CN205803319U - A kind of equipment of the ultra-low-loss fiber prefabricated rods preparing pure silicon core covering fluorine doped - Google Patents
A kind of equipment of the ultra-low-loss fiber prefabricated rods preparing pure silicon core covering fluorine doped Download PDFInfo
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- CN205803319U CN205803319U CN201620461105.1U CN201620461105U CN205803319U CN 205803319 U CN205803319 U CN 205803319U CN 201620461105 U CN201620461105 U CN 201620461105U CN 205803319 U CN205803319 U CN 205803319U
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Abstract
The equipment of a kind of ultra-low-loss fiber prefabricated rods preparing pure silicon core covering fluorine doped of this utility model refers to a kind of body of powder using vapour deposition process to obtain, and carries out fluorine doped to prepare the equipment of the ultra-low-loss fiber prefabricated rods of pure silicon core covering fluorine doped in covering.Described equipment includes target rod, settling chamber, surrounding layer blowtorch, middle covering blowtorch, auxiliary blowtorch, sandwich layer blowtorch, suspension rod, exhaustor, overburden cavity and graphite heating resistance furnace；Top, settling chamber is provided with overburden cavity, overburden cavity is built with suspension rod, suspension rod is provided with hook, suspension rod is connected with hoisting mechanism, target rod is suspended on the hook of the suspension rod being connected with hoisting mechanism, is sequentially arranged with surrounding layer blowtorch, middle covering blowtorch, auxiliary blowtorch, sandwich layer blowtorch in side, bottom, settling chamber；Graphite sintering stove includes quartz suspension rod, black box, cover plate, quartz furnace core tube, graphite furnace core tube, gas piping, target rod, body of powder, graphite heating body and gas mass flow controller.
Description
Technical field
The equipment of a kind of ultra-low-loss fiber prefabricated rods preparing pure silicon core covering fluorine doped of this utility model refers to one
Plant the body of powder using vapour deposition process to obtain, covering carries out fluorine doped to prepare the ultra-low loss light of pure silicon core covering fluorine doped
The equipment of fine prefabricated rods.
Background technology
Preform is the raw material of fiber manufacturing, and it is typically to be formed sandwich layer and bag by the material of different refractivity
Layer.Silicon dioxide is the major matrix material manufacturing preform, improves the refractive index of sandwich layer by mixing germanium at sandwich layern core So that core refractive rate is more than pure silicon cladding indexn siO2 , thus meet the total reflection condition of fiber-optic transfer, i.e. reach
Certain core bag refractive index contrast Δn。
Δn =n core ^2-n siO2 ^2/2n core ^2≈n core -n siO2 /n core
Along with fiber to the home, the integration of three networks, IPTV service increase, the demand of the network bandwidth is also grown with each passing day.At present,
For optical fiber, bandwidth can be improved by reducing fibre loss, namely mix germanium by reduction sandwich layer and reduce Rayleigh scattering, with
Time, also need the anti-bending strength improving optical fiber to meet optical fiber installation in narrow and small environment.If simply reducing sandwich layer doping to contain
Amount cannot realize the Δ n value needed for fiber-optic transfer and the anti-bending strength of optical fiber.Therefore, ultra-low-loss fiber prefabricated rods is being manufactured
Time, typically take the method that pure silicon core combines covering fluorine doped, it is achieved with the common Δ that G.652 optical fiber is identicalnValue.For ultralow
Loss optical fiber prefabricated rods relative index of refraction is Δn=Δn + +Δn - , wherein Δn + =0(sandwich layer is pure silicon core), it is,
Δn =Δn - =n clad ^2-n siO2 ^2/2n clad ^2≈n clad -n siO2 /n clad
More effective method is incorporation fluorine element in body of powder at present, such as, utilize gas in prefabricated rods manufacture process
Phase sedimentation (VAD, OVD, MCVD, PCVD) etc. makes fluoro-gas mix in barred body.Manage outer method (VAD, OVD) not limited by size
Making, deposition efficiency is high, can be applicable in large-scale optical fiber prefabricating stick manufacture, but is fluorinated containing of gaseous state by flame hydrolysis
Compound joins in quartz glass, due to by the fluorine dividing potential drop around flame temperature, silica dioxide granule and OH-Cause etc. factor
Fluorine doped concentration is low, it is impossible to realizes efficient fluorine doped and produces.Manage interior method (PCVD, MCVD) although efficient fluorine-doped can be realized to be produced,
But by base tube size limitation, it is impossible to accomplish scale production or prepare large scale fluorine-doped optical fiber preform rod or sleeve pipe.For this
A little problems, patent CN104402213 discloses the silicon dioxide using axial vapor deposition preparation to have compacted zone and weaker zone
Loose media, and by being passed through dehydrated air and fluoride gas, by loose media dehydration and fluorine is incorporated in weaker zone.Patent
CN103224325 discloses the loose media in body of powder with gap structure, it may have compacted zone and weaker zone structure, and in
Be passed through in central hole dehydrated air and in fluoride atmosphere fluorine doped.Patent CN1345295 discloses the powder with hollow structure
Body, helium injection in central axis space, carry out fluorine doped in fluoro-gas is passed through from bottom to top sintering furnace.But in actual production
In, owing to there is this structure of compacted zone, if density is big, then it is unfavorable for that loose media is dehydrated, causes optical fiber water peak height；If density
Little, the fluorine element of incorporation still penetrates into sandwich layer, is unfavorable for being formed the refractive index profile of step change type.If in the fabrication process will
Pure silicon core plug and mix F covering sleeve pipe be fabricated separately, the step such as collapsing again, also considerably increase the complexity of process.
Summary of the invention
This utility model purpose is for above-mentioned weak point, it is provided that a kind of ultra-low loss preparing pure silicon core covering fluorine doped
The equipment of preform, is that a kind of body of powder fluorine doped using vapour deposition process to prepare prepares ultra-low-loss fiber prefabricated rods
Equipment.The fluoride wherein used, comprises element F in its molecule, diffuse into body of powder in pyroprocess.Deposited powder body
Core layer raw material is Silicon chloride., oxygen, carbon monoxide, helium, and the raw material of deposition fluorine doped inner cladding is Silicon chloride., oxygen and one
The gases such as carbonoxide, the raw material of deposition fluorine doped surrounding layer is Silicon chloride., oxygen and the gas such as hydrogen or methane.By axial gas
Phase depositing operation, carries out deposition of core layer and interior surrounding layer, forms silicon dioxide powder opisthosoma.By deposition between sandwich layer and covering
Middle auxiliary blowtorch heats, and makes core layer surface vitrification.Then body of powder is positioned in high temperature furnace, carries out fluorine doped, glass chemical industry
Skill, finally realizes ultra-low-loss fiber prefabricated rods high-purity, efficient and produces, due to without Powder Rod is carried out deshydroxy process, this
Sample is greatly simplified production procedure, for manufacturing the ultra-low-loss fiber prefabricated rods of large scale covering fluorine doped, it is provided that a kind of operation letter
Single, the new way of energy-saving practical.
The equipment of a kind of ultra-low-loss fiber prefabricated rods preparing pure silicon core covering fluorine doped is to take techniques below scheme real
Existing:
The equipment of a kind of ultra-low-loss fiber prefabricated rods preparing pure silicon core covering fluorine doped includes target rod, settling chamber, outsourcing
Layer blowtorch, middle covering blowtorch, auxiliary blowtorch, sandwich layer blowtorch, suspension rod, exhaustor, overburden cavity and graphite heating resistance furnace.
Top, settling chamber is provided with overburden cavity, and overburden cavity is built with suspension rod, and suspension rod is provided with hook, suspension rod and lifting
Mechanism is connected, and target rod is suspended on the hook of the suspension rod being connected with hoisting mechanism, is sequentially arranged with outsourcing in side, bottom, settling chamber
Layer blowtorch, middle covering blowtorch, auxiliary blowtorch, sandwich layer blowtorch, be provided with exhaustor in side, top, settling chamber, be used for getting rid of deposition
Indoor exhaust air.
Graphite sintering stove include quartz suspension rod, black box, cover plate, quartz furnace core tube, graphite furnace core tube, gas piping,
Target rod, body of powder, graphite heating body, gas mass flow controller.Body of powder is connected with quartz suspension rod by target rod, sintering
During, quartz suspension rod can move up and down, and rotation.Gas mass flow controller is installed on gas piping.Mixing F sintering
During, gas mass flow controller control He and fluorochemical gaseous mixture, be passed through the gas piping of quartz furnace core tube
It is positioned at graphite heating body upper zone.Body of powder is placed in quartz furnace core tube, from top to bottom by being produced by graphite heating body
High-temperature region.Quartz furnace core tube is in graphite furnace core tube, and graphite heating body is centered around outside graphite furnace core tube.Sealed by cover plate
Quartz furnace core tube, quartz suspension rod, through black box, arranges 4 layers of isolation, by black box gas tube in every layer in black box
Road is passed through N2Carry out sealing gland.
The method preparing the ultra-low-loss fiber prefabricated rods of pure silicon core covering fluorine doped, first selects the target of a glass material
Rod, by the chlorohydric acid pickling 1 ~ 2h of 10%, and is dried.Target rod is suspended on the suspension rod hook being connected with hoisting mechanism, uses
VAD technique carries out the SiO 2 powder of axial vapor deposition, sandwich layer and covering and is deposited in target rod.By using monitor to visit
Head sensing caput, according to the scope of sensing caput, is controlled suspension rod by electric-control system PLC method and promotes speed.When caput exists
During the induction region set, system promotes suspension rod accordingly；After once deposition caput departs from induction zone, chuck stops promoting.So,
Go round and begin again, the most gradually deposit, form the body of powder of axial deposition.
In deposition process, sandwich layer blowtorch is passed through oxygen, carbon monoxide, Silicon chloride., helium and nitrogen mixture, tetrachloro
SiClx forms silicon dioxide with oxygen by pyroreaction, and is attached to target rod end face, forms the weaker zone with certain density.
Be centered around core layer surface having certain thickness silicon dioxide layer is inner cladding, inner cladding blowtorch is passed through oxygen, carbon monoxide,
Silicon chloride. and nitrogen mixed gas.Be centered around the silicon dioxide layer on inner cladding surface be by inner cladding blowtorch above surrounding layer
Blowtorch deposition is formed, and is passed through oxygen, hydrogen or methane, Silicon chloride. and nitrogen in surrounding layer blowtorch.It is positioned at sandwich layer blowtorch
And between inner cladding blowtorch, have the most angled multiple auxiliary blowtorch, blowtorch is passed through oxygen, carbon monoxide carries out calcination
Core layer surface, thus form certain thickness dense glass layer in core layer surface.Body of powder stops after depositing to preseting length
Deposition, unloads body of powder from VAD chuck, in transfer to transport establishment.
By prepared body of powder from transport establishment again transfer on the suspension rod of graphite sintering stove, carry out powder bed fluorine doped,
Vitrification.First, body of powder fluorine doped at 1100 ~ 1200 DEG C, fluorine doped time 2 ~ 5h, it is passed through fluoro-gas, helium, argon mixing
Gas；Carry out vitrification sintering, 8 ~ 20h at 1300 ~ 1500 DEG C, be passed through helium, argon mixed gas.After terminating,
Obtain transparent bubble-free pure silicon core, the ultra-low-loss fiber prefabricated rods of fluorine doped covering.
Wherein, described auxiliary blowtorch quantity can 2 ~ 5, be dispersed in and be perpendicular in axial same plane.The powder of deposition
Opisthosoma, inner cladding thickness is 4.5 ~ 6.5 with the ratio of core layer thickness, and surrounding layer thickness is 7.5 ~ 15.5 with the ratio of core layer thickness.
The chemical reaction occurred in sandwich layer, inner cladding, surrounding layer blowtorch is as follows:
CO(g)+O2(g)→CO2(g), △ H=-283.0kJ/moL
H2(g)+O2(g)→H2O (g), △ H=-243.0kJ/moL
H2O(g)→H2O (l), △ H=-42.0kJ/moL
SiCl4(l)+O2(g)→SiO2(s)+Cl2(g), △ H=1052kJ/moL
A kind of method of ultra-low-loss fiber prefabricated rods preparing pure silicon core covering fluorine doped is as follows:
1, target rod pretreatment
Select the material of quartz glass material as deposition target rod.The target rod of selection is carried out pickling, uses 10% concentration
Soak with hydrochloric acid 1h ~ 2h, removes the impurity being attached to target rod surface, then repeatedly rinses with deionized water, finally dry.
2, the preparation of the ultra-low-loss fiber prefabricated rods of pure silicon core covering fluorine doped
The first step: pretreated target rod is clamped on the suspension rod hook of VAD equipment, with Silicon chloride., oxygen, an oxygen
Change carbon, helium are with nitrogen mixture as unstrpped gas, and the flow proportional of various unstrpped gases is 1:1.5:1:1:0.3 ~ 1:3:
3:1:0.5, after being passed through the sandwich layer blowtorch of quartz material, the raw material silicon dioxide microparticle that pyroreaction generates in flame, deposition
To the target rod surface vertical with blowtorch.According to caput position in induction zone, gradually promote suspension rod, form the powder of axial distribution
Opisthosoma.In corresponding auxiliary blowtorch, being passed through carbon monoxide, oxygen, ratio is 2:1 ~ 1:2.In above auxiliary blowtorch
In covering blowtorch, Silicon chloride., oxygen, carbon monoxide and the nitrogen being passed through, its flow proportional is 1:1:1:0.3 ~ 1.5:1:2:
0.3.In the surrounding layer blowtorch of the top, Silicon chloride., oxygen, hydrogen (or methane) and the nitrogen being passed through, its flow proportional is
1:1:1:0.5~3:1:3:1
Second step: silicon dioxide powder opisthosoma deposition obtained is placed in graphite heating resistance furnace.By furnace core tube and quartz
Bell is fitted, and uses the black box between oil-sealing measures sealed sintering stove cover plate and suspension rod and cover plate.Then, suspension rod rotates speed
Degree is 3r/min ~ 15r/min.Being passed through Ar, fluoride, He mixed gas, wherein fluoride is CF4、C2F6、C3F8、SF6、
SiF4、C2F2Cl2、SOF2One of which or two or more combinations, gas flow ratio is 0.2:4:2 ~ 0.4:15:3, sinters furnace temperature
Degree is stable at 1100 DEG C ~ 1200 DEG C, and logical fluorine time 2h ~ 5h, Powder Rod from top to bottom passes through the thermal treatment zone.After logical fluorine terminates, again
Being passed through He, Ar mixed gas and carry out vitrification, gas flow ratio is 2:1 ~ 10:1, and sintering furnace temperature stabilization is 1300 DEG C ~ 1500
DEG C, constant temperature 8h ~ 20h, Powder Rod is the most from top to bottom by the thermal treatment zone, after vitrification terminates, closes source of the gas.By logical fluorine, glass
After glass, can obtain transparent, hydroxy radical content is low, the ultra-low-loss fiber prefabricated rod cladding fluorine doped of pure silicon core covering fluorine doped pure
Silicon core ultra-low-loss fiber prefabricated rods.
This utility model compared with prior art technical characterstic is:
1. the equipment of the ultra-low-loss fiber prefabricated rods that this utility model prepares pure silicon core covering fluorine doped use VAD one
Formula depositing operation prepares the preform of multiple structure, and it comprises sandwich layer, compacted zone, inner cladding and surrounding layer.At sandwich layer, interior
The raw material being passed through non-hydrogen-containing compound in covering reacts, it is to avoid hydroxyl produces；Surrounding layer is passed through hydrogen-containing compound with
Silicon chloride. reacts, and is greatly improved deposition efficiency, it is achieved the cored needed for integral type deposition compares structure.
2. between sandwich layer and inner cladding, use many auxiliary blowtorch heating, make core layer surface densification, vitrification, it is ensured that
Hydroxyl in surrounding layer does not penetrates in sandwich layer.During fluorine doped, the dense glass layer formed due to core layer surface blocks
Fluorine, to the diffusion of pure silicon core sandwich layer, can form the refractive index profile of phase step type distribution.
3. utilizing helium gas molecules little, heat-transfer capability is high, is passed through a certain proportion of helium, can improve powder in sandwich layer deposition
Rod heat transfer efficiency in During Vitrification in vitro, it is to avoid because of the phenomenon of the heat transfer property difference that dense glass layer causes, can effectively change
The transparency of kind sandwich layer glass.
4. sandwich layer and inner cladding use the sedimentation produced without hydroxyl, simplify body of powder sintering process so that sandwich layer hydroxyl
Base content is less than 3ppm less than 0.1ppm, surrounding layer hydroxy radical content, it is achieved without logical chlorine deshydroxy technique, reduce production cost,
Realize the production of energy-conserving and environment-protective.
Accompanying drawing explanation
Below with reference to accompanying drawing, the utility model is described in further detail:
Fig. 1 is the body of powder depositing device schematic diagram preparing ultra-low-loss fiber prefabricated rods in this utility model.
Fig. 2 is the top view configuring 3 auxiliary lamps in gas-phase deposition.
Fig. 3 is the cross-sectional layer structural representation of Powder Rod
Fig. 4 is the radial distribution structural representation of Powder Rod.
The preform that in Fig. 5 this utility model prepared by comparative example, uses Fourier transform infrared spectrum instrument FTIR to detect stone
The light transmission rate figure of English glass.
Fig. 6 is the preform of embodiment 1 preparation in this utility model, uses Fourier transform infrared spectrum instrument FTIR detection
The light transmission rate figure of quartz glass.
Fig. 7 is that the preform of this utility model embodiment 2 preparation is with radially-arranged graded-index profile.
Fig. 8 is the spectrum damage figure that this utility model embodiment 4 prepares the optical fiber of ultra-low-loss fiber preform.
Fig. 9 be a kind of ultra-low-loss fiber prefabricated rods preparing pure silicon core covering fluorine doped of this utility model equipment in graphite
Sintering furnace schematic diagram.
Figure 10 be a kind of ultra-low-loss fiber prefabricated rods preparing pure silicon core covering fluorine doped of the present invention equipment in graphite burn
Black box structure for amplifying schematic diagram in freezing of a furnace.
Label declaration in figure, 1, target rod, 2, settling chamber, 3, surrounding layer blowtorch, 4, middle covering blowtorch, 5, auxiliary lamp, 6, core
Layer blowtorch, 7, suspension rod, 8, overburden cavity, 9, exhaustor, 10, prefabricated rods sandwich layer, 11, the vitrification of core layer surface fine and close
Layer, 12, prefabricated rod cladding, 13, quartz suspension rod, 14, black box, 15, cover plate, 16, quartz furnace core tube, 17, graphite furnace core tube,
18, black box gas piping, 19, target rod, 20, body of powder, 21, graphite heating body, 22, gas mass flow controller, 23,
Gas piping.
Detailed description of the invention
1-10 referring to the drawings, the equipment of a kind of ultra-low-loss fiber prefabricated rods preparing pure silicon core covering fluorine doped includes target rod
1, settling chamber 2, surrounding layer blowtorch 3, middle covering blowtorch 4, auxiliary blowtorch 5, sandwich layer blowtorch 6, suspension rod 7, exhaustor 9, overburden
Cavity 8 and graphite heating resistance furnace.Top, settling chamber 2 is provided with overburden cavity 8, and overburden cavity 8 is built with suspension rod
7, suspension rod 7 is provided with hook, and suspension rod 7 is connected with hoisting mechanism, and target rod 1 is suspended on the hook of the suspension rod being connected with hoisting mechanism
On, it is sequentially arranged with surrounding layer blowtorch 3, middle covering blowtorch 4, auxiliary blowtorch 5, sandwich layer blowtorch 6 in side, bottom, settling chamber 2, heavy
Long-pending side, top, room 2 is provided with exhaustor 9, is used for getting rid of waste gas in settling chamber 2.
In this utility model, comparative example (comparative example) and the preform of embodiment 1 preparation, use fourier infrared light
The light transmission rate figure (accompanying drawing 5,6) of spectrometer FTIR detection quartz glass, wherein, at 2.73um wavelength, transmitance is the least, shows sample
Hydroxyl (OH in product-) content is the highest.According to Lamber-Beer's Law, can calculate the hydroxyl concentration in quartz glass, formula is such as
Under:
C OH =[M OH /(ε×ρ)]×(1/d)×log 10 (I 0 /I)
In above-mentioned formula,C OH For hydroxyl mass concentration in quartz, ppm (10-6)；M OH For hydroxyl molal weight, g/mol；ε
For quartz glass specific absorbance at 2.73 μm, L/mol cm；ρFor quartz density, g/cm3；D is thickness of sample, mm；log 10 (I 0 /I)Absorbance for sample.
Referring to the drawings 9,10, in the equipment of a kind of ultra-low-loss fiber prefabricated rods preparing pure silicon core covering fluorine doped, graphite burns
Freezing of a furnace includes quartz suspension rod 13, black box 14, cover plate 15, quartz furnace core tube 16, graphite furnace core tube 17, black box gas tube
Road 18, target rod 19, body of powder 20, graphite heating body 21 and gas mass flow controller 22.20 body of powder by target rod 19 with
Quartz suspension rod 13 is connected, and in sintering process, quartz suspension rod 13 can move up and down, and rotation.On gas piping 23, gas is installed
Weight flow controller 22.In mixing F sintering process, gas mass flow controller 22 control He and fluorochemical mixes
Closing gas, the gas piping 23 being passed through quartz furnace core tube 16 is positioned at graphite heating body upper zone.Body of powder 20 is placed in quartz stove
Core pipe 16, from top to bottom by the high-temperature region produced by graphite heating body 21.Quartz furnace core tube 16 is arranged in graphite furnace core tube
17, graphite heating body 21 is centered around outside graphite furnace core tube 17.Carry out sealing quartz furnace core tube 16, quartz suspension rod 13 by cover plate 15
Through black box 14,4 layers of isolation are set in black box 14, every layer is passed through N by black box gas piping 182Carry out gas
Envelope.
Gas mass flow controller 22 uses commercially available MFC gas mass flow controller.
A kind of method of ultra-low-loss fiber prefabricated rods preparing pure silicon core covering fluorine doped is as follows:
1, target rod pretreatment
Select the material of quartz glass material as deposition target rod.The target rod of selection is carried out pickling, uses 10% concentration
Soak with hydrochloric acid 1h ~ 2h, removes the impurity being attached to target rod surface, then repeatedly rinses with deionized water, finally dry.
2, the preparation of the ultra-low-loss fiber prefabricated rods of pure silicon core covering fluorine doped
The first step: pretreated target rod is clamped on the suspension rod hook of VAD equipment, with Silicon chloride., oxygen, an oxygen
Change carbon, helium are with nitrogen mixture as unstrpped gas, and the flow proportional of various unstrpped gases is 1:1.5:1:1:0.3 ~ 1:3:
3:1:0.5, after being passed through the sandwich layer blowtorch of quartz material, the raw material silicon dioxide microparticle that pyroreaction generates in flame, deposition
To the target rod surface vertical with blowtorch.According to caput position in induction zone, gradually promote suspension rod, form the powder of axial distribution
Opisthosoma.In corresponding auxiliary blowtorch, being passed through carbon monoxide, oxygen, ratio is 2:1 ~ 1:2.In above auxiliary blowtorch
In covering blowtorch, Silicon chloride., oxygen, carbon monoxide and the nitrogen being passed through, its flow proportional is 1:1:1:0.3 ~ 1.5:1:2:
0.3.In the surrounding layer blowtorch of the top, Silicon chloride., oxygen, hydrogen (or methane) and the nitrogen being passed through, its flow proportional is
1:1:1:0.5~3:1:3:1
Second step: silicon dioxide powder opisthosoma deposition obtained is placed in graphite heating resistance furnace.By furnace core tube and quartz
Bell is fitted, and uses the black box between oil-sealing measures sealed sintering stove cover plate and suspension rod and cover plate.Then, suspension rod rotates speed
Degree is 3r/min ~ 15r/min.Being passed through Ar, fluoride, He mixed gas, wherein fluoride is CF4、C2F6、C3F8、SF6、
SiF4、C2F2Cl2、SOF2One of which or two or more combinations, gas flow ratio is 0.2:4:2 ~ 0.4:15:3, sinters furnace temperature
Degree is stable at 1100 DEG C ~ 1200 DEG C, and logical fluorine time 2h ~ 5h, Powder Rod from top to bottom passes through the thermal treatment zone.After logical fluorine terminates, again
Being passed through He, Ar mixed gas and carry out vitrification, gas flow ratio is 2:1 ~ 10:1, and sintering furnace temperature stabilization is 1300 DEG C ~ 1500
DEG C, constant temperature 8h ~ 20h, Powder Rod is the most from top to bottom by the thermal treatment zone, after vitrification terminates, closes source of the gas.By logical fluorine, glass
After glass, can obtain transparent, hydroxy radical content is low, the pure silicon core ultra-low-loss fiber prefabricated rods of covering fluorine doped.
Wherein, described auxiliary blowtorch quantity is 2 ~ 5, is dispersed in and is perpendicular in axial same plane.The powder of deposition
Opisthosoma, inner cladding thickness is 4.5 ~ 6.5 with the ratio of core layer thickness, and surrounding layer thickness is 7.5 ~ 15.5 with the ratio of core layer thickness.
Below in conjunction with embodiment, the utility model is described in further detail:
Comparative example (comparative example): manufacture the fluorine-doped optical fiber preform rod of Φ 200mm × 1600mm
(1) select the material of quartz glass material as deposition target rod.The target rod of selection carries out pickling, and employing 10% is dense
The soak with hydrochloric acid 1.5h of degree, removes the impurity being attached to target rod surface, then repeatedly rinses with deionized water, finally dry.
(2) pretreated target rod is clamped on the suspension rod hook of VAD equipment.With Silicon chloride., oxygen, hydrogen and nitrogen
Gas mixture is respectively 5g/min, 11.3L/min, 10L/min, 2L/min as unstrpped gas, the flow of various unstrpped gases,
After being passed through the sandwich layer blowtorch of quartz material, the raw material silicon dioxide microparticle that pyroreaction generates in flame, deposit to and blowtorch
Vertical target rod surface, forms relatively compact silicon dioxide layer.In covering blowtorch above sandwich layer blowtorch, four chlorinations being passed through
Silicon, oxygen, hydrogen and nitrogen, its flow is respectively 60g/min, 30L/min, 60L/min, 22.5L/min, formation of deposits density
Of a relatively loose powder bed.System, according to caput position in induction zone, gradually promotes suspension rod, thus forms axial distribution
Body of powder, after reaching certain rod length, stops deposition.Body of powder is unloaded from suspension rod, transfers to transport on rod car.
(3) go to depositing, on fortune rod car, the silicon dioxide powder opisthosoma obtained on the suspension rod of graphite heating resistance furnace, and
Use latch locking.Body of powder is placed in sintering furnace, and fit furnace core tube and quartz bell, use oil-sealing measures sealed sintering stove
Black box between cover plate and suspension rod and cover plate.Opening suspension rod rotary speed is 9r/min.By being passed through institute bottom furnace core tube
The gas needed, passes first into Ar, Cl2, He mixed gas carry out deshydroxy, gas flow is 6L/min, 57L/min, 57L/ respectively
Min, sintering furnace temperature stabilization is at 1000 DEG C, and deshydroxy time 4h, after deshydroxy terminates.It is passed through Ar, SiF again4, He, gas flow divides
Not Wei 6L/min, 190L/min, 50L/min, sintering furnace temperature stabilization is at 1150 DEG C, and logical fluorine time 3.5h, Powder Rod is by upper
Under pass through the thermal treatment zone.After logical fluorine terminates, be again passed through He, Ar mixed gas and carry out vitrification, gas flow be 90L/min,
15L/min, sintering furnace temperature stabilization is at 1400 DEG C, and constant temperature 14h, Powder Rod is the most from top to bottom by the thermal treatment zone, and vitrification is tied
Shu Hou, closes source of the gas.After logical fluorine, vitrification, can obtain transparent, hydroxy radical content is low, the pure silicon core of covering fluorine doped is ultralow
Loss optical fiber prefabricated rods.
By Fourier transform infrared spectrum instrument FTIR detection sandwich layer hydroxy radical content be 6.8ppm, outsourcing hydroxy radical content up to
18ppm.Detecting refractive index profile by PK2600 instrument, it mixes the △ n of F layer-For-0.304%, the ultra-low-loss fiber of preparation
After prefabricated stick drawn wire, optical fiber 1550nm decay 0.172dB/km, 1383nm decay to 1.35dB/km.
Embodiment 1: manufacture the ultra-low-loss fiber prefabricated rods of the pure silicon core covering fluorine doped of Φ 200mm × 1600mm
(1) select the material of quartz glass material as deposition target rod.The target rod of selection carries out pickling, and employing 10% is dense
The soak with hydrochloric acid 1h of degree, removes the impurity being attached to target rod surface, then repeatedly rinses with deionized water, finally dry.
(2) pretreated target rod is clamped on the suspension rod hook of VAD equipment.With Silicon chloride., oxygen, an oxidation
Carbon, helium and nitrogen mixture are respectively 5g/min, 7.5L/min, 5L/ as unstrpped gas, the flow of various unstrpped gases
Min, 5L/min, 1.5L/min, after being passed through the sandwich layer blowtorch of quartz material, the raw material titanium dioxide that pyroreaction generates in flame
Silicon particle, deposits to the target rod surface vertical with blowtorch.Above sandwich layer, configure in 2 mutually perpendicular auxiliary blowtorch, each
Being passed through carbon monoxide, oxygen in blowtorch, flow is respectively 8L/min, 4L/min so that core layer surface dense glass.In auxiliary
In inner cladding blowtorch above blowtorch, Silicon chloride., oxygen, carbon monoxide and the nitrogen being passed through, its flow is respectively 20g/
min、20L/min、20L/min、6L/min.In the surrounding layer blowtorch of the top, Silicon chloride., oxygen, hydrogen and the nitrogen being passed through
Gas, its flow is respectively 40g/min, 40L/min, 40L/min, 8L/min.System according to caput position in induction zone, by
Gradually promote suspension rod, thus form the body of powder of axial distribution, after reaching certain rod length, stop deposition.By body of powder from suspension rod
Upper unloading, transfers to transport on rod car.
(3) go to depositing, on fortune rod car, the silicon dioxide powder opisthosoma obtained on the suspension rod of graphite heating resistance furnace, and
Use latch locking.Body of powder is placed in sintering furnace, and fit furnace core tube and quartz bell, use oil-sealing measures sealed sintering stove
Black box between cover plate and suspension rod and cover plate.Opening suspension rod rotary speed is 3r/min.It is passed through Ar, CF4With C2F6Gaseous mixture
Body, He, gas flow is respectively 4L/min, 80L/min, 40L/min, and sintering furnace temperature stabilization, at 1100 DEG C, leads to fluorine time 2h,
Powder Rod from top to bottom passes through the thermal treatment zone.After logical fluorine terminates, again it is passed through He, Ar mixed gas and carries out vitrification, gas flow
For 50L/min, 25L/min, sintering furnace temperature stabilization at 1300 DEG C, constant temperature 8h, Powder Rod the most from top to bottom by the thermal treatment zone,
After vitrification terminates, close source of the gas.After logical fluorine, vitrification, can obtain transparent, hydroxy radical content is low, covering fluorine doped pure
Silicon core ultra-low-loss fiber prefabricated rods.
By Fourier transform infrared spectrum instrument FTIR detection sandwich layer hydroxy radical content less than 0.1ppm, outsourcing hydroxy radical content is
2.16ppm.Detecting refractive index profile by PK2600 instrument, its △ n mixing F covering is-0.326%, and cored ratio is 8.5, preparation
Ultra-low-loss fiber prefabricated stick drawn wire after optical fiber 1550nm decay 0.168dB/km, 1383nm decay to 0.316dB/km.
Embodiment 2: manufacture the ultra-low-loss fiber prefabricated rods of the pure silicon core covering fluorine doped of Φ 200mm × 1600mm
(1) select the material of quartz glass material as deposition target rod.The target rod of selection carries out pickling, and employing 10% is dense
The soak with hydrochloric acid 1.5h of degree, removes the impurity being attached to target rod surface, then repeatedly rinses with deionized water, finally dry.
(2) pretreated target rod is clamped on the suspension rod hook of VAD equipment.With Silicon chloride., oxygen, an oxidation
Carbon, helium and nitrogen mixture are respectively 5g/min, 11.3L/min, 10L/ as unstrpped gas, the flow of various unstrpped gases
Min, 5L/min, 2L/min, after being passed through the sandwich layer blowtorch of quartz material, the raw material silicon dioxide that pyroreaction generates in flame
Microgranule, deposits to the target rod surface vertical with blowtorch.Above sandwich layer, configure 3 auxiliary blowtorch and be 120 °, in each blowtorch
Being passed through carbon monoxide, oxygen, flow is respectively 6L/min, 6L/min so that core layer surface dense glass.On auxiliary blowtorch
In the inner cladding blowtorch of side, Silicon chloride., oxygen, carbon monoxide and the nitrogen being passed through, its flow is respectively 25g/min, 20L/
min、30L/min、6L/min.In the surrounding layer blowtorch of the top, Silicon chloride., oxygen, hydrogen and the nitrogen being passed through, its flow
It is respectively 60g/min, 30L/min, 60L/min, 22.5L/min.System, according to caput position in induction zone, gradually promotes
Suspension rod, thus form the body of powder of axial distribution, after reaching certain rod length, stop deposition.Body of powder is unloaded from suspension rod,
Transfer to transport on rod car.
(3) go to depositing, on fortune rod car, the silicon dioxide powder opisthosoma obtained on the suspension rod of graphite heating resistance furnace, and
Use latch locking.Body of powder is placed in sintering furnace, and fit furnace core tube and quartz bell, use oil-sealing measures sealed sintering stove
Black box between cover plate and suspension rod and cover plate.Opening suspension rod rotary speed is 9r/min.It is passed through Ar, SiF4, He, gas stream
Amount is respectively 6L/min, 190L/min, 50L/min, sintering furnace temperature stabilization at 1150 DEG C, logical fluorine time 3.5h, Powder Rod by
Upper and under pass through the thermal treatment zone.After logical fluorine terminates, being again passed through He, Ar mixed gas and carry out vitrification, gas flow is 90L/
Min, 15L/min, sintering furnace temperature stabilization is at 1400 DEG C, and constant temperature 14h, Powder Rod is the most from top to bottom by the thermal treatment zone, glass
Change after terminating, close source of the gas.After logical fluorine, vitrification, can obtain transparent, hydroxy radical content is low, the pure silicon core of covering fluorine doped
Ultra-low-loss fiber prefabricated rods.
By Fourier transform infrared spectrum instrument FTIR detection sandwich layer hydroxy radical content less than 0.1ppm, outsourcing hydroxy radical content is
1.89ppm.Detecting refractive index profile by PK2600 instrument, its △ n mixing F covering is-0.41%, and cored ratio is 12.6, preparation
Ultra-low-loss fiber prefabricated stick drawn wire after optical fiber 1550nm decay 0.170dB/km, 1383nm decay to 0.321dB/km.
Embodiment 3: manufacture the ultra-low-loss fiber prefabricated rods of the pure silicon core covering fluorine doped of Φ 200mm × 1600mm
(1) select the material of quartz glass material as deposition target rod.The target rod of selection carries out pickling, and employing 10% is dense
The soak with hydrochloric acid 2h of degree, removes the impurity being attached to target rod surface, then repeatedly rinses with deionized water, finally dry.
(2) pretreated target rod is clamped on the suspension rod hook of VAD equipment.With Silicon chloride., oxygen, an oxidation
Carbon, helium and nitrogen mixture are respectively 5g/min, 15L/min, 15L/ as unstrpped gas, the flow of various unstrpped gases
Min, 5L/min, 2.5L/min, after being passed through the sandwich layer blowtorch of quartz material, the raw material titanium dioxide that pyroreaction generates in flame
Silicon particle, deposits to the target rod surface vertical with blowtorch.Above sandwich layer, configure 5 auxiliary blowtorch and be 72 °, each blowtorch
In be passed through carbon monoxide, oxygen, flow is respectively 4L/min, 8L/min so that core layer surface dense glass.At auxiliary blowtorch
Top inner cladding blowtorch in, Silicon chloride., oxygen, carbon monoxide and the nitrogen being passed through, its flow be respectively 30g/min,
20L/min、40L/min、6L/min.In the surrounding layer blowtorch of the top, Silicon chloride., oxygen, hydrogen and the nitrogen being passed through, its
Flow is respectively 60g/min, 20L/min, 60L/min, 20L/min.System, according to caput position in induction zone, gradually carries
Rise suspension rod, thus form the body of powder of axial distribution, after reaching certain rod length, stop deposition.Body of powder is unloaded from suspension rod
Carry, transfer to transport on rod car.
(3) go to depositing, on fortune rod car, the silicon dioxide powder opisthosoma obtained on the suspension rod of graphite heating resistance furnace, and
Use latch locking.Body of powder is placed in sintering furnace, and fit furnace core tube and quartz bell, use oil-sealing measures sealed sintering stove
Black box between cover plate and suspension rod and cover plate.Opening suspension rod rotary speed is 15r/min.It is passed through Ar, SOF2, He, gas
Flow is respectively 8L/min, 300L/min, 60L/min, sintering furnace temperature stabilization at 1200 DEG C, logical fluorine time 5h, Powder Rod by
Upper and under pass through the thermal treatment zone.After logical fluorine terminates, being again passed through He, Ar mixed gas and carry out vitrification, gas flow is 150L/
Min, 15L/min, sintering furnace temperature stabilization is at 1500 DEG C, and constant temperature 20h, Powder Rod is the most from top to bottom by the thermal treatment zone, glass
Change after terminating, close source of the gas.After logical fluorine, vitrification, can obtain transparent, hydroxy radical content is low, the pure silicon core of covering fluorine doped
Ultra-low-loss fiber prefabricated rods.
By Fourier transform infrared spectrum instrument FTIR detection sandwich layer hydroxy radical content less than 0.1ppm, outsourcing hydroxy radical content is
2.95ppm.Detecting refractive index profile by PK2600 instrument, its △ n mixing F covering is-0.43%, and cored ratio is 15.2, preparation
Ultra-low-loss fiber prefabricated stick drawn wire after optical fiber 1550nm decay 0.169dB/km, 1383nm decay to 0.318dB/km.
Embodiment 4: manufacture the ultra-low-loss fiber prefabricated rods of the pure silicon core covering fluorine doped of Φ 200mm × 1600mm
(1) select the material of quartz glass material as deposition target rod.The target rod of selection carries out pickling, and employing 10% is dense
The soak with hydrochloric acid 2h of degree, removes the impurity being attached to target rod surface, then repeatedly rinses with deionized water, finally dry.
(2) pretreated target rod is clamped on the suspension rod hook of VAD equipment.With Silicon chloride., oxygen, an oxidation
Carbon, helium and nitrogen mixture are respectively 5g/min, 15L/min, 15L/ as unstrpped gas, the flow of various unstrpped gases
Min, 5L/min, 2.5L/min, after being passed through the sandwich layer blowtorch of quartz material, the raw material titanium dioxide that pyroreaction generates in flame
Silicon particle, deposits to the target rod surface vertical with blowtorch.Above sandwich layer, configure 4 auxiliary blowtorch and be 90 °, each blowtorch
In be passed through carbon monoxide, oxygen, flow is respectively 4L/min, 8L/min so that core layer surface dense glass.At auxiliary blowtorch
Top inner cladding blowtorch in, Silicon chloride., oxygen, carbon monoxide and the nitrogen being passed through, its flow be respectively 30g/min,
20L/min、40L/min、6L/min.In the surrounding layer blowtorch of the top, Silicon chloride., oxygen, methane and the nitrogen being passed through, its
Flow is respectively 45g/min, 15L/min, 45L/min, 15L/min.System, according to caput position in induction zone, gradually carries
Rise suspension rod, thus form the body of powder of axial distribution, after reaching certain rod length, stop deposition.Body of powder is unloaded from suspension rod
Carry, transfer to transport on rod car.
(3) go to depositing, on fortune rod car, the silicon dioxide powder opisthosoma obtained on the suspension rod of graphite heating resistance furnace, and
Use latch locking.Body of powder is placed in sintering furnace, and fit furnace core tube and quartz bell, use oil-sealing measures sealed sintering stove
Black box between cover plate and suspension rod and cover plate.Opening suspension rod rotary speed is 15r/min.It is passed through Ar, SF6And SOF2Mixing
Gas, He, gas flow is respectively 10L/min, 375L/min, 75L/min, and sintering furnace temperature stabilization is at 1200 DEG C, during logical fluorine
Between 5h, Powder Rod from top to bottom passes through the thermal treatment zone.After logical fluorine terminates, again it is passed through He, Ar mixed gas and carries out vitrification, gas
Flow is 180L/min, 18L/min, and sintering furnace temperature stabilization is at 1500 DEG C, and constant temperature 20h, Powder Rod the most from top to bottom passes through
The thermal treatment zone, after vitrification terminates, closes source of the gas.After logical fluorine, vitrification, can obtain transparent, hydroxy radical content is low, doped cladding layer
The pure silicon core ultra-low-loss fiber prefabricated rods of fluorine.
By Fourier transform infrared spectrum instrument FTIR detection sandwich layer hydroxy radical content less than 0.1ppm, outsourcing hydroxy radical content is
2.84ppm.Detecting refractive index profile by PK2600 instrument, its △ n mixing F covering is-0.437%, and cored ratio is 14.8, system
After standby ultra-low-loss fiber prefabricated stick drawn wire, optical fiber 1550nm decay 0.163dB/km, 1383nm decay to 0.325dB/km.
Described ultra-low-loss fiber (Ultra Low Loss, ULL), Ministry of Industry and Information communication science and technology committee director is in July, 2013
At " research and development and the development of ultra-low-loss fiber should be strengthened " (http://www.iccsz.com/site/cn/News/2013/
07/02/20130702223713708504.htm) one the article pointed out: in the industry according to fibre loss, optical fiber is roughly divided into commonly
Optical fiber, low loss fiber, ultra-low-loss fiber three class, wherein, at ordinary optic fibre 1550nm wavelength to decay to 0.20dB/km left
The right side, the decay at low loss fiber, ultra-low-loss fiber 1550nm wavelength is respectively smaller than 0.185dB/km, 0.170dB/km.
The sandwich layer of ordinary optic fibre typically mixes the earth silicon material of Ge element, improves the refractive index of sandwich layer, and covering is pure two
Silica material, thus form core/wrap certain refractive index contrast.
The sandwich layer of ultra-low-loss fiber is generally pure silicon dioxide material, and covering is the earth silicon material of fluorine doped, is formed
Core/wrap certain refractive index contrast.
Ultra-low-loss fiber prefabricated rods described in the utility model is the prefabricated rods drawing ultra-low-loss fiber.
Claims (3)
1. the equipment of the ultra-low-loss fiber prefabricated rods preparing pure silicon core covering fluorine doped, it is characterised in that: include target rod, sink
Long-pending room, surrounding layer blowtorch, middle covering blowtorch, auxiliary blowtorch, sandwich layer blowtorch, suspension rod, exhaustor, overburden cavity and graphite add
Thermal resistance stove；Top, settling chamber is provided with overburden cavity, and overburden cavity is provided with hook built with suspension rod, suspension rod,
Suspension rod is connected with hoisting mechanism, and target rod is suspended on the hook of the suspension rod being connected with hoisting mechanism, depends in side, bottom, settling chamber
Secondary equipped with surrounding layer blowtorch, middle covering blowtorch, auxiliary blowtorch, sandwich layer blowtorch, side, top, settling chamber is provided with exhaustor, uses
In getting rid of deposition indoor exhaust air；
Graphite sintering stove include quartz suspension rod, black box, cover plate, quartz furnace core tube, graphite furnace core tube, gas piping, target rod,
Body of powder, graphite heating body and gas mass flow controller；Body of powder is connected with quartz suspension rod by target rod, sintering process
In, quartz suspension rod moves up and down, and rotation；Gas mass flow controller is installed on gas piping；Body of powder is placed in quartz
Furnace core tube, from top to bottom by the high-temperature region produced by graphite heating body, quartz furnace core tube in graphite furnace core tube, graphite heating
Body is centered around outside graphite furnace core tube, carries out sealing quartz furnace core tube by cover plate, and quartz suspension rod is through black box.
The equipment of a kind of ultra-low-loss fiber prefabricated rods preparing pure silicon core covering fluorine doped the most according to claim 1, its
It is characterised by: 4 layers of isolation are set in black box, every layer is passed through N by black box gas piping2Carry out sealing gland.
The equipment of a kind of ultra-low-loss fiber prefabricated rods preparing pure silicon core covering fluorine doped the most according to claim 1, its
It is characterised by: in mixing F sintering process, gas mass flow controller controls He and fluorochemical gaseous mixture, be passed through stone
The gas piping of English furnace core tube is positioned at graphite heating body upper zone.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106007355A (en) * | 2016-05-19 | 2016-10-12 | 中天科技精密材料有限公司 | Method and equipment for preparing ultralow-loss optical fiber perform with fluorine-doped pure silicon core cladding |
| RU2713011C1 (en) * | 2017-08-23 | 2020-02-03 | Чэнду Футун Оптикал Коммьюникейшн Текнолоджис Ко., Лтд. | Optical fiber and method of its production |
| CN111320376A (en) * | 2018-12-15 | 2020-06-23 | 中天科技精密材料有限公司 | Optical fiber preform and method for manufacturing the same |
| CN111320374A (en) * | 2018-12-15 | 2020-06-23 | 中天科技精密材料有限公司 | Optical fiber preform and method for manufacturing the same |
| CN111847866A (en) * | 2020-07-14 | 2020-10-30 | 复旦大学 | Low-loss optical fiber preform outer cladding layer, preparation equipment and preparation method thereof, and optical fiber |
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2016
- 2016-05-19 CN CN201620461105.1U patent/CN205803319U/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106007355A (en) * | 2016-05-19 | 2016-10-12 | 中天科技精密材料有限公司 | Method and equipment for preparing ultralow-loss optical fiber perform with fluorine-doped pure silicon core cladding |
| CN106007355B (en) * | 2016-05-19 | 2019-02-15 | 中天科技精密材料有限公司 | A kind of method and its equipment of the ultra-low-loss fiber prefabricated rods preparing pure silicon core covering fluorine doped |
| RU2713011C1 (en) * | 2017-08-23 | 2020-02-03 | Чэнду Футун Оптикал Коммьюникейшн Текнолоджис Ко., Лтд. | Optical fiber and method of its production |
| CN111320376A (en) * | 2018-12-15 | 2020-06-23 | 中天科技精密材料有限公司 | Optical fiber preform and method for manufacturing the same |
| CN111320374A (en) * | 2018-12-15 | 2020-06-23 | 中天科技精密材料有限公司 | Optical fiber preform and method for manufacturing the same |
| CN111320376B (en) * | 2018-12-15 | 2023-09-12 | 中天科技精密材料有限公司 | Optical fiber preform and method for manufacturing the same |
| CN111320374B (en) * | 2018-12-15 | 2023-09-26 | 中天科技精密材料有限公司 | Optical fiber preform and method for manufacturing the same |
| CN111847866A (en) * | 2020-07-14 | 2020-10-30 | 复旦大学 | Low-loss optical fiber preform outer cladding layer, preparation equipment and preparation method thereof, and optical fiber |
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