CN114152322B - Monitoring device for chemical vapor deposition liquid source material - Google Patents
Monitoring device for chemical vapor deposition liquid source material Download PDFInfo
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- CN114152322B CN114152322B CN202111475259.8A CN202111475259A CN114152322B CN 114152322 B CN114152322 B CN 114152322B CN 202111475259 A CN202111475259 A CN 202111475259A CN 114152322 B CN114152322 B CN 114152322B
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- liquid source
- flexible metal
- metal hose
- vapor deposition
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01G—WEIGHING
- G01G17/00—Apparatus for or methods of weighing material of special form or property
- G01G17/04—Apparatus for or methods of weighing material of special form or property for weighing fluids, e.g. gases, pastes
Abstract
The invention relates to a monitoring device for chemical vapor deposition liquid source materials. The liquid source bottle is used for containing reaction source materials of the chemical vapor deposition coating; the liquid source bottle is placed on a tray, and the tray is fixed on the weight sensor. The weight sensor monitors the change of the total weight of the tray and the liquid source bottle to monitor the residual amount of the liquid source in real time; an inlet and an outlet of the liquid source bottle are provided with automatic stop valves, and the other ends of the automatic stop valves are connected with a chemical vapor deposition coating system through flexible metal hoses; the vacuum gauge is connected with the flexible metal hose and used for monitoring the vacuum degree in the flexible metal hose. The chemical vapor deposition source material monitoring device realizes the monitoring of the residual material in the chemical reaction liquid source bottle and can effectively improve the use efficiency and the safety of the chemical vapor deposition source material.
Description
Technical Field
The invention relates to the technical field of coating, in particular to a device for monitoring chemical vapor deposition liquid source materials, which is a device for monitoring the residual amount of the chemical vapor deposition liquid source materials in a liquid source bottle.
Background
Chemical vapor deposition is a coating technique with a wide range of applications. The technique utilizes one or more source materials containing film elements to chemically react on the surface of a substrate to form a solid film. Chemical vapor deposition has been widely used for purifying materials, developing new crystals, preparing various single crystal, polycrystalline or glassy inorganic thin film materials, deriving atomic layer deposition, organometallic chemical vapor deposition and other key coating techniques with great significance in the semiconductor field.
The chemical source material is the core for realizing the chemical vapor deposition technology, and the source material capable of realizing the chemical vapor deposition is usually gas and liquid, so that the chemical vapor deposition method has higher value; the chemical activity is high, and chemical reaction and even explosion can occur when the air leaks; on the other hand, the source materials are generally highly toxic and leakage in the air can endanger the life and environmental safety of personnel. The chemical source material is therefore typically stored in dedicated cylinders. In the chemical vapor deposition process, the steel cylinder is replaced when the residual quantity of the source material reaches a certain value by monitoring the source material in the steel cylinder in real time, so that the utilization rate of the source material can be effectively improved, the waste and the environmental pollution caused by excessive residual source material are avoided, or the life safety of dangerous workers is leaked in the re-canning process. On the other hand, the monitoring of the residual materials in the source bottle can avoid coating failure caused by insufficient source materials and improve the chemical vapor deposition efficiency.
Disclosure of Invention
The invention provides a monitoring device for a chemical vapor deposition liquid source material, which can monitor the weight of a liquid source in a steel cylinder in real time and realize the real-time monitoring of the residual amount of the liquid source.
The invention adopts the following technical scheme:
the utility model provides a monitoring devices of chemical vapor deposition liquid source material, includes liquid source bottle, tray, weighing sensor, first pneumatic stop valve, first flexible metal collapsible tube, first vacuum gauge.
The liquid source bottle is used for containing reaction source materials of the chemical vapor deposition coating; the liquid source bottle comprises a stainless steel bottle body, a liquid injection port, a gasified liquid output port and a first manual stop valve on a pipeline of the gasified liquid output port, wherein the liquid injection port and the gasified liquid output port are positioned on the stainless steel bottle body; the gasified liquid outlet is connected with a gasified liquid outlet pipeline.
Optionally, the liquid source bottle includes a carrier gas injection port and a second manual shut-off valve for the carrier gas injection port. The carrier gas injection port is positioned on the stainless steel bottle body, the carrier gas injection port is connected with a carrier gas injection port pipeline, and the second manual stop valve is arranged on the carrier gas injection port pipeline. The liquid injection port is sealed after injecting the liquid source material.
The liquid source bottle is placed on a tray, the tray is fixed on a weight sensor, and the weight sensor monitors the change of the total weight of the tray and the liquid source bottle to monitor the residual amount of the liquid source in real time;
the first pneumatic stop valve is arranged on one side, away from the liquid container, of the first manual stop valve, and the other end of the first pneumatic stop valve is connected with the chemical vapor deposition coating system through a flexible metal hose;
the first vacuum gauge is fixed on the chemical vapor deposition coating system and connected with the first flexible metal hose through a first tee joint for monitoring the vacuum degree in the flexible metal hose.
The monitoring device for the chemical vapor deposition liquid source material further comprises a mass flow meter of carrier gas, a second manual stop valve, a second pneumatic stop valve, a second flexible metal hose, a second vacuum gauge, a third stop valve and the like for a liquid source bottle needing carrier gas.
The mass flow meter is used for injecting inert gas into the liquid source bottle, the second pneumatic stop valve is installed on one side, far away from the stainless steel bottle body, of the second manual stop valve, the other end of the second pneumatic stop valve is connected with the mass flow meter through a second flexible metal hose, and the second vacuum gauge is connected with the second flexible metal hose through a second tee joint; and the mass flow meter and the second vacuum gauge are fixed on the chemical vapor deposition coating system.
The second flexible metal hose is connected with the vacuum pump through a third tee joint, and is connected with and disconnected from the vacuum pump through a third stop valve. The third stop valve is a manual or automatic stop valve.
The monitoring device for the chemical vapor deposition liquid source material is used for monitoring the weight of the liquid source, and comprises the following working processes:
(1) Measuring the weight m of an empty liquid source bottle 1 ；
(2) Before the liquid source is injected into the source bottle, the empty liquid source bottle is provided with a first pneumatic stop valve and a corresponding connecting pipeline at the output port of the source bottle, optionally, a second pneumatic stop valve and a corresponding connecting pipeline are arranged at the carrier gas injection port of the source bottle, and the total weight m is measured 2 ；
(3) And injecting a chemical vapor deposition liquid source material into the source bottle, sealing the source bottle, placing the source bottle on the tray, connecting the other outlet of the first pneumatic stop valve to the chemical vapor deposition coating system by using a first flexible metal hose, and optionally connecting the other outlet of the second pneumatic stop valve to the chemical vapor deposition coating system by using a second flexible metal hose. Recording weight sensor reading m 3 ；
(4) During the film coating process, the reading m of the weight sensor is monitored 3 If m is 3 ≤1.1×m 2 Replacing the source bottle;
(5) Measuring the weight m of a used source bottle 4 Then m is 4 -m 1 Is the weight of the remaining chemical reaction precursor in the source bottle.
The device for monitoring the chemical vapor deposition liquid source material comprises the following steps:
(1) Installing the outlet end of a first flexible metal hose connected with a liquid source bottle on a gas path of a chemical vapor deposition coating system;
(2) Keeping the first manual stop valve closed, keeping the first pneumatic stop valve closed, pumping the first flexible metal hose of the liquid output port by using a vacuum pump, and if the experiment vacuum degree V is reached 1 If the first flexible metal hose and the communicated gas circuit are normal, otherwise, the pipeline is overhauled until the experiment vacuum degree V is reached 1 ；
(3) Opening the first pneumatic stop valve, pumping the vacuum of the pipeline between the first flexible metal hose and the first manual stop valve by using a vacuum pump, and if the experimental vacuum degree V is reached 1 If not, the pipeline is overhauled until the experimental vacuum degree V can be reached 1 ；
(4) Opening the first manual stop valve at the outlet of the liquid source gas cylinder, and measuring the vacuum degree V in the flexible hose at the outlet 1 (ii) a Alternatively, for a liquid source bottle containing a carrier gas injection port, the following steps are also required:
(5) Installing the outlet end of a second flexible metal hose connected with a liquid source bottle on the gas path of a carrier gas inlet system; the gas path of the carrier gas inlet system comprises a second tee joint, a mass flow meter, a third tee joint and a third stop valve. The outlet of the third stop valve is connected to a vacuum pump.
(6) Keeping the second pneumatic stop valve closed, opening the third stop valve, pumping a second flexible metal hose of the carrier gas injection port by using a vacuum pump, and if the experimental vacuum degree V is reached 1 If the test vacuum degree V is not reached, the second flexible metal hose and the communicated gas circuit are judged to be normal, otherwise, the pipeline is overhauled until the test vacuum degree V is reached 1 。
(7) Opening the second pneumatic stop valve, and pumping the vacuum of the pipeline between the second flexible metal hose and the second pneumatic stop valve by using a vacuum pumpIf the experimental vacuum degree V is reached 1 If not, the pipeline is overhauled until the experimental vacuum degree V can be reached 1 (ii) a The third stop valve is closed.
(8) Injecting inert gas into the carrier gas inlet pipeline by using the mass flowmeter to enable the vacuum degree value V in the carrier gas inlet pipeline 2 Greater than V 1 And opening a second manual stop valve of the carrier gas injection port of the liquid source bottle, and stopping gas injection of the mass flowmeter.
In the monitoring device for the chemical vapor deposition liquid source material, the vacuum pump for pumping the vacuum of the metal hose uses a vacuum pump which works independently or a vacuum pump of a chemical vapor deposition coating system.
When the liquid source is not used, the first pneumatic stop valve and the second pneumatic stop valve are kept closed; when the liquid source is used, firstly, the first pneumatic stop valve and the second pneumatic stop valve are kept closed, the first flexible metal hose and the second flexible metal hose are respectively pumped by using a vacuum pump, if the experimental vacuum degree is reached, the flexible metal hose and a communicated gas circuit are judged to be normal, and the first pneumatic stop valve and the second pneumatic stop valve are respectively opened; otherwise, closing the first and second manual stop valves of the liquid source bottle, overhauling the pipeline until the experimental vacuum degree can be reached, re-opening the first manual stop valve according to the steps (2) - (4), and re-opening the second manual stop valve according to the steps (6) - (8).
In the monitoring device for the chemical vapor deposition liquid source material, the pneumatic stop valve is preferably a high-temperature-resistant stop valve.
According to the monitoring device for the chemical vapor deposition liquid source material, when the liquid source material is used, a vacuum gauge is used for measuring the vacuum degree in the flexible metal hose all the time, if the vacuum degree is remarkably poor, and if the vacuum degree is more than or equal to 0.5 atmosphere, the pneumatic stop valve is closed immediately, so that the liquid source is prevented from being leaked.
Compared with the monitoring method of the chemical vapor deposition liquid source material adopted at present, the invention has the technical advantages that:
(1) The method for monitoring the weight of the liquid source bottle is adopted, the universally applicable method for monitoring the amount of the liquid remaining in the steel bottle is provided, and the effective detection of the remaining amount of the liquid source is realized.
(2) By monitoring the residual quantity of the liquid in real time, the reliability of chemical vapor deposition can be ensured, and coating failure caused by liquid source exhaustion is reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1: a monitoring device for chemical vapor deposition liquid source material is disclosed.
FIG. 2 is a schematic diagram: a monitoring device for chemical vapor deposition liquid source material includes a carrier gas injection port and a vaporized liquid gas outlet port.
In the figure, 101 liquid source bottle, 102 tray, 103 weight sensor, 104 first manual stop valve, 105 first pneumatic stop valve, 106 first flexible metal hose, 107 first connector, 108 first tee, 109 first vacuum gauge, 110 vacuum chamber, 111 data transmission and control circuit, 112 industrial control computer, 201 carrier gas injection port, 202 second manual stop valve, 203 second pneumatic stop valve, 204 second flexible metal hose, 205 second connector, 206 second vacuum gauge, 207 second tee, 208 mass flowmeter, 209 third tee, 210 third stop valve.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
FIG. 1 shows a monitoring device for a chemical vapor deposition liquid source material containing only a vaporized liquid delivery outlet, comprising: the device comprises a liquid source bottle 101, a tray 102, a weight sensor 103, a first manual stop valve 104, a first pneumatic stop valve 105, a first flexible metal hose 106, a first joint 107, a first tee joint 108, a first vacuum gauge 109, a vacuum chamber 110, a data transmission and control circuit 111 and an industrial control computer 112.
The liquid source bottle 101 is used for containing reaction source materials of chemical vapor deposition coating, and comprises a stainless steel bottle body, a liquid injection port, a gasified liquid output port and a first manual stop valve 104 on a gasified liquid output port pipeline. The gasified liquid outlet is connected with a gasified liquid outlet pipeline, and the first manual stop valve 104 and the first pneumatic stop valve 105 are both arranged on the gasified liquid outlet pipeline. The liquid injection port and the gasified liquid output port are both arranged on the stainless steel bottle body. The gasified liquid outlet conduit is connected to a first flexible metal hose 106 through a first joint 107.
The liquid source bottle 101 is placed on a tray 102, the tray is fixed on a weight sensor 103, and a fastening structure is arranged on the tray and used for fixing the liquid source bottle.
The weight sensor 103 monitors the remaining amount of the liquid source in real time by monitoring the change of the total weight of the tray 102 and the liquid source bottle 101.
The first pneumatic stop valve 105 is installed on one side of the first manual stop valve 104 far away from the stainless steel bottle body, and the other end of the first pneumatic stop valve 105 is connected with the first flexible metal hose 106 through the first joint 107.
The first pneumatic stop valve 105 is preferably an all-metal vacuum stop valve with high temperature resistance.
The first flexible metal hose 106 is a stainless steel corrugated pipe. A first flexible metal hose 106 is connected to a first port of a first tee 108. The first vacuum gauge 109 is connected to the second port of the first tee 108, and the vacuum chamber 110 of the coating system is connected to the third port of the tee.
The first vacuum gauge 109 is fixed on the chemical vapor deposition coating system device and is used for monitoring the vacuum degree in the first flexible metal hose 106.
The data transmission and control circuit 111 inputs the readings of the weight sensor 103 and the first vacuum gauge 109 into the industrial computer 112, and outputs a control signal to the first pneumatic stop valve 105, which is output by the industrial computer 112.
The monitoring device for the chemical vapor deposition liquid source material is characterized in that the working process of monitoring the weight of the liquid source is as follows:
(1) Measuring the weight m of an empty liquid source bottle 101 1 ；
(2) Before the empty liquid source bottle 101 is filled with liquid, a first pneumatic stop valve 105 and corresponding connecting pipes are installed at the outlet of the source bottle, and the total weight m is measured 2 ；
(3) Injecting chemical vapor deposition liquid source material into the source bottle, sealing the source bottle, placing the source bottle on the tray 102, connecting another outlet of the first pneumatic stop valve 105 to the chemical vapor deposition coating system by a first flexible metal hose 106, and recording the reading m of the weight sensor 3 . The chemical vapor deposition coating system comprises a first tee joint 108, a first vacuum gauge 109, a vacuum chamber 110 and the like, wherein a first flexible metal hose 106 is connected with the chemical vapor deposition coating system through one port connected with the first tee joint 108.
(4) During the film coating process, the reading m of the weight sensor is monitored 3 If m is 3 ≤(1.1)×m 2 Then the source bottle is replaced;
(5) Measuring the weight m of a used source bottle 4 Then m is 4 -m 1 Is the weight of the remaining chemical reaction precursor in the source bottle.
In the monitoring device for chemical vapor deposition liquid source material, the first manual stop valve 104 is opened by:
(1) The outlet end of a first flexible metal hose 106 connected with the liquid source bottle 101 is arranged on the chemical vapor deposition coating system; the chemical vapor deposition coating system comprises a first tee joint 108, a first vacuum gauge 109, a vacuum chamber 110 and the like, wherein the first flexible metal hose 106 is connected with the chemical vapor deposition coating system through a first port connected with the first tee joint 108.
(2) Keeping the first manual cut-off valve 104 closed, keeping the first pneumatic cut-off valve 105 closed, pumping a first flexible metal hose 106 of the liquid outlet by a vacuum pump, if a certain vacuum degree V is reached 1 If not, the pipeline is overhauled until the specific vacuum degree V is reached 1 ；
(3) The first pneumatic cut-off valve 105 is opened and the vacuum in the line between the first flexible metal hose 106 and the first manual cut-off valve 104 and the first pneumatic cut-off valve 105 is pumped by means of a vacuum pump if a certain vacuum degree V is reached 1 If not, the pipeline is overhauled until the specific vacuum degree V can be reached 1 ；
(4) The first manual stop valve 104 at the outlet of the liquid source bottle 101 is opened, and the vacuum degree V in the flexible hose at the outlet is measured 1 ；
When the liquid source is not in use, the first pneumatic stop valve 105 remains closed; when using a liquid source, the first pneumatic stop valve 105 is first kept closed and the first flexible metal hose 106 is pumped with a vacuum pump if a certain vacuum level V is reached 1 If the first flexible metal hose 106 and the gas path communicated with the first flexible metal hose are normal, the first pneumatic stop valve 105 is opened; otherwise, the first manual stop valve 104 of the liquid source bottle 101 is closed, the pipeline is overhauled until a certain vacuum degree can be reached, and the first manual stop valve is reopened according to the process described in the steps (2) to (4). In the present invention, the specific vacuum degree generally means a vacuum degree required to be set for an experiment.
During the use of the liquid source material, the first step is utilizedA vacuum gauge 109 measures the vacuum V in the first flexible metal hose 106 from beginning to end 1 If the vacuum degree is obviously poor, for example, the vacuum degree is more than or equal to 0.5 atmosphere, the first pneumatic stop valve 105 is immediately closed to avoid the leakage of the liquid source.
Example 2
Fig. 2 shows another embodiment of the present invention, which is different from fig. 1 in that: for the liquid source bottle 101 requiring carrier gas, the source bottle does not include a vaporized liquid outlet, and further includes a carrier gas inlet 201, and a second manual stop valve 202 of the carrier gas inlet 201. The monitoring device is characterized in that a second pneumatic stop valve 203, a second flexible metal hose 204, a second connector 205, a second vacuum gauge 206, a second tee 207, a mass flow meter 208, a third tee 209 and a third stop valve 210 are sequentially connected to the second manual stop valve 202 in the direction away from the source bottle 101.
The carrier gas injection port 201 is located on the stainless steel bottle body of the liquid source bottle 101, the carrier gas injection port 201 is connected with a carrier gas injection port pipeline, and the second manual stop valve 202 and the second pneumatic stop valve 203 are both arranged on the carrier gas injection port pipeline. The carrier gas injection inlet conduit is in communication with the second flexible metal hose 204. A second flexible metal hose 204 is connected to a first port of a second tee 207 by a second connector 205.
The second vacuum gauge 206 is connected to a second port of the second tee 207, connected to the second flexible metal hose 204 through the second tee 207, and fixed to the chemical vapor deposition coating system apparatus, for monitoring a vacuum degree in the second flexible metal hose 204.
The mass flow meter 208 is connected to a third port of the second tee for injecting carrier gas into the second flexible metal hose 204, thereby promoting the vaporization of the liquid in the liquid source bottle 101. The carrier gas is an inert gas.
The second flexible metal hose 204 is also connected with the vacuum pump through a third tee 209, and is controlled to be connected with and disconnected from the vacuum pump through a third stop valve 210. The third shut-off valve 210 may be a manual or pneumatic shut-off valve.
For the monitoring device of the chemical vapor deposition liquid source material comprising the carrier gas injection port, the opening method of the manual valve is as follows:
(1) The outlet end of a first flexible metal hose 106 connected with the liquid source bottle 101 is arranged on the chemical vapor deposition coating system;
(2) Keeping the first manual cut-off valve 104 closed, keeping the first pneumatic cut-off valve 105 closed, pumping a first flexible metal hose 106 of the liquid outlet by means of a vacuum pump, if a certain vacuum degree V is reached 1 If the first flexible metal hose and the communicated gas circuit are normal, otherwise, the pipeline is overhauled until a specific vacuum degree V is reached 1 ；
(3) The first pneumatic cut-off valve 105 is opened and the vacuum in the line between the first flexible metal hose 106 and the first manual cut-off valve 104 is pumped by means of a vacuum pump if a certain vacuum level V is reached 1 If not, the pipeline is overhauled until the specific vacuum degree V can be reached 1 ；
(4) The first manual cut-off valve 104 of the outlet of the liquid source bottle 101 is opened, and the vacuum degree V in the first flexible metal hose 106 of the outlet is measured 1 ；
(5) The outlet end of a second flexible metal hose 204 connected with the liquid source bottle 101 is arranged on the gas path of the carrier gas inlet system; the gas path of the carrier gas inlet system comprises a second tee 207, a mass flow meter 208, a third tee 209 and a third stop valve 210. The outlet of the third shut-off valve 210 is connected to a vacuum pump.
(6) Keeping the second manual cut-off valve 202 closed, keeping the second pneumatic cut-off valve 203 closed, opening the third cut-off valve 210, pumping the second flexible metal hose 204 of the carrier gas injection port by using a vacuum pump, and if the experimental vacuum degree V is reached 1 If not, the pipeline is overhauled until the experimental vacuum degree V is reached 1 ；
(7) The second pneumatic stop valve 203 is opened, the vacuum pump is used for pumping the vacuum of the pipeline between the second flexible metal hose 204 and the second pneumatic stop valve 202, and if the experimental vacuum degree V is reached 1 Judging the second flexible metal hose 204 and the phaseThe communicated gas path is normal, otherwise, the pipeline is overhauled until the experimental vacuum degree can be reached; the third shut-off valve 210 is closed.
(8) Injecting inert gas into the carrier gas inlet pipeline by using the mass flowmeter 208 to enable the vacuum degree value V in the carrier gas inlet pipeline 2 Greater than V 1 The second manual shutoff valve 202 of the carrier gas injection port of the liquid source bottle is opened to stop the gas injection of the mass flow meter.
When the liquid source is not in use, the first pneumatic stop valve 105 and the second pneumatic stop valve 203 are kept closed; when using the liquid source, first the first pneumatic stop valve 105 and the second pneumatic stop valve 203 are kept closed, the first flexible metal hose 106 and the second flexible metal hose 204 are respectively pumped by the vacuum pump, if the vacuum degree measured by the second vacuum gauge 206 and the first vacuum gauge 109 and the second vacuum gauge 206 reaches a certain vacuum degree V 1 If so, the air path between the first flexible metal hose 106 and the second flexible metal hose 204 is determined to be normal. Injecting inert gas into the carrier gas inlet pipeline by using the mass flowmeter 208 to enable the vacuum degree value V measured by the second vacuum gauge 206 in the carrier gas inlet pipeline 2 Greater than the vacuum degree V measured by the first vacuum gauge 109 1 The first and second pneumatic cutoff valves 105 and 203 are opened. Otherwise, the first manual cut-off valve 104 and the second manual cut-off valve 202 of the liquid source bottle 101 are closed, the pipeline is repaired until a certain vacuum degree can be reached, the first manual cut-off valve 104 is re-opened according to the process described in the steps (2) to (4), and the second manual cut-off valve 202 is re-opened according to the process described in the steps (6) to (8).
In the present invention, the specific vacuum degree generally refers to the vacuum degree required to be set for the experiment.
During the use of the liquid source material, the first vacuum gauge 109 and the second vacuum gauge 206 are respectively used to measure the vacuum degree V in the first flexible metal hose 106 and the second flexible metal hose 204 at all times 1 And V 2 If the vacuum degree is obviously reduced, for example, the vacuum degree is more than or equal to 0.5 atmosphere, the first pneumatic stop valve 105 and the second pneumatic stop valve 203 are immediately closed to avoid the leakage of the liquid source.
The vacuum pump for pumping vacuum of the metal hose connected to the third cut-off valve 210 is a vacuum pump of a chemical vapor deposition coating system, and can also be directly connected to the vacuum pump.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention.
Claims (6)
1. The monitoring device for the chemical vapor deposition liquid source material is characterized by comprising a liquid source bottle, a tray, a weight sensor, a first pneumatic stop valve, a first flexible metal hose and a first vacuum gauge;
the liquid source bottle is used for containing reaction source materials of the chemical vapor deposition coating; the liquid source bottle comprises a stainless steel bottle body, a liquid injection port, a gasified liquid output port and a first manual stop valve on a gasified liquid output port pipeline, wherein the liquid injection port and the gasified liquid output port are positioned on the stainless steel bottle body, and the gasified liquid output port is connected with the gasified liquid output port pipeline; the liquid source bottle also comprises a carrier gas injection port and a second manual stop valve of the carrier gas injection port, the carrier gas injection port is positioned on the stainless steel bottle body, the carrier gas injection port is connected with a carrier gas injection port pipeline, and the second manual stop valve is arranged on the carrier gas injection port pipeline; the liquid injection port is sealed after liquid source materials are injected;
the liquid source bottle is placed on a tray, the tray is fixed on a weight sensor, and the weight sensor monitors the change of the total weight of the tray and the liquid source bottle to monitor the residual amount of the liquid source in real time;
the first pneumatic stop valve is arranged on one side, away from the stainless steel bottle body, of the first manual stop valve, and the other end of the first pneumatic stop valve is connected with the chemical vapor deposition coating system through a first flexible metal hose;
the first vacuum gauge is fixed on the chemical vapor deposition coating system, is connected with the first flexible metal hose through a first tee joint and is used for monitoring the vacuum degree in the first flexible metal hose;
for a liquid source bottle needing carrier gas, the monitoring device further comprises a mass flow meter of the carrier gas, a second pneumatic stop valve, a second flexible metal hose, a second vacuum gauge and a third stop valve;
the mass flow meter is used for injecting inert gas into the liquid source bottle, the second pneumatic stop valve is installed on one side, far away from the stainless steel bottle body, of the second manual stop valve, the other end of the second pneumatic stop valve is connected with the mass flow meter through a second flexible metal hose, and the second vacuum gauge is connected with the second flexible metal hose through a second tee joint; the mass flowmeter and the second vacuum gauge are fixed on the chemical vapor deposition coating system;
the second flexible metal hose is also connected with a vacuum pump through a third tee joint, and the connection and the disconnection with the vacuum pump are controlled through a third stop valve; the third stop valve is a manual or automatic stop valve;
the working process of monitoring the weight of the liquid source by using the device comprises the following steps:
(1) Measuring the weight m of an empty liquid source bottle 1 ；
(2) Before the liquid source is injected into the liquid source bottle, an empty liquid source bottle is provided with a first pneumatic stop valve and a corresponding connecting pipeline at an output port of the liquid source bottle, a second pneumatic stop valve and a corresponding connecting pipeline at a carrier gas injection port of the liquid source bottle, and the total weight m is measured 2 ；
(3) Injecting a chemical vapor deposition liquid source material into a liquid source bottle, sealing the liquid source bottle, placing the liquid source bottle on a tray, connecting the other outlet of the first pneumatic stop valve to the chemical vapor deposition coating system by using a first flexible metal hose, and connecting the other outlet of the second pneumatic stop valve to the chemical vapor deposition coating system by using a second flexible metal hose; recording weight sensor reading m 3 ；
(4) During the film coating process, the reading m of the weight sensor is monitored 3 If m is 3 ≤1.1×m 2 Then the liquid source bottle is replaced;
(5) Measuring the weight m of a used liquid source bottle 4 Then m is 4 -m 1 Is the weight of the remaining chemical reaction precursor in the liquid source bottle.
2. The apparatus for monitoring chemical vapor deposition liquid source material as claimed in claim 1, wherein the method for opening the first manual cut-off valve comprises the steps of:
(1) Installing the outlet end of a first flexible metal hose connected with a liquid source bottle on a gas path of a chemical vapor deposition coating system;
(2) Keeping the first manual stop valve closed, keeping the first pneumatic stop valve closed, pumping the first flexible metal hose of the gasified liquid output port by using a vacuum pump, and if the experiment vacuum degree V is reached 1 If not, the pipeline is overhauled until the experimental vacuum degree V is reached 1 ；
(3) Opening the first pneumatic stop valve, pumping the vacuum of the pipeline between the first flexible metal hose and the first manual stop valve by using a vacuum pump, and if the experimental vacuum degree V is reached 1 If not, the pipeline is overhauled until the experimental vacuum degree V can be reached 1 ；
(4) Opening the first manual stop valve at the outlet of the liquid source gas cylinder, and measuring the vacuum degree V in the flexible hose at the outlet 1 ；
For a liquid source bottle containing a carrier gas injection port, the following steps are also required:
(5) Installing the outlet end of a second flexible metal hose connected with a liquid source bottle on the gas path of a carrier gas inlet system; the gas path of the carrier gas inlet system comprises a second tee joint, a mass flow meter, a third tee joint and a third stop valve; the outlet of the third stop valve is connected to a vacuum pump;
(6) Keeping the second pneumatic stop valve closed, opening the third stop valve, pumping a second flexible metal hose of the carrier gas injection port by using a vacuum pump, and if the experimental vacuum degree V is reached 1 Then, the second flexible metal is judged to be softThe pipe and the communicated gas circuit are normal, otherwise, the pipeline is overhauled until the experimental vacuum degree V is reached 1 ；
(7) Opening the second pneumatic stop valve, pumping the vacuum of the pipeline between the second flexible metal hose and the second pneumatic stop valve by using a vacuum pump, and if the experimental vacuum degree V is reached 1 If the second flexible metal hose and the communicated gas circuit are normal, otherwise, the pipeline is overhauled until the experiment vacuum degree V can be reached 1 (ii) a Closing the third stop valve;
(8) Injecting inert gas into the carrier gas inlet pipeline by using a mass flowmeter to enable the vacuum degree value V in the carrier gas inlet pipeline 2 Greater than V 1 And opening a second manual stop valve of the carrier gas injection port of the liquid source bottle, and stopping the gas injection of the mass flow meter.
3. The apparatus for monitoring the source material of chemical vapor deposition liquid according to claim 1, wherein the vacuum pump for drawing the vacuum of the metal hose is an independently operated vacuum pump or a vacuum pump of a chemical vapor deposition coating system.
4. The apparatus of claim 2, wherein the first and second pneumatic shut-off valves remain closed when the liquid source is not in use; when the liquid source is used, firstly, the first pneumatic stop valve and the second pneumatic stop valve are kept closed, the first flexible metal hose and the second flexible metal hose are respectively pumped by using a vacuum pump, if the experimental vacuum degree is reached, the flexible metal hose and a communicated gas circuit are judged to be normal, and the first pneumatic stop valve and the second pneumatic stop valve are respectively opened; otherwise, closing the first and second manual cut-off valves of the liquid source bottle, servicing the pipeline until the experimental vacuum can be reached, re-opening the first manual cut-off valve according to steps (2) - (4) of claim 2, and re-opening the second manual cut-off valve according to steps (6) - (8) of claim 2.
5. The apparatus of claim 1, wherein the first and second pneumatic shut-off valves are high temperature-resistant shut-off valves.
6. The apparatus of claim 1, wherein the vacuum gauge is used to measure the vacuum degree in the flexible metal hose during the use of the liquid source material, and the pneumatic stop valve is closed immediately when the vacuum degree is greater than or equal to 0.5 atm to avoid the leakage of the liquid source.
Priority Applications (1)
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| JP3856397B2 (en) * | 1994-07-08 | 2006-12-13 | 株式会社日立国際電気 | Wafer processing method for semiconductor manufacturing apparatus and semiconductor manufacturing apparatus |
| JP2000306907A (en) * | 1999-04-26 | 2000-11-02 | Sony Corp | Liquid source device |
| CN104120407B (en) * | 2014-07-31 | 2016-06-29 | 沈阳大学 | A kind of for chemical vapour deposition (CVD) liquid charging stock vaporization feed device and using method |
| CN108982645A (en) * | 2018-07-24 | 2018-12-11 | 江南大学 | A kind of integrated form online test method of nano-coating technique |
| CN109234701B (en) * | 2018-09-28 | 2020-11-10 | 航天材料及工艺研究所 | Device and method for chemical vapor deposition of rhenium layer |
| CN111595408B (en) * | 2020-04-30 | 2022-10-28 | 江苏微导纳米科技股份有限公司 | Equipment for measuring liquid level in constant-temperature closed container, film coating device and method for measuring liquid level |
| CN214496472U (en) * | 2020-12-29 | 2021-10-26 | 安徽中飞科技有限公司 | Gas replacement control system |
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