CN115010360A - Preparation method of optical fiber preform, optical fiber preform and optical fiber - Google Patents

Preparation method of optical fiber preform, optical fiber preform and optical fiber Download PDF

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Publication number
CN115010360A
CN115010360A CN202210825227.4A CN202210825227A CN115010360A CN 115010360 A CN115010360 A CN 115010360A CN 202210825227 A CN202210825227 A CN 202210825227A CN 115010360 A CN115010360 A CN 115010360A
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inner cladding
optical fiber
flow rate
fiber preform
gas
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CN115010360B (en
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何亮
陈京京
周建峰
吴椿烽
沈一春
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Zhongtian Technology Advanced Materials Co ltd
Jiangsu Zhongtian Technology Co Ltd
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Zhongtian Technology Advanced Materials Co ltd
Jiangsu Zhongtian Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01Manufacture of glass fibres or filaments
    • C03B37/012Manufacture of preforms for drawing fibres or filaments
    • C03B37/014Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01Manufacture of glass fibres or filaments
    • C03B37/012Manufacture of preforms for drawing fibres or filaments
    • C03B37/014Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/01446Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01Manufacture of glass fibres or filaments
    • C03B37/02Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
    • C03B37/025Manufacture 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
    • C03B37/027Fibres composed of different sorts of glass, e.g. glass optical fibres
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/50Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57Improving the yield, e-g- reduction of reject rates

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Manufacture, Treatment Of Glass Fibers (AREA)

Abstract

The invention provides a preparation method of an optical fiber preform, the optical fiber preform and an optical fiber. The preparation method of the optical fiber preform of the present invention comprises: carrying out deposition treatment on the seed rod, and sequentially forming a core layer, a first inner cladding layer, a second inner cladding layer and a third inner cladding layer on the outer surface of the seed rod to obtain a powder loose body; sequentially carrying out dehydroxylation treatment and vitrification sintering on the powder loose body to obtain a glass rod; carrying out deposition treatment on the glass rod to obtain an optical fiber preform; wherein, the powder density of the first inner cladding, the powder density of the second inner cladding and the powder density of the third inner cladding are reduced in sequence; the powder density of the first inner cladding, the second inner cladding and the third inner cladding are all more than 0.21g/cm 2 . The optical fiber preform obtained by the method can form an optical fiber preform which has excellent bending resistance and service life, can be well butted with a G652 optical fiber and conforms to various wavesThe required optical fiber is transmitted in the section.

Description

Preparation method of optical fiber preform, optical fiber preform and optical fiber
Technical Field
The invention relates to the technical field of optical fiber preparation, in particular to a preparation method of an optical fiber preform, the optical fiber preform and an optical fiber.
Background
As broadband services begin to be fiber-to-the-home, the key point in the construction of communication networks is the development from core networks to fiber access networks. In the construction of an optical fiber access network, an optical fiber cable including an optical fiber needs to be placed in a crowded pipeline, or the optical fiber cable including the optical fiber needs to be bent many times and then fixed in a line receiving end in a narrow space such as a junction box or a socket, so that the optical fiber is squeezed and bent to attenuate a signal. Therefore, more and more optical fiber manufacturers are beginning to research and manufacture optical fibers having excellent bending resistance and less bending loss when being wired in a narrow space.
The prior art has attempted to improve the bend resistance of optical fibers by the following methods, respectively: for example, the mode field diameter of the fiber is reduced, and/or the cut-off wavelength of the fiber is increased to try to improve the bending resistance of the fiber, but the fiber with small mode field diameter cannot form a good connection with the common G652 fiber, so that the large connection loss is generated, the increase space of the cut-off wavelength of the fiber is limited, and if the cut-off wavelength exceeds 1260nm, the fiber does not meet the requirement of full-band transmission; or, an inner cladding with a low-refraction groove is formed on the outer side of the core rod in a melting and shrinking mode, when the optical fiber is bent, the refractive index of the optical fiber can be reduced by using the cladding with the low-refraction groove, so that the optical fiber can form total reflection transmission, and signal attenuation caused by bending of the optical fiber is avoided, but the size and interface problems are easy to occur between the core rod and the inner cladding with the low-refraction groove due to the melting and shrinking mode, and the service life of the optical fiber is influenced; in addition, can also improve the energy constraint ability of optical fiber core layer through trompil in order to provide the air bed in optic fibre on optical fiber perform to reduce the bending loss of optic fibre, but trompil on optical fiber perform reduces optical fiber perform's production efficiency easily, and then reduces the production efficiency of optic fibre.
Therefore, it is urgently needed to provide an optical fiber which has excellent bending resistance and service life, can realize good butt joint with a G652 optical fiber, meets transmission requirements of various wavebands, and has simple preparation process and low production cost.
Disclosure of Invention
The optical fiber preform obtained by the method can form an optical fiber which has excellent bending resistance and service life, can be well butted with a G652 optical fiber and meets the transmission requirements of various wavebands, and the preparation method is simple in process and low in production cost.
The optical fiber preform is prepared by the preparation method of the optical fiber preform, can be used for preparing optical fibers which have excellent bending resistance and service life, can be well butted with G652 optical fibers and meet the transmission requirements of various wave bands, and is simple in preparation process and low in production cost.
The invention provides an optical fiber which is prepared according to the optical fiber preform, has excellent bending resistance and service life, can be well butted with a G652 optical fiber and meets the transmission requirements of various wave bands, and has simple preparation process and low production cost.
The invention provides a preparation method of an optical fiber preform, which comprises the following steps:
carrying out deposition treatment on the seed rod, and sequentially forming a core layer, a first inner cladding layer, a second inner cladding layer and a third inner cladding layer on the outer surface of the seed rod to obtain a powder loose body;
sequentially carrying out dehydroxylation treatment and vitrification sintering on the powder loose body to obtain a glass rod;
carrying out deposition treatment on the glass rod to obtain the optical fiber perform rod;
wherein the powder density of the first inner cladding, the powder density of the second inner cladding and the powder density of the third inner cladding are sequentially reduced;
the powder density of the first inner cladding, the powder density of the second inner cladding and the powder density of the third inner cladding are all more than 0.21g/cm 2
The method for preparing an optical fiber preform as described above, wherein the first inner cladding has a soot density of 0.26 to 0.29g/cm 2 (ii) a And/or the presence of a gas in the gas,
the powder density of the second inner cladding is 0.24-0.27 g/cm 2 (ii) a And/or the presence of a gas in the gas,
the powder density of the third inner cladding is 0.22-0.25 g/cm 2
The method for fabricating an optical fiber preform as described above, wherein a core layer raw material is deposited on an outer surface of the seed rod, and the core layer is formed on the outer surface of the seed rod;
wherein, the core layer raw materials include: silicon tetrachloride, germanium tetrachloride, hydrogen, oxygen, and argon;
the flow of the silicon tetrachloride is 2-5 g/min, the flow of the germanium tetrachloride is 300-500 mg/min, the flow of the hydrogen is 7-9L/min, the flow of the oxygen is 10-15L/min, and the flow of the argon is 5-10L/min; and/or the presence of a gas in the atmosphere,
and in the deposition process of the core layer, the temperature is 800-1000 ℃.
The method for preparing an optical fiber preform as described above, wherein a first inner cladding raw material is deposited on the outer surface of the core layer, and the first inner cladding is formed on the outer surface of the core layer;
wherein, the first inner cladding raw material comprises: silicon tetrachloride, hydrogen, oxygen and argon;
the flow rate of the silicon tetrachloride is 25-30 g/min, the flow rate of the hydrogen is 90-100L/min, the flow rate of the oxygen is 45-50L/min, and the flow rate of the argon is 10-20L/min; and/or the presence of a gas in the gas,
and in the deposition process of the first inner cladding, the temperature is 1300-1400 ℃.
The method for preparing an optical fiber preform as described above, wherein a second inner cladding raw material is deposited on the outer surface of the first inner cladding, and the second inner cladding is formed on the outer surface of the first inner cladding;
wherein, the second inner cladding raw material comprises: silicon tetrachloride, hydrogen, oxygen and argon;
the flow rate of the silicon tetrachloride is 25-30 g/min, the flow rate of the hydrogen is 85-95L/min, the flow rate of the oxygen is 40-45L/min, and the flow rate of the argon is 10-20L/min; and/or the presence of a gas in the gas,
and in the deposition process of the second inner cladding, the temperature is 1250-1350 ℃.
The method for fabricating an optical fiber preform as described above, wherein a third inner cladding raw material is deposited on the outer surface of the second inner cladding, and the third inner cladding is formed on the outer surface of the second inner cladding;
wherein, the third inner cladding raw material comprises: silicon tetrachloride, hydrogen, oxygen, and argon;
the flow rate of the silicon tetrachloride is 25-30 g/min, the flow rate of the hydrogen is 80-85L/min, the flow rate of the oxygen is 35-40L/min, and the flow rate of the argon is 10-20L/min; and/or the presence of a gas in the atmosphere,
and in the deposition process of the third inner cladding, the temperature is 1250-1350 ℃.
The method for fabricating an optical fiber preform as described above, wherein the soot bulk is dehydroxylated using a dehydroxylated feedstock;
the dehydroxylation raw material comprises: chlorine, helium, and fluoride;
the flow rate of the chlorine is 500-1000 cc/min, the flow rate of the helium is 15-25L/min, and the flow rate of the fluoride is 200-500 cc/min; and/or the presence of a gas in the gas,
in the de-hydroxylation treatment process, the temperature is 1000-1100 ℃, and the pressure is 5-10 Pa.
The method for manufacturing an optical fiber preform as described above, wherein the glass rod is obtained by performing the vitrification sintering of the soot body subjected to the dehydroxylation treatment using a vitrification raw material;
the vitrification raw material comprises: helium and fluoride;
the flow rate of the helium is 15-25L/min, and the flow rate of the fluoride is 100-500 cc/min; and/or the presence of a gas in the gas,
in the process of vitrification sintering, the temperature is 1350-1500 ℃, and the pressure is 10-15 Pa.
The invention also provides an optical fiber preform, wherein the optical fiber preform is prepared according to the preparation method of the optical fiber preform.
The invention also provides an optical fiber, wherein the optical fiber is obtained by stretching the optical fiber preform.
The preparation method of the optical fiber preform rod controls the powder density of the first inner cladding, the second inner cladding and the third inner cladding to be more than 0.21g/cm in the preparation process 2 The number of the inner cladding layers is reduced in sequence, a low-refractive-index inner cladding layer with gradient can be formed on the outer surface of the core layer, the inner cladding layer with the gradient can effectively restrain light when the optical fiber is bent, and light leakage is avoided to increase bending loss of the optical fiber; the preparation method has simple process and low production cost, is beneficial to obtaining the optical fiber which has long service life, can realize good butt joint with the G652 optical fiber and meets the transmission requirements of various wave bands.
The optical fiber perform rod is prepared according to the preparation method of the optical fiber perform rod, the optical fiber perform rod can prepare the optical fiber which has excellent bending resistance and service life, can realize good butt joint with the G652 optical fiber and meets the transmission requirements of various wave bands, and the preparation process of the optical fiber perform rod is simple and the production cost is low.
The optical fiber is prepared according to the optical fiber preform, has excellent bending resistance and service life, can be well butted with a G652 optical fiber, meets the transmission requirements of various wave bands, and has the advantages of simple preparation process and low production cost.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the related art, the drawings used in the description of the embodiments of the present invention or the related art are briefly introduced below. It is obvious that the drawings in the following description are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
FIG. 1 is a schematic structural view of a deposition apparatus according to some embodiments of the present invention;
FIG. 2 is a schematic diagram of a sintering apparatus according to some embodiments of the present invention.
Description of reference numerals:
1: seed rods;
2: a deposition chamber;
3: a core layer burner;
4: a first inner clad burner;
5: an air outlet;
6: a powder compact;
7: a glass tube;
8: a heating body;
9: a pressure controller;
10: an exhaust port;
11: an air inlet;
12: a second inner clad burner;
13: and a third inner cladding burner.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A first aspect of the present invention provides a method for preparing an optical fiber preform, comprising the steps of:
carrying out deposition treatment on the seed rod, and sequentially forming a core layer, a first inner cladding layer, a second inner cladding layer and a third inner cladding layer on the outer surface of the seed rod to obtain a powder loose body;
sequentially carrying out dehydroxylation treatment and vitrification sintering on the powder loose body to obtain a glass rod;
carrying out deposition treatment on the glass rod to obtain an optical fiber preform;
wherein, the powder density of the first inner cladding, the powder density of the second inner cladding and the powder density of the third inner cladding are reduced in sequence;
the powder density of the first inner cladding, the powder density of the second inner cladding and the powder density of the third inner cladding are all more than 0.21g/cm 2
It can be understood that the method for preparing an optical fiber preform of the present invention comprises: depositing the seed rod to form a core layer on the outer surface of the seed rod to obtain a core rod, then depositing a first inner cladding layer on the outer surface of the core layer, depositing a second inner cladding layer on the outer surface of the first inner cladding layer, and finally depositing a third inner cladding layer on the outer surface of the second inner cladding layer to obtain a powder loose body which sequentially comprises the seed rod, the core layer, the first inner cladding layer, the second inner cladding layer and the third inner cladding layer from inside to outside; then carrying out dehydroxylation treatment on the powder loose body to remove water in the powder loose body, then carrying out vitrification sintering on the powder loose body from which the water is removed to sinter the powder loose body into a glass rod, wherein the dehydroxylation treatment and the vitrification sintering are generally doped with fluoride, and after the dehydroxylation treatment and the vitrification sintering, the fluoride enters a second inner cladding and a third inner cladding so that the second inner cladding and the third inner cladding form a fluorine-doped layer, while the fluoride hardly enters a first inner cladding which forms an optical layer, so that the powder loose body after the dehydroxylation treatment and the vitrification sintering forms the glass rod which sequentially comprises a seed rod, a core layer, the optical layer (the first inner cladding), the fluorine-doped layer (the second inner cladding and the third inner cladding from inside to outside; and finally, carrying out outer cladding deposition treatment on the glass rod to form a pure silicon dioxide outer cladding on the outer surface of the glass rod, and then carrying out dehydroxylation treatment and vitrification sintering treatment to obtain the optical fiber preform.
In the present invention, the powder density of the first inner cladding, the powder density of the second inner cladding, and the powder density of the third inner cladding may decrease in an arithmetic progression, or may decrease irregularly.
The seed rod of the present invention is not particularly limited, and a seed rod commonly used in the art may be selected, for example, the seed rod may be a graphite rod or a ceramic rod.
The present invention is not limited to the specific deposition method, and may adopt a deposition method commonly used in the art, for example, VAD (vapor axial deposition method) and/or OVD ((outer vapor deposition method) — in some embodiments, VAD may be adopted to perform deposition treatment on the seed rod, and the core layer, the first inner cladding layer, the second inner cladding layer and the third inner cladding layer are sequentially formed on the outer surface of the seed rod, or OVD may be adopted to perform deposition treatment on the glass rod, so as to obtain the optical fiber preform.
The powder density of the first inner cladding, the second inner cladding and the third inner cladding is controlled to be more than 0.21g/cm in the preparation process 2 The gradient inner cladding with low refractive index can be formed on the outer surface of the core layer, and the inner cladding with low refractive index can effectively restrict light when the optical fiber is bent, so that light leakage is avoided, and the bending loss of the optical fiber is prevented from being increased; the preparation method can also obtain the optical fiber with larger mode field diameter and larger cut-off wavelength, and the optical fiber can be well butted with the G652 optical fiber and meet the transmission requirements of various wave bands. The preparation method of the invention also has the advantages of simple process, low production cost and suitability for wide popularization and application.
It is worth mentioning that the preparation method of the invention is to directly deposit the inner cladding layer on the outer side of the core rod (the seed rod deposited with the core layer), compared with the prior art in which the inner cladding layer with the low refractive index groove is formed by fusing and shrinking on the outer side of the core rod, in the optical fiber preform rod obtained by the preparation method of the invention, the problems of size and interface between the core rod and the inner cladding layer with the low refractive index groove do not exist, which is beneficial to prolonging the service life of the optical fiber.
In some embodiments of the present invention, the first and second electrodes are,the powder density of the first inner cladding is 0.26-0.29 g/cm 2 (ii) a And/or the presence of a gas in the atmosphere,
the powder density of the second inner cladding is 0.24-0.27 g/cm 2 (ii) a And/or the presence of a gas in the atmosphere,
the powder density of the third inner cladding is 0.22-0.25 g/cm 2
In the invention, when the powder densities of the first inner cladding layer, the second inner cladding layer and the third inner cladding layer meet the ranges, the low-refractive-index inner cladding layer with gradient can be better formed on the outer surface of the core layer, and the low-refractive-index inner cladding layer with gradient can effectively restrain light when the optical fiber is bent, thereby avoiding light leakage from increasing the bending loss of the optical fiber.
In some embodiments of the invention, the core layer feedstock is deposited on an outer surface of the seed rod to form a core layer on the outer surface of the seed rod;
wherein, the core layer raw materials include: silicon tetrachloride, germanium tetrachloride, hydrogen, oxygen, and argon;
the flow rate of the silicon tetrachloride is 2-5 g/min, the flow rate of the germanium tetrachloride is 300-500 mg/min, the flow rate of the hydrogen is 7-9L/min, the flow rate of the oxygen is 10-15L/min, and the flow rate of the argon is 5-10L/min; and/or the presence of a gas in the gas,
and in the deposition process of the core layer, the temperature is 800-1000 ℃.
According to the invention, the refractive index of the core layer can be improved by adopting germanium tetrachloride, hydrogen is combustible gas, oxygen is combustion-supporting gas, and argon is inert gas. When the core layer raw material and the temperature of the core layer in the deposition process accord with the range defined by the parameters, the core layer with high refractive index can be efficiently formed on the outer surface of the seed rod under the condition of saving cost, and the transmission efficiency of the optical fiber is favorably improved.
In some embodiments of the invention, a first inner cladding raw material is deposited on the outer surface of the core layer, forming a first inner cladding on the outer surface of the core layer;
wherein, first inner cladding raw materials include: silicon tetrachloride, hydrogen, oxygen, and argon;
the flow rate of the silicon tetrachloride is 25-30 g/min, the flow rate of the hydrogen is 90-100L/min, the flow rate of the oxygen is 45-50L/min, and the flow rate of the argon is 10-20L/min; and/or the presence of a gas in the atmosphere,
and in the deposition process of the first inner cladding, the temperature is 1300-1400 ℃.
According to the invention, when the first inner cladding raw material and the temperature of the first inner cladding deposition process accord with the parameters, the first inner cladding can be efficiently formed on the outer surface of the core layer, so that the preparation efficiency of the optical fiber preform is improved.
In some embodiments of the invention, the second inner cladding raw material is deposited on the outer surface of the first inner cladding, and the second inner cladding is formed on the outer surface of the first inner cladding;
wherein, the second inner cladding raw materials include: silicon tetrachloride, hydrogen, oxygen and argon;
the flow rate of the silicon tetrachloride is 25-30 g/min, the flow rate of the hydrogen is 85-95L/min, the flow rate of the oxygen is 40-45L/min, and the flow rate of the argon is 10-20L/min; and/or the presence of a gas in the gas,
and in the deposition process of the second inner cladding, the temperature is 1250-1350 ℃.
According to the invention, when the second inner cladding raw material and the temperature of the second inner cladding deposition process accord with the parameters, the second inner cladding can be efficiently formed on the outer surface of the first inner cladding, and the preparation efficiency of the optical fiber preform is improved.
In some embodiments of the present invention, a third inner cladding raw material is deposited on the outer surface of the second inner cladding, and a third inner cladding is formed on the outer surface of the second inner cladding;
wherein, the third inner cladding raw materials include: silicon tetrachloride, hydrogen, oxygen and argon;
the flow rate of the silicon tetrachloride is 25-30 g/min, the flow rate of the hydrogen is 80-85L/min, the flow rate of the oxygen is 35-40L/min, and the flow rate of the argon is 10-20L/min; and/or the presence of a gas in the atmosphere,
according to the invention, when the third inner cladding raw material and the temperature of the third inner cladding deposition process accord with the parameters, the third inner cladding can be efficiently formed on the outer surface of the second inner cladding, and the preparation efficiency of the optical fiber preform is improved.
In the invention, as the first inner cladding raw material, the second inner cladding raw material and the third inner cladding raw material do not contain fluoride, no waste gas containing fluoride is generated in the process of forming the first inner cladding, the second inner cladding and the third inner cladding, the corrosion of the waste gas containing fluoride on preparation equipment can be avoided, and the influence on the preparation treatment capacity can be further avoided; and because the fluoride is not contained in first inner cladding raw materials, second inner cladding raw materials and third inner cladding raw materials, consequently in the deposition process of first inner cladding, second inner cladding and third inner cladding, can not permeate fluoride in to the sandwich layer, be favorable to maintaining the high refracting index of sandwich layer, and then make the optic fibre have excellent transmission performance.
In some embodiments of the invention, the powdered compact is dehydroxylated using a dehydroxylated feedstock;
the dehydroxylation raw material comprises: chlorine, helium, and fluoride;
the flow rate of chlorine is 500-1000 cc/min, the flow rate of helium is 15-25L/min, and the flow rate of fluoride is 200-500 cc/min; and/or the presence of a gas in the gas,
in the process of the dehydroxylation treatment, the temperature is 1000-1100 ℃, and the pressure is 5-10 Pa.
In the present invention, the fluoride can reduce the refractive index of the inner cladding, the fluoride is not particularly limited in the present invention, and the fluoride commonly used in the art can be selected, for example, the fluoride can include SiF 4 、CF 4 、SF 6 And C 2 F 6 At least one of (1).
According to the invention, when the dehydroxylation raw material and the temperature and pressure in the dehydroxylation treatment process meet the parameters, the moisture in the powder loose body can be efficiently removed, the subsequent vitrification sintering is facilitated, the glass rod can be efficiently obtained, and the preparation efficiency of the optical fiber preform rod is improved.
In some embodiments of the invention, the dehydroxylated powder compact is vitrified sintered using a vitrification raw material to obtain a glass rod;
the vitrification raw materials comprise: helium and fluoride;
the flow rate of helium is 15-25L/min, and the flow rate of fluoride is 100-500 cc/min; and/or the presence of a gas in the atmosphere,
in the process of vitrification sintering, the temperature is 1350-1500 ℃, and the pressure is 10-15 Pa.
According to the invention, when the vitrification raw material and the temperature and pressure in the vitrification sintering process meet the parameters, the powder loose body with moisture removed can be efficiently vitrified and sintered to form a glass rod, so that the preparation efficiency of the optical fiber preform is improved.
In the invention, because the fluoride is used in the dehydroxylation treatment and the vitrification sintering process, the fluoride can permeate into the third inner cladding and the second inner cladding in the dehydroxylation treatment and the vitrification sintering process, and the permeation amount of the fluoride in the third inner cladding and the second inner cladding is gradually reduced, so that the refractive index of the third inner cladding is favorably smaller than that of the second inner cladding, the refractive index of the second inner cladding is favorably smaller than that of the first inner cladding which is not doped with fluorine, and a gradient low-refractive-index inner cladding is favorably formed on the outer surface of the core rod.
In some embodiments of the present invention, the seed rod may be subjected to a deposition process using a deposition apparatus to form a powder porous body, and then the powder porous body may be subjected to a dehydroxylation sintering process using a sintering apparatus to obtain a glass rod.
FIG. 1 is a schematic structural view of a deposition apparatus according to some embodiments of the present invention. As shown in fig. 1, the deposition apparatus of the present invention includes a deposition chamber 2, a core layer burner 3, a first inner cladding burner 4, a second inner cladding burner 12, and a third inner cladding burner 13; wherein, the seed rod 1 is positioned inside the deposition chamber 2 and can move up and down relative to the deposition chamber 2, and the deposition chamber 2 is provided with an exhaust outlet 5; the core layer burner 3, the first inner clad burner 4, the second inner clad burner 12, and the third inner clad burner 13 are all used for the deposition process of the seed rod 1.
In a specific embodiment, the seed rod 1 may be installed inside the deposition chamber 2, the core layer raw material is introduced into the core layer burner 3, and the core layer raw material is deposited on the outer surface of the seed rod 1 by using the core layer burner 3 at a certain temperature to form a core layer; then, introducing a first inner cladding raw material into the first inner cladding burner 4, and depositing the first inner cladding raw material on the outer surface of the core layer by using the first inner cladding burner 4 at a certain temperature to form a first inner cladding; then, introducing a second inner cladding raw material into the second inner cladding burner 12, and depositing the second inner cladding raw material on the outer surface of the first inner cladding by using the second inner cladding burner 12 at a certain temperature to form a second inner cladding; finally, third inner cladding raw materials are introduced into the third inner cladding burner 13, and are deposited on the outer surface of the second inner cladding by using the third inner cladding burner 13 at a certain temperature to form a powder loose body containing the third inner cladding; wherein, in each step of deposition treatment, the seed rod 1 is moved up and down relative to the deposition chamber 2 to make each layer deposited more uniform, and the exhaust gas generated after the deposition treatment is exhausted through the exhaust outlet 5.
FIG. 2 is a schematic diagram of a sintering apparatus according to some embodiments of the present invention. As shown in fig. 2, the deposition apparatus of the present invention comprises a glass tube 7, a heating body 8, and a pressure controller 9; wherein, the powder loose body 6 is positioned inside the glass tube 7 and can move up and down relative to the glass tube 7, an air inlet 11 is arranged below the glass tube 7, and an air outlet 10 is arranged above the glass tube 7; the heating body 8 is used for heating the glass tube 7, and the pressure controller 9 is used for controlling the pressure inside the glass tube 7.
In a specific embodiment, the temperature of the heating body 8 is raised to a specific value, the powder loose body 6 is inserted into the glass tube 7, a dehydroxylation raw material is introduced into the glass tube 7 through the air inlet 11, the powder loose body 6 moves up and down to be dehydroxylated through the heating body 8, and waste gas generated by the dehydroxylation treatment is discharged through the air outlet 10; then raising the temperature of the heating body 8 to a specific value, introducing a vitrification sintering raw material into the glass tube 7 through the air inlet 11, enabling the powder loose body 6 subjected to dehydroxylation to move up and down and to be vitrified and sintered through the heating body 8 to obtain a glass rod, and discharging waste gas generated by vitrification sintering through the air outlet 10; wherein, the pressure controller 9 is used to control the pressure in the glass tube 7 during the dehydroxylation process and the vitrification sintering process.
A second aspect of the present invention provides an optical fiber preform, which is prepared according to the above method for preparing an optical fiber preform.
In some embodiments, in the optical fiber preform prepared by the above preparation method of the present invention, the length of the optical fiber preform is 1500-2000 mm, the outer diameter of the preform is 140-160 mm, the radius of the core layer of the optical fiber after drawing is 3.5-4.5 μm, the radius of the first inner cladding is 7-11.5 μm, the radius of the second inner cladding is 9-13 μm, the radius of the third inner cladding is 12.5-17.5 μm, and the outer diameter of the outer cladding is 62.5 μm; the relative refractive index Δ n1 of the core layer is 0.35% to 0.42%, the relative refractive index Δ n2 of the first inner cladding is-0.03% to-0.1%, and the relative refractive index Δ n3 of the fluorine-doped layer (the second inner cladding and the third inner cladding) is-0.15% to-0.30%, where the relative refractive index Δ n1 is 0.35% to 0.42%, and the relative refractive index Δ n3 of the fluorine-doped layer is-0.15% to-0.30% i =n i -n 0 ,n i For the corresponding refractive index of each layer, n 0 Refractive index of pure silica glass.
The optical fiber preform is prepared according to the preparation method of the optical fiber preform, can be used for preparing optical fibers which have excellent bending resistance and service life, can be well butted with G652 optical fibers and meet the transmission requirements of various wave bands, and is simple in preparation process and low in production cost.
A third aspect of the present invention provides an optical fiber obtained by drawing the above optical fiber preform.
In the invention, the optical fiber perform is stretched to a target size, and the optical fiber is obtained.
In some embodiments, the performance index of the optical fiber obtained after drawing the optical fiber preform is: attenuation at the wavelength of 1310nm is lower than 0.335dB/km, attenuation at the wavelength of 1383nm is lower than 0.285dB/km, attenuation at the wavelength of 1550nm is lower than 0.185dB/km, the cable wavelength is less than 1260nm, zero dispersion wavelength is 1305-1324 nm, and Mode Field Diameter (MFD) is 8.45-9.0 um. Therefore, the optical fiber provided by the invention has excellent bending resistance and long service life, can be well butted with a G652 optical fiber, meets the transmission requirements of various wavebands, and has the advantages of simple preparation process and low production cost.
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto.
Example 1
The preparation method of the optical fiber of the embodiment comprises the following steps:
1) performing deposition treatment on the seed rod by using deposition equipment shown in fig. 1, and sequentially forming a core layer, a first inner cladding layer, a second inner cladding layer and a third inner cladding layer on the outer surface of the seed rod to obtain a powder loose body;
wherein, in the deposition process of the core layer, the temperature is 850 ℃, and the core layer comprises the following raw materials: the flow rate of the silicon tetrachloride is 4g/min, the flow rate of the germanium tetrachloride is 330mg/min, the flow rate of the hydrogen is 8.5L/min, the flow rate of the oxygen is 15L/min, and the flow rate of the argon is 8L/min;
in the deposition process of the first inner cladding, the temperature is 1400 ℃, and the raw materials of the first inner cladding comprise: the flow rate of the silicon tetrachloride is 25g/min, the flow rate of the hydrogen is 100L/min, the flow rate of the oxygen is 50L/min, and the flow rate of the argon is 15L/min;
in the deposition process of the second inner cladding, the temperature is 1300 ℃, and the raw materials of the first inner cladding comprise: the flow rate of the silicon tetrachloride is 25g/min, the flow rate of the hydrogen is 90L/min, the flow rate of the oxygen is 45L/min, and the flow rate of the argon is 15L/min;
in the deposition process of the third inner cladding, the temperature is 1250 ℃, and the raw materials of the first inner cladding comprise: the flow rate of the silicon tetrachloride is 25g/min, the flow rate of the hydrogen is 80L/min, the flow rate of the oxygen is 40L/min, and the flow rate of the argon is 15L/min.
2) Carrying out dehydroxylation treatment and vitrification sintering on the powder loose body by using sintering equipment shown in FIG. 2 to obtain a glass rod;
wherein, in the dehydroxylation process, the temperature is 1100 ℃, the pressure is 10Pa, and the dehydroxylation raw materials comprise:chlorine, helium and SiF 4
The flow rate of chlorine gas is 500cc/min, the flow rate of helium gas is 20L/min, SiF 4 The flow rate of (2) is 500 cc/min;
in the process of vitrification sintering, the temperature is 1450 ℃, the pressure is 15Pa, and vitrification raw materials comprise: helium and SiF 4 (ii) a Helium flow rate of 20L/min, SiF 4 The flow rate of (2) was 500 cc/min.
3) Extending the glass rod to enable the outer diameter of the glass rod to be 40-50 mm, confirming the refractive index profile structure of the glass rod through a PK2600 test, and designing the outer cladding dimension;
4) according to the size of the outer cladding, depositing silicon dioxide powder on the outer surface of the extended glass rod to form the outer cladding, and then carrying out dehydroxylation vitrification on the glass rod provided with the outer cladding to obtain an optical fiber preform;
wherein, the length of the optical fiber prefabricated rod is 1500mm, and the outer diameter is 150 mm;
5) and carrying out wire drawing treatment on the optical fiber preform to obtain the optical fiber.
Example 2
The optical fiber of this example was prepared in substantially the same manner as in example 1, except that:
in the step 1), in the deposition process of the core layer, the flow rate of silicon tetrachloride is 4.1g/min, and the flow rate of germanium tetrachloride is 340 mg/min;
and in the deposition process of the third inner cladding, the flow of the silicon tetrachloride is 28 g/min.
In the step 2), the temperature is 1050 ℃ and the pressure is 8Pa during the dehydroxylation treatment process, and SiF 4 The flow rate of (2) is 300 cc/min;
in the process of vitrification sintering, the temperature is 1400 ℃, the pressure is 12Pa, SiF 4 The flow rate of (2) was 400 cc/min.
Example 3
The optical fiber of this example was prepared in substantially the same manner as in example 1, except that:
in the step 1), in the deposition process of the core layer, the flow rate of silicon tetrachloride is 4.5g/min, the flow rate of germanium tetrachloride is 380mg/min, the flow rate of hydrogen is 8.8L/min, and the flow rate of oxygen is 16L/min;
in the deposition process of the second inner cladding, the flow rate of the silicon tetrachloride is 28g/min, and the flow rate of the hydrogen is 92L/min;
in the deposition process of the third inner cladding, the flow of the silicon tetrachloride is 30g/min, and the flow of the hydrogen is 82L/min.
In the step 2), the temperature is 1010 ℃, the pressure is 5Pa and SiF is adopted in the process of dehydroxylation treatment 4 The flow rate of (2) is 200 cc/min;
in the process of vitrification sintering, the temperature is 1350 ℃, the pressure is 10Pa, and SiF 4 The flow rate of (2) is 250 cc/min.
Comparative example 1
The method for producing the optical fiber of the present comparative example includes the steps of:
1) depositing the raw material of the core layer on the outer surface of the seed rod by VAD (vapor deposition) method, and forming the core layer and a first cladding layer on the outer surface of the seed rod to obtain the core rod;
wherein, in the deposition process of the core layer, the temperature is 850 ℃, and the core layer comprises the following raw materials: the flow rate of the silicon tetrachloride is 3.5g/min, the flow rate of the germanium tetrachloride is 350mg/min, the flow rate of the hydrogen is 7.5L/min, the flow rate of the oxygen is 15L/min, and the flow rate of the argon is 8L/min;
during the deposition of the first cladding, the temperature was 1300 ℃, and the cladding raw materials included: the flow rate of the silicon tetrachloride is 25g/min, the flow rate of the silicon tetrafluoride is 500cc/min, the flow rate of the hydrogen is 70L/min, the flow rate of the oxygen is 30L/min, and the flow rate of the argon is 15L/min.
2) Setting OVD deposition size according to the size of a required fluorine-doped quartz sleeve to obtain a fluorine-doped loose body, then introducing 300-1000 cc/min silicon tetrafluoride according to the requirement of a delta n3 refractive index in dehydroxylation and vitrification to obtain a corresponding fluorine-doped quartz glass rod, and carrying out hole drilling, honing and polishing treatment on the fluorine-doped quartz glass rod to form a transparent fluorine-doped quartz sleeve;
respectively processing and extending the core rod obtained in the step 1) and the fluorine-doped quartz sleeve obtained in the step 2) to a certain size, then carrying out corrosion pickling, and then carrying out fusion shrinkage treatment to obtain a fusion rod;
the melting and shrinking process is to burn the fluorine-doped quartz sleeve and the core rod by oxyhydrogen and to melt and shrink the fluorine-doped quartz sleeve and the core rod on the core rod; and (3) a melting and shrinking process: and plugging the core rod into the fluorine-doped quartz sleeve, vacuumizing one side of the fluorine-doped quartz sleeve, burning the fluorine-doped quartz sleeve from the other side by flame of a spray gun, so that the fluorine-doped quartz sleeve is fused on the core rod, the hydrogen flow is 150L/min, the oxygen flow is 300L/min, and the moving speed of the spray gun is 5-15 mm/min.
4) Extending the melt-down rod to enable the outer diameter of the melt-down rod to be 30-50 mm, confirming the refractive index profile structure of the melt-down rod through a PK2600 test, and designing the outer cladding dimension;
5) according to the size of the outer cladding, depositing silicon dioxide powder on the outer surface of the extended fused rod to form the outer cladding, and then carrying out dehydroxylation vitrification on the fused rod provided with the outer cladding to obtain an optical fiber preform;
wherein, the length of the optical fiber prefabricated rod is 1500mm, and the outer diameter is 150 mm;
6) and carrying out wire drawing treatment on the optical fiber preform to obtain the optical fiber.
Performance testing
1. Powder density of the powder bulk layers
The powder densities ρ of the powder bulk inner claddings (including the first inner cladding, the second inner cladding, and the third inner cladding) of examples 1-3 were tested separately (including the powder density ρ 1 of the first inner cladding, the powder density ρ 2 of the second inner cladding, and the powder density ρ 3 of the third inner cladding), and the results of the tests are shown in table 1,
the powder density is calculated from the weight of the raw material deposited for each layer and the volume of each layer.
2. Relative refractive index and outer diameter of each layer of optical fiber
The optical fibers of examples 1 to 3 and comparative example were tested for the outer diameter Ra of the core layer, the outer diameter Rb of the optical layer (first inner cladding), and the outer diameter Rc of the fluorine-doped layer (second inner cladding and third inner cladding), respectively, and the relative refractive index Deltan of the core layer of the optical fibers 1 Relative refractive index of optical layer (first inner cladding) delta n 2 And the relative refractive index delta n of the fluorine-doped layer (the second inner cladding and the third inner cladding) 3 Test resultsAs shown in the table 2, see,
the refractive index profile was obtained by testing using a PK2600 test meter and then calculated to obtain the dimensions and refractive index of each layer.
3. Transmission performance
The signal attenuation of the optical fibers in the test examples 1-3 and the comparative example at different wavelengths is shown in the table 3, and the test method refers to the attenuation coefficient of the transmission performance measurement method in GB/T15972.40-2008.
4. Cable wavelength and mode field diameter
The cable wavelengths and mode field diameters of the optical fibers of examples 1 to 3 and comparative example were measured, respectively, and the results are shown in Table 3, with reference to the cut-off wavelength of the transmission performance measuring method in GB/T15972.44-2017 and the mode field diameter in GB/T15972.45-2008
5. Bending loss
The optical fibers of examples 1 to 3 and comparative example were wound ten turns with a winding diameter of 15mm, and the macrobending of the optical fibers was tested, the test results are shown in table 3, and the test method refers to the macrobending loss of the transmission performance measurement method of GB/T15972.47-2008.
TABLE 1
Figure BDA0003746236590000151
TABLE 2
Δn 1 /% Ra/μm Δn 2 /% Rb/μm Δn 3 /% Rc/μm
Comparative example 1 0.370 3.9 0 7.5 -0.30 13.0
Example 1 0.355 4.0 -0.07 8.0 -0.25 16.4
Example 2 0.380 4.1 -0.06 9.0 -0.20 16.8
Example 3 0.430 4.2 -0.04 11.0 -0.18 17.2
As can be seen from table 2, the method for preparing an optical fiber preform according to the embodiment of the present invention can form a gradient-decreasing low refractive index inner cladding layer on the outer side of the core layer.
TABLE 3
Figure BDA0003746236590000161
As can be seen from table 3, the optical fiber prepared in the embodiment of the present invention has excellent bending resistance, transmission performance and service life, and can realize good butt joint with the G652 optical fiber and meet transmission requirements of various wave bands, and the optical fiber has a simple preparation process and low production cost.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. A method for preparing an optical fiber preform, comprising the steps of:
carrying out deposition treatment on the seed rod, and sequentially forming a core layer, a first inner cladding layer, a second inner cladding layer and a third inner cladding layer on the outer surface of the seed rod to obtain a powder loose body;
sequentially carrying out dehydroxylation treatment and vitrification sintering on the powder loose body to obtain a glass rod;
carrying out deposition treatment on the glass rod to obtain the optical fiber perform rod;
wherein the powder density of the first inner cladding, the powder density of the second inner cladding and the powder density of the third inner cladding are sequentially reduced;
the powder density of the first inner cladding, the powder density of the second inner cladding and the powder density of the third inner cladding are all more than 0.21g/cm 2
2. The method for preparing an optical fiber preform according to claim 1, wherein the first inner cladding has a soot density of 0.26 to 0.29g/cm 2 (ii) a And/or the presence of a gas in the atmosphere,
the powder density of the second inner cladding is 0.24-0.27 g/cm 2 (ii) a And/or the presence of a gas in the atmosphere,
the powder density of the third inner cladding is 0.22-0.25 g/cm 2
3. The method for preparing an optical fiber preform according to claim 1 or 2, wherein a core layer raw material is deposited on an outer surface of the seed rod, and the core layer is formed on the outer surface of the seed rod;
wherein, the core layer raw materials include: silicon tetrachloride, germanium tetrachloride, hydrogen, oxygen, and argon;
the flow of the silicon tetrachloride is 2-5 g/min, the flow of the germanium tetrachloride is 300-500 mg/min, the flow of the hydrogen is 7-9L/min, the flow of the oxygen is 10-15L/min, and the flow of the argon is 5-10L/min; and/or the presence of a gas in the gas,
and in the deposition process of the core layer, the temperature is 800-1000 ℃.
4. A method for preparing an optical fiber preform according to any of claims 1-3, wherein a first inner cladding raw material is deposited on the outer surface of the core layer to form the first inner cladding layer on the outer surface of the core layer;
wherein, the first inner cladding raw material comprises: silicon tetrachloride, hydrogen, oxygen and argon;
the flow rate of the silicon tetrachloride is 25-30 g/min, the flow rate of the hydrogen is 90-100L/min, the flow rate of the oxygen is 45-50L/min, and the flow rate of the argon is 10-20L/min; and/or the presence of a gas in the gas,
and in the deposition process of the first inner cladding, the temperature is 1300-1400 ℃.
5. The method for preparing an optical fiber preform according to any of claims 1-4, wherein a second inner cladding raw material is deposited on the outer surface of the first inner cladding, and the second inner cladding is formed on the outer surface of the first inner cladding;
wherein, the second inner cladding raw material comprises: silicon tetrachloride, hydrogen, oxygen and argon;
the flow rate of the silicon tetrachloride is 25-30 g/min, the flow rate of the hydrogen is 85-95L/min, the flow rate of the oxygen is 40-45L/min, and the flow rate of the argon is 10-20L/min; and/or the presence of a gas in the gas,
and in the deposition process of the second inner cladding, the temperature is 1250-1350 ℃.
6. A method for preparing an optical fiber preform according to any of claims 1-5, wherein a third inner cladding raw material is deposited on the outer surface of the second inner cladding, and the third inner cladding is formed on the outer surface of the second inner cladding;
wherein, the third inner cladding raw material comprises: silicon tetrachloride, hydrogen, oxygen and argon;
the flow rate of the silicon tetrachloride is 25-30 g/min, the flow rate of the hydrogen is 80-85L/min, the flow rate of the oxygen is 35-40L/min, and the flow rate of the argon is 10-20L/min; and/or the presence of a gas in the gas,
and in the deposition process of the third inner cladding, the temperature is 1250-1350 ℃.
7. The method for fabricating an optical fiber preform according to any one of claims 1 to 6, wherein the soot body is dehydroxylated using a dehydroxylated feedstock;
the dehydroxylation raw material comprises: chlorine, helium, and fluoride;
the flow rate of the chlorine is 500-1000 cc/min, the flow rate of the helium is 15-25L/min, and the flow rate of the fluoride is 200-500 cc/min; and/or the presence of a gas in the gas,
in the de-hydroxylation treatment process, the temperature is 1000-1100 ℃, and the pressure is 5-10 Pa.
8. The method for preparing an optical fiber preform according to any of claims 1 to 7, wherein the soot body subjected to the dehydroxylation treatment is subjected to the vitrification sintering using a vitrification raw material to obtain the glass rod;
the vitrification raw material comprises: helium and fluoride;
the flow rate of helium is 15-25L/min, and the flow rate of fluoride is 100-500 cc/min; and/or the presence of a gas in the gas,
in the process of vitrification sintering, the temperature is 1350-1500 ℃, and the pressure is 10-15 Pa.
9. An optical fiber preform, characterized in that it is produced according to the method for producing an optical fiber preform according to any one of claims 1 to 8.
10. An optical fiber obtained by drawing the optical fiber preform of claim 9.
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