CN112939443B - High borosilicate glass cladding cesium iodide single crystal core optical fiber and preparation method and application thereof - Google Patents
High borosilicate glass cladding cesium iodide single crystal core optical fiber and preparation method and application thereof Download PDFInfo
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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
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/01205—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
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- 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
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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
- C03B37/10—Non-chemical treatment
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/05—Construction or shape of optical resonators; Accommodation of active medium therein; Shape of active medium
- H01S3/06—Construction or shape of active medium
- H01S3/063—Waveguide lasers, i.e. whereby the dimensions of the waveguide are of the order of the light wavelength
- H01S3/067—Fibre lasers
- H01S3/06708—Constructional details of the fibre, e.g. compositions, cross-section, shape or tapering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/05—Construction or shape of optical resonators; Accommodation of active medium therein; Shape of active medium
- H01S3/06—Construction or shape of active medium
- H01S3/063—Waveguide lasers, i.e. whereby the dimensions of the waveguide are of the order of the light wavelength
- H01S3/067—Fibre lasers
- H01S3/06708—Constructional details of the fibre, e.g. compositions, cross-section, shape or tapering
- H01S3/06716—Fibre compositions or doping with active elements
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Abstract
The invention relates to a high borosilicate glass cladding cesium iodide single crystal fiber core optical fiber and a preparation method and application thereof. The optical fiber of the invention takes high borosilicate glass as a cladding and cesium iodide as a fiber core, and the preparation method comprises the following steps: processing high borosilicate glass into a rod shape, and processing one end of the rod-shaped glass into a cavity; filling cesium iodide into the cavity, compacting, and closing the opening end of the cavity to obtain an assembled optical fiber preform; obtaining a precursor optical fiber through wire drawing; carrying out heat treatment and annealing treatment on the precursor optical fiber to obtain a high borosilicate glass cladding cesium iodide single crystal core optical fiber; the optical fiber obtained by the method has better mechanical strength, and protects the cesium iodide single crystal fiber core of the optical fiber from being oxidized and deliquesced by air; can be applied to infrared light transmission and infrared band optical fiber lasers.
Description
Technical Field
The invention relates to the technical field of optical fibers, in particular to a high borosilicate glass cladding cesium iodide single crystal fiber core optical fiber and a preparation method and application thereof.
Background
In the field of optical communications, the transmission bandwidth of silica glass optical fibers currently in commercial use can be from 1260nm to 1675nm, with a total width of 415 nm. Silica glass fibers are only suitable for optical transmission at wavelengths less than 2.4 μm. At present, quartz glass optical fibers cannot be used for optical fibers for laser transmission of medium and far infrared bands, and in order to widen the transmission bandwidth of the optical fibers, other optical fiber materials which are beneficial to medium and far infrared light transmission besides quartz glass must be researched.
The optical fiber materials commonly used in the infrared band at present are fluoride glass optical fiber and chalcogenide glass optical fiber. Although the fluoride glass optical fiber theoretically has extremely low loss and high damage threshold, the fluoride glass optical fiber is difficult to prepare and use due to short glass frit property, easy crystallization, low mechanical strength and easy hygroscopicity; and the infrared cut-off wavelength of the fluoride glass fiber is only 7-9 μm. Although chalcogenide glass optical fibers have ultrahigh nonlinearity (the highest among glass optical fibers), chalcogenide glass optical fibers have the problems of short material property, easy crystallization, low mechanical strength and relatively high optical fiber loss, so that the preparation of low-loss chalcogenide glass optical fibers is difficult. These have limited the development of fluoride glass optical fibers and chalcogenide glass optical fibers.
Furthermore, there are obvious technical shortboards for fiber lasers with glass as the gain medium: 1) Too low thermal conductivity forms a large temperature gradient in the optical fiber to trigger a thermal lens effect, so that the quality of light beams is greatly influenced; 2) Nonlinear effects such as Stimulated Raman Scattering (SRS) and Stimulated Brillouin Scattering (SBS) limit further increases in output power to some extent.
The Chinese patent application with the publication number of CN109669232A discloses a single crystal semiconductor core optical fiber and a preparation method thereof, and the preparation method of the single crystal semiconductor core optical fiber mainly comprises the step of using a glass capillary as a cladding to realize full wrapping on an unmelted single crystal fiber core, so that a single crystal fiber core optical fiber structure is formed. There are the following disadvantages: 1. the prepared optical fiber is short and cannot be prepared into an ultra-long optical fiber; 2. in the preparation process of the optical fiber, the fiber core material is not completely melted, so that the combination of the fiber core material and the cladding material is not tight; 3. in the preparation step of the optical fiber, the process of wet etching the monocrystalline semiconductor rod needs the contact of the core material and water, so that some core materials which are easily dissolved in water cannot be prepared into the monocrystalline optical fiber by the method.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a high borosilicate glass cladding cesium iodide single-crystal core optical fiber.
The invention also aims to provide a preparation method of the high borosilicate glass cladding cesium iodide single crystal core optical fiber.
The invention also aims to provide the application of the high borosilicate glass cladding cesium iodide single-crystal core optical fiber in the transmission of infrared light.
The invention also aims to provide application of the high borosilicate glass cladding cesium iodide single-crystal core optical fiber in preparation of an infrared fiber laser.
The invention relates to a preparation method of a high borosilicate glass cladding cesium iodide single crystal core optical fiber, which comprises the following steps:
(1) Pretreatment of the high borosilicate glass cladding: processing high borosilicate glass into a rod shape, and processing one end of the rod-shaped glass into a cavity;
(2) Assembling the optical fiber preform: filling cesium iodide into the cavity in the step (1), and closing the opening end of the cavity;
(3) Drawing an optical fiber: drawing the optical fiber preform rod in the step (2) to obtain a high borosilicate glass cladding cesium iodide crystal core precursor optical fiber;
(4) And (3) heat treatment: and (4) heating the high borosilicate glass cladding cesium iodide crystal core precursor optical fiber in the step (3) for heat treatment, and annealing to obtain the high borosilicate glass cladding cesium iodide single crystal core optical fiber.
Preferably, the rod-shaped glass in the step (1) is cylindrical, and the cavity is a cylindrical pit processed along the central axis of the cylindrical glass.
Preferably, in the step (1), the diameter of the cylindrical glass is 12-30mm, and the length of the cylindrical glass is 80-150mm; the diameter of the cylindrical pit is 3-5mm, and the length of the cylindrical pit is 60-130mm.
Preferably, the processing mode of the step (1) is mechanical processing; mechanical polishing or chemical polishing is particularly preferably adopted, so that the optical performance of the prepared optical fiber material can be improved.
Preferably, in the step (2), cesium iodide is filled in the cylindrical pit in the step (1) and compacted, so that cesium iodide powder in the cylindrical pit is isolated from air; the cesium iodide is cesium iodide powder or a cesium iodide crystal bar. The compaction can make the prepared high borosilicate glass cladding cesium iodide crystal core precursor optical fiber more continuous and compact, and is beneficial to subsequent heat treatment. The cesium iodide powder is completely isolated from air, so that the reaction of the fiber core cesium iodide with water and oxygen in the air in the high-temperature drawing process can be prevented.
Preferably, in step (2), the open end of the cylindrical pit is closed with refractory mortar material or clay.
Preferably, the temperature for drawing in the step (3) is 900-1000 ℃.
Preferably, the temperature of the heat treatment in the step (4) is 630-650 ℃, and the time of the heat treatment is 2-3h; the annealing treatment is carried out by cooling to the normal temperature at a cooling rate of 0.05-0.1 ℃/h.
According to the high borosilicate glass cladding cesium iodide single crystal core optical fiber prepared by the method, the cladding is high borosilicate glass, and the core is cesium iodide single crystal. The method can be applied to the transmission of infrared light and the preparation of infrared fiber lasers.
The single crystal optical fiber is a special optical fiber with a crystal core material, and can simultaneously have the advantages of strong waveguide characteristic, large heat dissipation area and easy integration of the traditional glass optical fiber, and the advantages of high temperature resistance, high thermal conductivity, high damage threshold, high nonlinear effect threshold and the like of the bulk crystal. The light transmission range of the preferred high borosilicate glass cladding cesium iodide single crystal core optical fiber covers the near ultraviolet to far infrared region, and the optical fiber material is excellent in performance and is used for infrared light transmission and infrared fiber laser manufacturing.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1) The invention adopts a fiber core melting method to prepare the precursor optical fiber, has no limit on the length of the precursor optical fiber, can prepare longer single crystal optical fiber by matching with a later heat treatment technology, and can overcome the defects that the optical fiber prepared by the prior art is shorter and can not prepare ultra-long optical fiber.
2) In the high-temperature wire drawing process, the fiber core material of the prefabricated rod is melted, the cladding glass is softened, the combination of the core cladding interface is tighter, and the defect of untight combination of the fiber core material and the cladding material caused by the fact that the fiber core material is not melted in the preparation process of the optical fiber in the prior art can be overcome.
3) The invention does not need to contact with water in the preparation process of the optical fiber, and can overcome the defect that the fiber core material which is easy to dissolve in water can not be prepared into the single crystal optical fiber by the method because the fiber core material needs to contact with the water in the process of corroding the single crystal semiconductor rod by a wet method in the prior art.
4) According to the invention, high borosilicate glass and cesium iodide are combined to form the composite material optical fiber; selecting high borosilicate glass as a cladding, cesium iodide as a fiber core, wherein the viscosity of the high borosilicate glass cladding material is matched with the melting point of the cesium iodide fiber core, and the fiber core semiconductor is in a liquid state; in addition, the drawing temperature is low, and the low drawing temperature can reduce the diffusion of oxygen ions in the glass to a cesium iodide core so as to reduce the optical loss; and because of the existence of the high borosilicate cladding glass, the core material is sealed in the cladding, and the oxidation caused by the contact with air is avoided.
(5) The high borosilicate glass cladding cesium iodide single crystal fiber core optical fiber is a composite material, the fiber core material is cesium iodide single crystal, and the light transmission range of the fiber core covers the region from near ultraviolet to far infrared; the cladding material is high borosilicate glass, can provide better mechanical strength for the optical fiber, and protects the cesium iodide single crystal fiber core of the optical fiber from air oxidation and deliquescence.
(6) The invention provides a preparation idea of a single crystal fiber core optical fiber, namely, a cesium iodide crystal fiber core/glass cladding composite material optical fiber precursor is prepared by adopting a fiber core melting method process, and the prepared precursor optical fiber is prepared into the composite material optical fiber which is small in size, good in heat dissipation performance and easy to integrate by utilizing a heat treatment process.
Drawings
FIG. 1 is a schematic view of an optical fiber preform obtained in example 1;
FIGS. 2a and 2b are optical microscope images of the precursor optical fiber of example 1 before and after heat treatment, respectively;
FIG. 3 is a scanning electron micrograph of a cesium iodide core in a heat-treated optical fiber obtained in example 1;
FIG. 4 is an X-ray diffraction pattern of cesium iodide powder, cesium iodide single crystal, and cesium iodide core in a precursor optical fiber and cesium iodide core in a heat treated optical fiber of example 1;
fig. 5 is a raman spectrum of the cesium iodide powder, the cesium iodide single crystal, and the cesium iodide core in the precursor optical fiber and the cesium iodide core in the optical fiber after heat treatment of example 1.
Detailed Description
The following examples are included to further illustrate the practice of the invention, but are not intended to limit the practice or protection of the invention. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
The preparation method of the high borosilicate glass cladding cesium iodide single crystal core optical fiber comprises the following steps:
(1) Machining the high borosilicate clad glass: processing a large block of high borosilicate cladding glass into a cylinder with the diameter of 7mm and the length of 150mm, and processing the center of the cladding glass into a cylindrical pit with the diameter of 3mm and the length of 130mm along the axis, wherein the cylindrical pit does not penetrate through the whole glass cylinder; the surface of the cylindrical glass and the inner surface of the cylindrical pit are both subjected to mechanical and chemical polishing;
(2) Assembling the optical fiber preform: filling a cesium iodide crystal bar into a cylindrical pit of a high borosilicate glass cylinder in a glove box to isolate water and oxygen, and sealing the opening end of the cylindrical pit of the high borosilicate glass bar by using a refractory mortar material to completely isolate the cesium iodide crystal bar in the pit from air; forming an optical fiber preform;
(3) Drawing an optical fiber: the assembled optical fiber preform is placed on a wire drawing tower for wire drawing, the wire drawing temperature is 960 ℃, a continuous high borosilicate glass cladding cesium iodide crystal core precursor optical fiber can be obtained, and the diameter of the optical fiber can be adjusted by controlling the wire drawing according to the requirement;
(4) Heat treatment of high borosilicate glass cladding cesium iodide crystal core precursor optical fiber: and (3) putting the prepared precursor optical fiber into a muffle furnace for heat treatment, preserving the heat for 3h at 630 ℃, and annealing to room temperature at the speed of 0.1 ℃/h to finally obtain the high borosilicate glass cladding cesium iodide single crystal fiber core optical fiber. The fiber core before heat treatment of the precursor optical fiber is obvious polycrystalline particles and is not dense, and the fiber core after heat treatment is continuous and compact.
As shown in FIG. 1, the cesium iodide powder in the high borosilicate glass clad cylindrical pit is densely packed, and the open end of the high borosilicate glass rod cylindrical pit is closed with a refractory mortar material to isolate the cesium iodide powder in the central hole from air. FIGS. 2a and 2b are optical microscope images of the precursor optical fiber before and after heat treatment in example 1, wherein a part is a microscope image of the precursor optical fiber before heat treatment, and b part is a microscope image of the precursor optical fiber after heat treatment; as shown in fig. 2a, 2b and 3, the cesium iodide core becomes continuous and dense after heat treatment, and meets the basic requirement of light transmission. As shown in fig. 4, the X-ray diffraction patterns of the cesium iodide single crystal and the cesium iodide core in the optical fiber after heat treatment both have only one diffraction peak, which indicates that the cesium iodide core after heat treatment is a single crystal or a polycrystal with good orientation. As shown in fig. 5, raman spectra of the cesium iodide single crystal and the cesium iodide core in the optical fiber after heat treatment correspond to each other, and it can be similarly explained that the cesium iodide core after heat treatment is a single crystal or a polycrystal having a good orientation.
Example 2
The preparation method of the high borosilicate glass cladding cesium iodide single crystal core optical fiber comprises the following steps:
(1) Machining the high borosilicate clad glass: processing a large block of high borosilicate cladding glass into a cylinder with the diameter of 30mm and the length of 80mm, and processing the center of the cladding glass into a cylindrical pit with the diameter of 3mm and the length of 60mm along the axis, wherein the cylindrical pit does not penetrate through the whole glass cylinder; the surface of the cylindrical glass and the inner surface of the cylindrical pit are both subjected to mechanical and chemical polishing;
(2) Assembling the optical fiber preform: tightly filling cesium iodide powder (with the purity of 99.999%) into a cylindrical pit of a high borosilicate glass cylinder in a glove box, compacting to isolate water and oxygen, and sealing the open end of the cylindrical pit of the high borosilicate glass rod by using a refractory mortar material to completely isolate the cesium iodide powder in the cylindrical pit from air; thus forming an optical fiber preform;
(3) Drawing an optical fiber: the assembled optical fiber preform is placed on a drawing tower for drawing at the drawing temperature of 940 ℃, so that a continuous high borosilicate glass cladding cesium iodide crystal fiber core precursor optical fiber can be obtained, and the diameter of the optical fiber can be adjusted by controlling drawing parameters as required;
(4) Heat treatment of high borosilicate glass cladding cesium iodide crystal core precursor optical fiber: and (3) putting the prepared precursor optical fiber into a muffle furnace for heat treatment, preserving the heat for 2h at 630 ℃, and annealing to room temperature at the speed of 0.05 ℃/h to obtain the high borosilicate glass cladding cesium iodide single crystal fiber core optical fiber. The effect of the heat treatment can be found in example 1.
Example 3
The preparation method of the high borosilicate glass cladding cesium iodide single crystal core optical fiber comprises the following steps:
(1) Machining the high borosilicate cladding glass: processing a large block of high borosilicate cladding glass into a cylinder with the diameter of 12mm and the length of 150mm, and processing the center of the cladding glass into a cylindrical pit with the diameter of 5mm and the length of 130mm along an axis, wherein the cylindrical pit does not penetrate through the whole glass cylinder; the surface of the cylindrical glass and the inner surface of the cylindrical pit are both subjected to mechanical and chemical polishing;
(2) Assembling an optical fiber preform: tightly filling cesium iodide powder (with the purity of 99.999%) into a cylindrical pit of a high borosilicate glass cylinder in a glove box and compacting to isolate water and oxygen, and sealing the open end of the cylindrical pit of the high borosilicate glass rod by using a refractory mortar material to completely isolate the cesium iodide powder in the cylindrical pit from air, thereby forming an optical fiber preform;
(3) Drawing an optical fiber: the assembled optical fiber preform is placed on a drawing tower for drawing at 990 ℃, so that a continuous high borosilicate glass cladding cesium iodide crystal core precursor optical fiber can be obtained, and the diameter of the optical fiber can be adjusted by controlling drawing parameters as required;
(4) Heat treatment of a high borosilicate glass cladding cesium iodide crystal core precursor optical fiber: and (3) putting the prepared precursor optical fiber into a muffle furnace for heat treatment, preserving the heat for 2h at 650 ℃, and annealing to room temperature at the cooling rate of 0.1 ℃/h to finally obtain the high borosilicate glass cladding cesium iodide single crystal fiber core optical fiber. The effect of the heat treatment can be found in example 1.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (7)
1. A preparation method of a high borosilicate glass cladding cesium iodide single crystal core optical fiber is characterized by comprising the following steps:
(1) Pretreatment of the high borosilicate glass cladding: processing high borosilicate glass into a rod shape, and processing one end of the rod-shaped glass into a cavity; the rod-shaped glass is cylindrical, and the cavity is a cylindrical pit formed by processing along the central axis of the cylindrical glass; the diameter of the cylindrical glass is 12-30mm, and the length of the cylindrical glass is 80-150mm; the diameter of the cylindrical pit is 3-5mm, and the length of the cylindrical pit is 60-130mm;
(2) Assembling the optical fiber preform: filling cesium iodide into the cavity in the step (1), and closing the opening end of the cavity;
(3) Drawing an optical fiber: drawing the optical fiber preform rod in the step (2) to obtain a high borosilicate glass cladding cesium iodide crystal core precursor optical fiber; the temperature of the wire drawing is 900-1000 ℃;
(4) And (3) heat treatment: heating the high borosilicate glass cladding cesium iodide crystal core precursor optical fiber obtained in the step (3) for heat treatment, and annealing to obtain the high borosilicate glass cladding cesium iodide single crystal core optical fiber; the temperature of the heat treatment is 630-650 ℃, and the time of the heat treatment is 2-3h; the annealing treatment is carried out by cooling to the normal temperature at a cooling rate of 0.05-0.1 ℃/h.
2. The method according to claim 1, wherein in step (1), the processing is mechanical polishing or chemical polishing.
3. The method of claim 2, wherein in the step (2), cesium iodide is filled in the cylindrical pits of the step (1) and compacted to isolate the cesium iodide powder in the cylindrical pits from air; the cesium iodide is cesium iodide powder or a cesium iodide crystal bar.
4. A method according to claim 3, wherein in step (2), the open end of the cylindrical pit is closed with refractory mortar material or clay.
5. A high borosilicate glass clad cesium iodide single core optical fiber made by the method of any of claims 1 to 4.
6. Use of the high borosilicate glass clad cesium iodide single crystal core optical fiber of claim 5 in the transmission of infrared light.
7. Use of a high borosilicate glass clad cesium iodide single crystal core fiber as claimed in claim 5 for the preparation of an infrared fiber laser.
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