CN108002698B - Method for manufacturing optical fiber preform - Google Patents
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- CN108002698B CN108002698B CN201711226949.3A CN201711226949A CN108002698B CN 108002698 B CN108002698 B CN 108002698B CN 201711226949 A CN201711226949 A CN 201711226949A CN 108002698 B CN108002698 B CN 108002698B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture 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]
- C03B37/018—Manufacture 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] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
- C03B37/01807—Reactant delivery systems, e.g. reactant deposition burners
- C03B37/01815—Reactant deposition burners or deposition heating means
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Abstract
The invention discloses a method for manufacturing an optical fiber preform rod, which mainly comprises the steps of depositing an optical fiber preform rod intermediate, doping alkali metal elements and forming a rod, and is characterized in that when the alkali metal elements are doped in the optical fiber preform rod intermediate by adopting a diffusion method, all parts of the optical fiber preform rod intermediate are kept at the temperature of 500 ℃ and 1000 ℃, and the diffusion time is 5-300 minutes. Compared with the prior art, the method has the advantages that the alkali metal is doped in the lower temperature range of 500-1000 ℃, the crystallization temperature of the quartz glass can be effectively avoided, and the risk of crystallization is reduced, so that the scrappage caused by overhigh attenuation caused by crystallization is reduced; moreover, the material is diffused in an environment with uniform temperature, so that the crystallization caused by temperature rise and fall circulation can be avoided; in addition, the distribution of the alkali metal content can be optimized, compared with the diffusion at the temperature of 1800-2200 ℃ in the prior art, the diffusion of the alkali metal can be more intensively distributed in the core layer of the optical fiber preform, the diffusion to the cladding is reduced, the concentration of the core layer is improved, and the attenuation of the optical fiber is reduced.
Description
Technical Field
The invention relates to the technical field of optical fiber communication, in particular to a manufacturing method of an optical fiber preform.
Background
Optical communication has the characteristics of large transmission capacity, long transmission distance, high transmission speed and the like, and is widely applied to optical communication systems such as long-distance trunk lines, metropolitan area networks, access networks and the like. In recent years, with the explosive growth of IP traffic, communication networks are advancing to next-generation systems, and building an optical fiber infrastructure with a huge transmission capacity is the foundation of next-generation networks.
The attenuation coefficient of the optical fiber is one of the most important performance index indexes of the optical fiber, the relay distance of optical fiber communication is determined to a great extent, the smaller the attenuation coefficient of the optical fiber is, the longer the transmission distance of the optical signal carried by the optical fiber is, and the smaller the attenuation amplitude of the optical signal carried by the optical fiber is under the same transmission distance, so that the optical signal to noise ratio OSNR in the optical fiber communication can be effectively improved by reducing the attenuation coefficient, and the transmission distance of a system are further improved. In long-distance optical fiber communication, optical signals are transmitted through the relay station, and if the attenuation coefficient of the optical fiber is smaller, the distance between the relay stations can be farther, so that the number of the relay stations is greatly reduced, and the operation cost is greatly reduced. Therefore, in the manufacture of optical fiber, it is difficult and hot to reduce the attenuation coefficient of the optical fiber.
The existing technology for reducing the attenuation coefficient mainly comprises the following steps: 1. viscosity matching and coefficient of thermal expansion matching. The optical fiber profile design and material components are optimized, the viscosity matching and the thermal expansion coefficient of a core layer and a cladding layer of the optical fiber are improved, and the optical fiber attenuation caused by drawing stress can be reduced. 2. Reducing the concentration of the core dopant and increasing the concentration of the core dopants Ge and F will increase the rayleigh scattering loss caused by the concentration fluctuation factor, for example, the pure silicon core technology is currently commonly used to manufacture ultra-low attenuation optical fibers. 3. Alkali metal, alkaline earth metal or chlorine element are doped, and the temperature and the virtual temperature of the glass can be reduced by the alkali metal, the alkaline earth metal or the chlorine element, so that the adjustment of a glass network structure is facilitated, and the Rayleigh scattering loss caused by density fluctuation factors is reduced.
In CN 102627398A, CN102627400A, CN106458696, a glass tube is heated to 1500-. The heat source moving speed is 30mm/min-100mm/min, the reciprocating movement times are 15-30 times, and the doping time is at least 5 hours if the length of the liner tube is 1 m. The obvious disadvantages of the method are high required temperature, long diffusion time, low production efficiency and no contribution to large-scale production; in addition, the movement of the heating furnace causes the temperature of the liner tube to circularly rise and fall, so that the crystallization is easier, and the longitudinal distribution of alkali metal is also easier to cause uneven.
In patent CN106458696A, the core layer of the optical fiber preform is divided into three parts, each part is doped independently, so as to realize the doping of alkali metal elements, the process can prepare an optical fiber with very low attenuation, but each core part in the process needs to be subjected to deposition, collapsing and burning, the outer diameter is reduced, and the whole preparation process flow is complex and not beneficial to large-scale production.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for manufacturing an ultra-low attenuation optical fiber preform aiming at the defects in the prior art, effectively avoid the crystallization temperature of quartz glass, and reduce the risk of crystallization, thereby reducing the scrap caused by overhigh attenuation caused by crystallization.
The technical scheme adopted by the invention for solving the problems is as follows:
a method for manufacturing an ultra-low attenuation optical fiber preform rod comprises the steps of depositing an optical fiber preform rod intermediate body, doping alkali metal elements, melting and shrinking and the like, and is characterized in that when the alkali metal elements are doped in the optical fiber preform rod intermediate body by adopting a diffusion method, all parts of the optical fiber preform rod intermediate body are kept at the temperature of 500-1000 ℃ for diffusion, and the diffusion time is 5-300 minutes, preferably 30-150 minutes.
The invention provides a method for manufacturing an ultralow attenuation optical fiber preform, which comprises the following steps:
s1: depositing an optical fiber preform intermediate: depositing a core layer and a part of the core layer required by the optical fiber to form an intermediate body of the optical fiber preform by using a chemical vapor deposition process (PCVD or MCVD) in a tube;
s2: intermediate doped alkali metal compound: putting the intermediate of the optical fiber preform into a heat preserving furnace, heating the alkali metal source compound to provide continuous alkali metal source steam, maintaining each part of the intermediate of the optical fiber preform at 500-1000 ℃ for diffusion doping with alkali metal, wherein the diffusion time is 5-300 minutes, and then forming a rod to obtain the optical fiber preform with the central part containing alkali metal elements.
In the manufacturing method of the optical fiber preform, the alkali metal element in the core layer of the optical fiber preform is introduced by a diffusion method, ions and partial gas molecules can be diffused and enter due to the special network structure of the silicon dioxide, and the diffusion rate is increased under higher temperature and pressure difference. Alkali metal ions can enter a network structure of silicon dioxide, so that structural adjustment is facilitated, and the viscosity is reduced. However, the addition of the alkali metal element promotes the generation of crystals in the intermediate of the optical fiber preform, and a temperature at which the crystallization is easily carried out is avoided in order to prevent the crystallization. Therefore, the diffusion temperature is set to be 500-1000 ℃ in the low-temperature range, the alkali metal source compound can not only be normally diffused, but also can avoid the crystallization temperature, and the risk of crystallization is reduced, so that the overhigh attenuation caused by crystallization is reduced. Besides, the diffusion is carried out at the low temperature range of 500-1000 ℃, the diffusion rate is slower, the accumulation of alkali metal elements on the inner surface is facilitated, the diffusion into the inner cladding is avoided, and the Rayleigh scattering coefficient of the core layer is reduced, so that the attenuation is reduced.
In the method for manufacturing the optical fiber preform, preferably, the holding furnace is heated to the required diffusion temperature and then placed into the intermediate of the optical fiber preform for diffusion, so that the cyclic replacement of temperature rise and fall of the intermediate of the optical fiber preform in the diffusion process is reduced, and the formation of crystals in the heating and cooling processes is reduced.
In the above method for manufacturing an optical fiber preform, the alkali metal source compound is heated by an external heat source to generate a vapor, and the carrier gas may be O under the action of the carrier gas2，N2And the flow rate of the carrier gas is 1-10SLM, and the carrier gas is diffused outwards from the inner surface of the intermediate body of the optical fiber preform rod through the diffusion furnace region.
In the above-described method for producing an optical fiber preform, the amount of the alkali metal element entering the diffusion region can also be adjusted by changing the temperature of the vapor of the alkali metal source compound, the source gas temperature supplied by the alkali metal vapor source being 200-1500 ℃.
According to the scheme, the alkali metal source compound is an alkali metal halide, and the halogen comprises F, Cl, Br, I and At. The alkali metal halide is any combination of the two, for example: NaF, NaCl, NaBr, KCl, KBr, etc., but are not limited to these five.
According to the above scheme, the alkali metal source compound may also be other compounds, such as NaCO3、KNO3And the like.
According to the above aspect, the alkali metal source compound preferably has a purity of 99.9% or more, and is preferably in the form of a powder.
In the above method for producing an optical fiber preform, the alkali metal element is diffused so that the solid core rod contains the alkali metal element in an average concentration of 0.2ppm or more in the core layer. The alkali metal element is preferably sodium, potassium or the like.
According to the scheme, the alkali metal in the core layer of the optical fiber preform is one or a mixture of more than one of Li, Na, K, Rb and Cs.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with the prior art, the method has the advantages that the alkali metal is doped in the lower temperature range of 500-1000 ℃, the crystallization temperature of the quartz glass can be effectively avoided, and the risk of crystallization is reduced, so that the scrappage caused by overhigh attenuation caused by crystallization is reduced; in addition, in the environment diffusion with uniform temperature, the circulation of temperature rise and fall can be avoided, and the risk of crystallization is also avoided.
2. The diffusion doping of alkali metal in the heat preservation furnace can optimize the distribution of the alkali metal content, and the low-temperature diffusion speed at 500-.
3. According to the invention, alkali metal is doped in the heat preservation furnace in a diffusion mode, so that the diffusion time can be greatly shortened, the heating and heat preservation furnace can heat the effective deposition area of the whole glass liner tube and dope the area simultaneously, and the doping time is greatly saved; compared with the diffusion of a moving heating furnace, the time can be greatly shortened to 1/2 or less, and the advantage is more obvious in the diffusion of the intermediate with longer and thicker deposition area.
Description of the drawings:
fig. 1 is a schematic structural view of a heating and holding furnace according to an embodiment of the present invention. 1 is an air inlet pipe, 2 is alkali metal source heating equipment, 3 is an alkali metal source, 4 is a heating insulation box, 5 is a heat insulation baffle, 6 is a deposited glass liner pipe, 7 is a sealing chuck, and 8 is an air outlet pipe.
FIG. 2 is a graph showing the distribution of the alkali metal content in the optical fibers obtained in comparative example 1 and example 2.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the content of the present invention, but the present invention is not limited to the following examples.
The following are definitions and descriptions of some of the attributes involved in the present invention:
ppm: parts per million by weight, the value of weight% (wt%) multiplied by a factor of 10000 can be converted to ppm.
From the most central axis of the fiber, the layer defined as the layer closest to the axis is the core layer and the outermost layer of the fiber, i.e., the pure silica layer, is defined as the fiber outer cladding layer, depending on the change in refractive index.
An optical fiber preform comprising a core layer having a higher refractive index and a clad layer having a lower refractive index, the core layer of the optical fiber preform containing an alkali metal element, and the clad layer portion comprising an appropriate amount of fluorine and being free of the alkali metal element. And carrying out high-temperature wire drawing on the optical fiber preform to obtain the optical fiber with lower attenuation, wherein the optical fiber comprises a glass part and a polymer coating part.
In the invention, the step of doping the intermediate of the optical fiber preform with the alkali metal compound adopts the following devices: including heating insulation can 4, the vertical both ends of heating insulation can 4 run through to dispose thermal-insulated end plate 5, correspond respectively at the vertical both ends of heating insulation can 4 and set up the sealing joint 7 that links to each other with optical fiber perform's midbody both ends are sealed, the sealing joint of one end is connected with intake pipe 1, the sealing joint 7 of the other end is connected with outlet duct 8. The air inlet pipe 1 is connected with an air tank, the air is one or more of inert gas, oxygen, freon, compressed gas and other auxiliary gases, and is used for constantly keeping stable positive pressure of the whole air supply source, and the pressure value range is 10-10000Pa, preferably 10-2000 Pa. The powdery alkali metal source compound 3 is placed in a glass tube at the front end of an intermediate body of the optical fiber preform rod, the alkali metal source compound 3 is heated and volatilized by adopting a heating device 2, and the volatilized alkali metal source compound steam enters the intermediate body of the optical fiber preform rod along with carrier gas and enters a core layer structure through deposition or diffusion.
Example 1
A method for manufacturing an optical fiber preform specifically comprises the following steps:
s1: depositing an optical fiber preform intermediate: depositing a core layer, an inner cladding and a sunken cladding required by the optical fiber on the silica glass liner tube by using a plasma chemical vapor deposition Process (PCVD) to form an intermediate of an optical fiber preform; the middle core layer part is a silicon dioxide layer, the inner cladding part is doped with 0.9% of fluorine, and the depressed cladding part contains 1.5% of fluorine;
s2: intermediate doped alkali metal compound: placing the intermediate of the optical fiber preform into a heat preservation furnace, connecting two ends with sealing joints of an air inlet and an air outlet respectively, selecting KBr with the purity of 99.99% as an alkali metal source compound, and taking N as a carrier gas2And (3) heating at 800 ℃ to provide continuous alkali metal source steam at the flow rate of 5SLM, maintaining each part of the intermediate of the preform at 700 ℃ for diffusion for 40 minutes, and forming the preform to obtain the optical fiber preform with the central part containing the alkali metal element.
The optical fiber preform is drawn to obtain the optical fiber with ultralow attenuation, the relative refractive index of an optical fiber core layer is about 0, and the radius of the optical fiber core layer is 5.5 mu m.
Example 2
A method for manufacturing an optical fiber preform specifically comprises the following steps:
s1: depositing an optical fiber preform intermediate: depositing a core layer, an inner cladding layer and a sunken cladding layer required by the optical fiber on the silica glass liner tube by using a plasma chemical vapor deposition Process (PCVD) to form an intermediate body of the optical fiber preform, which is the same as the embodiment 1;
s2: intermediate doped alkali metal compound: placing the intermediate of the optical fiber preform into a heat preservation furnace, connecting two ends with sealing joints of an air inlet and an air outlet respectively, selecting KBr with the purity of 99.99% as an alkali metal source compound, and taking O as a carrier gas2And the flow rate is 3SLM, continuous alkali metal source steam is provided under the heating of 800 ℃, all parts of the intermediate of the prefabricated rod are kept at 900 ℃ for diffusion for 60 minutes, and then the prefabricated rod is formed, so that the optical fiber prefabricated rod with the central part containing alkali metal elements is obtained.
The optical fiber preform is drawn to obtain the optical fiber with ultralow attenuation, the relative refractive index of an optical fiber core layer is about-0.10%, and the radius of the optical fiber core layer is 5.5 mu m.
Example 3
A method for manufacturing an optical fiber preform specifically comprises the following steps:
s1: depositing an optical fiber preform intermediate: depositing a core layer, an inner cladding layer and a sunken cladding layer required by the optical fiber on the silica glass liner tube by using a plasma chemical vapor deposition Process (PCVD) to form an intermediate body of the optical fiber preform, which is the same as the embodiment 1;
s2: intermediate doped alkali metal compound: placing the intermediate of the optical fiber preform into a heat preservation furnace, connecting two ends with sealing joints of an air inlet and an air outlet respectively, selecting KBr with the purity of 99.99% as an alkali metal source compound, and taking N as a carrier gas2And heating at 800 ℃ to provide continuous alkali metal source steam at the flow rate of 1SLM, maintaining each part of the intermediate of the preform to diffuse at 1000 ℃ for 40 minutes, and forming the preform to obtain the optical fiber preform with the central part containing the alkali metal element.
The optical fiber preform is drawn to obtain the optical fiber with ultralow attenuation, the relative refractive index of an optical fiber core layer is about 0.1%, and the radius of the optical fiber core layer is 5.5 mu m.
Comparative example 1
This comparative example differs from example 2 in that: each part of the intermediate of the prefabricated rod is kept at 1800 ℃ for diffusion, and the diffusion time is 60 minutes; the remaining steps were the same as in example 2.
Comparative example 2
This comparative example differs from example 2 in that: each part of the intermediate of the prefabricated rod is kept to be diffused at 2000 ℃, and the diffusion time is 60 minutes; the remaining steps were the same as in example 2.
TABLE 1 alkali metal doping Process parameters and resulting fiber test results
The optical fiber preform prepared by the embodiment has no bubbles caused by crystallization and no scrapped product caused by excessive attenuation due to crystallization, and shows that the diffusion temperature is low, so that the crystallization temperature of quartz glass can be effectively avoided, and the risk of crystallization is reduced.
As can be seen from Table 1: although the diffusion temperature of the doped alkali metal is reduced, the alkali metal halide can still be diffused into a human glass network structure, so that the Rayleigh scattering is reduced, and the attenuation of the optical fiber is reduced; compared with the comparative examples 1 and 2, under the same other conditions and different doping temperatures (namely diffusion temperatures), the peak content of alkali metal diffused at the core layer of the optical fiber at low temperature is lower, but the attenuation is close to or lower than that of the diffusion at high temperature, because the alkali metal element is diffused into the cladding at high temperature and is combined with F in the cladding, the Rayleigh scattering coefficient of the inner cladding is improved, and the integral attenuation is influenced; moreover, the diffusion time of doping in the diffusion furnace is greatly shortened, and the overall production efficiency is improved.
As can be seen from fig. 2, when example 2 is compared with comparative example 1, it is found that: the diffusion temperature of the doped alkali metal of the comparative example is higher, the peak concentration of the alkali metal element of the optical fiber core layer is slightly higher, the diffusion distance is far, and partial alkali metal element enters the cladding; when the diffusion temperature of the doped alkali metal is lower, the alkali metal elements of the optical fiber core layer can be better concentrated in the core layer, the diffusion to the cladding is reduced, the core cladding viscosity matching can be effectively improved, and the attenuation is reduced.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, many modifications and changes can be made without departing from the inventive concept of the present invention, and these modifications and changes are within the protection scope of the present invention.
Claims (8)
1. A method for manufacturing optical fiber prefabricated rod includes such steps as depositing the intermediate of optical fiber prefabricated rod, doping alkali metal element, and forming rod, and features that when the alkali metal element is doped in the intermediate of optical fiber prefabricated rod by diffusion method, the temp of each part of intermediate of optical fiber prefabricated rod is maintained at 900 deg.C, and the diffusion time is 30-150 min.
2. A method for fabricating an optical fiber preform according to claim 1, characterized by the specific steps of:
s1: depositing an optical fiber preform intermediate: depositing a core layer and a part of the core layer required by the optical fiber to form an intermediate of the optical fiber preform by using an in-tube chemical vapor deposition process;
s2: intermediate doped alkali metal compound: putting the intermediate of the optical fiber preform into a heat preservation furnace, heating the alkali metal source compound to provide continuous alkali metal source steam, maintaining each part of the intermediate of the optical fiber preform to diffuse at the temperature of 700-900 ℃, wherein the diffusion time is 30-150 minutes, and then forming a rod to obtain the optical fiber preform with the central part containing the alkali metal element.
3. A method for fabricating an optical fiber preform according to claim 2, wherein the alkali metal source compound is heated by an external heat source to generate a vapor, and the vapor is diffused outwardly from the inner surface of the intermediate body of the optical fiber preform through the diffusion furnace region by a carrier gas having a flow rate of 1 to 10 SLM.
4. The method of claim 2, wherein the source gas temperature provided by the source of alkali metal vapor is 200-1500 ℃.
5. A method for fabricating an optical fiber preform according to claim 2, wherein the alkali metal source compound is an alkali metal halide.
6. A method for fabricating an optical fiber preform according to claim 2, wherein the purity of the alkali metal source compound is 99.9% or more.
7. A method for fabricating an optical fiber preform according to claim 2, wherein the core layer of the optical fiber preform contains alkali metal elements at an average concentration of 0.2ppm or more.
8. A method for fabricating an optical fiber preform according to claim 2, wherein the preform is drawn to obtain an optical fiber having a core layer containing an alkali metal element at an average concentration of 0.2ppm or more.
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| CN109231811A (en) * | 2018-11-16 | 2019-01-18 | 长飞光纤光缆股份有限公司 | A kind of preform implantation equipment |
| CN109133608B (en) * | 2018-11-16 | 2022-02-01 | 长飞光纤光缆股份有限公司 | Doping equipment for optical fiber preform |
| CN111847867B (en) * | 2020-07-21 | 2022-06-14 | 复旦大学 | Optical fiber preform and preparation method thereof |
| CN114075037B (en) * | 2020-08-21 | 2023-10-03 | 中天科技精密材料有限公司 | Alkali metal doped optical fiber and preparation method thereof |
| CN113200675A (en) * | 2021-04-13 | 2021-08-03 | 江苏永鼎股份有限公司 | Method for doping alkali metal and optical fiber preform |
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