CN218951493U - Vacuum control system of chemical vapor deposition furnace for preparing zinc sulfide and zinc selenide materials - Google Patents
Vacuum control system of chemical vapor deposition furnace for preparing zinc sulfide and zinc selenide materials Download PDFInfo
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- CN218951493U CN218951493U CN202223185255.9U CN202223185255U CN218951493U CN 218951493 U CN218951493 U CN 218951493U CN 202223185255 U CN202223185255 U CN 202223185255U CN 218951493 U CN218951493 U CN 218951493U
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Abstract
The utility model discloses a vacuum control system of a chemical vapor deposition furnace for preparing zinc sulfide and zinc selenide materials, which comprises a deposition furnace, a filter vat, an electric vacuum pressure control valve and a vacuum pump which are sequentially connected in series by adopting a vacuum pipeline, wherein a vacuum meter cooling device is arranged on the vacuum pipeline between the deposition furnace and the filter vat, the vacuum meter cooling device is connected with a resistance vacuum meter and a film vacuum meter, the electric vacuum pressure control valve comprises a valve body, a valve core, a position sensor and a motor assembly, the valve core is arranged in the valve body, the position sensor is arranged on the surface of the valve body and acquires threshold signals of the maximum stroke and the minimum stroke of the valve core, the motor assembly is connected with the valve core and controls the valve core to act, and the electrode control device is connected with a controller through a signal converter and is also connected with the film vacuum meter. The utility model can accurately measure the vacuum degree in the ZnS and ZnSe deposition process and realize the accurate control of the reaction pressure.
Description
Technical Field
The utility model relates to the technical field of vacuum equipment, in particular to a vacuum control system of a chemical vapor deposition furnace for preparing zinc sulfide and zinc selenide materials.
Background
Zinc sulfide (ZnS) and zinc selenide (ZnSe) are two important infrared optical materials, and have wide application in the fields of infrared thermal imaging and CO2 lasers, and the preparation method mainly comprises a hot pressing method (HP), a physical vapor deposition method (PVD) and a chemical vapor deposition method (CVD), wherein ZnS and ZnSe optical materials prepared by adopting a CVD technology have the advantages of high purity, high density, small absorption, excellent optical performance and the like, are easy to realize large-size material preparation, and are the main stream technology for producing high-quality ZnS and ZnSe materials at present. The basic principle is as follows: by Zn and H 2 S(H 2 Se) as raw material, inert gas as carrier and diluent gas, zn steam and H under the unloading of inert gas 2 S(H 2 Se) gas enters a deposition chamber to react Zn+H on a heated graphite substrate 2 S(e)＝ZnS(e)+H 2 The residual gas is exhausted from the deposition chamber through a vacuum system. The process for preparing ZnS and ZnSe materials by chemical vapor deposition technology has the following characteristics: (1) The feedstock does not react completely within the deposition chamber, typically at about 98%, and the Zn vapor entering the deposition chamber is typically kept in excess, typically Zn and H, to control the quality of the material 2 S(H 2 Se) is 1.1:1, residual Zn vapour and H 2 S(H 2 Se) enters a vacuum system along with the discharge of inert gas, zn steam becomes solid Zn powder in the vacuum system, and H 2 S(H 2 Se) gas is unstable at high temperature and is partially decomposed to produce S (Se) powder. (2) The deposition reaction is carried out under heating, with a typical deposition chamber temperature of 600-800 ℃. (3) The deposition period is long, and the typical deposition period is 20-30 days, like the thickness of prism-grade ZnSe exceeds 70mm, and the deposition period is more than 50 days.
In the chemical vapor deposition technology, the reaction pressure and the vacuum degree of a deposition chamber in the deposition process are important factors influencing the quality of deposited materials, and the vacuum degree in the deposition process needs to be accurately controlled. The deposition process of ZnS and ZnSe materials is analyzed, and factors influencing vacuum accurate control are as follows:
(1) Powder is generated in the deposition process, and the accumulation of the powder generates resistance to influence the pumping force of a vacuum system along with the extension of time, so that the vacuum degree is a continuously-changing process;
(2) The residual gas containing H 2 、H 2 S (e) component, wherein the gas temperature is higher, and the vacuum gauge is usually close to the deposition chamber, so that the accuracy, stability and repeatability of the measurement of the vacuum gauge are affected;
(3) Instability of the vacuum system caused by continuous operation for a long time.
Therefore, a vacuum system which is suitable for the deposition characteristics of ZnS and ZnSe materials and can stably realize the accurate control of the reaction vacuum degree in the long-time deposition process is designed, and is one of key factors for preparing high-quality ZnS and ZnSe materials.
Disclosure of Invention
The utility model aims to solve the technical problems and provide a vacuum control system of a chemical vapor deposition furnace for preparing zinc sulfide and zinc selenide materials, which can accurately measure the vacuum degree in the ZnS and ZnSe deposition process and realize the accurate control of the reaction pressure.
In order to solve the technical problems, the utility model provides a vacuum control system of a chemical vapor deposition furnace for preparing zinc sulfide and zinc selenide materials, which comprises a deposition furnace, a filter vat, an electric vacuum pressure control valve and a vacuum pump which are sequentially connected in series by adopting vacuum pipelines, wherein a vacuum gauge cooling device is arranged on the vacuum pipeline between the deposition furnace and the filter vat, the vacuum gauge cooling device is connected with a resistance vacuum gauge and a film vacuum gauge, the electric vacuum pressure control valve comprises a valve body, a valve core, a position sensor and a motor component, the valve core is arranged in the valve body, the position sensor is arranged on the surface of the valve body and collects threshold signals of the maximum stroke and the minimum stroke of the valve core, the motor component is connected with the valve core and controls the valve core to act, and the motor component is connected with a controller through a signal converter and is also connected with the film vacuum gauge.
Further, the resistance vacuum metering processIs 10 -1 Pa—10 5 Pa; the measuring range of the film vacuum gauge is 10Pa-10KPa.
Further, the vacuum gauge cooling device is of a tubular structure and is provided with an inner wall interlayer, a spiral metal pipeline is arranged in the inner wall interlayer, and two ends of the spiral metal pipeline are respectively connected with a cooling inlet pipe and a cooling outlet pipe.
Further, the valve core is of a V-shaped structure.
Further, the filter vat is double-deck water-cooling structure, the filter vat is inside to be equipped with high temperature filter bag.
Further, a three-way pipe is arranged on the vacuum pipeline between the vacuum pump and the electric vacuum pressure control valve, a first vacuum pump electromagnetic valve is arranged between the vacuum pump and one end of the three-way pipe, the other end of the three-way pipe is connected with a second vacuum pump electromagnetic valve, and the second vacuum pump electromagnetic valve is connected with a standby pump.
Furthermore, the vacuum pipelines at two sides of the electric vacuum pressure control valve are connected through a bypass pipeline, and a bypass electromagnetic valve is arranged on the bypass pipeline.
Further, the controller is programmable and has a PID adjustment function.
The utility model has the beneficial effects that:
(1) The dual-path vacuum gauge is adopted, the background vacuum stage of the deposition furnace is pumped before the deposition is started, and the vacuum degree of the deposition furnace is measured by the resistance vacuum gauge in the cooling process after the deposition is finished, so that the pressure is not required to be controlled, the selection of the measuring range of the film vacuum gauge is facilitated, and the measurement sensitivity of the film vacuum gauge is improved; the gas pumped from the deposition furnace at this stage passes through the filter barrel and then goes through the bypass pipeline, and at this time, the electric vacuum pressure control valve is in a closed state, so that the gas is prevented from passing through a narrow channel between the valve core and the valve seat in the control valve, the efficiency is improved, and meanwhile, the maximum stroke of the valve core can be designed according to the flow rate of the reaction gas and the control parameter of the reaction pressure, and the sensitivity of controlling the vacuum degree is improved.
(2) The vacuum gauge cooling device is designed, the influence of high-temperature gas on the measurement accuracy of the resistance vacuum gauge and the film vacuum gauge can be reduced, in addition, the film vacuum gauge is adopted for measuring the vacuum degree in the deposition stage, feedback data are used for controlling, the interference of gas components on vacuum measurement values is avoided, and the accuracy, stability and reliability of vacuum measurement are improved.
(3) The filter vat is arranged on the vacuum pipeline, so that the influence of powder generated in the deposition process on the rear end valve and the vacuum pump can be effectively prevented, and the stability of the vacuum system is ensured.
(4) The electric vacuum pressure control valve is electrically driven, so that the problem of poor sensitivity of pneumatic driving caused by unstable pressure is avoided, and the valve core is of a V-shaped structure and has higher sensitivity. The motor component can enable the valve core to reciprocate along the central line, so that the flow area between the valve core and the valve seat is changed, and the purpose of regulating and controlling the pressure is achieved.
Drawings
FIG. 1 is a schematic diagram of a vacuum control system of a chemical vapor deposition furnace according to the present utility model;
FIG. 2 is a schematic cross-sectional view of a cooling device for a vacuum gauge according to the present utility model.
Detailed Description
The present utility model will be further described with reference to the accompanying drawings and specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the utility model and practice it.
Referring to FIG. 1, an embodiment of a vacuum control system of a chemical vapor deposition furnace for preparing zinc sulfide and zinc selenide materials of the utility model comprises a deposition furnace 2, a filter vat 3, an electric vacuum pressure control valve 4 and a vacuum pump 5 which are sequentially connected in series by adopting a vacuum pipeline 1, wherein the vacuum pump vacuumizes the deposition furnace through the vacuum pipeline, powder generated in the deposition furnace can be blocked by the filter vat, the subsequent electric vacuum pressure control valve and the vacuum pump are prevented from being blocked, the performance is influenced, the electric vacuum pressure control valve regulates the pressure, and the vacuum pressure is controlled with high precision; because the deposition furnace has higher temperature in the vacuumizing process, the filter vat is designed into a double-layer water-cooling structure, and the high-temperature filter bag 14 is arranged in the filter vat, so that the powder is effectively blocked while the temperature is reduced.
A vacuum gauge cooling device 6 is arranged on a vacuum pipeline between the deposition furnace and the filter vat, the vacuum gauge cooling device is connected with a resistance vacuum gauge 8 and a film vacuum gauge 9, and the range of the resistance vacuum gauge is 10 -1 Pa—10 5 Pa; the measuring range of the film vacuum gauge is 10Pa-10KPa; the resistance vacuum gauge is used for measuring the vacuum degree of the deposition furnace, the measuring range is large, and the film vacuum gauge is used for participating in measurement when controlling the pressure. Referring to fig. 2, the vacuum gauge cooling device is of a tubular structure and is provided with an inner wall interlayer 21, a spiral metal pipeline 22 is arranged in the inner wall interlayer, two ends of the spiral metal pipeline are respectively connected with a cooling inlet pipe 23 and a cooling outlet pipe 24, the cooling mode can be water cooling or air cooling, the cooling effect is good, the structure is simple, and high-temperature gas can be cooled by the vacuum gauge cooling device in the vacuumizing process, so that the accuracy, stability and repeatability of measurement of the resistance vacuum gauge and the film vacuum gauge are ensured.
The electric vacuum pressure control valve comprises a valve body 10, a valve core, a position sensor and a motor component 11, wherein the valve core is arranged in the valve body, the position sensor is arranged on the surface of the valve body and is used for collecting threshold signals of the maximum stroke and the minimum stroke of the valve core, the motor component is connected with the valve core and controls the valve core to act, the motor component is connected with a controller 13 through a signal converter 12, the controller is further connected with a film vacuum gauge, the input end of the signal converter is connected with the output end of the controller through a signal cable, the output end of the signal converter is connected with a motor control device of the motor component through the signal cable, the controller is used for collecting data measured by the film vacuum gauge, after processing, a digital instruction is sent to the signal converter, the signal converter is used for converting the digital signal into an analog signal to be transmitted to the motor control device, and driving the valve core to move, and the flow area between the valve core and a valve seat is changed. The electric vacuum pressure control valve is electrically driven, so that the problem of poor sensitivity of pneumatic driving caused by unstable pressure is avoided, and the valve core is of a V-shaped structure and has higher sensitivity. The valve core can reciprocate along the central line by adjusting the rotating speed and the direction of the motor component, so that the flow area between the valve core and the valve seat of the valve body is changed, and the purposes of regulating and controlling the pressure and adjusting the response time are achieved. The maximum stroke threshold of the valve core is set through the position sensor, so that the flux requirement is met.
A three-way pipe 15 is arranged on a vacuum pipeline between the vacuum pump and the electric vacuum pressure control valve, a first vacuum pump electromagnetic valve 16 is arranged between the vacuum pump and one end of the three-way pipe, the other end of the three-way pipe is connected with a second vacuum pump electromagnetic valve 17, the second vacuum pump electromagnetic valve is connected with a standby pump 18, when the vacuum pump works abnormally, the standby pump can continue to vacuumize, and the two vacuum pumps are in a logic interlocking relationship, namely, only one vacuum pump and the electromagnetic valve are in an electrified starting state. The vacuum pipelines at the two sides of the electric vacuum pressure control valve are also connected through a bypass pipeline 19, a bypass electromagnetic valve 20 is arranged on the bypass pipeline, and the electric vacuum pressure control valve has larger flow and improves efficiency in the process of pumping the background vacuum of the deposition furnace before the deposition and cooling after the deposition is finished. The controller is programmable and has PID regulating function, which satisfies the effect of high-precision regulation.
Specifically, the ZnS material is prepared by adopting the system:
installing a crucible and a deposition chamber containing raw material Zn in a deposition furnace, vacuumizing, discharging gas through a filter barrel along a bypass pipeline through a vacuum pump, closing an electric vacuum control valve, when the vacuum degree of the deposition chamber is measured by a resistance vacuum gauge to be less than 10Pa, starting crucible heating and deposition chamber heating, when the temperature of the deposition chamber reaches 650 ℃, closing a bypass electromagnetic valve on the bypass pipeline after the temperature of the crucible reaches 580 ℃, starting the electric vacuum control valve, discharging gas through the filter barrel and the electric vacuum control valve through the vacuum pump, and discharging raw material gas H 2 The mixed gas of S and Ar is controlled by a gas mass flow meter to be introduced into a deposition chamber, ar gas is controlled by the gas mass flow meter to be introduced into a crucible to carry Zn steam into the deposition chamber, a controller is started to control, the vacuum degree control value is set to be 5000+/-50 Pa, and deposition is started. In the deposition process, the film vacuum gauge transmits signals to the controller, the controller processes the signals and then sends digital instructions to the signal converter, the signal converter converts the digital signals into analog signals and transmits the analog signals to the motor control device, the corresponding action of the valve core is driven, the deposition process is finished after lasting for 20 days, the gas mass flowmeter is closed, the electric vacuum control valve is closed, and the bypass pipe is startedAnd (5) starting a cooling program until the temperature reaches the room temperature.
The process parameters recorded by the controller show that the vacuum degree is 5000+/-100 Pa, the lowest value is 4935Pa, and the highest value is 5070Pa in the whole deposition process.
ZnS material with the maximum dimension phi 450 mm is prepared, and the absorption coefficient (@10.6 μm) is smaller than 0.2cm after test -1 The optical uniformity (@ 10.6 μm) was better than 100ppm and the performance was excellent.
The ZnSe material is prepared by adopting the system:
the crucible containing raw material Zn and the deposition chamber are arranged in a deposition furnace, background vacuum is pumped, at the moment, gas is discharged through a vacuum pump along a bypass pipeline through a filter vat, an electric vacuum control valve is closed, when the vacuum degree of the deposition chamber is measured by a resistance vacuum gauge and is smaller than 10Pa, the crucible is started to heat, the deposition chamber is heated, when the temperature of the deposition chamber reaches 750 ℃, the crucible temperature reaches 560 ℃, the bypass pipeline is closed, the electric vacuum control valve is started, at the moment, gas is discharged through the filter vat and the electric vacuum control valve through the vacuum pump, mixed gas of raw material gas H2Se and Ar is controlled by a gas mass flowmeter to be introduced into the deposition chamber, ar gas is controlled by the gas mass flowmeter to be introduced into the crucible to carry Zn steam into the deposition chamber, an automatic control program of a controller is started, a vacuum degree control value is set to 3000+/-50 Pa, and deposition is started. In the deposition process, the film vacuum gauge transmits signals to the controller, the controller processes the signals and then sends digital instructions to the signal converter, the signal converter converts the digital signals into analog signals and transmits the analog signals to the motor control device, the corresponding action of the valve core is driven, the deposition process is finished after lasting 40 days, the gas mass flowmeter is closed, the electric vacuum control valve is closed, the bypass pipeline is started, and the cooling program is started until the temperature reaches the room temperature.
The process parameters recorded by the controller show that the vacuum degree is 3000+/-100 Pa, the lowest value is 2910Pa, and the highest value is 3095Pa in the whole deposition process. ZnSe material with maximum dimension phi 300 x 50mm is prepared, and the absorption coefficient (@10.6 μm) is smaller than 0.0005cm after test -1 The optical uniformity (@ 0.633 μm) was better than 3ppm and the performance was excellent.
Stability was tested against the above system:
a frequency converter is added to the vacuum pump, and the frequency can be continuously changed between 0 and 50.
Installing a crucible and a deposition chamber containing raw material Zn in a deposition furnace, vacuumizing, exhausting gas through a filter barrel along a bypass pipeline and a vacuum pump, closing an electric vacuum control valve, when the vacuum degree of the deposition chamber is measured by a resistance vacuum gauge to be less than 10Pa, starting crucible heating and deposition chamber heating, when the temperature of the deposition chamber reaches 650 ℃, closing the bypass pipeline, starting the electric vacuum control valve, exhausting gas through the filter barrel and the electric vacuum control valve and the vacuum pump, and discharging raw material gas H 2 The mixed gas of S and Ar is controlled by a gas mass flow meter to be introduced into a deposition chamber, ar gas is controlled by the gas mass flow meter to be introduced into a crucible to carry Zn steam into the deposition chamber, a controller is started, the vacuum degree control value is set to be 5000+/-50 Pa, and deposition is started. In the deposition process, the film vacuum gauge transmits signals to the controller, the controller processes the signals and then sends digital instructions to the signal converter, and the signal converter converts the digital signals into analog signals and transmits the analog signals to the motor control device to drive the valve core to act correspondingly.
After the deposition process, the frequency of the frequency converter is adjusted to be 10, the pumping speed of the vacuum pump is reduced, the vacuum value of the deposition chamber is increased, the valve core of the electric vacuum control valve is lifted to the maximum travel threshold value, the controller is triggered to give an instruction, a buzzing alarm is sent out, the vacuum pump and the first vacuum pump electromagnetic valve are closed, the standby pump and the second vacuum pump electromagnetic valve are started, the valve core falls back, the alarm is finished, and the regulation and control functions of the electric vacuum control valve are recovered until the vacuum degree is stabilized in the set control value range. And after the deposition is continued for 15 days, closing the gas mass flowmeter, closing the electric vacuum control valve, starting the bypass pipeline, and starting the cooling program until the temperature reaches the room temperature.
The process parameters recorded by the controller show that the time from the start of adjusting the frequency converter to the restoration of the vacuum degree to the control value lasts less than 1 minute, the highest vacuum value 5150Pa, the lowest vacuum value 4902Pa and the change of the vacuum degree in the rest time period are all in a normal range.
ZnS material with the maximum dimension phi of 450 mm is prepared, the absorption coefficient (@10.6 μm) is smaller than 0.2cm < -1 > through test, the optical uniformity (@10.6 μm) is better than 100ppm, the performance is excellent, the performance of the ZnS material is not different from that of the material prepared in the normal deposition process, and the system can ensure the stability and the material quality in the long-time deposition process.
The utility model can realize the intelligent and accurate control of the vacuum degree of the deposition furnace when preparing the zinc sulfide and zinc selenide materials by chemical vapor deposition, can control the vacuum degree to any value of 10Pa-10KPa, improves the accuracy and sensitivity of reaction pressure control, and can continuously work stably and reliably for a long time, thereby preparing high quality so as to improve the quality of ZnS and ZnSe materials.
The above embodiments are only for illustrating the technical solution of the present utility model, and are not limiting thereof; although the utility model has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present utility model.
Claims (7)
1. The utility model provides a preparation zinc sulfide, zinc selenide material's chemical vapor deposition stove vacuum control system, its characterized in that includes deposition stove, filter vat, electronic vacuum pressure control valve and the vacuum pump that adopts the vacuum pipeline to establish ties in proper order, be provided with vacuum gauge cooling device on the vacuum pipeline between deposition stove and the filter vat, vacuum gauge cooling device is connected with resistance vacuum gauge and film vacuum gauge, electronic vacuum pressure control valve includes valve body, case, position sensor and motor element, the case sets up in the valve body, position sensor sets up at the valve body surface and gathers the maximum and minimum threshold value signal of stroke of case, and motor element is connected and control the case action with the case, motor element passes through signal converter and is connected with the controller, the controller is still connected with film vacuum gauge.
2. The vacuum control system of the chemical vapor deposition furnace for preparing zinc sulfide and zinc selenide materials according to claim 1, wherein the vacuum gauge cooling device is of a tubular structure and is provided with an inner wall interlayer, a spiral metal pipeline is arranged in the inner wall interlayer, and two ends of the spiral metal pipeline are respectively connected with a cooling inlet pipe and a cooling outlet pipe.
3. The vacuum control system of chemical vapor deposition furnace for preparing zinc sulfide and zinc selenide materials according to claim 1, wherein the valve core is of a V-shaped structure.
4. The vacuum control system of the chemical vapor deposition furnace for preparing zinc sulfide and zinc selenide materials according to claim 1, wherein the filter vat is of a double-layer water-cooling structure, and a high-temperature filter bag is arranged inside the filter vat.
5. The vacuum control system of the chemical vapor deposition furnace for preparing zinc sulfide and zinc selenide materials according to claim 1, wherein a three-way pipe is arranged on a vacuum pipeline between the vacuum pump and the electric vacuum pressure control valve, a first vacuum pump electromagnetic valve is arranged between the vacuum pump and one end of the three-way pipe, the other end of the three-way pipe is connected with a second vacuum pump electromagnetic valve, and the second vacuum pump electromagnetic valve is connected with a standby pump.
6. The vacuum control system of the chemical vapor deposition furnace for preparing zinc sulfide and zinc selenide materials according to claim 5, wherein the vacuum pipelines at two sides of the electric vacuum pressure control valve are connected through a bypass pipeline, and a bypass electromagnetic valve is arranged on the bypass pipeline.
7. The chemical vapor deposition furnace vacuum control system for preparing zinc sulfide and zinc selenide materials according to claim 1, wherein the controller is programmable and has a PID regulating function.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202223185255.9U CN218951493U (en) | 2022-11-30 | 2022-11-30 | Vacuum control system of chemical vapor deposition furnace for preparing zinc sulfide and zinc selenide materials |
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| CN202223185255.9U CN218951493U (en) | 2022-11-30 | 2022-11-30 | Vacuum control system of chemical vapor deposition furnace for preparing zinc sulfide and zinc selenide materials |
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