CN107151092B - A kind of preparation method and doped single crystal multi-core optical fiber of doped single crystal multi-core optical fiber - Google Patents

A kind of preparation method and doped single crystal multi-core optical fiber of doped single crystal multi-core optical fiber Download PDF

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CN107151092B
CN107151092B CN201710258664.1A CN201710258664A CN107151092B CN 107151092 B CN107151092 B CN 107151092B CN 201710258664 A CN201710258664 A CN 201710258664A CN 107151092 B CN107151092 B CN 107151092B
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optical fiber
core
single crystal
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doped single
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CN107151092A (en
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张涛
辛一凡
王敬轩
佟成国
李见奇
耿涛
王鹏飞
苑立波
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Harbin Engineering University
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01Manufacture of glass fibres or filaments
    • C03B37/012Manufacture of preforms for drawing fibres or filaments
    • C03B37/01205Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
    • C03B37/01262Depositing additional preform material as liquids or solutions, e.g. solution doping of preform tubes or rods
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01Manufacture of glass fibres or filaments
    • C03B37/012Manufacture of preforms for drawing fibres or filaments
    • C03B37/014Manufacture 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]
    • C03B37/01446Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering

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  • Optical Fibers, Optical Fiber Cores, And Optical Fiber Bundles (AREA)

Abstract

The present invention is to provide a kind of preparation method of doped single crystal multi-core optical fiber and doped single crystal multi-core optical fibers.Doped single crystal multi-core optical fiber be same silica clad include there are two or more doped single crystal fibre core, fibre-optic waveguide structure is constituted by low refractive index silica quartz glass and high refractive index doped single crystal.It is to obtain optical fiber preform, porous capillary is obtained through drawing again, then doped crystal melt is injected into more micropores in quartz capillary formation polycrystal fibre core under high temperature and pressure, finally by Transverse Heated make fibre core complete single crystallization and etc. prepare silica clad doped single crystal multi-core optical fiber.By the way that melt injection in capillary porous is combined with later period crystal growth, the doped single crystal multi-core optical fiber grown with this method has many advantages, such as controllable string diameter length, fibre core quantity and position arbitrary arrangement, can be used for phase-modulator, photoswitch and the interferometer etc. of microminiature and the regulation of online photon.

Description

A kind of preparation method and doped single crystal multi-core optical fiber of doped single crystal multi-core optical fiber
Technical field
The present invention relates to a kind of optical fiber, in particular to a kind of doped single crystal multi-core optical fiber.The invention further relates to this The manufacturing method of optical fiber.
Background technique
Single crystal fiber is also referred to as crystal fibre or fibrous crystal, and it is fibrous monocrystalline that it, which is by crystal material growth, Body, for diameter at several microns between hundreds of microns, it has both the function of bulk crystals and general silica fibre.With bulk crystals phase Than single crystal fiber has the characteristics that small in size, integrated level is high, can be coupled with silica fibre, has compared with general silica fibre Have that quality is high, physical effect is strong, function is complete, can preferably match with all kinds of visible lasers with non-visible light wave band, energy The advantages that transmission for high power laser, has important practical value in opto-electronics.
Common pure monocrystalline body function is limited, to obtain desired physical property, often needs to mix in crystal miscellaneous Prime element, such as incorporation Mg element can enhance resisting laser damage ability, incorporation titanium, hydrogen member in nonlinear optics lithium columbate crystal Element can improve crystal refractive index;A certain amount of phosphorus is mixed in semiconductor silicon crystal, obtains n-type semiconductor, is mixed a certain amount of Aluminium is sowed, and p-type semiconductor is obtained;Lanthanide series is mixed in crystal can obtain fluorescent characteristic material etc..
Common crystal optical fibre growing method has, and (1) EFG technique, the document and report being related to has: [1] Norio Ohnishi and Takafumi Yao,A Novel Growth Technique for Single-Crystal Fibers: The Micro-Czochralski(μ-CZ)Method,Jpn.J.Appl.Phys.,28(2):L278-L280;1989;[2] Dae-Ho Yoon,Ichiro Yonenaga,Tsuguo Fukuda,Norio Ohnishi,Crystal growth of dislocation-free LiNbO3single crystals by micro pulling down method, J.Cryst.Growth,142:339-343,1994;[3] Zhong Heyu, Hou Yinchun, wooden fork peaceful three, Chen Xingda, Wang Renshu, lithium niobate The growth of single crystal fiber, silicate journal, 19 (6): 527-531,1991.Such growing method is melt from aperture or convex It is drawn in the mold risen, oriented growth is carried out after feed-in seed crystal.Its major advantage can continuously grow longer and special cross-section Optical fiber, but limited by mold materials, it is difficult to dystectic brilliant fibre is grown, and is difficult to avoid that pollution problem.(2) laser heating pedestal Method, the document and report being related to have: [4] Yalin Lu, Dajani A.Iyad, and R.J.Knize, Fabrication and characterization of periodically poled lithium niobate single crystal fibers,Integrated Ferroelectrics,90:53-62,2007;[5] Japan Patent Production of Single Crystal Optical Fiber,Bibliographic data:JPH0375292(A)―1991-03-29.It should Method is to utilize CO2Laser is thermally formed local melting zone, continuously grows mono-crystlling fibre after feed-in seed crystal.This method advantage is, It does not need pollution-free under mold and high temperature, high-melting-point optical fiber can be grown, growth rate is fast, but the limit by growth conditions System can only often be made short fiber, and be difficult to control fibre diameter.(3) straight forming method, the document and report being related to have: [6]P.Rudolph,T.Fukuda,Fiber crystal growth from the melt,Crystal Research and Technology,34:3–40,1999;[7]J.Ballato,T.Hawkins,and P.Foy et al.Silicon optical fiber.Optics Express.2008 16:18675-18683;[8]Yi-Chung Huang,and Jau- Sheng Wang et al.Preform fabrication and fiber drawing of 320nm broadband Cr- doped fibers,Optics Express.2007,15:14382-14388.This method is to melt using capillary effect Body disposable crystallisation solidification obtains crystal core fibre at crystal optical fibre, or by rod-in-tube technique and wire-drawing technology.However such is made Short fiber can only be made in Preparation Method, and fibre core is difficult to ensure as monocrystal.(4) other growing methods, such as Japan Patent (Fibrous Oxide Optical Single Crystal and Its Production,Bibliographic data: JPH08278419 (A) -1996-10-22) a kind of preparation method of lithium columbate crystal core fibre is given, this method is to utilize Growth technology grows one layer of low-refraction oxide monocrystal covering on single crystal fiber surface.In the crystal optical fibre preparation method In, epitaxial layer oxide ester mp must be lower than single crystal fiber fusing point, while being limited by epitaxial layer melt, shift mechanism etc., growth Crystal optical fibre it is shorter, and outer diameter is larger.In addition, such as United States Patent (USP) (Method of cladding single crystal optical fiber,Patent Number,5077087;Claddings for single crystal optical fibers and devices and methods and apparatus for making such Claddings, Patent Number, 5037181) describe a kind of preparation method of doped lithium columbate single crystal fiber, this method By high-temperature process the oxide coating coated in single crystal fiber surface layer is diffused into optical fiber, playing reduces monocrystalline light Fine superficial layer refractive index.In the crystal optical fibre preparation method, crystal optical fibre covering intermediate ion is parabolically distributed, covering folding Penetrate rate distribution also can gradually successively decrease from outside to inside, will lead to fibre loss increase.In addition, this method poor controllability, diffusion path Degree is uneven, and diffusion depth should not control, and properties of product stability is poor.In addition, a kind of Chinese patent (microstructure cladding monocrystalline Optical fiber and preparation method, CN102298170A;One kind having bragg structure cladding monocrystalline optical fiber and preparation method, CN102253445A the single crystal fiber preparation method of a kind of microstructure cladding and crystal core composition) is disclosed.This method is, first Hollow covering set is prepared, micro-dimension monocrystal is inserted into hollow covering set, then heating, which stretches covering set, makes fibre core quilt Covering set wraps, and microstructure cladding monocrystalline optical fiber is made.The shortcomings that method for preparing optical fiber, is, first, due to surface electrostatic Sucking action is difficult to be inserted into micro- monocrystal of long scale in covering set micropore;Second, quartz glass softening temperature point and crystalline substance The big difference of bulk melting point causes fibre core melt volatilization generation occur discontinuously during stretching covering set or lack, Yi Jishi English is dissolved in fibre core melt, is generated impurity pollution and is hindered the crystallization process of fibre core melt, does not become monocrystal;Third, Covering set draw temperature gradient, which is much higher than, to be promoted fibre core melt crystallization forming core, grows up to form the temperature gradient power of monocrystalline, is not met The dynamic conditions of crystal growth.
In conclusion crystal optical fibre involved by front, or be difficult to ensure for no cladding structure or fibre core as monocrystalline Body, and the fibre core of a clean crystals is usually contained only in optical fiber, it is not related to ion doping, therefore prepared crystal optical fibre Function limitation is unable to satisfy further Fibre Optical Sensor, tencel integrated device demand.
Summary of the invention
The purpose of the present invention is to provide a kind of simple process is practical, optical fiber silica clad outer diameter and monocrystalline core diameter obtained Controllably, the preparation method of the uniform doped single crystal multi-core optical fiber of crystalline quality.The object of the invention is also to provide one kind to have both The doped single crystal multi-core optical fiber of the function of bulk crystals and general silica fibre.
Doped single crystal multi-core optical fiber of the invention the preparation method comprises the following steps:
Step 1: optical fiber preform is obtained by accumulation beam method or quartz pushrod punch method, and with oxyhydrogen flame to porous Preform one end carries out heating sealing, then cooperation pumping, air charging system, using fiber drawing tower at 1900 DEG C or more Optical fiber preform is drawn into porous capillary by temperature;
Step 2: crucible in the platinum equipped with doped polycrystalline powder is nested in the tungsten outer crucible of sealing, is placed together Doped polycrystalline powder in the temperature heating in high temperature Muffle furnace with a little higher than polycrystal powder fusing point causes in crucible is completely melt It is in an overheated state, inert gas is then filled with into outer crucible inside by outer crucible sealing cover one raised inner hole, is maintained Constant positive pressure, porous capillary one end is inserted into interior crucible melt from another raised inner hole on outer crucible sealing cover, more The hole capillary other end is connected with external air extractor, so that constant negative pressure is formed in capilar bore, in inflation positive pressure and pumping Under suction function, melt liquid be rapidly filled with capillary it is porous in, cooling eliminate optical fiber internal stress, melt solidification become more Crystalline substance obtains doped polycrystalline multi-core optical fiber;
Step 3: being placed in the horizontal fiber with rolling clamp for the doped polycrystalline multi-core optical fiber of preparation and draw on cone machine, For optical fiber while transverse rotation, micro- heating device moves heating optical fiber along guide rail from one end to the other side, in micro- heating device Heart temperature is higher than fibre core polycrystalline bulk melting point but lower than quartzy softening point temperature, and the fibre core in doped polycrystalline multi-core optical fiber is heated at this time At melt, extramural cladding keeps quartz glass solid-state, and fibre core is molten under micro-dimensioned capillary inner hole and the effect of temperature gradient power Body crystallization nucleation, growing up generates monocrystal, and doped single crystal multi-core optical fiber is made;
Step 4: after the fiber core between fixture both ends completes single crystallization, the fiber section of mobile non-single crystallization is extremely Rolling clamp both ends, repeat the process of step 1 to three, and the fibre core in whole doped polycrystalline multi-core optical fiber all realizes single crystallization.
The manufacturing method of doped single crystal multi-core optical fiber of the invention can also include:
1, the method for obtaining optical fiber preform is: quartzy capillary stick first chosen, forms accumulation beam with accumulation technology, it will Quartzy capillary stick in accumulation beam on two or more position replaces with the quartz capillary of same material, and then accumulation is got one's things ready Enter in thin-walled quartz glass tube, constitute combined type optical fiber preform, and with oxyhydrogen flame to optical fiber preform one end into Row heating sealing.
2, the method for obtaining optical fiber preform is: beating two or more through-hole on one section of stuffed quartz stick, then The thin-walled quartz ampoule of upper same outer diameter is welded in quartz pushrod one end, constitutes welded type optical fiber preform, and use hydrogen-oxygen Flame carries out heating sealing to the optical fiber preform other end.
Doped single crystal multi-core optical fiber of the invention is: silica clad is included there are two crystal fibre core, two crystal fibre core positions It is set to asymmetric or symmetric distribution.
Doped single crystal multi-core optical fiber of the invention is: in silica clad while containing there are three crystal fibre core, three crystal fibres Core position is distributed at isosceles triangle or linear type.
Doped single crystal multi-core optical fiber of the invention is: in silica clad while containing there are four crystal fibre core, four crystal fibres The distribution of core position rectangularity.
Doped single crystal multi-core optical fiber of the invention is: in silica clad while containing there are five crystal fibre core, five crystal fibres Core position is symmetrically distributed.
Doped single crystal multi-core optical fiber of the invention, it is different according to fibre core material and Doped ions, it can also realize difference The multi-core optical fiber of monocrystalline fibre core and different ions doping.
Doped single crystal multi-core optical fiber of the invention be same silica clad include there are two or more doped single crystal fibre core, And fibre core crystalline melting point is lower than silica clad softening point.
The present invention provides a kind of functions of having both bulk crystals and general silica fibre, and bulk doped crystal is had Desirable physical, optical characteristics and optical fiber light conductivity and geometry organically combine, can be applied to Fibre Optical Sensor, new The doped single crystal multi-core optical fiber of fiber type integrated device.The present invention also provides a kind of preparation process is simple and practical, light obtained Fine silica clad outer diameter and monocrystalline core diameter is controllable, manufacturing method of the uniform doped single crystal multi-core optical fiber of crystalline quality.
Compared with prior art, advantages of the present invention are as follows:
1, the doped single crystal multi-core optical fiber made has both the function of bulk crystals and general silica fibre, and bulk doping is brilliant The light conductivity and geometry of desirable physical, optical characteristics possessed by body and optical fiber organically combine, and can be made more The optical fiber optical device of kind function is widely used in novel optical fiber sensing and fiber optic communication field.
2, contain multiple crystal fibre cores simultaneously in the doped single crystal multi-core optical fiber silica clad made, can flexibly realize The doped single crystal optical fiber of a variety of fibre core arrangements, preparation process are simple and practical.
3, in doped single crystal multi-core optical fiber preparation process, porous capillary is prepared first, then utilizes high pressure technique will Melt is filled into porous, finally realizes fibre core single crystallization using heating post processing mode.Based on this technical process, Ke Yifang Just the preparation of the multi-core optical fiber of different monocrystalline fibre core materials and doping is realized, crystal defect is few, and the monocrystalline core fibre of growth is longer.
The invention of above-mentioned optic fibre manufacturing technology has widened the type of doped single crystal multi-core optical fiber, especially to doping For the preparation method of monocrystalline multi-core optical fiber, manufacture craft is simple, and cheap cost will be helpful to it to introduce to the market.
Detailed description of the invention
Fig. 1 is unsymmetrical twin-core doped single crystal fiber cross-sections schematic diagram shown in embodiment one;
Fig. 2 to Fig. 3 is two kinds of unsymmetrical diplopore preform schematic cross-sections shown in embodiment one;
Fig. 4 is unsymmetrical diplopore capillary schematic cross-section shown in embodiment one;
Fig. 5 is that unsymmetrical twin-core doped polycrystalline body optical fiber shown in embodiment one prepares schematic diagram;
Fig. 6 is double crucible partial enlarged views shown in Fig. 5;
Fig. 7 (a) is the sealing cover main view of outer crucible shown in Fig. 6, and Fig. 7 (b) is the close of outer crucible shown in Fig. 6 Cover top view;
Fig. 8 is the gasket structure schematic diagram of outer crucible shown in Fig. 6;
Fig. 9 (a) is the sealing nut main view on outer crucible shown in Fig. 6, and Fig. 9 (b) is outer crucible shown in Fig. 6 On sealing nut top view;
Figure 10 is the technique signal of fibre core single crystallization in unsymmetrical twin-core doped polycrystalline body optical fiber shown in embodiment one Figure;
Figure 11 is the thermo parameters method schematic diagram being heated in fiber cores shown in Figure 10 on optical fiber axial direction direction;
Figure 12 (a) is extremely other doped single crystal multi-core optical fiber schematic cross-sections with 12 (e).
Specific embodiment
It illustrates with reference to the accompanying drawing and the present invention is described in more detail:
The meaning of each appended drawing reference on Figure of description are as follows: 1- doped single crystal fibre core;2- silica clad;3- quartz glass wool Thin stick;4- quartz glass capillary;5- thin-walled quartz ampoule;6- quartz glass filler rod;7- quartz pushrod;8- through-hole;9- pore; 10- silica clad;11- high-purity argon gas cylinder;12- pressure display table;13- rubber tube;14- furnace heating elements;15- tungsten pipe;16- Heating furnace;17- porous capillary;18- rubber tube;19- vacuum pump;20- alumina fiber mat;21- tungsten crucible;22- platinum earthenware Crucible;23- melt;24- zirconium oxide keeps the temperature sand;25- external screw thread;26- inner hole;27- external screw thread;28- round taper hole;29- internal screw thread; 30- inner hole;31- seal cap aperture;32- internal screw thread;33- fiber spinning fixture;The micro- electric furnace of 34-;35- doped polycrystalline body is more Core fibre;36- guide rail;37- monocrystalline core;38- silica clad;39- fibre core melting zone;40- polycrystalline core;41- polycrystalline core and melting zone Solid liquid interface;The solid liquid interface of 42- monocrystalline core and melting zone;I- combined type unsymmetrical diplopore preform;II-welded type is non- Symmetric figure diplopore preform;III-unsymmetrical diplopore capillary;IV-bis- crucibles;V-outer crucible sealing cover;VI-outer earthenware Crucible gasket;Sealing nut on VII-outer crucible;The micro- heating furnace transverse shifting speed of v-;T1Single-crystal region temperature;T2Melting zone temperature Degree;T3Polycrystalline temperature.
Embodiment one
Fig. 1 is the cross-sectional view of the first Magnesium-doped lithium niobate monocrystal twin-core fiber of the invention, and fibre core 1 is Magnesium-doped lithium niobate monocrystal, fibre core position are in asymmetric distribution, and covering 2 is quartz, and the refractive index of fibre core 1 is greater than covering 2 Refractive index.
Inside and outside double crucibles have been used in manufacturing process of the invention.In conjunction with Fig. 6, outer crucible 21 uses tungsten material, above With tungsten material sealing cover V, the alumina fibre gasket VI of high temperature resistant (1800 DEG C), outer crucible sealing are filled therebetween Contain a sealing nut VII on lid V, porous capillary 17 passes through on aperture 31 and sealed crucible lid V on sealing nut VII It after round taper hole 28, is inserted into the melt 23 of interior crucible, the gap between porous capillary and round taper hole uses aluminium oxide Fiber mat 20 is sealed.Interior crucible 22 uses platinum material, and the inside contains doped polycrystalline powder, the gap between inside and outside crucible Sand 24 is kept the temperature filled with zirconium oxide, plays the role of heat preservation and fixed interior crucible 22;In conjunction with Fig. 7, sealed crucible lid V is convex containing two The inner hole risen, wherein pore area external screw thread 25 and small inner hole 26, high purity inert gas are injected into outer earthenware from hole 26 in a protrusion Inside crucible 21, pore area external screw thread 27 and tapered bore 28 in another protrusion, it is close that tapered bore 28 is filled with alumina fibre Packing 20, sealed crucible lid V have internal screw thread 29, it cooperates with the external screw thread on crucible 21 is tightly connected;In conjunction with Fig. 8, oxidation Two round holes 30 are had on aluminum fiber gasket VI, wherein a circular hole is communicated with the aperture 26 on sealing cover V, another circular hole and Round taper hole 28 on sealing cover V communicates;In conjunction with Fig. 9, sealing nut VII has an aperture 31, and optical fiber 17 passes through this hole, nut Inner surface has internal screw thread 32, the cooperation sealed connection of external screw thread 27 of it and inner hole raised on outer crucible sealing cover V.
In conjunction with Fig. 2 to Fig. 5, Figure 10 and Figure 11, Magnesium-doped lithium niobate monocrystal twin-core fiber shown in embodiment one Preparation method comprises the steps of:
1) choosing length is the quartz glass capillary stick 3 that 700mm outer diameter is 1mm, and close-packed hexagonal accumulates to form accumulation beam, will The quartzy capillary stick on center and a non-center position in accumulation beam replaces with equal length, inside/outside diameter size Quartz capillary 4, then accumulation is got one's things ready is into an internal-and external diameterLong 750mm Quartz glass tube 5 in, the end face of quartz glass tube 5 is exposed in accumulation beam side end, accumulates between beam and quartz glass tube 5 Fill diameter in gapQuartzy capillary stick 6, combined type optical fiber preform I is formd, such as Fig. 2 It is shown;Heating sealing is carried out to optical fiber preform one end with oxyhydrogen flame, another exposing has the end of accumulation beam to be equipped with pumping Gas and air charging system are evacuated the gap between capillary stick, capillary and outer layer quartz socket tube, and vacuum degree maintains 0.3 ×105Pa or more;Capillary inside is inflated, capillary internal pressure is made to maintain~1000Pa;On wire-drawer-tower with Optical fiber preform is drawn into outer diameter by 1900 DEG C or more of temperatureDiplopore capillary III, as shown in figure 4, Diplopore capillary includes twoUnsymmetrical micropore 9 and silica clad 10.
2) platinum will be placed in doped with the congruent polycrystalline lithium niobate powder (Li/Nb=48.6:51.4) of micro-oxidation magnesium It in crucible 22, is then nested in tungsten crucible 21, is put into togerther in high temperature Muffle furnace 16, the diplopore capillary being placed in Muffle furnace 17 one end of pipe is inserted into polycrystalline lithium niobate powder after passing through the round taper hole 28 on sealed crucible lid V, and the capillary other end passes through It is connected by hose 18 with external air extractor 19 after Muffle furnace, on band 15 one end of internal thread tungsten pipe and sealed crucible lid V External screw thread 25 be connected, 15 other end of tungsten pipe is connected by hose 13 with the high-purity high pressure argon gas bottle 11 in outside after passing through Muffle furnace It connects;Muffle furnace is warming up to 1250 DEG C of a little higher than lithium niobate crystal bulk melting point, but lower than quartzy softening temperature, so that mixing in crucible Miscellaneous polycrystal powder is completely melt to be in hot melt state, and porous capillary still keeps quartz glass solid-state at this time, and one end does not have Enter into the melt 23 of interior crucible;By high-purity argon gas cylinder 11, pressure display table 12, hose 13 and tungsten pipe 15, in outside earthenware 21 Portion is filled with gas, maintains constant positive pressure 0.2 × 106Mpa or more;By vacuum pump 19 and hose 18, to porous capillary pore 17 internal air exhaustings form constant negative pressure 0.5 × 105Mpa or more, under inflation positive pressure and pumping suction function, melt liquid 23 It is rapidly filled in porous in capillary, maintains positive pressure and negative pressure value constant, room temperature is down to process control cooling method, eliminate Optical fiber internal stress, the solidification of fibre core melt become polycrystalline, form mg-doped lithium niobate polycrystal twin-core fiber 35;
3) horizontal fiber that doped polycrystalline body twin-core fiber 35 is placed in rolling clamp 33 is drawn on cone machine, such as Figure 10 institute Show, optical fiber is rotated with the speed of~10r/min, and micro- electric furnace 34 is under stepper motor drive, along guide rail from one end to another End heating optical fiber is moved slowly with v=30~50mm/h speed;The a little higher than lithium niobate fibre core polycrystal of micro- heating device center temperature 1250 DEG C of fusing point, but lower than quartzy 1730 DEG C of softening point temperature.By taking one of fibre core as an example, as shown in figure 11, doped polycrystalline Fibre core in body twin-core fiber is heated to form melting zone 39, and respectively there are a solid liquid interface 41 and 42 in two sides, and extramural cladding 38 is still protected Hold quartz glass solid-state;In the core region of heating, the temperature gradient of the solid liquid interface 42 between melting zone 39 and monocrystal 37 is (T2-T1), in the region, under micro-dimensioned capillary inner hole and the effect of temperature gradient power, fibre core melt crystallization forming core is grown up Monocrystal 37 is generated, the single crystallization process of fibre core is completed;Another solid liquid interface 41 is melting zone 39 when micro- heating furnace moves forward With the interface between polycrystal 40, the temperature gradient in the region is (T1-T3), T here2> T1=T3;When between 33 both ends of fixture Fiber core complete single crystallization after, above-mentioned mistake is repeated several times to rolling clamp both ends in the fiber section of mobile non-single crystallization Journey, the fibre core in whole doped polycrystalline body twin-core fiber so all realize single crystallization.
Embodiment two
In conjunction with Fig. 3 and Fig. 4, the preparation method of another Magnesium-doped lithium niobate monocrystal twin-core fiber of the invention For in one section of diameterTwo diameters are made a call on the stuffed quartz stick II of length 70mmHole 8, then in quartz pushrod The thin-walled quartz ampoule of upper same outer diameter is welded in one end, carries out heating sealing, structure to the cell quartz stick other end with oxyhydrogen flame At welded type diplopore preform, air charging system is installed in quartz ampoule one end, is inflated inside device to hole 8, maintains positive pressure Power is in~1000Pa;Diplopore preform is drawn by outer diameter with 1900 DEG C or more of temperature on wire-drawer-tower Diplopore capillary III, diplopore capillary include twoAsymmetric micropore 9 and silica clad 10.Remaining work Skill process is the same as example 1.
The preparation method of the doped single crystal multi-core optical fiber illustrated according to the present invention can also realize fibre core difference arrangement knot The monocrystalline multi-core optical fiber of structure.Such as: it may be constructed according to position difference of the doped single crystal twin-core fiber in covering circular cross-section Unsymmetrical twin-core fiber (as shown in Figure 1), symmetric figure twin-core fiber (shown in such as Figure 12 (a)) either other any angle positions Set the twin-core fiber of relationship.Identical process can prepare the doped single crystal multi-core optical fiber of other types, such as isosceles three Angular three core fibre (shown in such as Figure 12 (b)), three core fibre of linear type (shown in such as Figure 12 (c)), rectangle four-core fiber is (as schemed Shown in 12 (d)), five core fibre of symmetric figure (shown in such as Figure 12 (e)).
The preparation method of the doped single crystal multi-core optical fiber illustrated according to the present invention, according to fibre core material and Doped ions Difference can also realize the multi-core optical fiber of different monocrystalline fibre cores and doping.Such as: magnesium lithium tantalate list is mixed with nonlinear effect (incorporation substance is magnesia, and in preparation process, it is a little higher than that Muffle furnace and optical fiber to draw cone machining power on furnace temp for brilliant multi-core optical fiber Monocrystalline lithium tantalate fusing point, but lower than quartzy softening temperature);(mix substance is the semiconductor silicon single crystal multi-core optical fiber of p-doped or aluminium Phosphorus or aluminium simple substance, in preparation process, Muffle furnace and optical fiber to draw cone machining power on a little higher than silicon single crystal fusing point of furnace temp, but are lower than Quartzy softening temperature);(incorporation substance is borontrifluoride samarium, preparation to samarium calcium fluoride mono crystal multi-core optical fiber etc. of mixing with laser characteristics In the process, Muffle furnace and optical fiber to draw cone machining power on a little higher than calcium fluoride mono crystal fusing point of furnace temp, but lower than quartz softening temperature Degree).

Claims (7)

1. a kind of preparation method of doped single crystal multi-core optical fiber, it is characterized in that:
Step 1: optical fiber preform is obtained by accumulation beam method or quartz pushrod punch method, and with oxyhydrogen flame to porous optical fiber Prefabricated rods one end carries out heating sealing, then cooperation pumping, air charging system, the temperature using fiber drawing tower at 1900 DEG C or more Optical fiber preform is drawn into porous capillary;
Step 2: crucible in the platinum equipped with doped polycrystalline powder is nested in the tungsten outer crucible of sealing, is placed in height together The doped polycrystalline powder in interior crucible is caused to be completely melt to be in the temperature heating of a little higher than polycrystal powder fusing point in warm Muffle furnace Then superheat state is filled with inert gas into outer crucible inside by outer crucible sealing cover one raised inner hole, maintains constant Normal pressure, porous capillary one end are inserted into interior crucible melt from another raised inner hole on outer crucible sealing cover, porous hair The tubule other end is connected with external air extractor, so that constant negative pressure is formed in capilar bore, in inflation positive pressure and pumping negative pressure Under effect, melt liquid be rapidly filled with capillary it is porous in, cooling eliminate optical fiber internal stress, melt solidification become polycrystalline, obtain To doped polycrystalline multi-core optical fiber;
Step 3: being placed in the horizontal fiber with rolling clamp for the doped polycrystalline multi-core optical fiber of preparation and draw on cone machine, optical fiber While transverse rotation, micro- heating device moves heating optical fiber, micro- heating device center temperature along guide rail from one end to the other side Degree is higher than fibre core polycrystalline bulk melting point but lower than quartzy softening point temperature, and the fibre core in doped polycrystalline multi-core optical fiber is heated to form at this time Melt, extramural cladding keep quartz glass solid-state, the fibre core melt under micro-dimensioned capillary inner hole and the effect of temperature gradient power Crystallization nucleation, growing up generates monocrystal, and doped single crystal multi-core optical fiber is made;
Step 4: after the fiber core between fixture both ends completes single crystallization, the fiber section of mobile non-single crystallization extremely rotates Fixture both ends, repeat the process of step 3, and the fibre core in whole doped polycrystalline multi-core optical fiber all realizes single crystallization.
2. the preparation method of doped single crystal multi-core optical fiber according to claim 1, it is characterized in that: it is prefabricated to obtain porous optical fiber The method of stick is: the quartzy capillary stick of first selection forms accumulation beam with accumulation technology, will accumulate in beam on two or more position Quartzy capillary stick replaces with the quartz capillary of same material, and then accumulation is got one's things ready in thin-walled quartz glass tube, constitutes multiple Box-like optical fiber preform, and heating sealing is carried out to optical fiber preform one end with oxyhydrogen flame.
3. the preparation method of doped single crystal multi-core optical fiber according to claim 1, it is characterized in that: it is prefabricated to obtain porous optical fiber The method of stick is: beating two or more through-hole on one section of stuffed quartz stick, then welds upper same outer diameter in quartz pushrod one end The thin-walled quartz ampoule of size, constitute welded type optical fiber preform, and with oxyhydrogen flame to the optical fiber preform other end into Row heating sealing.
4. doped single crystal multi-core optical fiber made from a kind of preparation method of doped single crystal multi-core optical fiber described in claim 1, Be characterized in: silica clad is included there are two crystal fibre core, and two crystal fibre core positions are distributed at asymmetric or symmetric.
5. doped single crystal multi-core optical fiber made from a kind of preparation method of doped single crystal multi-core optical fiber described in claim 1, Be characterized in: in silica clad while containing there are three crystal fibre core, three crystal fibre core positions are divided at isosceles triangle or linear type Cloth.
6. doped single crystal multi-core optical fiber made from a kind of preparation method of doped single crystal multi-core optical fiber described in claim 1, It is characterized in: in silica clad while containing there are four crystal fibre core, four crystal fibre core position rectangularity distributions.
7. doped single crystal multi-core optical fiber made from a kind of preparation method of doped single crystal multi-core optical fiber described in claim 1, Be characterized in: crystal fibre core there are five containing in silica clad simultaneously, five crystal fibre core positions are symmetrically distributed.
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