CN110217981A - A kind of single crystal fiber and preparation method thereof - Google Patents
A kind of single crystal fiber and preparation method thereof Download PDFInfo
- Publication number
- CN110217981A CN110217981A CN201910504127.XA CN201910504127A CN110217981A CN 110217981 A CN110217981 A CN 110217981A CN 201910504127 A CN201910504127 A CN 201910504127A CN 110217981 A CN110217981 A CN 110217981A
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- Prior art keywords
- glass
- single crystal
- crystal fiber
- preparation
- clad
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
- C03B37/025—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from reheated softened tubes, rods, fibres or filaments, e.g. drawing fibres from preforms
- C03B37/027—Fibres composed of different sorts of glass, e.g. glass optical fibres
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/02—Optical fibres with cladding with or without a coating
- G02B6/02395—Glass optical fibre with a protective coating, e.g. two layer polymer coating deposited directly on a silica cladding surface during fibre manufacture
Abstract
The invention discloses a kind of single crystal fiber and preparation method thereof, single crystal fiber includes fibre core, inner cladding and surrounding layer, and fibre core is solid mono-crystlling fibre.Preparation method includes preparing the prefabricated rods of the matched more tubular glass of internal-and external diameter；Wire drawing is carried out to prefabricated rods, obtains the glass-clad of double-layer structure；Solid mono-crystlling fibre is inserted into inner cladding, heating is carried out and draws cone, obtain the single crystal fiber with glass-clad.Tubular element material that the present invention uses, quantity, size, position is adjustable, and optically and thermally performance can be matched with monocrystal material to the greatest extent, so as to ensure the mode quality and high power operating of single crystal fiber；Also have many advantages, such as that structure is simple simultaneously, it is convenient to prepare, and it is the ideal covering preparation method of single crystal fiber that the covering for having broken traditional single crystal fiber, which prepares the bottleneck that difficult,.
Description
Technical field
The invention belongs to crystal optical fibre fields, more particularly, to a kind of single crystal fiber and preparation method thereof.
Background technique
Crystal optical fibre is different from conventional quartz optical fiber, is with crystal (such as: sapphire, YAG, sesquichloride crystal) conduct
Medium, a kind of special construction between traditional fiber and bulk crystals using waveguiding structure as beam Propagation channel.Cause
And crystal optical fibre the advantages of being provided with optical fiber and crystal medium simultaneously.Compared with conventional quartz optical fiber, crystal optical fibre has more preferable
Physical property.By taking YAG crystal as an example, thermal conductivity an order of magnitude higher than glass optical fiber, therefore the heat dissipation of YAG crystal optical fibre
Performance is more preferable；Secondly, the fusing point of YAG crystal has reached about 2000 DEG C, there is the damage threshold bigger than silica fibre.In addition,
The stimulated Brillouin scattering coefficient of YAG crystal optical fibre is 10 times of quartz glass optical fiber, therefore has higher excited Brillouin
Scatter threshold value.These physical characteristics, it is possible to which the output power bottleneck for inherently solving current high-capacity optical fiber laser is beaten
The power limit of broken optical fiber laser, obtains the output of higher power.In addition, high temperature, high pressure, intense radiation, strong electromagnetic, easily
It fires the extreme environments such as explosive, strong corrosive and is widely present in the numerous areas such as industry, national defence, aerospace, such as: metallurgy, petroleum
Exploitation, thermal power generation, nuclear energy power generation, aerospace detection, missile guidance and internal combustion engine, engine, turbine and rocket propulsion
Deng.However, few sensors are capable of providing accurately and reliably temperature, pressure, health operating at present under these extreme conditions
Etc. information, this also becomes the problem lain across in scientific circles and industry.Due to crystal optical fibre with higher fusing point and more preferably
Corrosion resistance, thus sensed in extreme circumstances using crystal optical fibre substitution silica fibre and also have become the hair of industry
Exhibition trend.
The covering of single crystal fiber will at least meet the refractive index lower than crystal fibre core, the thermal expansion coefficient close to fibre core, tool
There is the chemical structure at heat chemistry and mechanical stability, core-clad interface and balance each other and stablizes these characteristics.Single crystal fiber
Clad material mainly includes glass material and two kinds of crystalline material, and crystalline material covering is generally used and specifically physically or chemically applied
Coating process, higher to reaction condition demand, preparation process is relative complex, and the Crystal cladding refractive index prepared can not regulate and control.With
Compare, the optical properties such as the refractive index of glass material such as lanthanide glass, quartz glass, silicate glass etc. and thermal expansion coefficient
It may be implemented to regulate and control on a large scale with thermal property, so as to ensure the mode quality and high power operating of crystal optical fibre.
The hot drawing process for being suitable for the materials such as traditional silica fibre at present is not particularly suited for crystalline material, crystalline material
It will become glassy state under hot-drawn environment, and existing crystal optical fibre preparation process has no cladding structure, is not stricti jurise
On optical fiber, naked fibre is easy by pollutant effects in environment to be generated serious decaying, and furthermore naked fibre and air be between the two
Refractive index it is too big, the refractive index in air is uneven, and fluctuation is big, bad control.Crystal naked fibre adds covering that can enhance
Mechanical performance, constitutes optical waveguide at thermal property, can control transmission mode, and then be applied to optical-fiber laser, so crystal
Material is needed by being further processed addition cladding structure to form crystal optical fiber.
Summary of the invention
In view of the drawbacks of the prior art, the purpose of the present invention is to provide a kind of single crystal fibers and preparation method thereof, it is intended to
The covering preparation for solving conventional crystal optical fiber is higher to demands such as experimental facilities, reaction conditions, and preparation process is relative complex to be asked
Topic.
To achieve the above object, it is an aspect of this invention to provide that providing a kind of single crystal fiber, including fibre core, inner cladding
And surrounding layer；Fibre core is solid mono-crystlling fibre；The outside of fibre core is successively coated with inner cladding and surrounding layer from inside to outside.
Preferably, the shape of inner cladding is round, hexagon or octagon.
Preferably, evenly distributed single-layer or multi-layer glass tube between inner cladding and surrounding layer, number are 3~200.
Preferably, the clad material of single crystal fiber is lanthanide glass, quartz glass, silicate glass or phosphate glass
Glass.
Preferably, the inside diameter ranges of the covering of single crystal fiber are 10 μm~1mm, are matched with the size of fibre core.
Preferably, the material of monocrystalline fibre core is sapphire, yttrium-aluminium-garnet (YAG), luteium oxide (Lu2O3), zirconium oxide
(ZrO2), borate (Ca4O(BO3)3) or any of the above-described kind of monocrystalline is rare earth doped, transition metal element doped, mixes
Miscellaneous rare earth ion includes Nd3+、Yb3+、Tm3+、Ho3+、Er3+、Pr3+、Sm2+Deng transition metal ions includes Cr3+、Ti3+、Ni2+、
Co2+Deng.
The glass-clad of single crystal fiber provided by the invention and the refractive index of monocrystalline core material are as shown in table 1:
Table 1
It is another aspect of this invention to provide that providing a kind of preparation method of single crystal fiber, comprising:
(1) prefabricated rods of the matched more tubular glass of internal-and external diameter are prepared；
(2) wire drawing is carried out to prefabricated rods, obtains the glass-clad of double-layer structure；
(3) it by the inner cladding of solid mono-crystlling fibre insertion glass-clad, carries out heating and draws cone, obtain with glass-clad
Single crystal fiber.
It is primarily design structure, prepares the prefabricated rods of glass-clad, glass-clad is made in hot-drawn；Micro-structure light is used again
Fibre draws cone technique that cladding structure melting is coated on solid mono-crystlling fibre and constitutes single crystal fiber.
Further, the prefabricated rods of the matched more tubular glass of internal-and external diameter are prepared specifically includes the following steps:
(1) multiple first glass are uniformly fixed according to inner cladding preset shape and is in control a stack；
(2) laminated components are inserted into the second glass tube.
Preferably, the prefabricated rods for preparing the matched more tubular glass of internal-and external diameter further include the laminated components and the second glass
The same end of glass pipe is fixed.
Preferably, controlled when carrying out wire drawing to the prefabricated rods using two stage pressures, wherein inside stack using it is micro- just
Pressure；Using the micro-positive pressure or tiny structure less than the former between second glass tube and stack.
Preferably, the glass-clad thickness control that heating draws cone to be prepared is in 10um~2mm.
Preferably, the length range for the single crystal fiber being prepared is 1cm~100cm.
Contemplated above technical scheme through the invention, compared with prior art, can obtain it is following the utility model has the advantages that
1, the present invention provides a kind of single crystal fibers with glass-clad structure, compared to the preparation of conventional crystal optical fiber
The Crystal cladding for growing low-refraction using physical/chemical gas-phase deposition on naked fibre surface, exist to experimental facilities,
Many defects such as the demands such as reaction condition are higher, and the amorphous cladding index of preparation is uncontrollable, and crystal growth rate is limited are asked
Topic, the optical property between glass material and monocrystal material that the present invention uses match with calorifics, and process simply may be used
Row, material and preparation cost are low, greatly reduce the covering preparation process difficulty of single crystal fiber, have broken traditional single crystal fiber
Coat demand of the Crystal cladding to experimental facilities, reaction condition etc. is higher, and preparation process is relative complex, light heat performance can not
Many barriers such as regulation；
2, the present invention provides a kind of, and cone technique is drawn in the single crystal fiber heating with glass-clad, by preparing wire drawing
Obtained glass-clad center is inserted directly into existing solid mono-crystlling fibre, is ensuring not occurring between fibre core and covering opposite move
After dynamic, glass-clad is made just to be nested in solid mono-crystlling fibre by control heating temperature, tensile speed and stretching time
On, and guarantee that the specific form structure of glass tube itself does not change, obtain the single crystal fiber with core pack arrangement；
3, the present invention studies different shape using the close glass material of refractive index and thermal expansion coefficient as clad material
Influence with the glass-clad of structure to single crystal fiber waveguide performance, the optical properties such as glass materials refractive index and thermal expansion coefficient
It may be implemented to regulate and control on a large scale with thermal property, so as to ensure the mode quality and high power operating of single crystal fiber；
4, the single crystal fiber with glass-clad that the present invention obtains is that the laser of based single crystal optical fiber or sensor mention
Research foundation is supplied, single crystal fiber not only has many advantages, such as optical fiber, as good, light-weight, small in size, the anti-electromagnetism of light conductivity is dry
It disturbs, and since itself material is monocrystalline, so the characteristic intrinsic with monocrystalline again, theoretically single crystal fiber allows to export
Energy can reach 50 times of current glass optical fiber, and single crystal fiber is expected to break the output limit of existing fiber laser, make optical fiber
The output power of laser realizes that great-leap-forward increases.In addition, it is dry to be also widely applied to high temperature, high pressure, intense radiation, strong electromagnetic
It disturbs, is inflammable and explosive, the extreme environments such as strong corrosive.
Detailed description of the invention
Fig. 1 is single crystal fiber structural schematic diagram provided by the invention；
Fig. 2 is the cladding structure schematic diagram of single crystal fiber provided in an embodiment of the present invention；
Fig. 3 is the cladding structure schematic diagram for the single crystal fiber that further embodiment of this invention provides；
Fig. 4 is the structural schematic diagram of the covering preparation facilities of single crystal fiber provided in an embodiment of the present invention；
Fig. 5 is the structural schematic diagram of single crystal fiber provided in an embodiment of the present invention；
Fig. 6 is the drawing cone schematic diagram of single crystal fiber provided in an embodiment of the present invention；
Fig. 7 is the drawing cone system block diagram of single crystal fiber provided in an embodiment of the present invention；
Attached drawing mark:
1, surrounding layer, 2, inner cladding, 3, prefabricated rods folder, 4, two stage pressure control joints, 5, prefabricated rods, 6, heating furnace, 7,
Laser diameter measuring instrument, 8, traction device, 9, cutter device, 10, glass-clad, 11, fibre core.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting conflict each other can be combined with each other.
As shown in Figure 1, the present invention provides a kind of single crystal fiber, including fibre core, inner cladding and surrounding layer；Fibre core is solid
Mono-crystlling fibre；The outside of fibre core is successively coated with inner cladding and surrounding layer from inside to outside.
Specifically, the shape of inner cladding is round, hexagon or octagon.
Specifically, evenly distributed single-layer or multi-layer glass tube between inner cladding and surrounding layer, number are 3~200.
Specifically, the clad material of single crystal fiber is lanthanide glass, quartz glass, silicate glass or phosphate glass
Glass.
Specifically, the inside diameter ranges of the covering of single crystal fiber are 10 μm~1mm, are matched with the size of fibre core.
Specifically, the material of fibre core is sapphire, yttrium-aluminium-garnet (YAG), luteium oxide (Lu2O3), zirconium oxide (ZrO2)、
Borate (Ca4O(BO3)3) or any of the above-described kind of monocrystalline rare earth doped, transition metal element doped, the rare earth of doping
Ion includes Nd3+、Yb3+、Tm3+、Ho3+、Er3+、Pr3+、Sm2+Deng transition metal ions includes Cr3+、Ti3+、Ni2+、Co2+Deng.
It is another aspect of this invention to provide that providing a kind of preparation method of single crystal fiber, comprising:
(1) prefabricated rods of the matched more tubular glass of internal-and external diameter are prepared；
(2) wire drawing is carried out to prefabricated rods, obtains the glass-clad of double-layer structure；
(3) it by the inner cladding of solid mono-crystlling fibre insertion glass-clad, carries out heating and draws cone, obtain with glass-clad
Single crystal fiber.
Further, the prefabricated rods of the matched more tubular glass of internal-and external diameter are prepared specifically includes the following steps:
(1) multiple first glass are uniformly fixed according to inner cladding preset shape and is in control a stack；
(2) laminated components are inserted into the second glass tube.
Specifically, the prefabricated rods for preparing the matched more tubular glass of internal-and external diameter further include the laminated components and described
The same end of two glass tubes is fixed.
Specifically, controlled when carrying out wire drawing to the prefabricated rods using two stage pressures, wherein inside stack using it is micro- just
Pressure；Using the micro-positive pressure or tiny structure less than the former between second glass tube and stack.
Specifically, the length range for the single crystal fiber being prepared is 1cm~100cm.
As shown in Fig. 2, the covering of single crystal fiber include positioned at outermost surrounding layer and surrounding layer inner surface setting by
The fibre core that several tubulose original parts stack the inner cladding of composition and determined by inner cladding.Wherein inner cladding is with a tubulose member
Centered on part, uniform ring is around one layer of several tubular element.As shown in figure 3, inner cladding is centered on a tubular element,
Even several tubular elements of circular multilayer layer.
Wherein clad material is silicate glass and air, and fibre core is monocrystalline Lu2O3Fiber, the monocrystalline with glass-clad
Method for preparing optical fiber is summarized are as follows: the monocrystalline naked fibre of micron-scale is inserted into capillary by design structure, arrangement and drawing capillary
In pipe inner cladding, local heating draws cone to obtain the single crystal fiber with glass-clad.
The preparation methods of prefabricated rods the following steps are included:
(1) selecting specification is outer diameter 20mm, internal diameter 14mm and outer diameter 13mm, internal diameter 9mm, and length is the silicate of 40cm
Glass tube carries out casing, and the joining place of two certain one end of pipe is fastened with raw material band.
(2) 5 outer diameter 2.50mm, internal diameter 1.95mm are taken, length is the silicate glass tubule of 45cm, is with wherein one
Center, around its evenly distributed 4 other tubule, one end is fixed using AB glue, guarantees that it is not relatively moved.
(3) 5 hole laminated components are inserted into the ring sleeve in (1), and one end of laminated components will have more about 3cm,
The port of the port and outer ring winding raw material band, the port that laminated components are fixed with AB glue is in the same direction, laminated components and outer ring casing
Between one end joining place also with raw material band winding stopper fixation, to guarantee that it is not relatively moved.
Preparation facilities is as shown in figure 4, include that prefabricated rods press from both sides 3, two stage pressure control joints 4, heating furnace 6, laser diameter measuring instrument
7, traction device 8 and cutter device 9.
The drawing methods of prefabricated rods the following steps are included:
(1) fixing end of prefabricated rods 6 is put into two special stage pressure control joints 4, two stage pressure control interfaces 5 are by pre-
Stick folder 3 processed is clamped, and to 50mbar micro-positive pressure is used inside the laminated components, use -2.50KPa is micro- negative inside external eyelet thimble
Prefabricated rods are inserted into moderate oven, and guarantee that prefabricated rods are located at the center of moderate oven by pressure.
(2) moderate oven 6 is waited to heat up, the temperature setting of four heating zones of moderate oven is respectively 880 DEG C, 983 DEG C, 740
DEG C, 400 DEG C, wherein final stage be annealing section.After Heating Zone Temperature slowly reaches set temperature, fire door is used under moderate oven
Heating state of the sem observation prefabricated rods in furnace is reflected, after prefabricated rods softening is turned around, chieftain is cut, passes sequentially through fiber sharp
Light caliper 7, traction device 8, finally the fixed length cutting capillary glass tube at cutter device 9
(3) it controls into rod speed (default νfeed=0.5mm/min), silk speed (default ν is received in adjustmentdraw=0.32m/min)
It can reach required fiber size (dfiber=800 μm, 78 μm of capillary center bore).Fixed length cutting is long at cutter device 10
The capillary glass tube of 40cm, what is obtained is the glass-clad 10 to post-processing.
As shown in figure 5, the mono-crystlling fibre 11 of long 45cm is inserted into glass-clad by 30 μm of outer diameter, one end is fixed to guarantee it
It does not relatively move.
The drawing of single crystal fiber is bored the following steps are included: as shown in fig. 6, the single crystal fiber that Fig. 5 is obtained is fixed on drawing frustum
On, wait the temperature of heating zone to rise to 850 DEG C, drawing is bored in 100 μm/min along the drawing cone speed control at cone direction both ends is drawn
Fiber cross-sections before show that there are certain gaps between mono-crystlling fibre and capillary pipe-in-pipe, draw the single crystal fiber after cone to cut
Face shows that covering has been nested on mono-crystlling fibre, and the specific form structure of covering does not change.Fig. 7 is of the invention real
Optical fiber used in example draws cone system, and main includes drawing cone machine host, atmospheric control etc..By drawing the monocrystalline light after boring
Fine outer diameter is 310 μm, 280 μm of cladding thickness.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of single crystal fiber, which is characterized in that including fibre core, inner cladding and surrounding layer；
The fibre core is solid mono-crystlling fibre；The outside of the fibre core is successively coated with inner cladding and surrounding layer from inside to outside.
2. single crystal fiber according to claim 1, which is characterized in that the shape of the inner cladding be round, hexagon or
Person's octagon.
3. single crystal fiber according to claim 1, which is characterized in that the clad material of the single crystal fiber is group of the lanthanides glass
Glass, quartz glass, silicate glass or phosphate glass.
4. single crystal fiber according to any one of claims 1 to 3, which is characterized in that the covering of the single crystal fiber it is interior
Diameter range is 10 μm~1mm.
5. single crystal fiber according to claim 1, which is characterized in that the material of the fibre core is sapphire, yttroalumite pomegranate
Stone, luteium oxide, zirconium oxide, borate or any of the above-described kind of crystal it is rare earth doped, transition metal element doped.
6. a kind of preparation method of single crystal fiber, which comprises the following steps:
(1) prefabricated rods of the matched more tubular glass of internal-and external diameter are prepared；
(2) wire drawing is carried out to the prefabricated rods, obtains the glass-clad of double-layer structure；
(3) solid mono-crystlling fibre is inserted into the inner cladding of the glass-clad, carries out heating and draw cone, obtains with glass-clad
Single crystal fiber.
7. preparation method according to claim 6, which is characterized in that described to prepare the matched more tubular glass of internal-and external diameter
Prefabricated rods specifically includes the following steps:
(1) multiple first glass are uniformly fixed according to inner cladding preset shape and is in control a stack；
(2) stack is inserted into the second glass tube.
8. preparation method according to claim 6, which is characterized in that have between inner cladding and surrounding layer evenly distributed
Single-layer or multi-layer hollow glass tube.
9. preparation method according to claim 7, which is characterized in that described to prepare the matched more tubular glass of internal-and external diameter
Prefabricated rods further include that the same end of the stack and second glass tube is fixed.
10. preparation method according to claim 6, which is characterized in that used when the progress wire drawing to the prefabricated rods
The control of two stage pressures, wherein uses positive pressure inside stack；Using just less than the former between second glass tube pipe and stack
Pressure or negative pressure.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021087716A1 (en) * | 2019-11-05 | 2021-05-14 | 南京同溧晶体材料研究院有限公司 | Phosphate glass coated europium-lutetium-doped sapphire crystal material and preparation method therefor |
| CN112939443A (en) * | 2021-01-29 | 2021-06-11 | 华南理工大学 | High borosilicate glass cladding cesium iodide single crystal core optical fiber and preparation method and application thereof |
| CN115182044A (en) * | 2022-07-27 | 2022-10-14 | 山东铂锐激光科技有限公司 | Method for preparing sesquioxide single crystal optical fiber cladding |
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| CN102253445A (en) * | 2011-07-14 | 2011-11-23 | 北京交通大学 | Single crystal fiber with Bragg structure cladding 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 |
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- 2019-06-12 CN CN201910504127.XA patent/CN110217981A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102253445A (en) * | 2011-07-14 | 2011-11-23 | 北京交通大学 | Single crystal fiber with Bragg structure cladding 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 (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021087716A1 (en) * | 2019-11-05 | 2021-05-14 | 南京同溧晶体材料研究院有限公司 | Phosphate glass coated europium-lutetium-doped sapphire crystal material and preparation method therefor |
| CN112939443A (en) * | 2021-01-29 | 2021-06-11 | 华南理工大学 | High borosilicate glass cladding cesium iodide single crystal core optical fiber and preparation method and application thereof |
| CN115182044A (en) * | 2022-07-27 | 2022-10-14 | 山东铂锐激光科技有限公司 | Method for preparing sesquioxide single crystal optical fiber cladding |
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Application publication date: 20190910 |