CN112299703B - Doping solution spraying device and spraying method - Google Patents
Doping solution spraying device and spraying method Download PDFInfo
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- CN112299703B CN112299703B CN202011269166.5A CN202011269166A CN112299703B CN 112299703 B CN112299703 B CN 112299703B CN 202011269166 A CN202011269166 A CN 202011269166A CN 112299703 B CN112299703 B CN 112299703B
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- 238000005507 spraying Methods 0.000 title claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 86
- 239000010453 quartz Substances 0.000 claims abstract description 67
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 67
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- 238000003860 storage Methods 0.000 claims abstract description 12
- 230000001105 regulatory effect Effects 0.000 claims abstract description 6
- 238000004364 calculation method Methods 0.000 claims abstract description 3
- 239000010410 layer Substances 0.000 claims description 37
- 150000002500 ions Chemical class 0.000 claims description 31
- 230000008021 deposition Effects 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- 238000002955 isolation Methods 0.000 claims description 7
- 230000015654 memory Effects 0.000 claims description 7
- 239000012792 core layer Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000013307 optical fiber Substances 0.000 abstract description 17
- 230000001276 controlling effect Effects 0.000 abstract description 3
- 238000012797 qualification Methods 0.000 abstract description 2
- -1 rare earth ions Chemical class 0.000 description 15
- 238000000034 method Methods 0.000 description 9
- 238000000151 deposition Methods 0.000 description 8
- 229910052769 Ytterbium Inorganic materials 0.000 description 7
- 229910052761 rare earth metal Inorganic materials 0.000 description 7
- 239000000835 fiber Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 150000004697 chelate complex Chemical class 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000003028 elevating effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General 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 provides a doping solution spraying device and a spraying method, wherein the doping solution spraying device comprises a solution storage, a guide pipe, a sprayer, a hard hollow pipe, a quartz reaction pipe, an electric lifting table, a guide rail, a speed sensor, a nitrogen conveying pipe with a pressure regulating valve and a supporting seat, one end of the hollow pipe is connected with a solution storage, the other end of the hollow pipe is connected with the solution spraying device, the solution storage is used for controlling the pressure of a solution, uniformly conveying the solution, the feeding speed is controlled by controlling the conveying nitrogen, the ion solution flows out through the hard hollow pipe 4 and enters the sprayer to be sprayed out, the speed sensor is received in real time, the position information of the sprayer is obtained through calculation, and the ion solution is sprayed into the quartz reaction pipe for a plurality of times through the reciprocating movement of the electric lifting table. The ion solution doping device has the advantages of simple structure, convenient operation and strong controllability, and can be used for doping various ion solutions with different concentrations. The qualification rate and the optical fiber loss of the optical fiber are improved, the beam quality of the optical fiber laser is improved, and the use requirements in all aspects are met.
Description
Technical Field
The invention relates to an optical fiber preform preparation device, in particular to a doping solution spraying device and a spraying method.
Background
With the development of laser technology, the laser is widely applied to military and civil fields, and meanwhile, the requirements on the laser are higher and higher, and the laser has high quality, high power and high efficiency, which are important criteria for judging the quality of the laser. In recent years, a laser fiber laser doped with rare earth ions has been paid attention to gradually because of the advantages of good beam quality, small volume, high speed, long service life and the like. And has been widely used in various fields such as laser welding, medical field, laser communication, etc.
The core part of the laser fiber laser is the rare earth ion doped fiber, the rare earth ion doped fiber preform is the necessary part for drawing the rare earth ion doped fiber, and the rare earth ion doped doping process is divided into two main types, namely a liquid phase doping method and a gas phase doping method. The liquid phase doping method is to soak the loose layer with ion solution to make the ions in the ion solution absorbed by the loose layer, so as to achieve the purpose of doping rare earth ions. The liquid phase doping method is easy to generate the phenomena of uneven doping concentration, falling off of the isolation layer and the like, and the solution soaking process flow is complex. The gaseous reactant is used to directly produce RE ion compound in quartz reaction tube to reach the aim of doping. However, since the chelate complex itself contains carbon element, carbon deposition is liable to occur, and the loss of the optical fiber becomes high. And the gas phase doping method can condense the gaseous reactants into solid state due to the slight reduction of the temperature due to the saturated gaseous reactants, do not participate in the reaction, and easily block the pipeline.
Disclosure of Invention
In view of the problems of the prior art, the invention provides a doping solution spraying device and a doping solution spraying method. By adopting the telescopic ion solution spraying mode, the problems of uneven ion concentration and easy falling of loose layers are solved, so that the purposes of improving the optical fiber absorption uniformity, reducing the optical fiber loss and improving the light beam quality and the optical fiber service life of the optical fiber laser are achieved. The specific technical scheme is, a doping solution sprinkler, including solution memory, pipe, sprinkler, stereoplasm hollow tube, quartz reaction tube, electric lift platform, guide rail, speed sensor, take nitrogen gas conveyer pipe and the supporting seat of pressure regulating valve, its characterized in that: the sprayer is of a telescopic structure with a plurality of layers of cylinders with round cavities, the cylinder at the uppermost layer is provided with a vertical pipe with the same layer number, the vertical pipe is matched with the soft pipe of the pipe, the cylinder at each layer is provided with a non-concentric round through hole, the vertical pipe is respectively communicated with the cylinder at the uppermost layer, the outer side face of the round cavity of each layer of cylinder comprises at least three radial thin through holes which are uniformly distributed along the circumferential surface, the solution memories are fixed on the upper end face of the supporting seat, a nitrogen conveying pipe with a pressure regulating valve is fixed above the liquid level of the solution memories, the inner diameter of the pipe is 17-18mm, the pipe with a plurality of hollow soft pipes in the pipe is respectively extended out of the two ends of the pipe, one end of each soft pipe is respectively arranged at the bottom of the liquid level of each solution memory, the other end of each soft pipe is respectively connected with the vertical pipe of the sprayer, the sprayer is fixed on the hard hollow pipe, one end of the hard hollow pipe with the sprayer is inserted into a quartz reaction pipe, the other end of each hard hollow pipe is fixed in the pipe, the quartz reaction pipe has the inner diameter of 20mm-25mm, the reaction part at the upper end, the reaction part is composed of a supporting part and the lower end reaction part, the length of the reaction part is 600+/-10 mm, and the length of the supporting part is 500+/-10 mm; the electric lifting platform is vertically fixed on the chuck of the side end face of the supporting seat, the sprayer is positioned at the upper end of the supporting part of the quartz reaction tube and is at the initial position of the sprayer, the electric lifting platform is arranged in the guide rail, the guide rail direction is the same as the direction of the quartz reaction tube, the hard hollow tube is fixed on the electric lifting platform in an interference fit manner, and the speed sensor is fixed on the electric lifting platform.
The outer diameter of the sprayer is 20-21mm, and the length of the sprayer is 25-30 mm; the inner diameter of the round cavity is 18-19mm, and the height is 10-11mm.
The loose layer is deposited in the quartz reaction tube, so that the inner diameter of the reaction part of the quartz reaction tube is 20-mm-25 mm, and the curvature of the support part of the quartz reaction tube after the loose layer is deposited is small, so that the rigid hollow tube and the sprayer enter the reaction part of the quartz reaction tube.
The spraying method comprises (a) adopting a quartz tube as a quartz reaction tube for deposition, and depositing an isolation layer on the inner wall of the quartz reaction tube for preventing impurity ions in the quartz reaction tube from entering the core layer; secondly, depositing a loose layer in a reaction part of the quartz reaction tube deposited with the isolation layer, wherein the loose layer is an unsintered, opaque and porous deposition layer used for adsorbing solute ions in a solution, the inner diameter of the reaction part of the quartz reaction tube is 20-mm-25 mm after the loose layer is deposited in the quartz reaction tube, and the curvature of the support part of the quartz reaction tube after the loose layer is deposited is small, so that the rigid hollow tube and the sprayer enter the reaction part of the quartz reaction tube; thirdly, fixing the supporting part of the quartz reaction tube on a chuck of a supporting seat, connecting one end of a hard hollow tube fixed on an electric lifting table with a sprayer, inserting the sprayer into the initial position of the sprayer at the uppermost end of the reaction part of the quartz reaction tube, fixing the other end of the hard hollow tube on a guide tube, and cleaning the hard hollow tube and the sprayer by deionized water before using; starting an electric lifting table, wherein the electric lifting table drives a sprayer at the lower end of a rigid hollow pipe to axially move into a designated position of a quartz reaction pipe, a speed sensor on the electric lifting table receives position information of the sprayer in real time, the stepping speed range of the sprayer is controlled to be 1-10 mm/s, a nitrogen inlet switch is simultaneously opened, a plurality of hose pipeline switches in an ion solution storage are opened, the flow rate of ion solution is controlled to be 3ml/s, ytterbium ion solution enters a guide pipe through a hose and is respectively connected with a circular cavity of the sprayer, the ytterbium ion solution is sprayed out through radial fine holes of the sprayer, and the flow rate range of the ion solution sprayed to the quartz reaction pipe by the sprayer is controlled to be 1-6 ml/s; (V) when the ytterbium ion solution spraying reaches the designated quantity, closing a pipeline switch between a hose of the ion solution storage and the guide pipe, closing a nitrogen inlet pressure valve, stopping spraying the ion solution by the sprayer, and enabling the electric lifting table to drive the hard hollow pipe and the sprayer to do reverse axial movement until the sprayer returns to the initial position, and closing the electric lifting table; sixthly, after the ion solution is injected, a small amount of liquid remains in the hose and the sprayer, and the hose and the sprayer are purged and cleaned up to avoid polluting or blocking a pipeline; and (seventh), loosening the chuck of the supporting seat, taking down the quartz reaction tube, mounting the quartz reaction tube on a rod making lathe, standing, drying and finishing doping the ion solution.
The invention has the advantage that ion solution doping with different varieties and different concentrations can be carried out. The method solves the problem that the concentration of the ion solution is uneven when the preform is soaked in the traditional method, and further improves the qualification rate of the optical fiber, thereby reducing the loss of the optical fiber and improving the beam quality of the optical fiber laser. And the solution flow rate or the sprinkler stepping speed can be controlled so as to control the doping ion concentration of the optical fiber preform, thereby meeting the use requirements in various aspects.
Description of the drawings:
FIG. 1 is a schematic perspective view of the structure of the present invention;
FIG. 2 is a schematic perspective view of the sprinkler structure of the present invention;
fig. 3 is a cross-sectional view of the sprinkler A-A of the present invention.
The specific embodiment is as follows:
the invention is further described below with reference to the drawings and examples.
Example 1
The ytterbium-doped optical fiber preform is manufactured in a relatively common mode.
As shown in fig. 1, 2 and 3, the ytterbium-doped optical fiber preform is manufactured in a relatively common manner. The thickness of the inner wall of the selected quartz reaction tube 6 is about 23mm, the length of the reaction part 6-2 is about 600mm, and the length of the support part 6-1 is about 500 mm. The length of the selected hard hollow tube 4 is about 1150mm, the outer diameter is about 4.5 and mm, the hard hollow tube can be made of materials with elasticity and rigidity such as fluoroplastic, the inner diameter is about 3.5mm, the outer diameter of the sprinkler 3 is about 20.5mm, the inner diameter is about 19mm, the height is 25mm, the inner diameter of the round cavity 3-1 is 18mm and the height is 10mm, six radial thin through holes 3-2 uniformly distributed along the circumference are arranged on the side surface of each cavity, the outer diameter of the guide tube 2 is 18.5mm, the length requirement is related to the placement position of an actual instrument, and the phenomenon that the hard hollow tube 4 is not folded is ensured.
The solution storages 1 are fixed on the upper end face of the supporting seat 11, a nitrogen delivery pipe 10 with a pressure regulating valve is fixed above the liquid level of each solution storage 1, the inner diameter of the guide pipe 2 is 17-18mm, the inner part of the guide pipe is provided with a plurality of hollow soft guide pipes 2-1, the soft guide pipes 2-1 extend out of the two ends of the guide pipe 2 respectively, one ends of the soft guide pipes 2-1 are respectively arranged at the bottom of the liquid level of each solution storage 1, the other ends of the soft guide pipes are respectively connected with the vertical pipes 3-3 of each layer of round cavity 3-1 of the spraying 3, the spraying device 3 is fixed on the hard hollow pipe 4, one end of the hard hollow pipe 4 with the spraying device 3 is inserted into the quartz reaction pipe 6, the other end of the hard hollow pipe 4 with the spraying device 3 is fixed in the guide pipe 2, the supporting part 6-1 of the quartz reaction pipe 6 is vertically fixed on the chuck 11-1 on the side end face of the supporting seat 11, the spraying device 3 is positioned at the upper end of the supporting part 6-1 of the quartz reaction pipe 6, the electric lifting table 7 is the initial position of the spraying device 3, the electric lifting table 7 is arranged in the guide rail 8, the direction of the electric lifting table is the same as the direction of the quartz reaction pipe 6, the hard hollow pipe 4 is fixed on the electric lifting table 7 in an interference fit, and the electric lifting table 7 is fixed on the electric lifting table 9.
The spraying steps are as follows:
a quartz tube is used as a quartz reaction tube 6 for deposition, and an isolation layer is deposited on the inner wall of the quartz reaction tube 6 for preventing impurity ions in the quartz reaction tube 6 from entering the core layer.
Secondly, loose layer deposition is carried out on the reaction part 6-2 of the quartz reaction tube 6 deposited with the isolation layer, and the loose layer is an unsintered, opaque and porous deposition layer for adsorbing solute ions in the solution;
(III) fixing the support part 6-1 of the quartz reaction tube 6 on the chuck 11-1 of the support base 11, inserting a rigid hollow tube 4 fixed on the electric elevating table 7 with one end of the rigid hollow tube 4 connected with the sprinkler 3 into the initial position of the sprinkler 3 at the uppermost end of the reaction part 6-2 of the quartz reaction tube 6, fixing the other end of the rigid hollow tube 4 on the guide tube 2,
fourthly, starting the electric lifting table 7, wherein the electric lifting table 7 drives the sprayer 3 at the lower end of the hard hollow tube 4 to axially move into the designated position of the quartz reaction tube 6, the stepping speed is 3mm/s, simultaneously, the nitrogen inlet switch is turned on, a hose pipeline switch in the ytterbium ion solution storage 1 is turned on, the flow rate of ytterbium ion solution is controlled to be 3ml/s, the ytterbium ion solution enters the guide tube 2 through the bottom extending hose 2-1, and the radial thin through hole 3-2 of the sprayer 3 reaching the top is sprayed out.
(V), when the ytterbium ion solution is sprayed to reach the designated quantity, closing a pipeline switch between the ion solution reservoir and the hose 2-1 of the conduit 2, closing a nitrogen inlet pressure valve, stopping spraying the ion solution by the sprayer 3, driving the hard hollow tube 4 and the sprayer 3 to do reverse axial movement by the electric lifting table until the sprayer 3 returns to the initial position, and closing the electric lifting table 7;
sixthly, after the ion solution is injected, a small amount of liquid remains in the hose 2-1 and the sprayer 3, and the hose 2-1 and the sprayer 3 are purged and cleaned up to avoid pollution or blockage of a pipeline;
and (seventh), loosening the chuck 11-1 of the supporting seat 11, taking down the quartz reaction tube 6, mounting the quartz reaction tube on a rod making lathe, standing, drying and finishing the doping of the ion solution.
Principle of operation
The electric lifting table 7 is in interference fit with the connection of the guide pipe 2, the electric lifting table 7 is provided with a motor driving device, and the motor driving device drives the electric lifting table 7 to move up and down on the guide rail 8 along the vertical direction to enter or leave the quartz reaction tube 6. The baffle is made in the horizontal direction so that the electric lifting table 7 does not move in any horizontal direction. And meanwhile, the speed sensor on the electric lifting table is received in real time, and the position information of the sprayer 3 is obtained through calculation.
The feeding speed of the ionic solution is controlled by controlling the nitrogen to be conveyed, the liquid level of the ionic solution is low under the action of pressure, and the nitrogen solution flows out through the hard hollow tube 4 and enters a sprayer to be sprayed out.
The manufacturing process of the optical fiber preform doped with other rare earth ions and the optical fiber preform doped with other kinds of co-ions can refer to the embodiment, and corresponding devices such as an ion solution conveying pipeline, a gas valve, a flowmeter and the like are required to be added, and other operations are the same as those of the first embodiment.
Claims (4)
1. The utility model provides a doping solution sprinkler, includes solution storage (1), pipe (2), sprinkler (3), stereoplasm hollow tube (4), quartz reaction tube (6), electric lift platform (7), guide rail (8), speed sensor (9), take nitrogen gas conveyer pipe (10) and supporting seat (11) of pressure regulating valve, its characterized in that: the sprayer (3) is of a telescopic structure of a cylinder with a round cavity (3-1) in a multilayer manner, the uppermost cylinder (3-4) is provided with a vertical pipe (3-3) with the same layer number, the vertical pipe is matched with a hose (2-1) of a conduit (2), each layer of cylinder is provided with a pipe with a plurality of non-concentric round cavities (3-1) in which the vertical pipe (3-3) is respectively communicated with the uppermost cylinder, the outer side of the round cavity (3-1) of each layer of cylinder (3-4) is provided with a plurality of radial fine through holes (3-2) with the number not less than three, the radial fine through holes are uniformly distributed along the circumference, a plurality of solution memories (1) are fixed on the upper end face of a supporting seat (11), a nitrogen conveying pipe (10) with a pressure regulating valve is fixed above the liquid level of the plurality of the solution memories (1), the inner diameter of the conduit (2) is 17-18mm, the hoses with a plurality of hollow hoses (2-1) respectively extend out of two ends of the conduit (2), one end of each hose (2-1) is respectively placed at the bottom of each liquid level memory (1) and the other end of each hose (2-1) is respectively fixed on the other end of the sprayer (3) with the rigid pipe (3) and the rigid pipe (3) is inserted into the hollow pipe (3) and the rigid sprayer (3) is fixed on the end of the rigid pipe (3), the other end is fixed in the guide pipe (2), the inner diameter of the quartz reaction tube (6) is 20mm-25mm, the quartz reaction tube consists of an upper end supporting part (6-1) and a lower end reaction part (6-2), the length of the reaction part (6-2) is 600+/-10 mm, and the length of the supporting part (6-1) is 500+/-10 mm; the electric lifting device is vertically fixed on a chuck (11-1) on the side end face of a supporting seat (11), a sprayer (3) is positioned at the upper end of a supporting part (6-1) of a quartz reaction tube (6), an electric lifting table (7) is arranged in a guide rail (8), the direction of the guide rail (8) is the same as that of the quartz reaction tube (6), a hard hollow tube (4) is fixed on the electric lifting table (7) in an interference fit manner, at the moment, the initial position of the sprayer (3) is the initial position, and a speed sensor (9) is fixed on the electric lifting table (7).
2. A doping solution spraying apparatus as defined in claim 1, wherein: the outer diameter of the sprinkler (3) is 20-21mm, the length is 25-30mm, the inner diameter of the round cavity (3-1) is 18-19mm, and the height is 10-11mm.
3. A doping solution spraying apparatus as defined in claim 1, wherein: the loose layer is deposited in the quartz reaction tube (6), so that the inner diameter of the reaction part (6-2) of the quartz reaction tube (6) is 20-25 mm, and the curvature of the support part (6-1) of the quartz reaction tube (6) after the loose layer is deposited is small, so that the hard hollow tube (4) and the sprayer (3) enter the reaction part (6-2) of the quartz reaction tube.
4. A spraying method using a doping solution spraying apparatus according to claim 1, characterized in that: the spraying method comprises the following steps of,
firstly, a quartz tube is adopted as a quartz reaction tube (6) for deposition, an isolation layer is deposited on the inner wall of the quartz reaction tube (6) and is used for preventing impurity ions in the quartz reaction tube (6) from entering a core layer;
secondly, loose layer deposition is carried out on the reaction part (6-2) of the quartz reaction tube (6) deposited with the isolation layer, the loose layer is an unsintered, opaque and porous deposition layer which is used for adsorbing solute ions in solution, after the loose layer deposition in the quartz reaction tube (6), the inner diameter of the reaction part (6-2) of the quartz reaction tube (6) is made to be 20mm-25mm, and the curvature of the support part (6-1) of the quartz reaction tube (6) after the loose layer deposition is small, so that the hard hollow tube (4) and the sprayer (3) enter the reaction part (6-2) of the quartz reaction tube;
fixing a supporting part (6-1) of the quartz reaction tube (6) on a chuck (11-1) of a supporting seat (11), fixing a hard hollow tube (4) on the guide tube (2), connecting one end of the hard hollow tube (4) with a sprayer (3) and inserting the hard hollow tube into the uppermost end of the reaction part (6-2) of the quartz reaction tube (6), fixing the hard hollow tube (4) on an electric lifting table (7), and cleaning the hard hollow tube (4) and the sprayer (3) by deionized water before use;
fourthly, starting an electric lifting table (7), wherein the electric lifting table (7) drives a sprayer (3) at the lower end of a hard hollow pipe (4) to axially move into a designated position of a quartz reaction pipe (6), a speed sensor on the electric lifting table receives position information of the sprayer (3) through calculation in real time, the stepping speed range of the sprayer (3) is controlled to be 1mm/s-10mm/s, a nitrogen inlet switch is simultaneously opened, hose pipeline switches in a plurality of solution storages (1) filled with ionic solution are opened, the flow rate of the ionic solution is controlled to be 3ml/s, the ionic solution enters a guide pipe (2) through a hose (2-1) and is respectively connected with a circular cavity (3-1) of the sprayer (3), the ionic solution is sprayed out through radial fine through holes (3-2) of the sprayer (3), and the flow rate range of the ionic solution sprayed by the sprayer (3) to the quartz reaction pipe (6) is controlled to be 1ml/s-6ml/s;
turning off a pipeline switch between the ion solution storage and the hose (2-1) of the guide pipe (2) when the ion solution is sprayed to a specified quantity, turning off a nitrogen inlet pressure valve, stopping spraying the ion solution by the sprayer (3), driving the hard hollow pipe (4) and the sprayer (3) to do reverse axial movement by the electric lifting table until the sprayer (3) returns to an initial position, and turning off the electric lifting table (7);
sixthly, after the ion solution is injected, a little liquid remains in the hose (2-1) and the sprayer (3), and the hose (2-1) and the sprayer (3) are purged and cleaned up to avoid pollution or blockage of a pipeline;
and seventhly, loosening the chuck (11-1) of the supporting seat (11), taking down the quartz reaction tube (6), mounting the quartz reaction tube on a rod making lathe, standing, drying and finishing doping the ion solution.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011269166.5A CN112299703B (en) | 2020-11-13 | 2020-11-13 | Doping solution spraying device and spraying method |
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| CN202011269166.5A CN112299703B (en) | 2020-11-13 | 2020-11-13 | Doping solution spraying device and spraying method |
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| CN112299703B true CN112299703B (en) | 2024-03-12 |
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| CN217479333U (en) * | 2022-03-09 | 2022-09-23 | 华为技术有限公司 | Apparatus for doping a substrate tube comprising a porous layer |
| CN116040932A (en) * | 2022-11-23 | 2023-05-02 | 中国电子科技集团公司第四十六研究所 | Homogenized solution doping device and spraying method |
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