CN106007359B - A kind of preparation method of preform - Google Patents
A kind of preparation method of preform Download PDFInfo
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- CN106007359B CN106007359B CN201610580287.9A CN201610580287A CN106007359B CN 106007359 B CN106007359 B CN 106007359B CN 201610580287 A CN201610580287 A CN 201610580287A CN 106007359 B CN106007359 B CN 106007359B
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- alkali metal
- preparation
- major diameter
- bushing pipe
- glass tube
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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
- C03B37/01807—Reactant delivery systems, e.g. reactant deposition burners
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General 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)
- Manufacture, Treatment Of Glass Fibers (AREA)
Abstract
The invention discloses a kind of preparation methods of preform, the sandwich layer and part of clad of preform are prepared by gas-phase deposition in pipe, it is characterized in that the inlet end in glass bushing pipe concatenates a major diameter glass tube, alkali metal source is placed in the major diameter glass tube；Having heaters is arranged in major diameter glass tube periphery；When depositing covering, heater is closed, coverstock gas, which enters in glass bushing pipe and deposits, forms covering；When deposition of core layer, heater, core layer raw material gas, which is carried, forms sandwich layer since the evaporated alkali metal source of heating enters in glass bushing pipe together and deposits.Alkali-metal-doped is carried out during plug deposition in the present invention, and alkali metal content is more evenly distributed, and can overcome the problems, such as that diffusion method alkali metal is unevenly distributed in glass tube, can be substantially reduced optical fiber attenuation.
Description
Technical field
The present invention relates to a kind of preparation methods of preform, belong to technical field of optical fiber communication.
Background technique
Fiber optic communication has the characteristics that big transmission capacity, long transmission distance, transmission speed are fast, is widely used in long distance line
The optical communication networks such as net, Metropolitan Area Network (MAN) and access net.Reducing fiber attenuation coefficient can effectively improve the biography of optical fiber telecommunications system
Defeated distance greatly reduces the quantity and cost of relay station, to optimization Transmission system structure and cuts operating costs with important meaning
Justice.How to reduce fiber attenuation coefficient becomes the hot spot that major optical fiber manufacturer is competitively studied.
The existing technology for reducing fiber attenuation coefficient is mainly the following：1. viscosity matching and matched coefficients of thermal expansion.
Optimize fibre profile design and material component, improves the viscosity matching and matched coefficients of thermal expansion of material, reduce wire drawing stress and make
At optical fiber attenuation.2. reducing the concentration of sandwich layer dopant.The reduction of the concentration of sandwich layer dopant germanium or fluorine can reduce concentration
Rayleigh scattering loss caused by the factor is fluctuated, for example, generalling use pure silicon core technology at present to reduce the Ge-doped amount of sandwich layer, is manufactured
Ultralow attenuating fiber.3. doped alkali metal or chlorine element.Alkali metal or chlorine element can reduce glass viscosity and virtual temperature
Degree, to reduce Rayleigh scattering loss caused by the density fluctuation factor.
Alkali-metal-doped technology has been demonstrated experimentally the decaying that can be effectively reduced optical fiber, especially applies in ultralow decaying
It in the preparation of optical fiber, can play the role of making something perfect even more perfect, be forward position and the hot spot of current optical fiber manufacturing technology field research.
Document US7088900B1 proposes that a kind of low attenuation optical fiber of alkali metal containing, alkali metal content are not less than 20ppm
Wt%, decaying of the optical fiber at 1550nm wavelength be lower than 0.178dB/km, text in without reference to incorporation alkali metal method.Document
US7524780B2, US20050063663A1 and US7469559B2 are put into alkali metal source in glass inside pipe wall, pass through pipe
Interior diffusion method incorporation alkali metal is to improve optical fiber attenuation.Document US9250386B2 is put into alkali metal source in glass inside pipe wall,
The heating of glass pipe outer wall mixes alkali metal oxide by diffusion in glass, and obtained optical fiber is at 1550nm wavelength
Decaying can achieve 0.17dB/km hereinafter, it is this heating diffusion method incorporation alkali metal glass inside and outside wall formed concentration gradient,
It is unevenly distributed.Document US20140127507A1, US9229160B2, CN102627400B, CN102603179A,
CN102627398A, CN103502164A, CN104093674A, CN102617033A, CN103502164A and
CN102730977A, by the alkali metal source in the heat source heatable glass tube of continuous moving, by being diffused in glass tube
Wall mixes alkali metal, and doping process is complicated.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of predispersed fiber in view of the deficiency of the prior art
The preparation method of stick processed, not only simple process is controllable for it, but also the alkali metal content mixed in prepared prefabricated rods and optical fiber
It is evenly distributed, can obviously reduce optical fiber attenuation.
The present invention be solve the problems, such as it is set forth above used by technical solution be：
A kind of preparation method of preform prepares preform, including deposition using gas-phase deposition in pipe
Part of clad and sandwich layer, it is characterised in that concatenate a major diameter glass tube in the inlet end of glass bushing pipe, alkali metal source is placed in
In the major diameter glass tube；Having heaters is arranged in major diameter glass tube periphery；When depositing covering, heater, packet are closed
Layer unstrpped gas, which enters in glass bushing pipe and deposits, forms covering；When deposition of core layer, heater, core layer raw material gas is carried
The heated alkali metal source volatilized, which enters in glass bushing pipe together and is deposited into, mixes alkali sandwich layer.
According to the above scheme, vapour deposition process includes plasma chemical vapor deposition (PCVD), improvedization in the pipe
Learn vapor deposition (MCVD) and other methods that deposition prepares preform in glass bushing pipe.
According to the above scheme, the internal diameter of the major diameter glass tube is greater than the internal diameter of glass bushing pipe；The major diameter glass
Pipe both ends are communicated with inlet-end manifold and the welding of glass bushing pipe respectively, and recessed with one sagging annular of glass lined inner tube layer formation
Slot.
According to the above scheme, the glass bushing pipe is the quartz glass tube with certain outer diameter, internal diameter, wall thickness and length,
Base tube for being vapor-deposited in pipe.
According to the above scheme, the alkali metal source is alkali halide, i.e., is made of alkali metal element and halogen
Compound.Wherein, alkali metal element includes Li, Na, K, Rb, Cs；Halogen includes F, Cl, Br, I, At；Alkali halide is alkali
Any combination in metallic element and halogen, such as KCl, NaCl, KBr, NaBr etc., but it is not limited to these four.
According to the above scheme, the alkali metal source can also be containing Li, Na, K, Rb, the alkali metal elements such as Cs its
His compound, such as Na2CO3, KNO3, Na2SO3Etc..
According to the above scheme, the purity of the alkali metal source is preferably powdered greater than 99.9%.
According to the above scheme, the additive amount of alkali metal source is 1-500g in the major diameter glass tube.Preferably, big straight
Lower edge line of the height no more than glass bushing pipe of alkali metal source is held in diameter glass tube.
According to the above scheme, the heater is heating furnace or flame, and heating furnace can be resistance furnace or induction furnace.Its
In, heating furnace is heated from the side of major diameter glass tube, is either encased or is partly encased and is heated；Flame can be hydrogen
The flame of the other fuel combustions of oxygen flame the latter.
According to the above scheme, the temperature that the heater provides is 500-1000 DEG C.
According to the above scheme, the coverstock gas mainly includes SiCl4And O2, can also include GeCl4、SF6、CF4With
C2F6Deng；The core layer raw material gas mainly includes SiCl4、GeCl4And O2, can also include SF6、CF4And C2F6Deng.
According to the above scheme, the sandwich layer refers to that prefabricated rods center corresponds to the area within fiber optic hub diameter 8-12um or so
Domain.
According to the above scheme, the covering refers to that prefabricated rods center corresponds to the region other than fibre diameter 8-12um or so.
According to the above scheme, alkali metal weight content is 5-2000ppm in the resulting prefabricated rods of the present invention and optical fiber.
According to the above scheme, the resulting prefabricated rods drawing optic fibre of the present invention, optical fiber decay to 0.165- at 1550nm
0.175dB/km；Preferably, optical fiber decays to 0.160-0.165dB/km at 1550nm；It is highly preferred that optical fiber exists
0.150-0.160dB/km is decayed at 1550nm.
Compared with prior art, the beneficial effects of the invention are as follows：
1. alkali-metal-doped is carried out during plug sandwich layer deposition in the present invention, alkali metal content distribution is more equal
It is even, it can overcome the problems, such as that diffusion method alkali metal is unevenly distributed in glass tube, can be substantially reduced optical fiber attenuation.
2. the present invention is dopeded alkali metal on one side deposit while during plug sandwich layer deposition, plug deposit alkali afterwards
Metal-doped is to complete, not extra consumption doping time, it is possible to reduce equipment use cost.
Detailed description of the invention
Fig. 1 is the schematic diagram that PCVD deposition process mixes alkali metal in embodiment 1.Wherein, 11 be glass bushing pipe, and 12 be Sheng
The major diameter glass tube of alkali metal source is put, 13 be alkali metal source, and 14 be heater, and 15 be holding furnace, and 16 be resonant cavity.
Fig. 2 is the schematic diagram that MCVD deposition process mixes alkali metal in embodiment 2.Wherein, 21 be glass bushing pipe, and 22 be Sheng
The major diameter glass tube of alkali metal source is put, 23 be alkali metal source, and 24 be heater, and 25 be blowtorch.
Fig. 3 is the present invention compared with alkali metal content is distributed in preform prepared by glass tube heating diffusion method
Figure.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment and attached drawing content that the present invention is furture elucidated, but this
Invention is not limited solely to the following examples.
Embodiment 1
As shown in Figure 1, manufacturing preform by PCVD depositing operation, holding furnace 15 is anti-by the deposition of glass bushing pipe 11
Region is answered to surround, resonant cavity 16 can be moved left and right in 11 periphery of glass bushing pipe, be given between holding furnace 15 and glass bushing pipe 11
Deposition reaction region provides heat source；A major diameter glass tube 12, the major diameter glass are concatenated in the inlet end of glass bushing pipe 11
12 both ends of pipe are communicated with inlet-end manifold and the welding of glass bushing pipe 11 respectively, and are installed one in 12 outside of major diameter glass tube and added
Hot device 14；The internal diameter of major diameter glass tube 12 is greater than the internal diameter of glass bushing pipe 11.
Using device as described in Figure 1, the preparation method of preform, its step are as follows：
1) 5-50g alkali metal source KBr13 is contained in major diameter glass tube 12；
2) plug covering deposits：Heater 14 is closed, the inlet end of glass bushing pipe 11 leads to coverstock gas, coverstock
Gas SiCl4(flow 875sccm) and O2(flow 2750sccm) further includes GeCl4(flow is 0~10sccm) and C2F6
(flow is 27~53sccm) deposition in glass bushing pipe 11 forms covering, and then covering continues after having deposited in covering inner wall
Deposition of core layer；
3) plug sandwich layer deposits：The inlet end for having deposited the glass bushing pipe 11 of covering is passed through core layer raw material gas SiCl4(stream
Amount is 800sccm), GeCl4(flow is 0~10sccm) and O2(flow 2700sccm) further includes C2F6(1~3sccm),
It opens heater 14 to heat to major diameter glass tube 12, heter temperature is set as 700-800 DEG C, and alkali metal source is due to heating
Gaseous state is formed, and is brought into glass bushing pipe 11 by gas carrier of core layer raw material gas in the covering that glass bushing pipe 11 is deposited
Continue deposition on inner wall and form sandwich layer, mixes alkali metal while the deposition of sandwich layer；
4) after covering, sandwich layer deposition, collapsing is carried out by high-temperature heating in collapsing lathe and obtains solid plug, it will
This plug combines resulting prefabricated rods with outer tube and carries out wire drawing, and alkali metal content is 25-2000ppm (with weight in gained optical fiber
Measure content meter), optical fiber decays to 0.150-0.175dB/km at 1550nm.
In the present embodiment when alkali metal source doping process parameter difference, obtained prefabricated rods carry out wire drawing preparation respectively
Optical fiber, gained optical fiber carry out attenuation test and constituent content test, and acquired results are as shown in table 1.
1 alkali-metal-doped technological parameter of table and gained test optical fiber result
Embodiment 2
As shown in Fig. 2, manufacturing preform by MCVD depositing operation, blowtorch 25 can be moved along glass bushing pipe 21 or so
It is dynamic, heat source is provided to deposition reaction region；A major diameter glass tube 22, the major diameter are concatenated in the inlet end of glass bushing pipe 21
22 both ends of glass tube are communicated with inlet-end manifold and the welding of glass bushing pipe 21 respectively, and install one in 22 outside of major diameter glass tube
A heater 24；The internal diameter of major diameter glass tube 22 is greater than the internal diameter of glass bushing pipe 21.
Using device as described in Figure 2, the preparation method of preform, its step are as follows：
1) 5-50g alkali metal source NaBr23 is contained in major diameter glass tube 22；
2) plug covering deposits：Heater 24 is closed, the inlet end of glass bushing pipe 21 leads to coverstock gas, coverstock
Gas SiCl4(flow 420sccm) and O2(flow 1300sccm) further includes GeCl4(flow is 0~10sccm) and C2F6
(flow deposits in glass bushing pipe 21 for 13~26sccm and forms covering；
3) plug sandwich layer deposits：The inlet end of glass bushing pipe 21 is passed through core layer raw material gas SiCl4(flow is
400sccm)、GeCl4(flow is 0~10sccm) and O2(flow 1200sccm) further includes C2F6(1~3sccm) is opened
Heater 24 is heated to major diameter glass tube 22, and heter temperature is set as 700-800 DEG C, and alkali metal source is due to being thermally formed
Gaseous state, and the deposition in glass bushing pipe 21 is brought into glass bushing pipe 21 as gas carrier using core layer raw material gas and forms sandwich layer,
Alkali metal is mixed while the deposition of sandwich layer；
4) after covering, sandwich layer deposition, collapsing is carried out by high-temperature heating in collapsing lathe and obtains solid plug, it will
This plug combines resulting prefabricated rods with outer tube and carries out wire drawing, and alkali metal content is 20-2000ppm (with weight in gained optical fiber
Measure content meter), optical fiber decays to 0.150-0.175dB/km at 1550nm.
In the present embodiment when alkali metal source doping process parameter difference, obtained prefabricated rods carry out wire drawing preparation respectively
Optical fiber, gained optical fiber carry out attenuation test and constituent content test, and acquired results are as shown in table 2.
2 alkali-metal-doped technological parameter of table and gained test optical fiber result
Control test
With the alkali metal of the incorporation same amount of the heart in a fiber, (such as K, fiber optic hub alkali metal weight content are 20-
For 200ppm), the alkali metal content of optical fiber center is identical, the present invention and glass tube heating diffusion method acquired results such as Fig. 3
(using the alkali metal element content of electron probe microanalysis (EPMA) measurement fiber core layer) compares the present invention and expands with glass tube heating
Distribution situation of the alkali metal content along optical fiber radial direction in arching pushing.As shown in Figure 3：The alkali gold of glass tube heating diffusion method incorporation
Belong to and form concentration gradient in glass inside and outside wall, causes alkali metal in optical fiber radially to gradually decrease, be unevenly distributed, and it is of the invention
Alkali metal is mixed in sandwich layer deposition process using sedimentation, alkali metal is radially distributed uniformly in gained optical fiber.
The above is only a preferred embodiment of the present invention, it is noted that come for those of ordinary skill in the art
It says, without departing from the concept of the premise of the invention, several modifications and variations can also be made, these belong to of the invention
Protection scope.
Claims (10)
1. a kind of preparation method of preform prepares preform, including deposition core using gas-phase deposition in pipe
Layer and part of clad, it is characterised in that concatenate a major diameter glass tube in the inlet end of glass bushing pipe, alkali metal source is placed at
In the major diameter glass tube；Having heaters is arranged in major diameter glass tube periphery；When depositing covering, heater, covering are closed
Unstrpped gas, which enters in glass bushing pipe and deposits, forms covering；When deposition of core layer, heater, core layer raw material gas carries warp
The alkali metal source of heating volatilization, which enters in glass bushing pipe together and is deposited into, mixes alkali sandwich layer.
2. a kind of preparation method of preform according to claim 1, it is characterised in that the major diameter glass
The internal diameter of pipe is greater than the internal diameter of glass bushing pipe；Phase is welded with inlet-end manifold and glass bushing pipe respectively in major diameter glass tube both ends
It is logical.
3. a kind of preparation method of preform according to claim 1, it is characterised in that the alkali metal source
For alkali halide.
4. a kind of preparation method of preform according to claim 1, it is characterised in that the alkali metal source
To contain Li, Na, K, Rb, the substance of one or more of Cs element.
5. a kind of preparation method of preform according to claim 1, it is characterised in that the alkali metal source
Purity be greater than 99.9%.
6. a kind of preparation method of preform according to claim 1, it is characterised in that the major diameter glass
The additive amount of alkali metal source is 1-500g in managing.
7. a kind of preparation method of preform according to claim 1, it is characterised in that gas phase is heavy in the pipe
Area method includes that plasma chemical vapor deposition, improved chemical vapor deposition and other depositions in glass bushing pipe prepare optical fiber
The method of prefabricated rods.
8. a kind of preparation method of preform according to claim 1, it is characterised in that the heater is to add
Hot stove or flame.
9. a kind of preparation method of preform according to claim 1, it is characterised in that the heater provides
Temperature be 500-1000 DEG C.
10. a kind of preparation method of preform according to claim 1, it is characterised in that the coverstock gas
It mainly include SiCl4And O2；The core layer raw material gas mainly includes SiCl4、GeCl4And O2。
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| CN106007359B true CN106007359B (en) | 2018-11-23 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107162401B (en) * | 2017-05-31 | 2019-11-26 | 长飞光纤光缆股份有限公司 | A method of preparing ultralow attenuating fiber |
| CN107032595B (en) * | 2017-05-31 | 2020-10-30 | 长飞光纤光缆股份有限公司 | Preparation method and device for optical fiber preform rod by doping alkali metal |
| CN111847867B (en) * | 2020-07-21 | 2022-06-14 | 复旦大学 | Optical fiber preform and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20060130530A1 (en) * | 2004-12-21 | 2006-06-22 | Anderson James G | Method of doping silica glass with an alkali metal, and optical fiber precursor formed therefrom |
| EP2952490A4 (en) * | 2013-02-04 | 2016-10-05 | Sumitomo Electric Industries | Optical-fiber preform and method for manufacturing optical-fiber preform |
| CN103193398B (en) * | 2013-04-28 | 2016-11-16 | 成都富通光通信技术有限公司 | A kind of preparation method of high-speed wire-drawing formed high-temperature resistant optical fiber |
| CN103992030A (en) * | 2014-02-18 | 2014-08-20 | 长飞光纤光缆股份有限公司 | Preparation method for rare earth doped optical fiber prefabricated bar |
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