Filling system for tetraethyl orthosilicate and filling process thereof

Abstract

The application discloses a kind of tetraethyl orthosilicate filling system and its filling process, the tetraethyl orthosilicate filling system includes sealed cabin with sealed space in, the sealed cabin is equipped with for placing steel bottle filling area;Tetraethyl orthosilicate stock solution pipeline sealing is worn on the sealed cabin, and sealing is worn on the liquid phase mouth of steel bottle and is installed, the discharge end of the tetraethyl orthosilicate stock solution pipeline is inserted in the bottom in steel bottle, the tetraethyl orthosilicate stock solution pipeline is used to fill tetraethyl orthosilicate stock solution in steel bottle;Detection pipeline sealing is worn on the sealed cabin, and the detection pipeline is connected with the tetraethyl orthosilicate stock solution pipeline;Gas phase pipeline is arranged in the sealed space and is connected with the gas phase mouth of steel bottle;Protective gas pipeline sealing is worn on the sealed cabin, and is connected with the tetraethyl orthosilicate stock solution pipeline and gas phase pipeline respectively.The tetraethyl orthosilicate filling system of the application can avoid secondary pollution of tetraethyl orthosilicate in the filling process.

Description

Technical Field

[0001] This invention relates to the field of semiconductor technology, and in particular to a tetraethyl orthosilicate filling system and filling process thereof. Background Technology

[0002] TEOS (tetraethyl orthosilicate) is mainly used in the preparation of epitaxial materials in integrated circuits, playing an important role in the development of the semiconductor industry. It is a high-end chemical for microelectronics and an important precursor material for third-generation semiconductor materials and emerging semiconductor industries.

[0003] When filling steel cylinders with 9N grade tetraethyl orthosilicate, existing filling systems and processes may introduce impurities, causing secondary contamination and reducing the purity of the tetraethyl orthosilicate in the cylinders after filling, thus failing to meet the standards for use in the semiconductor field.

[0004] The information disclosed in this background section is intended only to enhance the understanding of the overall background of the invention and should not be construed as an admission or in any way implying that the information constitutes prior art known to those skilled in the art. Summary of the Invention

[0005] The purpose of this invention is to provide a tetraethyl orthosilicate filling system that can avoid secondary contamination of tetraethyl orthosilicate during the filling process.

[0006] To achieve the above objectives, embodiments of the present invention provide a tetraethyl orthosilicate filling system, comprising:

[0007] A sealed chamber having a sealed space inside, the sealed chamber having a filling area for placing steel cylinders;

[0008] A tetraethyl orthosilicate raw material pipeline is sealed and installed on the sealed chamber. The tetraethyl orthosilicate raw material pipeline is sealed and installed on the liquid phase port of the steel cylinder. The discharge end of the tetraethyl orthosilicate raw material pipeline is inserted into the bottom of the steel cylinder. The tetraethyl orthosilicate raw material pipeline is used to fill the steel cylinder with tetraethyl orthosilicate raw material.

[0009] A detection pipeline, sealed and installed on the sealed chamber, is connected to the tetraethyl orthosilicate raw liquid pipeline and is used to transport the liquid in the cylinder to the outside of the sealed chamber in order to detect the purity of the liquid in the cylinder.

[0010] A gas phase pipeline is installed within the sealed space and connected to the gas phase port of the gas cylinder;

[0011] A protective gas pipeline is sealed and installed on the sealed chamber. The protective gas pipeline is connected to the tetraethyl orthosilicate raw liquid pipeline and the gas phase pipeline, respectively.

[0012] A valve is installed upstream of the connection point between the tetraethyl orthosilicate raw material pipeline and the detection pipeline, and a valve is installed at the connection point between the gas phase pipeline and the protective gas pipeline.

[0013] In one or more embodiments of the present invention, the filling system further includes a sealed exhaust gas pipe passing through the sealed chamber, the exhaust gas pipe being connected to a gas phase pipe, and a valve being provided on the gas phase pipe at the connection point with the exhaust gas pipe.

[0014] In one or more embodiments of the present invention, the filling system further includes a vacuum pipe that is sealed through the sealed chamber, the vacuum pipe being connected to a gas phase pipe, and a valve being provided on the gas phase pipe at the connection point with the vacuum pipe.

[0015] In one or more embodiments of the present invention, the gas phase pipeline is connected to the tetraethyl orthosilicate raw liquid pipeline via a connecting pipeline, and a valve is provided on the connecting pipeline.

[0016] In one or more embodiments of the present invention, the filling system further includes a sealed air duct passing through the sealed chamber, the air duct being connected to the sealed space for introducing air into the sealed space.

[0017] In one or more embodiments of the present invention, the sealed chamber has a plurality of filling areas for placing steel cylinders.

[0018] In one or more embodiments of the present invention, the bottom of the sealed chamber is provided with a waste liquid outlet communicating with the sealed space.

[0019] In one or more embodiments of the present invention, the filling system further includes a waste liquid pipe sealed through the sealed chamber, the waste liquid pipe being connected to the tetraethyl orthosilicate raw liquid pipe for discharging tetraethyl orthosilicate waste liquid.

[0020] Embodiments of the present invention also provide a filling process for tetraethyl orthosilicate, based on the tetraethyl orthosilicate filling system described above, the filling process for tetraethyl orthosilicate includes the following steps:

[0021] Place the cylinder in the filling area and connect the cylinder to the tetraethyl orthosilicate raw material pipeline and the gas phase pipeline of the filling system;

[0022] When there is no residual liquid in the cylinder, open all the valves on each pipeline of the filling system to perform vacuuming, then inject protective gas, and then perform vacuuming again.

[0023] Open the valve at the gas phase port of the cylinder to perform vacuuming, close all valves on the gas phase pipeline, open the valve at the liquid phase port of the cylinder, and fill the cylinder with tetraethyl orthosilicate stock solution.

[0024] After the tetraethyl orthosilicate stock solution is filled, the liquid in the cylinder is tested through the testing pipeline. If it is qualified, the valve at the liquid phase port is closed, the valve at the gas phase port is opened to fill with nitrogen, the pressure is maintained, and the valve at the gas phase port is closed.

[0025] In one or more embodiments of the present invention, the filling process further includes the following steps:

[0026] When there is residual tetraethyl orthosilicate in the cylinder, open the valves at both the gas phase port and the liquid phase port on the cylinder, inject protective gas, and allow at least part of the residual tetraethyl orthosilicate in the cylinder to flow sequentially through the tetraethyl orthosilicate raw liquid pipeline and the detection pipeline before being tested;

[0027] If the purity of the residual tetraethyl orthosilicate is qualified, open all the valves on each pipeline of the filling system. After the residual liquid in the tetraethyl orthosilicate raw liquid pipeline flows back into the cylinder, close the valves at the gas phase port and liquid phase port on the cylinder, perform vacuum treatment, inject protective gas, and then perform vacuum treatment again.

[0028] Compared with the prior art, the tetraethyl orthosilicate filling system according to the present invention, through the cooperation between the sealed chamber and various pipelines and through a specific filling process, can avoid secondary contamination of tetraethyl orthosilicate during the filling process and ensure the purity of tetraethyl orthosilicate in the cylinder after filling. Attached Figure Description

[0029] Figure 1 This is a schematic diagram of a tetraethyl orthosilicate filling system according to an embodiment of the present invention.

[0030] Explanation of key figure labels:

[0031] 1. Sealed chamber; 11. Sealed space; 12. Filling area; 21. Tetraethyl orthosilicate raw material pipeline; 22. Detection pipeline; 23. Gas phase pipeline; 24. Protective gas pipeline; 25. Exhaust gas pipeline; 26. Vacuum pipeline; 27. Connecting pipeline; 28. Air pipeline; 29. ​​Waste liquid pipeline; 13. Waste liquid outlet; 4. Cylinder; 3. Valve; 41. Liquid phase port; 42. Gas phase port. Detailed Implementation

[0032] The specific embodiments of the present invention will now be described in detail with reference to the accompanying drawings, but it should be understood that the scope of protection of the present invention is not limited to the specific embodiments.

[0033] Unless otherwise expressly stated, throughout the specification and claims, the term "comprising" or its variations such as "including" or "comprises" shall be understood to include the stated elements or components without excluding other elements or other components.

[0034] like Figure 1 As shown, a preferred embodiment of the tetraethyl orthosilicate filling system according to the present invention includes a sealed chamber 1, a tetraethyl orthosilicate raw material pipeline 21, a detection pipeline 22, a gas phase pipeline 23, and a protective gas pipeline 24; the sealed chamber 1 has a sealed space 11, and a filling area 12 for placing a steel cylinder 4 is provided within the sealed chamber 1; the tetraethyl orthosilicate raw material pipeline 21 is sealed and installed on the liquid phase port 41 of the steel cylinder 4, and the discharge end of the tetraethyl orthosilicate raw material pipeline 21 is inserted into the bottom of the steel cylinder 4. The tetraethyl orthosilicate raw material pipeline 21 is used to fill the steel cylinder 4 with tetraethyl orthosilicate raw material; the detection pipeline 22 is sealed through the sealed chamber 1 and is connected to the tetraethyl orthosilicate raw material pipeline 21. It is used to transport the liquid in the steel cylinder 4 to the outside of the sealed chamber 1 to detect the purity of the liquid in the steel cylinder 4; the gas phase pipeline 23 is set in the sealed space 11 and is connected to the gas phase port 42 of the steel cylinder 4; the protective gas pipeline 24 is sealed through the sealed chamber 1 and is connected to both the tetraethyl orthosilicate raw material pipeline 21 and the gas phase pipeline 23.

[0035] It is understood that the tetraethyl orthosilicate filling system of the present invention can be used to fill the steel cylinder 4 with 9N grade (inorganic purity) tetraethyl orthosilicate. Through the cooperation between the sealed chamber 1 and various pipes, and through a specific filling process, secondary contamination of tetraethyl orthosilicate during the filling process can be avoided, and the purity of tetraethyl orthosilicate in the steel cylinder 4 after filling can be ensured.

[0036] A valve 3 is installed upstream of the connection between the tetraethyl orthosilicate raw material pipeline 21 and the detection pipeline 22, and a valve 3 is also installed upstream of the connection between the gas phase pipeline 23 and the protective gas pipeline 24. The upstream location can be considered as being based on the flow direction of the tetraethyl orthosilicate raw material in the tetraethyl orthosilicate raw material pipeline 21 when the steel cylinder 4 is filled with tetraethyl orthosilicate raw material.

[0037] Specifically, the protective gas can be an inert gas such as nitrogen or argon; preferably, nitrogen is preferred as it is abundant and inexpensive. The tetraethyl orthosilicate (TES) stock solution pipeline 21 connects to an external pipeline or TES source, allowing the TES stock solution to enter the filling system and fill cylinder 4. The testing pipeline 22 connects to an external laboratory or testing system, allowing the liquid to be tested to enter the external laboratory or testing system for purity testing.

[0038] Specifically, the protective gas pipeline 24 is connected to the tetraethyl orthosilicate raw liquid pipeline 21, and a valve 3 is installed on the protective gas pipeline 24.

[0039] In one specific embodiment, the filling system further includes a sealed exhaust gas pipe 25 passing through the sealed chamber 1. The exhaust gas pipe 25 is connected to a gas phase pipe 23. A valve 3 is installed at the connection point between the gas phase pipe 23 and the exhaust gas pipe 25 to control the opening and closing of the gas phase pipe 23 and the exhaust gas pipe 25. The exhaust gas pipe 25 serves to discharge exhaust gas. In addition, a valve 3 is also installed on the exhaust gas pipe 25 to control the opening and closing of the exhaust gas pipe 25.

[0040] In one specific embodiment, the filling system further includes a vacuum pipe 26 sealed through the sealed chamber 1. The vacuum pipe 26 is connected to the gas phase pipe 23. A valve 3 is installed at the connection point between the gas phase pipe 23 and the vacuum pipe 26 to control the opening and closing of the gas phase pipe 23 and the vacuum pipe 26. The vacuum pipe 26 serves to evacuate the entire gas phase pipe 23, the tetraethyl orthosilicate raw material pipe 21, and the steel cylinder 4, and, in conjunction with the protective gas pipe 24, fills them with protective gas, thus achieving a displacement function.

[0041] In one specific embodiment, the gas phase pipeline 23 and the tetraethyl orthosilicate raw material pipeline 21 are connected by a connecting pipeline 27, on which a valve 3 is installed. This arrangement allows for vacuuming of the tetraethyl orthosilicate raw material pipeline 21 via the connecting pipeline 27 during vacuuming.

[0042] In one specific embodiment, the filling system further includes an air duct 28 that is sealed through the sealed chamber 1 and is connected to the sealed space 11 for introducing air into the sealed space 11.

[0043] In one specific embodiment, the sealed chamber 1 has multiple filling areas 12 for placing the steel cylinders 4.

[0044] In one specific embodiment, the bottom of the sealed chamber 1 is provided with a waste liquid outlet 13 that communicates with the sealed space 11. When a leak occurs in the pipeline of the tetraethyl orthosilicate filling system, the liquid can flow out through the waste liquid outlet 13 at the bottom of the sealed chamber 1.

[0045] It is understandable that a valve 3 can be installed at the waste liquid outlet 13, or a pipe can be sealed and connected to the waste liquid outlet 13, and a valve 3 can be installed on the pipe. When the valve 3 is closed, the sealed space 11 is kept as closed as possible.

[0046] In one specific embodiment, the filling system further includes a waste liquid pipe 29 sealed through the sealed chamber 1. The waste liquid pipe 29 is connected to the tetraethyl orthosilicate raw material pipe 21 and is used to discharge tetraethyl orthosilicate waste liquid. Sometimes the steel cylinder 4 to be filled is recycled from the customer and may contain some residual tetraethyl orthosilicate liquid. When the purity of the residual tetraethyl orthosilicate liquid does not meet the filling requirements, it can be considered as tetraethyl orthosilicate waste liquid. The residual tetraethyl orthosilicate liquid can be discharged by injecting protective gas into the gas phase port 42, allowing it to pass through the tetraethyl orthosilicate raw material pipe 21 into the waste liquid pipe 29.

[0047] Embodiments of the present invention also provide a filling process for tetraethyl orthosilicate. Based on the tetraethyl orthosilicate filling system described above, the filling process for tetraethyl orthosilicate includes the following steps:

[0048] S1. Place the cylinder in the filling area and connect the cylinder to the tetraethyl orthosilicate raw material pipeline and the gas phase pipeline of the filling system;

[0049] S2. When there is no residual liquid in the cylinder, open all the valves on each pipeline of the filling system, perform vacuuming, then inject protective gas, and then perform vacuuming again.

[0050] It should be noted that the process of opening all valves on all pipelines in the filling system includes the pipeline containing the tetraethyl orthosilicate stock solution.

[0051] S3. Open the valve at the gas phase port on the cylinder to perform vacuuming, close all valves on the gas phase pipeline, open the valve at the liquid phase port on the cylinder, and fill the cylinder with tetraethyl orthosilicate stock solution.

[0052] S4. After the tetraethyl orthosilicate stock solution is filled, the liquid in the cylinder is tested through the testing pipeline. If it is qualified, the valve at the liquid phase port is closed, the valve at the gas phase port is opened to fill with nitrogen, the pressure is maintained, and the valve at the gas phase port is closed.

[0053] Specifically, the steps for testing the liquid inside the cylinder through the testing pipeline are as follows: open the valve at the gas phase port to fill with nitrogen gas, pressurize the cylinder with nitrogen gas, and force the liquid (tetraethyl orthosilicate) inside into the testing pipeline, which then enters the external laboratory or the analytical instrument in the testing system for testing.

[0054] In one specific embodiment, the filling process further includes the following steps:

[0055] S2' When there is residual tetraethyl orthosilicate in the cylinder, open both the gas and liquid phase valves on the cylinder and inject protective gas. This allows at least a portion of the residual tetraethyl orthosilicate in the cylinder to flow sequentially through the tetraethyl orthosilicate raw material pipeline and the testing pipeline before testing. If the purity of the residual tetraethyl orthosilicate is qualified, open all valves on each pipeline of the filling system. After the residual liquid in the tetraethyl orthosilicate raw material pipeline flows back into the cylinder, close the valves at the gas and liquid phase valves on the cylinder, perform vacuuming, inject protective gas, and then perform vacuuming again.

[0056] It is understandable that the cylinders to be filled can be uncontaminated cylinders, meaning that there is no liquid or other contaminants inside. Cylinders to be filled can also be recycled cylinders from customers. These recycled cylinders can be considered as cylinders that previously contained 9N grade tetraethyl orthosilicate, but the customer did not completely use up the tetraethyl orthosilicate, leaving some residual tetraethyl orthosilicate liquid.

[0057] That is, after step S1 is completed, depending on whether there is residual tetraethyl orthosilicate in the cylinder, step S2 or step S2' is performed. After step S2 or step S2' is completed, steps S3 and S4 are performed.

[0058] The specific process of filling tetraethyl orthosilicate according to the present invention will be described in detail below.

[0059] (1) The steel cylinders returned by customers usually contain more or less tetraethyl orthosilicate than they can use, leaving some tetraethyl orthosilicate residue.

[0060] (2) When the cylinder is returned, we first connect it to the filling area, and then introduce nitrogen through the gas phase port to pressurize the cylinder. This way, the residual tetraethyl orthosilicate liquid inside will be forced out and sent to the laboratory for analysis via the testing pipeline.

[0061] (3) If it is not up to standard, nitrogen gas is introduced through the gas phase port to pressurize it and force out all the residual liquid inside, which is then sent to the waste liquid tank through the waste liquid pipeline.

[0062] (4) If it is qualified, prepare to start filling.

[0063] (5) After all the pipelines to the gas cylinder are connected, we must first open the valves on the tetraethyl orthosilicate (TES) raw material pipeline, the testing pipeline, the gas phase pipeline, the waste liquid pipeline, and the connecting pipelines, and then evacuate the pipelines. Before connection, the inside of the pipelines is exposed to air; the pipelines are filled with air. After connecting the gas cylinder, the air inside remains. If this air enters the gas cylinder, it will contaminate the TES, preventing it from achieving the required 9N purity. Therefore, after connection, open all valves and evacuate the pipeline to remove all air. Then, fill the pipeline with nitrogen, and then discharge the nitrogen through the exhaust port. Evacuate the pipeline again, replacing the pipeline five times. Next, open the valve on the gas cylinder to remove the nitrogen that was previously used for pressurization. Then, close all valves on the gas phase port pipeline, and open the valve at the liquid phase port for filling. After filling, analyze the gas. If it is qualified, close the valve at the liquid phase port, and then open the valve at the gas phase port to fill with nitrogen and maintain pressure.

[0064] The foregoing description of specific exemplary embodiments of the invention is for illustrative and explanatory purposes. These descriptions are not intended to limit the invention to the precise forms disclosed, and it will be apparent that many changes and variations can be made in accordance with the foregoing teachings. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application, thereby enabling those skilled in the art to implement and utilize various different exemplary embodiments of the invention, as well as various different choices and variations. The scope of the invention is intended to be defined by the claims and their equivalents.

Claims

1. A tetraethyl orthosilicate filling system, characterized in that, include: A sealed chamber having a sealed space inside, the sealed chamber having a filling area for placing steel cylinders; A tetraethyl orthosilicate raw material pipeline is sealed and installed on the sealed chamber. The tetraethyl orthosilicate raw material pipeline is sealed and installed on the liquid phase port of the steel cylinder. The discharge end of the tetraethyl orthosilicate raw material pipeline is inserted into the bottom of the steel cylinder. The tetraethyl orthosilicate raw material pipeline is used to fill the steel cylinder with tetraethyl orthosilicate raw material. A detection pipeline, sealed and installed on the sealed chamber, is connected to the tetraethyl orthosilicate raw liquid pipeline and is used to transport the liquid in the cylinder to the outside of the sealed chamber in order to detect the purity of the liquid in the cylinder. A gas phase pipeline is installed within the sealed space and connected to the gas phase port of the gas cylinder; A protective gas pipeline is sealed and installed on the sealed chamber. The protective gas pipeline is connected to the tetraethyl orthosilicate raw liquid pipeline and the gas phase pipeline, respectively. A valve is installed upstream of the connection point between the tetraethyl orthosilicate raw material pipeline and the detection pipeline, and a valve is installed at the connection point between the gas phase pipeline and the protective gas pipeline.

2. The tetraethyl orthosilicate filling system as described in claim 1, characterized in that, The filling system also includes a sealed exhaust gas pipe that passes through the sealed chamber. The exhaust gas pipe is connected to a gas phase pipe, and a valve is provided at the connection point between the gas phase pipe and the exhaust gas pipe.

3. The tetraethyl orthosilicate filling system as described in claim 1, characterized in that, The filling system also includes a vacuum pipe that is sealed through the sealed chamber. The vacuum pipe is connected to a gas phase pipe, and a valve is provided at the connection point between the gas phase pipe and the vacuum pipe.

4. The tetraethyl orthosilicate filling system as described in claim 3, characterized in that, The gas phase pipeline is connected to the tetraethyl orthosilicate raw liquid pipeline via a connecting pipe, and a valve is installed on the connecting pipe.

5. The tetraethyl orthosilicate filling system as described in claim 1, characterized in that, The filling system also includes a sealed air duct that passes through the sealed chamber and is connected to the sealed space for introducing air into the sealed space.

6. The tetraethyl orthosilicate filling system as described in claim 1, characterized in that, The sealed chamber has multiple filling areas for placing steel cylinders.

7. The tetraethyl orthosilicate filling system as described in claim 1, characterized in that, The bottom of the sealed chamber is provided with a waste liquid outlet that communicates with the sealed space.

8. The tetraethyl orthosilicate filling system as described in claim 1, characterized in that, The filling system also includes a waste liquid pipe that is sealed through the sealed chamber and is connected to the tetraethyl orthosilicate raw liquid pipe for discharging tetraethyl orthosilicate waste liquid.

9. A filling process for tetraethyl orthosilicate, based on the tetraethyl orthosilicate filling system according to any one of claims 1 to 8, characterized in that, The filling process of the tetraethyl orthosilicate includes the following steps: Place the cylinder in the filling area and connect the cylinder to the tetraethyl orthosilicate raw material pipeline and the gas phase pipeline of the filling system; When there is no residual liquid in the cylinder, open all the valves on each pipeline of the filling system to perform vacuuming, then inject protective gas, and then perform vacuuming again. Open the valve at the gas phase port of the cylinder to perform vacuuming, close all valves on the gas phase pipeline, open the valve at the liquid phase port of the cylinder, and fill the cylinder with tetraethyl orthosilicate stock solution. After the tetraethyl orthosilicate stock solution is filled, the liquid in the cylinder is tested through the testing pipeline. If it is qualified, the valve at the liquid phase port is closed, the valve at the gas phase port is opened to fill with nitrogen, the pressure is maintained, and the valve at the gas phase port is closed.

10. The filling process for tetraethyl orthosilicate as described in claim 9, characterized in that, The filling process also includes the following steps: When there is residual tetraethyl orthosilicate in the cylinder, open the valves at both the gas phase port and the liquid phase port on the cylinder, inject protective gas, and allow at least part of the residual tetraethyl orthosilicate in the cylinder to flow sequentially through the tetraethyl orthosilicate raw liquid pipeline and the detection pipeline before being tested; If the purity of the residual tetraethyl orthosilicate is qualified, open all the valves on each pipeline of the filling system. After the residual liquid in the tetraethyl orthosilicate raw liquid pipeline flows back into the cylinder, close the valves at the gas phase port and liquid phase port on the cylinder, perform vacuum treatment, inject protective gas, and then perform vacuum treatment again.

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