CN107151092A - The preparation method and doped single crystal multi-core fiber of a kind of doped single crystal multi-core fiber - Google Patents

The preparation method and doped single crystal multi-core fiber of a kind of doped single crystal multi-core fiber Download PDF

Info

Publication number
CN107151092A
CN107151092A CN201710258664.1A CN201710258664A CN107151092A CN 107151092 A CN107151092 A CN 107151092A CN 201710258664 A CN201710258664 A CN 201710258664A CN 107151092 A CN107151092 A CN 107151092A
Authority
CN
China
Prior art keywords
core
single crystal
fiber
doped
doped single
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201710258664.1A
Other languages
Chinese (zh)
Other versions
CN107151092B (en
Inventor
张涛
辛凡
辛一凡
王敬轩
佟成国
李见奇
耿涛
王鹏飞
苑立波
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Harbin Engineering University
Original Assignee
Harbin Engineering University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Harbin Engineering University filed Critical Harbin Engineering University
Priority to CN201710258664.1A priority Critical patent/CN107151092B/en
Publication of CN107151092A publication Critical patent/CN107151092A/en
Application granted granted Critical
Publication of CN107151092B publication Critical patent/CN107151092B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Glass Compositions (AREA)
  • 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 fiber and doped single crystal multi-core fiber.Doped single crystal multi-core fiber is the doped single crystal fibre core containing two and the above in same silica clad, and fibre-optic waveguide structure is constituted by low refractive index silica quartz glass and high index of refraction doped single crystal.It is to obtain optical fiber preform, again porous capillary is obtained through drawing, then doped crystal melt is injected into formation polycrystal fibre core in many micropores in quartz capillary under high temperature, high pressure, eventually passes Transverse Heated so that fibre core completes the steps such as single crystallization to prepare silica clad doped single crystal multi-core fiber.By the way that melt injection in capillary porous is combined with later stage crystal growth, the doped single crystal multi-core fiber grown with this method has the advantages that controllable string diameter length, fibre core quantity and position arbitrary arrangement, phase-modulator, photoswitch and interferometer regulated and controled available for microminiature and online photon etc..

Description

The preparation method and doped single crystal multi-core fiber of a kind of doped single crystal multi-core fiber
Technical field
The present invention relates to a kind of optical fiber, more particularly to a kind of doped single crystal multi-core fiber.The invention further relates to this The manufacture method of optical fiber.
Background technology
Single crystal fiber is also referred to as crystal fibre or fibrous crystal, it be by crystal material growth be fibrous monocrystalline Body, diameter is arrived at several microns between hundreds of microns, and it has both the function of bulk crystals and general silica fibre.With bulk crystals phase Than the features such as single crystal fiber has small volume, integrated level height, can be coupled with silica fibre has compared with general silica fibre There is quality height, physical effect is strong, function is complete, preferably can match with all kinds of visible lasers with non-visible light wave band, energy The advantages of transmission for high power laser, there is important practical value in opto-electronics.
Common pure monocrystalline body function is limited, to obtain desired physical property, and often needs mix miscellaneous in crystal Prime element, such as Mg elements are mixed in nonlinear optics lithium columbate crystal can strengthen resisting laser damage ability, incorporation titanium, hydrogen member Element can improve crystal refractive index;A certain amount of phosphorus is mixed in semiconductor silicon crystal, n-type semiconductor is obtained, mixed a certain amount of Aluminium is sowed, and obtains p-type semiconductor;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 Drawn in the mould 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 has:[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.Should Method is to utilize CO2Laser is thermally formed after local melting zone, feed-in seed crystal and continuously grows mono-crystlling fibre.This method advantage is, Do not need pollution-free under mould and high temperature, high-melting-point optical fiber can be grown, growth rate is fast, but is limited by growth conditions System, can only often be made short fiber, and be difficult to control to fibre diameter.(3) straight forming method, the document and report being related to has: [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 so that melting using capillary effect Body disposable crystallisation solidification obtains crystal core fibre into crystal optical fibre, or by rod-in-tube technique and wire-drawing technology.But such is made Short fiber can only be made in Preparation Method, and fibre core is difficult to ensure that 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 is in one layer of low-refraction oxide monocrystal covering of single crystal fiber superficial growth.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 outside dimension is larger.Further, 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 so that the oxide coating for being coated in single crystal fiber top layer is diffused into optical fiber, reduction monocrystalline light is played Fine superficial layer refractive index.In the crystal optical fibre preparation method, crystal optical fibre covering intermediate ion is parabolically distributed, its covering folding Penetrate rate distribution also can gradually successively decrease from outside to inside, fibre loss can be caused to increase.In addition, this method poor controllability, diffusion path Degree is uneven, and diffusion depth should not be controlled, properties of product less stable.In addition, a kind of Chinese patent (microstructure cladding monocrystalline Optical fiber and preparation method, CN102298170A;One kind has bragg structure cladding monocrystalline optical fiber and preparation method, CN102253445A the single crystal fiber preparation method that a kind of microstructure cladding and crystal core are constituted) is disclosed.This method is, first Hollow covering set is prepared, micro-dimension monocrystal is inserted into hollow covering set, then heating stretching covering set makes fibre core quilt Covering set is wrapped, and microstructure cladding monocrystalline optical fiber is made.The method for preparing optical fiber the disadvantage is that, first, due to surface electrostatic Sucking action, it is difficult to which micro- monocrystal of long yardstick is inserted into covering set micropore;Second, quartz glass softening temperature point and crystalline substance The big difference of bulk melting point, causes to occur fibre core melt volatilization generation during covering set is stretched discontinuously or lacks, Yi Jishi English is dissolved in fibre core melt, is produced impurity pollution and is hindered the crystallization process of fibre core melt, does not become monocrystal;Third, Covering set draw temperature gradient is not met far above promoting fibre core melt crystallization forming core, growing up to form the thermograde power of monocrystalline The dynamic conditions of crystal growth.
In summary, involved crystal optical fibre before, or to be difficult to ensure that without cladding structure, or fibre core as monocrystalline The fibre core of a clean crystals is generally comprised only in body, and optical fiber, is not related to ion doping, therefore prepared crystal optical fibre Function limitation, it is impossible to meet further Fibre Optical Sensor, tencel integrated device demand.
The content of the invention
It is an object of the invention to provide a kind of technique is simple and practical, obtained optical fiber silica clad external diameter and monocrystalline core diameter The preparation method of the uniform doped single crystal multi-core fiber of controllable, crystalline quality.The present invention also aims to provide one kind to have both The doped single crystal multi-core fiber of the function of bulk crystals and general silica fibre.
The preparation method of doped single crystal multi-core fiber of the present invention is:
Step one:Optical fiber preform is obtained by accumulating beam method or quartz pushrod punch method, and with oxyhydrogen flame to porous Preform one end carries out heating sealing, then coordinates pumping, aerating device, using fiber drawing tower more than 1900 DEG C Optical fiber preform is drawn into porous capillary by temperature;
Step 2:It will be equipped with crucible in the platinum of doped polycrystalline powder to be nested in sealed tungsten outer crucible, place together Doped polycrystalline powder in being caused in high temperature Muffle furnace with the temperature heating of a little higher than polycrystal powder fusing point in crucible is completely melt In superheat state, inert gas is then filled with into outer crucible inside by outer crucible closure one raised endoporus, maintained Constant positive pressure, porous capillary one end is more from another raised endoporus on outer crucible closure is inserted into interior crucible melt The hole capillary other end is connected with outside air extractor so that constant negative pressure is formed in capilar bore, in inflation malleation 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 many Crystalline substance, obtains doped polycrystalline multi-core fiber;
Step 3:The doped polycrystalline multi-core fiber of preparation is positioned over into the horizontal fiber with rolling clamp to draw on cone machine, Optical fiber is while transverse rotation, and micro- heater is moved in heating optical fiber, micro- heater from one end to the other side along guide rail Heart temperature is higher than fibre core polycrystalline bulk melting point but less than quartzy softening point temperature, and now the fibre core in doped polycrystalline multi-core fiber is heated Into melt, extramural cladding keeps quartz glass solid-state, and fibre core melts under micro-dimensioned capillary endoporus and thermograde dynamic action Body crystallization nucleation, generation monocrystal of growing up, are made doped single crystal multi-core fiber;
Step 4:After the fiber core between fixture two ends completes single crystallization, the fiber section of mobile non-single crystallization is extremely Fibre core in rolling clamp two ends, the process of repeat step one to three, whole doped polycrystalline multi-core fiber all realizes single crystallization.
The manufacture method of the doped single crystal multi-core fiber of the present invention can also include:
1st, obtaining the method for optical fiber preform is:Quartzy capillary rod is first chosen, beam is accumulated with accumulation technology formation, will Quartzy capillary rod in accumulation beam on two and above position replaces with the quartz capillary of phase 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 optical fiber preform one end is entered with oxyhydrogen flame Row heating sealing.
2nd, obtaining the method for optical fiber preform is:Two and above through hole are made a call on one section of stuffed quartz rod, then The thin-walled quartz ampoule of equal outside dimension is welded in quartz pushrod one end, welded type optical fiber preform is constituted, and use hydrogen-oxygen Flame carries out heating sealing to the optical fiber preform other end.
The present invention doped single crystal multi-core fiber be:Containing two crystal fibre cores in silica clad, two crystal fibre core positions It is set to asymmetric or symmetric distribution.
The present invention doped single crystal multi-core fiber be:Simultaneously containing three crystal fibre cores, three crystal fibres in silica clad Core position is distributed into isosceles triangle or in-line.
The present invention doped single crystal multi-core fiber be:Simultaneously containing four crystal fibre cores, four crystal fibres in silica clad The rectangularity distribution of core position.
The present invention doped single crystal multi-core fiber be:Simultaneously containing five crystal fibre cores, five crystal fibres in silica clad Core position is symmetrically distributed.
The doped single crystal multi-core fiber of the present invention, it is different according to fibre core material and Doped ions, difference can also be realized Monocrystalline fibre core and the multi-core fiber of different ions doping.
The doped single crystal multi-core fiber of the present invention is the doped single crystal fibre core containing two and the above in same silica clad, And fibre core crystalline melting point is less than silica clad softening point.
The invention provides a kind of function of having both bulk crystals and general silica fibre, block doped crystal is had Desirable physical, the light conductivity and geometry of optical characteristics and optical fiber organically combine, can be applied to Fibre Optical Sensor, new The doped single crystal multi-core fiber of fiber type integrated device.Present invention also offers a kind of preparation technology is simple and practical, obtained light Fine silica clad external diameter and monocrystalline core diameter are controllable, the manufacture method of the uniform doped single crystal multi-core fiber of crystalline quality.
Compared with prior art, advantages of the present invention is:
1st, the doped single crystal multi-core 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 and optical fiber that body has are organically combined, and can be made many The optical fiber optical device of function is planted, is widely used in novel optical fiber sensing and fiber optic communication field.
2nd, contain multiple crystal fibre cores simultaneously in the doped single crystal multi-core fiber silica clad made, can flexibly realize The doped single crystal optical fiber of a variety of fibre core arrangements, preparation technology is simple and practical.
3rd, in doped single crystal multi-core fiber preparation process, porous capillary is prepared first, then utilizes high pressure technique will Filling melt realizes fibre core single crystallization using heating post processing mode in porous, finally.Based on this technical process, Ke Yifang Just the preparation of the multi-core 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 species of doped single crystal multi-core fiber, especially to doping For the preparation method of monocrystalline multi-core fiber, manufacture craft is simple, and cheap cost will be helpful to it to introduce to the market.
Brief description of the drawings
Fig. 1 is the 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 the unsymmetrical diplopore capillary schematic cross-section shown in embodiment one;
Fig. 5 is that the unsymmetrical twin-core doped polycrystalline body optical fiber shown in embodiment one prepares schematic diagram;
Fig. 6 is double crucible partial enlarged drawings shown in Fig. 5;
Fig. 7 (a) is the closure front view of the outer crucible shown in Fig. 6, and Fig. 7 (b) is the close of the outer crucible shown in Fig. 6 Cover top view;
Fig. 8 is the gasket structure schematic diagram of the outer crucible shown in Fig. 6;
Fig. 9 (a) is the sealing nut front view on the outer crucible shown in Fig. 6, and Fig. 9 (b) is the outer crucible shown in Fig. 6 On sealing nut top view;
Figure 10 illustrates for the technique of fibre core single crystallization in the unsymmetrical twin-core doped polycrystalline body optical fiber shown in embodiment one Figure;
Figure 11 is along the thermo parameters method schematic diagram in the heated fiber cores on optical fiber axial direction direction shown in Figure 10;
Figure 12 (a) is extremely other doped single crystal multi-core fiber schematic cross-sections with 12 (e).
Embodiment
Illustrate below in conjunction with the accompanying drawings and the present invention is described in more detail:
The implication of each reference is on Figure of description:1- doped single crystal fibre cores;2- silica clads;3- quartz glass wools Thin rod;4- quartz glass capillaries;5- thin-walled quartz ampoules;6- quartz glass filler rods;7- quartz pushrods;8- through holes;9- pores; 10- silica clads;11- high-purity argon gas cylinders;12- pressure display tables;13- rubber tubes;14- furnace heating elements;15- tungsten pipes;16- Heating furnace;17- porous capillaries;18- rubber tubes;19- vavuum pumps;20- alumina fiber mats;21- tungsten crucibles;22- platinum earthenwares Crucible;23- melts;24- zirconium oxides are incubated sand;25- external screw threads;26- endoporus;27- external screw threads;28- round taper holes;29- internal threads; 30- endoporus;31- seal cap apertures;32- internal threads;33- fiber spinning fixtures;The micro- electric furnaces of 34-;35- doped polycrystalline bodies are more Core fibre;36- guide rails;37- monocrystalline cores;38- silica clads;39- fibre cores melting zone;40- polycrystalline cores;41- polycrystalline core and melting zone Solid liquid interface;42- monocrystalline core and the solid liquid interface in melting zone;I- combined type unsymmetrical diplopore preforms;II-welded type is non- Symmetric figure diplopore preform;III-unsymmetrical diplopore capillary;IV-bis- crucibles;V-outer crucible closure;VI-outer earthenware Crucible sealing gasket;Sealing nut on VII-outer crucible;The micro- heating furnace transverse shifting speed of v-;T1- single-crystal region temperature;T2- melting zone temperature Degree;T3- polycrystalline temperature.
Embodiment one
Fig. 1 is the cross-sectional view of the first Magnesium-doped lithium niobate monocrystal twin-core fiber of the present invention, and fibre core 1 is Magnesium-doped lithium niobate monocrystal, fibre core position is in asymmetric distribution, and covering 2 is quartz, and the refractive index of fibre core 1 is more than covering 2 Refractive index.
Inside and outside pair of crucible has been used in the manufacturing process of the present invention.With reference to Fig. 6, outer crucible 21 uses tungsten material, above With tungsten material closure V, the alumina fibre sealing 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 is passed through on aperture 31 and sealed crucible lid V on sealing nut VII After round taper hole 28, it is inserted into the melt 23 of interior crucible, the space between porous capillary and round taper hole uses aluminum oxide Fiber mat 20 is sealed.Interior crucible 22 uses platinum material, and the inside contains the gap between doped polycrystalline powder, inside and outside crucible Sand 24 is incubated filled with zirconium oxide, insulation is played and fixed interior crucible 22 is acted on;With reference to Fig. 7, sealed crucible lid V is convex containing two The endoporus risen, wherein raised interior a pore area external screw thread 25 and small endoporus 26, high purity inert gas is injected into outer earthenware from hole 26 Inside crucible 21, another raised interior pore area external screw thread 27 and tapered bore 28, tapered bore 28 are close filled with alumina fibre Packing 20, sealed crucible lid V carries internal thread 29, and it is connected with the external screw thread fitted seal on crucible 21;With reference to Fig. 8, oxidation Two circular ports 30 are carried on aluminum fiber sealing gasket VI, wherein a circular hole is communicated with the aperture 26 on closure V, another circular hole and Round taper hole 28 on closure V is communicated;With reference to Fig. 9, sealing nut VII carries an aperture 31, and optical fiber 17 passes through this hole, nut Inner surface carries internal thread 32, and it is connected with the fitted seal of external screw thread 27 of raised endoporus on outer crucible closure V.
With reference to Fig. 2 to Fig. 5, Figure 10 and Figure 11, Magnesium-doped lithium niobate monocrystal twin-core fiber shown in embodiment one Preparation method is comprised the steps of:
1) it is the quartz glass capillary rod 3 that 700mm external diameters are 1mm to choose length, and close-packed hexagonal accumulates to form accumulation beam, will The quartzy capillary rod on center and a non-central location in accumulation beam replaces with equal length, inside/outside diameter size Quartz capillary 4, then accumulation, which is got one's things ready into an internal-and external diameter, isLong 750mm Quartz glass tube 5 in, the end face of quartz glass tube 5 is exposed in accumulation beam side termination, between accumulation beam and quartz glass tube 5 Fill diameter in spaceQuartzy capillary rod 6, form combined type optical fiber preform I, such as Fig. 2 It is shown;Carry out heating sealing to optical fiber preform one end with oxyhydrogen flame, it is another expose the termination for having accumulation beam and be provided with take out Gas and aerating device, are evacuated, vacuum maintains 0.3 to the space between capillary rod, capillary and outer layer quartz socket tube ×105More than Pa;Capillary inside is inflated, capillary internal pressure is maintained~1000Pa;On wire-drawer-tower with Optical fiber preform is drawn into external diameter by more than 1900 DEG C of temperatureDiplopore capillary III, as shown in figure 4, Diplopore capillary includes twoUnsymmetrical micropore 9, and silica clad 10.
2) by doped with the congruent polycrystalline lithium niobate powder (Li/Nb=48.6 of micro-oxidation magnesium:51.4) it is positioned over platinum In crucible 22, then it is nested in tungsten crucible 21, is put into together in high temperature Muffle furnace 16, is positioned over the diplopore capillary in Muffle furnace The one end of pipe 17 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 is passed through It is connected after Muffle furnace by flexible pipe 18 with outside air extractor 19, with female one end of tungsten pipe 15 and sealed crucible lid V External screw thread 25 be connected, the other end of tungsten pipe 15 pass through Muffle furnace after be connected by flexible pipe 13 with outside high-purity high pressure argon gas bottle 11 Connect;Muffle furnace is warming up to a little higher than 1250 DEG C of lithium niobate crystal bulk melting point, but less than quartzy softening temperature so that mixing in crucible Miscellaneous polycrystal powder is completely melt to be in hot melt state, and now porous capillary still keeps quartz glass solid-state, and its one end does not have Enter into the melt 23 of interior crucible;By high-purity argon gas cylinder 11, pressure display table 12, flexible pipe 13 and tungsten pipe 15, in outside earthenware 21 Portion's insufflation gas, maintain constant positive pressure 0.2 × 106More than Mpa;By vavuum pump 19 and flexible pipe 18, to porous capillary pore 17 internal air exhaustings, form constant negative pressure 0.5 × 105More than Mpa, in inflation malleation with being evacuated under suction function, melt liquid 23 It is rapidly filled with porous in capillary, maintains malleation and negative pressure value constant, room temperature is down to programme-control cooling method, eliminates Optical fiber internal stress, fibre core melt solidification becomes polycrystalline, forms mg-doped lithium niobate polycrystal twin-core fiber 35;
3) doped polycrystalline body twin-core fiber 35 is positioned over into the horizontal fiber of rolling clamp 33 to draw on cone machine, such as Figure 10 institutes Show, optical fiber is rotated with~10r/min speed, micro- electric furnace 34 is under stepper motor drive, along guide rail from one end to another End heating optical fiber is slowly moved with v=30~50mm/h speed;The a little higher than lithium niobate fibre core polycrystal of micro- heater center temperature 1250 DEG C of fusing point, but less 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 is a solid liquid interface 41 and 42 both sides, and extramural cladding 38 is still protected Hold quartz glass solid-state;The thermograde of solid liquid interface 42 between the core region of heating, melting zone 39 and monocrystal 37 is (T2-T1), in the region, under micro-dimensioned capillary endoporus and thermograde dynamic action, fibre core melt crystallization forming core, grow 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 is moved forward With the interface between polycrystal 40, the thermograde in the region is (T1-T3), T here2> T1=T3;When between the two ends of fixture 33 Fiber core complete after single crystallization, above-mentioned mistake is repeated several times to rolling clamp two ends in the fiber section of mobile non-single crystallization Fibre core in journey, so whole doped polycrystalline body twin-core fiber all realizes single crystallization.
Embodiment two
With reference to 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 length 70mm stuffed quartz rod IIHole 8, then in quartz pushrod The thin-walled quartz ampoule of the upper equal outside dimension of one end welding, heating sealing, structure are carried out with oxyhydrogen flame to the cell quartz rod other end Into welded type diplopore preform, install and be inflated inside aerating device, device to hole 8 in quartz ampoule one end, maintain malleation Power is in~1000Pa;Diplopore preform is drawn into by external diameter with more than 1900 DEG C of temperature on wire-drawer-tower Diplopore capillary III, diplopore capillary include twoAsymmetric micropore 9, and silica clad 10.Remaining work Skill process is identical with embodiment one.
According to the preparation method of doped single crystal multi-core fiber set forth in the present invention, fibre core difference arrangement knot can also be realized The monocrystalline multi-core fiber of structure.For example: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)) or other any angles position Put the twin-core fiber of relation.Identical process can prepare the doped single crystal multi-core fiber of other species, such as isosceles three Angular three core fibre (shown in such as Figure 12 (b)), the core fibre of in-line three (shown in such as Figure 12 (c)), rectangle four-core fiber is (as schemed Shown in 12 (d)), the core fibre of symmetric figure five (shown in such as Figure 12 (e)).
According to the preparation method of doped single crystal multi-core fiber set forth in the present invention, according to fibre core material and Doped ions Difference, can also realize the multi-core fiber of different monocrystalline fibre cores and doping.For example:Magnesium lithium tantalate list is mixed with nonlinear effect (during incorporation material is magnesia, preparation process, electric furnace temperature is a little higher than on Muffle furnace and optical fiber to draw cone machining for brilliant multi-core fiber Monocrystalline lithium tantalate fusing point, but less than quartzy softening temperature);(mix material is the semiconductor silicon single crystal multi-core fiber of p-doped or aluminium In phosphorus or aluminium simple substance, preparation process, a little higher than silicon single crystal fusing point of electric furnace temperature on Muffle furnace and optical fiber to draw cone machining, but be less than Quartzy softening temperature);(incorporation material is borontrifluoride samarium to samarium calcium fluoride mono crystal multi-core fiber etc. of mixing with laser characteristics, and is prepared During, a little higher than calcium fluoride mono crystal fusing point of electric furnace temperature on Muffle furnace and optical fiber to draw cone machining, but less than quartz softening temperature Degree).

Claims (7)

1. a kind of preparation method of doped single crystal multi-core fiber, it is characterized in that:
Step one:Optical fiber preform is obtained by accumulating beam method or quartz pushrod punch method, and with oxyhydrogen flame to porous optical fiber Prefabricated rods one end carries out heating sealing, then coordinates pumping, aerating device, utilizes temperature of the fiber drawing tower more than 1900 DEG C Optical fiber preform is drawn into porous capillary;
Step 2:It will be equipped with crucible in the platinum of doped polycrystalline powder to be nested in sealed tungsten outer crucible, height be positioned over 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 Superheat state, is then filled with inert gas into outer crucible inside by outer crucible closure one raised endoporus, maintains constant Normal pressure, porous capillary one end is from another raised endoporus on outer crucible closure is inserted into interior crucible melt, porous hair The tubule other end is connected with outside air extractor so that constant negative pressure is formed in capilar bore, in inflation malleation 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 fiber;
Step 3:The doped polycrystalline multi-core fiber of preparation is positioned over into the horizontal fiber with rolling clamp to draw on cone machine, optical fiber While transverse rotation, micro- heater moves heating optical fiber, micro- heater center temperature from one end to the other side along guide rail Higher than fibre core polycrystalline bulk melting point but less than quartzy softening point temperature, now the fibre core in doped polycrystalline multi-core fiber is heated to form molten Body, extramural cladding keeps quartz glass solid-state, the fibre core melt knot under micro-dimensioned capillary endoporus and thermograde dynamic action Crystalline form core, generation monocrystal of growing up, are made doped single crystal multi-core fiber;
Step 4:After the fiber core between fixture two ends completes single crystallization, the fiber section of mobile non-single crystallization extremely rotates Fibre core in fixture two ends, the process of repeat step one to three, whole doped polycrystalline multi-core fiber all realizes single crystallization.
2. the manufacture method of doped single crystal multi-core fiber according to claim 1, it is characterized in that:Obtain porous optical fiber prefabricated The method of rod is:Quartzy capillary rod is first chosen, with accumulation technology formation accumulation beam, by two in accumulation beam and above position Quartzy capillary rod replaces with the quartz capillary of phase 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 manufacture method of doped single crystal multi-core fiber according to claim 1, it is characterized in that:Obtain porous optical fiber prefabricated The method of rod is:Two and above through hole are made a call on one section of stuffed quartz rod, then the equal external diameter in the welding of quartz pushrod one end The thin-walled quartz ampoule of size, constitutes welded type optical fiber preform, and the optical fiber preform other end is entered with oxyhydrogen flame Row heating sealing.
4. doped single crystal multi-core fiber made from a kind of manufacture method of the doped single crystal multi-core fiber described in claim 1, its It is characterized in:Containing two crystal fibre cores in silica clad, two crystal fibre core positions are distributed into asymmetric or symmetric.
5. doped single crystal multi-core fiber made from a kind of manufacture method of the doped single crystal multi-core fiber described in claim 1, its It is characterized in:Simultaneously containing three crystal fibre cores in silica clad, three crystal fibre core positions are divided into isosceles triangle or in-line Cloth.
6. doped single crystal multi-core fiber made from a kind of manufacture method of the doped single crystal multi-core fiber described in claim 1, its It is characterized in:Simultaneously containing four crystal fibre cores, four crystal fibre core position rectangularity distributions in silica clad.
7. doped single crystal multi-core fiber made from a kind of manufacture method of the doped single crystal multi-core fiber described in claim 1, its It is characterized in:Simultaneously containing five crystal fibre cores in silica clad, five crystal fibre core positions are symmetrically distributed.
CN201710258664.1A 2017-04-19 2017-04-19 A kind of preparation method and doped single crystal multi-core optical fiber of doped single crystal multi-core optical fiber Active CN107151092B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710258664.1A CN107151092B (en) 2017-04-19 2017-04-19 A kind of preparation method and doped single crystal multi-core optical fiber of doped single crystal multi-core optical fiber

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710258664.1A CN107151092B (en) 2017-04-19 2017-04-19 A kind of preparation method and doped single crystal multi-core optical fiber of doped single crystal multi-core optical fiber

Publications (2)

Publication Number Publication Date
CN107151092A true CN107151092A (en) 2017-09-12
CN107151092B CN107151092B (en) 2019-09-27

Family

ID=59792641

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710258664.1A Active CN107151092B (en) 2017-04-19 2017-04-19 A kind of preparation method and doped single crystal multi-core optical fiber of doped single crystal multi-core optical fiber

Country Status (1)

Country Link
CN (1) CN107151092B (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108411359A (en) * 2018-02-27 2018-08-17 同济大学 A kind of method of the interior growth Crystal cladding of metal tube
CN108456926A (en) * 2018-02-27 2018-08-28 同济大学 A kind of method of the interior growth crystal optical fibre fibre core of Crystal cladding
CN108594359A (en) * 2018-05-09 2018-09-28 上海大学 Niobic acid lithium doping silica fibre
CN109592894A (en) * 2018-12-25 2019-04-09 通鼎互联信息股份有限公司 A kind of drawing optical fibers sealing device and encapsulating method
CN111170629A (en) * 2020-01-09 2020-05-19 华南理工大学 Fiber core single crystallization post-processing method and fiber core single crystallization device
CN111424318A (en) * 2020-06-10 2020-07-17 眉山博雅新材料有限公司 Method for preparing doped YAG single crystal optical fiber
CN112255710A (en) * 2020-11-03 2021-01-22 山东大学 Full single crystal optical fiber modified based on ion implantation technology, preparation method, numerical aperture regulation and control and application thereof
CN114355504A (en) * 2021-12-16 2022-04-15 中科南京未来能源系统研究院 Preparation method of semiconductor core fiber

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1605894A (en) * 2004-11-18 2005-04-13 上海大学 Magneto-optic effect photon crystal fiber and manufacturing method thereof
CN102298170A (en) * 2011-08-22 2011-12-28 北京交通大学 Microstructure cladding monocrystalline optical fiber and preparation method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1605894A (en) * 2004-11-18 2005-04-13 上海大学 Magneto-optic effect photon crystal fiber and manufacturing method thereof
CN102298170A (en) * 2011-08-22 2011-12-28 北京交通大学 Microstructure cladding monocrystalline optical fiber and preparation method

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108411359A (en) * 2018-02-27 2018-08-17 同济大学 A kind of method of the interior growth Crystal cladding of metal tube
CN108456926A (en) * 2018-02-27 2018-08-28 同济大学 A kind of method of the interior growth crystal optical fibre fibre core of Crystal cladding
CN108411359B (en) * 2018-02-27 2020-11-27 同济大学 Method for growing crystal cladding in metal tube
CN108594359A (en) * 2018-05-09 2018-09-28 上海大学 Niobic acid lithium doping silica fibre
CN109592894A (en) * 2018-12-25 2019-04-09 通鼎互联信息股份有限公司 A kind of drawing optical fibers sealing device and encapsulating method
CN111170629A (en) * 2020-01-09 2020-05-19 华南理工大学 Fiber core single crystallization post-processing method and fiber core single crystallization device
CN111170629B (en) * 2020-01-09 2022-06-07 华南理工大学 Fiber core single crystallization post-processing method and fiber core single crystallization device
CN111424318A (en) * 2020-06-10 2020-07-17 眉山博雅新材料有限公司 Method for preparing doped YAG single crystal optical fiber
US11136690B1 (en) 2020-06-10 2021-10-05 Meishan Boya Advanced Materials Co., Ltd. Method for preparing doped yttrium aluminum garnet single crystal fiber by performing a cylindrical surface polishing operation and growing a cladding layer
CN112255710A (en) * 2020-11-03 2021-01-22 山东大学 Full single crystal optical fiber modified based on ion implantation technology, preparation method, numerical aperture regulation and control and application thereof
CN114355504A (en) * 2021-12-16 2022-04-15 中科南京未来能源系统研究院 Preparation method of semiconductor core fiber
CN114355504B (en) * 2021-12-16 2024-03-12 中科南京未来能源系统研究院 Preparation method of semiconductor core fiber

Also Published As

Publication number Publication date
CN107151092B (en) 2019-09-27

Similar Documents

Publication Publication Date Title
CN107151092B (en) A kind of preparation method and doped single crystal multi-core optical fiber of doped single crystal multi-core optical fiber
CN106980152B (en) Method for preparing embedded lithium niobate or lithium tantalate single-crystal-core optical fiber and single-crystal-core optical fiber
CN108418085B (en) Full crystal optical fiber and cladding manufacturing process
CN1984850B (en) Optical fiber and its preform as well as method and apparatus for fabricating them
KR101375622B1 (en) Silica glass crucible with barium-doped inner wall
JP4466813B2 (en) Glass preform and method for producing the same
CN105264125B (en) Garnet type single crystal and its manufacture method
CN111170629B (en) Fiber core single crystallization post-processing method and fiber core single crystallization device
CN102815864B (en) Preparation method of photonic crystal optical fiber
EP0348935B1 (en) Method for producing glass preform for optical fiber
CN106995277A (en) A kind of preparation method of chalcogenide glass photon crystal optical fiber preformed rod
CN108456926A (en) A kind of method of the interior growth crystal optical fibre fibre core of Crystal cladding
CN103361727A (en) Sapphire single crystal and making method thereof
CN106477874A (en) A kind of fiber core index modulation method
CN103255477B (en) The growing method of a kind of shaped sapphire crystal and equipment
US11352713B2 (en) Heat shield structure for single crystal production furnace and single crystal production furnace
CN1583617A (en) Method for preparing photon crystal optical fibre and apparatus therefor
CN1084398C (en) Equipment for growing high-temp oxide crystal
JP2021517975A (en) Photonic crystal fiber and its manufacturing method
CN116791200A (en) Device and method for growing silicon carbide crystal by liquid phase method
CN101228299A (en) Silicon single crystal drawing device and method thereof
CN201406482Y (en) Metallic heater for growing big size vanadic acid illinium crystals by top seed crystal soaking growing method
TW202117098A (en) A semiconductor crystal growth apparatus
CN219342380U (en) Thermal field
CN104692650A (en) Equipment and method for preparing optical fiber

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant