to
Secondary to pass through metal pressure ring and vacuum furnace top, realization thermal insulation layer is fixedly connected with vacuum drying oven.
10. device according to claim 9, it is characterised in that: be equipped with polytetrafluoro between the thermal insulation layer and metal pressure ring
Ethylene pad, is equipped with perfluor O-ring between the thermal insulation layer and vacuum drying oven, the diameter of section of perfluor O-ring is 6~12mm, sealing
Decrement is the 1/4~1/2 of diameter of section.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811353111.5A CN109264985B (en) | 2018-11-14 | 2018-11-14 | Degassing method and device for optical fiber preform |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811353111.5A CN109264985B (en) | 2018-11-14 | 2018-11-14 | Degassing method and device for optical fiber preform |
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| CN109264985A true CN109264985A (en) | 2019-01-25 |
| CN109264985B CN109264985B (en) | 2023-09-22 |
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Cited By (5)
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| CN110885184A (en) * | 2019-10-25 | 2020-03-17 | 烽火通信科技股份有限公司 | Common-rail optical fiber drawing device and drawing method thereof |
| CN111186999A (en) * | 2020-02-18 | 2020-05-22 | 通鼎互联信息股份有限公司 | Vacuum wire drawing furnace for manufacturing optical fiber |
| CN113248131A (en) * | 2021-05-31 | 2021-08-13 | 中天科技精密材料有限公司 | Optical fiber preform, and apparatus and method for manufacturing the same |
| CN113277728A (en) * | 2021-07-01 | 2021-08-20 | 中国计量大学 | Optical fiber drawing furnace suitable for fluoride glass |
| CN115947537A (en) * | 2022-12-24 | 2023-04-11 | 藤仓烽火光电材料科技有限公司 | Surface treatment device and surface treatment method for quartz core rod |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113248131A (en) * | 2021-05-31 | 2021-08-13 | 中天科技精密材料有限公司 | Optical fiber preform, and apparatus and method for manufacturing the same |
| CN113248131B (en) * | 2021-05-31 | 2021-09-17 | 中天科技精密材料有限公司 | Optical fiber preform, and apparatus and method for manufacturing the same |
| CN113277728A (en) * | 2021-07-01 | 2021-08-20 | 中国计量大学 | Optical fiber drawing furnace suitable for fluoride glass |
| CN115947537A (en) * | 2022-12-24 | 2023-04-11 | 藤仓烽火光电材料科技有限公司 | Surface treatment device and surface treatment method for quartz core rod |
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| Publication number | Publication date |
|---|---|
| CN109264985B (en) | 2023-09-22 |
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