CN111153590B - Germanium tetrachloride tympanic bulla device of high accuracy - Google Patents
Germanium tetrachloride tympanic bulla device of high accuracy Download PDFInfo
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- CN111153590B CN111153590B CN201911408159.6A CN201911408159A CN111153590B CN 111153590 B CN111153590 B CN 111153590B CN 201911408159 A CN201911408159 A CN 201911408159A CN 111153590 B CN111153590 B CN 111153590B
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- 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]
- C03B37/01413—Reactant delivery systems
- C03B37/01433—Reactant delivery systems for delivering and depositing additional reactants as liquids or solutions, e.g. for solution doping of the porous glass preform
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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]
- C03B37/01413—Reactant delivery systems
- C03B37/0142—Reactant deposition burners
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Abstract
The utility model relates to a germanium tetrachloride tympanic bulla device of high accuracy, including special gas distribution cabinet, evaporation plant control assembly, evaporating pot, blowtorch, ventilation exhaust subassembly, and to the first pipeline and the second pipeline that the evaporating pot lets in the germanium tetrachloride raw materials, to the third pipeline that the evaporating pot lets in argon gas, by the fourth pipeline, the intercommunication that the evaporating pot evaporates out boil-off gas the fifth pipeline of third pipeline and fourth pipeline, to the blowtorch lets in boil-off gas's sixth pipeline, to ventilation exhaust subassembly carminative seventh pipeline and eighth pipeline. According to the high-precision germanium tetrachloride bubbling device, the pressure and the flow of the bubbling gas are accurately controlled by improving equipment such as a programmable logic controller, a proportional solenoid valve and an automatic valve, the problems of bubbles, cracking, standard exceeding of optical parameters and the like of a core layer of a core rod of an optical fiber preform rod are avoided, the product quality of the preform rod is greatly improved, and the production cost is reduced.
Description
Technical Field
The application belongs to the technical field of optical fiber preform core rod manufacturing, and particularly relates to a germanium tetrachloride bubbling device with high precision.
Background
In the process of manufacturing the optical fiber preform, the core rod of the optical fiber preform and the optical fiber preform are respectively manufactured by a two-step method of VAD (axial vapor deposition) and OVD (outside rod chemical vapor deposition). The VAD method is characterized in that silicon dioxide SiO2 powder is deposited and attached to the surface of a rotating quartz target rod by utilizing a thermophoresis principle to manufacture a VAD loose body, and the VAD loose body is vitrified at high temperature of 1500 ℃ to finally manufacture a transparent optical fiber preform core rod. The optical refractive index of the core layer of the optical fiber preform rod needs to be improved by doping Gecl4 (germanium tetrachloride), and the stability of the Gecl4 doping effect directly influences the optical performance of the core rod and influences the product quality of the optical fiber preform rod.
Generally, the Gecl4 doping process is mainly performed by a bubbling method, a direct high-temperature evaporation method, and the like. The traditional VAD deposition adopts a bubbling tank to bubble a Gecl4 raw material, mainly utilizes hot carrier gas (argon or nitrogen and the like) to introduce a low-temperature Gecl4 raw material, gasifies and carries Gecl4 steam to enter a steam pipeline, and finally generates germanium dioxide GeO2 powder through VAD blowtorch and oxyhydrogen high-temperature hydrolysis reaction. The bubbling efficiency is mainly influenced by factors such as carrier gas flow, Gecl4 liquid level, liquid area, evaporation tank temperature and dispersion degree of carrier gas bubbles. Particularly, the Gecl4 feeding in the evaporation tank causes pressure fluctuation in the evaporation tank, and the actual evaporation capacity and the doping density of the core layer GeO2 are directly influenced. The fluctuation of the liquid level of the evaporation tank causes the change of the vaporization concentration of Gecl4, so the charging operation of Gecl4 raw materials in the evaporation tank needs to be carried out after the deposition is finished, and the doping stability of the subsequent deposition is ensured.
In the current industry, the Gecl4 raw material feeding mode under the off-line of the evaporating pot is divided into a manual mode and an automatic mode, but the problems of pressure fluctuation in the evaporating pot in the feeding process (as shown in figure 4) exist, the Gecl4 evaporation flow fluctuation in the deposition process (as shown in figure 5) is caused, and the problems of bubble generation (as shown in c in figure 8), cracking (as shown in b in figure 8), overproof optical parameters and the like of a core layer of a core rod of an optical preform rod are caused. The product value is directly reduced due to the bubbles appearing in the core rod layer, the core rod layer cracks to cause product loss, the core rod is easy to break and smash the sintering furnace in the vitrification stage, equipment and products are all scrapped, and the production cost is increased due to the fact that the optical parameters of the core rod exceed the standard and are scrapped.
For example, the invention patent CN103803790A discloses a high-precision germanium tetrachloride supply method and device, which realizes the functions of Gecl4 high-temperature evaporation and Gecl4 online charging by modifying a bubbling device, realizes the control of Gecl4 vapor flow by means of evaporation pipeline temperature control, and reduces the fluctuation of optical parameters, but does not provide a method for precisely controlling the evaporation flow of Gecl4 after offline charging in the traditional bubbling process. The utility model Chinese patent CN206232608U discloses a germanium tetrachloride liquid level automatic control system, through with the help of high accuracy infrared sensor realization under the off-line state bubbling device automatic material conveying function, does not mention its evaporation flow accurate control's method behind the Gecl4 reinforced yet.
Therefore, in order to avoid the problems of the increase of pressure fluctuation in the evaporation tank caused by the raw material charging of the Gecl4 in the off-line state of the evaporation tank and the bubbles, cracking, overproof optical parameters and the like of the core layer of the optical preform rod caused by the evaporation flow fluctuation of the Gecl4, a high-precision germanium tetrachloride bubbling device is needed.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: in order to solve the defects of the traditional bubbling process in the prior art, the high-precision germanium tetrachloride bubbling device with accurately controlled evaporation flow is provided.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a high-precision germanium tetrachloride bubbling device comprises a special gas distribution cabinet, an evaporation equipment control component, an evaporation tank, a blast lamp and a ventilation exhaust component, a first pipeline and a second pipeline for introducing germanium tetrachloride raw materials into the evaporation tank, a third pipeline for introducing argon into the evaporation tank, a fourth pipeline for evaporating evaporation gas from the evaporation tank, a fifth pipeline for communicating the third pipeline and the fourth pipeline, a sixth pipeline for introducing evaporation gas into the blowtorch, a seventh pipeline and an eighth pipeline for exhausting gas to the ventilation and exhaust assembly, the two ends of the first pipeline and the second pipeline are connected with the special gas distribution cabinet and the evaporating pot, one end of the third pipeline and one end of the fourth pipeline are connected with the evaporating pot, the two ends of the sixth pipeline are connected with the blowtorch and the other end of the fourth pipeline, and the two ends of the seventh pipeline and the eighth pipeline are connected with the ventilation and exhaust assembly and the sixth pipeline.
In one embodiment, the evaporation tank body is provided with an upper liquid level window and a lower liquid level window, the upper liquid level window is used for marking a first liquid level, and the lower liquid level window is used for marking a second liquid level.
In one embodiment, the first pipeline, the second pipeline, the third pipeline, the fourth pipeline, the fifth pipeline, the sixth pipeline and the eighth pipeline are respectively provided with a third automatic valve, a fourth automatic valve, a fifth automatic valve, a sixth automatic valve, a seventh automatic valve, an eighth automatic valve and a ninth automatic valve, the first pipeline is provided with a first pressure regulating valve, the second pipeline is provided with a manual valve and a second pressure regulating valve, and the seventh pipeline is provided with a proportional solenoid valve.
In one embodiment, the special gas distribution cabinet further comprises a programmable logic controller, the special gas distribution cabinet and the third and fourth pipelines are respectively provided with a first pressure sensor, a second pressure sensor and a third pressure sensor, the first pressure sensor, the third automatic valve and the fourth automatic valve are connected with the programmable logic controller, the first pressure sensor records pressure and feeds back the pressure to the programmable logic controller to adjust the third automatic valve and the fourth automatic valve, the second pressure sensor, the third pressure sensor and the proportional solenoid valve are connected with the programmable logic controller, and the magnitude of electric signals fed back to the programmable logic controller through the second pressure sensor and the third pressure sensor is used for adjusting the proportional solenoid valve.
In one embodiment, the system further comprises a mass flow controller arranged at the inlet end of the third pipeline, the inlet end of the mass flow controller is connected with an argon input pipe and a nitrogen input pipe, and the evaporation equipment control assembly is connected with and controls the mass flow controller to control the input amount of argon and nitrogen.
In one embodiment, the argon input pipe and the nitrogen input pipe are respectively provided with a first automatic valve and a second automatic valve, the second automatic valve controls argon to enter the third pipeline during deposition, and the first automatic valve controls nitrogen to enter and purge the third pipeline, the fifth pipeline and the eighth pipeline after deposition.
In one embodiment, the fifth automatic valve is used for controlling the flow of argon gas into the evaporation tank, and the eighth automatic valve is used for controlling the flow of the evaporation gas into the torch.
In one embodiment, the torch is a quartz torch.
In one embodiment, when the germanium tetrachloride raw material is introduced, if the pressure recorded by the first pressure sensor is lower than 30 psi or exceeds 45 psi, the electrical signal of the first pressure sensor is fed back to the programmable logic controller to close the third automatic valve and the fourth automatic valve; after the introduction of the germanium tetrachloride raw material is finished, if the pressure recorded by the third pressure sensor exceeds 20 psi, the electrical signal of the third pressure sensor is fed back to the programmable logic controller to adjust the proportional solenoid valve.
In one embodiment, the vaporization apparatus control assembly includes an audible and visual alarm, and the first pressure sensor registers a pressure below 30 psi or above 45 psi and the audible and visual alarm sounds an alarm.
The invention has the beneficial effects that: according to the high-precision germanium tetrachloride bubbling device, accurate control of pressure and flow of bubbling gas is realized by means of improvement of a PLC (programmable logic controller), a proportional solenoid valve, an automatic valve and other devices, the problems that pressure fluctuation in a tube is increased due to Gecl4 raw material feeding in an off-line state of an evaporation tank and bubble, cracking, standard exceeding of optical parameters and the like of a core layer of an optical fiber preform rod are caused by Gecl4 evaporation flow fluctuation are solved, the product quality of the preform rod is greatly improved, and the production cost is reduced.
Drawings
The technical solution of the present application is further explained below with reference to the drawings and the embodiments.
FIG. 1 is a schematic diagram of a high precision germanium tetrachloride bubbling apparatus according to an embodiment of the present application;
FIG. 2 is a PLC control schematic diagram in the process of charging the evaporation tank Gecl4 according to the embodiment of the application;
FIG. 3 is a schematic diagram of PLC control in a deposition process according to an embodiment of the present application;
FIG. 4 is a diagram showing the bubbling effect of germanium tetrachloride in an abnormal state according to an embodiment of the present application;
FIG. 5 is a second diagram illustrating the bubbling effect of germanium tetrachloride in an abnormal state according to an embodiment of the present invention;
FIG. 6 is a graph showing the bubbling effect of the evaporation tank Gecl4 manually filled according to the example of the present application;
FIG. 7 is a graph of bubbling effect after automatic charging of an evaporation tank Gecl4 according to an embodiment of the present application;
FIG. 8 is a different external view of a core layer of a core rod for an optical fiber preform according to an embodiment of the present application;
FIG. 9 is a box normal distribution plot of the standard deviation of relative refractive indices for a single core rod according to an embodiment of the present application;
FIG. 10 is a box normal distribution plot of relative refractive index minima for a single core rod according to an embodiment of the present application.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
In the description of the present application, it is to be understood that the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientation or positional relationship indicated in the drawings for convenience in describing the present application and for simplicity in description, and are not intended to indicate or imply that the referenced devices or elements must have a particular orientation, be constructed in a particular orientation, and be operated in a particular manner, and are not to be considered limiting of the scope of the present application. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the invention, the meaning of "a plurality" is two or more unless otherwise specified.
In the description of the present application, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art through specific situations.
The technical solutions of the present application will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
As shown in figure 1, the high-precision germanium tetrachloride bubbling device comprises an evaporation equipment control assembly 1 and an evaporation tank 2, wherein an upper visible liquid level window and a lower visible liquid level window are arranged on the tank body of the evaporation tank 2, and the upper visible liquid level window (for marking a first liquid level 3) and the lower visible liquid level window (for marking a second liquid level 4) are respectively arranged on the upper part and the lower part. The automatic control system further comprises a first pipeline 10, wherein the first pipeline 10 is sequentially provided with a first pressure regulating valve 11 and a third automatic valve 12; the automatic control valve further comprises a second pipeline 14, and a hand valve 15, a second pressure regulating valve 16 and a fourth automatic valve 13 are sequentially arranged on the second pipeline 14. In a non-deposition state, the evaporation tank 2 is in an off-line mode, when the raw material in the Gecl4 of the evaporation tank 2 falls to the liquid level two 4, the evaporation tank 2 needs to be charged, and one charging mode of the evaporation tank 2 can be selected, wherein one mode is manual charging, and the other mode is automatic charging.
The manual feeding mode: the fourth automatic valve 13 and the hand valve 15 are manually opened in sequence, then the opening degree of the second pressure regulating valve 16 is regulated, and the Gecl4 raw material is branched into a second pipeline 14 to enter the evaporation tank 2 through a VMB cabinet (special gas distribution cabinet). When manual feeding is carried out, the opening degree of the second pressure regulating valve 16 needs to be finely adjusted manually each time.
The automatic feeding mode: the fourth automatic valve 13 and the third automatic valve 12 are opened manually in sequence, and Gecl4 raw materials are branched into a first pipeline 10 through the VMB cabinet to enter the evaporation tank 2. When automatic feeding is carried out, the opening degree of the first pressure regulating valve 11 is kept fixed.
As shown in FIG. 1, the vaporization apparatus control unit 1 is used to control MFC (mass flow controller) 5 for Ar and N2The flow rates (argon and nitrogen flow rates) are set, and during deposition, the vaporization apparatus control assembly 1 sets the Ar flow rate through the MFC 5. At the end of the deposition, the evaporation apparatus control assembly 1 sets N via the MFC 52And (4) flow rate. The front end of the MFC 5 is provided with a first automatic valve 8And a second automatic valve 9. During the deposition, the second automatic valve 9 controls the flow of Ar into the third pipe 17, and when the deposition is finished, the first automatic valve 8 controls the flow of N2Purging the third conduit 17, the fifth conduit 23, the conduit eight 30. The third conduit 17 and the fourth conduit 20 are provided with a fifth automatic valve 19 and a sixth automatic valve 21 in this order, the fifth automatic valve 19 controlling the flow of Ar into the evaporation tank 2, the sixth automatic valve 21 controlling the flow of the evaporation gas into the fourth conduit 20, and the eighth automatic valve 26 controlling the flow of the evaporation gas (along the sixth conduit 25) into the VAD torch 37.
As shown in FIG. 1, the fifth pipe 23 communicates the third pipe 17 and the fourth pipe 20, and the fifth pipe 23 is provided with a seventh automatic valve 24. After 50 minutes of deposition, the seventh automatic valve 24 was closed. At the end of the deposition, the seventh automatic valve 24 is opened and the control N2 purges the third duct 17, the fifth duct 23, the duct eight 30, and finally into the VENT system (ventilation exhaust assembly) 6.
As shown in fig. 1, the first pressure sensor 7, the third automatic valve 12, and the fourth automatic valve 13 are connected to a PLC controller (programmable logic controller) 29, and the first pressure sensor 7 records pressure and feeds back the pressure to the PLC controller 29 to control the third automatic valve 12 and the fourth automatic valve 13. The second pressure sensor 18, the third pressure sensor 22 and the proportional solenoid valve 28 are connected with a PLC 29, and the proportional solenoid valve 28 is adjusted by the electric signals fed back to the PLC 29 by the second pressure sensor 18 and the third pressure sensor 22.
In one embodiment, the evaporation equipment control assembly 1 controls the opening and closing of each valve, the valve is driven to open and close by compressed air, the manual valve 15 is a manual diaphragm valve, the pressure regulating valves 1 and 2 are needle valves, and the proportional solenoid valve 28 is a proportional-integral regulating valve.
In one embodiment, the evaporation tank has a heating function, is made of 316 stainless steel and is used for heating Gecl4 raw materials, and the tank body is arranged into a cylinder, has the volume of about 20L and resists 60 psi (pound force per square inch).
In one embodiment, the VAD torch is a quartz torch used for chemical vapor axial deposition.
The invention also discloses a high-precision methodThe control method of the germanium tetrachloride bubbling device comprises the following steps: when the apparatus is in standby, the second automatic valve 9, the third automatic valve 12, the fourth automatic valve 13, the fifth automatic valve 19, the sixth automatic valve 21, the eighth automatic valve 26, and the proportional solenoid valve 28 are kept closed, the first automatic valve 8, the seventh automatic valve 24, and the ninth automatic valve 31 are opened, and N is2And purging the third pipeline 17, the fifth pipeline 23 and the eighth pipeline 26 in sequence, and finally discharging the purged gas into the VENT system 6.
Further, when the Gecl4 liquid level in the evaporation tank 2 drops to the height level two 4: 300mm, when the manual feeding mode is selected by the evaporating pot 2, the fourth automatic valve 13 and the hand valve 15 are manually opened in sequence, then the opening degree of the second pressure regulating valve 16 is adjusted to 0.5-4 circles, the feeding rate is controlled to be 100-160 sccm (milliliter per minute under the standard condition), when the Gecl4 raw material enters the evaporating pot 2 through the VMB cabinet shunting second pipeline 14, feeding is finished after 30-50 minutes, the second pressure regulating valve 16, the hand valve 15, the fourth automatic valve 13 are closed in sequence, and the Gecl4 liquid level height liquid level is one 3: 350 mm, the apparatus continues to stand for 1 hour, and deposition can then take place. When the automatic feeding mode is selected for the evaporating pot 2, the fourth automatic valve 13 and the third automatic valve 12 are manually opened in sequence, the opening degree of the first pressure regulating valve 11 is kept for 0.5-2 circles, the feeding rate is controlled to be 160-200 sccm, after the Gecl4 raw material enters the evaporating pot through the VMB cabinet shunting first pipeline 10, feeding is finished after 20-30 minutes, and the Gecl4 liquid level height is 3: 350 mm, the third automatic valve 12 and the fourth automatic valve 13 are closed in sequence, the apparatus continues to stand by for 1 hour, and then deposition can be carried out.
In the feeding process, the first pressure sensor 7 records that the pressure P1 is 30-45 psi, if the pressure is lower than 30 psi or exceeds 45 psi, synchronously, an electric signal is fed back to the PLC 29, the third automatic valve 12 and the fourth automatic valve 13 are closed, the feeding process is suspended, the evaporation equipment control assembly 1 gives out an audible and visual alarm, and technicians wait for on-site supervision of the process state of the VMB cabinet. After the feeding is finished, the third pressure sensor 22 records that the normal range of the pressure P2 is 10.0-20.0 psi, if the pressure exceeds 20 psi, an electric signal is synchronously fed back to the PLC controller 29 to adjust the proportional solenoid valve, and the pressure fluctuation of P2 is rapidly reduced to the normal range, as shown in FIG. 2, the PLC control principle is adopted.
After the deposition is started, the first automatic valve 8, the fifth automatic valve 19, the sixth automatic valve 21 and the ninth automatic valve 31 are closed, the second automatic valve 9, the seventh automatic valve 24 and the eighth automatic valve 26 are opened synchronously, and the normal range of Ar pressure fluctuation P3 recorded by the second pressure sensor 18 is 1.0-5.0 psi in the first 50 minutes. 50 minutes after the deposition starts, synchronously, the seventh automatic valve 24 is closed, the fifth automatic valve 19 and the sixth automatic valve 21 are opened, the second pressure sensor 18 records that the normal range of the pressure fluctuation P4 of the evaporation gas is 0-1.0 psi, the second pressure sensor 18 records that the normal range of the fluctuation range DeltaP 1 of the pressure fluctuation P4 of the evaporation gas is 0-0.1 psi, if the pressure of the P4 exceeds 1.0 psi or the fluctuation range DeltaP 1 exceeds 0.1 psi and lasts for 10 milliseconds, synchronously, the electric signal feedback PLC controller 29 adjusts the proportional solenoid valve 28, the evaporation gas is discharged into the VENT system 6 through a pipeline seven 27, and the pressure fluctuation size and the fluctuation range DeltaP 1 of the P4 are quickly reduced to the normal ranges.
The third pressure sensor 22 records a normal range of boil-off gas pressure levels P5 of 10.0 to 20.0 psi for the first 50 minutes after deposition begins. 50 minutes after the deposition starts, synchronously, the seventh automatic valve 24 is closed, the fifth automatic valve 19 and the sixth automatic valve 21 are opened, when the third pressure sensor 22 records that the normal range of the pressure fluctuation P6 of the evaporation gas is 0-0.5 psi, the normal range of the fluctuation range DeltaP 2 is 0-0.1 psi, if the pressure exceeds 0.5 psi or the fluctuation range exceeds 0.1 psi and lasts for 10 milliseconds, synchronously, an electric signal is fed back to the PLC controller 29 to adjust the proportional electromagnetic valve 28, the evaporation gas is discharged into the VENT system 6 through a pipeline seven 27, and the size of P6 and the fluctuation range DeltaP 2 are quickly reduced to the normal range, as shown in FIG. 3, the PLC control principle is shown.
Further, the deposition is ended and the apparatus enters a standby state.
The present invention also provides several implementation scenarios.
Implementation scenario 1: when equipment standby, manual feeding is selected to the evaporating pot 2, the fourth automatic valve 13 and the hand valve 15 are opened manually in sequence, then the opening degree of the second pressure regulating valve 16 is adjusted to 3 circles, the feeding rate is controlled to be 150 sccm, when Gecl4 raw materials flow into the evaporating pot 2 through the VMB cabinet shunting second pipeline 14, in the feeding process, the first pressure sensor 7 records the pressure P1: 35.0 to 35.5 psi. After 40 minutes, the feeding is finished, the second pressure regulating valve 16, the hand valve 15 and the fourth automatic valve 13 are closed in sequence, and the third pressure sensor 22 records the pressure P2: 15.0 psi. Gecl4 liquid level height level one 3: 350 mm, the apparatus was left standing for 1 hour before deposition scheduling.
As shown in fig. 4, under the conventional apparatus and control method, within 50 minutes from the start of deposition, the second pressure sensor 18 records Ar pressure fluctuation P3: 2.5-4.0 psi, and 50 minutes after the beginning of deposition, the second pressure sensor 18 records that the peak value of the pressure fluctuation P4 of the evaporation gas reaches 13.5si, which is far beyond the process requirement range. In comparison with fig. 6, the second pressure sensor 18 records the Ar pressure fluctuation P3 within 50 minutes of the start of deposition: 1.0 to 1.7 psi. 50 minutes after the deposition starts, synchronously closing the seventh automatic valve 24, opening the fourth automatic valve 13 and the sixth automatic valve 21, opening the proportional electromagnetic valve 28 by the PLC 29, recording the instantaneous peak value of the evaporation gas pressure fluctuation P4 to 2.3 psi by the second pressure sensor 18, recording the evaporation gas pressure fluctuation P4 and the fluctuation range delta P1 which are all stabilized at 0-0.2 psi and 0-0.1 psi in 12 hours of deposition, and synchronously recording the evaporation gas pressure fluctuation P6 and the fluctuation range delta P2 which are all stabilized at 0-1.0 psi and 0-0.07 psi by the third pressure sensor 22 after the process requirement range is reached.
After the process is finished, the SiO deposited and attached to the surface of the quartz target rod 322The (silicon dioxide) powder is transferred to a sintering furnace and vitrified at a high temperature of 1500 ℃, and finally, a transparent optical fiber preform core rod 32 is manufactured for appearance and optical parameter detection, as shown in a in fig. 8, the core rod core layer 33 and the core rod cladding layer 34 are detected to be normal, and no crack 35 or no bubble 36 appears.
Specific example 2: when equipment standby, automatic material conveying is selected to evaporating pot 2, and the manual work is opened and is opened fourth automatic valve 13, third automatic valve 12 in proper order, and 2 circles of size are kept to first air-vent valve 11 aperture, control feeding rate 180sccm, wait for Gecl4 raw materials to pass through VMB cabinet reposition of redundant personnel first pipeline 10 and get into evaporating pot 2, finish reinforced after 25 minutes of time, close third automatic valve 12, fourth automatic valve 13 in proper order, Gecl4 liquid level height liquid level one 3: 350 mm, the third pressure sensor 22 records the pressure P2: 13.5 psi. The apparatus continued to stand for 1 hour before deposition scheduling.
As shown in fig. 5, under the conventional apparatus and control method, within 50 minutes from the start of deposition, the second pressure sensor 18 records Ar pressure fluctuation P3: 1.2-1.4 psi, and synchronously, recording the fluctuation range DeltaP 1 of the evaporation gas pressure fluctuation P4 by the second pressure sensor 18 50 minutes after the beginning of deposition: 0.1-0.2 psi, far exceeding the process requirement range. In comparison with fig. 7, the second pressure sensor 18 records the Ar pressure fluctuation P3 within 50 minutes of the start of deposition: 1.2 to 1.4 psi. 50 minutes after the deposition starts, synchronously closing the seventh automatic valve 24, opening the fourth automatic valve 13 and the sixth automatic valve 21, opening the proportional electromagnetic valve 28 by the PLC 29, recording that the pressure fluctuation P4 of the evaporation gas instantly drops to 0.2 psi by the second pressure sensor 18, recording that the pressure fluctuation P4 and the fluctuation range DeltaP 1 of the evaporation gas are all stabilized at 0-0.5 psi and 0-0.1 psi within 11.5 hours of deposition, and recording that the pressure fluctuation P6 and the fluctuation range DeltaP 2 of the evaporation gas are all stabilized at 0-0.5 psi and 0-0.05 psi by the third pressure sensor 22 after the process requirement range is reached.
After the process is finished, the SiO deposited and attached to the surface of the quartz target rod 322Transferring the powder to a sintering furnace, vitrifying at 1500 ℃ to finally manufacture a transparent optical fiber preform core rod 32, and detecting the appearance and optical parameters, wherein as shown in a in fig. 8, the core rod core layer 33 is detected to be normal, and no crack 35 or bubble 36 appears.
The optical fiber preform rod prepared by the device and the control method of the invention is detected and compared by an optical fiber preform analyzer to find that:
as shown in FIG. 9, the relative refractive index standard deviation average value 0.0230% of the single core rod is effectively reduced to 0.0213% and the standard deviation of 0.0106% is reduced to 0.0063%;
as shown in fig. 10, the average value of relative refractive index difference of a single core rod is effectively reduced to 0.0080% and the standard deviation is reduced to 0.0039% and 0.0014%;
the invention has the beneficial effects that: according to the high-precision germanium tetrachloride bubbling device, accurate control of pressure and flow of bubbling gas is realized by means of improvement of a PLC (programmable logic controller), a proportional solenoid valve, an automatic valve and other devices, the problems that pressure fluctuation in a tube is increased due to Gecl4 raw material feeding in an off-line state of an evaporation tank and bubble, cracking, standard exceeding of optical parameters and the like of a core layer of an optical fiber preform rod are caused by Gecl4 evaporation flow fluctuation are solved, the product quality of the preform rod is greatly improved, and the production cost is reduced.
In light of the foregoing description of the preferred embodiments according to the present application, it is to be understood that various changes and modifications may be made without departing from the spirit and scope of the invention. The technical scope of the present application is not limited to the contents of the specification, and must be determined according to the scope of the claims.
Claims (7)
1. A high-precision germanium tetrachloride bubbling device is characterized by comprising a special gas distribution cabinet, an evaporation equipment control assembly, an evaporation tank, a blast lamp and a ventilation exhaust assembly, a first pipeline and a second pipeline for introducing germanium tetrachloride raw materials into the evaporation tank, a third pipeline for introducing argon into the evaporation tank, a fourth pipeline for evaporating evaporation gas from the evaporation tank, a fifth pipeline for communicating the third pipeline and the fourth pipeline, a sixth pipeline for introducing evaporation gas into the blowtorch, a seventh pipeline and an eighth pipeline for exhausting gas to the ventilation and exhaust assembly, the two ends of the first pipeline and the second pipeline are connected with the special gas distribution cabinet and the evaporating pot, one end of the third pipeline and one end of the fourth pipeline are connected with the evaporating pot, two ends of the sixth pipeline are connected with the blowtorch and the other end of the fourth pipeline, and two ends of the seventh pipeline and the eighth pipeline are connected with the ventilation and exhaust assembly and the sixth pipeline;
an upper liquid level window and a lower liquid level window are arranged on the evaporation tank body, the liquid level window positioned above is used for marking a first liquid level, and the liquid level window positioned below is used for marking a second liquid level;
the first pipeline, the second pipeline, the third pipeline, the fourth pipeline, the fifth pipeline, the sixth pipeline and the eighth pipeline are respectively provided with a third automatic valve, a fourth automatic valve, a fifth automatic valve, a sixth automatic valve, a seventh automatic valve, an eighth automatic valve and a ninth automatic valve, the first pipeline is provided with a first pressure regulating valve, the second pipeline is provided with a manual valve and a second pressure regulating valve, and the seventh pipeline is provided with a proportional electromagnetic valve;
the special gas distribution cabinet, the third pipeline and the fourth pipeline are respectively provided with a first pressure sensor, a second pressure sensor and a third pressure sensor, the first pressure sensor, the third automatic valve and the fourth automatic valve are connected with the programmable logic controller, the first pressure sensor records pressure and feeds back the pressure to the programmable logic controller to adjust the third automatic valve and the fourth automatic valve, the second pressure sensor, the third pressure sensor and the proportional solenoid valve are connected with the programmable logic controller, and the proportional solenoid valve is adjusted by feeding back electric signals to the programmable logic controller through the second pressure sensor and the third pressure sensor.
2. The high-precision germanium tetrachloride bubbling device according to claim 1, further comprising a mass flow controller arranged at the inlet end of the third pipeline, wherein an argon input pipe and a nitrogen input pipe are connected to the inlet end of the mass flow controller, and the evaporation equipment control assembly is connected with and controls the mass flow controller to control the input amount of argon and nitrogen.
3. The high precision germanium tetrachloride bubbling device according to claim 2, wherein a first automatic valve and a second automatic valve are respectively arranged on the argon gas input pipe and the nitrogen gas input pipe, the second automatic valve controls the argon gas to enter the third pipeline during deposition, and the first automatic valve controls the nitrogen gas to enter and purge the third pipeline, the fifth pipeline and the eighth pipeline when deposition is finished.
4. The high precision germanium tetrachloride bubbling device according to claim 1, wherein said fifth automated valve is used to control the flow of argon into said evaporation tank and said eighth automated valve is used to control the flow of said evaporation gas into said torch.
5. The high precision germanium tetrachloride bubbling device according to claim 1, wherein said torch is a quartz torch.
6. The high precision germanium tetrachloride bubbling device according to claim 1, wherein when the germanium tetrachloride raw material is introduced, if the pressure recorded by the first pressure sensor is lower than 30 psi or exceeds 45 psi, the electrical signal of the first pressure sensor is fed back to the programmable logic controller to close the third automatic valve and the fourth automatic valve; after the introduction of the germanium tetrachloride raw material is finished, if the pressure recorded by the third pressure sensor exceeds 20 psi, the electrical signal of the third pressure sensor is fed back to the programmable logic controller to adjust the proportional solenoid valve.
7. The high precision germanium tetrachloride bubbling apparatus according to claim 6, wherein said evaporation equipment control module comprises an audible and visual alarm, and said first pressure sensor registers that pressure is below 30 psi or above 45 psi and said audible and visual alarm gives an alarm.
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