CN113307511A - Quartz optical fiber and preparation method and device thereof - Google Patents

Quartz optical fiber and preparation method and device thereof Download PDF

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CN113307511A
CN113307511A CN202110652462.1A CN202110652462A CN113307511A CN 113307511 A CN113307511 A CN 113307511A CN 202110652462 A CN202110652462 A CN 202110652462A CN 113307511 A CN113307511 A CN 113307511A
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coating
optical fiber
quartz
microcrystalline glass
fiber
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CN113307511B (en
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杨亮亮
贾金升
张卓
王晓章
曹珊珊
孙勇
张洋
赵冉
孔壮
那天一
王一苇
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China Building Materials Academy CBMA
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10—Coating
    • C03C25/48—Coating with two or more coatings having different compositions
    • C03C25/54—Combinations of one or more coatings containing organic materials only with one or more coatings containing inorganic materials only
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0018—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents
    • C03C10/0027—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents containing SiO2, Al2O3, Li2O as main constituents
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10—Coating
    • C03C25/24—Coatings containing organic materials
    • C03C25/26—Macromolecular compounds or prepolymers
    • C03C25/28—Macromolecular compounds or prepolymers obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • C03C25/285—Acrylic resins
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10—Coating
    • C03C25/42—Coatings containing inorganic materials

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Surface Treatment Of Glass Fibres Or Filaments (AREA)

Abstract

The invention relates to a quartz optical fiber and a preparation method and a device thereof, wherein the preparation method comprises the following steps: coating microcrystalline glass liquid on the surface of the quartz bare fiber to form a microcrystalline glass coating before the temperature of the drawn quartz bare fiber is reduced to the glass transition temperature of the quartz bare fiber; cooling, coating organic paint on the surface of the microcrystalline glass coating to form an organic coating, and obtaining the quartz optical fiber, wherein the expansion coefficient of the microcrystalline glass is less than 5 multiplied by 10‑7The temperature is 1200-1400 ℃; the core layer and the skin layer of the quartz bare fiber are both made of quartz glass materials. The invention adopts a high-temperature online coating method to form the microcrystalline glass coating with low expansion coefficient on the surface of the quartz bare fiber, thereby improving the stretching of the quartz fiberThe effect of strength.

Description

Quartz optical fiber and preparation method and device thereof
Technical Field
The invention relates to the technical field of quartz optical fibers, in particular to a quartz optical fiber and a preparation method and a preparation device thereof.
Background
The optical fiber is composed of a bare fiber and a resin layer wrapping the outer side of the bare fiber, the breaking force of the optical fiber can only bear 5-6 kg of force generally, and when the external acting force exceeds the range, the optical fiber can be broken.
The optical fiber tensile strength is an important performance parameter of optical fiber transmission, and if the optical fiber is broken, signals cannot be transmitted directly, so that the optical fiber tensile strength is improved, and the improvement of the reliability of the optical fiber is an important link.
The compact coating is coated on the surface of the optical fiber, so that the optical fiber can be sealed and is not corroded by the outside, and high anti-fatigue parameters and strength are generated. At present, the surface of an optical fiber is mainly coated with a polymer such as silicone, fluorine resin, acrylic resin, etc. to form an organic coating. Since the strength of the organic coating is much less than that of the optical fiber, the main contribution of such organic coating to the strength of the optical fiber is to protect the surface of the optical fiber from damage, and the breakage of the silica optical fiber is mainly determined by the silica glass portion. However, before the organic coating is applied, micro cracks are inevitably generated on the surface of the optical fiber during drawing, and the micro cracks can reduce the tensile strength of the optical fiber; moreover, during use, these micro-cracks are continuously enlarged, gradually decreasing the mechanical strength of the fiber. Meanwhile, after the optical fiber has microcracks, breakpoints are usually formed in the optical fiber, although the surface of the optical fiber is not broken, the transmission of light is actually influenced, and when the light meets the breakpoints, reflection is generated to influence the transmission.
Disclosure of Invention
The invention mainly aims to provide a quartz optical fiber, a preparation method and a device thereof, and aims to solve the technical problem of improving the tensile strength of the quartz optical fiber by forming a microcrystalline glass coating with a low expansion coefficient on the surface of the quartz bare fiber by adopting a high-temperature online coating method.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. According to the preparation method of the quartz optical fiber provided by the invention, before the temperature of the drawn quartz bare fiber is reduced to the glass transition temperature of the drawn quartz bare fiber, microcrystalline glass liquid is coated on the surface of the quartz bare fiber to form a microcrystalline glass coating; cooling, coating organic paint on the surface of the microcrystalline glass coating to form an organic coating, and obtaining the quartz optical fiber, wherein the expansion coefficient of the microcrystalline glass is less than 5 multiplied by 10-7The temperature is 1200-1400 ℃; the core layer and the skin layer of the quartz bare fiber are both made of quartz glass materials.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
Preferably, in the method for manufacturing a silica optical fiber, the coating temperature of the microcrystalline glass liquid is 1200 ℃ to 1450 ℃;
the temperature range before the glass transition temperature is 1200-1600 ℃.
Preferably, in the preparation method of the silica optical fiber, during the coating process, the thickness of the microcrystalline glass coating is controlled to be 2% to 6% of the filament diameter of the silica bare fiber.
Preferably, in the method for producing a silica optical fiber, the glass ceramics is Li-Al-Si glass ceramics.
Preferably, in the method for producing a silica optical fiber, the components of the Li-Al-Si based glass ceramics include, in parts by mass: li245-49 parts of O and Al2O329 to 32 parts of SiO216 to 20 portions of TiO 22 to 4 parts of Sb2O30.3-0.4 part and 0.1-0.5 part of ZnO.
Preferably, in the method for manufacturing a silica optical fiber, the microcrystalline glass has a coefficient of expansion of 5 × 10-9～5×10-7/° c; the organic coating is acrylic resin, organic silica gel or polyimide.
The object of the present invention and the technical problem to be solved are also achieved by the following technical means. According to the present invention, a device for manufacturing a silica optical fiber is provided, which comprises: the device comprises an optical fiber perform fusion drawing mechanism, a microcrystalline glass coating mechanism, an organic coating mechanism and a traction mechanism which are sequentially arranged from top to bottom, wherein the optical fiber perform fusion drawing mechanism is used for fusing and drawing the optical fiber perform into a quartz bare fiber; the microcrystalline glass coating mechanism comprises a first coating cup, wherein the first coating cup is used for containing microcrystalline glass liquid, the first coating cup is arranged in a cavity surrounded by insulating bricks, heating parts are arranged around the first coating cup, insulating cotton is filled in a gap between the insulating bricks and the first coating cup, an optical fiber lead hole is formed in the top of the first coating cup, and an optical fiber lead hole is formed in the bottom of the first coating cup; the organic coating mechanism comprises a second coating cup for containing organic coating; the traction mechanism is used for providing power for drawing the optical fiber;
an optical fiber auxiliary traction mechanism is arranged between the microcrystalline glass coating mechanism and the organic coating mechanism, so that the axis of the quartz bare fiber from the optical fiber perform melting and drawing mechanism is superposed with the axis of the microcrystalline glass coating mechanism and the axis of the organic coating mechanism;
temperature sensors are arranged at an optical fiber lead hole, an optical fiber outlet hole of the first coating cup, a microcrystalline glass liquid containing position in the first coating cup, a top inlet, an organic coating containing position in the second coating cup and a bottom outlet of the second coating cup, and the temperature sensors are respectively connected with a programmable logic controller through corresponding signal transmitters; the programmable logic controller is connected with the main control computer.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
Preferably, in the foregoing apparatus, the platinum coating cup includes a cup body and a fiber leading-out part, the fiber leading-out part is detachably connected to the bottom of the cup body, the fiber leading-out hole is located at the top of the cup body, and the fiber leading-out hole is located at the bottom of the fiber leading-out part.
The object of the present invention and the technical problem to be solved are also achieved by the following technical means. According to the quartz optical fiber provided by the invention, the quartz optical fiber sequentially comprises a quartz bare fiber, a microcrystalline glass coating and an organic coating from inside to outside; wherein the expansion coefficient of the microcrystalline glass used for the microcrystalline glass coating is less than 5 multiplied by 10-7The temperature is 1200-1400 ℃; the core layer and the skin layer of the quartz bare fiber are both made of quartz glass materials.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
Preferably, in the silica optical fiber, the glass ceramics is Li-Al-Si glass ceramics.
Preferably, the silica optical fiber described above, wherein the Li-Al-Si based glass ceramics comprises, in parts by mass: li245-49 parts of O and Al2O329 to 32 parts of SiO216 to 20 portions of TiO 22 to 4 parts of Sb2O30.3-0.4 part and 0.1-0.5 part of ZnO.
Preferably, the silica optical fiber described above, wherein said microcrystalline glass has a coefficient of expansion of 5 x 10-9～5×10-7/° c; the thickness of the microcrystalline glass coating is 2% -6% of the diameter of the quartz bare fiber;
the organic coating is made of acrylic resin, organic silica gel or polyimide.
By the technical scheme, the quartz optical fiber and the preparation method and device thereof provided by the invention at least have the following advantages:
1. the invention adopts a high-temperature online coating method, before the organic coating is coated and the temperature of the drawn quartz bare fiber is reduced to the glass transition temperature, the surface of the quartz bare fiber is coated with microcrystalline glass liquid, and the expansion coefficient of the microcrystalline glass is limited to be less than 5 multiplied by 10-7The microcrystalline glass coating with low expansion coefficient is formed on the surface of the quartz bare fiber, so that the tensile strength of the quartz fiber is improved. On one hand, the components and the performances of the microcrystalline glass and the quartz optical fiber are very similar, so that the microcrystalline glass and the surface of the quartz bare optical fiber have better bonding performance; on the other hand, because the expansion coefficient of the microcrystalline glass is smaller than that of the quartz bare fiber, and the expansion coefficient of the microcrystalline glass has higher matching degree with that of the quartz bare fiber, the low expansion characteristic of the microcrystalline glass coating can form pre-stress on the surface of the quartz fiber in the cooling process of the coated quartz fiber, so that the generation of microcracks in the quartz fiber is reduced, the expansion of the microcracks in the quartz fiber is inhibited, the tensile strength of the quartz fiber is improved, and the mechanical life of the fiber is prolonged.
2. According to the invention, the microcrystalline glass liquid is coated on the surface of the quartz bare fiber before the temperature of the quartz bare fiber is reduced to the glass transition temperature of the quartz bare fiber, so that the microcrystalline glass coating with the low expansion coefficient is formed, and then the organic coating is coated, so that the quartz optical fiber with the double coatings is obtained. On the basis of the existing enhancement of coating organic coating, the tensile strength of the quartz optical fiber is further improved. It is also confirmed from the examples that the tensile strength of the silica optical fiber coated with the microcrystalline glass coating is improved by about 5 to 6% compared with the tensile strength of the silica optical fiber not coated with the microcrystalline glass coating, so that the tensile strength of the silica optical fiber coated with the microcrystalline glass coating exceeds 6GPa and even reaches 6.136 GPa.
3. According to the invention, the microcrystalline glass coating is coated on the surface of the quartz bare fiber by adopting an online high-temperature coating method, and because the expansion coefficient of the prepared microcrystalline glass coating is lower than that of the quartz fiber and the expansion coefficient of the microcrystalline glass coating and that of the quartz fiber have higher matching degree, the generation and expansion of microcracks on the surface of the quartz fiber can be reduced in the cooling process of the quartz fiber coated with the microcrystalline glass coating. The method has the characteristics of good flexibility, easy operation, high efficiency and the like, and is easy to realize mass production.
4. The invention also provides a device for implementing the online high-temperature coating method, which is characterized in that a microcrystalline glass coating mechanism and an organic coating mechanism are sequentially arranged below the optical fiber perform melting and drawing mechanism, the microcrystalline glass coating mechanism comprises a first coating cup, the first coating cup is arranged in a cavity defined by insulating bricks, heating parts are arranged around the first coating cup, microcrystalline glass liquid is contained in the first coating cup, the first coating cup can ensure the high-temperature fluidity of the microcrystalline glass liquid during high-temperature coating, and a quartz bare fiber from the optical fiber perform melting and drawing mechanism passes through the microcrystalline glass liquid in the first coating cup to complete coating, so that the online high-temperature coating of the microcrystalline glass liquid is realized. The device is convenient to operate and easy to realize automatic production.
5. The device controls the coating thickness by controlling the aperture of the optical fiber outlet hole at the bottom of the coating cup, so that the thickness of the coated microcrystalline glass coating is uniform and controllable, the uniformity of the optical fiber is excellent, the uniformity of the coating thickness in a micron level is ensured, and the out-of-roundness of the coated optical fiber diameter is lower than 0.1%.
6. The first coating cup adopting the device provided by the invention is a platinum coating cup and comprises a cup body and an optical fiber leading-out part, wherein the optical fiber leading-out part is detachably connected to the bottom of the cup body, and an optical fiber outlet hole is positioned at the bottom of the optical fiber leading-out part.
7. The tensile strength of the quartz optical fiber obtained by the invention is more than 6GPa, and the quartz optical fiber can meet the occasions with high-strength use requirements, such as high-grade communication optical fibers.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a schematic cross-sectional view of a silica optical fiber obtained by the method according to one embodiment of the present invention;
FIG. 2 is a schematic view showing the construction of an apparatus for manufacturing a silica optical fiber according to an embodiment of the present invention;
fig. 3 is a schematic cross-sectional view of a microcrystalline molten glass coating mechanism in the apparatus shown in fig. 2.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description of the method for preparing an improved silica optical fiber and the method and apparatus for preparing the same according to the present invention will be made with reference to the accompanying drawings and preferred embodiments, and the detailed description thereof will be made with reference to the following detailed description of the embodiments, structures, features and effects. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The preparation method of the quartz optical fiber provided by one embodiment of the invention specifically comprises the following steps:
step 1, before the temperature of the drawn quartz bare fiber is reduced to the glass transition temperature, coating microcrystalline glass liquid on the surface of the quartz bare fiber to form a microcrystalline glass coating, wherein the expansion coefficient of the microcrystalline glass is less than 5 multiplied by 10-7Per DEG C, the preferred coefficient of expansion of the glass-ceramic is 5X 10-9～5×10-7The temperature is 1200-1400 ℃; the core layer and the skin layer of the quartz bare fiber are both made of quartz glass materials.
The preparation method of the microcrystalline glass liquid specifically comprises the following steps: heating the microcrystalline glass raw material to be molten, clarifying to obtain microcrystalline glass liquid, and carrying out heat preservation on the microcrystalline glass liquid at the temperature of 1200-1450 ℃.
The step of coating the microcrystalline glass liquid specifically comprises the following steps: and (3) passing the high-temperature quartz bare fiber (the temperature is higher than the glass transition temperature Tg) through the microcrystalline glass liquid, and coating the microcrystalline glass liquid on the surface of the quartz bare fiber to form a microcrystalline glass coating.
In some embodiments, the coating temperature of the microcrystalline glass liquid is 1200-1450 ℃;
the temperature range before the glass transition temperature is 1200 ℃ to 1600 ℃, preferably 1300 ℃ to 1500 ℃.
In coating the glass-ceramic liquid, the temperature of the glass-ceramic liquid is preferably similar to or slightly higher than that of the silica bare fiber, for example, when the temperature of the glass-ceramic liquid is 1200 ℃, the temperature of the silica bare fiber is preferably lowered to about 1200 ℃ to 1300 ℃ and passed through the glass-ceramic liquid.
Glass transition temperature (Tg) is an important characteristic parameter of a material, and many properties of glass change sharply around the Tg. The glass transition temperature of the quartz glass is substantially between 1120 ℃ and 1180 ℃. According to the embodiment of the invention, when the microcrystalline glass liquid is coated, the temperature of the quartz bare fiber is selected to be 1200-1600 ℃, the temperature is higher than the glass transition temperature of the quartz glass, the quartz bare fiber is not hardened, namely, microcracks are not generated, and the microcrystalline glass liquid is coated at the temperature to play a role in reducing the microcracks in the quartz fiber. Meanwhile, because the coating temperature of the microcrystalline glass liquid is close to the temperature of the quartz bare fiber, the temperature cannot drop suddenly due to the coating of the microcrystalline glass liquid, so that the influence of the coating on the quartz bare fiber is prevented.
The "silica bare fiber" refers to a bare fiber drawn by melting a silica optical fiber preform in a high-temperature graphite furnace at a temperature of 1700 ℃ to 2200 ℃, and is composed of only a core and a cladding.
The "drawn quartz bare fiber" refers to a high-temperature quartz bare fiber which is not cooled from an optical fiber preform melt-drawing mechanism, and the temperature is generally about 1600 ℃ to 1750 ℃.
The core and the cladding of the silica bare fiber are made of silica glass materials, namely the core of the silica bare fiber is made of pure silica glass or doped silica glass material with high refractive index, and the corresponding cladding material is made of doped silica glass with low refractive index or pure silica glass. Further preferably, the core layer is doped SiO2Doping species include, but are not limited to Ge, Al, P, Ti, Cl, and Br, e.g., GeO2Doped silicon dioxide; the cladding is pure quartz glass which can be regarded as pure SiO2。
In this step 1, the glass ceramics satisfying the conditions include, but are not limited to: li2O-Al2O3-SiO2Glass ceramics (i.e., Li-Al-Si glass ceramics) and Li2O-Al2O3-SiO2-P2O5Microcrystalline glass and Li2O-Al2O3-SiO2-B2O3Microcrystalline glass and Li2O-MgO-Al2O3-SiO2Microcrystalline glass and Li2O-ZnO-Al2O3-SiO2Microcrystalline glass, ZnO-MgO-Al2O3-SiO2Is microcrystalline glass, BaO-Al2O3-SiO2Microcrystalline glass and ZnO-Al2O3-SiO2One or more kinds of glass ceramics.
Furthermore, the microcrystalline glass is Li-Al-Si series microcrystalline glass. This is because the microcrystalline glass of this system has excellent thermal shock resistance, high strength and low expansion coefficient, and is the best system to be studied.
In a preferred embodiment, the Li-Al-Si based glass ceramics comprises the following components in parts by mass: li245-49 parts of O and Al2O329 to 32 parts of SiO216 to 20 portions of TiO 22 to 4 parts of Sb2O30.3-0.4 part and 0.1-0.5 part of ZnO.
Furthermore, in the coating process, the thickness of the microcrystalline glass coating is controlled to be 2% -6% of the filament diameter of the quartz bare fiber.
Further, the non-circularity of the filament diameter of the coated silica optical fiber is less than 0.1%.
And 2, cooling the quartz optical fiber coated in the step 1, and coating an organic coating on the outside of the microcrystalline glass coating when the quartz optical fiber is cooled to a set temperature to form an organic coating, so as to obtain the quartz optical fiber, as shown in fig. 1, 1 is the quartz optical fiber, wherein 11 is a quartz bare fiber, 12 is a microcrystalline glass coating, and 13 is an organic coating.
The set temperature in this step is the coating temperature of the organic coating, and the value of the set temperature needs to be determined according to the selected organic coating, and is generally around normal temperature, for example, the coating temperature of the acrylic resin is normal temperature, and the set temperature here is normal temperature.
In some embodiments, the organic coating is an acrylic resin, a silicone, or a polyimide. Preferably, the organic coating is an acrylic resin.
In some embodiments, when the components of the glass ceramics comprise, in parts by mass: li245-49 parts of O and Al2O329 to 32 parts of SiO216 to 20 portions of TiO 22 to 4 parts of Sb2O30.3-0.4 parts and 0.1-0.5 parts of ZnO, the step 1 specifically comprises the following steps:
(1) preparing materials: weighing the base powder Li2O、Al2O3And SiO2Powder of crystal nucleus agent TiO2Clarifying agent powder Sb2O3And ZnO powder, mixing and uniformly stirring the weighed powder, and adding the powder into a high-temperature container for 4-6 times in order to prevent the powder from splashing during feeding;
(2) melting: preheating a corundum crucible in an air atmosphere, slowly heating to 1200-1450 ℃, preserving heat for 10-30 minutes, preferably preserving heat for 20 minutes at 1350 ℃, then adding 4-6 parts of powder into the corundum crucible in batches for melting, keeping the temperature of a melting material at 1200-1450 ℃, and preserving heat for 30-60 minutes; clarifying for 1.5-2.5 h at 1500-1550 ℃, preferably for 2h at 1520 ℃ after the powder is completely melted, discharging to obtain microcrystalline glass liquid, and preserving the temperature of the microcrystalline glass liquid at 1200-1450 ℃.
In the step (2), adding 4-6 parts of powder into a corundum crucible for melting in several times, specifically comprising the following steps: preheating a corundum crucible in a muffle furnace at 800 ℃ for 2 hours, heating to 1200 ℃, adding 1 part of the powder, heating to 1430 ℃ in 15min, preserving heat for 20min, then sequentially adding the rest powder, adding each part of the powder, preserving heat for 20min, and then adding the next part of the powder. In the process of melting, a small amount of additive is adopted to avoid splashing, ensure the uniformity of material components and simultaneously require enough time to clarify the glass-ceramic liquid.
(3) Injecting the microcrystalline glass clear liquid in the corundum crucible into a platinum coating cup under an optical fiber perform melting and drawing mechanism, and preserving the temperature of the platinum coating cup at 1200-1450 ℃; adjusting the axis position of a quartz bare fiber from an optical fiber perform melt-drawing mechanism to coincide with the axis of an optical fiber outlet hole at the bottom of a platinum coating cup, and passing the high-temperature quartz bare fiber through microcrystalline glass liquid in the platinum coating cup before the temperature of the drawn quartz bare fiber is reduced to the glass transition temperature of the quartz bare fiber, preferably at 1200-1600 ℃, so that the microcrystalline glass liquid is coated on the surface of the high-temperature quartz bare fiber and is led out from the optical fiber outlet hole at the bottom of the platinum coating cup, and a microcrystalline glass coating is formed on the surface of the high-temperature quartz bare fiber; meanwhile, the thickness of the microcrystalline glass coating is controlled by the aperture of the optical fiber outlet hole at the bottom of the platinum coating cup.
It should be noted that the bare quartz fiber is rapidly cooled after being drawn from the optical fiber preform melting and drawing mechanism, and therefore, after drawing, the bare quartz fiber needs to pass through the platinum coating cup as fast as possible, and a heat preservation device is additionally arranged between the optical fiber preform melting and drawing mechanism and the platinum coating cup, and if necessary, a heating device can be further arranged to prevent the bare quartz fiber from being reduced below the glass transition temperature of the bare quartz fiber.
In the present embodiment, the thickness of the glass ceramic coating is controlled by the size of the fiber hole at the bottom of the platinum coating cup, for example: if the filament diameter of the drawn silica bare fiber is 115.74 μm and the aperture of the fiber outlet hole is 125 μm, the thickness of the coated microcrystalline glass coating is about 4.63 μm, and the coating thickness is 4% of the filament diameter of the silica bare fiber (before coating).
Experimental research shows that when the thickness of the microcrystalline glass coating is 2% -6% of the filament diameter of the quartz bare fiber, the microcrystalline glass coating can better improve the tensile strength of the quartz bare fiber, the effect of the microcrystalline glass coating is not obvious when the thickness of the microcrystalline glass coating is too thin, and the microcrystalline glass coating and the quartz glass are poor in bonding performance and easy to delaminate when the thickness of the microcrystalline glass coating is too thick.
The transition temperature of the quartz glass is about 1200 ℃, and the thermal shock damage to the quartz glass caused by high temperature is very small, so that the microcrystalline glass liquid only needs to meet the temperature higher than the transition temperature of the quartz glass by 1200 ℃, and the microcrystalline glass liquid is ensured to be in liquid state flow when the temperature is higher than 1200 ℃. In the embodiment of the invention, the quartz bare fiber is coated and molded by the microcrystalline glass liquid above the glass transition temperature of the quartz bare fiber. This is because the transition temperature of the quartz glass is about 1200 ℃, and it has been found through a large number of experiments that the quartz glass generates less microcracks above the transition temperature and is less likely to expand. Therefore, after the surface of the high-temperature quartz optical fiber is coated with the microcrystalline glass low-expansion coating, the generation and the expansion of the microcracks can be greatly weakened in the subsequent cooling process. Therefore, the melting temperature of the microcrystalline glass is selected to be 1200-1400 ℃, the temperature of the liquid crystal glass for coating the microcrystalline glass liquid before the glass transition temperature of the quartz optical fiber is ensured to be not less than 1200 ℃, but the melting temperature of the microcrystalline glass is not too high, and the requirements on a coating mechanism, energy consumption and the like are increased when the melting temperature of the microcrystalline glass is higher than 1400 ℃, and the coating temperature of the microcrystalline glass is preferably the same as or close to the temperature of the quartz optical fiber during coating.
The coating environment can be in vacuum or air, and the quartz glass does not reach a hardening state and generate cracks no matter in vacuum or air because the coating is at high temperature; the microcrystalline glass material system is also an oxide, so that coating under vacuum or air atmosphere is feasible.
According to the embodiment of the invention, the microcrystalline glass coating and the organic coating are sequentially coated on the surface of the quartz glass, so that the quartz optical fiber with double coatings is obtained. The embodiment of the invention improves the tensile strength of the quartz optical fiber through the double coatings so as to break through the limitation of the tensile strength of the existing quartz optical fiber and meet the application of the quartz optical fiber in the modern high-end science and technology field.
The quartz glass is used as a brittle material, and the generation and the expansion of micro cracks on the surface of the quartz optical fiber are easily caused in the processes of drawing and cooling. Therefore, the present embodiment applies the glass-ceramic liquid to the surface of the bare silica fiber by using the high-temperature in-line coating method before applying the organic coating layer and before the temperature of the bare silica fiber after drawing is lowered to the glass transition temperature thereof, and defines that the expansion coefficient of the glass-ceramic is less than 5 × 10-7and/DEG C, forming a microcrystalline glass coating with a low expansion coefficient on the surface of the quartz bare fiber, wherein in the cooling process of the coated quartz fiber, the low expansion characteristic of the microcrystalline glass coating can form a pre-stress on the surface of the quartz fiber so as to reduce the generation of microcracks in the quartz fiber and inhibit the expansion of the microcracks in the quartz fiber, thereby improving the tensile strength of the quartz fiber and prolonging the mechanical life of the fiber. It is also an important advantage that the pre-stress will make the surface of the silica fiber have greater hardness and abrasion resistance, so that the surface of the silica fiber is not easily damaged, thereby reducing the requirements for the manufacturing conditions of the fiber and increasing the reliability of the silica fiber. The expansion coefficient of the microcrystalline glass is smaller than that of the quartz bare fiber, the expansion coefficient of the microcrystalline glass is closer to that of the quartz bare fiber, and the microcrystalline glass has higher matching degree. In the process of cooling the coated quartz optical fiber, due to the low expansion characteristic of the microcrystalline glass coating, a pre-stress layer can be formed on the surface of the quartz bare fiber, so that the effect of improving the tensile strength of the quartz optical fiber is achieved. The reinforcing mechanism can further improve the tensile strength of the quartz optical fiber on the basis of the existing reinforcing of the coating organic coating. The data relating to the examples also confirm thisThe conclusion is that the tensile strength of the silica optical fiber coated with the microcrystalline glass coating is improved by about 5-6% compared with the tensile strength of the silica optical fiber not coated with the microcrystalline glass coating, so that the tensile strength of the silica optical fiber coated with the microcrystalline glass coating exceeds 6GPa and even reaches 6.136GPa, and the technical problem that the existing silica optical fiber is easy to break is solved.
The coefficient of expansion of pure silica glass (silica bare fiber) is about 5X 10-7The microcrystalline glass material has a coefficient of expansion of less than 5X 10 at/° C-7Preferably, the coefficient of expansion is 5X 10/. degree.C-8The low expansion material which is near/DEG C and has higher strength per se is used as the optical fiber coating to reduce the tensile stress and even form the compressive stress on the surface of the quartz optical fiber, so that the generation and the expansion of micro cracks of the quartz optical fiber coated with the microcrystalline glass coating are reduced in the cooling process. Further research shows that the microcrystalline glass coating with low expansion coefficient can improve the tensile strength of the quartz optical fiber, and experimental data also verifies that the tensile strength of the quartz optical fiber can be really improved by coating the low-expansion microcrystalline glass on the surface of the quartz optical fiber at high temperature. This is different from the existing organic coating, because the organic coating requires a lower coating temperature, and it is necessary to coat the optical fiber when the optical fiber is cooled to the coating temperature of the organic coating, and during the cooling process, the micro cracks on the surface of the quartz optical fiber are generated, and the micro cracks generated by coating the organic coating are not reduced.
As shown in fig. 2 and 3, another embodiment of the present invention provides an apparatus for manufacturing a silica optical fiber, which is used for implementing the aforementioned manufacturing method, and includes: the device comprises an optical fiber perform fusion drawing mechanism 2, a microcrystalline glass coating mechanism 3, an organic coating mechanism 4 and a traction mechanism 5 which are arranged in sequence from top to bottom, wherein the optical fiber perform fusion drawing mechanism 2 is used for fusing and drawing the optical fiber perform into a quartz bare fiber; the microcrystalline glass coating mechanism 3 comprises a first coating cup 31 for containing microcrystalline glass liquid 32, the first coating cup 31 is placed in a cavity surrounded by a heat-insulating brick 35, a heating component 33 such as a heating resistance wire is arranged around the first coating cup 31, heat-insulating cotton 34 is filled in a gap between the heat-insulating brick 35 and the first coating cup 31, an optical fiber lead hole 36 is arranged at the top of the first coating cup 31, and an optical fiber outlet hole 37 is arranged at the bottom of the first coating cup 31; the organic coating mechanism 4 comprises a second coating cup 41 for containing organic coating 42; the traction mechanism 5 is used for providing power for drawing the optical fiber;
an optical fiber auxiliary traction mechanism 6 is arranged between the microcrystalline glass coating mechanism 3 and the organic coating mechanism 4, so that the axis of the quartz bare fiber coming out of the optical fiber perform melting and drawing mechanism 2 is superposed with the axis of the microcrystalline glass coating mechanism 3 and the axis of the organic coating mechanism 4;
temperature sensors (not shown in the figure) are arranged at the optical fiber lead hole 36, the optical fiber outlet hole 37, the microcrystalline glass liquid containing position in the first coating cup, the top inlet, the organic coating containing position in the second coating cup 41 and the bottom outlet of the first coating cup, and are respectively connected with a programmable logic controller through corresponding signal transmitters; the programmable logic controller is connected with a main control computer (not shown in the figure).
The temperature of the microcrystalline glass liquid contained in the first coating cup needs to be measured so as to ensure that the temperature is higher than 1200 ℃ and constant, so that the coating process is stable. The temperature control can be detected on line by a thermocouple or a temperature measuring gun so as to realize automatic coating.
The temperature of the quartz optical fiber at different stages and the temperature inside the coating cup are monitored in real time on a main control computer. The device simple structure can realize automatic coating, has guaranteed the coating effect of quartz optical fiber when the coating.
Further, the first coating cup 31 is a platinum coating cup and includes a cup body and an optical fiber leading-out component, the optical fiber leading-out component is detachably connected to the bottom of the cup body, the optical fiber leading-out hole 36 is located at the top of the cup body, and the optical fiber leading-out hole 37 is located at the bottom of the optical fiber leading-out component.
According to the device provided by the embodiment of the invention, the platinum coating cup is divided into two parts, the optical fiber leading-out component is detachably connected to the bottom of the cup body, the optical fiber outlet hole with a proper aperture can be selected according to needs, and the aperture of the optical fiber outlet hole can be conveniently adjusted by replacing the optical fiber leading-out component so as to obtain the required coating thickness.
The platinum coating cup can ensure the high-temperature fluidity of the microcrystalline glass liquid during high-temperature coating and ensure the uniformity of the coating thickness on the micron scale. Although the platinum coating cup is high in price when the device is built at the beginning, the platinum coating cup is stable and not easy to wear, and can be stably used for a long time.
As shown in fig. 1, a silica optical fiber 1 according to still another embodiment of the present invention includes, in order from inside to outside: a quartz bare fiber 11, a microcrystalline glass coating 12 and an organic coating 13; wherein the expansion coefficient of the microcrystalline glass used for the microcrystalline glass coating 12 is less than 5 multiplied by 10-7The melting temperature is 1200-1400 ℃, and the core layer and the skin layer of the quartz bare fiber 11 are made of quartz glass materials.
Further, the silica fiber is obtained by the preparation method of the silica fiber. The microcrystalline glass coating is formed by coating before the temperature of the drawn quartz bare fiber is reduced to the glass transition temperature, and because the expansion coefficient of the microcrystalline glass is smaller than that of the quartz bare fiber and the expansion coefficient of the microcrystalline glass has higher matching degree with that of the quartz bare fiber, in the cooling process of the coated quartz fiber, the low expansion characteristic of the microcrystalline glass coating can form pre-stress on the surface of the quartz fiber so as to reduce the generation of micro cracks in the quartz fiber and inhibit the expansion of the micro cracks in the quartz fiber, thereby improving the tensile strength of the quartz fiber and prolonging the mechanical life of the fiber.
In some embodiments, the glass-ceramic is a Li-Al-Si based glass-ceramic.
Further, the above-mentioned Li-Al-Si based glass ceramicsThe components comprise the following components in parts by mass: li245-49 parts of O and Al2O329 to 32 parts of SiO216 to 20 portions of TiO 22 to 4 parts of Sb2O30.3-0.4 part and 0.1-0.5 part of ZnO.
In some embodiments, the microcrystalline glass has a coefficient of expansion of 5 x 10-9～5×10-7/° c; the thickness of the microcrystalline glass coating is 2% -6% of the diameter of the quartz bare fiber; the organic coating is made of acrylic resin, organic silica gel or polyimide.
The tensile strength of the quartz optical fiber obtained by the embodiment of the invention is more than 6GPa, and the quartz optical fiber can meet the occasions with high-strength use requirements, such as high-grade communication optical fibers.
The present invention will be further described with reference to the following specific examples, which should not be construed as limiting the scope of the invention, but rather as providing those skilled in the art with certain insubstantial modifications and adaptations of the invention based on the teachings of the invention set forth herein.
In the following examples of the present invention, the components referred to may be commercially available unless otherwise specified, and the methods referred to may be conventional unless otherwise specified.
Example 1
(1) Weighing Li2329g of O powder and Al2O3216g of powder of SiO2127.6g of powder, TiO220.6g of powder Sb2O32.5g of powder and 1.5g of ZnO powder; mixing and uniformly stirring the weighed powder, and then averagely dividing the powder into 6 parts, wherein each part is 116 g;
(2) preheating a 500mL corundum crucible in a muffle furnace at 800 ℃ for 2 hours, heating to 1200 ℃, adding 1 part of the powder obtained in the step (1), heating to 1430 ℃ in 15min, preserving heat for 20min, then sequentially adding 2 nd part of the powder, preserving heat for 20min, and sequentially adding 6 th part of the powder; clarifying for 2 hours at 1520 ℃ after the powder is completely melted; preheating a platinum coating cup to 1430 ℃, preserving heat, and introducing molten glass of the corundum crucible into the platinum coating cup at high temperature;
(3) introducing a drawn high-temperature quartz bare fiber from the top of an optical fiber preform melting and drawing mechanism, adjusting the axis position of the high-temperature quartz bare fiber from the optical fiber preform melting and drawing mechanism to enable the axis position to coincide with the axis of an optical fiber outlet hole at the bottom of a platinum coating cup, and when the temperature of the drawn high-temperature quartz bare fiber is reduced to 1700 ℃, enabling the high-temperature quartz bare fiber to penetrate through the platinum coating cup, coating the clarified liquid on the surface of the quartz bare fiber, and leading out from the optical fiber outlet hole at the bottom of the platinum coating cup to form a microcrystalline glass coating; wherein the filament diameter of the quartz bare fiber before coating is 115.74 μm, the aperture of the fiber outlet hole at the bottom of the platinum coating cup is 125 μm, the thickness of the microcrystalline glass coating is close to 4.63 μm, and the thickness of the microcrystalline glass coating is 4% of the filament diameter of the quartz bare fiber before coating;
(4) and (4) after the coated quartz optical fiber obtained in the step (3) is cooled to normal temperature, coating acrylic resin on the surface of the microcrystalline glass coating to form an organic coating, and thus obtaining the quartz optical fiber with the wire diameter of 250 mu m and the double coatings.
Part 31 of the specification for the optical fiber test method according to the national standard GB/T15972.31-2008: method and procedure for measuring mechanical properties-tensile strength-the strength of the prepared silica optical fiber was measured to obtain a tensile strength of 6.136 GPa.
Example 2
(1) Weighing Li2312g of O powder and Al2O3218g of powder, SiO2Powder 130g, TiO2Powder 27g, Sb2O32g of powder and 3g of ZnO powder. Mixing and uniformly stirring the weighed powder, and then averagely dividing the powder into 6 parts, wherein each part is 115.3 g;
(2) preheating a 500mL corundum crucible in a muffle furnace at 800 ℃ for 2 hours, heating to 1200 ℃, adding 1 part of the powder obtained in the step (1), heating to 1400 ℃ in 15min, preserving heat for 20min, then sequentially adding the 2 nd part of the powder, preserving heat for 20min, and sequentially adding the 6 th part of the powder according to the above; after the powder is completely melted, clarifying for 2 hours at 1550 ℃; preheating a platinum crucible coating cup to 1430 ℃, preserving heat, and introducing molten glass of the corundum crucible into the platinum coating cup at high temperature;
(3) drawing by adopting the same process as that of the embodiment 1, and when the temperature of the drawn high-temperature quartz bare fiber is reduced to 1650 ℃, enabling the high-temperature quartz bare fiber to penetrate through the platinum coating cup, so that the clarified liquid is coated on the surface of the quartz bare fiber and is led out from an optical fiber outlet hole at the bottom of the platinum coating cup to form a microcrystalline glass coating; wherein the filament diameter of the quartz bare fiber before coating is 120.19 μm, the aperture of the fiber outlet hole at the bottom of the platinum coating cup is 125 μm, the thickness of the microcrystalline glass coating is close to 2.4 μm, and the thickness of the microcrystalline glass coating is 2% of the filament diameter of the quartz bare fiber before coating.
(4) And (4) after the coated quartz optical fiber obtained in the step (3) is cooled to normal temperature, coating acrylic resin on the surface of the microcrystalline glass coating to form an organic coating, and thus obtaining the quartz optical fiber with the wire diameter of 250 mu m and the double coatings.
Part 31 of the specification for the optical fiber test method according to the national standard GB/T15972.31-2008: method and procedure for measuring mechanical properties-tensile strength-the strength of the prepared silica optical fiber was measured to obtain a tensile strength of 6.095 GPa.
Example 3
(1) Weighing Li2325g of O powder and Al powder2O3212g of powder, SiO2110g of powder, TiO214g of powder, Sb2O32g of powder and 1g of ZnO powder. Mixing and uniformly stirring the weighed powder, and then averagely dividing the powder into 6 parts, wherein each part is 110.7 g;
(2) preheating a 500mL corundum crucible in a muffle furnace at 800 ℃ for 2 hours, heating to 1200 ℃, adding 1 part of the powder obtained in the step (1), heating to 1500 ℃ in 15min, preserving heat for 20min, then sequentially adding the 2 nd part of the powder, preserving heat for 20min, and sequentially adding the 6 th part of the powder according to the above; clarifying for 2 hours at 1500 ℃ after the powder is completely melted; preheating a platinum crucible coating cup to 1430 ℃, preserving heat, and introducing molten glass of the corundum crucible into the platinum coating cup at high temperature;
(3) drawing by adopting the same process as that of the embodiment 1, and when the temperature of the drawn high-temperature quartz bare fiber is reduced to 1750 ℃, enabling the high-temperature quartz bare fiber to penetrate through a platinum coating cup, so that the clarified liquid is coated on the surface of the quartz bare fiber and is led out from an optical fiber outlet hole at the bottom of the platinum coating cup to form a microcrystalline glass coating; wherein the filament diameter of the quartz bare fiber before coating is 111.61 μm, the aperture of the fiber outlet hole at the bottom of the platinum coating cup is 125 μm, the thickness of the microcrystalline glass coating is close to 6.70 μm, and the thickness of the microcrystalline glass coating is 6% of the filament diameter of the quartz bare fiber before coating.
(4) And (4) after the coated quartz optical fiber obtained in the step (3) is cooled to normal temperature, coating acrylic resin on the surface of the microcrystalline glass coating to form an organic coating, and thus obtaining the quartz optical fiber with the wire diameter of 250 mu m and the double coatings.
Part 31 of the specification for the optical fiber test method according to the national standard GB/T15972.31-2008: method and procedure for measuring mechanical properties-tensile strength-the strength of the prepared silica optical fiber was measured to obtain a tensile strength of 6.079 GPa.
Comparative example
The same process as that of example 1 was used for drawing, and after the drawn silica bare fiber was cooled to a certain temperature, the acrylic resin organic coating was applied to the silica bare fiber to obtain a silica fiber with a filament diameter of 250 μm, which was coated with only the organic coating and not with the microcrystalline glass coating.
Part 31 of the specification for the optical fiber test method according to the national standard GB/T15972.31-2008: method and procedure for measuring mechanical properties-tensile strength-uncoated silica fiber was subjected to strength testing to obtain a tensile strength of 5.785 GPa.
As can be seen from examples 1 to 3 and comparative example, the tensile strength (6.136GPa) of the silica optical fiber obtained in example 1 was improved by about 6.06% over the tensile strength (5.785GPa) of the silica optical fiber obtained in comparative example; the tensile strength (6.095GPa) of the silica optical fiber obtained in example 2 is improved by about 5.35% compared with the tensile strength (5.785GPa) of the silica optical fiber obtained in the comparative example; the tensile strength (5.785GPa) of the silica optical fiber obtained in example 3 was improved by about 5.07% compared with the tensile strength (6.079GPa) of the silica optical fiber obtained in comparative example.
It can be seen from the above that the tensile strength of the silica optical fiber with double coating obtained by the method of embodiments 1 to 3 of the present invention is further improved compared with the tensile strength of the silica optical fiber coated with only the organic coating obtained by the comparative example.
According to the invention, the microcrystalline glass coating is formed on the surface of the quartz bare fiber by adopting a high-temperature online coating method, and after cooling, the organic coating is formed on the surface of the microcrystalline glass coating to obtain the quartz fiber with the double coatings, so that the tensile strength of the quartz fiber can be further improved on the basis of the existing organic coating enhancement. The microcrystalline glass and the quartz glass have very similar components and performances, so that the microcrystalline glass and the quartz glass have better bonding performance with the surface of the quartz bare fiber, and the effect of improving the tensile strength of the quartz fiber is achieved. Meanwhile, because the expansion coefficient of the microcrystalline glass is smaller than that of the quartz bare fiber, and the expansion coefficient of the microcrystalline glass has higher matching degree with that of the quartz bare fiber, the low expansion characteristic of the microcrystalline glass coating can form pre-stress on the surface of the quartz fiber in the cooling process of the coated quartz fiber, so that the generation of microcracks in the quartz fiber is reduced, the expansion of the microcracks in the quartz fiber is inhibited, the tensile strength of the quartz fiber is improved, and the mechanical life of the fiber is prolonged. When the method is used for communication optical fibers, the method reduces breakpoints inside the optical fibers, and can improve the transmission efficiency of light.
In the description of the present invention, it should be noted that the terms "upper", "lower", "horizontal", "vertical", and the like indicate orientations or positional relationships based on methods or positional relationships shown in the drawings, and are only for convenience of describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
In addition, in the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "connected" and "connected" should be interpreted broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (12)

1. A method for preparing a silica optical fiber, comprising: coating microcrystalline glass liquid on the surface of the quartz bare fiber to form a microcrystalline glass coating before the temperature of the drawn quartz bare fiber is reduced to the glass transition temperature of the quartz bare fiber; cooling, coating organic paint on the surface of the microcrystalline glass coating to form an organic coating, and obtaining the quartz optical fiber, wherein the expansion coefficient of the microcrystalline glass is less than 5 multiplied by 10-7The temperature is 1200-1400 ℃; the core layer and the skin layer of the quartz bare fiber are both made of quartz glass materials.
2. The method of manufacturing a silica optical fiber according to claim 1,
the coating temperature of the microcrystalline glass liquid is 1200-1450 ℃;
the temperature range before the glass transition temperature is 1200-1600 ℃.
3. The method for preparing a silica optical fiber according to claim 1 or 2, wherein the thickness of the microcrystalline glass coating layer is controlled to be 2% to 6% of the filament diameter of the silica bare fiber during the coating process.
4. The method of manufacturing a silica optical fiber according to claim 1 or 2, wherein the glass-ceramics is Li-Al-Si based glass-ceramics.
5. The method of manufacturing a silica optical fiber according to claim 4,
the Li-Al-Si series glass ceramics comprises the following components in parts by mass: li245-49 parts of O and Al2O329 to 32 parts of SiO216 to 20 portions of TiO22 to 4 parts of Sb2O30.3-0.4 part and 0.1-0.5 part of ZnO.
6. The method of manufacturing a silica optical fiber according to claim 2,
the expansion coefficient of the microcrystalline glass is 5 multiplied by 10-9～5×10-7/℃；
The organic coating is acrylic resin, organic silica gel or polyimide.
7. An apparatus for manufacturing a silica optical fiber, comprising: the device comprises an optical fiber perform fusion drawing mechanism, a microcrystalline glass coating mechanism, an organic coating mechanism and a traction mechanism which are sequentially arranged from top to bottom, wherein the optical fiber perform fusion drawing mechanism is used for fusing and drawing the optical fiber perform into a quartz bare fiber; the microcrystalline glass coating mechanism comprises a first coating cup, wherein the first coating cup is used for containing microcrystalline glass liquid, the first coating cup is arranged in a cavity surrounded by insulating bricks, heating parts are arranged around the first coating cup, insulating cotton is filled in a gap between the insulating bricks and the first coating cup, an optical fiber lead hole is formed in the top of the first coating cup, and an optical fiber lead hole is formed in the bottom of the first coating cup; the organic coating mechanism comprises a second coating cup for containing organic coating; the traction mechanism is used for providing power for drawing the optical fiber;
an optical fiber auxiliary traction mechanism is arranged between the microcrystalline glass coating mechanism and the organic coating mechanism, so that the axis of the quartz bare fiber from the optical fiber perform melting and drawing mechanism is superposed with the axis of the microcrystalline glass coating mechanism and the axis of the organic coating mechanism;
temperature sensors are arranged at an optical fiber lead hole, an optical fiber outlet hole of the first coating cup, a microcrystalline glass liquid containing position in the first coating cup, a top inlet, an organic coating containing position in the second coating cup and a bottom outlet of the second coating cup, and the temperature sensors are respectively connected with a programmable logic controller through corresponding signal transmitters; the programmable logic controller is connected with the main control computer.
8. The apparatus of claim 7, wherein the first paint cup is a platinum paint cup comprising a cup body and a fiber pigtail component removably attached to a bottom of the cup body, the fiber pigtail hole being located at a top of the cup body, the fiber pigtail hole being located at a bottom of the fiber pigtail component.
9. A quartz optical fiber is characterized by comprising a quartz bare fiber, a microcrystalline glass coating and an organic coating in sequence from inside to outside; wherein the expansion coefficient of the microcrystalline glass used for the microcrystalline glass coating is less than 5 multiplied by 10-7The temperature is 1200-1400 ℃; the core layer and the skin layer of the quartz bare fiber are both made of quartz glass materials.
10. The silica optical fiber according to claim 9,
the microcrystalline glass is Li-Al-Si series microcrystalline glass.
11. The silica optical fiber according to claim 10,
the Li-Al-Si series glass ceramics comprises the following components in parts by mass: li245-49 parts of O and Al2O329 to 32 parts of SiO216 to 20 portions of TiO22 to 4 parts of Sb2O30.3-0.4 part and 0.1-0.5 part of ZnO.
12. The silica optical fiber according to claim 9,
the expansion coefficient of the microcrystalline glass is 5 multiplied by 10-9～5×10-7/° c; the thickness of the microcrystalline glass coating is 2% -6% of the diameter of the quartz bare fiber;
the organic coating is an acrylic resin coating, an organic silica gel coating or a polyimide coating.
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