CN111285599A - Method for preparing optical fiber preform cladding by in-tube chemical vapor deposition method - Google Patents
Method for preparing optical fiber preform cladding by in-tube chemical vapor deposition method Download PDFInfo
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- CN111285599A CN111285599A CN202010013524.XA CN202010013524A CN111285599A CN 111285599 A CN111285599 A CN 111285599A CN 202010013524 A CN202010013524 A CN 202010013524A CN 111285599 A CN111285599 A CN 111285599A
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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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/70—Control measures
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Abstract
The invention discloses a method for preparing optical fiber preform cladding by a tube-in chemical vapor deposition method6Etching the inner wall of a high-purity quartz liner tube at high temperature to ensure that the inner wall of the liner tube is smooth and is convenient for deposition, and then introducing SiCl4，GeCl4And SF6And reacting the reaction gas at high temperature to deposit the optical cladding. Compared with the traditional pure SiO2Design of the cladding in SiO2Ge and F element are doped in the cladding, so that the refractive index of the optical cladding is consistent with that of the external liner tube, the advantages of effectively reducing the attenuation of the optical fiber, improving the red light performance of the optical fiber and avoiding the problem of optical fiber welding countershaft caused by Trench.
Description
Technical Field
The invention belongs to the technical field of optical fiber preparation, and particularly relates to a method for preparing an optical fiber preform cladding by a tube chemical vapor deposition method.
Background
With the continuous development of optical fiber communication technology, the requirements on optical fiber preparation technology are higher and higher, the preparation of an optical fiber preform is a core technology in the field of optical fiber preparation, the parameters of the optical fiber preform directly determine the performance and the application of an optical fiber, at present, the preparation of an optical fiber core rod cladding generally adopts a pure SiO2 cladding design, namely only SiO2 is deposited as an optical cladding, and the defect is that the attenuation of the optical fiber can be ensured to be at a lower level only by depositing a thicker cladding. Meanwhile, the deposition of the pure silicon cladding requires higher temperature, and the non-roundness and the tortuosity of the liner tube are deteriorated due to the excessively high deposition temperature, so that the non-roundness and the tortuosity of the preform are influenced. Thus, there is a need for improvements and optimizations in the existing preform cladding preparation techniques.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing an optical fiber preform cladding by a tube chemical vapor deposition method, which can effectively optimize the defects of a pure silicon cladding of an optical fiber core rod and reduce the attenuation of an optical fiber.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for preparing optical fiber preform cladding by tube chemical vapor deposition method is provided, which comprises the following steps,
1) using a quartz liner tube as a base tube, and respectively extending and connecting quartz extension tubes at two ends of the liner tube;
2) installing a rotary joint at the air inlet end of the liner tube, and clamping the liner tube on a deposition lathe;
3) introducing SF into the pipe6Etching the inner wall of the liner tube by gas at high temperature;
4) introducing SiCl into the tube4、GeCl4、SF6And O2Depositing an optical cladding, wherein the refractive index of the optical cladding is consistent with that of the liner tube;
5) depositing an optical core layer on the inner wall of the optical cladding glass;
6) performing fusion shrinkage on the deposited hollow preform;
7) introduction of SF6And etching the inner wall of the core layer by the gas.
According to the technical scheme, the method further comprises the following steps: the hollow prefabricated rod is subjected to compaction and polishing; then, the core rod is subjected to a stretch-breaking and rod-dropping operation by using an oxyhydrogen flame hand-held torch.
According to the technical scheme, after the step 1) is finished, the liner tube is respectively cleaned by using an alkaline cleaning agent, mixed acid of hydrofluoric acid and nitric acid and pure water, and high-purity N is used2And (5) blowing and drying.
According to the technical scheme, the used complex acid is prepared by matching hydrofluoric acid and nitric acid according to the proportion of 6: 1.
According to the technical scheme, SiCl is introduced in the step 4)4、GeCl4、SF6And O2And preparing the Si-Ge-F optical cladding glass.
According to the technical scheme, the thickness of the Si-Ge-F optical cladding glass is 2-10 mm.
According to the technical scheme, wherein SiCl is adopted4The flow rate of (1) is 250-300 sccm, GeCl4The flow rate of (1) is 150-200 sccm, SF6The flow rate of (1) is 3to 4sccm, wherein O2The flow rate of (A) is 1.8 times of the total flow rate of the first three.
According to the technical scheme, the pressure difference between the air outlet end and the atmospheric pressure is controlled to be 0-1.2 torr, the pressure difference between the air inlet end and the air outlet end is controlled to be 2-3 torr, the deposition temperature is controlled to be 1800-1900 ℃, and the heat source moving speed is 70-100 mm/min.
The invention has the following beneficial effects: the method can effectively optimize the defects of the pure silicon cladding of the optical fiber core rod and reduce the attenuation of the optical fiber.
Drawings
The invention will be further described with reference to the accompanying drawings and examples, in which:
FIG. 1 is a process flow diagram of example 1 of the present invention;
FIG. 2 is a cross-sectional refractive index profile of a preform prepared in example 1 of the present invention;
FIG. 3 is a cross-sectional refractive index profile of a preform fabricated by a conventional process.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1:
referring to fig. 1, an embodiment of the present invention provides a method for preparing a cladding layer of an optical fiber preform by a tube-in-tube chemical vapor deposition method, including the following steps:
1) preparing a clean liner tube with two ends connected with extension tubes, installing a rotary joint at an air inlet end, installing the liner tube on a deposition lathe, starting a special Recipe, preheating the liner tube, and gradually increasing the temperature to 1200 ℃;
2) introducing SF into the liner pipe at 1700 DEG C6，,O2Etching the liner tube for a plurality of times;
3) introducing SiCl at 1750 DEG C4，GeCl4，SF6，,O2The gas is waited, the heat source moves several times repeatedly to deposit Si-Ge-F optical cladding glass;
4) introducing SiCl with corresponding flow according to the type of the preform4，GeCl4，SF6，O2Isogas deposition of optical core glass;
5) performing fusion shrinkage on the deposited hollow preform to reduce the diameter of an inner hole of the hollow preform to 2-4 mm;
6) after completion of the collapsing, 2 passes of high purity O were performed2Purging, and gradually reducing the temperature to 1600 ℃;
7) introducing SF at 1600 DEG C6，O2Etching the inner wall for 1 time;
8) after the etching is finished, high-purity O is introduced2Purging, and gradually raising the temperature to 1700 ℃;
9) continuously heating, reducing the moving speed of a heat source to 2.5-20 mm/min, keeping the pressure difference between the air outlet end and the atmospheric pressure at-0.2-0.1 torr, and the temperature at 1850-2150 ℃, and sintering the hollow preform into a solid preform;
10) polishing the solid prefabricated rod after being burnt to make the solid prefabricated rod transparent;
11) the preform was subjected to a stretch-breaking and rod-dropping operation using an oxyhydrogen flame burner.
Observation of FIG. 3 and FIG. 3, it can be seen that SiO is generated during deposition using a conventional pure silicon cladding design2The cladding has a refractive index slightly lower than that of the substrate tube, so that a depressed refractive index (Trench) is formed between the substrate tube and the optical core, which is disadvantageous for the optical fiber to be welded to the axis during use, and pure SiO2The design of the cladding is not conducive to reducing the attenuation of the fiber in the 1383nm band (water peak) and the 600nm to 800nm band.
In the new process for preparing the core rod cladding, the traditional pure silicon cladding or fluorine-doped cladding design is abandoned, the brand-new fluorine-germanium co-doped cladding design is used, the refractive index of the deposited optical is consistent with that of a high-purity quartz liner tube, the refractive index matching of the optical cladding and the liner tube is realized, the refractive index profile curve of the prepared preform is shown in figure 2, the refractive index curves of the optical cladding and the liner tube are basically flush, the refractive index sag is avoided, the attenuation of the optical fiber is ensured to be at a lower level, and the time for welding the optical fiber to the axis is reduced.
Example 2:
the method for preparing the optical fiber preform cladding by the tube chemical vapor deposition method comprises the following steps:
1) preparation work before deposition: the method comprises the steps of extension connection of a liner tube, cleaning and drying, tube loading, residual stress release, liner tube correction and the like;
2) using SF6Etching and cleaning the inner wall of the liner tube for a plurality of times at 1650 ℃ to ensure that the inner wall of the liner tube is smooth and easy to deposit;
3) depositing a plurality of layers of optical cladding glass on the inner wall of the liner tube; introducing SiCl4，GeCl4，SF6，O2Preparing Si-Ge-F optical cladding glass by using equal gas, wherein the thickness of the Si-Ge-F optical cladding glass is 2-10 mm, and SiCl is adopted4The flow rate of (1) is 250-300 sccm, GeCl4The flow rate of (1) is 150-200 sccm, SF6OfThe flow rate is 3-4 sccm, and the flow rate of O2 is 1.8 times of the total flow rate of the three parts; controlling the pressure difference between the air outlet end and the atmospheric pressure to be 0-1.2 torr, controlling the pressure difference between the air inlet end and the air outlet end to be 2-3 torr, controlling the deposition temperature to be 1700-1800 ℃ and controlling the heat source moving speed to be 70-100 mm/min.
4) Introducing high-purity O2Purging is carried out;
5) depositing a plurality of optical core layers on the inner wall of the optical fiber cladding; introducing SiCl4，GeCl4，SF6，O2And preparing a plurality of layers of optical core layer glass by using the gases.
6) Carrying out a plurality of times of melting and shrinking processes on the deposited hollow prefabricated rod until the diameter of the inner hole of the hollow prefabricated rod reaches a burnable condition; the controllable sintering conditions in the hollow preform are as follows: collapsing the diameter of the inner hole to 2-4 mm; and during the fusion, controlling the pressure difference between the air outlet end of the hollow preform and the ambient pressure to be-0.2-0.1 torr, controlling the rotating speed of the preform to be 15-40 rpm, controlling the moving speed of a heat source to be 30-50 mm/min, and controlling the temperature to be 2000-2150 ℃.
7) Introduction of SF6Etching the inner wall of the core layer at high temperature;
8) adjusting the pressure of the tube to micro negative pressure, reducing the moving speed of a heat source, and sintering the hollow preform into a solid preform;
9) polishing the solid prefabricated rod after being burnt to remove SiO on the surface2Microparticles;
10) and breaking the polished transparent solid preform rod, and discharging the rod.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (8)
1. A method for preparing optical fiber preform cladding by chemical vapor deposition in a tube is characterized by comprising the following steps,
1) using a quartz liner tube as a base tube, and respectively extending and connecting quartz extension tubes at two ends of the liner tube;
2) installing a rotary joint at the air inlet end of the liner tube, and clamping the liner tube on a deposition lathe;
3) introducing SF into the pipe6Etching the inner wall of the liner tube by gas at high temperature;
4) introducing SiCl into the tube4、GeCl4、SF6And O2Depositing an optical cladding, wherein the refractive index of the optical cladding is consistent with that of the liner tube;
5) depositing an optical core layer on the inner wall of the optical cladding glass;
6) performing fusion shrinkage on the deposited hollow preform;
7) introduction of SF6And etching the inner wall of the core layer by the gas.
2. The method of preparing an optical fiber preform cladding by in-tube chemical vapor deposition according to claim 1, further comprising: the hollow prefabricated rod is subjected to compaction and polishing; then, the core rod is subjected to a stretch-breaking and rod-dropping operation by using an oxyhydrogen flame hand-held torch.
3. The method for preparing a clad of an optical fiber preform according to claim 1 or 2, wherein after the completion of the step 1), the substrate tube is cleaned with an alkaline cleaner, a mixed acid of hydrofluoric acid and nitric acid, and pure water, respectively, and high purity N is used2And (5) blowing and drying.
4. The method of preparing a clad for an optical fiber preform according to claim 3, wherein the complex acid is prepared by mixing hydrofluoric acid and nitric acid at a ratio of 6: 1.
5. The method of preparing an optical fiber preform cladding by in-tube chemical vapor deposition according to claim 1 or 2, wherein SiCl is introduced in the step 4)4、GeCl4、SF6And O2And preparing the Si-Ge-F optical cladding glass.
6. The method of preparing an optical fiber preform cladding by an in-tube chemical vapor deposition method according to claim 5, wherein the thickness of the Si-Ge-F optical cladding glass is 2to 10 mm.
7. The method of claim 5 in which the SiCl is used to prepare the optical fiber preform cladding4The flow rate of (1) is 250-300 sccm, GeCl4The flow rate of (1) is 150-200 sccm, SF6The flow rate of (1) is 3to 4sccm, wherein O2The flow rate of (A) is 1.8 times of the total flow rate of the first three.
8. The method of claim 5, wherein the pressure difference between the outlet end and the atmospheric pressure is controlled to be 0-1.2 torr, the pressure difference between the inlet end and the outlet end is controlled to be 2-3 torr, the deposition temperature is controlled to be 1800-1900 ℃, and the heat source moving speed is 70-100 mm/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115385566A (en) * | 2022-09-27 | 2022-11-25 | 武汉长盈通光电技术股份有限公司 | Method for preparing elliptical core optical fiber prefabricated rod |
| CN115417591A (en) * | 2022-09-14 | 2022-12-02 | 武汉长盈通光电技术股份有限公司 | Method for preparing polarization maintaining optical fiber stress rod by FCVD |
| CN115557692A (en) * | 2022-09-07 | 2023-01-03 | 武汉长盈通光电技术股份有限公司 | Preparation method of large-numerical-aperture preform |
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| AU2066800A (en) * | 2000-03-06 | 2001-09-13 | University Of Sydney, The | Method of fabricating a preform |
| CN102249533A (en) * | 2011-04-28 | 2011-11-23 | 长飞光纤光缆有限公司 | Method for manufacturing large-size low-water-peak prefabricated rod |
| CN102757179A (en) * | 2012-08-02 | 2012-10-31 | 长飞光纤光缆有限公司 | Method for preparing large-size optical fiber preform |
| CN109399909A (en) * | 2018-09-06 | 2019-03-01 | 上海至纯洁净系统科技股份有限公司 | A kind of method that PCVD technique makes low hydroxyl optical fiber prefabricated rod mandrel |
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2020
- 2020-01-07 CN CN202010013524.XA patent/CN111285599A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2066800A (en) * | 2000-03-06 | 2001-09-13 | University Of Sydney, The | Method of fabricating a preform |
| CN102249533A (en) * | 2011-04-28 | 2011-11-23 | 长飞光纤光缆有限公司 | Method for manufacturing large-size low-water-peak prefabricated rod |
| CN102757179A (en) * | 2012-08-02 | 2012-10-31 | 长飞光纤光缆有限公司 | Method for preparing large-size optical fiber preform |
| CN109399909A (en) * | 2018-09-06 | 2019-03-01 | 上海至纯洁净系统科技股份有限公司 | A kind of method that PCVD technique makes low hydroxyl optical fiber prefabricated rod mandrel |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115557692A (en) * | 2022-09-07 | 2023-01-03 | 武汉长盈通光电技术股份有限公司 | Preparation method of large-numerical-aperture preform |
| CN115417591A (en) * | 2022-09-14 | 2022-12-02 | 武汉长盈通光电技术股份有限公司 | Method for preparing polarization maintaining optical fiber stress rod by FCVD |
| CN115385566A (en) * | 2022-09-27 | 2022-11-25 | 武汉长盈通光电技术股份有限公司 | Method for preparing elliptical core optical fiber prefabricated rod |
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Address after: No.80, Gaoxin 5th Road, Donghu Development Zone, Wuhan City, Hubei Province Applicant after: Wuhan changyingtong Optoelectronic Technology Co.,Ltd. Address before: 430205 No. five, No. 80, hi tech Development Zone, East Lake New Technology Development Zone, Hubei, Wuhan Applicant before: YANGTZE OPTICAL ELECTRONIC Co.,Ltd. |
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