CN211946809U - Germanium tetrachloride tympanic bulla device of high accuracy - Google Patents
Germanium tetrachloride tympanic bulla device of high accuracy Download PDFInfo
- Publication number
- CN211946809U CN211946809U CN201922473545.5U CN201922473545U CN211946809U CN 211946809 U CN211946809 U CN 211946809U CN 201922473545 U CN201922473545 U CN 201922473545U CN 211946809 U CN211946809 U CN 211946809U
- Authority
- CN
- China
- Prior art keywords
- pipeline
- automatic valve
- pressure sensor
- valve
- germanium tetrachloride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- IEXRMSFAVATTJX-UHFFFAOYSA-N tetrachlorogermane Chemical compound Cl[Ge](Cl)(Cl)Cl IEXRMSFAVATTJX-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 241000197194 Bulla Species 0.000 title abstract description 8
- 208000002352 blister Diseases 0.000 title abstract description 8
- 238000001704 evaporation Methods 0.000 claims abstract description 98
- 230000008020 evaporation Effects 0.000 claims abstract description 75
- 239000007789 gas Substances 0.000 claims abstract description 43
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 229910052786 argon Inorganic materials 0.000 claims abstract description 15
- 238000009826 distribution Methods 0.000 claims abstract description 11
- 238000009423 ventilation Methods 0.000 claims abstract description 9
- 230000008021 deposition Effects 0.000 claims description 34
- 239000007788 liquid Substances 0.000 claims description 30
- 230000005587 bubbling Effects 0.000 claims description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 230000001105 regulatory effect Effects 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 239000010453 quartz Substances 0.000 claims description 6
- 238000010926 purge Methods 0.000 claims description 5
- 230000000007 visual effect Effects 0.000 claims description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims 2
- 239000013307 optical fiber Substances 0.000 abstract description 15
- 230000003287 optical effect Effects 0.000 abstract description 14
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000009467 reduction Effects 0.000 abstract description 3
- 230000002026 carminative effect Effects 0.000 abstract 1
- 238000000151 deposition Methods 0.000 description 34
- 238000000034 method Methods 0.000 description 26
- 230000008569 process Effects 0.000 description 16
- 235000012239 silicon dioxide Nutrition 0.000 description 8
- 101100298225 Caenorhabditis elegans pot-2 gene Proteins 0.000 description 7
- 239000012792 core layer Substances 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 6
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000010410 layer Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000009834 vaporization Methods 0.000 description 4
- 230000008016 vaporization Effects 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910000619 316 stainless steel Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229940119177 germanium dioxide Drugs 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001089 thermophoresis Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000004017 vitrification Methods 0.000 description 1
Images
Landscapes
- Chemical Vapour Deposition (AREA)
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. The utility model discloses germanium tetrachloride tympanic bulla device of high accuracy realizes tympanic bulla gas pressure, the accurate control of flow through improving with the help of equipment such as programmable logic controller, proportional solenoid valve, automatic valve, avoids optical fiber perform plug sandwich layer bubble, fracture, optical parameter scheduling problem that exceeds standard, has greatly improved the product quality of perform, reduction in production cost.
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 figure 8 c), cracking (as shown in figure 8 b), overproof optical parameters and the like of a core layer of a core rod of an optical preform rod are caused. The value of the product is directly reduced due to the occurrence of bubbles in the core rod layer, the core rod layer cracks to cause product loss, and the core rod is easy to crack and smash the sintering furnace core pipe in the vitrification stage, so that equipment and products are completely scrapped, and the scrapping of the optical parameters of the core rod exceeding the standard increases the production cost.
The utility model discloses a method and equipment for supplying germanium tetrachloride with high precision is mentioned as disclosed in chinese utility model patent CN103803790A, realizes the function of Gecl4 high temperature evaporation and Gecl4 online charging by reforming the bubbling device, realizes the control of Gecl4 vapor flow with the help of evaporation pipeline temperature control, reduces the fluctuation of optical parameters, but does not provide the method for accurately controlling the evaporation flow after Gecl4 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.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is: 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 utility model provides a technical scheme that its technical problem adopted is:
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 and nitrogen 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 first automatic valve controls argon to enter the third pipeline during deposition, and the second 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 30psi or exceeds 45psi, 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 20psi, 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 30psi or above 45psi and the audible and visual alarm sounds an alarm.
The utility model has the advantages that: the utility model discloses germanium tetrachloride bubbling device of high accuracy realizes tympanic bulla gas pressure, flow accurate control through improving with the help of equipment such as programmable logic controller, proportional solenoid valve, automatic valve, avoids the reinforced bubble that causes intraductal pressure fluctuation grow, the optical fiber perform plug sandwich layer that Gecl4 evaporation flow fluctuation brought of Gecl4 raw materials under the evaporating pot off-line state to appear, fracture, optical parameter scheduling problem that exceeds standard, has greatly improved the product quality of perform, reduction in production cost.
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, unless otherwise specified, "a plurality" means two or more.
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 38 (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 material is branched into the first pipeline 10 to enter the evaporation tank 2 through the VMB cabinet 38. 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 MFC 5 is provided at the front end with a first automatic valve 8 and a second automatic valve 9. During the deposition, the first automatic valve 9 controls the flow of Ar into the third pipe 17, and when the deposition is finished, the second automatic valve 8 controls the flow of N2Purging the third, fifth and eighth conduits 17, 23, 30. The third pipe 17 and the fourth pipe 20 are sequentially provided with a fifth automatic valve 19 and a sixth automatic valve 21, the fifth automatic valve 19 is used for controlling the flow of Ar into the evaporation tank 2, the sixth automatic valve 21 is used for controlling the flow of the evaporation gas into the fourth pipe 20, and the eighth automatic valve 26 is used for controlling the flow of the evaporation gas into the VAD torch.
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 eighth duct 30, eventually discharging 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 a pneumatic diaphragm valve and is driven to open and close by compressed air, the hand valve 15 is a manual diaphragm valve, the pressure regulating valve is a needle valve, 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 utility model also discloses a germanium tetrachloride tympanic bulla device's of high accuracy control method: when the apparatus is in standby, the first automatic valve 8, 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 second automatic valve 9, 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 30 in sequence, and finally discharging 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 regulated 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 is shunted by the VMB cabinet 38 to enter the evaporating pot 2 through the second pipeline 14, feeding is finished after 30-50 minutes, the second pressure regulating valve 16, the hand valve 15 and the fourth automatic valve 13 are sequentially closed, and the first liquid level height liquid level of the Gecl4 is 3: 350mm, 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 opened in sequence by manual work, the opening degree of the first pressure regulating valve 11 is kept 0.5-2 circles, the feeding rate is controlled to be 160-200 sccm, after Gecl4 raw materials are shunted through the VMB cabinet 38, the first pipeline 10 enters the evaporating pot, feeding is finished after 20-30 minutes, and the Gecl4 liquid level height is one 3: 350mm, 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 30psi or exceeds 45psi, 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 38. 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 20psi, 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 1.0psi or the fluctuation range DeltaP 1 exceeds 0.1psi 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 20.0psi 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 0.5psi or the fluctuation range exceeds 0.1psi 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 utility model discloses still provide a plurality of concrete implementation sight.
Implementation scenario 1: when the equipment standby, the 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 150sccm, when Gecl4 raw materials flow into the evaporating pot 2 through the VMB cabinet 38 and the 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: 350mm, 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 fifth automatic valve 19 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 2.3psi by the second pressure sensor 18, recording the evaporation gas pressure fluctuation P4 and the fluctuation range DeltaP 1 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 DeltaP 2 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, depositing SiO attached to the surface of the quartz target rod2The (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 fig. 8a, the core rod core layer 33 is detected to be normal, no crack 35 exists, and no bubble 36 appears.
Implementation scenario 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 38 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: 350mm, the third pressure sensor 22 records the pressure P2: 13.5 psi. The apparatus continued to stand by for 30 minutes before the deposition schedule was performed.
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, the seventh automatic valve 24 is closed, the fourth automatic valve 13 and the sixth automatic valve 21 are opened, the PLC 29 opens the proportional electromagnetic valve 28, the second pressure sensor 18 records that the pressure fluctuation P4 of the evaporation gas instantly drops to 0.2psi, 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 after the process requirement range is reached, synchronously, the third pressure sensor 22 records that the pressure fluctuation P6 of the evaporation gas and the fluctuation range DeltaP 2 of the evaporation gas are all stabilized at 0-0.5 psi and 0-0.05 psi.
After the process is finished, depositing SiO attached to the surface of the quartz target rod2Transferring 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 fig. 8a, the core rod core layer 33 is detected to be normal, and no crack 35 or bubble 36 appears.
The utility model discloses the optical fiber perform plug that device and control method prepared detects contrast discovery through optical fiber perform analysis appearance optical parameter:
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 utility model has the advantages that: the utility model discloses germanium tetrachloride bubbling device of high accuracy realizes tympanic bulla gas pressure, flow accurate control through improving with the help of equipment such as programmable logic controller, proportional solenoid valve, automatic valve, avoids the reinforced bubble that causes intraductal pressure fluctuation grow, the optical fiber perform plug sandwich layer that Gecl4 evaporation flow fluctuation brought of Gecl4 raw materials under the evaporating pot off-line state to appear, fracture, optical parameter scheduling problem that exceeds standard, has greatly improved the product quality of perform, reduction in production cost.
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 (10)
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 and nitrogen 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.
2. The high-precision germanium tetrachloride bubbling device according to claim 1, wherein an upper liquid level window and a lower liquid level window are arranged on the evaporation tank body, 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.
3. The high precision germanium tetrachloride bubbling device according to claim 1, wherein 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 are respectively arranged on said first pipeline, said second pipeline is provided with a manual valve and a second pressure regulating valve, and said seventh pipeline is provided with a proportional solenoid valve.
4. The high-precision germanium tetrachloride bubbling device according to claim 3, further comprising a programmable logic controller, wherein 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 an electric signal 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.
5. 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.
6. The high precision germanium tetrachloride bubbling device according to claim 5, 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 first automatic valve controls the argon gas to enter the third pipeline during deposition, and the second automatic valve controls the nitrogen gas to enter and purge the third pipeline, the fifth pipeline and the eighth pipeline when deposition is finished.
7. The high precision germanium tetrachloride bubbling device according to claim 3, 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.
8. The high precision germanium tetrachloride bubbling device according to claim 1, wherein said torch is a quartz torch.
9. The high precision germanium tetrachloride bubbling device according to claim 4, wherein when the germanium tetrachloride raw material is introduced, if the pressure recorded by the first pressure sensor is lower than 30psi or exceeds 45psi, 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 20psi, the electrical signal of the third pressure sensor is fed back to the programmable logic controller to adjust the proportional solenoid valve.
10. The high precision germanium tetrachloride bubbling apparatus according to claim 9, wherein said evaporation equipment control module comprises an audible and visual alarm, and said first pressure sensor registers a pressure below 30psi or above 45psi and said audible and visual alarm gives an alarm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922473545.5U CN211946809U (en) | 2019-12-31 | 2019-12-31 | Germanium tetrachloride tympanic bulla device of high accuracy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922473545.5U CN211946809U (en) | 2019-12-31 | 2019-12-31 | Germanium tetrachloride tympanic bulla device of high accuracy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN211946809U true CN211946809U (en) | 2020-11-17 |
Family
ID=73180784
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201922473545.5U Expired - Fee Related CN211946809U (en) | 2019-12-31 | 2019-12-31 | Germanium tetrachloride tympanic bulla device of high accuracy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN211946809U (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111153590A (en) * | 2019-12-31 | 2020-05-15 | 江苏通鼎光棒有限公司 | Germanium tetrachloride tympanic bulla device of high accuracy |
| CN113666625A (en) * | 2021-07-30 | 2021-11-19 | 浙江富通光纤技术有限公司 | Method for processing prefabricated rod |
| CN114646434A (en) * | 2022-03-20 | 2022-06-21 | 山西太钢不锈钢股份有限公司 | Automatic detection device for air tightness of all-hydrogen bell-type furnace load space and use method |
-
2019
- 2019-12-31 CN CN201922473545.5U patent/CN211946809U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111153590A (en) * | 2019-12-31 | 2020-05-15 | 江苏通鼎光棒有限公司 | Germanium tetrachloride tympanic bulla device of high accuracy |
| CN111153590B (en) * | 2019-12-31 | 2022-03-25 | 江苏通鼎光棒有限公司 | Germanium tetrachloride tympanic bulla device of high accuracy |
| CN113666625A (en) * | 2021-07-30 | 2021-11-19 | 浙江富通光纤技术有限公司 | Method for processing prefabricated rod |
| CN114646434A (en) * | 2022-03-20 | 2022-06-21 | 山西太钢不锈钢股份有限公司 | Automatic detection device for air tightness of all-hydrogen bell-type furnace load space and use method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN211946809U (en) | Germanium tetrachloride tympanic bulla device of high accuracy | |
| EP1148033B1 (en) | Oxy-boost control in furnaces | |
| EP0018068B1 (en) | Adjustable vapour deposition apparatus | |
| JP5399798B2 (en) | Optical fiber preform manufacturing method and optical fiber preform manufacturing apparatus | |
| EP2145864B1 (en) | Quartz glass manufacturing method and quartz glass manufacturing apparatus | |
| CN104788014B (en) | A kind of preform prepares and the method for drawing optical fibers | |
| EP2166271A2 (en) | Hydrogen supply equipment | |
| CN111153590B (en) | Germanium tetrachloride tympanic bulla device of high accuracy | |
| CN112876044A (en) | Chemical deposition method and device for high-purity low-hydroxyl high-uniformity quartz glass | |
| EP1517863B1 (en) | Method and device for vaporizing a liquid reactant in manufacturing a glass preform | |
| EP0200215B1 (en) | Raw material supplying device and process for using this device | |
| CN101481207B (en) | Apparatus for manufacturing optical fiber preform part | |
| CN200988773Y (en) | Device for preparing high optic uniformity CVDZnS ball cover | |
| CN100387525C (en) | Equipment and technique for fabricating large size CVD ZnS material in high evenness | |
| CN110923676B (en) | Annealing equipment and process for multispectral zinc sulfide window | |
| CN106277744A (en) | A kind of high deposition rate PCVD technique makes the method for single-mode fiber plug | |
| CN111548002B (en) | Method for producing porous glass base material for optical fiber | |
| US20190112216A1 (en) | Fabrication apparatus and fabrication method for porous glass base material | |
| CN112299702A (en) | OVD deposition equipment and method for automatically adjusting deposition speed to match target weight | |
| CN214218577U (en) | OVD (over-the-counter) deposition equipment capable of automatically adjusting deposition speed to match target weight | |
| US11878929B2 (en) | Manufacturing apparatus and manufacturing method of porous glass base material | |
| CN218860552U (en) | Branch purging valve mechanism and glass kiln bubbling system control cabinet structure | |
| CN114735926A (en) | Device and method for preparing high-quality quartz for semiconductor mask | |
| JPS6081035A (en) | Manufacture of base material for optical fiber | |
| JPH0332501Y2 (en) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20220815 Address after: 215233 Xiaoping Avenue, eight Town, Zhen Ze town, Wujiang District, Suzhou, Jiangsu 8 Patentee after: TONGDING INTERCONNECTION INFORMATION Co.,Ltd. Patentee after: JIANGSU TONGDING OPTICAL WAND Co.,Ltd. Address before: 215000 no.583 Caizi Road, Wujiang Economic and Technological Development Zone, Suzhou City, Jiangsu Province Patentee before: JIANGSU TONGDING OPTICAL WAND Co.,Ltd. |
|
| TR01 | Transfer of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20201117 |