CN111056740B - Device and method for preparing active optical fiber preform by PCVD method - Google Patents
Device and method for preparing active optical fiber preform by PCVD method Download PDFInfo
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- CN111056740B CN111056740B CN202010030680.7A CN202010030680A CN111056740B CN 111056740 B CN111056740 B CN 111056740B CN 202010030680 A CN202010030680 A CN 202010030680A CN 111056740 B CN111056740 B CN 111056740B
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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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/20—Specific substances in specified ports, e.g. all gas flows specified
- C03B2207/26—Multiple ports for glass precursor
- C03B2207/28—Multiple ports for glass precursor for different glass precursors, reactants or modifiers
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/42—Assembly details; Material or dimensions of burner; Manifolds or supports
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Abstract
The invention discloses a device and a method for preparing an active optical fiber preform by a PCVD method, wherein the device comprises a PCVD device and a doping device, the doping device comprises a gasification unit, a gas phase transmission unit and a gas phase deposition unit, the gas phase deposition unit comprises a liner tube, the gasification unit comprises a common deposition raw material supply subunit, a co-doped raw material supply subunit and a rare earth halide raw material supply subunit, the co-doped raw material supply subunit comprises a high-temperature evaporation tank, and the rare earth halide raw material supply subunit comprises a high-temperature evaporation cavity; the gas phase transmission unit comprises a high-temperature conveying pipe, a first conveying pipe, a second conveying pipe and a third conveying pipe, at least one high-temperature evaporation cavity is arranged in the liner pipe and close to the PCVD furnace, and the first conveying pipe penetrates through the high-temperature conveying pipe and the high-temperature evaporation cavity in sequence and then stretches into the liner pipe. The method adopts the device to prepare the active optical fiber preform. The invention has good sealing performance and expandability, and can realize the preparation of various active special optical fiber preformed bars by using a PCVD method.
Description
Technical Field
The invention relates to the technical field of optical fiber preparation, in particular to a device and a method for preparing an active optical fiber preform by a PCVD method.
Background
The optical fiber preform is an important basic material for manufacturing optical fibers and optical cables, and is a key core technology in the optical fiber production flow. At present, the domestic process for preparing the preform mainly comprises a vapor axial deposition method (VAD), an external vapor deposition method (OVD), a modified chemical external vapor deposition Method (MCVD) and a plasma deposition method (PCVD), wherein the MCVD and the PCVD belong to an in-tube deposition method, and the VAD and the OVD belong to an external deposition method. The external deposition method gets rid of the size limitation of the quartz tube, can prepare a large-size optical fiber preform, has great advantages in manufacturing cost, and has been widely used for manufacturing communication optical fiber preforms. While MCVD and PCVD are in-tube deposition methods, the preform produced is limited in both core and cladding dimensions by the dimensions of the deposited quartz tube, so that the share of applications in the field of large-size, low-cost communication fibers has been gradually reduced in recent years. However, the in-tube method has great advantages in control precision in the field of special optical fibers, in particular to PCVD, which has low single-layer deposition thickness and a plurality of layers and is very suitable for preparing special optical fibers with complex structural design.
In addition, the existing preparation methods of rare earth doped optical fiber perform mainly include a solution method, a gas phase method, a sol-gel method and the like, and among them, a solution doping method and an evolution method thereof are widely adopted. Although the MCVD solution doping technology has the advantages of simple operation, high flexibility and the like, with the continuous rising of other doping technologies and technical optimization, the method for doping rare earth ions in the optical fiber has increasingly shown the limitations, in particular the repeatability is difficult to control and the preparation capability of the large fiber core preform is not provided. The sol-gel method is difficult to control impurities, is always plagued by the problem of higher optical fiber loss, and is not widely applied at present. The rare earth ion gas phase method doping has the gas phase doping consistency with the optical fiber preform base raw material, and greatly improves the doping uniformity, the doping controllability, the interface optimization, the background loss, the optical fiber reliability and the simplification and the repeatability of the preparation process.
At present, most rare earth ion gas phase doping methods are used in combination with MCVD, but according to the report of the current literature, the rare earth doped optical fiber prepared by the MCVD gas phase doping method is still not ideal in loss level due to the limitation of equipment defects, technical level and other factors. On the other hand, the size of the prefabricated rod prepared by the MCVD method is very small, so that the optical fiber drawn by a single prefabricated rod is relatively short, and the batch performance consistency of the rare earth doped optical fiber product is relatively poor. And because the preparation yield of the rare earth doped preform is low and the size of the preform is small, the cost of the rare earth doped optical fiber is high, and the rare earth doped optical fiber is a problem to be solved urgently.
Disclosure of Invention
The invention aims to provide a device and a method for preparing an active optical fiber preform by a PCVD method, which can fully combine the advantages of a good control precision of in-tube deposition and a gas phase doping method by the PCVD method and solve the preparation problem of a large-core-diameter rare earth doped preform and the inherent limitation problem of a solution method.
One aspect of the present invention provides a device for preparing an active optical fiber preform by a PCVD method, comprising a PCVD device and a doping device, wherein the doping device comprises a gasification unit, a gas phase transmission unit and a gas phase deposition unit, and the gas phase deposition unit comprises a liner tube rotatably penetrating into a PCVD furnace of the PCVD device;
the gasification unit comprises a common deposition raw material supply subunit, a co-doped raw material supply subunit and a rare earth halide raw material supply subunit, wherein the co-doped raw material supply subunit comprises a high-temperature evaporation tank arranged outside the liner tube, and the rare earth halide raw material supply subunit comprises at least one high-temperature evaporation cavity arranged inside the liner tube;
the gas phase transmission unit comprises a high-temperature conveying pipe, at least one first conveying pipe connected with a first gas source, a second conveying pipe connected with a common deposition raw material supply subunit and a third conveying pipe connected with a codoped raw material supply subunit, wherein the second conveying pipe and the third conveying pipe penetrate through the high-temperature conveying pipe and then stretch into the liner pipe, the at least one high-temperature evaporation cavity is arranged in the liner pipe and is close to the PCVD furnace, and each first conveying pipe penetrates through the high-temperature conveying pipe and one of the high-temperature evaporation cavities in sequence and then stretches into the liner pipe.
According to one embodiment of the apparatus for preparing an active optical fiber preform by the PCVD method, the high-temperature evaporation cavity is made of pure quartz or ceramic material and is arranged at a position 10mm to 100mm away from the PCVD furnace, the high-temperature heating furnace is arranged outside the liner tube at the position of the high-temperature evaporation cavity, and the temperature control range of the high-temperature heating furnace is 50-1000 ℃, and the temperature control precision is +/-1 ℃.
According to one embodiment of the device for preparing the active optical fiber preform by the PCVD method, the cavity of the high-temperature heating furnace is a cylindrical cavity with two open ends and can wrap the liner tube where the high-temperature evaporation cavity is located, and the high-temperature heating furnace is a semi-open heating furnace with the upper part of the furnace body being openable by control or manual operation.
According to one embodiment of the device for preparing the active optical fiber preform by the PCVD method, the external diameter of the high-temperature heating furnace is 300-600 mm, the length of the high-temperature heating furnace is 300-600 mm, the diameter of the cavity is 40-70 mm, and two ends of the liner tube are respectively connected with the fixed structure through rotary sealing.
According to one embodiment of the apparatus for preparing an active optical fiber preform by the PCVD method, the high-temperature evaporation cavity is filled with rare earth halide raw materials, the high-temperature evaporation tank is filled with co-doped raw materials, the high-temperature evaporation tank comprises an evaporation tank and a heater, and the temperature control range of the heater is 50-400 ℃.
According to one embodiment of the apparatus for preparing an active optical fiber preform by a PCVD method, the high temperature conveying pipe comprises an inner heating layer, an outer heat insulation layer and a central conveying cavity, and the first conveying pipe, the second conveying pipe and the third conveying pipe all penetrate through the conveying cavity, wherein the heating temperature of the high temperature conveying pipe is 50-400 ℃, and the appearance temperature of the high temperature conveying pipe after heat insulation is below 70 ℃.
According to one embodiment of the apparatus for preparing an active optical fiber preform by PCVD method of the present invention, the first gas source is helium or chlorine, and the common deposition raw material provided by the common deposition raw material supplying subunit comprises SiCl 4 、GeCl 4 、C 2 F 6 And/or POCl 3 And oxygen or helium as a second gas source, wherein the high-temperature evaporation tank is connected with a third gas source through a pipeline provided with a mass flow controller, and the third gas source is oxygen or helium.
In another aspect, the invention provides a method for preparing an active optical fiber preform by using the device for preparing the active optical fiber preform by using the PCVD method.
An embodiment of a method for preparing an active optical fiber preform by a PCVD method according to the present invention, the method comprises the steps of:
s1: assembling the device and adding predetermined common deposition raw materials, co-dopant raw materials and rare earth halide raw materials into the common deposition raw material supply subunit, the co-dopant raw material supply subunit and the rare earth halide raw material supply subunit respectively;
s2: taking helium as a first gas source to be introduced into the device for gas replacement, drying the rare earth halide raw material in the first gas source to be introduced into the device after the gas replacement is completed, and stopping introducing the gas after the gas replacement is completed;
s3: heating a common deposition raw material supply subunit, a codoped raw material supply subunit and a rare earth halide raw material supply subunit, respectively providing each gas phase raw material into a liner tube, and adjusting PCVD furnace parameters to respectively perform cladding layer and core layer deposition;
s4: and (5) unloading the deposited liner tube after the core layer is deposited, and melting and shrinking to prepare the active optical fiber preform.
Compared with the prior art, the device and the method for preparing the active optical fiber preform by the PCVD method can realize that rare earth ions are directly transmitted to the liner tube through the gas phase and are directly deposited into the fiber core area of the preform by the PCVD method; the single-layer deposition by PCVD is only about 1um, so that the structural design of the complex special optical fiber can be realized; meanwhile, the adopted gas phase method can prepare the fiber core of the large-size prefabricated rod, the preparation cost of the rare earth doped optical fiber prefabricated rod can be greatly reduced, and the drawn optical fiber length is increased due to the fact that the size of a single prefabricated rod is increased, and the performance consistency of rare earth doped optical fiber products is also greatly improved.
Drawings
Fig. 1 is a schematic view showing the overall structure of an apparatus for preparing an active optical fiber preform by a PCVD method according to an exemplary embodiment of the present invention.
Fig. 2 is a schematic cross-sectional view showing a high temperature delivery pipe in an apparatus for preparing an active optical fiber preform by a PCVD method according to an exemplary embodiment of the present invention.
Fig. 3 shows a schematic structure of a high temperature evaporation chamber in an apparatus for preparing an active optical fiber preform by PCVD according to an exemplary embodiment of the present invention.
Fig. 4 is a schematic cross-sectional view showing a high-temperature heating furnace in an apparatus for preparing an active optical fiber preform by a PCVD method according to an exemplary embodiment of the present invention.
Fig. 5a is a schematic view showing a partial structure of two high temperature evaporation chambers included in an apparatus for PCVD manufacturing an active optical fiber preform according to another exemplary embodiment of the present invention, and fig. 5b is a schematic view showing a cross-sectional structure of a high temperature delivery pipe including two high temperature evaporation chambers included in an apparatus for PCVD manufacturing an active optical fiber preform according to another exemplary embodiment of the present invention.
Reference numerals illustrate:
1-PCVD stove, 2-resonator, 3-magnetron, 4-high temperature heating furnace, 5, 25, 26-high temperature evaporation chamber, 6-bushing pipe, 7-high temperature conveying pipe, 8-high temperature evaporation jar, 9-evaporation jar, 10-second conveying pipe, 11-first conveying pipe, 12-third conveying pipe, 21, 22, 23, 24-conveying pipe, 13-first rotary seal, 14-vacuum pump interface, 15-second rotary seal, 16-mass flow controller, 17-zone of heating, 18-zone of heating, 19-upper portion of high temperature heating furnace, 20-lower portion of high temperature heating furnace.
Detailed Description
All of the features disclosed in this specification, or all of the steps in a method or process disclosed, may be combined in any combination, except for mutually exclusive features and/or steps.
Any feature disclosed in this specification may be replaced by alternative features serving the same or equivalent purpose, unless expressly stated otherwise. That is, each feature is one example only of a generic series of equivalent or similar features, unless expressly stated otherwise.
Fig. 1 is a schematic view showing the overall structure of an apparatus for preparing an active optical fiber preform by a PCVD method according to an exemplary embodiment of the present invention.
As shown in fig. 1, the apparatus for preparing an active optical fiber preform by a PCVD method according to an exemplary embodiment of the present invention includes a PCVD apparatus and a doping apparatus, wherein the PCVD apparatus may perform heating and vapor deposition operations of a liner using existing related apparatuses, for example, components including a PCVD furnace 1, a resonator 2, a magnetron 3, etc.; the doping device is matched with the PCVD device to provide gas phase raw materials and meet the related requirements of the PCVD method, so that the active optical fiber preform is prepared.
The doping apparatus of the present invention comprises a gasification unit, a gas phase transport unit and a gas phase deposition unit comprising a liner 6 rotatably arranged in a PCVD furnace of the PCVD apparatus, the liner 6 preferably being a quartz glass liner.
The gasification unit comprising a device for providing a gas such as SiCl 4 A common deposition material supply subunit (not shown) for supplying common deposition materials such as AlCl 3 A co-dopant raw material supply subunit of the co-dopant and a rare earth halide raw material supply subunit for providing rare earth halides. Specifically, the co-dopant feedstock supply sub-unit comprises a high temperature evaporation tank 8 disposed outside the liner 6, the rare earth halide feedstock supply sub-unit comprises at least one high temperature evaporation chamber 5 disposed inside the liner 6, the high temperature evaporation chamber 5 providing a gaseous phase of rare earth halide, and the high temperature evaporation tank 8 providing a gaseous phase of co-dopant.
The gas phase transmission unit of the invention comprises a high temperature transmission pipe 7, at least one first transmission pipe 11 connected with a first gas source, a second transmission pipe 10 connected with a common deposition raw material supply subunit and a third transmission pipe 12 connected with a co-doped raw material supply subunit, wherein the second transmission pipe 10 and the third transmission pipe 12 penetrate through the high temperature transmission pipe 7 and then extend into the liner pipe 6. Wherein, at least one high temperature evaporation cavity 5 is arranged in the liner tube 6 near the PCVD furnace 1, and each first conveying pipe 11 sequentially passes through the high temperature conveying pipe 7 and one high temperature evaporation cavity 5 and then stretches into the liner tube 6.
Fig. 2 is a schematic cross-sectional view showing a high temperature delivery pipe in an apparatus for preparing an active optical fiber preform by a PCVD method according to an exemplary embodiment of the present invention. As shown in fig. 2, the high temperature transfer tube 7 comprises an inner heating layer 17, an outer insulating layer 18 and a central transfer chamber through which the first transfer tube 11, the second transfer tube 10 and the third transfer tube 12 all pass. Wherein the heating temperature of the high-temperature conveying pipe is 50-400 ℃, the appearance temperature of the high-temperature conveying pipe after heat insulation is below 70 ℃, and the state stability of the gas phase raw materials in each conveying pipe can be ensured through the heating action of the high-temperature conveying pipe.
Fig. 3 shows a schematic structure of a high temperature evaporation chamber in an apparatus for preparing an active optical fiber preform by PCVD according to an exemplary embodiment of the present invention. As shown in fig. 3, the high-temperature evaporation cavity 5 is arranged in the liner tube near the PCVD furnace for doping rare earth halide with high melting point, and the high-temperature evaporation tank 8 arranged outside the liner tube is used for doping co-dopant with lower melting point temperature, so that the doping device and the gas end of the PCVD can be in sealing connection with the gas end in a rotating sealing way at a lower temperature, and the severe sealing environment requirement of the PCVD can be easily met.
Wherein, the high temperature evaporation cavity 5 contains rare earth halide raw material, the high temperature evaporation tank 8 contains co-doped raw material, the high temperature evaporation tank 8 comprises an evaporation tank 7 and a heater, and the temperature control range of the heater is 50-400 ℃.
Preferably, the high temperature evaporation chamber 5 is made of pure quartz or ceramic material and is arranged at a position 10mm to 100mm away from the PCVD furnace, the high temperature heating furnace 4 is arranged outside the liner tube where the high temperature evaporation chamber 5 is arranged, the temperature control range of the high temperature heating furnace is 50-1000 ℃, the temperature control precision is +/-1 ℃, and the high temperature heating furnace is used for heating the high temperature evaporation chamber and the rare earth halide therein so as to provide gas phase rare earth halide into the liner tube. In addition, two or more high-temperature evaporation chambers 5 can be designed according to the actual requirement, and one or more high-temperature evaporation chambers are only required to be added in the liner tube at the corresponding position of the high-temperature heating furnace, and one or more conveying pipelines and one or more carrier gas controls are added in the high-temperature conveying pipe.
Fig. 4 is a schematic cross-sectional view showing a high-temperature heating furnace in an apparatus for preparing an active optical fiber preform by a PCVD method according to an exemplary embodiment of the present invention. As shown in fig. 4, the cavity of the high-temperature heating furnace 4 is a cylindrical cavity with two open ends and can wrap a liner tube at the position of the high-temperature evaporation cavity, the high-temperature heating furnace is a semi-open heating furnace with the upper part of the furnace body being openable by control or manual operation, for example, the high-temperature heating furnace comprises an upper part 19 and a lower part 20, and the high-temperature evaporation cavity and rare earth halide therein can be rapidly cooled after the furnace body is opened. Preferably, the outer diameter of the high-temperature heating furnace 4 is 300-600 mm, the length is 300-600 mm, and the cavity diameter is 40-70 mm; two ends of the liner tube 6 are respectively connected with a fixed structure through rotary seals, for example, one end of the liner tube 6 is connected with a high-temperature conveying pipe through a first rotary seal 15, the other end of the liner tube is connected with the tail end of a lathe through a second rotary seal 13, and a vacuum pump interface 14 is further arranged at the connection part of the liner tube and the tail end of the lathe so as to realize vacuumizing treatment in the liner tube.
The first air source is helium or chlorine, and can be used for purging, drying or carrying rare earth halide; the common deposition raw material supplied from the common deposition raw material supply subunit comprises SiCl 4 、GeCl 4 、C 2 F 6 And/or POCl 3 And oxygen or helium as a second gas source, the second gas source being primarily used for carrying common deposition materials; the high temperature evaporation tank 8 is connected to a third gas source, which is oxygen or helium and is a carrier tape for the co-blend, by a line provided with a mass flow controller 16.
Fig. 5a is a schematic view showing a partial structure of two high temperature evaporation chambers included in an apparatus for PCVD manufacturing an active optical fiber preform according to another exemplary embodiment of the present invention, and fig. 5b is a schematic view showing a cross-sectional structure of a high temperature delivery pipe including two high temperature evaporation chambers included in an apparatus for PCVD manufacturing an active optical fiber preform according to another exemplary embodiment of the present invention.
As shown in fig. 5a and 5b, according to another embodiment of the present invention, two high temperature evaporation chambers 25, 26 are provided in the apparatus to achieve doping of two rare earth halides, two first delivery pipes connected to a first gas source are provided respectively and pass through the high temperature delivery pipe 7 and the high temperature evaporation chambers 25, 26 respectively in succession; four conveying pipes 21, 22, 23 and 24, namely two first conveying pipes, one second conveying pipe and one third conveying pipe, are arranged in the high-temperature conveying pipe 7 at the moment, and all penetrate through the conveying cavities of the high-temperature conveying pipes. Of course, the invention can also be provided with a plurality of high-temperature evaporation cavities according to the requirement.
The invention also provides a method for preparing the active optical fiber preform by adopting the device for preparing the active optical fiber preform by adopting the PCVD method, which comprises the following steps.
Step S1:
the apparatus is assembled and predetermined common deposition raw materials, co-dopant raw materials, and rare earth halide raw materials are added to the common deposition raw material supply subunit, the co-dopant raw material supply subunit, and the rare earth halide raw material supply subunit, respectively. Specifically, the raw materials are selected according to the doping preform to be prepared.
Step S2:
and (3) taking helium as a first gas source to be introduced into the device for gas replacement, taking chlorine as the first gas source to be introduced into the device for drying the rare earth halide raw material after the gas replacement is completed, and stopping introducing the gas after the gas replacement is completed. The purpose of purging and drying is to ensure the purity of the raw materials and to ensure the quality of the product produced by deposition.
Step S3:
and heating the common deposition raw material supply subunit, the codoped raw material supply subunit and the rare earth halide raw material supply subunit, respectively providing each gas phase raw material into the liner tube, and respectively performing cladding layer and core layer deposition by adjusting PCVD furnace parameters. Wherein heating is required to heat to above the melting point of the feedstock to form a gas phase feedstock; the control parameters of the PCVD furnace include temperature, pressure, microwave power, etc.
Step S4:
and (5) unloading the deposited liner tube after the core layer is deposited, and melting and shrinking to prepare the active optical fiber preform.
After the core layer is deposited, the microwave power is immediately turned off, the high-temperature heating furnace 4 is turned off, and the upper part 19 of the furnace body is opened, so that the rare earth halide is rapidly cooled and condensed in the high-temperature evaporation cavity. And unloading the deposited lining pipe and fusing in a lathe to obtain the solid active optical fiber preform.
The invention will be further illustrated with reference to specific examples.
Example 1: preparation of rare earth Yb doped prefabricated rod
The basic PCVD apparatus is prepared and put in a state to be operated, and the doping apparatus is prepared and put in a state to be operated.
Weighing rare earth halide YbCl 3 35 g and anhydrous AlCl 3 150 g, ybCl 3 Added to the high temperature evaporation chamber 5 to remove AlCl 3 Added to the evaporation tank 9, the high temperature evaporation chamber 5 and the evaporation tank 9 were purged with He 200sccm (standard milliliters per minute) and 500sccm, respectively, and gas substitution was completed. Reuse of Cl 2 YbCl in 100sccm to high temperature evaporation chamber 5 3 Drying for half an hourStopping the Cl feeding after completion 2 . The high-temperature heating furnace 4 corresponding to the high-temperature evaporation cavity 5 is heated to 820 ℃, and the heater corresponding to the evaporation tank 9 is heated to 155 ℃.
A high-purity quartz glass tube with an outer diameter of 36mm, an inner diameter of 30mm and a length of 2m is used as a liner tube, the temperature of the PCVD furnace 1 is set to 1050 ℃, the pressure in the tube is set to 20bar, the high-frequency power is controlled to be constant at 5000W, and the deposition of the cladding layer and the core layer is respectively carried out.
Wherein, the cladding deposition parameters are as follows: siCl is introduced into the reactor 4 Flow 600sccm, POCl 3 Flow 10sccm, C 2 F 6 Flow 5sccm, O 2 Flow rate: 2000sccm. The core deposition parameters were as follows: siCl is introduced into the reactor 4 Flow 300sccm, C 2 F 6 Flow 200sccm, O 2 Flow rate: 2000sccm, ybCl 3 Flow rate (carrier gas He): 260sccm, alCl 3 Flow rate: 240sccm.
After the core layer is deposited, immediately turning off microwave power, turning off the high-temperature heating furnace 4 and opening the upper part 19 of the furnace body to enable YbCl to be generated 3 Rapidly cooling and condensing in the cavity. And unloading the deposited quartz tube, and smelting and shrinking in a rod forming lathe to prepare the solid rare earth Yb doped prefabricated rod.
Example 2: preparation of Er-Yb co-doped optical fiber preform
In the embodiment, erCl which is a raw material for doping Er-Yb co-doped preform is needed 3 And codoped YbCl 3 、AlCl 3 And POCl 3 Basic material SiCl 4 Therein ErC l3 、YbCl 3 And AlCl 3 High temperature volatilization devices are required. According to the invention, two high temperature evaporation chambers 25, 26 are required, and the schematic structure is shown in fig. 5 a.
The basic PCVD apparatus is prepared and put in a state to be operated, and the doping apparatus is prepared and put in a state to be operated.
Weighing rare earth halides ErC 3 7 g, ybCl 3 35 g and anhydrous AlCl 3 150 g, erCl 3 、YbCl 3 And AlCl 3 Added to the high temperature evaporation chambers 26, 25 and the evaporation tank 9, respectively, gas substitution was performed using He. Is reused after completionCl 2 YbCl in 100sccm vs. high temperature evaporation chamber 25, 26 3 、ErCl 3 Drying for half an hour, stopping introducing Cl after completion 2 . The high temperature heating furnace 4 corresponding to the high temperature evaporation chambers 25 and 26 is heated to 790 ℃, and the heater corresponding to the evaporation tank 9 is heated to 155 ℃.
A high-purity quartz tube with the outer diameter of 36mm, the inner diameter of 30mm and the length of 2m is used as a liner tube, the temperature of the PCVD furnace 1 is set to 1050 ℃, the pressure in the tube is 20bar, the high-frequency power is controlled to be constant at 5000W, and the deposition of a cladding layer and a core layer is respectively carried out.
Wherein, the cladding deposition parameters are as follows: siCl is introduced into the reactor 4 Flow 300sccm, POCl 3 Flow 12.5sccm, C 2 F 6 The flow rate was 3.5sccm. O (O) 2 Flow rate: 3500sccm. The core deposition parameters were as follows: siCl is introduced into the reactor 4 Flow 300sccm, POCl 3 Flow 115sccm, O 2 Flow rate: 2000sccm, erCl3 flow (carrier gas He): 25sccm, ybCl 3 Flow rate (carrier gas He): 175ccm, alCl 3 Flow rate: 180sccm.
After the core layer is deposited, the microwave power is immediately turned off, the high-temperature heating furnace 4 is turned off, and the upper part 19 of the furnace body is turned on, so that ErCl is obtained 3 、YbCl 3 Rapidly cooling and condensing in the cavity. And unloading the deposited quartz tube, and carrying out fusion shrinkage on the quartz tube in a rod forming lathe to prepare the solid Er-Yb doped prefabricated rod.
The invention is not limited to the specific embodiments described above. The invention extends to any novel one, or any novel combination, of the features disclosed in this specification, as well as to any novel one, or any novel combination, of the steps of the method or process disclosed.
Claims (7)
1. The device for preparing the active optical fiber preform by the PCVD method is characterized by comprising a PCVD device and a doping device, wherein the doping device comprises a gasification unit, a gas phase transmission unit and a gas phase deposition unit, and the gas phase deposition unit comprises a liner tube which is rotatably arranged in a PCVD furnace of the PCVD device in a penetrating way;
the gasification unit comprises a common deposition raw material supply subunit, a co-doped raw material supply subunit and a rare earth halide raw material supply subunit, wherein the co-doped raw material supply subunit comprises a high-temperature evaporation tank arranged outside the liner tube, and the rare earth halide raw material supply subunit comprises at least one high-temperature evaporation cavity arranged inside the liner tube;
the gas phase transmission unit comprises a high-temperature conveying pipe, at least one first conveying pipe connected with a first gas source, a second conveying pipe connected with a common deposition raw material supply subunit and a third conveying pipe connected with a codoped raw material supply subunit, wherein the second conveying pipe and the third conveying pipe penetrate through the high-temperature conveying pipe and then stretch into the liner pipe, the at least one high-temperature evaporation cavity is arranged in the liner pipe (6) close to the PCVD furnace, and each first conveying pipe penetrates through the high-temperature conveying pipe and one of the high-temperature evaporation cavities and then stretches into the liner pipe;
the high-temperature evaporation cavity is made of pure quartz or ceramic materials and is arranged at a position 10mm to 100mm away from the PCVD furnace, a high-temperature heating furnace is arranged outside the liner tube at the position of the high-temperature evaporation cavity, the temperature control range of the high-temperature heating furnace is 790-1000 ℃, and the temperature control precision is +/-1 ℃;
the high-temperature evaporation cavity is filled with rare earth halide raw materials, the high-temperature evaporation tank is filled with co-doped raw materials, and comprises an evaporation tank and a heater, wherein the temperature control range of the heater is 50-400 ℃.
2. The apparatus for preparing an active optical fiber preform by a PCVD method according to claim 1, wherein the cavity of the high temperature heating furnace is a cylindrical cavity with both ends open and can wrap a liner tube where the high temperature evaporation cavity is located, and the high temperature heating furnace is a semi-open heating furnace with an upper part of a furnace body being opened by control or manual operation.
3. The apparatus for preparing an active optical fiber preform by a PCVD method according to claim 1, wherein the outer diameter of the high temperature heating furnace (4) is 300mm to 600mm, the length is 300mm to 600mm, the diameter of the cavity is 40mm to 70mm, and both ends of the liner tube are respectively connected with the fixed structure by rotary sealing.
4. The apparatus for preparing an active optical fiber preform by a PCVD method according to claim 1, wherein the high temperature delivery pipe comprises a heating layer of an inner layer, a heat insulation layer of an outer layer, and a central delivery chamber, through which the first delivery pipe, the second delivery pipe, and the third delivery pipe all pass, wherein a heating temperature of the high temperature delivery pipe is 50 to 400 ℃ and an external temperature of the high temperature delivery pipe after heat insulation is below 70 ℃.
5. The apparatus for preparing an active optical fiber preform by a PCVD method according to claim 1, wherein the first gas source is helium or chlorine, and the common deposition raw material supplied from the common deposition raw material supplying subunit comprises SiCl 4 、GeCl 4 、C 2 F 6 And/or POCl 3 And oxygen or helium as a second gas source, wherein the high-temperature evaporation tank is connected with a third gas source through a pipeline provided with a mass flow controller, and the third gas source is oxygen or helium.
6. A method for preparing an active optical fiber preform by a PCVD method, characterized in that the preparation of the active optical fiber preform is performed by using the apparatus for preparing an active optical fiber preform according to any one of claims 1 to 5.
7. The method for preparing an active optical fiber preform by the PCVD method according to claim 6, comprising the steps of:
s1: assembling the device and adding predetermined common deposition raw materials, co-dopant raw materials and rare earth halide raw materials into the common deposition raw material supply subunit, the co-dopant raw material supply subunit and the rare earth halide raw material supply subunit respectively;
s2: taking helium as a first gas source to be introduced into the device for gas replacement, drying the rare earth halide raw material in the first gas source to be introduced into the device after the gas replacement is completed, and stopping introducing the gas after the gas replacement is completed;
s3: heating a common deposition raw material supply subunit, a codoped raw material supply subunit and a rare earth halide raw material supply subunit, respectively providing each gas phase raw material into a liner tube, and adjusting PCVD furnace parameters to respectively perform cladding layer and core layer deposition;
s4: and (5) unloading the deposited liner tube after the core layer is deposited, and melting and shrinking to prepare the active optical fiber preform.
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