ALD source packaging cylinder leak detection device and method

Abstract

The present invention relates to a leak detection device for an ALD source sub-packaging cylinder. The device includes a transfer chamber connected to a vacuum pump via a cold trap, a weighing device disposed within the transfer chamber, and a sub-packaging cylinder placed on the weighing device. The sub-packaging cylinder stores an ALD source. The outer wall of the transfer chamber is coated with a heating element, and the transfer chamber is also connected to a pressure gauge. The present invention also discloses a leak detection method for an ALD source sub-packaging cylinder. The present invention can effectively detect the leakage rate of a cylinder containing an ALD source, is safe and convenient to operate, and significantly reduces the possibility of safety risks caused by leakage in the ALD source sub-packaging cylinder.

Description

Technical Field

[0001] The present invention relates to the technical field of leak detection, and in particular to a leak detection device and method for an ALD source packaging cylinder. Background Art

[0002] ALD (Atomic Layer Deposition) is a method of forming a deposited film by alternately introducing pulses of a vapor-phase precursor into a reactor, where it chemically adsorbs and reacts on a deposition substrate. Due to the active nature of the chemical vapor deposition precursor source (ALD source), its production process often requires a highly clean, oxygen-free, and water-free system environment. The ALD source needs to be packaged in sealed steel cylinders to ensure its quality and prevent it from being deteriorated by external influences. To ensure that the ALD source can be stored in water-free and oxygen-free conditions, the packaging cylinders must be highly sealed, and therefore, the cylinders must be leak-tested.

[0003] Currently, the primary method for detecting leaks in refill cylinders is through helium mass spectrometry leak detectors. However, these leak detectors can only detect empty cylinders based on helium gas evaporation and are unable to effectively detect the leak rate of cylinders already loaded with ALD sources, thus failing to meet operational requirements. Therefore, it is crucial to quickly and easily detect leaks in loaded cylinders. Summary of the Invention

[0004] Therefore, the technical problem to be solved by the present invention is to overcome the defect in the prior art that the leak detector cannot effectively detect the leakage rate of the cylinder containing the ALD source.

[0005] In order to solve the above technical problems, the present invention provides a leak detection device for ALD source sub-packaging cylinders, including a transfer chamber, which is connected to a vacuum pump via a cold trap, a weighing device is provided inside the transfer chamber, and the sub-packaging cylinders are placed on the weighing device. ALD sources are stored in the sub-packaging cylinders, the outer wall of the transfer chamber is coated with a heating element, and the transfer chamber is also connected to a pressure gauge.

[0006] In one embodiment of the present invention, the cold trap and the transfer chamber are connected via a delivery pipe, and the outer wall of the delivery pipe is also coated with the heating element.

[0007] In one embodiment of the present invention, the delivery pipeline is a stainless steel corrugated pipe or a stainless steel braided hose.

[0008] In one embodiment of the present invention, a valve is provided on the delivery pipeline.

[0009] In one embodiment of the present invention, the heating element includes a covering body, the covering body covers the outer wall of the transfer bin, the covering body is provided with an electric heating element, or the interior of the covering body is filled with heat transfer oil.

[0010] In one embodiment of the present invention, a warehouse door is provided on the side of the transfer warehouse.

[0011] In one embodiment of the present invention, the cold trap is a liquid nitrogen cold trap.

[0012] A method for leak detection of an ALD source packaging cylinder comprises the following steps:

[0013] S1) Place the cylinder containing the ALD source on a weighing device inside the transfer chamber and add liquid nitrogen to the cold trap;

[0014] S2) heating the transfer chamber using a heating element until the temperature inside the transfer chamber reaches the ultimate vacuum boiling point of the ALD source;

[0015] S3) defining the vacuum degree corresponding to the ultimate vacuum boiling point as M1, and the preset vacuum degree in the transfer chamber as M2; wherein M2≤M1;

[0016] Open the cold trap and use the vacuum pump to evacuate the transfer chamber until the pressure gauge shows that the actual vacuum degree in the transfer chamber reaches M2, so that the transfer chamber reaches the detection state;

[0017] S4) The transfer bin is maintained in the detection state until a set time. If the weight of the sub-filling cylinder measured by the weighing device decreases, it indicates that the sub-filling cylinder has leakage. Otherwise, it indicates that there is no leakage.

[0018] In one embodiment of the present invention, the set time in step S4) is 0.5 to 2 hours.

[0019] In one embodiment of the present invention, the ALD source is one of TDMAT, 3DMAS, BDEAS, TEMAHf, TMGa or TEGa.

[0020] The above technical solution of the present invention has the following advantages over the prior art:

[0021] The leak detection device and method for the sub-packaging cylinder described in the present invention can effectively detect the leakage rate of the cylinder containing the ALD source. The operation is safe and convenient, and the possibility of safety risks caused by leakage in the sub-packaging cylinder of the ALD source is greatly reduced. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] In order to make the contents of the present invention more clearly understood, the present invention is further described in detail below based on specific embodiments of the present invention in conjunction with the accompanying drawings.

[0023] Figure 1 1 is a schematic structural diagram of a leak detection device for an ALD source packaging cylinder according to the present invention;

[0024] Description of the accompanying drawings: 1. Transfer chamber; 2. Cold trap; 3. Vacuum pump; 4. Weighing device; 5. Dispensing cylinder; 6. Delivery pipeline; 7. Heating element; 8. Pressure gauge; DETAILED DESCRIPTION

[0025] The present invention will be further described below with reference to the accompanying drawings and specific embodiments so that those skilled in the art can better understand the present invention and implement it. However, the embodiments are not intended to limit the present invention.

[0026] Reference Figure 1 As shown, this embodiment discloses a leak detection device for an ALD source sub-packaging cylinder 5, comprising a transfer bin 1, which is connected to a vacuum pump 3 via a cold trap 2, a weighing device 4 is provided inside the transfer bin 1, and the sub-packaging cylinder 5 is placed on the weighing device 4, wherein the ALD source is stored inside the sub-packaging cylinder 5, a heating element 7 is coated on the outer wall of the transfer bin 1, and a pressure gauge 8 is also connected to the transfer bin 1 for detecting the vacuum degree inside the transfer bin 1.

[0027] Among them, the vacuum pump 3 is used to evacuate the transfer chamber 1; the cold trap 2 is used to collect the leaked ALD source; and the weighing device 4 is used to weigh the sub-packaging cylinder 5.

[0028] In one embodiment, the cold trap 2 and transfer chamber 1 are connected by a delivery pipe 6, the outer wall of which is also coated with a heating element 7. If the aliquot cylinder 5 leaks, the ALD source remains vaporized while passing through the heated delivery pipe 6 and is then collected by the cold trap 2 as condensation.

[0029] In one embodiment, the delivery pipeline 6 is made of a stainless steel bellows or a stainless steel braided hose, which has advantages such as good chemical stability and corrosion resistance.

[0030] In one embodiment, a valve is provided on the delivery pipeline 6 to control the on / off of the delivery channel.

[0031] In one embodiment, the heating element 7 includes a covering body, which covers the outer wall of the transfer bin 1 , and the electric heating element 7 is provided on the covering body, or the interior of the covering body is filled with heat-conducting oil.

[0032] The covering body can be a belt body or a sleeve body.

[0033] In one embodiment, a door is provided on the side of the transfer chamber 1, and the heating element 7 can be arranged away from the door to better facilitate opening or closing of the door.

[0034] In one embodiment, the cold trap 2 is a liquid nitrogen cold trap 2 .

[0035] In one embodiment, the weighing device 4 is located in the lower middle portion of the transfer bin 1 to facilitate the placement of larger-sized steel cylinders.

[0036] In one embodiment, the cold trap 2 can be made of stainless steel or high borosilicate material.

[0037] The transfer chamber 1 is connected to the glove box (anhydrous and oxygen-free). It has left and right doors, with the left door opening to reveal the glove box. The ALD source dispensing process involves first transferring empty cylinders through the transfer chamber 1 via vacuum exchange into the glove box. The ALD source is then filled into the cylinders, sealed, and placed back into the transfer chamber 1 for leak testing.

[0038] The above device utilizes the glove box's transfer chamber 1, eliminating the need for extensive additional modifications and enhancing its functionality. When not being used for leak detection, the transfer chamber 1 can serve as a replacement for the normal transfer chamber 1 operating in anhydrous and oxygen-free conditions. This not only enables quick and convenient leak detection of source cylinders, but also ensures the diverse applications of the transfer chamber 1 and the safety of cylinder leak detection.

[0039] The leak detection device for dispensing cylinders in the above embodiment can be used to determine if ALD source cylinders are leaking before they are transferred out of the glove box. This is done by heating and evacuating the transfer chamber, and then weighing the dispensing cylinders within the chamber. The entire leak detection process is performed within the glove box's transfer chamber, further reducing the possibility of source cylinders leaking into the outside air.

[0040] A method for leak detection of ALD source sub-packaging cylinders using the leak detection device includes the following steps:

[0041] S1) placing the sub-filled cylinder 5 containing the ALD source on the weighing device 4 inside the transfer chamber 1, and adding liquid nitrogen to the cold trap 2;

[0042] S2) heating the transfer chamber 1 using the heating element 7 until the temperature inside the transfer chamber 1 reaches the ultimate vacuum boiling point of the ALD source;

[0043] S3) defining the vacuum degree corresponding to the ultimate vacuum boiling point as M1, and the preset vacuum degree in the transfer chamber 1 as M2; wherein M2≤M1;

[0044] Open the cold trap 2 and use the vacuum pump 3 to evacuate the transfer chamber 1 until the pressure gauge 8 shows that the actual vacuum degree in the transfer chamber 1 reaches M2, so that the transfer chamber 1 reaches the detection state;

[0045] S4) The transfer bin 1 is maintained in the detection state until the set time. If the weight of the sub-filling cylinder 5 measured by the weighing device 4 decreases, it indicates that the sub-filling cylinder 5 has leakage. Otherwise, it indicates that there is no leakage.

[0046] When the transfer chamber 1 reaches the detection state, the transfer chamber 1 is in an ultimate vacuum state.

[0047] In addition, if the sub-packaging cylinder 5 is leaking, the leakage rate can be calculated based on the weight reduction of the sub-packaging source cylinder.

[0048] In one embodiment, while the transfer bin 1 is heated by the heating element 7 , the heating element 7 coated on the outer wall of the delivery pipe 6 also heats the delivery pipe 6 at the same time.

[0049] In one embodiment, the set time in step S4) is 0.5 to 2 hours.

[0050] In one embodiment, the ALD source is one of TDMAT [Tetrakis(dimethylamino)titanium(IV)], 3DMAS [Tris(dimethylamino)silane], BDEAS [Bis(diethylamino)silane], TEMAHf [Tetrakis(ethylmethylamino)hafnium], TMGa [Trimethylgallium], or TEGa [Triethylgallium].

[0051] Among them, TDMAT is in liquid state at room temperature.

[0052] In one embodiment, the weighing device 4 is communicatively connected to a controller, and the controller is located outside the transfer bin 1. The weighing device 4 is used to transmit weighing data to the controller so that the weighing data of the weighing device 4 can be obtained externally or remotely.

[0053] The above controller may be a PLC controller.

[0054] The following is a specific example to illustrate the leak detection method for the ALD source cylinder:

[0055] Example 1:

[0056] The leak detection method for filling cylinders includes the following steps:

[0057] S1) placing the sub-packaging cylinder 5 containing TDMAT on the weighing device 4 inside the transfer warehouse 1, and adding liquid nitrogen to the cold trap 2;

[0058] S2) heating the transfer chamber 1 using the heating element 7 until the temperature inside the transfer chamber 1 reaches the ultimate vacuum boiling point of TDMAT: 80° C. (the boiling point of TDMAT at 0.1 torr);

[0059] S3) M1 = 0.1 torr;

[0060] Open the cold trap 2 and use the vacuum pump 3 to evacuate the transfer chamber 1 until the pressure gauge shows that the actual vacuum degree in the transfer chamber 1 reaches M2, and M2 ≤ 0.1 torr, so that the transfer chamber 1 reaches the detection state;

[0061] S4) The transfer bin 1 is maintained in the detection state for 1 hour, and the weighing weight of the sub-filling cylinder 5 displayed by the weighing device 4 remains unchanged, indicating that there is no leakage in the sub-filling cylinder 5.

[0062] Example 2:

[0063] The leak detection method for filling cylinders includes the following steps:

[0064] S1) placing the sub-packaging cylinder 5 containing 3DMAS on the weighing device 4 inside the transfer chamber 1, and adding liquid nitrogen to the cold trap 2;

[0065] S2) heating the transfer chamber 1 using the heating element 7 until the temperature inside the transfer chamber 1 reaches the ultimate vacuum boiling point of 3DMAS: 30° C. (the boiling point of 3DMAS at 0.1 torr);

[0066] S3) M1 = 0.1 torr;

[0067] Open the cold trap 2 and use the vacuum pump 3 to evacuate the transfer chamber 1 until the pressure gauge shows that the actual vacuum degree in the transfer chamber 1 reaches M2, and M2 ≤ 0.1 torr, so that the transfer chamber 1 reaches the detection state;

[0068] S4) The transfer chamber 1 is maintained in the detection state for 0.5 hours, and the weighing weight of the sub-filling cylinder 5 displayed by the weighing device 4 remains unchanged, indicating that there is no leakage in the sub-filling cylinder 5.

[0069] Example 3

[0070] The leak detection method for filling cylinders includes the following steps:

[0071] S1) placing the BDEAS sub-filled cylinder 5 on the weighing device 4 inside the transfer chamber 1, and adding liquid nitrogen to the cold trap 2;

[0072] S2) heating the transfer chamber 1 using the heating element 7 until the temperature inside the transfer chamber 1 reaches the ultimate vacuum boiling point of BDEAS: 25° C. (the boiling point of BDEAS at 0.1 torr);

[0073] S3) M1 = 0.1 torr;

[0074] Open the cold trap 2 and use the vacuum pump 3 to evacuate the transfer chamber 1 until the pressure gauge shows that the actual vacuum degree in the transfer chamber 1 reaches M2, and M2 ≤ 0.1 torr, so that the transfer chamber 1 reaches the detection state;

[0075] S4) The transfer bin 1 is maintained in the detection state for 0.5 hours, and the weighing weight of the sub-filling cylinder 5 displayed by the weighing device 4 decreases, indicating that the sub-filling cylinder 5 is leaking.

[0076] Example 4

[0077] The leak detection method for filling cylinders includes the following steps:

[0078] S1) placing the sub-packaging cylinder 5 containing TEMAHf on the weighing device 4 inside the transfer chamber 1, and adding liquid nitrogen to the cold trap 2;

[0079] S2) heating the transfer chamber 1 using the heating element 7 until the temperature inside the transfer chamber 1 reaches the ultimate vacuum boiling point of TEMAHf: 80° C. (the boiling point of TEMAHf at 0.1 torr);

[0080] S3) M1 = 0.1 torr;

[0081] Open the cold trap 2 and use the vacuum pump 3 to evacuate the transfer chamber 1 until the pressure gauge shows that the actual vacuum degree in the transfer chamber 1 reaches M2, and M2 ≤ 0.1 torr, so that the transfer chamber 1 reaches the detection state;

[0082] S4) The transfer bin 1 is maintained in the detection state for 1 hour, and the weighing weight of the sub-filling cylinder 5 displayed by the weighing device 4 decreases, indicating that the sub-filling cylinder 5 is leaking.

[0083] Example 5

[0084] The leak detection method for filling cylinders includes the following steps:

[0085] S1) placing the sub-packaging cylinder 5 containing TMGa on the weighing device 4 inside the transfer chamber 1, and adding liquid nitrogen to the cold trap 2;

[0086] S2) making the internal temperature of the transfer chamber 1 reach the ultimate vacuum boiling point of TMGa: room temperature (the boiling point of TMGa at 0.1 torr);

[0087] S3) M1 = 0.1 torr;

[0088] Open the cold trap 2 and use the vacuum pump 3 to evacuate the transfer chamber 1 until the pressure gauge shows that the actual vacuum degree in the transfer chamber 1 reaches M2, and M2 ≤ 0.1 torr, so that the transfer chamber 1 reaches the detection state;

[0089] S4) The transfer bin 1 is maintained in the detection state for 0.5 hours, and the weighing weight of the sub-filling cylinder 5 displayed by the weighing device 4 decreases, indicating that the sub-filling cylinder 5 is leaking.

[0090] Example 6

[0091] The leak detection method for filling cylinders includes the following steps:

[0092] S1) placing the sub-packaging cylinder 5 containing TEGa on the weighing device 4 inside the transfer chamber 1, and adding liquid nitrogen to the cold trap 2;

[0093] S2) heating the transfer chamber 1 using the heating element 7 until the temperature inside the transfer chamber 1 reaches the ultimate vacuum boiling point of TEGa: 20° C. (the boiling point of TEGa at 0.1 torr);

[0094] S3) M1 = 0.1 torr;

[0095] Open the cold trap 2 and use the vacuum pump 3 to evacuate the transfer chamber 1 until the pressure gauge shows that the actual vacuum degree in the transfer chamber 1 reaches M2, and M2 ≤ 0.1 torr, so that the transfer chamber 1 reaches the detection state;

[0096] S4) The transfer bin 1 is maintained in the detection state for 0.5 hours, and the weighing weight of the sub-filling cylinder 5 displayed by the weighing device 4 decreases, indicating that the sub-filling cylinder 5 is leaking.

[0097] The leak detection device and method for the sub-packaging cylinder of the above-mentioned embodiment can effectively detect the leakage rate of the cylinder containing the ALD source. The operation is safe and convenient, which greatly reduces the possibility of safety risks caused by leakage of the sub-packaging cylinder of the ALD source. At the same time, it can also effectively prevent the ALD source leaked during the detection process from entering the outside air and causing adverse effects.

[0098] Obviously, the above embodiments are merely examples for clarity of explanation and are not intended to limit the implementation methods. Those skilled in the art will appreciate that other variations or modifications can be made based on the above description. It is not necessary and impossible to enumerate all implementation methods here. Obvious variations or modifications arising therefrom remain within the scope of protection of the present invention.

Claims

1. A leak detection method for an ALD source packaging cylinder, characterized by: A leak detection device for an ALD source sub-packaging cylinder includes a transfer chamber connected to a cold trap and a vacuum pump, a weighing device disposed within the transfer chamber, and a sub-packaging cylinder placed on the weighing device. The sub-packaging cylinder stores an ALD source. The outer wall of the transfer chamber is coated with a heating element. The transfer chamber is also connected to a pressure gauge. The transfer chamber is provided with a left door and a right door. The left door opens to reveal a glove box. When not being leak-checked, the transfer chamber serves as a replacement for a normal transfer chamber operating in anhydrous and oxygen-free conditions. The method includes the following steps: S1) Place the cylinder containing the ALD source on the weighing device inside the transfer chamber and add liquid nitrogen to the cold trap; S2) heating the transfer chamber using a heating element until the temperature inside the transfer chamber reaches the ultimate vacuum boiling point of the ALD source; S3) defines the vacuum degree corresponding to the ultimate vacuum boiling point as M1, the preset vacuum degree within the transfer chamber is M2; wherein, ; Open the cold trap and use the vacuum pump to evacuate the transfer chamber until the pressure gauge shows that the actual vacuum degree in the transfer chamber reaches M2, so that the transfer chamber reaches the detection state; S4) maintaining the transfer bin in the detection state for a set time; if the weight of the sub-filled cylinder measured by the weighing device decreases, it indicates that the sub-filled cylinder is leaking; otherwise, it indicates that there is no leakage; The ALD source packaging process before step S1 is as follows: first, the empty cylinder is sent into the glove box through vacuum exchange in the transfer chamber; then the ALD source is filled into the cylinder. After the filling is completed, the cylinder is sealed and then placed in the transfer chamber for leak detection.

2. The leak detection method for an ALD source sub-packaging cylinder according to claim 1, characterized in that: The set time in step S4) is 0.5 to 2 hours.

3. The leak detection method for an ALD source packaging cylinder according to claim 1, characterized in that: The ALD source is one of TDMAT, 3DMAS, BDEAS, TEMAHf, TMGa or TEGa.

4. The leak detection method for an ALD source sub-packaging cylinder according to claim 1, characterized in that: The cold trap and the transfer bin are connected via a delivery pipe, and the outer wall of the delivery pipe is also covered with the heating element.

5. The leak detection method for an ALD source sub-packaging cylinder according to claim 4, characterized in that: The delivery pipeline is made of stainless steel corrugated pipe or stainless steel braided hose.

6. The leak detection method for an ALD source sub-packaging cylinder according to claim 5, characterized in that: The delivery pipeline is provided with a valve.

7. The leak detection method for an ALD source sub-packaging cylinder according to claim 1, characterized in that: The heating element comprises a covering body, the covering body covering the outer wall of the transfer bin, an electric heating element is provided on the covering body, or the interior of the covering body is filled with heat-conducting oil.

8. The leak detection method for an ALD source packaging cylinder according to claim 1, characterized in that: The cold trap is a liquid nitrogen cold trap.

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