CN112266162B - Fluorine-doped quartz tube suitable for large-size optical fiber preform and preparation method thereof - Google Patents
Fluorine-doped quartz tube suitable for large-size optical fiber preform and preparation method thereof Download PDFInfo
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- CN112266162B CN112266162B CN202011208238.5A CN202011208238A CN112266162B CN 112266162 B CN112266162 B CN 112266162B CN 202011208238 A CN202011208238 A CN 202011208238A CN 112266162 B CN112266162 B CN 112266162B
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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]
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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]
- C03B37/01446—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
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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]
- C03B37/01446—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
- C03B37/01453—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering for doping the preform with flourine
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- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
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- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a preparation method of a fluorine-doped quartz tube suitable for a large-size optical fiber preform, which comprises the following steps: depositing quartz powder on the surface of a target rod to obtain a loose powder rod; fully dehydrating the obtained loose powder rod to obtain a purified loose powder rod; introducing CF into sintering furnace 4 And helium, and under certain temperature and pressure conditions, preheating and pressurizing the purified loose powder rod to obtain a purified fluorine-doped loose rod; introducing CF into sintering furnace 4 And helium, sintering the purified fluorine-doped loose rod after preheating and pressurizing treatment; and drilling and processing an inner hole of the sintered glass rod to obtain the fluorine-doped quartz tube. The fluorine-doped quartz tube obtained by the preparation method not only has lower refractive index, but also has larger size, and can meet the use requirement of a large-size optical fiber preform.
Description
Technical Field
The invention relates to the field of optical fiber preform manufacturing, in particular to a fluorine-doped quartz tube suitable for a large-size optical fiber preform and a preparation method thereof.
Background
Quartz ferrules have been developed for a considerable period of time as a well known optical fiber preform, which has reached a high level in process control and size. Generally, the quartz sleeve in the conventional sense is not required to have optical quality, but with the increase of optical fiber requirements and performances, refractive index requirements are gradually put forward for the quartz sleeve, and then the quartz sleeve becomes an important role in optical performance improvement. Among them, the continuous melting method is used for preparing quartz thin-skin tubes with low refractive index, which occupies most markets in a quite long time.
It has been known that a silica ferrule can be used for improving optical performance of an optical fiber, and researches on a ferrule having optical characteristics have been increasingly conducted. US patent 5837334 proposes a method for preparing a low refractive index quartz sleeve by VAD or OVD process, but the dopant volatilizes during manufacture, the refractive index range of the material is difficult to control, and the problem of large refractive index fluctuation in the radial direction and the axial direction occurs.
Chinese patent CN101314515a provides a method for preparing a quartz tube, which adopts quartz sand to melt into a quartz ingot, and adopts the methods of machining and tube drawing to prepare the quartz ingot into a quartz tube with certain specification. This has the disadvantage that only quartz tubes having no optical properties can be produced, and it is difficult to produce a quartz tube material having a certain profile structure and refractive index profile.
Chinese patent CN103553320B provides a method for preparing a low refractive index quartz tube by PCVD, wherein the relative refractive index of the quartz layer can reach-1.5% to-0.3%, the cross-sectional structure can have various forms (CN 103553320B fig. 8-12), the inner diameter of the sleeve is equal to or greater than 24mm, and the outer diameter is less than or equal to 63mm; chinese patent CN103951182a provides a combination of improved chemical vapor deposition (MCVD) and outside tube vapor deposition (OVD) methods for producing a sleeve with deep refractive index or complex refractive index profile with a refractive index difference up to-0.0053 (CN 103951182a fig. 3); the two patents have the obvious disadvantage of being relatively small in size and difficult to directly use with light bars greater than 120mm and above.
With the continuous decrease of the price of the optical fiber, the advantages of the large-size and oversized optical rods are more obvious, the large-size optical rod occupation ratio in the sales of the optical rods is increased to 80%, the corresponding small-size fluorine-doped sleeve cannot meet the use requirement, and a large-size sleeve production process with low refractive index is necessary to be developed to meet the requirement of the large-size optical rods.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a fluorine-doped quartz tube suitable for large-size optical fiber preforms and a preparation method thereof; the fluorine-doped quartz tube obtained by the preparation method not only has lower refractive index, but also has larger size, and can meet the use requirement of a large-size optical fiber preform.
In order to achieve the technical purpose and the technical effect, the invention is realized by the following technical scheme:
a preparation method of fluorine-doped quartz tube suitable for large-size optical fiber perform comprises the following steps:
(1) Deposition of
Depositing quartz powder on the surface of a target rod to obtain a loose powder rod;
(2) Dewatering
Transferring the loose powder rod obtained in the step (1) into a sintering furnace, and introducing 0.5-2L/min of chlorine gas at 900-1200 ℃ for full dehydration treatment to obtain a purified loose powder rod;
(3) Preheating and pressurizing
Charging a sintering furnace with a material containing CF 4 Mixed gas I with helium and at 900-1200 DEG CUnder the temperature condition and the pressure condition of 60-130 Pa, the purified loose powder rod rotates at the speed of 2mm/min so as to perform preheating and pressurizing treatment on the purified loose powder rod, and the purified fluorine-doped loose powder rod is obtained;
(4) Sintering
Charging a sintering furnace with a material containing CF 4 Sintering the purified fluorine-doped loose rod subjected to preheating and pressurizing treatment at the temperature of 1300-1500 ℃ to completely vitrify the purified fluorine-doped loose rod, preserving heat for 4-8 hours after vitrification to obtain a sintered glass rod, taking out the sintered glass rod, and cooling to room temperature;
(5) Drilling and bore treatment
Mechanically drilling the sintered glass rod to form a hollow quartz tube with an inner hole; and honing the inner hole of the hollow quartz tube to obtain the fluorine-doped quartz tube suitable for the large-size optical fiber preform.
Further, the deposition process in step (1) employs a VAD or OVD process.
Further, during the deposition in the step (1), CF is also introduced into the deposition center 4 The flow rate is 0-800 ml/min.
Further, the loose powder rod obtained in the step (1) has the diameter of 300-350 mm and the average density of 0.3-0.6 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the And the density of the loose powder rod is the largest at the radius of 20-40 mm.
Further, the time of the preheating and pressurizing treatment in the step (3) is set according to the following formula,
wherein,,
h is preheating treatment time, and the unit is min;
d is the inner diameter size of a furnace core pipe of the sintering furnace, and the unit is mm;
l is the total length of a furnace core tube of the sintering furnace, and the unit is mm;
v is CF led into furnace core tube 4 Flow in L/min.
Further, CF in the mixed gas I introduced in the step (3) 4 And helium in a ratio of 4:1; CF in the mixed gas II introduced in the step (4) 4 And helium is present in a ratio of 1:8.
Furthermore, when the inner hole diameter of the fluorine-doped quartz tube is required to be larger than 30mm, the fluorine-doped quartz tube with the inner hole diameter larger than 30mm is obtained by adopting the matching of drilling and blowing tube drawing processes; the method comprises the following steps: firstly, machining a small hole with the inner diameter of 5-20 mm in a mechanical drilling mode in a sintered glass rod, then softening the sintered glass rod, and blowing N into the small hole 2 The small holes are synchronously enlarged, and then the softened sintered glass rod is stretched by a stretching process, so that the fluorine-doped quartz tube with the inner hole diameter of more than 30mm is finally obtained.
The invention also provides a fluorine-doped quartz tube which is suitable for the large-size optical fiber preform and is obtained by the preparation method, wherein the fluorine-doped quartz tube is provided with an inner hole, the outer diameter of the fluorine-doped quartz tube is 120-160 mm, the length of the fluorine-doped quartz tube is 1400-1600 mm, and the relative refractive index of the outer layer is-0.65% -0.40%.
The invention has the beneficial effects that:
according to the preparation method, after the loose powder rod is dehydrated, the purified loose powder rod is placed under the temperature condition of 900-1200 ℃ and the pressure condition of 60-130 Pa for preheating and pressurizing treatment, the diffusion effect is realized through the preheating and pressurizing process, so that the fluorine doping agent can be diffused to the central position of the loose powder rod, and after the preheating and pressurizing treatment for a certain time, the pressure is reduced for sintering, and the fluorine doping quartz tube suitable for the large-size optical fiber preform rod is obtained. The fluorine component in the fluorine-doped quartz tube obtained by the preparation method can diffuse towards the central position, so that the refractive index of the central position of the quartz tube is reduced, and the relative refractive index of the outer layer of the obtained fluorine-doped quartz tube reaches a lower level; meanwhile, the fluorine-doped quartz tube with larger size can be obtained by using the preparation method of the invention, so that the fluorine-doped quartz tube is suitable for large-size optical fiber preforms.
The fluorine-doped quartz tube obtained by the preparation method has the advantages of large size and low refractive index, and can meet the use requirement of large-size optical fiber perform.
Drawings
FIG. 1 is a schematic view of the radial structure of a fluorine-doped quartz tube according to the present invention.
FIG. 2 is a graph showing the radial density distribution of the loose powder rod obtained in the step (1) in the production method of the present invention.
Fig. 3 to 5 are schematic views of three refractive index profiles of fluorine-doped quartz tubes obtained by the preparation method of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings so that the advantages and features of the present invention can be more easily understood by those skilled in the art, thereby making clear and defining the scope of the present invention.
A preparation method of fluorine-doped quartz tube suitable for large-size optical fiber perform comprises the following steps:
(1) Deposition of
Depositing quartz powder on the surface of the target rod by VAD or OVD process, and introducing CF during deposition 4 The flow is 0-800 ml/min, and loose powder sticks are obtained; the VAD process or the OVD process is a conventional deposition process and will not be described in detail herein;
the diameter of the loose powder rod obtained in the step (1) is 300-350 mm, and the average density is 0.3-0.6 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the As shown in FIG. 2, the loose powder rod has the greatest density at the radius of 20-40 mm;
(2) Dewatering
Transferring the loose powder rod obtained in the step (1) into a sintering furnace, and introducing 0.5-2L/min of chlorine gas at 900-1200 ℃ for full dehydration treatment to obtain a purified loose powder rod;
(3) Preheating and pressurizing
Charging a sintering furnace with a material containing CF 4 And helium, and rotating the purified loose powder rod at a speed of 2mm/min under the temperature condition of 900-1200 ℃ and the pressure condition of 60-130 Pa so as to preheat and pressurize the purified loose powder rodTreating, namely obtaining a purified fluorine-doped loose powder rod after preheating and pressurizing treatment; CF in the first mixed gas 4 And helium in a ratio of 4:1;
wherein the time of the preheating and pressurizing treatment is set according to the following formula,
in the method, in the process of the invention,
h is preheating treatment time, and the unit is min;
d is the inner diameter size of a furnace core pipe of the sintering furnace, and the unit is mm;
l is the total length of a furnace core tube of the sintering furnace, and the unit is mm;
v is CF led into furnace core tube 4 Flow rate in L/min;
(4) Sintering
Charging a sintering furnace with a material containing CF 4 Sintering the purified fluorine-doped loose rod subjected to preheating and pressurizing treatment at the temperature of 1300-1500 ℃ to completely vitrify the purified fluorine-doped loose rod, preserving heat for 4-8 hours after vitrification to obtain a sintered glass rod, taking out the sintered glass rod, and cooling to room temperature; CF in the mixed gas II 4 And helium in a ratio of 1:8;
(5) Drilling and bore treatment
Mechanically drilling the sintered glass rod to form a hollow quartz tube with an inner hole; and honing the inner hole of the hollow quartz tube to obtain the fluorine-doped quartz tube suitable for the large-size optical fiber preform.
When the inner hole diameter R of the obtained fluorine-doped quartz tube is required 1 When the diameter of the fluorine-doped quartz tube is larger than 30mm, the fluorine-doped quartz tube with the inner hole diameter of larger than 30mm is obtained by adopting the matching of drilling and blowing tube drawing processes; the method comprises the following steps: firstly, machining a small hole with the inner diameter of 5-20 mm in a mechanical drilling mode in a sintered glass rod, then softening the sintered glass rod, and blowing N with a certain pressure into the small hole 2 The small holes are synchronously enlarged, and then the stretching process is utilized to softenAnd stretching the sintered glass rod to finally obtain the fluorine-doped quartz tube with the inner hole diameter larger than 30 mm.
As shown in fig. 1, the fluorine-doped quartz tube suitable for large-sized optical fiber preforms obtained by the above-described preparation method has an inner bore, i.e., the quartz tube has an innermost core layer and an outermost outer layer; and the outer diameter R of the fluorine-doped quartz tube 2 120-160 mm, 1400-1600 mm in length and-0.65-0.40% in relative refractive index of the outer layer.
As shown in fig. 3 to 5, the fluorine-doped quartz tube with three refractive index profiles can be obtained by adjusting different process conditions of the preparation method; wherein, the refractive index profile shown in FIG. 3 is a flat profile structure, and the refractive index height difference between the outer layer and the core layer of the quartz tube is 0, so as to achieve a flat structure; the refractive index profile shown in FIG. 4 is of a middle convex profile structure, and the refractive index of the outer layer of the quartz tube is lower than that of the core layer; the refractive index profile shown in fig. 5 is a concave profile structure in the middle, and the refractive index of the outer layer of the quartz tube is higher than that of the core layer, so that the dispersion and macrobending performance can be improved.
The process conditions for producing fluorine-doped quartz tubes having the three refractive index profile structures are shown in table 1 below.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related technical fields are included in the scope of the present invention.
Claims (6)
1. The preparation method of the fluorine-doped quartz tube suitable for the large-size optical fiber preform is characterized by comprising the following steps of:
(1) Deposition of
Depositing quartz powder on the surface of a target rod to obtain a loose powder rod; the diameter of the loose powder rod obtained in the step (1) is 300-350 mm,the average density is 0.3-0.6 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The density of the loose powder rod is maximum at the radius of 20-40 mm;
(2) Dewatering
Transferring the loose powder rod obtained in the step (1) into a sintering furnace, and introducing 0.5-2L/min of chlorine gas at 900-1200 ℃ for full dehydration treatment to obtain a purified loose powder rod;
(3) Preheating and pressurizing
Charging a sintering furnace with a material containing CF 4 The mixed gas I and helium rotates the purified loose powder rod at a speed of 2mm/min under the temperature condition of 900-1200 ℃ and the pressure condition of 60-130 Pa so as to perform preheating and pressurizing treatment on the purified loose powder rod to obtain a purified fluorine-doped loose powder rod;
the time of the preheating and pressurizing treatment in this step (3) is set according to the following formula,
；
wherein,,
h is preheating and pressurizing time, and the unit is min;
d is the inner diameter size of a furnace core pipe of the sintering furnace, and the unit is mm;
l is the total length of a furnace core tube of the sintering furnace, and the unit is mm;
v is CF led into furnace core tube 4 Flow rate in L/min;
(4) Sintering
Charging a sintering furnace with a material containing CF 4 Sintering the purified fluorine-doped loose rod subjected to preheating and pressurizing treatment at the temperature of 1300-1500 ℃ to completely vitrify the purified fluorine-doped loose rod, preserving heat for 4-8 hours after vitrification to obtain a sintered glass rod, taking out the sintered glass rod, and cooling to room temperature;
(5) Drilling and bore treatment
Mechanically drilling the sintered glass rod to form a hollow quartz tube with an inner hole; and honing the inner hole of the hollow quartz tube to obtain the fluorine-doped quartz tube suitable for the large-size optical fiber preform.
2. The method for preparing a fluorine-doped silica tube suitable for use in a large-sized optical fiber preform according to claim 1, wherein the deposition process in step (1) employs a VAD or OVD process.
3. The method for preparing fluorine-doped silica tube suitable for large-size optical fiber preform according to claim 1, wherein CF is further introduced into the deposition center during the deposition in step (1) 4 The flow rate is 0-800 ml/min.
4. The method for preparing fluorine-doped silica tube suitable for large-size optical fiber preform according to claim 1, wherein CF in the mixed gas I introduced in the step (3) 4 And helium in a ratio of 4:1; CF in the mixed gas II introduced in the step (4) 4 And helium is present in a ratio of 1:8.
5. The method for preparing a fluorine-doped quartz tube suitable for a large-size optical fiber preform according to claim 1, wherein when the inner hole diameter of the fluorine-doped quartz tube is required to be larger than 30mm, the fluorine-doped quartz tube with the inner hole diameter of larger than 30mm is obtained by adopting the matching of drilling and blowing tube drawing processes; the method comprises the following steps: firstly, machining a small hole with the inner diameter of 5-20 mm in a mechanical drilling mode in a sintered glass rod, then softening the sintered glass rod, and blowing N into the small hole 2 The small holes are synchronously enlarged, and then the softened sintered glass rod is stretched by a stretching process, so that the fluorine-doped quartz tube with the inner hole diameter of more than 30mm is finally obtained.
6. A fluorine-doped silica tube suitable for large-size optical fiber preforms obtained by the method of any one of claims 1 to 5, characterized in that: the fluorine-doped quartz tube is provided with an inner hole, the outer diameter of the fluorine-doped quartz tube is 120-160 mm, the length of the fluorine-doped quartz tube is 1400-1600 mm, and the relative refractive index of the outer layer is-0.65% -0.40%.
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