CN109678334B - Multi-core composite material optical fiber with chalcogenide glass core layer/tellurate glass cladding layer and preparation method thereof - Google Patents
Multi-core composite material optical fiber with chalcogenide glass core layer/tellurate glass cladding layer and preparation method thereof Download PDFInfo
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- CN109678334B CN109678334B CN201910068149.6A CN201910068149A CN109678334B CN 109678334 B CN109678334 B CN 109678334B CN 201910068149 A CN201910068149 A CN 201910068149A CN 109678334 B CN109678334 B CN 109678334B
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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
- C03B37/01265—Manufacture of preforms for drawing fibres or filaments starting entirely or partially from molten glass, e.g. by dipping a preform in a melt
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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
- C03B37/01211—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments by inserting one or more rods or tubes into a tube
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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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2203/00—Fibre product details, e.g. structure, shape
- C03B2203/32—Eccentric core or cladding
Abstract
The invention provides a multi-core composite with tellurate glass cladding/chalcogenide glass core layerA material optical fiber and a preparation method thereof. The cladding of the multi-core composite material is multi-component tellurate glass: (88-x) TeO2‑6Bi2O3‑xLi2O-6ZnO, wherein x is 6-14, and the core layer is a chalcogenide glass: (40-y) Ge-ySb-60Se, wherein y is 6-12. The invention fully utilizes the respective high nonlinearity and low phonon energy of tellurate glass and chalcogenide glass and the large refractive index difference between the tellurate glass and the chalcogenide glass to realize the integration of various functions of the composite material optical fiber and the multi-core optical fiber, and has very important application prospect in the fields of mid-infrared laser, supercontinuum, photon integration and the like.
Description
Technical Field
The invention relates to the field of special optical fibers, in particular to a chalcogenide glass core layer/tellurate glass cladding multi-core composite material optical fiber and a preparation method thereof.
Technical Field
Compared with the common single-material optical fiber, the composite material optical fiber has the characteristics of large adjustable range of core cladding refractive index difference and numerical aperture value, easy regulation of dispersion and nonlinear value and the like, and can integrate the respective advantages of two composite materials. Therefore, the composite optical fiber taking tellurate, chalcogenide, fluoride and other mid-infrared glass as core cladding composition materials has important application prospects in the fields of mid-infrared laser, mid-infrared super-continuum spectrum, parametric oscillation, sensing and the like.
Composite optical fibers have developed more rapidly in recent years. In 2009, Chaudhari et al designed a composite fiber with borate glass as the cladding and chalcogenide glass as the core, and obtained by theoretical calculation that the zero dispersion point of the fiber has been adjusted to the near infrared band. In 2015, the university of Toyota, Japan, reports a composite material optical fiber with tellurate glass as a core layer and phosphate glass as a cladding layer, and the dispersion and nonlinearity can be adjusted and controlled. However, the above reported composite optical fibers are limited to the conventional step-type structure, so they are limited in terms of optical transmission mode and mode field modulation. The multi-core fiber has a special structure, so that the multi-core fiber has great advantages in the two aspects. However, most of the existing multi-core optical fibers adopt air holes, so that the structure of the multi-core optical fiber is fragile, and the application of the multi-core optical fiber is greatly limited.
Disclosure of Invention
In view of the above problems, the present invention provides a multi-core composite optical fiber having a chalcogenide glass core layer/a tellurate glass cladding layer, which fully utilizes the high nonlinearity and low phonon energy of chalcogenide glass and tellurate glass, and the large refractive index difference between the chalcogenide glass and the tellurate glass to realize the integration of various functions of the composite optical fiber and the multi-core optical fiber.
The technical scheme of the invention is as follows:
the cladding of the multi-core composite material optical fiber is multi-component tellurate glass, and the specific component is (88-x) TeO2-6Bi2O3-xLi2O-6ZnO, wherein x is 6-14; the core layer is chalcogenide glass and comprises the following specific components: (40-y) Ge-ySb-60Se, wherein y is 6-12.
Based on the above scheme, the invention further optimizes as follows:
the diameter of the multi-core composite material optical fiber is 125-300 mu m.
The plurality of holes corresponding to the core layer on the section of the cladding layer are arranged in a plurality of circles concentrically.
The cross section of the cladding layer is in a regular polygon shape corresponding to the plurality of holes of the core layer.
A preparation method of the multi-core composite material optical fiber comprises the following steps:
1) mixing the raw materials of the cladding layer and the core layer, and respectively preparing a tellurate glass preform and a chalcogenide glass preform by a melt quenching method;
2) placing the chalcogenide glass prefabricated rod in a soft glass infrared wire drawing tower, and obtaining a small chalcogenide glass rod by a hot drawing method; punching the tellurate glass preform to obtain a porous tellurate preform;
3) placing the small chalcogenide glass rod in a hollow hole of a porous tellurate glass prefabricated rod to obtain a multi-core composite material optical fiber prefabricated rod with a tube rod structure;
4) and placing the multicore composite optical fiber preform in a soft glass infrared drawing tower, and preparing the multicore composite optical fiber with the chalcogenide glass core layer/tellurate glass cladding by a hot drawing method.
And (4) protecting by using inert gas in the hot drawing process in the step 2) and the step 4).
In the step 2), the hot drawing temperature is 400-440 ℃, and the size range of the small rods of the chalcogenide glass preform obtained by drawing is 0.5-1 mm.
In the step 2), a mechanical punching method is adopted to prepare the porous tellurate glass perform rod, and the aperture is 0.5-1 mm.
In the step 4), the hot drawing temperature is 400-440 ℃, and the diameter of the drawn optical fiber is 125-300 μm.
The preparation method comprises two hot drawing processes, wherein the first hot drawing process is to draw the chalcogenide glass preform into a small rod, and the second hot drawing process is to prepare the multi-core composite material optical fiber by using a rod-tube method. Because chalcogenide glass is very easy to be oxidized at high temperature, inert gases such as argon, nitrogen and the like are adopted for protection in the two hot drawing processes. In addition, in the second thermal drawing process, because the prefabricated rod is of a tube-rod structure, the pressure difference between the rod and the tube needs to be kept, and the prepared optical fiber core cladding is ensured to be tightly attached.
The invention has the beneficial effects that:
1. the multi-core composite material optical fiber is successfully prepared by skillfully selecting two different systems of mid-infrared glass with mutually matched thermal performance properties such as viscosity, thermal expansion coefficient, glass softening temperature and the like as cladding and core materials, so that the integration of various functions of the mid-infrared composite material optical fiber and the multi-core optical fiber is realized. The method has very important application prospect in the fields of mid-infrared laser, super-continuum spectrum and photon integration.
2. The preparation method has the advantages of simple preparation process, strong operability and high success rate.
Drawings
FIG. 1 is a schematic diagram of a process for fabricating a multi-core composite optical fiber preform according to the present invention;
fig. 2 is a schematic end view of a multi-core composite optical fiber according to the present invention.
The reference numbers illustrate:
1-a porous tellurate glass preform; 2-chalcogenide glass rods; 3-cladding; 4-core layer.
Detailed Description
Three examples are given below to illustrate the invention in detail.
The specific formulations of the cladding and core layers of the three examples are shown in table 1 below.
TABLE 1
The procedure for example 1 was as follows:
1. respectively preparing a tellurate glass preform and a chalcogenide glass preform by a molten quenching method; wherein the diameter of the tellurate glass prefabricated rod is 20mm, and the diameter of the chalcogenide glass prefabricated rod is 12 mm;
2. placing the prepared chalcogenide glass preform into a soft glass infrared drawing tower, and obtaining a chalcogenide glass small rod with the outer diameter of 0.5mm by a hot drawing method; wherein the hot drawing temperature is 400 ℃, and the protective gas is N2The gas flow is 0.5L/min;
3. performing punching treatment on the tellurite glass preform obtained in the step 1 by a mechanical punching method, wherein the aperture is 0.5mm (keeping a positive tolerance), and obtaining a porous tellurite preform;
4. placing the small chalcogenide glass rod obtained in the step 2 into a hollow hole of the porous tellurate glass preform rod obtained in the step 3 (as shown in figure 1) to obtain a multi-core composite material optical fiber preform rod with a tube rod structure;
5. placing the multi-core composite material optical fiber preform obtained in the step (4) in a soft glass infrared drawing tower, and preparing the multi-core composite material optical fiber (the end surface structure is shown in figure 2) with the chalcogenide glass core layer/tellurate glass cladding by a hot drawing method, wherein the wire diameter of the multi-core composite material optical fiber is 125 microns; wherein the hot drawing temperature is 400 ℃, and the protective gas is N2The gas flow is 0.5L/min, and the pressure difference between the inside and the outside of the tube bar is kept to be-5 KPa.
The procedure for example 2 was as follows:
1. respectively preparing a tellurate glass preform and a chalcogenide glass preform by a molten quenching method; wherein the diameter of the tellurate glass prefabricated rod is 20mm, and the diameter of the chalcogenide glass prefabricated rod is 12 mm;
2. placing the prepared chalcogenide glass preform into a soft glass infrared drawing tower, and obtaining a chalcogenide glass small rod with the outer diameter of 0.8mm by a hot drawing method; wherein the hot drawing temperature is 420 ℃, the protective gas is Ar, and the gas flow is 1L/min;
3. performing punching treatment on the tellurite glass preform obtained in the step 1 by a mechanical punching method, wherein the aperture is 0.8mm (keeping a positive tolerance), and obtaining a porous tellurite preform;
4. placing the small chalcogenide glass rod obtained in the step 2 into a hollow hole of the porous tellurate glass preform rod obtained in the step 3 (as shown in figure 1) to obtain a multi-core composite material optical fiber preform rod with a tube rod structure;
5. placing the multi-core composite material optical fiber preform obtained in the step (4) in a soft glass infrared drawing tower, and preparing the multi-core composite material optical fiber (the end surface structure is shown in figure 2) with the chalcogenide glass core layer/tellurate glass cladding by a hot drawing method, wherein the wire diameter of the multi-core composite material optical fiber is 200 mu m; wherein the hot drawing temperature is 420 ℃, the protective gas is Ar, the gas flow is 1L/min, and the pressure difference between the inside and the outside of the tube rod is kept to be-5 KPa.
The procedure for example 3 was as follows:
1. respectively preparing a tellurate glass prefabricated rod and a chalcogenide glass prefabricated rod by using a traditional melting quenching method; wherein the diameter of the tellurate glass prefabricated rod is 20mm, and the diameter of the chalcogenide glass prefabricated rod is 12 mm;
2. placing the prepared chalcogenide glass preform into a soft glass infrared drawing tower, and obtaining a chalcogenide glass small rod with the outer diameter of 1.0mm by a hot drawing method; wherein the hot drawing temperature is 440 ℃, the protective gas is He, and the gas flow is 1.5L/min;
3. and (3) punching the tellurate glass preform rod obtained in the step (1) by a mechanical punching method, wherein the aperture is 1.0mm (keeping a positive tolerance), and thus obtaining the porous tellurate glass preform rod.
4. Placing the small chalcogenide glass rod obtained in the step 2 into a hollow hole of the porous tellurate glass preform rod obtained in the step 3 (as shown in figure 1) to obtain a multi-core composite material optical fiber preform rod with a tube rod structure;
5. placing the multi-core composite material optical fiber preform obtained in the step (4) in a soft glass infrared drawing tower, and preparing the multi-core composite material optical fiber (the end surface structure is shown in figure 2) with the chalcogenide glass core layer/tellurate glass cladding by a hot drawing method, wherein the wire diameter of the multi-core composite material optical fiber is 300 mu m; wherein the hot drawing temperature is 440 ℃, the protective gas is He, the gas flow is 1.5L/min, and the pressure difference between the inside and the outside of the tube rod is kept to be-5 KPa.
The multi-core composite material optical fiber is successfully obtained in the preparation process, and an expected effect is obtained through experimental tests. The high-quality multi-core composite material optical fiber (small core package eccentricity, smooth surface and good roundness) can be further ensured to be prepared by strictly controlling the uniformity of the temperature field of the heating furnace, the size of the airflow of the protective gas and the pressure difference between the inside and the outside of the tube rod.
Claims (9)
1. A multi-core composite material optical fiber with a chalcogenide glass core layer/tellurate glass cladding layer is characterized in that:
the cladding is multi-component tellurate glass, and the specific component is (88-x) TeO2-6Bi2O3-xLi2O-6ZnO, wherein x is 6-14;
the core layer is chalcogenide glass and comprises the following specific components: (40-y) Ge-ySb-60Se, wherein y is 6-12.
2. The multi-core composite optical fiber with chalcogenide glass core/tellurate glass cladding as claimed in claim 1, wherein: the diameter of the multi-core composite material optical fiber is 125-300 mu m.
3. The multi-core composite optical fiber with chalcogenide glass core/tellurate glass cladding as claimed in claim 1, wherein: the plurality of holes corresponding to the core layer on the section of the cladding layer are arranged in a plurality of circles concentrically.
4. The multi-core composite optical fiber with chalcogenide glass core/tellurate glass cladding as claimed in claim 1, wherein: the cross section of the cladding layer is in a regular polygon shape corresponding to the plurality of holes of the core layer.
5. A method for making the multicore composite optical fiber of claim 1, comprising the steps of:
1) mixing the raw materials of the cladding layer and the core layer, and respectively preparing a tellurate glass preform and a chalcogenide glass preform by a melt quenching method;
2) placing the chalcogenide glass prefabricated rod in a soft glass infrared wire drawing tower, and obtaining a small chalcogenide glass rod by a hot drawing method; punching the tellurate glass preform to obtain a porous tellurate preform;
3) placing the small chalcogenide glass rod in a hollow hole of a porous tellurate glass prefabricated rod to obtain a multi-core composite material optical fiber prefabricated rod with a tube rod structure;
4) and placing the multicore composite optical fiber preform in a soft glass infrared drawing tower, and preparing the multicore composite optical fiber with the chalcogenide glass core layer/tellurate glass cladding by a hot drawing method.
6. The method of claim 5, wherein: and (4) protecting by using inert gas in the hot drawing process in the step 2) and the step 4).
7. The method of claim 5, wherein: in the step 2), the hot drawing temperature is 400-440 ℃, and the size range of the small rods of the chalcogenide glass preform obtained by drawing is 0.5-1 mm.
8. The method of claim 5, wherein: in the step 2), a mechanical punching method is adopted to prepare the porous tellurate glass perform rod, and the aperture is 0.5-1 mm.
9. The method of claim 5, wherein: in the step 4), the hot drawing temperature is 400-440 ℃, and the diameter of the drawn optical fiber is 125-300 μm.
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JPS62272731A (en) * | 1986-05-21 | 1987-11-26 | Hitachi Ltd | Infrared ray transmission equipment |
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EP1393105A4 (en) * | 2001-04-12 | 2006-03-22 | Omniguide Inc | High index-contrast fiber waveguides and applications |
KR100772501B1 (en) * | 2005-06-30 | 2007-11-01 | 한국전자통신연구원 | Tellurite glass composite, optical waveguide and optical amplifier using the same |
CN101620295A (en) * | 2008-07-01 | 2010-01-06 | 湖南大学 | Large mode area multi-core fiber |
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US9207398B2 (en) * | 2012-06-28 | 2015-12-08 | The United States Of America, As Represented By The Secretary Of The Navy | Multi-core optical fibers for IR image transmission |
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