Using method of special storage device for high-purity germanium tetrachloride for optical fiber

Abstract

The invention relates to a use method of a storage device special for high-purity germanium tetrachloride for optical fibers. The use method comprises the following steps that S1, all parts of the device are cleaned and dried; s2, the device is assembled; comprising the following steps that B1, a refrigeration temperature control device is assembled and fixed in an outer tank body; b2, the upper outer tank body and the inner tank body are assembled and fixed; b3, assembling the inner tank body and the outer tank body; b4, filler is injected, and the tank body is fixed; and S3, the assembled tank body is verified, and final cleaning is conducted. The method comprises the following steps that C1, electrical connection is conducted; step C2, manual verification of inflation is carried out; step C3, automatically verifying inflation; step C4, verifying a gas wall; step C5, refrigeration temperature control verification; step C6, cleaning before filling; the method is combined with the storage device for use, and sealing and storage failures of the device can be avoided as much as possible.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of chemical reagent storage devices, in particular to a use method of a special storage device for high-purity germanium tetrachloride for optical fibers. BACKGROUND

[0002] Germanium tetrachloride (GeCl4) for optical fibers is a key chemical raw material in optical fiber manufacturing, mainly used for preparing germanium-doped optical fibers. Its core role is to add germanium elements in the core part of the optical fiber to increase the refractive index, thereby optimizing the signal transmission performance, such as achieving high bandwidth, low loss and wide wavelength range, etc. The material is widely used in communication, laser technology, optical fiber sensing and other fields.

[0003] The purity of germanium tetrachloride for optical fibers is extremely high, but due to the corrosive nature of germanium tetrachloride itself, and its tendency to produce toxic gases and decompose in water, there are strict requirements for its preparation, storage and transportation, especially the requirement for sealing. Otherwise, impurities may be produced to fail to meet the requirements. In the existing storage operation, corrosion-resistant stainless steel tanks are usually used as storage containers in dry and low-temperature environments, but during use, when opening the storage tank to take out part of the raw material or when sampling the germanium tetrachloride in the tank, the tank opening or discharge opening will inevitably be in contact with the outside world. If the humidity of the environment is high at this time, impurities will be produced by the contact between the germanium tetrachloride and the outside world, affecting the product quality. Therefore, a special storage device is urgently needed. Since it is a special storage device, its use is different from existing equipment. If it is used according to existing equipment, it may not be able to avoid re-failure. Therefore, when providing the equipment, the use method thereof also needs to be provided. SUMMARY

[0004] To solve or partially solve the problems in the related art, the application provides a use method of a special storage device for high-purity germanium tetrachloride for optical fibers, which can avoid the contact between the product and the outside world when taking and sampling.

[0005] The application discloses a special storage device for high-purity germanium tetrachloride for optical fibers, which comprises a refrigeration temperature control device and further comprises: An outer tank body is provided in two parts, namely an upper outer tank body and a lower outer tank body, and the upper outer tank body and the lower outer tank body are detachably and tightly connected. A baffle is arranged at the bottom of the lower outer tank body to divide the lower outer tank body into a bottom refrigeration temperature control device cavity; and An inner tank body is provided with a nitrogen cylinder cavity on the outside, and a nitrogen cylinder is arranged in the nitrogen cylinder cavity. A tank opening is arranged at the top of the inner tank body. An air duct is arranged on the outer top of the inner tank body near the tank opening, and an air hole is arranged on the inner tank body below the tank opening to communicate the air duct with the inside of the inner tank body. The air duct is connected to the nitrogen cylinder in the nitrogen cylinder cavity through an air pipe; and A tank cover is provided with a pump, the liquid inlet of the pump is connected with an inner pipe inserted into the inner tank body, and the liquid outlet of the pump is connected with an outer pipe, and the outer pipe is provided with a valve. The inner tank body is arranged in the outer tank body and forms a sandwich, and the refrigeration temperature control device is arranged in the refrigeration temperature control device cavity, and the evaporator copper pipe of the refrigeration temperature control device is arranged in the sandwich.

[0006] Optionally, the baffle is an annular plate with a hollow in the middle, and the plate is provided with a mounting hole for placing the evaporator copper pipe.

[0007] Optionally, the sandwich is filled with a filler.

[0008] Optionally, the filler is a heat insulation and structural support filler.

[0009] Optionally, the upper outer tank body and the inner tank body are connected as a whole at the tank neck through a connecting filler.

[0010] Optionally, the air duct is arranged around the tank shoulder, and the air holes are arranged in multiple and inclined upward.

[0011] Optionally, the inclination angle of the air holes is 5-15 degrees.

[0012] Optionally, a pressure sensor is embedded at the top of the tank mouth, an electromagnetic air valve is arranged on the air pipe, the pressure sensor and the electromagnetic air valve are connected to a first controller integrated with display and control, and the first controller is embedded on the outer tank body.

[0013] Optionally, the connection between the upper outer tank body and the lower outer tank body is constructed with an upper mounting table and a lower mounting table that are embedded with each other, and the upper mounting table and the lower mounting table are fastened by screws after being embedded.

[0014] Optionally, a corrosion-resistant sealing ring is constructed at the bottom of the tank cover.

[0015] A use method of a high-purity germanium tetrachloride special storage device for optical fibers, comprising the following steps: S1: washing and drying each part of the device; S2: assembling the device; comprising the following steps: Step B1: assembling and fixing the refrigeration temperature control device in the outer tank body; Step B2: assembling and fixing the upper outer tank body and the inner tank body; Step B3: assembling the inner and outer tank bodies; Step B4: injecting the filler and fixing the tank body; S3: verifying and finally cleaning the assembled tank body: comprising the following steps: Step C1: electrical connection; Step C2: manual verification of inflation; Step C3: automatic verification of inflation; Step C4: air wall verification; Step C5: refrigeration temperature control verification; Step C6: pre-filling cleaning.

[0016] Optionally, in S1, the tank body is mainly divided into an outer tank body that can be divided into two parts, an inner tank body that is integrally formed, and a tank cover; the tank body is in a disassembled state before cleaning, and each part of the tank body is cleaned separately before the tank body is assembled, and each part is dried without any water after cleaning; during cleaning, an automatic cleaning device can be used to perform high-strength rotary cleaning on the inner tank body.

[0017] Optionally, when the inner tank body is cleaned, a 0.5MPA high-pressure water gun is used to spray 0.5MPA high-pressure water flow into the air passage from the connection port, and after drying, a 0.5MPA high-pressure air flow is used for a second time to blow the air passage.

[0018] Optionally, in step B1, the refrigeration temperature control device is first installed and fixed on the inner bottom of the lower outer tank body, and the evaporator copper pipe is installed and fixed on the baffle and arranged to be located in the interlayer between the inner tank body and the outer tank body, and the entire refrigeration temperature control device is connected to form an independent device or system that can refrigerate and control the refrigeration temperature.

[0019] Optionally, in step B2, the upper outer tank body and the inner tank body are connected as a whole at the tank neck by a connecting filler, and different connection methods are used according to different materials.

[0020] Optionally, in step B3, the assembled upper outer tank body is covered on the lower outer tank body, and the inner tank body is inserted into the lower outer tank body; two vertical plates are arranged between the two evaporator copper pipes to connect the lower outer tank body as a whole, so that after the inner tank body is inserted into the outer tank body, the tank wall of the outer tank body and the pipe wall of the inner tank body jointly form a filling cavity with the two vertical plates.

[0021] Optionally, when the inner and outer tank bodies are assembled, one of the filling cavities is used as a reserved cavity for electric wires and control lines, and the control lines and electric wires are pre-buried in the cavity and connected to the components during assembly.

[0022] Optionally, before assembly, a thermal insulation or heat insulation layer is first applied to the wall surfaces of the inner tank body, or a material that has both thermal insulation or heat insulation and supporting functions is selected as the filler when selecting the filler.

[0023] Optionally, in step B4, the bolt hole is injected as a filler into the hole, and the filler is injected between the inner and outer tank bodies to fill the clamping, and after the filling is fixed and formed, the upper outer tank body and the lower outer tank body are fastened by bolts.

[0024] Optionally, in S3, the following steps are included. Step C1: The wires of the pressure sensor, the electromagnetic gas valve, and the cold temperature control device are passed through the reserved channel and connected to the first controller, and the high-pressure nitrogen cylinder is placed in the nitrogen cylinder cavity and connected to the electromagnetic gas valve and the gas channel. Step C2: The first controller and the pressure sensor at the tank opening are manually checked, first the first controller controls the opening and closing of the electromagnetic gas valve to check whether the nitrogen can be normally blown out from the gas hole, and then the pressure sensor is triggered to check whether the pressure of the pressure sensor can control the nitrogen to be normally blown out from the gas hole. Step C3: Verification is performed by installing the tank cover, when the tank cover is opened, the pressure sensor can normally control the nitrogen to be blown out from the gas hole, and when the tank cover is closed, whether the tank can reach the predetermined pressure. Step C4: A high-precision humidity sensor is placed in the tank and outside the tank, the electromagnetic gas valve is opened to form a gas wall and overflow gas, the external humidity is changed, and whether the humidity in the tank changes is checked. Step C5: The storage temperature of the inner tank body which has completed installation and verification of steps C2, C3 and C4 is kept at a preset temperature to verify whether it can normally cool and maintain at the set temperature. Step C6: Before filling, germanium tetrachloride is used for the final cleaning of the inner tank body.

[0025] The technical scheme provided by the application can include the following beneficial effects: The device can avoid the influence of environmental temperature and humidity on the purity of germanium tetrachloride when storing germanium tetrachloride, and can keep the germanium tetrachloride in a suitable storage environment through temperature control, and can still avoid the entry of external air when the tank body is opened, thereby ensuring the purity of high-purity germanium tetrachloride for optical fibers, avoiding the reduction of purity and affecting the quality. By using the method in combination with the storage device, the sealing and storage failure of the device can be avoided as much as possible, and the purity of high-purity germanium tetrachloride for optical fibers can be ensured when storing the germanium tetrachloride.

[0026] It should be understood that the above general description and the following detailed description are only exemplary and explanatory, and cannot limit the application. BRIEF DESCRIPTION OF DRAWINGS

[0027] The above and other objects, features and advantages of the present application will become more apparent from the following detailed description when taken in conjunction with the accompanying drawings in which like reference characters refer to like parts throughout the figures, and wherein:

[0028] Figure 1 is a structural schematic diagram of an embodiment of the present application; Figure 2 is a sectional view of A-A of an embodiment of the present application; Figure 3 is a sectional view of B-B of an embodiment of the present application; Figure 4 is a sectional view of C-C of an embodiment of the present application; Figure 5 is an upper and lower bending structure of an evaporator copper tube of an embodiment of the present application; Figure 6 is a sectional view of installation of a nitrogen cylinder of an embodiment of the present application; Reference Signs: 1, outer tank body; 11, upper outer tank body; 111, upper mounting table; 12, lower outer tank body; 121, baffle; 122, refrigeration temperature control device cavity; 123, mounting hole; 124, inner tank cavity; 125, lower mounting table; 2, inner tank body; 21, nitrogen cylinder cavity; 22, nitrogen cylinder; 23, threaded air valve; 24, electromagnetic air valve; 25, air pipe; 26, air passage; 27, air hole; 28, connecting filler; 29, pressure sensor; 210, tank opening; 3, tank cover; 31, pump; 32, inner tube; 33, outer tube; 34, valve; 4, filler; 5, refrigeration temperature control device; 51, evaporator copper tube; 6, sealing ring. DETAILED DESCRIPTION

[0029] Embodiments of the present application will be described more fully hereinafter with reference to the accompanying drawings, in which embodiments of the application are shown. This application may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the application to those skilled in the art.

[0030] It should be understood that, although the terms "first", "second", "third", etc. can be used in this application to describe various information, these information should not be limited to these terms. These terms are only used to distinguish the same type of information from each other. For example, the first information can also be referred to as the second information, and similarly, the second information can also be referred to as the first information without departing from the scope of the application. Therefore, the features defined with "first", "second" can explicitly or implicitly include one or more of the features. In the description of the present application, the meaning of "a plurality of" is two or more, unless otherwise specifically limited.

[0031] In the description of the present application, it should be understood that the orientation or positional relationship indicated by the terms "length", "width", "upper", "lower", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer" and the like is based on the orientation or positional relationship shown in the drawings, and is only for the convenience of describing the present application and simplifying the description, and does not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as a limitation of the present application.

[0032] Unless otherwise specifically defined and limited, the terms "mounting", "connecting", "connecting", "fixing" and the like should be broadly understood, for example, can be fixed connection, can also be detachable connection, or integral; can be mechanical connection, can also be electrical connection; can be directly connected, can also be indirectly connected through an intermediate medium; can be the internal communication of two elements or the interaction relationship between two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0033] In view of the above problems, the embodiments of the present application provide a high-purity germanium tetrachloride storage device special for optical fiber, which will be described in detail below in combination with the drawings.

[0034] As Figure 1 , Figure 2 , Figure 3 and Figure 4The illustrated high-purity germanium tetrachloride storage device for optical fibers includes a cooling and temperature control device 5 and an outer tank 1. The outer tank 1 is divided into two parts: an upper outer tank 11 and a lower outer tank 12, which are detachably and securely connected. The bottom of the lower outer tank 12 is divided by a baffle 121, creating a bottom cooling and temperature control device cavity 122. The outer tank 1 is designed with two detachably and securely connected parts to facilitate the manufacturing and use of the entire device. This structure can be modified according to specific needs, such as designing it as two mutually detachable and securely connected parts. The detachable connection in this application uses bolts for easy installation of the cooling and temperature control device 5. The cooling and temperature control device 5 in this application can be a conventional refrigerator cooling and temperature control device or system. In this application, the compressor, condenser, expansion valve, and other components required for refrigeration and temperature control are installed in the bottom refrigeration and temperature control device cavity 122. The evaporator is remade to accommodate the tank design of this application. The evaporator of this application is constructed using evaporator copper tube 51, that is, a copper tube is bent into an S-shape and then arranged in a ring along the inside of the tank. This application uses... Figure 5 The structure shown is bent upwards and downwards, then rolled into a cylindrical shape and inserted into the tank. In this way, the low temperature generated by the evaporator copper tube 51 in the refrigeration system is transferred to the tank, thereby achieving low-temperature control of the tank. During this process, appropriate controllers and intelligent control systems are set up as needed, and temperature sensors are placed in suitable locations to detect the temperature of the tank. The controller controls the entire refrigeration temperature control device to maintain the tank's interior at a suitable temperature for germanium tetrachloride storage.

[0035] The application also comprises an inner tank 2 for containing germanium tetrachloride, the outer part of the inner tank 2 is provided with a nitrogen cylinder cavity 21, and a nitrogen cylinder 22 is arranged in the nitrogen cylinder cavity 21; the top of the inner tank 2 is provided with a tank opening 210; a gas channel 26 is arranged on the outer top of the inner tank 2 close to the tank opening 210, and a gas hole 27 is arranged on the inner tank 2 below the tank opening 210 to communicate the gas channel 26 with the inside of the inner tank 2; the gas channel 26 is communicated to the nitrogen cylinder 22 in the nitrogen cylinder cavity 21 through a gas pipe 25; in this way, after the inner tank 2 is filled with germanium tetrachloride, the tank opening can be sealed by the nitrogen in the nitrogen cylinder 22, so as to avoid the volatilization of germanium tetrachloride in the inner tank; on the other hand, the nitrogen continuously released from the nitrogen cylinder 22 forms a gas wall to seal the tank opening 210, and at the same time, the nitrogen is continuously released to the outside, so as to avoid the tank opening 210 from being opened or the inside germanium tetrachloride storage space from being changed, and the outside air from entering the tank to reduce the purity of germanium tetrachloride or cause pollution; in particular, the moisture in the air is prevented from entering the tank to react with germanium tetrachloride to reduce the purity of germanium tetrachloride. Therefore, the nitrogen in the nitrogen cylinder 22 is compressed nitrogen, so as to continuously supply the nitrogen.

[0036] The application also comprises a sealable tank cover 3 which can be opened and closed, the tank cover 3 is provided with a pump 31, the inlet of the pump 31 is connected with an inner pipe 32 which is inserted into the inner tank 2, the outlet of the pump 31 is connected with an outer pipe 33, and the outer pipe 33 is provided with a valve 34. In this way, after the tank is sealed, the germanium tetrachloride in the tank can be pumped out by controlling the start of the pump 31; the valve 34 is arranged mainly to prevent the water vapor in the distance from the pump 31 to the outlet of the pipe to reduce the purity of germanium tetrachloride; and the distance between the outlet of the pump and the tank is too short to cause the water vapor in the cavity of the pump itself. In the process of use, the influence of the pumping of germanium tetrachloride can be reduced by reasonably controlling the start and stop of the pump 31 and the opening and closing of the valve 34; in this way, the valve 34 is a check valve, and the opening of the pump 31 generates a certain pressure to automatically open the valve 34; in this way, the backflow of the outside air into the pump body or the tank after the pump 31 is stopped is avoided.

[0037] In the application, the inner tank 2 is arranged in the outer tank 1 to form a sandwich, and the refrigeration temperature control device 5 is arranged in the refrigeration temperature control device cavity 122 to form an evaporator in the sandwich; in this way, the temperature of the whole tank can be controlled to be in a suitable temperature range which is beneficial to the storage of germanium tetrachloride.

[0038] The application avoids the influence of environmental temperature and humidity on the purity of germanium tetrachloride when storing the germanium tetrachloride by letting the tank body have a temperature control nitrogen continuous air seal, and the germanium tetrachloride is kept in a proper storage environment through temperature control, and the tank body can still avoid the entry of external air when being opened through the nitrogen continuous air seal, thereby ensuring the purity of high-purity germanium tetrachloride for optical fibers and avoiding the reduction of the purity.

[0039] In an embodiment, in order to facilitate the placement and fixation of the evaporator copper pipe 51, the baffle 121 is an annular plate with a hollow in the middle to facilitate the installation and fixation of components such as compressors, condensers, expansion valves, etc., and the plate is provided with a mounting hole 123 for placing the evaporator copper pipe 51, which is fixed when passing through the mounting hole, and then connected with the expansion valve and the compressor. It should be noted that after the refrigeration temperature control device 5 is installed, a layer of heat insulation layer or a layer of heat insulation layer is preferably arranged between the inner tank body 2 and the top of the baffle 121 to separate the inner tank body 2 from the heat generated by the condenser. At the same time, an air outlet is needed to be opened on the outer tank body, and a fan is needed to be arranged to cool it if necessary. In this way, the storage temperature of the inner tank body 2 can be controlled as long as the equipment is powered on, so that the pure tank can be used for transportation while being stored. Of course, if possible, a filling material that simultaneously considers heat preservation or insulation and structural support, such as rock wool, glass wool or rigid polyurethane foam, is directly used as the filling material.

[0040] In an embodiment, since the inner tank body 2 is placed in the outer tank body 1 and forms a sandwich, the application is filled with a filling material 4 in the sandwich. On the one hand, it is to make the inner and outer tank bodies form a whole, and on the other hand, it is to make the inner and outer tank bodies have levels, mainly temperature levels. In this way, the filling material 4 is a heat insulation and structural support filling material. Specifically, a layer of heat insulation layer is arranged on the inner side of the outer tank body 1, and then a structural support filling material is poured into the space between the heat insulation layer and the inner tank body 2 to support the inner and outer tank bodies, so that the inner and outer tank bodies form a whole in mechanical structure and form levels in temperature change, which is convenient for the refrigeration temperature control device 5 to maintain the low temperature of the inner tank body 2 and also avoids the escape of temperature to the outer layer.

[0041] In an embodiment, in order to form the tank body and reduce components, the upper outer tank body 11 and the inner tank body 2 are connected at the tank neck through a connecting filling material to form a whole. For example, when the inner and outer tank bodies are both made of stainless steel, a piece of stainless steel can be used to connect the two into a whole by welding. When the inner and outer materials are inconsistent, the two can be connected into a whole by an intermediate filling material using a connecting material such as glue, which is convenient for installation.

[0042] In one embodiment, the application uses nitrogen to seal the tank mouth 210, so the gas hole 27 is extremely critical, in the application, the gas channel 26 is arranged around the tank shoulder, preferably at the junction of the tank shoulder and the tank mouth corner, the gas channel 26 is connected with the inner tank body 2 as a whole by welding, and a connecting port is arranged at the position close to the nitrogen cylinder cavity 21 of the gas channel 26 as an interface for communication with the nitrogen cylinder. The gas hole 27 is arranged in multiple and inclined upward, and the inclination angle of the gas hole 27 is selected from 5 degrees to 15 degrees, and preferably 0 degree. In this way, after the germanium tetrachloride filling is completed, the liquid surface is just below the gas hole 27, and the multiple gas holes 27 blow out the other with a certain pressure to form a upward convex cone-shaped gas wall, and at the same time, due to the sealing of the bottom space, when the tank mouth 210 is opened, the excess other will escape outward, combined with the gas wall to prevent the external space from entering.

[0043] In one embodiment, after the sealing of the tank body cover with the tank cover 3 after the sealing is completed, the tank body cannot be filled with gas all the time, and the internal sealing needs to reach the required pressure. At the same time, the sealing needs to work when the tank cover 3 is opened, so the triggering condition is to judge the opening of the tank cover 3, and the condition can be converted into the change of the gas pressure in the tank body or the pressure change between the tank cover and the tank body. Therefore, the top of the tank mouth 210 is embedded with a pressure sensor 29, and a pressure sensor is also arranged in the gas channel 26. The gas pipe 25 is provided with an electromagnetic gas valve 24, and the two pressure sensors 29 and the electromagnetic gas valve 24 are connected to a first controller integrated with display and control, which is embedded on the outer tank body 1. In this way, when the pressure sensor in the gas channel 26 detects that the gas pressure in the tank body reaches the sealing requirement, the opening of the electromagnetic gas valve 24 is stopped, the nitrogen cylinder 22 is closed, and the tank body is normally sealed and stored; when the tank body is opened, the pressure between the tank cover 3 and the tank body changes, at the same time, the internal space also changes, and the pressure also changes, so the first controller controls the electromagnetic gas valve 24 to open a certain opening degree, and fills the nitrogen into the tank body to change; when the tank cover 3 is completely opened, the control gas controls the electromagnetic gas valve 24 to be completely opened at the moment to form a gas wall at the tank mouth 210 and prevent external air from entering the tank body.

[0044] In one embodiment, in order to facilitate the plug-in use of the nitrogen cylinder 22, such as Figure 6As shown, the nitrogen cylinder cavity 21 and the nitrogen cylinder 22 are both set as cylindrical shape, a cylindrical rotating groove with internal thread is set at the bottom of the nitrogen cylinder cavity 21, a connecting pipe is set at the bottom of the groove, a gas needle is set at the center of the groove bottom, and air holes are set around the gas needle and connected with the connecting pipe; the bottle mouth of the nitrogen cylinder 22 is provided with external thread and is screwed with the cylindrical rotating groove, a needle guide valve like a basketball or a tire valve is set in the bottle mouth, when the nitrogen cylinder 22 is screwed in the cylindrical rotating groove, the needle guide valve is opened by the gas needle to release the gas in the nitrogen cylinder 22, and then the gas is connected to the electromagnetic valve 24 through the connecting pipe as an electrically controlled switch to control the release of the nitrogen. A rotating handle is set at the bottom of the nitrogen cylinder 22, when the nitrogen cylinder 22 is inserted into the nitrogen cylinder cavity 21 and is opposite to the cylindrical rotating groove, the rotating handle is rotated to fix the nitrogen cylinder 22 and guide the nitrogen. A cavity cover is set at the outside of the nitrogen cylinder cavity 21 to cover the whole nitrogen cylinder cavity 21.

[0045] In an embodiment, in order to facilitate the embedded connection of the upper outer tank body 11 and the lower outer tank body 12, an upper mounting table 111 and a lower mounting table 125 are configured at the connection of the upper outer tank body 11 and the lower outer tank body 12, and the upper mounting table 111 and the lower mounting table 125 are embedded and fastened by screws after embedding.

[0046] In an embodiment, a corrosion-resistant sealing ring 6 is configured at the bottom of the tank cover 3 to be sealed after the tank cover 3 covers the whole tank body, and the connection mode of the tank cover 3 and the tank body can be selected according to specific needs, such as threaded connection, external cover pressing, or plunger, etc.

[0047] In an embodiment, the use method of the high-purity germanium tetrachloride special storage device for optical fibers in the above-mentioned embodiment includes the following steps: S1: cleaning and drying each part of the device; S2: assembling the device, including the following steps: Step B1: assembling and fixing the refrigeration temperature control device 5 in the outer tank body 1; Step B2: assembling and fixing the upper outer tank body 11 and the inner tank body 2; Step B3: assembling the inner and outer tank bodies; Step B4: injecting the filler and fixing the tank body; S3: verifying and finally cleaning the assembled tank body: including the following steps: Step C1: electrical connection; Step C2: manual verification of inflation; Step C3: automatic verification of inflation; Step C4: air wall verification; Step C5: refrigeration temperature control verification; Step C6: pre-filling cleaning.

[0048] Wherein, In step S1, the tank is mainly divided into two parts of the outer tank 1 which can be disassembled, the inner tank 2 which is integrally formed, and the tank cover 3. The tank is in a disassembled state before cleaning. Each part of the tank is cleaned separately before assembly, and is dried without any water after cleaning. In the cleaning process, the inner tank 2 can be cleaned by automatic cleaning equipment with high strength rotation. For example, high temperature 0.5MPA high pressure spray gun is used for cleaning, or special equipment is used for high power cleaning. It should be noted that when cleaning the inner tank 2, the air duct 26 needs to be sprayed with 0.5MPA high pressure water gun from the connecting port to the air duct 26, and then blown with 0.5MPA high pressure air after drying.

[0049] In step S2, the device is assembled; including the following steps: Step B1: refrigeration temperature control device 5 is assembled and fixed in the outer tank 1: first install and fix the refrigeration temperature control device 5 in the lower outer tank 12, and install and fix the evaporator copper pipe 51 on the baffle 121, and arrange the evaporator copper pipe 51 to be located in the interlayer between the inner tank 2 and the outer tank 1, and connect the whole refrigeration temperature control device 5 to become an independent device or system which can cool and control the refrigeration temperature.

[0050] Step B2: assemble and fix the upper outer tank 11 and the inner tank 2: connect the upper outer tank 11 and the inner tank 2 at the tank neck by connecting filler to form a whole, and use different connection methods to fix according to different materials. When the tank is made of corrosion-resistant metal, the two can be connected as a whole by welding. The reason for such setting is to facilitate the arrangement and placement of the air duct 26. The air duct 26 is connected with the inner tank 2 as a whole by welding, and a connecting port is arranged near the nitrogen cylinder cavity 21 of the air duct 26.

[0051] Step B3: Assembly of inner and outer tank bodies: the assembled upper outer tank body 11 is covered on the lower outer tank body 12, and the inner tank body 2 is inserted into the lower outer tank body 12; two vertical plates are arranged between the two evaporator copper pipes 51 clamped by the inner tank body 2 and the lower outer tank body 12. The two vertical plates are arranged on the inner side walls of the lower outer tank body 12 and the upper outer tank body 11 in advance, and are disconnected at the upper mounting table 111 and the lower mounting table 125 and connected by a plug-in structure. If necessary, two Z-shaped positioning blocks embedded in each other are arranged at the connection to close the inner tank body 2 in the upper outer tank body 11 and the lower outer tank body 12, and the positioning is performed when the embedding is performed. The upper outer tank body 11 and the lower outer tank body 12 are connected as a whole, so that after the inner tank body 2 is inserted into the outer tank body 1, the tank wall of the lower outer tank body 12 and the pipe wall of the inner tank body 2 jointly form a filling cavity with the two vertical plates for filling the filler.

[0052] It should be noted that when the inner and outer tank bodies are assembled, one of the filling cavities is used as a reserved cavity for electric wires and control lines during the arrangement of the vertical plates, and the control lines and electric wires are pre-buried in the cavity and connected to each other during the assembly. At the same time, before the assembly, a layer of thermal insulation layer is coated on the wall surface of the inner tank body 2 except the outer wall, or when the filler 4 is selected, a material that has both thermal insulation and supporting functions is selected as the filler.

[0053] Step B4: injection of filler and fixation of tank body: the bolt hole is used as the filler injection hole, the filler is injected between the inner and outer tank bodies to clamp and fill, and after the filler is injected and fixed, the upper outer tank body 11 and the lower outer tank body 12 are fastened by bolts. The bolt hole, which is used as the filler injection hole, is also used as one of the fastening connection structures for connecting the inner and outer tank bodies. A screw thread or a screw tooth is arranged in the bolt hole, and then the bolt is fastened. At the same time, the bolt is also screwed into the filler to connect the inner and outer tank bodies.

[0054] Step S3: verification of the assembled tank body and final cleaning, including the following steps: Step C1: electrical connection; the electric wires and control lines of the pressure sensor 29, the electromagnetic air valve 24, and the cold temperature control device are passed through the reserved channel and connected to the first controller, and the high-pressure nitrogen cylinder 22 is placed in the nitrogen cylinder cavity 21 and connected to the electromagnetic air valve 24 and the air duct 26.

[0055] Step C2: manual verification of inflation; the first controller and the pressure sensor 29 at the tank opening are used to manually check whether the nitrogen gas can be normally blown out of the air hole 27 by controlling the opening and closing of the electromagnetic air valve 24, and then whether the nitrogen gas can be normally blown out of the air hole 27 by the pressure of the pressure sensor 29. If not, check the connection equipment and control equipment again and verify again.

[0056] Step C3: verification of inflation or sealing; verification by installing the tank cover 3, when the tank cover 3 is opened, whether the pressure sensor 29 can normally control the nitrogen gas to be blown out from the air hole 27, when the tank cover 3 is closed, whether the tank can reach the predetermined pressure, if not, check the connection equipment and control equipment and verify again.

[0057] Step C4: verification of air wall; place a high-precision humidity sensor in the tank and outside the tank, open the electromagnetic air valve 24 to form an air wall and overflow gas, change the external humidity, and check whether the humidity in the tank changes, if it changes, check whether the air pressure of the formed air wall reaches the sealing pressure requirement, adjust the pressure and verify again.

[0058] Step C5: verification of refrigeration temperature control; control and verify whether the storage temperature of the inner tank body 2 installed and verified in steps C2, C3 and C4 can be normally refrigerated and maintained at the set temperature.

[0059] Step C6: cleaning before filling; before filling, the inner tank body 2 is finally cleaned with germanium tetrachloride.

[0060] After the completion of the application, the first control nitrogen cylinder 22 is filled with nitrogen gas at the top and maintained at a certain pressure, and the use is completed. When the tank cover 3 is opened, due to the loosening of the tank cover 3, the internal pressure changes, and at the same time the pressure sensor 29 detects that the tank cover 3 is opened, the first controller controls the electromagnetic air valve 24 to appropriately fill nitrogen gas, and when the tank cover 3 is completely opened, it normally operates, so that the air hole 27 sprays gas flow to form an air wall at the tank opening and overflow gas flow outward, so as to avoid the entry of external air into the tank. As long as the tank opening 210 is in an open state, the air wall and the outward overflow gas flow exist all the time, even if the product in the tank is sampled or other taken out operation, the external air will not enter the tank, even if the product in the tank is taken out a certain capacity, the empty space will be filled with nitrogen gas released by the nitrogen cylinder 22, and the storage environment in the tank is maintained, avoiding the volatilization of the product and the contact with external moisture.

[0061] By using the method of the application in combination with the storage device, the sealing and storage failure of the device can be avoided as much as possible, and the purity of the high-purity germanium tetrachloride for optical fiber storage can be ensured not to be reduced due to sampling or opening during use.

[0062] Finally, it should be noted that the terms "first" and "second", and the like, are used herein only to distinguish one identification entity from another, and do not require or imply these entities to be in any physical or logical order. Moreover, the terms "comprising", "including", or any other variation thereof, are intended to cover a non-exclusive inclusion, such that processes, methods, articles, or apparatuses that comprise, include, or are otherwise encompassed by a series of elements, do not require that all of the elements be present, only that some, but not necessarily all, of the elements are present to provide the processes, methods, articles, or apparatuses.

[0063] The units described as separate components may or may not be physically separate, and the components displayed as units may or may not be physical units, i.e. may be located in one place, or may be distributed to multiple network units. Part or all of the units can be selected according to actual needs to achieve the purpose of the embodiment.

[0064] The above has described the embodiments of the present application, and the above description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and changes are obvious to those skilled in the art without departing from the scope and spirit of the described embodiments. The selection of the terms used herein is intended to best explain the principles, practical application or improvement of the technology in the market of the embodiments, or to enable other ordinary skilled in the art to understand the embodiments disclosed herein.

Claims

1. A method of using a high-purity germanium tetrachloride storage device for optical fibers, characterized in that: Includes the following steps: S1: Clean and dry all parts of the device; S2: Assemble the device; It includes the following steps: Step B1: The refrigeration temperature control device (5) is assembled and fixed inside the outer tank (1); Step B2: Assemble and fix the outer tank (11) and the inner tank (2); Step B3: Assembly of the inner and outer tanks; Step B4: Inject the filler and secure the tank; S3: Verify the assembled tank and perform final cleaning: It includes the following steps: Step C1: Electrical connection; Step C2: Manual inflation verification; Step C3: Automatic inflation verification; Step C4: Airwall verification; Step C5: Refrigeration temperature control verification; Step C6: Cleaning before filling.

2. The method of using the high-purity germanium tetrachloride storage device for optical fibers according to claim 1, characterized in that: In S1, the tank is mainly divided into an outer tank (1) that can be separated into two parts, an inner tank (2) formed in one piece, and a tank cover (3). The tank is in a disassembled state before cleaning. Before the tank is assembled, each part of the tank is cleaned separately and dried after cleaning without leaving any moisture. During the cleaning process, an automatic cleaning device can be used to perform high-intensity rotation cleaning on the inner tank (2).

3. The method of using the high-purity germanium tetrachloride storage device for optical fibers according to claim 2, characterized in that: When cleaning the inner tank (2), the air passage (26) needs to be sprayed with high-pressure water from the connection port into the air passage (26) first, and then blown clean by high-pressure air after drying.

4. The method of using the high-purity germanium tetrachloride storage device for optical fibers according to claim 1, characterized in that: In step B1, the refrigeration temperature control device (5) is first installed and fixed at the bottom of the lower outer tank (12), and the evaporator copper tube (51) is installed and fixed on the baffle (121) and the evaporator copper tube (51) is arranged so that it is located in the interlayer between the inner tank (2) and the outer tank (1). The entire refrigeration temperature control device (5) is connected so that it becomes an independent device or system that can refrigerate and control the refrigeration temperature.

5. The method of using the high-purity germanium tetrachloride storage device for optical fibers according to claim 1, characterized in that: In step B2, the outer tank (11) and the inner tank (2) are connected as a whole at the neck of the tank by connecting filler, and different connection methods are used according to different materials.

6. The method of using the high-purity germanium tetrachloride storage device for optical fibers according to claim 1, characterized in that: In step B3, the assembled upper outer tank (11) is placed over the lower outer tank (12), and the inner tank (2) is inserted into the lower outer tank (12). Two vertical plates are set between the two evaporator copper tubes (51) in the clamping chamber and connected to the lower outer tank (12) as a whole so that after the inner tank (2) is inserted into the outer tank (1), the tank wall of the outer tank (1) and the tube wall of the inner tank (2) together with the two vertical plates form a filling cavity.

7. The method of using a high-purity germanium tetrachloride storage device for optical fibers according to claim 6, characterized in that: When assembling the inner and outer tanks, one of the filling cavities is used as a reserved cavity for electrical wires and control lines when setting the vertical plate. During assembly, the control lines and electrical wires are pre-embedded in this cavity and connected to the various components.

8. The method of using a high-purity germanium tetrachloride storage device for optical fibers according to claim 7, characterized in that: Before assembly, the other walls except the outer wall of the inner tank (2) are coated with a heat insulation layer before installation, or when selecting the filler (4), a material that has both heat insulation and support functions is selected as the filler.

9. The method of using the high-purity germanium tetrachloride storage device for optical fibers according to claim 1, characterized in that: In step B4, the bolt hole is used as a filler injection hole to inject filler between the inner and outer tanks to clamp and fill them. After filling and fixing, the upper outer tank (11) and the lower outer tank (12) are fastened together with bolts.

10. The method of using a high-purity germanium tetrachloride storage device for optical fibers according to claim 1, characterized in that: S3 includes the following steps; Step C1: Pass the wires and control wires of the pressure sensor (29), the solenoid valve (24), and the cold temperature control device through the reserved channel and connect them to the first controller. At the same time, place the high-pressure nitrogen cylinder (22) into the nitrogen cylinder cavity (21) and connect the solenoid valve (24) and the gas channel (26). Step C2: Manually verify the nitrogen gas through the first controller and the pressure sensor (29) at the can opening. First, check whether nitrogen gas can be blown out normally from the gas hole (27) by controlling the opening and closing of the solenoid valve (24) through the first controller; then check whether the nitrogen gas can be blown out normally from the gas hole (27) by triggering the pressure sensor (29); Step C3: Verify by installing the can lid (3). When the can lid (3) is open, check whether the pressure sensor (29) can control the nitrogen gas to blow out from the vent (27) normally. When the can lid (3) is closed, check whether the can can reach the predetermined pressure. Step C4: Place a high-precision humidity sensor inside and outside the tank, open the solenoid valve (24) to form an air wall and overflow gas, change the different external humidity, and check whether the humidity inside the tank changes; Step C5: After installation and verification of normal operation steps C2, C3 and C4, the storage temperature of the inner tank (2) is adjusted to maintain the preset temperature to verify whether it can cool normally and maintain the set temperature. Step C6: Before filling, the inner tank (2) is cleaned with germanium tetrachloride.

Images