MO liquid precursor split charging device

Abstract

The utility model provides a split charging device for an MO liquid precursor, and relates to the technical field of split charging equipment. The device comprises a glove box, a high-pressure gas cylinder, a source storage tank, a gas inlet pipeline, a liquid outlet pipe, a weighing instrument and a stainless steel funnel. The high-purity inert gas in the high-pressure gas cylinder pushes the liquid precursor to flow into the source bottle to be filled from the source storage tank through the liquid outlet pipe, the weighing instrument is combined to monitor the split charging amount in real time, and efficient, safe and accurate split charging is achieved. The split charging system is simple in structure, does not use any electronic element, only depends on the physical principle, and avoids low efficiency and potential safety hazards in traditional manual operation.

Description

Technical Field

[0001] This utility model relates to the field of packaging equipment technology, and more specifically, to a packaging device for MO liquid precursors. Background Technology

[0002] Liquid MO precursors (metal-organic precursors) are widely used in semiconductor deposition processes. For example, various MO precursors (commonly such as TMA, DIPAS, and TiCl4) are required as reactants in thin-film deposition processes like MOCVD and ALD. Most wafer foundries and equipment manufacturers that use large quantities of MO precursors typically purchase large quantities at once to save on procurement costs. These are then stored in large source bottles in glove boxes and repackaged, ranging from tens of grams to several kilograms, into equipment source bottles when needed.

[0003] Traditional methods for packaging liquid precursors:

[0004] First, the purchased storage tanks will be placed in a glove box, which is filled with N2 or Ar inert gas. The glove box is usually under positive pressure, with a pressure range of 1-5 bar. Maintaining positive pressure inside the box is to provide a stable inert environment and prevent air from entering the glove box.

[0005] 1. The source bottle to be filled is placed into the glove box through a transfer chamber. Disposable pasteurized pipettes are used to slowly transfer the source from the storage tank to the target source bottle. The pipettes are typically made of transparent polyethylene (PE) and can draw 5-10 mL at a time. The volume is drawn sequentially according to the required weight, and the source bottle is then weighed to obtain the current weight. This method is often inefficient due to the limitations of the pipettes; for example, filling 1 kg of source requires hundreds of draws, taking at least several tens of minutes. This method is also difficult to operate manually, and it is very easy to spill liquid outside the source bottle during the manual transfer process using pasteurized pipettes, resulting in waste and contamination of the glove box.

[0006] 2. The source is poured directly from the filling port of the storage tank into the target source bottle manually. The storage tank is usually large in weight and volume, which requires a high level of physical strength from the operator, making the operation very difficult. In addition, it is easy to spill a large amount of liquid during pouring, which has a high risk factor and makes it impossible to accurately obtain the target weight. Utility Model Content

[0007] This invention discloses a dispensing device for MO liquid precursors, which aims to solve the problems mentioned above.

[0008] The present invention adopts the following solution:

[0009] A dispensing device for MO liquid precursors includes a glove box, and further includes: a high-pressure gas cylinder, a liquid storage tank, and a weighing instrument disposed within the glove box; wherein, the high-pressure gas cylinder is connected to the liquid level in the liquid storage tank via an inlet pipe, and a pressure reducing valve is provided on the inlet pipe to control the inlet pressure; the liquid storage tank is provided with an outlet pipe extending below the liquid level, and the other end of the outlet pipe extends above the source bottle to be filled, and the high-pressure gas in the high-pressure gas cylinder forces the liquid precursor in the liquid storage tank through the outlet pipe to be dispensed onto the source bottle to be filled; the weighing instrument is disposed below the source bottle to accurately control the dispensing amount in the source bottle.

[0010] Furthermore, the high-pressure gas cylinder is filled with high-purity inert gas, and the gas purity is ≥99.999%.

[0011] Furthermore, the pressure range of the gas inside the high-pressure cylinder is 1MPa-13MPa.

[0012] Furthermore, pressure gauges are installed at both ends of the pressure reducing valve.

[0013] Furthermore, a stainless steel funnel is provided at the inlet of the source bottle to be filled to facilitate the filling of the liquid precursor.

[0014] Furthermore, the glove box is filled with high-purity inert gas, and the pressure range inside the glove box is 0.1-0.5 MPa.

[0015] Furthermore, both the air inlet pipe and the liquid outlet pipe are made of stainless steel.

[0016] Furthermore, a first manual valve and a second manual valve are respectively provided on the air inlet pipe and the liquid outlet pipe to control the opening and closing of the air inlet pipe and the liquid outlet pipe, respectively.

[0017] Furthermore, the outlet pipe includes a first pipe section disposed inside the storage tank and a second pipe section disposed outside the storage tank, and the first pipe section and the second pipe section are connected by a VCR connector.

[0018] Furthermore, the high-pressure gas cylinder is provided with a gas cylinder inlet for replenishing high-pressure gas, and the liquid storage tank is provided with a filling port for replenishing liquid precursor.

[0019] Beneficial effects:

[0020] 1. The system has a simple structure, all components are readily available, and the operating principle is simple and easy to implement, simplifying the operation steps and procedures.

[0021] 2. It has a high safety factor, which greatly avoids the risk of precursor leakage due to human error in the original traditional packaging method.

[0022] 3. The dispensing efficiency is significantly improved compared to traditional methods, and the target filling amount can be accurately obtained by controlling the flow rate and observing the scale reading. Attached Figure Description

[0023] Figure 1 This is a schematic diagram of the overall structure and principle of a dispensing device for MO liquid precursor according to an embodiment of this utility model;

[0024] Figure 2 This is a schematic diagram of the storage tank of a dispensing device for MO liquid precursor according to an embodiment of this utility model;

[0025] Figure reference numerals: 1. High-pressure gas cylinder; 2. Gas cylinder inlet; 3. Third hand valve; 4. Gas inlet pipeline; 5. Pressure reducing valve; 6. First hand valve; 7. Metal sealing joint; 8. Filling port; 9. VCR joint; 10. Liquid storage tank; 11. Liquid precursor; 12. First pipe section; 13. Second hand valve; 14. Second pipe section; 15. Funnel; 16. Plug; 17. Weighing instrument; 18. Gas cylinder outlet; 19. Source bottle to be filled; 20. Filling inlet; 21. Glove box. Detailed Implementation

[0026] Combination Figure 1 and Figure 2 As shown, this embodiment provides a dispensing device for MO liquid precursors, including a glove box 21, and further including: a high-pressure gas cylinder 1, a storage tank 10, and a weighing instrument 17 disposed in the glove box 21; wherein, the high-pressure gas cylinder 1 is connected to the liquid level above the liquid level in the storage tank 10 through an air inlet pipe 4, and a pressure reducing valve 5 is provided on the air inlet pipe 4 to control the air inlet pressure; the storage tank 10 is provided with a liquid outlet pipe extending below the liquid level, and the other end of the liquid outlet pipe extends above the source bottle 19 to be filled, and the high-pressure gas in the high-pressure gas cylinder 1 forces the liquid precursor 11 in the storage tank 10 through the liquid outlet pipe to be dispensed onto the source bottle 19 to be filled; the weighing instrument 17 is disposed below the source bottle 19 to accurately control the dispensing amount in the source bottle 19 to be filled.

[0027] In this embodiment, the glove box 21 is an existing device with a sealed interior, providing a closed operating space for the user. The glove box 21 is filled with a high-purity (>99.999%) inert gas, such as N2 or Ar. The pressure range inside the glove box 21 is 0.1-0.5 MPa. The pressure inside the box is always maintained as positive relative to the ambient pressure. This is because most MO precursors react violently with air, so all processes of dispensing precursors must be completed within the environment of the glove box 21.

[0028] The high-pressure gas cylinder 11 is required to be filled with inert gases such as high-purity nitrogen or argon, with a gas purity requirement of 5N or higher (i.e., gas purity ≥ 99.999%), to meet the gas purity requirements for transporting the MO source and minimize contamination of the precursor. The pressure range of the gas in the high-pressure gas cylinder 11 is 1-13 MPa.

[0029] The high-pressure gas cylinder 1 and the liquid storage tank 10 are connected via an inlet pipe 4. A pressure reducing valve 5 is installed on the inlet pipe 4. A first pressure gauge P1 with a range of 0-30 MPa and an accuracy of 1 MPa is installed upstream of the pressure reducing valve 5. A second pressure gauge P2 with a range of 0-1 MPa and an accuracy of 0.02 MPa is installed downstream of the pressure reducing valve 5. The inlet pipe 4 is connected to the gas cylinder outlet 18 of the high-pressure gas cylinder 1 and the inlet of the liquid storage tank 10 using 1 / 4-inch VCR metal sealing connectors 7, facilitating connection and ensuring sealing. The high-pressure gas cylinder 1 also has a gas cylinder inlet 2 for replenishing high-pressure gas; after the gas is used up, it is refilled through the gas cylinder inlet 2. Additionally, a third hand valve 3 is installed at the outlet of the high-pressure gas cylinder 1 to control the opening and closing of the high-pressure gas cylinder 1.

[0030] The storage tank 10 can be a dual-source bottle with a volume of 5L-50L. The storage tank 10 is equipped with a gas inlet, and a first manual valve 6 is installed at the gas inlet for controlling its opening and closing. A filling port 8 is also provided on the storage tank 10 for replenishing the liquid precursor 11. The gas inlet is located at the top of the storage tank 10, above the liquid level of the liquid precursor 11, and can apply pressure above the liquid level in the storage tank 10, thereby forcing the liquid precursor 11 out through the outlet pipe.

[0031] The storage tank 10 is equipped with a liquid outlet pipe, which can be made of 1 / 4-inch stainless steel. It should be noted that one end of the outlet pipe extends below the liquid level of the liquid precursor 11 inside the storage tank 10. A second hand valve 13 is provided on the outlet pipe to control its opening and closing. The outlet pipe includes a first pipe section 12 located inside the storage tank 10 and a second pipe section 14 located outside the storage tank 10. The first pipe section 12 and the second pipe section 14 are sealed together using a 1 / 4-inch VCR connector.

[0032] The source bottle 19 to be filled is a source bottle used on the coating equipment, and can be a dual-tube source bottle or a single-tube source bottle. The source bottle 19 to be filled is provided with a filling inlet 20, which is connected to the liquid outlet pipe, or the liquid outlet end of the liquid outlet pipe is positioned directly above the filling inlet 20. Preferably, a stainless steel funnel 15 can be provided at the filling inlet 20 of the source bottle 19 to facilitate the filling of the liquid precursor 11. During filling, the plug 16 of the filling inlet 20 of the source bottle to be filled is opened, and the funnel 15 is placed inside.

[0033] The weighing instrument 17 is an electronic digital display platform scale with a range of 50kg and an accuracy of 0.1g, used to observe the filling amount at any time during the dispensing process.

[0034] The packaging process is as follows:

[0035] After connecting all components and opening the filling plug 16 of the source bottle 19, place the source bottle 19 and plug 16 together on the electronic digital display scale. Place the funnel 15 into the inlet, with the outlet pipe directly opposite the opening of the funnel 15 to prevent leakage. Zero the electronic digital display scale reading to display the current net weight in real time. Then open the third hand valve 3, and open the first hand valve 6 and the second hand valve 13 of the storage tank 10 and the outlet pipe respectively. Slowly open the pressure reducing valve 5 while observing the liquid flow rate of the outlet pipe and the electronic digital display scale reading. Adjust the pressure reducing valve 5 to control the gas supply pressure. The pressure range can be 0.15-0.5 MPa. According to Pascal's Law, when the following conditions are met:

[0036] P2>ρgH+P3;

[0037] The liquid can be squeezed out of the storage tank 10 by air pressure and flow from the outlet pipe to the source bottle 19 to be filled.

[0038] Where P2 is the pressure at the rear end of pressure reducing valve 5, P3 is the pressure of glove box 21; ρ is the solution density of liquid precursor 11, H is the height from the liquid surface to the outlet pipe, and g is the gravity coefficient.

[0039] The dispensing rate can be adjusted by regulating the gas supply pressure. For example, the optimal dispensing rate is 5 mL / s when the gas supply pressure is 0.3 MPa. Observe the reading of the electronic digital display scale. When the reading is close to the target weight, reduce the pressure reducing valve 5 to decrease the flow rate to 1 mL / s. When the reading reaches the expected filling volume, close the pressure reducing valve 5, close the first hand valve 6 on the storage tank 10 and the second hand valve 13 on the dispensing pipe, and close the third hand valve 3. After the liquid flow rate has completely stopped, remove the funnel 15, install the plug 16 on the source bottle to be filled, and seal the inlet. The dispensing is now complete.

[0040] The dispensing system of this embodiment does not use any electronic components such as electric pumps, and the process consumes no electricity. It only uses the pressure of inert gas to drive the liquid flow, and the liquid flow rate can be controlled. It is a method of safely and efficiently dispensing liquid precursor 11 based solely on physical principles. Furthermore, the system only requires the installation of two standard stainless steel pipe fittings and a standard VCR connector, without requiring any other modifications to the structure of the storage tank 10. This dispensing system has a simple structure, all components are readily available, and the system's operating principle is simple and easy to implement, simplifying the operation process. It also has a high safety factor, greatly avoiding the risk of precursor leakage due to human error in traditional dispensing methods. In addition, the dispensing efficiency is significantly improved compared to traditional methods, and the target filling amount can be accurately obtained by controlling the flow rate and observing the scale reading.

[0041] It should be understood that the above are only preferred embodiments of the present utility model, and the protection scope of the present utility model is not limited to the above embodiments. All technical solutions that fall within the scope of the present utility model are protected by the present utility model.

[0042] The accompanying drawings used in the above description of the embodiments only show some embodiments of the present invention and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained from these drawings without creative effort.

Claims

1. A MO liquid precursor dispensing apparatus comprising a glove box, characterized in that, Also include: The high-pressure gas cylinder, liquid tank, weighing instrument arranged in the glove box; wherein, the high-pressure gas cylinder is connected to the liquid level above in the liquid tank through the gas inlet pipeline, and the pressure reducing valve is arranged on the gas inlet pipeline to control the gas inlet pressure; the liquid tank is provided with a liquid outlet pipe extending below the liquid level, and the other end of the liquid outlet pipe extends above the source bottle to be filled, and the liquid precursor in the liquid tank is pressed out through the liquid outlet pipe by the high-pressure gas in the high-pressure gas cylinder to the source bottle to be filled for sub-packaging; the weighing instrument is arranged below the source bottle to be filled to accurately control the sub-packaging amount in the source bottle to be filled.

2. The MO liquid precursor dispensing apparatus according to claim 1, wherein The high-pressure gas cylinder is filled with high-purity inert gas, and the gas purity is ≥99.999%.

3. The MO liquid precursor dispensing apparatus according to claim 2, wherein The pressure range of the gas in the high-pressure gas cylinder is 1MPa-13MPa.

4. The MO liquid precursor dispensing apparatus according to claim 1, wherein The pressure gauges are arranged at both ends of the pressure reducing valve.

5. The MO liquid precursor dispensing apparatus according to claim 1, wherein A stainless steel funnel is arranged at the inlet of the source bottle to be filled to facilitate the filling of the liquid precursor.

6. The MO liquid precursor dispensing apparatus according to claim 1, wherein The glove box is filled with high-purity inert gas, and the pressure range in the glove box is 0.1-0.5Mpa.

7. The MO liquid precursor dispensing apparatus according to claim 1, wherein The liquid outlet pipe includes a first pipe section arranged in the liquid tank and a second pipe section arranged outside the liquid tank, and the first pipe section and the second pipe section are connected through a VCR joint.

8. The MO liquid precursor dispensing apparatus according to claim 1, wherein First and second hand valves are arranged on the gas inlet pipeline and the liquid outlet pipe respectively to control the opening and closing of the gas inlet pipeline and the liquid outlet pipe respectively.

9. The MO liquid precursor dispensing apparatus according to claim 1, wherein The connection between the gas inlet pipeline and the gas outlet of the high-pressure source bottle and the gas inlet of the liquid tank adopts a 1 / 4inch VCR metal sealing joint.

10. The MO liquid precursor dispensing apparatus according to claim 1, wherein A gas cylinder inlet is arranged on the high-pressure gas cylinder for supplementing high-pressure gas, and a filling port is arranged on the liquid tank for supplementing liquid precursor.

Images