CN113200675A - Method for doping alkali metal and optical fiber preform - Google Patents

Method for doping alkali metal and optical fiber preform Download PDF

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Publication number
CN113200675A
CN113200675A CN202110393662.XA CN202110393662A CN113200675A CN 113200675 A CN113200675 A CN 113200675A CN 202110393662 A CN202110393662 A CN 202110393662A CN 113200675 A CN113200675 A CN 113200675A
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China
Prior art keywords
alkali metal
optical fiber
doping
fiber preform
solution
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Pending
Application number
CN202110393662.XA
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Chinese (zh)
Inventor
王龙飞
李凡
顾建宏
帅小立
刘顺
冀云磊
张佚
吴林清
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Jiangsu Yongding Fiber Technology Co ltd
Jiangsu Etern Co Ltd
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Jiangsu Yongding Fiber Technology Co ltd
Jiangsu Etern Co Ltd
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Application filed by Jiangsu Yongding Fiber Technology Co ltd, Jiangsu Etern Co Ltd filed Critical Jiangsu Yongding Fiber Technology Co ltd
Priority to CN202110393662.XA priority Critical patent/CN113200675A/en
Publication of CN113200675A publication Critical patent/CN113200675A/en
Priority to PCT/CN2021/113714 priority patent/WO2022217799A1/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/01205—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
    • C03B37/01262—Depositing additional preform material as liquids or solutions, e.g. solution doping of preform tubes or rods
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/01205—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
    • C03B37/01225—Means for changing or stabilising the shape, e.g. diameter, of tubes or rods in general, e.g. collapsing
    • C03B37/01257—Heating devices therefor

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

Abstract

The invention discloses a method for doping alkali metal and an optical fiber preform, comprising the following steps: s10, dissolving compound raw material alkali metal in the solution; s20, soaking the optical fiber preform loose body into the solution; and S30, taking the loose body of the optical fiber prefabricated rod out of the solution, drying, oxidizing and sintering to obtain the optical fiber prefabricated rod doped with alkali metal. The method for doping the alkali metal can realize the doping of the alkali metal without melting and gasifying the alkali metal compound raw material at high temperature, has simple process, good repeatability, good doping effect and low cost, and is very suitable for large-scale production.

Description

Method for doping alkali metal and optical fiber preform
Technical Field
The invention belongs to the technical field of optical fiber manufacturing, and particularly relates to an alkali metal doping method and an optical fiber preform.
Background
In the production of optical fiber preforms, the viscosity matching of the core layer and the cladding layer is generally required to be realized by doping with alkali metal elements (K, Na), thereby reducing the attenuation of the optical fiber. The alkali metal doping can effectively improve the viscosity matching between the core layer and the cladding layer of the optical fiber preform rod, effectively reduce the attenuation of the optical fiber, and is the leading edge and the hot spot of the research in the technical field of the current optical fiber manufacturing.
Patent US7088900B1 proposes an alkali metal-containing low attenuation optical fiber having an alkali metal content of not less than 20ppm wt%, and an optical fiber having a transmission loss of less than 0.178dB/km at a wavelength of 1550nm, and does not describe a method of doping with an alkali metal. The alkali metal doping provided in patents US20050063663a1, US7469559B2 and US7524780B2 is to put alkali metal compound raw material into the inner wall of the quartz tube and to dope alkali metal by the diffusion method in the tube. The patent US9250386B2 provides a vapor phase doping method, i.e. an alkali metal compound raw material is put into the inner wall of a quartz tube, and heated on the outer wall of the glass tube to melt the raw material into a vaporized state, so that the alkali metal is diffused and doped into a preform, and the loss of the prepared optical fiber at the 1550nm wavelength can be reduced by 0.17dB/km, and the alkali metal doped by the vapor phase method forms a concentration gradient on the inner and outer walls of the glass, and the distribution is not uniform. Documents US20140127507a1, US9229160B2, CN102627400B, CN102603179A, CN102627398A, CN103502164A, CN104093674A, CN102617033A, CN103502164A and CN102730977A all use a continuously moving heat source to heat the alkali metal compound raw material in the tube, and the alkali metal is doped into the inner wall of the glass tube by diffusion, so that the doping process is complicated. In patent CN106966581A, alkali metal doping is also performed by vapor phase method, but the method is different from patent XX 1. Specifically, the prepared preform loose body is placed in a graphite furnace with powdered KBr, the graphite furnace is heated, so that the KBr powder is melted into gas, the gas is doped into the preform loose body, and then K2O is formed after dehydration and oxidation reduction, so that the doping of K element is completed. Patent CN106396362A provides another method for doping alkali metal by vapor phase method, which is to dope alkali metal simultaneously during the deposition of core layer of core rod, so that the deposition of core rod is completed simultaneously with the doping of alkali metal. The invention takes out the gas volatilized after the alkali metal compound raw material is heated through the oxygen, so that the oxygen and the alkali metal compound raw material are pre-reacted in the heating process to generate the alkali metal oxide which needs to be doped into the optical fiber preform.
As can be seen from the above patents, the doping of alkali metal elements is mainly achieved by a gas phase method, i.e. by melting the alkali metal compound raw material powder into a gas phase at a high temperature (above 700 ℃), and this method requires a high temperature, is high in cost, is difficult to manufacture, and is not uniform in doping, which is not beneficial to reducing the manufacturing cost of the optical rod.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for doping alkali metal, which has the advantages of simple process, good repeatability and low cost.
In order to solve the above problems, the present invention provides a method of doping an alkali metal, comprising the steps of:
s10, dissolving the alkali metal compound raw material in the solution;
s20, soaking the optical fiber preform loose body into the solution;
and S30, taking the loose body of the optical fiber prefabricated rod out of the solution, drying, oxidizing and sintering to obtain the optical fiber prefabricated rod doped with alkali metal.
As a further improvement of the present invention, step S30 specifically includes the following steps:
s31, taking the loose body of the optical fiber preform out of the solution and putting the loose body into a sintering furnace;
and S32, drying, oxidizing and sintering the loose body of the optical fiber preform in a sintering furnace.
As a further improvement of the present invention, step S32 specifically includes the following steps:
s321, introducing nitrogen into the sintering furnace, and drying the loose body of the optical fiber preform by using the nitrogen;
s322, introducing chlorine and oxygen into the sintering furnace, and oxidizing the alkali metal compound to generate alkali metal oxide while dehydrating.
As a further improvement of the present invention, in step S33, helium gas is introduced into the sintering furnace simultaneously with chlorine gas and oxygen gas.
As a further improvement of the invention, the temperature in the sintering furnace is 900 ℃.
As a further improvement of the invention, the solution is any one of water, methanol or ethanol.
As a further improvement of the invention, the alkali metal compound raw material is KBr or NaBr.
As a further improvement of the present invention, the alkali metal compound raw material is powder.
As a further improvement of the present invention, in step S20, the optical fiber preform bulk is soaked in the solution for a time period of 1 hour or more.
In order to solve the above problems, the present invention also provides an optical fiber preform obtained by any one of the alkali metal doping methods described above.
The invention has the beneficial effects that:
the method for doping the alkali metal can realize the doping of the alkali metal without melting and gasifying the alkali metal compound raw material at high temperature, has simple process, good repeatability, good doping effect and low cost, and is very suitable for large-scale production.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention may be implemented in accordance with the content of the description, and in order to make the above and other objects, features, and advantages of the present invention more clearly understood, the following preferred embodiments are described in detail with reference to the accompanying drawings.
Drawings
Fig. 1 is a flow chart of a method of doping an alkali metal in a preferred embodiment of the present invention.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
As shown in fig. 1, a method for doping an alkali metal according to a preferred embodiment of the present invention comprises the steps of:
s10, dissolving the alkali metal compound raw material in the solution.
And S20, soaking the optical fiber preform loose body into the solution.
And S30, taking the loose body of the optical fiber prefabricated rod out of the solution, drying, oxidizing and sintering to obtain the optical fiber prefabricated rod doped with alkali metal.
In some embodiments, step S30 specifically includes the following steps:
and S31, taking the optical fiber preform loose body solution out to a sintering furnace.
And S32, drying, oxidizing and sintering the loose body of the optical fiber preform in a sintering furnace. Optionally, the temperature in the sintering furnace is 900 ℃.
In one embodiment, step S32 specifically includes the following steps:
s321, introducing nitrogen into the sintering furnace, and drying the loose body of the optical fiber preform by using the nitrogen.
S322, introducing chlorine and oxygen into the sintering furnace, and oxidizing the alkali metal compound to generate alkali metal oxide while dehydrating. Wherein chlorine is used for dehydration and oxygen is used for oxidation and dehydration.
Optionally, in step S33, helium gas is introduced into the sintering furnace while chlorine gas and oxygen gas are introduced into the sintering furnace. Among them, helium is used for heat conduction and dehydration.
Optionally, the solution is any one of water, methanol or ethanol. Optionally, the alkali metal compound raw material is KBr or NaBr.
In some embodiments, the alkali metal compound starting material is a powder, which facilitates dissolution.
In some embodiments, in step S20, the optical fiber preform bulk solution is soaked for 1 hour or more.
Some specific examples are as follows:
example 1: the concentration of the preparation is 6.6 x 10-3g/ml NaBr ethanol solution, immersing the optical fiber preform loose body in the solution for 1 hour, taking out, and using N2After drying, introducing oxygen and chlorine at 900 deg.C to generate Na2O, deposited in the bulk of the optical fiber preform, Na2The O concentration was 2000 ppm.
Example 2: the concentration of the preparation is 6.6 x 10-6g/ml NaBr water solution, immersing the optical fiber preform loose body in the solution for 1 hour, taking out, and using N2After drying, introducing oxygen and chlorine at 900 deg.C to generate Na2O, deposited in the bulk of the optical fiber preform, Na2The O concentration was 2 ppm.
Example 3: the concentration of the preparation is 5.05 x 10-3g/ml KBr methanol solution, immersing the loose body of optical fiber preform in the solution for 1 hr, taking out, and using N2After drying, introducing oxygen and chlorine at 900 ℃ to generate K2O, deposited in the bulk of the optical fiber preform, K2The O concentration was 2000 ppm.
Example 4: the concentration of the preparation is 5.05 x 10-6g/ml KBr ethanol solution, immersing the optical fiber preform loose body in the solution for 1 hour, taking out, and using N2After drying, introducing oxygen and chlorine at 900 ℃ to generate K2O, deposited in the bulk of the optical fiber preform, K2The O concentration was 2 ppm.
Example 5: the concentration of the preparation is 3.3 x 10-3g/ml KBr water solution, immersing the loose body of optical fiber preform in the solution for 1 hr, taking out, and using N2After drying, introducing oxygen and chlorine at 900 deg.C to generate Na2O, deposited in the bulk of the optical fiber preform, Na2The O concentration was 1000 ppm.
The invention also discloses an optical fiber preform which is obtained by the method for doping the alkali metal in any embodiment.
The method for doping the alkali metal can realize the doping of the alkali metal without melting and gasifying the alkali metal compound raw material at high temperature, has simple process, good repeatability, good doping effect and low cost, and is very suitable for large-scale production.
The above embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.

Claims (10)

1. A method of doping an alkali metal comprising the steps of:
s10, dissolving the alkali metal compound raw material in the solution;
s20, soaking the optical fiber preform loose body into the solution;
and S30, taking the loose body of the optical fiber prefabricated rod out of the solution, drying, oxidizing and sintering to obtain the optical fiber prefabricated rod doped with alkali metal.
2. The method for doping an alkali metal according to claim 1, wherein the step S30 specifically includes the steps of:
s31, taking the optical fiber preform loose solution out to a sintering furnace;
and S32, drying, oxidizing and sintering the loose body of the optical fiber preform in a sintering furnace.
3. The method for doping an alkali metal according to claim 2, wherein the step S32 specifically includes the steps of:
s321, introducing nitrogen into the sintering furnace, and drying the loose body of the optical fiber preform by using the nitrogen;
s322, introducing chlorine and oxygen into the sintering furnace, and oxidizing the alkali metal compound to generate alkali metal oxide while dehydrating.
4. The method of doping an alkali metal according to claim 3, wherein in step S33, helium gas is introduced into the sintering furnace simultaneously with chlorine gas and oxygen gas.
5. The method of doping an alkali metal according to claim 2, wherein the temperature in the sintering furnace is 900 degrees.
6. The method of doping an alkali metal according to claim 1, wherein the solution is any one of water, methanol, or ethanol.
7. The method of doping an alkali metal according to claim 1, wherein the alkali metal compound raw material is KBr or NaBr.
8. The method of doping an alkali metal according to claim 1, wherein the alkali metal compound raw material is a powder.
9. The method of doping an alkali metal according to claim 1, wherein the optical fiber preform is immersed in the soot solution for a period of time greater than or equal to 1 hour in step S20.
10. An optical fiber preform obtained by the method of doping an alkali metal according to any one of claims 1 to 9.
CN202110393662.XA 2021-04-13 2021-04-13 Method for doping alkali metal and optical fiber preform Pending CN113200675A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022217799A1 (en) * 2021-04-13 2022-10-20 江苏永鼎股份有限公司 Method for doping alkali metal and optical fiber preform

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4110093A (en) * 1974-04-22 1978-08-29 Macedo Pedro B Method for producing an impregnated waveguide
US4183620A (en) * 1976-12-30 1980-01-15 Pedro Buarque De Macedo Joint doped porous glass article with high modifier concentrations
CN1692086A (en) * 2002-08-28 2005-11-02 康宁股份有限公司 Low loss optical fiber and method for making same
CN1842499A (en) * 2003-08-29 2006-10-04 康宁股份有限公司 Optical fiber containing an alkali metal oxide and methods and apparatus for manufacturing same
CN108002698A (en) * 2017-11-29 2018-05-08 长飞光纤光缆股份有限公司 A kind of manufacture method of preform
JP2019218250A (en) * 2018-06-21 2019-12-26 古河電気工業株式会社 Method for manufacturing optical fiber and method for manufacturing optical fiber preform
CN111847867A (en) * 2020-07-21 2020-10-30 复旦大学 Optical fiber preform and preparation method thereof

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101066281B1 (en) * 2003-08-29 2011-09-20 코닝 인코포레이티드 Optical Fiber Containing an Alkali Metal Oxide and Methods and Apparatus for Manufacturing Same
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

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4110093A (en) * 1974-04-22 1978-08-29 Macedo Pedro B Method for producing an impregnated waveguide
US4183620A (en) * 1976-12-30 1980-01-15 Pedro Buarque De Macedo Joint doped porous glass article with high modifier concentrations
CN1692086A (en) * 2002-08-28 2005-11-02 康宁股份有限公司 Low loss optical fiber and method for making same
CN1842499A (en) * 2003-08-29 2006-10-04 康宁股份有限公司 Optical fiber containing an alkali metal oxide and methods and apparatus for manufacturing same
CN108002698A (en) * 2017-11-29 2018-05-08 长飞光纤光缆股份有限公司 A kind of manufacture method of preform
JP2019218250A (en) * 2018-06-21 2019-12-26 古河電気工業株式会社 Method for manufacturing optical fiber and method for manufacturing optical fiber preform
CN111847867A (en) * 2020-07-21 2020-10-30 复旦大学 Optical fiber preform and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022217799A1 (en) * 2021-04-13 2022-10-20 江苏永鼎股份有限公司 Method for doping alkali metal and optical fiber preform

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Application publication date: 20210803