CN109081575A - Preform and its manufacturing method - Google Patents
Preform and its manufacturing method Download PDFInfo
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- CN109081575A CN109081575A CN201710448220.4A CN201710448220A CN109081575A CN 109081575 A CN109081575 A CN 109081575A CN 201710448220 A CN201710448220 A CN 201710448220A CN 109081575 A CN109081575 A CN 109081575A
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- Prior art keywords
- layer
- blowtorch
- inner cladding
- surrounding layer
- oxygen
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 239000010410 layer Substances 0.000 claims abstract description 198
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 87
- 238000005253 cladding Methods 0.000 claims abstract description 75
- 238000000151 deposition Methods 0.000 claims abstract description 52
- 238000005245 sintering Methods 0.000 claims abstract description 40
- 238000010438 heat treatment Methods 0.000 claims abstract description 34
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011737 fluorine Substances 0.000 claims abstract description 27
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 27
- 239000012792 core layer Substances 0.000 claims abstract description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 74
- 239000007789 gas Substances 0.000 claims description 66
- 229910052786 argon Inorganic materials 0.000 claims description 47
- 230000008021 deposition Effects 0.000 claims description 46
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 43
- 239000001257 hydrogen Substances 0.000 claims description 43
- 229910052739 hydrogen Inorganic materials 0.000 claims description 43
- 239000001301 oxygen Substances 0.000 claims description 43
- 229910052760 oxygen Inorganic materials 0.000 claims description 43
- 238000000034 method Methods 0.000 claims description 42
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 40
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 35
- 239000005049 silicon tetrachloride Substances 0.000 claims description 35
- 239000000203 mixture Substances 0.000 claims description 26
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 23
- 239000000377 silicon dioxide Substances 0.000 claims description 21
- 235000012239 silicon dioxide Nutrition 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 14
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 9
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 239000011859 microparticle Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 229940119177 germanium dioxide Drugs 0.000 claims description 5
- IEXRMSFAVATTJX-UHFFFAOYSA-N tetrachlorogermane Chemical compound Cl[Ge](Cl)(Cl)Cl IEXRMSFAVATTJX-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 229910052732 germanium Inorganic materials 0.000 claims description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 2
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 claims description 2
- 239000013307 optical fiber Substances 0.000 abstract description 26
- 238000005452 bending Methods 0.000 abstract description 19
- 239000006185 dispersion Substances 0.000 abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 239000000843 powder Substances 0.000 description 34
- 239000000835 fiber Substances 0.000 description 15
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 9
- 238000007740 vapor deposition Methods 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 8
- 239000011521 glass Substances 0.000 description 7
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 238000000338 in vitro Methods 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- 238000004017 vitrification Methods 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 210000005239 tubule Anatomy 0.000 description 4
- 229910004014 SiF4 Inorganic materials 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000005137 deposition process Methods 0.000 description 3
- WMIYKQLTONQJES-UHFFFAOYSA-N hexafluoroethane Chemical compound FC(F)(F)C(F)(F)F WMIYKQLTONQJES-UHFFFAOYSA-N 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- QYSGYZVSCZSLHT-UHFFFAOYSA-N octafluoropropane Chemical compound FC(F)(F)C(F)(F)C(F)(F)F QYSGYZVSCZSLHT-UHFFFAOYSA-N 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 3
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 3
- 229910003978 SiClx Inorganic materials 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000003682 fluorination reaction Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000000253 optical time-domain reflectometry Methods 0.000 description 2
- 238000012946 outsourcing Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- LSJNBGSOIVSBBR-UHFFFAOYSA-N thionyl fluoride Chemical compound FS(F)=O LSJNBGSOIVSBBR-UHFFFAOYSA-N 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 101000856246 Arabidopsis thaliana Cleavage stimulation factor subunit 77 Proteins 0.000 description 1
- -1 C2F2Cl2 Chemical compound 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 229910003910 SiCl4 Inorganic materials 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- RGNPBRKPHBKNKX-UHFFFAOYSA-N hexaflumuron Chemical compound C1=C(Cl)C(OC(F)(F)C(F)F)=C(Cl)C=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F RGNPBRKPHBKNKX-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 230000008685 targeting Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—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]
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- 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)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
Abstract
The present invention provides a kind of manufacturing method of preform, comprising the following steps: provides sandwich layer, is sequentially depositing to form the first inner cladding and the second inner cladding in the core layer surface；The sandwich layer for being formed with the first inner cladding and the second inner cladding is integrally impregnated into hovering in heating zone, carries out deshydroxy, vitrifying sintering then to form quartz glass bar；Surrounding layer is formed on the quartz glass bar surface, obtains the preform.Preform in the present invention includes that preform size is big, the control of lower recess layer fluorine doped is accurate, bending property when realizing minor radius R≤5mm, optical fiber attenuation is low, dispersion is good, zero-dispersion wavelength≤1320nm characteristic, hydroxy radical content is low, meets and be better than the index of ITU-TG657B3.
Description
Technical field
The invention belongs to optical communication techniques, and in particular to a kind of preform and its manufacturing method.
Background technique
With the continuous development of optical fiber transmission technique, fiber to the home has become the important side of communication access net network construction
To.In practical FTTx fibre circuit process of deployment, it is often necessary to optical fiber lay-up operation is carried out in narrow or narrow space, it is special
Stealthy optical cable, the FTTD (fiber to the desk) not occurred in recent years even more propose optical cable installation laying, winding very strict
Requirement, optical fiber should have higher bending resistance lesser bending radius is small at this time.Therefore, it is necessary to design, develop system
The more excellent bend insensitive fiber of performance is produced, to meet the requirement of FTTx network construction and device miniaturization.According to
G.657 sonet standard requirement of the ITU-T to bend-insensitive, G.657.A1 the smallest bending radius is 10mm；G.657.A2 most
Small bending radius is 7.5mm；G.657.B3 the smallest bending radius be 5mm, wherein first two optical fiber be suitable for local area network,
Metropolitan Area Network (MAN) and FTTH (fiber to the home), and G.657.B3 optical fiber can meet the more stringent FTTD of condition (fiber to the desk) with
And it is applied in the environment such as indoor stealthy optical cable.
Meanwhile in recent years, the bandwidth requirement of personal home network is higher and higher, flow is increasing, G.657.B3 optical fiber
Not only there is good bending property, and decaying, Dispersive parameter require also to further increase, it should be close with G652D optical fiber
Or it is identical.
Since the performance of optical fiber depends on the performance of preform, currently manufactured bend insensitive fiber is prefabricated
The technique of stick mainly has tetra- kinds of processes of VAD, OVD, MCVD, PCVD, the above two belong to external deposition method, both rear to belong to pipe
Interior sedimentation.
Conventional technique has the disadvantage that
1. sedimentation (MCVD, PCVD) is limited by process conditions and size in managing, water peak attenuation by absorption is big, and manufacturing cost
Height, preform size are small, cannot achieve scale；
2. during currently used VAD manufacture plug, it is known that patent CN2010106090.0,
It is recessed by realizing in CN201210243973.9, US5032001, US7043125b2, CN176680, CN104991306 patent
Fall into layer design improves the macrobend performance of optical fiber to a certain extent, when bending radius is less than or equal to 10mm, macrobend performance
It is unable to reach requirement G.657.B3；Meanwhile research finds the depth and width size of recessed layer, it all can be to macrobend performance, light
Fine cutoff wavelength and dispersion influence, thus the lower recess fluorine doped layer of traditional VAD preparation be unable to accurately control its width and
Depth.
3. in patent CN201310300024.4, sandwich layer group is divided into SiO2-GeO2When-F-Cl, according to optical fiber quartz glass
Rayleigh scattering principle is unfavorable for guaranteeing uniformity, the consistency of material, the pad value of optical fiber also gets over it is found that sandwich layer doping
Greatly.Although meeting G.657.B3 decay indices, the existing market demand can not be adapted to, both met macrobend G.657.B3 or
Meet G652D decaying, Dispersive parameter.Meanwhile patent CN201310300024.4, ZL200910062855.6, CN104991306
In disclosed method, its design method is only referred to, the manufacturing method without specifically referring to preform, predispersed fiber
Stick processed stick technique processed itself is more demanding, is difficult to implement in actual production.
Summary of the invention
In view of the foregoing, it is necessary to which a kind of manufacturing method of preform is provided, comprising the following steps:
Sandwich layer is provided, is sequentially depositing to form the first inner cladding and the second inner cladding in the core layer surface；
The sandwich layer for being formed with the first inner cladding and the second inner cladding is integrally impregnated into hovering in heating zone, is then carried out
Deshydroxy, vitrifying sintering are to form quartz glass bar；
Surrounding layer is formed on the quartz glass bar surface, obtains the preform.
Further, the process for forming surrounding layer is to carry out the double-deck raw material using surrounding layer blowtorch to react to be formed, institute
Stating surrounding layer blowtorch includes blowtorch central core and blowtorch outer layer, and the blowtorch central core is used to be passed through fluoride and silicon tetrachloride,
The blowtorch outer layer is used to be passed through the mixture of fluoride, oxygen, hydrogen and argon gas, fluorine-containing to carry out the double-deck raw material reaction generation
SiO 2 powder particle deposits to the quartz glass bar surface.
Further, the sandwich layer uses sandwich layer blowtorch by vapor axial method (VAD), is passed through with germanium tetrachloride, four chlorinations
Silicon, oxygen, hydrogen and ar mixture carry out pyroreaction generation silica and germanium dioxide particle are heavy as unstrpped gas
Product forms, and the flow proportional of the unstrpped gas is 1:10:30:30:15~1:20:70:40:15.
Further, first inner cladding using the first inner cladding blowtorch and assists blowtorch by vapor axial method (VAD),
It is passed through the mixture of silicon tetrachloride, oxygen, hydrogen and argon gas to the first inner cladding blowtorch, carries out pyroreaction and generates dioxy
SiClx particle deposition in the core layer surface, the silicon tetrachloride, oxygen, hydrogen and argon gas the flow proportional of mixture be
5:10:10:1~5:8:15:1；It is passed through hydrogen, oxygen to the auxiliary blowtorch, the flame of the auxiliary blowtorch is coated with described
The silicon dioxide microparticle of core layer surface deposition.
Further, second inner cladding uses the second inner cladding blowtorch by vapor axial method (VAD), is passed through fluorination
Object, silicon tetrachloride, oxygen, hydrogen and argon gas mixture, carry out pyroreaction generate fluorine-containing silicon dioxide microparticle deposition and
Flow proportional at the mixture of, the fluoride, silicon tetrachloride, oxygen, hydrogen and argon gas be 0.1:5:10:10:1~
0.05:5:8:15:1。
Further, the heating zone is the heating zone of integrated agglomerating plant, the heating of the integral sintering equipment
The head of district reaches 2000mm or more.
Further, the formation surrounding layer includes forming lower recess layer, the first surrounding layer and the second outsourcing from inside to outside
Layer, the lower recess layer that formed are passed through the fluoride of the surrounding layer blowtorch, silicon tetrachloride, oxygen, hydrogen and argon gas
The flow proportional of mixture is 0.2:5:10:10:1~0.4:5:8:15:1, and the first surrounding layer of the formation is passed through the outsourcing
The layer fluoride of blowtorch, silicon tetrachloride, oxygen, hydrogen and argon gas the flow proportional of mixture be 0.1:5:10:10:1
~0.05:5:8:15:1, silicon tetrachloride, oxygen, hydrogen and the argon for forming the second surrounding layer and being passed through the surrounding layer blowtorch
The flow proportional of the mixture of gas is 5:10:10:1~5:8:15:1.
Further, the formation surrounding layer further includes that will be formed with lower recess layer, the first surrounding layer and the second surrounding layer
Quartz glass bar integrally impregnate hovering in heating zone, then carry out deshydroxy, vitrifying sintering.
Further, the formation surrounding layer further includes that will first be formed with lower recess layer quartz glass bar integrally to impregnate hovering
In heating zone, deshydroxy, fluorine doped, vitrifying sintering are carried out, then the first surrounding layer described in layer by layer deposition and described the from inside to outside
Two surrounding layers, deshydroxy, vitrifying are sintered again.
A kind of preform, the preform successively includes sandwich layer, the first inner cladding, the second inner cladding, recessed
Layer, the first surrounding layer and the second surrounding layer are fallen into,
The sandwich layer is the silica composition for mixing germanium (Ge), the relative fefractive index difference △ n of the sandwich layer1For 0.3%~
0.45%；
First inner cladding is pure silicon dioxide layer, the relative fefractive index difference △ n of first inner cladding2It is 0；
Second inner cladding is shallow fluorine doped layer, the relative fefractive index difference △ n of second inner cladding3For -0.05%~-
0.15%；
The lower recess layer is deep fluorine doped layer, the relative fefractive index difference △ n of the lower recess layer4For -0.25%~-
0.6%；
First surrounding layer is shallow fluorine doped layer, the relative fefractive index difference △ n of first surrounding layer5For -0.05%~-
0.15%；
Second surrounding layer is pure silicon dioxide layer, the relative fefractive index difference △ n of second surrounding layer6It is 0.
The present invention by using VAD technique, OVD technique, using impregnate hovering technique and using the double-deck raw material react by
The technique of layer deposition surrounding layer, the large-sized low-water-peak bend insensitive fiber being prepared include big (the stick diameter of preform size
D >=150mm), the control of lower recess layer fluorine doped is accurate, realizes bending property when minor radius R≤5mm (when optical fiber breaks into the bending of 1 circle
When radius is 5mm, the bending loss value obtained using two wavelength measurements of 1550nm, 1625nm is respectively in 0.05dB and 0.1dB
Within), optical fiber attenuation it is low (1310nm decaying≤0.334dB/km, 1383nm decaying≤0.334dB/km, 1550nm decaying≤
0.204dB/km), the spy of dispersion good (zero-dispersion slop≤0.085ps/ (nm^2*km), zero-dispersion wavelength≤1320nm)
Property, glass bar purity is high, hydroxy radical content is low (≤1ppm), meets and be better than the index of ITU-T G657B3.
Detailed description of the invention
For the above objects, features and advantages of the present invention can more be become apparent, below in conjunction with attached drawing to tool of the invention
Body embodiment elaborates, in which:
Fig. 1 is the manufacturing method flow chart of preform in the embodiment of the present invention；
Fig. 2 is the manufacture system schematic diagram of preform in the embodiment of the present invention；
Fig. 3 is vapor axial method (VAD) equipment schematic diagram in the manufacture system of preform in the embodiment of the present invention；
Fig. 4 is the top view of vapor axial method (VAD) equipment in Fig. 3；
Fig. 5 is integral sintering equipment schematic diagram in the manufacture system of preform in the embodiment of the present invention；
Fig. 6 is pipe outside vapor deposition (OVD) equipment signal in the manufacture system of preform in the embodiment of the present invention
Figure；
Fig. 7 is the side view of pipe outside vapor deposition (OVD) equipment in Fig. 6；
Fig. 8 is the top view of surrounding layer blowtorch in pipe outside vapor deposition (OVD) equipment in Fig. 6；
Fig. 9 is the front view of surrounding layer blowtorch in pipe outside vapor deposition (OVD) equipment in Fig. 6；
Figure 10 is the refractive index profile structure chart of preform in the embodiment of the present invention；
Figure 11 is the light transmission rate that preform in the embodiment of the present invention 1 is detected using Fourier transform infrared spectrum instrument FTIR
Figure；
Figure 12 is the optical fiber attenuation schematic diagram of preform in the embodiment of the present invention 1.
Main element symbol description
The present invention that the following detailed description will be further explained with reference to the above drawings.
Specific embodiment
Before describing the present invention, it should be noted that the present invention is not limited to specific embodiments discussed below.This
Field technical staff be appreciated that do not depart from the claims in the present invention spirit in the case where, can be to specific reality as described below
The mode of applying is changed and is modified.
A kind of manufacturing method of preform, as shown in Figure 1, comprising the following steps:
S101: sandwich layer is provided, is sequentially depositing to form the first inner cladding and the second inner cladding in the core layer surface；
S102: the sandwich layer for being formed with the first inner cladding and the second inner cladding is integrally impregnated into hovering in heating zone, so
Carry out deshydroxy, vitrifying sintering afterwards to form quartz glass bar；
S103: surrounding layer is formed on the quartz glass bar surface, obtains the preform.
Specifically, in conjunction with Fig. 3, in step s101, the target rod after pickling processes is clamped in the sunpender of VAD equipment 110
On 12 hooks, using germanium tetrachloride, silicon tetrachloride, oxygen, hydrogen and ar mixture as unstrpped gas, various unstrpped gases
Flow proportional is 1:10:30:30:15~1:20:70:40:15, and after being passed through sandwich layer blowtorch 7, unstrpped gas is anti-in flame high temperature
Silica, the germanium dioxide particle that should be generated, deposit to target rod surface.In first inner cladding blowtorch 8, four chlorinations that are passed through
Silicon, oxygen, hydrogen and argon gas, flow proportional are 5:10:10:1~5:8:15:1, and raw material is generated in the reaction of flame high temperature
Silicon dioxide microparticle deposits to the surface of sandwich layer powder loosening body.It assists being passed through hydrogen, oxygen, flame is coated in blowtorch 8a
The corresponding loosening body surface of first inner cladding.Wherein, as shown in figure 4, auxiliary blowtorch 8a and 8 same level of the first inner cladding blowtorch
Face, the two angle are 30 °~90 °, and the auxiliary blowtorch 8a quantity is 1~2.In second inner cladding blowtorch 9 of top, lead to
Entering fluoride, silicon tetrachloride, oxygen, hydrogen and argon gas, flow proportional is 0.1:5:10:10:1~0.05:5:8:15:1,
Middle fluoride is one kind of CF4, C2F6, C3F8, SF6, SiF4, C2F2Cl2, SOF2.Raw material is reacted in flame high temperature to be generated
Fluorine-containing silicon dioxide microparticle, deposit to the surface of the corresponding loosening body of the first inner cladding.Caput is incuded according to detector
Position promotes sunpender, gradually forms the powder loosening body being axially distributed.
In step s 102, in conjunction with Fig. 5, after VAD deposition, obtained powder loosening body is integrally impregnated hover in
The heating zone of integral sintering furnace carries out deshydroxy, vitrifying sintering.Powder loosening body is dropped to the heating zone of calandria 16
Interior, sunpender rotation speed is 10r/min~30r/min.It is passed through Ar, He, Cl2Mixed gas, gas flow ratio be 0.2:1:3~
0.2:3:1, Heating Zone Temperature are stablized at 1100 DEG C~1300 DEG C, time 6h~10h, and the pressure of furnace core tube 15 maintains 2~
4pa.The gas being passed through in During Vitrification in vitro is Ar, He mixed gas, and gas flow ratio is 1:5~1:15, quartz glassization temperature
Degree is stablized at 1400 DEG C~1600 DEG C, and constant temperature 4h~6h, furnace pressure maintains 1~2pa.After deshydroxy, vitrifying
Obtain quartz glass bar transparent, that hydroxy radical content is low.
In step s 103, in conjunction with Fig. 6, quartz glass bar 21 is placed on pipe outside vapor deposition (OVD) equipment 130
Fixed on synchronous chuck, in deposition process, 22 numbers of every group of surrounding layer blowtorch preferably single blowtorch can also 2~3 blowtorch/groups.
22 position of surrounding layer blowtorch can be centered around any position of quartz glass bar 21, it is ensured that air-exhausting duct 24 and surrounding layer blowtorch
22 centers are in same center can (as shown in Figure 7).The surrounding layer blowtorch 22 includes blowtorch central core and blowtorch outer layer, institute
It states blowtorch central core and is passed through fluoride and silicon tetrachloride, the blowtorch outer layer is passed through the mixing of fluoride, oxygen, hydrogen and argon gas
Object, wherein fluoride is CF4、C2F6、C3F8、SF6、SiF4、C2F2Cl2、SOF2One kind, the blowtorch outer layer includes tubule, institute
It states tubule and is passed through argon gas.Surrounding layer blowtorch 22 carries out the double-deck raw material reaction, generates fluorinated silicon dioxide powder by flame hydrolysis
Particle deposits to the quartz glass bar surface, layer by layer deposition from inside to outside is realized, using infrared caliper real-time monitoring powder
Loosening body outer diameter.It in deposition process, is deposited by starting point, after being at the uniform velocity moved to end, returns to starting point and deposit again, follow
Ring is repeatedly.According to the requirement of design profile, layer by layer deposition lower recess layer, the first surrounding layer and the second surrounding layer, reach from inside to outside
To after sets requirement, raw material flow is adjusted.Fluoride, silicon tetrachloride, oxygen, hydrogen and the argon flow ratio of lower recess layer deposition
Example is 0.2:5:10:10:1~0.4:5:8:15:1, fluoride, silicon tetrachloride used in the first outer cladding deposition, oxygen, hydrogen and
Argon flow ratio is 0.1:5:10:10:1~0.05:5:8:15:1, silicon tetrachloride, oxygen used in the second outer cladding deposition,
Hydrogen and argon flow ratio are 5:10:10:1~5:8:15:1.
The SiO 2 powder loosening body that deposition obtains is placed in heating zone and carries out deshydroxy, vitrifying sintering, technique stream
Journey is consistent with plug powder loosening body deshydroxy, vitrifying in step S102, finally obtained large-sized low-water-peak bend-insensitive
Single mode optical fiber prefabricated rods.
If it is as follows that surrounding layer prepares preparation process flow when increasing the fluorine doped glass refringence of lower recess layer:
The quartz glass bar 21 of preparation is placed on the synchronization chuck of pipe outside vapor deposition (OVD) equipment 130 it is fixed,
Deposition.In depositing operation similar step S103 prepared by surrounding layer, from inside to outside layer by layer deposition.After lower recess deposition, knot
Shu Fenmo loosening body deposition.
Obtained powder loosening body integrally impregnates hovering in progress deshydroxy, fluorine doped, glass in the heating zone of integral sintering furnace
Glassization sintering, i.e., drop to Powder Rod in the heating zone of integral sintering furnace, and sunpender rotation speed is 10r/min~30r/
min.It is passed through Ar, He, Cl2, fluoride mixed gas, wherein fluoride be CF4、C2F6、C3F8、SF6、SiF4、C2F2Cl2、SOF2
One of which, gas flow ratio are 0.2:1:3:0.1~0.2:3:1:0.06, and sintering furnace temperature is stablized 1100 DEG C~1300
DEG C, time 6h~10h, furnace pressure maintains 2~4pa.The gas being passed through in During Vitrification in vitro is Ar, He mixed gas, gas
Body flow-rate ratio is 1:5~1:15, and quartz glass temperature is stablized at 1400 DEG C~1600 DEG C, constant temperature 4h~6h, and furnace pressure is tieed up
It holds in 1~2pa.After deshydroxy, fluorine doped, vitrifying, quartz glass bar transparent, that hydroxy radical content is low can be obtained.
By glass bar obtained above, then it is placed on the synchronization chuck of OVD equipment 130 and fixes, it is successively heavy from inside to outside
Product the first surrounding layer, the second surrounding layer, obtained powder loosening body is placed into heating zone again and carries out deshydroxy, vitrifying is burnt
Knot, finally obtained large-sized low-water-peak bend-insensitive single-mode optical fiber prefabricated rods.
As shown in Fig. 2, the embodiment of the present invention also provides a kind of manufacture system 100 of bend insensitive fiber prefabricated rods, packet
Vapor axial method (VAD) equipment 110, integral sintering equipment 120 and pipe outside vapor deposition (OVD) equipment 140 are included, with described
The deposition of vapor axial method (VAD) equipment 110 forms sandwich layer 1, the first inner cladding 2 and the second inner cladding 3, obtains powder loosening body；
The powder loosening body is integrally impregnated to hovering in the integral sintering equipment 120, carries out deshydroxy, vitrifying sintering；Through
Pipe outside vapor deposition (OVD) equipment 140 deposits lower recess layer, the first surrounding layer and the second surrounding layer.In the present embodiment
In, integral sintering equipment 120 is integrated sintering furnace.
In Fig. 3, vapor axial method (VAD) equipment 110 includes sandwich layer blowtorch 7, the first inner cladding blowtorch 8, auxiliary
Blowtorch 8a, the second inner cladding blowtorch 9, plug deposition chamber 10, sunpender 12, plug deposition upper cavity 13 and exhaust pipe 14, it is described
Sandwich layer blowtorch 7, the first inner cladding blowtorch 8, the auxiliary blowtorch 8a and the second inner cladding blowtorch 9 are set to the core
In stick deposition chamber 10, be for respectively forming sandwich layer, the first inner cladding and the second inner cladding, as shown in figure 4, auxiliary blowtorch 8a with
First inner cladding blowtorch, 8 same level, the two angle are 30 °~90 °, and the auxiliary blowtorch 8a quantity is 1~2；Institute
Plug deposition chamber 10 is stated to connect with plug deposition upper cavity 13；The sunpender 12 is placed in the plug deposition upper cavity 13
It is interior, for clamping target rod；The exhaust pipe 14 is used for the gas being discharged in vapor axial method (VAD) equipment 110.
Optimize VAD technique in the embodiment of the present invention, assists blowtorch by increasing by 1~2 tunnel, increase the powder of the first inner cladding
Density (ρ=0.5~0.8g/cm^3), reduce or barrier deposition when sandwich layer Ge and the second inner cladding in fluorine element counterdiffusion, will
Fluorine element constrains in the second inner cladding, to avoid traditional center core layer by the diffusion of F and to Ge refractive index in sandwich layer
The counteracting of contribution is conducive to attenuation loss caused by improving doping concentration.
In Fig. 5, the integral sintering equipment 120 includes furnace core tube 15, graphite heating body 16, pressure gauge 18, sealing
Cover board 17, gas shunt electric control system 19 and master controller 20, the furnace core tube 15 includes built-in quartzy furnace core tube, outer
The graphite furnace core tube set, the furnace core tube 15 are bonded with the seal cover board 17, and the graphite heating body 16 is looped around the stone
Outside black furnace core tube, the hot length of the graphite heating body 16 is 2000mm or more, covers the integral sintering equipment 120
Longitudinal length installs the pressure gauge 18 on the outside of the furnace core tube 15, for monitoring the quartzy furnace core overpressure, and combines
The gas shunt device electric control system 19 is controlled the type and flow for the gas being respectively passed through, and makes quartzy furnace core tube internal pressure
Power is kept constant, and the master controller 20 is used to control the operation of the integral sintering equipment.
Using integral type sintering process, which is optimization sintering furnace hot-zone, and heating zone length, will up to 2000mm or more
Powder Rod is integrally immersed in the heating zone of furnace body, and the powder loosening body of unit volume carries out abundant, uniform deshydroxy and small
Removal of bubbles technique, not by Powder Rod in conventional sintering technique move up and down caused by uneven heating, low efficiency the phenomenon that, this
Kind integral type soaking technology greatly promotes efficiency and meets the requirement of glass bar purity is high, hydroxy radical content low (≤1ppm).Equipment
The upper automatic gas switching system of matching is, it can be achieved that any of various gases needed for deshydroxy, fluorine doped, vitrifying arranges in pairs or groups and control.
The △ n that the lower recess layer powder loosening body of OVD deposition is passed through into lower recess layer after fluorine doped4It can reach -0.4%~-0.6%, in fact
Optical fiber bending resistance under the conditions of existing minor radius.
In figure 6 and figure 7, pipe outside vapor deposition (OVD) equipment 140 includes chuck, surrounding layer blowtorch 22, surrounding layer spray
Lamp load transfer station 23 and air-exhausting duct 24.Every group of preferably single blowtorch of surrounding layer blowtorch number, can also 2~3 blowtorch/groups, it is described
Blowtorch position can be centered around any position of quartz glass bar 21, it is ensured that air-exhausting duct 24 is in same with 22 center of surrounding layer blowtorch
Center.During the deposition process, the surrounding layer blowtorch load transfer station 23 carries the quartz glass bar 21 and deposits by starting point,
After being at the uniform velocity moved to end, returns to starting point and deposit again, circulation is repeatedly.
OVD technique is optimized in inventive embodiments, such as Fig. 8 and Fig. 9,22 structure of surrounding layer blowtorch is that the double-deck raw material is anti-
It answers, the surrounding layer blowtorch includes blowtorch central core and blowtorch outer layer, in addition to the blowtorch central core in traditional handicraft is passed through fluorination
Object, SiCl4Outside raw material, the blowtorch outer layer is passed through the mixture of fluoride, oxygen, hydrogen and argon gas, the blowtorch outer layer packet
Include tubule, the tubule is passed through argon gas, improve the uniformity of fluoride gas flow and flow velocity, at the same by surrounding layer blowtorch 22 with
Exhaust outlet 24 is designed as being distributed in opposite directions, facilitates the targeting of raw material, it is ensured that fluoride, silicon tetrachloride are on powder loosening body surface
Abundant reactive deposition is carried out, realizes high effective deposition.Layer by layer deposition is used based on OVD technique, can precisely, effectively control lower recess layer
Width and uniformity also avoid in VAD technique radial one-step method preparation under conditions of the limitation of not managed interior method process
The non-uniform phenomenon of lower recess layer.
The present invention also provides a kind of bend insensitive fiber prefabricated rods, successively including in sandwich layer 1, the first inner cladding 2, second
Covering 3, lower recess layer 4, the first surrounding layer 5 and the second surrounding layer 6.
As shown in Figure 10, sandwich layer 1 is silica composition (the △ n for mixing Ge1=0.3%~0.45%) it is used for transmission light letter
Number, the first inner cladding 2 is pure silicon dioxide layer (△ n2=0) light, can be constrained to transmit in the core, the mould field for keeping optical fiber stable
Distribution, at the same obstruct the second inner cladding 3, in lower recess layer 4 fluorine element diffusion, reduce impurity composition in sandwich layer 1, improve optical fiber
Fade performance.Lower recess layer 4 is deep fluorine doped layer (△ n4=-0.25%~-0.6%), it is ensured that under the minor radius bending of optical fiber
Bending resistance；Second inner cladding 3 and the first surrounding layer 5 are shallow fluorine doped layer (△ n3、△n5Be -0.05%~-
0.15%), mainly as transition zone, to improve the viscosity of sandwich layer 1, lower recess layer 4, the second surrounding layer 6 in high temperature wire drawing
Match, avoid traditional handicraft center core layer 1 (big positive refracting power) and lower recess layer 4 (big negative index) and pure silicon dioxide surrounding layer it
Between the viscosity mismatch that occurs, cause the network structure defect of quartz glass in optical fiber, increase attenuation loss, meanwhile, this structure
There is buffer function when also may make fibre-optical bending stress, improve fiber strength.Second surrounding layer 6 is pure silicon dioxide layer (△
n6=0).
In embodiments of the present invention, relative fefractive index difference △ ni=[(ni-n0)/n0] * 100%, niAnd n0It is each right respectively
Answer the refractive index of fiber section and pure silicon dioxide glass.
Embodiment 1
By the target rod after pickling processes be clamped in VAD equipment sunpender hook on, with germanium tetrachloride, silicon tetrachloride, oxygen,
Hydrogen and ar mixture are used as unstrpped gas, the flow of various unstrpped gases is 100mL/min, 1.5L/min, 5.5L/min,
3.5L/min, 1.5L/min, after being passed through the sandwich layer blowtorch of quartz material, titanium dioxide of the raw material in the reaction generation of flame high temperature
Silicon, germanium dioxide particle deposit target rod surface.Using an auxiliary blowtorch, it is with both the first inner cladding blowtorch angles
60°.In first inner cladding blowtorch, silicon tetrachloride, oxygen, hydrogen and the argon gas being passed through, flow is respectively 10L/min, 18L/
Min, 27L/min, 2L/min, powder deposit to sandwich layer loosening body surface.In second inner cladding blowtorch, it is passed through carbon tetrafluoride, four
Silicon chloride, oxygen, hydrogen and argon gas, flow are respectively 150mL/min, 10L/min, 18L/min, 27L/min, 2L/min,
Powder deposits to the first inner cladding loosening body surface.The position of caput is incuded according to detector, is promoted sunpender, is gradually formed axial direction
The powder loosening body of distribution.Obtained powder loosening body carries out Density Detection, and the first inner cladding density is 0.54g/cm^3, and second
Inner cladding density is 0.28g/cm^3.
The SiO 2 powder loosening body that deposition obtains is placed in sintering furnace heating zone.Furnace core tube and quartzy bell are pasted
It closes, Powder Rod is dropped in the heating zone of calandria, sunpender rotation speed is 20r/min.It is passed through Ar, He, Cl2Gaseous mixture
Body, gas flow are 1L/min, 10L/min, 10L/min respectively, and sintering furnace temperature is stablized at 1200 DEG C, time 8h, furnace internal pressure
Power maintains 3pa.It is respectively 1L/min, 10L/min, quartz glass that Ar, He mixed gas flow are passed through in During Vitrification in vitro
Temperature is stablized at 1500 DEG C, and constant temperature 5h, furnace pressure maintains 2pa.After deshydroxy, vitrifying, transparent, hydroxyl can be obtained
The low quartz glass bar of content.By cutting, polish the sample of preparation, tested using Fourier infrared spectrograph, such as Figure 11,
Transmitance is smaller at 2.73um wavelength, shows that hydroxyl in sample (OH-) content is higher.According to Lamber-Beer's Law, can calculate
Hydroxyl concentration in quartz glass, formula are as follows:
COH=[MOH/(ε×ρ)]×(1/d)×log10(I0/I)
In above-mentioned formula, COHFor hydroxyl mass concentration in quartz, ppm (10-6)；MOHFor hydroxyl molal weight (g/mol)；ε
The absorptivity (L/molcm) for being quartz glass at 2.73 μm；ρ is quartzy density (g/cm3)；D is thickness of sample (mm)；
log10(I0/ I) be sample absorbance.The hydroxyl being calculated is 0.14ppm, is far below 1ppm.
The quartz glass bar of above-mentioned preparation is placed on the synchronization chuck of OVD equipment it is fixed, take 2 blowtorch/groups into
Row deposition.It is passed through carbon tetrafluoride, silicon tetrachloride, oxygen, hydrogen and argon gas, lights blowtorch gas, it is raw by flame hydrolysis
At fluorinated silicon dioxide powder particle deposit to mandrel surface, from inside to outside layer by layer deposition lower recess layer, the first surrounding layer and
Second surrounding layer.After the powder for reaching setting loose stick diameter, flow is adjusted.Carbon tetrafluoride, the tetrachloro of lower recess layer deposition
SiClx, oxygen, hydrogen and argon flow ratio are 600mL/min, 10L/min, 18L/min, 27L/min, 2L/min, outside first
It is respectively 150mL/min, 10L/min, 18L/ that covering, which deposits carbon tetrafluoride, silicon tetrachloride, oxygen, hydrogen and argon flow used,
Min, 27L/min, 2L/min, silicon tetrachloride, oxygen, hydrogen and argon flow used in the second outer cladding deposition are respectively 10L/
min、18L/min、27L/min、2L/min。
The SiO 2 powder loosening body that deposition obtains is placed in sintering furnace heating zone and carries out deshydroxy, vitrifying sintering,
Obtain the low water peak bend insensitive fiber prefabricated rods that stick diameter is 180mm, length is 1600mm.After prefabricated rods are extended 80mm,
It is tested using PK2600, each layer refringence of prefabricated rods is respectively △ n1=0.304%, △ n2=0, △ n3=-0.067%, △
n4=-0.322%, △ n5=-0.082%, △ n6=0.After prefabricated stick drawn wire, optical fiber through Meter Tests such as OTDR, PK2200,
When it is 5mm that optical fiber, which breaks into 1 circle bending radius, divided using the bending loss value that two wavelength measurements of 1550nm, 1625nm obtain
Not in 0.042dB and 0.095dB；Decaying at 1310nm, 1383nm and 1550nm wavelength be respectively 0.331dB/km,
0.288dB/km, 0.192dB/km (as shown in figure 12)；Zero-dispersion slop is 0.074ps/ (nm^2*km), zero-dispersion wavelength is
1316nm。
Embodiment 2
By the target rod after pickling processes be clamped in VAD equipment sunpender hook on, with germanium tetrachloride, silicon tetrachloride, oxygen,
Hydrogen and ar mixture are used as unstrpped gas, the flow of various unstrpped gases is 120mL/min, 1.8L/min, 6.6L/min,
4.2L/min, 1.8L/min, after being passed through the sandwich layer blowtorch of quartz material, titanium dioxide of the raw material in the reaction generation of flame high temperature
Silicon, germanium dioxide particle, deposit to target rod surface.Using 2 auxiliary blowtorch, it is with both the first inner cladding blowtorch angles
45°.In first inner cladding blowtorch, silicon tetrachloride, oxygen, hydrogen and the argon gas being passed through, flow is respectively 12L/min, 22L/
Min, 32L/min, 2.4L/min, powder deposit to sandwich layer loosening body surface.In second inner cladding blowtorch, be passed through ocratation,
Silicon tetrachloride, oxygen, hydrogen and argon gas, flow are respectively 180mL/min, 12L/min, 22L/min, 32L/min, 2.4L/
Min, powder deposit to the first inner cladding loosening body surface.The position of caput is incuded according to detector, is promoted sunpender, is gradually formed
The powder loosening body being axially distributed.Obtained powder loosening body carries out Density Detection, and the first inner cladding density is 0.71g/cm^3,
Second inner cladding density is 0.32g/cm^3.
The SiO 2 powder loosening body that deposition obtains is placed in sintering furnace heating zone.Furnace core tube and quartzy bell are pasted
It closes, Powder Rod is dropped in the hot-zone of calandria, sunpender rotation speed is 20r/min.It is passed through Ar, He, Cl2Mixed gas,
Gas flow is 1.5L/min, 15L/min, 15L/min respectively, and sintering furnace temperature is stablized at 1200 DEG C, time 8h, furnace pressure
Maintain 3pa.It is respectively 1.5L/min, 15L/min, quartz glass that Ar, He mixed gas flow are passed through in During Vitrification in vitro
Temperature is stablized at 1500 DEG C, and constant temperature 5h, furnace pressure maintains 2pa.After deshydroxy, vitrifying, transparent, hydroxyl can be obtained
The low quartz glass bar of content.By cutting, polishing the sample of preparation, is tested, be calculated using Fourier infrared spectrograph
Hydroxyl 0.25ppm, be far below 1ppm.
The quartz glass bar of above-mentioned preparation is placed on the synchronization chuck of OVD equipment it is fixed, take 3 blowtorch/groups into
Row deposition.It is passed through ocratation, silicon tetrachloride, oxygen, hydrogen and argon gas, lights blowtorch gas, it is raw by flame hydrolysis
At fluorinated silicon dioxide powder particle deposit to mandrel surface, layer by layer deposition from inside to outside monitors powder using infrared caliper
Last stick diameter.Lower recess layer deposition carbon tetrafluoride, silicon tetrachloride, oxygen, hydrogen and argon flow ratio be 720mL/min,
12L/min, 22L/min, 32L/min, 2.4L/min after the loose stick diameter of powder for reaching setting, terminate deposition.
Obtained powder loosening body is placed in sintering furnace heating zone and carries out deshydroxy, fluorine doped, vitrifying sintering.It will deposition
Obtained SiO 2 powder loosening body is placed in graphite heating resistance furnace.Furnace core tube is bonded with quartzy bell, by Powder Rod
It drops in the hot-zone of calandria, sunpender rotation speed is 20r/min.It is passed through Ar, He, Cl2, ocratation mixed gas, gas
Body flow is 1L/min, 10L/min, 10L/min, 400mL/min respectively, and sintering furnace temperature is stablized at 1200 DEG C, time 8h, furnace
Interior pressure maintains 4pa.It is respectively 1.5L/min, 15L/min, quartz that Ar, He mixed gas flow are passed through in During Vitrification in vitro
Glass transition temperature is stablized at 1500 DEG C, and constant temperature 5h, furnace pressure maintains 2pa.After deshydroxy, fluorine doped, vitrifying, it can obtain
Obtain the quartz glass bar transparent, hydroxy radical content is low.
By glass bar obtained above, then it is placed on the synchronization chuck of OVD equipment fixed, layer by layer deposition the from inside to outside
One surrounding layer, the second surrounding layer, carbon tetrafluoride, silicon tetrachloride, oxygen, hydrogen and argon flow used in the first outer cladding deposition point
Not Wei 180mL/min, 12L/min, 22L/min, 32L/min, 2.4L/min, silicon tetrachloride used in the second outer cladding deposition,
Oxygen, hydrogen and argon flow are respectively 12L/min, 22L/min, 32L/min, 2.4L/min, and the powder for reaching setting is loose
After stick diameter, terminate deposition.
Obtained powder loosening body, which is placed into again in sintering furnace heating zone, carries out deshydroxy, vitrifying sintering, finally obtains
Stick diameter be 200mm, the low water peak bend insensitive fiber prefabricated rods that length is 1600mm.After prefabricated rods are extended 80mm, adopt
It is tested with PK2600, each layer refringence of prefabricated rods is respectively △ n1=0.325%, △ n2=0, △ n3=-0.065%, △ n4
=-0.537%, △ n5=-0.072%, △ n6=0.After prefabricated stick drawn wire, optical fiber through Meter Tests such as OTDR, PK2200, when
Optical fiber breaks into 1 circle bending radius when being 5mm, and the bending loss value obtained using two wavelength measurements of 1550nm, 1625nm is distinguished
In 0.029dB and 0.045dB；Decaying at 1310nm, 1383nm and 1550nm wavelength is respectively 0.328dB/km, 0.306dB/
km,0.198dB/km；Zero-dispersion slop is 0.078ps/ (nm^2*km), zero-dispersion wavelength 1318nm.
Although the present invention has been disclosed by way of example above, it is not intended to limit the present invention., any technical field
Middle tool usually intellectual, without departing from the spirit and scope of the invention, when can make it is a little change and retouch, therefore it is of the invention
Protection scope after view attached claim institute circle.
Claims (10)
1. a kind of manufacturing method of preform, which comprises the following steps:
Sandwich layer is provided, is sequentially depositing to form the first inner cladding and the second inner cladding in the core layer surface；
The sandwich layer for being formed with the first inner cladding and the second inner cladding is integrally impregnated into hovering in heating zone, is then taken off
Hydroxyl, vitrifying sintering are to form quartz glass bar；
Surrounding layer is formed on the quartz glass bar surface, obtains the preform.
2. manufacturing method as described in claim 1, which is characterized in that the process for forming surrounding layer is sprayed using surrounding layer
Lamp carries out the double-deck raw material and reacts to be formed, and the surrounding layer blowtorch includes blowtorch central core and blowtorch outer layer, the blowtorch central core
For being passed through fluoride and silicon tetrachloride, the blowtorch outer layer is used to be passed through the mixture of fluoride, oxygen, hydrogen and argon gas,
The quartz glass bar surface is deposited to carry out the double-deck raw material reaction generation fluorinated silicon dioxide powder particle.
3. manufacturing method as described in claim 1, which is characterized in that the sandwich layer uses sandwich layer by vapor axial method (VAD)
Blowtorch is passed through using germanium tetrachloride, silicon tetrachloride, oxygen, hydrogen and ar mixture as unstrpped gas, it is raw to carry out pyroreaction
It is formed at silica and germanium dioxide particle deposition, the flow proportional of the unstrpped gas is 1:10:30:30:15~1:20:
70:40:15。
4. manufacturing method as described in claim 1, which is characterized in that first inner cladding is adopted by vapor axial method (VAD)
With the first inner cladding blowtorch and auxiliary blowtorch, silicon tetrachloride, oxygen, hydrogen and argon gas are passed through to the first inner cladding blowtorch
Mixture carries out pyroreaction generation silicon dioxide microparticle and is deposited on the core layer surface, the silicon tetrachloride, oxygen, hydrogen
Flow proportional with the mixture of argon gas is 5:10:10:1~5:8:15:1；It is passed through hydrogen, oxygen to the auxiliary blowtorch,
The flame of the auxiliary blowtorch is coated with the silicon dioxide microparticle of the core layer surface deposition.
5. manufacturing method as described in claim 1, which is characterized in that second inner cladding is adopted by vapor axial method (VAD)
With the second inner cladding blowtorch, it is passed through the mixture of fluoride, silicon tetrachloride, oxygen, hydrogen and argon gas, carries out pyroreaction generation
Fluorine-containing silicon dioxide microparticle deposits, the fluoride, silicon tetrachloride, oxygen, hydrogen and argon gas mixture flow
Ratio is 0.1:5:10:10:1~0.05:5:8:15:1.
6. manufacturing method as described in claim 1, which is characterized in that the heating zone is the heating of integrated agglomerating plant
The heating zone in area, the integral sintering equipment is up to 2000mm or more.
7. manufacturing method as claimed in claim 2, which is characterized in that the formation surrounding layer is recessed including being formed from inside to outside
It falls into layer, the first surrounding layer and the second surrounding layer, the formation lower recess layer and is passed through the fluoride of the surrounding layer blowtorch, four
Silicon chloride, oxygen, hydrogen and argon gas the flow proportional of mixture be 0.2:5:10:10:1~0.4:5:8:15:1, the shape
The mixture of the fluoride of the surrounding layer blowtorch, silicon tetrachloride, oxygen, hydrogen and argon gas is passed through at the first surrounding layer
Flow proportional is 0.1:5:10:10:1~0.05:5:8:15:1, the surrounding layer blowtorch for forming the second surrounding layer and being passed through
The silicon tetrachloride, oxygen, hydrogen and argon gas the flow proportional of mixture be 5:10:10:1~5:8:15:1.
8. manufacturing method as claimed in claim 7, which is characterized in that the formation surrounding layer further includes that will be formed with lower recess
The quartz glass bar of layer, the first surrounding layer and the second surrounding layer integrally impregnates hovering in heating zone, then carries out deshydroxy, vitrifying
Sintering.
9. manufacturing method as claimed in claim 7, which is characterized in that the formation surrounding layer further include will first be formed with it is recessed
It falls into layer quartz glass bar and integrally impregnates hovering in heating zone, carry out deshydroxy, fluorine doped, vitrifying sintering, then from inside to outside successively
First surrounding layer and second surrounding layer are deposited, again deshydroxy, vitrifying sintering.
10. a kind of preform, which is characterized in that the preform successively includes sandwich layer, the first inner cladding, in second
Covering, lower recess layer, the first surrounding layer and the second surrounding layer,
The sandwich layer is the silica composition for mixing germanium (Ge), the relative fefractive index difference △ n of the sandwich layer1For 0.3%~
0.45%；
First inner cladding is pure silicon dioxide layer, the relative fefractive index difference △ n of first inner cladding2It is 0；
Second inner cladding is shallow fluorine doped layer, the relative fefractive index difference △ n of second inner cladding3For -0.05%~-
0.15%；
The lower recess layer is deep fluorine doped layer, the relative fefractive index difference △ n of the lower recess layer4It is -0.25%~-0.6%；
First surrounding layer is shallow fluorine doped layer, the relative fefractive index difference △ n of first surrounding layer5For -0.05%~-
0.15%；
Second surrounding layer is pure silicon dioxide layer, the relative fefractive index difference △ n of second surrounding layer6It is 0.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110221383A (en) * | 2019-07-12 | 2019-09-10 | 杭州金星通光纤科技有限公司 | A kind of single mode optical fiber and its manufacturing method |
| CN112441737A (en) * | 2019-08-30 | 2021-03-05 | 中天科技精密材料有限公司 | Preparation method of optical fiber and powder rod sintering equipment |
| WO2021164443A1 (en) * | 2020-02-18 | 2021-08-26 | 中天科技精密材料有限公司 | Small-diameter optical fiber and preparation method therefor |
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| CN114907007A (en) * | 2022-06-15 | 2022-08-16 | 山东富通光导科技有限公司 | Method for doping fluorine in optical fiber preform loose body |
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| CN112441737A (en) * | 2019-08-30 | 2021-03-05 | 中天科技精密材料有限公司 | Preparation method of optical fiber and powder rod sintering equipment |
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| WO2021164443A1 (en) * | 2020-02-18 | 2021-08-26 | 中天科技精密材料有限公司 | Small-diameter optical fiber and preparation method therefor |
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| CN114349327A (en) * | 2022-01-18 | 2022-04-15 | 江苏亨通光导新材料有限公司 | Low-cost processing technology of bending insensitive single-mode optical fiber |
| CN114907007A (en) * | 2022-06-15 | 2022-08-16 | 山东富通光导科技有限公司 | Method for doping fluorine in optical fiber preform loose body |
| CN114907007B (en) * | 2022-06-15 | 2024-02-02 | 山东富通光导科技有限公司 | Method for doping fluorine in optical fiber preform loose body |
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