Atomic layer deposition coating method and system for device with high-aspect-ratio structure

Abstract

Provided are an atomic layer deposition coating method and system for a device with a high-aspect-ratio structure, comprising a reaction chamber, a vacuum pump connected to the reaction chamber, a pressurizing gas line, and a carrier gas line; a first valve (V1) is provided on a connecting line between the reaction chamber and the vacuum pump, and a second valve (V2) is provided on the pressurizing gas line connected to the reaction chamber; and a fifth valve (V5) is provided on the carrier gas line, the carrier gas line is respectively connected to a first source container and a second source container storing a reaction precursor, a third valve (V3) is provided on a connecting line between the first source container and the carrier gas line, and a fourth valve (V4) is provided on a connecting line between the second source container and the carrier gas line. Adjusting the opening and closing of a first valve (V1) and a second valve (V2) allows for pressurizing gas to enter a reaction chamber, which increases or decreases pressure in the reaction chamber, causing a reaction precursor to quickly enter a deep hole or trench of a device with a high-aspect-ratio structure, and be effectively adsorbed on surfaces within such devices.

Description

A method and system for atomic layer deposition of high aspect ratio devices

[0001] This application claims priority to Chinese Patent Application No. 202411576413.4, filed on November 6, 2024, entitled "An Atomic Layer Deposition Coating Method and System for High Aspect Ratio Structure Devices", the entire contents of which are incorporated herein by reference. Technical Field

[0002] This application relates to the field of semiconductor manufacturing technology, and in particular to an atomic layer deposition method and system for high aspect ratio structure devices. Background Technology

[0003] Atomic Layer Deposition (ALD) is a high-precision thin-film deposition technique based on Chemical Vapor Deposition (CVD). It deposits materials as single-atom films layer by layer onto the surface of a substrate using chemical vapor deposition. Specifically, two or more reactive precursors are introduced one at a time into the reaction chamber and adsorbed onto the substrate surface, with each precursor reaching saturation adsorption. During ALD deposition, the reactive precursors are deposited alternately, and the chemical reaction of a new atomic layer is directly related to the previous layer. Each reaction deposits only one atomic layer, making ALD a self-limiting reaction.

[0004] During atomic layer deposition (ALD), when the reaction precursors reach the surface of the substrate, they are deposited on the substrate surface. Between different reaction precursor pulses, the reaction chamber needs to be purged with an inert gas to remove excess reaction precursors that have not been adsorbed on the substrate surface, ensuring that the chemical reaction occurs only on the substrate surface.

[0005] With the advancement of technology, miniaturization is a trend in the microelectromechanical systems (MEMS) industry, and components with high aspect ratio structures are increasingly used, leading to a growing demand. In the semiconductor field, high aspect ratio microstructures refer to microstructures with a depth-to-width ratio greater than 10, formed on silicon wafers or other substrates through processes such as photolithography and etching. These structures typically take the form of deep holes or deep trenches. Related technologies use ALD (Alternating Deposition) to deposit thin films on substrates with high aspect ratio structures. However, the reactive precursors cannot effectively diffuse into the interior of these structures, resulting in incomplete material filling of structures such as deep holes and trenches, which severely impacts the operating efficiency of devices with high aspect ratio structures. Summary of the Invention

[0006] This application provides an atomic layer deposition method and system for high aspect ratio structure devices, to solve the problem that in existing atomic layer deposition methods for thin film deposition on the surface of devices with high aspect ratio structures, the reaction precursor cannot effectively diffuse into the interior of the high aspect ratio structure.

[0007] In a first aspect, this application provides an atomic layer deposition method for high aspect ratio structure devices, the atomic layer deposition method comprising:

[0008] A high aspect ratio structure device is placed inside the reaction chamber, and the reaction chamber is evacuated to a low vacuum state;

[0009] A first reaction precursor is introduced into the reaction chamber, and the introduction of the first reaction precursor is stopped when the introduction time of the first reaction precursor reaches a first time.

[0010] The reaction chamber is subjected to pressurized diffusion treatment. When the pressurized diffusion treatment time reaches the second time, the pressurized diffusion treatment is stopped and the reaction chamber is pumped back to a low vacuum state.

[0011] A second reaction precursor is introduced into the reaction chamber, and the introduction of the second reaction precursor is stopped when the introduction time of the second reaction precursor reaches a third time.

[0012] The reaction chamber is subjected to a pressurized diffusion process. When the pressurized diffusion process reaches a second time, the pressurized diffusion process is stopped and the reaction chamber is pumped back to a low vacuum state to complete the coating on the surface of the high aspect ratio structure device.

[0013] The reaction chamber in this application is connected to a pressurized gas pipeline. By adjusting the opening and closing of the first valve and the second valve, pressurized gas is introduced into the reaction chamber, causing the pressure in the reaction chamber to increase and decrease rapidly. This allows the reaction precursor to quickly enter the deep holes / channels of the high aspect ratio structure device and be effectively adsorbed within the high aspect ratio structure device.

[0014] In some possible implementations, performing a pressurized diffusion process on the reaction chamber, stopping the pressurized diffusion process when the time of the pressurized diffusion process reaches a second time, and pumping the reaction chamber back to a low vacuum state includes:

[0015] A constant flow rate of pressurized gas is introduced into the reaction chamber while the vacuuming of the reaction chamber is stopped. When the time for introducing the pressurized gas or the time for stopping the vacuuming of the reaction chamber reaches a second time, the introduction of the pressurized gas is stopped and the vacuuming of the reaction chamber continues until the reaction chamber is returned to a low vacuum state.

[0016] or,

[0017] The amount of pressurized gas introduced into the reaction chamber is made to change in an anti-periodic manner with the amount of gas pumped out of the reaction chamber. When the time of the anti-periodic change reaches a second time, the anti-periodic change is stopped and the reaction chamber is pumped back to a low vacuum state.

[0018] In some possible implementations, the reaction chamber is connected to a vacuum pump and a pressurized gas pipeline. A first valve is provided on the pipeline connecting the reaction chamber and the vacuum pump, and a second valve is provided on the pressurized gas pipeline connected to the reaction chamber. When a constant flow of pressurized gas is introduced into the reaction chamber and the vacuuming of the reaction chamber is stopped, the first valve is closed and the second valve is opened. When the time for introducing the pressurized gas or the time for stopping the vacuuming of the reaction chamber reaches a second time, the first valve is opened and the second valve is closed, and the vacuum pump continues to evacuate the reaction chamber until the reaction chamber reaches a low vacuum state.

[0019] In some possible implementations, the reaction chamber is connected to a vacuum pump and a pressurized gas pipeline. A first valve and a first butterfly valve are provided on the pipeline connecting the reaction chamber and the vacuum pump. The first butterfly valve is located between the first valve and the reaction chamber. A second valve and a second butterfly valve are provided on the pressurized gas pipeline connected to the reaction chamber. The second butterfly valve is located between the second valve and the reaction chamber. When the amount of pressurized gas introduced into the reaction chamber changes in an anti-periodic manner with the amount of gas pumped into the reaction chamber, the first valve and the second valve open. The opening degree of the first butterfly valve changes in an anti-periodic manner with the opening degree of the second butterfly valve. When the time of the anti-periodic change reaches a second time, the first valve and the second valve open, and the anti-periodic change in the opening degree of the first butterfly valve and the second butterfly valve stops.

[0020] In some possible implementations, the opening degree of the first butterfly valve and the opening degree of the second butterfly valve change in opposite directions periodically, including:

[0021] The opening degree of the first butterfly valve decreases from a preset opening degree to 0%, and then increases from 0% to the preset opening degree; the opening degree of the second butterfly valve increases from 0% to the preset opening degree, and then decreases from the preset opening degree to 0%.

[0022] In some possible implementations, when the reaction chamber is pressurized and diffused, the opening of the first butterfly valve and the opening of the second butterfly valve change in a continuous and synchronous reverse periodic manner. When the opening of the first butterfly valve decreases from a preset opening to 0%, the opening of the second butterfly valve increases from 0% to the preset opening. When the opening of the first butterfly valve increases from 0% to the preset opening, the opening of the second butterfly valve decreases from the preset opening to 0%.

[0023] In some possible implementations, when the time of the reverse periodic change reaches a second time, the opening of the first butterfly valve remains at a preset opening, the opening of the second butterfly valve remains at 0%, and the vacuum pump returns the reaction chamber to a low vacuum state.

[0024] The opening degrees of the first and second butterfly valves in this application are controllable. By simultaneously adjusting the opening degrees of the first and second butterfly valves, the reaction precursor can effectively enter the deep holes of the high aspect ratio structure device. At the same time, it effectively avoids the drawback of insufficient diffusion of the reaction precursor in the structure of the high aspect ratio structure device, and improves the phenomenon that the reaction precursor cannot be fully deposited in the deep holes or channels of the high aspect ratio structure device.

[0025] In some possible implementations, the reaction chamber is further connected to a carrier gas pipeline, which is equipped with a fifth valve. The carrier gas pipeline is connected to a first source bottle and a second source bottle, respectively. The first source bottle stores a first reaction precursor, and the second source bottle stores a second reaction precursor. A third valve is provided on the connection pipeline between the first source bottle and the carrier gas pipeline, and a fourth valve is provided on the connection pipeline between the second source bottle and the carrier gas pipeline. When a high aspect ratio structural device is placed in the reaction chamber, the vacuum pump, the first valve, the second valve, the third valve, the fourth valve, and the fifth valve are closed. When the reaction chamber is evacuated to a low vacuum state, the second valve, the third valve, and the fourth valve are closed, and the vacuum pump, the first valve, and the fifth valve are closed. When the first reaction precursor is introduced into the reaction chamber, the vacuum pump, the first valve, the third valve, and the fifth valve are opened, while the second valve and the fourth valve are closed. When the introduction time of the first reaction precursor reaches a first time, the vacuum pump, the first valve, and the fifth valve are opened, while the second valve, the third valve, and the fourth valve are closed. When the second reaction precursor is introduced into the reaction chamber, the vacuum pump, the first valve, the fourth valve, and the fifth valve are opened, while the second valve and the third valve are closed. When the introduction time of the second reaction precursor reaches a third time, the vacuum pump, the first valve, and the fifth valve are opened, while the second valve, the third valve, and the fourth valve are closed.

[0026] In some possible implementations, the reaction chamber is further connected to a carrier gas pipeline, which is equipped with a fifth valve. The carrier gas pipeline is connected to a first source bottle and a second source bottle, respectively. The first source bottle stores a first reaction precursor, and the second source bottle stores a second reaction precursor. A third valve is provided on the connection pipeline between the first source bottle and the carrier gas pipeline, and a fourth valve is provided on the connection pipeline between the second source bottle and the carrier gas pipeline. When a high aspect ratio structure device is placed in the reaction chamber, the vacuum pump, the first valve, the second valve, the third valve, the fourth valve, and the fifth valve are closed, and the opening degree of the first butterfly valve and the second butterfly valve is 0%. When the reaction chamber is evacuated to a low vacuum state, the third valve and the fourth valve are closed, and the vacuum pump, the first valve, the second valve, and the fifth valve are opened. The opening degree of the first butterfly valve is adjusted to a preset opening degree, and the opening degree of the second butterfly valve is 0%. When the first reaction precursor is introduced into the reaction chamber, the vacuum pump, the first source bottle, the second source bottle, and the third source bottle are connected to a second source bottle. The first, second, third, and fifth valves are open, and the fourth valve is closed. The opening degree of the first butterfly valve is a preset opening degree, and the opening degree of the second butterfly valve is 0%. When the introduction time of the first reaction precursor reaches the first time, the vacuum pump, the first, second, and fifth valves are open, and the third and fourth valves are closed. The opening degree of the first butterfly valve is a preset opening degree, and the opening degree of the second butterfly valve is 0%. When the second reaction precursor is introduced into the reaction chamber, the vacuum pump, the first, second, fourth, and fifth valves are open, and the third valve is closed. The opening degree of the first butterfly valve is a preset opening degree, and the opening degree of the second butterfly valve is 0%. When the introduction time of the second reaction precursor reaches the third time, the vacuum pump, the first, second, and fifth valves are open, and the third and fourth valves are closed. The opening degree of the first butterfly valve is a preset opening degree, and the opening degree of the second butterfly valve is 0%.

[0027] In some possible implementations, the preset opening is 70% to 90%.

[0028] In some possible implementations, the pressure inside the reaction chamber under low vacuum is 1–2 torr, and the pumping speed of the vacuum pump is 500–800 m / s. 3 / h, the flow rate of the carrier gas before passing through the fifth valve is 40-60 sccm, the first time is 0.1-10s, the second time is 1-20s, the third time is 0.1-15s, and the flow rate of the pressurized gas before passing through the second valve is 800-1500 sccm.

[0029] In some possible implementations, the pressurizing gas or carrier gas is any one of nitrogen, argon, helium, or neon.

[0030] In a second aspect, this application provides an atomic layer deposition coating system for high aspect ratio structure devices, which is used in the atomic layer deposition coating method described in the first aspect.

[0031] The atomic layer deposition coating system includes:

[0032] The reaction chamber, the vacuum pump connected to the reaction chamber, the pressurized gas pipeline, and the carrier gas pipeline;

[0033] A first valve is provided on the connecting pipeline between the reaction chamber and the vacuum pump, and a second valve is provided on the pressurizing gas pipeline connected to the reaction chamber;

[0034] A fifth valve is provided on the carrier gas pipeline. The carrier gas pipeline is connected to a first source bottle and a second source bottle. The first source bottle stores a first reaction precursor, and the second source bottle stores a second reaction precursor. A third valve is provided on the connecting pipeline between the first source bottle and the carrier gas pipeline, and a fourth valve is provided on the connecting pipeline between the second source bottle and the carrier gas pipeline. The carrier gas pipeline connects to the first source bottle and the second source bottle, which store the first reaction precursor and the second reaction precursor, respectively.

[0035] In some possible implementations, a first butterfly valve is provided on the connecting pipe between the reaction chamber and the vacuum pump, and the first butterfly valve is located between the first valve and the reaction chamber;

[0036] A second butterfly valve is provided on the pressurized gas pipeline connected to the reaction chamber, and the second butterfly valve is located between the second valve and the reaction chamber; wherein the opening degree of the first butterfly valve and the second butterfly valve is controllable.

[0037] As can be seen from the above, this application provides an atomic layer deposition method and system for high aspect ratio structural devices. The method includes placing the high aspect ratio structural device in a reaction chamber and evacuating the reaction chamber to a low vacuum state; introducing a first reaction precursor into the reaction chamber and stopping the introduction of the first reaction precursor when the introduction time reaches a first time; performing a pressure diffusion treatment on the reaction chamber and stopping the pressure diffusion treatment and evacuating the reaction chamber back to a low vacuum state when the pressure diffusion treatment time reaches a second time; introducing a second reaction precursor into the reaction chamber and stopping the introduction of the second reaction precursor when the introduction time reaches a third time; performing a pressure diffusion treatment on the reaction chamber and stopping the pressure diffusion treatment and evacuating the reaction chamber back to a low vacuum state when the pressure diffusion treatment time reaches a second time, thereby completing the deposition on the surface of the high aspect ratio structural device. This application controls the reaction chamber by coordinating the first and second valves, or by making reverse periodic changes in the opening of the first and second butterfly valves, so as to increase and decrease the pressure in the reaction chamber, thereby enabling the reaction precursor to quickly or effectively enter the deep holes / channels of the high aspect ratio structure device and be adsorbed into the high aspect ratio structure device. Attached Figure Description

[0038] To more clearly illustrate the technical solution of this application, the drawings used in the embodiments will be briefly introduced below. Obviously, for those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0039] Figure 1 is a schematic diagram of a traditional atomic layer deposition coating system;

[0040] Figure 2 is a schematic diagram comparing the atomic layer deposition coating method provided in this application with atomic layer deposition methods in related technologies;

[0041] Figure 3 is a schematic diagram of an atomic layer deposition coating system for high aspect ratio structure devices provided in an embodiment of this application;

[0042] Figure 4 is a schematic diagram of an atomic layer deposition coating system for high aspect ratio structure devices provided in an embodiment of this application;

[0043] Figure 5 is a flowchart of the atomic layer deposition method for high aspect ratio structure devices provided in this application;

[0044] Figure 6 is a pressure curve of the reaction chamber in Embodiment 1 of this application;

[0045] Figure 7 is a SEM image of the deposition sample prepared in Example 1 of this application;

[0046] Figure 8 is an EDS energy dispersive spectroscopy (EDS) analysis diagram of the deposited sample prepared in Example 1 of this application;

[0047] Figure 9 is a pressure curve of the reaction chamber in Embodiment 2 of this application;

[0048] Figure 10 is a SEM image of the deposited sample prepared in Example 2 of this application;

[0049] Figure 11 is an EDS energy dispersive spectroscopy (EDS) analysis diagram of the deposited sample prepared in Example 2 of this application;

[0050] Figure 12 is a pressure curve of the reaction chamber in Comparative Example 1 of this application;

[0051] Figure 13 is a SEM image of the deposition sample prepared in Comparative Example 1 of this application;

[0052] Figure 14 shows the EDS energy dispersive spectroscopy analysis of the deposited sample prepared in Comparative Example 1 of this application;

[0053] Figure 15 is a pressure curve of the reaction chamber in Embodiment 3 of this application;

[0054] Figure 16 is a SEM image of the deposited sample prepared in Example 3 of this application;

[0055] Figure 17 is an EDS energy dispersive spectroscopy (EDS) analysis diagram of the deposited sample prepared in Example 3 of this application;

[0056] Figure 18 is a pressure curve of the reaction chamber in Embodiment 4 of this application;

[0057] Figure 19 is a SEM image of the deposited sample prepared in Example 4 of this application;

[0058] Figure 20 is an EDS energy dispersive spectroscopy (EDS) analysis diagram of the deposited sample prepared in Example 4 of this application;

[0059] Figure 21 is a pressure curve of the reaction chamber in Comparative Example 2 of this application;

[0060] Figure 22 is a SEM image of the deposition sample prepared in Comparative Example 2 of this application;

[0061] Figure 23 shows the EDS energy dispersive spectroscopy analysis of the deposited sample prepared in Comparative Example 2 of this application;

[0062] Figure 24 is a diagram showing the relationship between the preset opening degree and the filling effect of the butterfly valve in Embodiment 2 of this application;

[0063] Figure 25 is a graph showing the relationship between the preset opening degree and the filling effect of the butterfly valve in Embodiment 4 of this application. Detailed Implementation

[0064] The embodiments will now be described in detail, examples of which are illustrated in the accompanying drawings. When the following description relates to the drawings, unless otherwise indicated, the same numbers in different drawings represent the same or similar elements. The embodiments described in the following examples do not represent all embodiments consistent with this application.

[0065] Atomic Layer Deposition (ALD) is a high-precision thin-film deposition technique based on Chemical Vapor Deposition (CVD). It deposits materials as single-atom films layer by layer onto a substrate surface using chemical vapor deposition. Specifically, two or more reaction precursors are introduced one at a time into the reaction chamber and adsorbed onto the substrate surface, with each precursor reaching saturation adsorption. During ALD deposition, the reaction precursors are deposited alternately, and the chemical reaction of a new atomic layer is directly related to the previous layer. Each reaction deposits only one atomic layer, making ALD a self-limiting reaction.

[0066] During atomic layer deposition (ALD), when the reaction precursors reach the surface of the substrate, they are deposited on the substrate surface. Between different reaction precursor pulses, the reaction chamber needs to be purged with an inert gas to remove excess reaction precursors that have not been adsorbed on the substrate surface, ensuring that the chemical reaction occurs only on the substrate surface.

[0067] With the advancement of technology, miniaturization is a trend in the MEMS industry, and components with high aspect ratio structures are increasingly used, leading to a growing demand. Related technologies employ the ALD process to deposit high aspect ratio structures. The equipment used, as shown in Figure 1, includes a vacuum pump, a reaction chamber, a first source bottle, a second source bottle, and carrier gas lines. The first source bottle stores a first reaction precursor, and the second source bottle stores a second reaction precursor. The ALD process involves the first and second reaction precursors alternately entering the reaction chamber using a "pulse + purge" method. After completing a set number of cycles, the reaction ends.

[0068] However, when using the above-mentioned ALD method to deposit thin films on the surface of devices with high aspect ratio structures, the first and second reaction precursors cannot diffuse into the high aspect ratio structure devices quickly and effectively, resulting in insufficient deposition in structures such as deep holes or trenches.

[0069] Based on this, this application provides an atomic layer deposition (ALD) method and system for high aspect ratio devices. The ALD method utilizes a combination of a boost diffuse process and an inert gas purging process. Through the coordinated control of a first valve and a second valve, or by the reverse periodic changes in the opening of the first and second butterfly valves, the pressure within the reaction chamber increases and decreases. This effectively avoids the drawback of insufficient diffusion of the reaction precursor on the surface of high aspect ratio devices and improves the phenomenon of insufficient deposition in structures such as deep holes or trenches. Figure 2 shows a comparative schematic diagram of the ALD method provided in this application and related ALD methods. In Figure 2a, the reaction precursor natural diffusion process of traditional ALD is shown, and in Figure 2b, the reaction precursor boost diffuse process mentioned in this application is shown. The inert gas purging process includes evacuating the reaction chamber to a low vacuum state and a purging operation; the cleaning in Figure 2 is the purging operation, and the pulse is the introduction of the first and / or second reaction precursors.

[0070] As shown in Figure 3, in some embodiments, this application provides an atomic layer deposition system for high aspect ratio structural devices. This atomic layer deposition system is used to implement an atomic layer deposition method for high aspect ratio structural devices. The atomic layer deposition system includes:

[0071] The reaction chamber, the vacuum pump connected to the reaction chamber, the pressurized gas pipeline, and the carrier gas pipeline;

[0072] A first valve V1 is provided on the connecting pipeline between the reaction chamber and the vacuum pump, and a second valve V2 is provided on the pressurized gas pipeline connected to the reaction chamber. The first valve V1 is used to control the vacuum pump's ability to evacuate the reaction chamber, and the second valve V2 is used to determine whether to introduce pressurized gas into the reaction chamber. The first valve V1 and the second valve V2 can be used to control the chamber pressure of the reaction chamber.

[0073] A fifth valve V5 is installed on the carrier gas pipeline. The carrier gas pipeline is connected to a first source bottle and a second source bottle. The first source bottle stores a first reaction precursor, and the second source bottle stores a second reaction precursor. A third valve V3 is installed on the connection line between the first source bottle and the carrier gas pipeline, and a fourth valve V4 is installed on the connection line between the second source bottle and the carrier gas pipeline. The third valve V3, the fourth valve V4, and the fifth valve V5 are used to control whether the first reaction precursor, the second reaction precursor, and the carrier gas are introduced, respectively.

[0074] In this embodiment, by adjusting the opening and closing of the first valve V1 and the second valve V2, pressurized gas is introduced into the reaction chamber, causing the pressure in the reaction chamber to increase and decrease rapidly. This allows the reaction precursor to quickly enter the deep holes / channels of the high aspect ratio structure device and be effectively adsorbed within the high aspect ratio structure device.

[0075] As shown in Figure 4, in some embodiments, this application also provides an atomic layer deposition coating system for high aspect ratio structural devices. Based on the structure disclosed in Figure 3, a first butterfly valve V6 is provided on the connecting pipeline between the reaction chamber and the vacuum pump, and the first butterfly valve V6 is located between the first valve V1 and the reaction chamber; a second butterfly valve V7 is provided on the pressurized gas pipeline connected to the reaction chamber, and the second butterfly valve V7 is located between the second valve V2 and the reaction chamber; wherein, the opening degree of the first butterfly valve V6 and the second butterfly valve V7 is controllable; the first butterfly valve V6 and the second butterfly valve V7 are used to control the pressure in the reaction chamber to rise and fall in a second time period, so that the pressure in the reaction chamber is dynamically changing. The first butterfly valve V6 is used to control the pumping volume of the vacuum pump, and the second butterfly valve V7 is used to control the inflow rate of the pressurized gas. After the reaction is completed, closing the first valve V1 effectively prevents the gas flow in the vacuum pump from flowing back into the reaction chamber, and closing the second valve V2 effectively prevents the pressurized gas from entering the reaction chamber.

[0076] In this application, the opening degrees of the first butterfly valve V6 and the second butterfly valve V7 are controllable. After the reaction precursor enters the reaction chamber, the opening degrees of the first butterfly valve V6 and the second butterfly valve V7 change in opposite directions periodically, causing the pressure inside the reaction chamber to increase and decrease. This allows the reaction precursor to effectively enter the deep holes of high aspect ratio structural devices, while effectively avoiding the drawback of insufficient diffusion of the reaction precursor in the structure of high aspect ratio structural devices, and improving the phenomenon that the reaction precursor cannot be fully deposited in deep holes or channels of high aspect ratio structural devices. The atomic layer deposition coating system provided in the embodiment shown in Figure 4 has a slower increase or decrease in pressure inside the reaction chamber during the pressurized diffusion process compared to the atomic layer deposition coating system shown in Figure 3, but it is still relatively fast compared to the prior art, that is, the pressure inside the reaction chamber increases and decreases more slowly.

[0077] As shown in Figure 5, in some embodiments, this application also provides an atomic layer deposition method for high aspect ratio structure devices, the method comprising:

[0078] The high aspect ratio structure device is placed in the reaction chamber, and the reaction chamber is evacuated to a low vacuum state;

[0079] A first reaction precursor is introduced into the reaction chamber, and the introduction of the first reaction precursor is stopped when the introduction time of the first reaction precursor reaches the first time.

[0080] The reaction chamber is subjected to pressurized diffusion treatment. When the pressurized diffusion treatment time reaches the second time, the pressurized diffusion treatment is stopped and the reaction chamber is pumped back to a low vacuum state.

[0081] A second reaction precursor is introduced into the reaction chamber, and the introduction of the second reaction precursor is stopped when the introduction time of the second reaction precursor reaches the third time.

[0082] The reaction chamber is subjected to pressurized diffusion treatment. When the pressurized diffusion treatment reaches the second time, the pressurized diffusion treatment is stopped and the reaction chamber is pumped back to a low vacuum state to complete the coating on the surface of the high aspect ratio structure device.

[0083] In this atomic layer deposition method, the pressurized diffusion process in the reaction chamber, and the pressurized diffusion process being stopped and the reaction chamber being evacuated to a low vacuum state when the pressurized diffusion process reaches a second time, includes:

[0084] A constant flow rate of pressurized gas is introduced into the reaction chamber while the vacuuming of the reaction chamber is stopped. When the time for introducing the pressurized gas or the time for stopping the vacuuming of the reaction chamber reaches the second time, the pressurized gas is stopped and the vacuuming of the reaction chamber continues until the reaction chamber is evacuated back to a low vacuum state.

[0085] or,

[0086] The amount of pressurized gas introduced into the reaction chamber is made to change in an anti-periodic manner with the amount of gas pumped out of the reaction chamber. When the time of the anti-periodic change reaches the second time, the anti-periodic change is stopped and the reaction chamber is pumped back to a low vacuum state.

[0087] Because the flow rate of the pressurized gas varies (constant or periodically changing), the atomic layer deposition coating process is also different. The implementation of atomic layer deposition coating methods also corresponds to atomic layer deposition coating systems with different structures, which will be introduced separately below.

[0088] In some embodiments, this application provides an atomic layer deposition method for high aspect ratio structural devices. This embodiment corresponds to the atomic layer deposition system for high aspect ratio structural devices shown in Figure 3. When the high aspect ratio structural device is placed in the reaction chamber, the reaction chamber door is opened, and simultaneously the vacuum pump, first valve V1, second valve V2, third valve V3, fourth valve V4, and fifth valve V5 are closed. After the high aspect ratio structural device is placed in the reaction chamber, the reaction chamber door is closed, and simultaneously the second valve V2, third valve V3, and fourth valve V4 are closed, while the vacuum pump, first valve V1, and fifth valve V5 are opened to evacuate the reaction chamber. When a first reaction precursor is introduced into the reaction chamber, the vacuum pump, First valve V1, third valve V3, and fifth valve V5 are opened, while second valve V2 and fourth valve V4 are closed. When the introduction time of the first reaction precursor reaches the first time, the vacuum pump, first valve V1, and fifth valve V5 are opened, while second valve V2, third valve V3, and fourth valve V4 are closed. When the second reaction precursor is introduced into the reaction chamber, the vacuum pump, first valve V1, fourth valve V4, and fifth valve V5 are opened, while second valve V2 and third valve V3 are closed. When the introduction time of the second reaction precursor reaches the third time, the vacuum pump, first valve V1, and fifth valve V5 are opened, while second valve V2, third valve V3, and fourth valve V4 are closed.

[0089] To facilitate a clear understanding of the function of each valve and for easy differentiation, the first valve V1, the second valve V2, the third valve V3, the fourth valve V4, and the fifth valve V5 will be referred to as vacuum angle valve V1, pressure boosting valve V2, source valve V3, source valve V4, and carrier gas valve V5, respectively, in the following text.

[0090] The atomic layer deposition method provided in this embodiment includes:

[0091] S1: Place the high aspect ratio structure device inside the reaction chamber and evacuate the reaction chamber to a low vacuum state. The high aspect ratio structure device has a high aspect ratio micro / nano structure. The pressure inside the reaction chamber under low vacuum is 1–2 torr.

[0092] The process of placing a high aspect ratio structure device inside the reaction chamber and evacuating the reaction chamber to a low vacuum state includes:

[0093] The high aspect ratio structure device is placed in the reaction chamber, carrier gas is introduced into the reaction chamber, and the vacuum pump is turned on to perform a vacuum operation on the reaction chamber.

[0094] When the pressure inside the reaction chamber reaches the preset pressure value, the first reaction precursor is introduced into the reaction chamber. The preset pressure value is 1-2 torr, and the pumping speed of the vacuum pump is 500-800 m / s. 3 / h, the flow rate of carrier gas before the carrier gas valve V5 is the same as the flow rate into the reaction chamber, both being 40-60 sccm.

[0095] Specifically, the door of the wafer loading platform inside the reaction chamber is opened, and high aspect ratio structural devices are placed. During this process, the vacuum pump, vacuum angle valve V1, pressure boosting valve V2, source valve V3, source valve V4, and carrier gas valve V5 are closed. It should be noted that when carrier gas valve V5 is closed, the carrier gas in the carrier gas pipeline pushes against carrier gas valve V5; when pressure boosting valve V2 is closed, the pressurized gas in the pressurized gas pipeline pushes against pressurized gas valve V2. After the high aspect ratio structural devices are placed, the door of the wafer loading platform inside the reaction chamber is closed, and the vacuum pump is turned on to perform a vacuuming operation on the reaction chamber. Carrier gas valve V5, vacuum pump, and vacuum angle valve V1 are opened, and the pumping speed of the vacuum pump is 500-800 m / s. 3 / h, the carrier gas flow rate is the same as above, the reaction chamber is evacuated to a low vacuum state, the pressure value of the reaction chamber is 1~2 torr, during this process, the pressure boosting valve V2 is closed, and the source valves V3 and V4 are closed.

[0096] The carrier gas valve V5 and vacuum pump are opened during vacuuming and closed after the coating of the high aspect ratio structure device surface is completed.

[0097] S2: Introduce the first reaction precursor into the reaction chamber, and stop introducing the first reaction precursor when the introduction time of the first reaction precursor reaches the first time.

[0098] Specifically, after the reaction chamber reaches a low vacuum state, source valve V3 opens, introducing the first reaction precursor. When the introduction time of the first reaction precursor reaches a first time, source valve V3 closes, stopping the introduction of the first reaction precursor. The first time is 0.1–10 s. The mass of the first source bottle is determined based on the actual reaction precursor. During this process, pressure boosting valve V2 is closed, source valve V4 is closed, vacuum angle valve V1 is open, and carrier gas valve V5 is open. For example, when the first reaction precursor is TMA (trimethylaluminum), the TMA feed rate is 1–2 mg, and the first time is 0.1–2 s; when the first reaction precursor is Cu(acac)₂ (copper acetylacetone), the Cu(acac)₂ feed rate is 1–3 mg, and the first time is 3–6 s.

[0099] S3: A constant flow rate of pressurized gas is introduced into the reaction chamber while the vacuum process is simultaneously stopped. When the time for introducing the pressurized gas or the time for stopping the vacuum process reaches a second time interval, the pressurized gas supply is stopped, and the vacuum process continues until the reaction chamber is returned to a low vacuum state. In some embodiments, after the reaction chamber is evacuated to a low vacuum state, a purging operation is also included. The inert gas purging process includes evacuating the reaction chamber to a low vacuum state and the purging operation. The purging operation takes 5–10 seconds.

[0100] In this process, when a constant flow of pressurized gas is introduced into the reaction chamber and the vacuuming of the reaction chamber is stopped at the same time, the operation of introducing pressurized gas and the operation of stopping the vacuuming of the reaction chamber are performed simultaneously. That is, when the pressurization valve V2 is opened, the vacuum angle valve V1 is closed. The time for introducing pressurized gas and the time for stopping the vacuuming of the reaction chamber are the same, both being the second time.

[0101] By adjusting the opening and closing of vacuum valve V1 and pressure boosting valve V2, pressurized gas is introduced into the reaction chamber, causing the pressure in the reaction chamber to increase and decrease rapidly. This allows the reaction precursor to quickly enter the deep holes / channels of the high aspect ratio structure device and be effectively adsorbed within the device.

[0102] In this embodiment, after each introduction of the reaction precursor gas, a large amount of pressurized gas is introduced, while the vacuum pump continuously evacuates the reaction chamber, causing the pressure in the reaction chamber to increase and decrease rapidly, so that the reaction precursor can diffuse fully within the reaction chamber. Therefore, this process is called pressurized diffusion treatment. A pressurized diffusion treatment is performed each time the reaction precursor is introduced for deposition. That is, the atomic layer deposition method provided in this application includes multiple pressurized diffusion treatments. Taking the deposition of two reaction precursors as an example, this atomic layer deposition method includes two pressurized diffusion treatments. The first pressurized diffusion treatment specifically includes:

[0103] During the first pressurized diffusion process, pressurized valve V2 is opened and vacuum valve V1 is closed, allowing pressurized gas to be introduced. When the pressurized gas introduction time or the time for stopping evacuation of the reaction chamber reaches a second time, pressurized valve V2 closes and vacuum valve V1 opens, where the second time is 1–20 seconds. During this process, source valves V3 and V4 remain closed, and carrier gas valve V5 remains open. When pressurized valve V2 is open, the maximum pressure inside the reaction chamber can reach 1.5–2.0 torr.

[0104] After closing the pressure boosting valve V2, the reaction chamber is evacuated to a low vacuum state. The flow rate of the pressurized gas before passing through the pressure boosting valve V2 is the same as the flow rate entering the reaction chamber, both being 800–1500 sccm. The inert gas purging process includes evacuating the reaction chamber to a low vacuum state and then purging. The purging operation takes 5–10 seconds.

[0105] For example, the pressurizing gas or carrier gas is any one of nitrogen, argon, helium, or neon.

[0106] S4: Introduce the second reaction precursor into the reaction chamber, and stop introducing the second reaction precursor when the introduction time of the second reaction precursor reaches the third time.

[0107] Specifically, when the reaction chamber reaches a low vacuum state again, source valve V4 opens, introducing the second reaction precursor. When the second reaction precursor has been introduced for a third time period (0.1–15 s), source valve V4 closes, stopping the introduction of the second reaction precursor. The mass of the second source bottle is determined based on the actual reaction precursor. During this process, pressure boosting valve V2 is closed, source valve V3 is closed, vacuum angle valve V1 is open, and carrier gas valve V5 is open. For example, when the second reaction precursor is H2O (liquid), the H2O input rate is 1–3 mg, and the third time period is 0.1–2 s; when the second reaction precursor is H2 (gaseous), the H2 input rate is 3–6 L, and the third time period is 5–15 s.

[0108] S5: Introduce pressurized gas with a constant flow rate into the reaction chamber while simultaneously stopping the evacuation of the reaction chamber. When the time for introducing the pressurized gas or the time for stopping the evacuation of the reaction chamber reaches the second time, stop introducing the pressurized gas and continue evacuating the reaction chamber until the reaction chamber is evacuated back to a low vacuum state.

[0109] After the second reaction precursor is introduced, pressurized gas is introduced to perform a second pressurized diffusion treatment, which specifically includes:

[0110] During the second pressurized diffusion process, pressurized valve V2 is opened and vacuum valve V1 is closed, allowing pressurized gas to be introduced. When the pressurized gas introduction time or the time for stopping evacuation of the reaction chamber reaches a second time, pressurized valve V2 closes and vacuum valve V1 opens to evacuate the reaction chamber to a low vacuum state; the second time is 1–20 seconds. During this process, source valves V3 and V4 remain closed, and carrier gas valve V5 remains open.

[0111] When the reaction chamber is evacuated to a low vacuum state, the booster valve V2, source valve V3, and source valve V4 remain closed, while the vacuum pump, vacuum angle valve V1, and carrier gas valve V5 remain open. After the reaction chamber reaches a low vacuum state, it is also purged with inert gas for 5–10 seconds.

[0112] Steps S2 to S5 constitute one deposition cycle. The number of deposition cycles is determined based on the desired film thickness, and steps S2 to S5 are repeated until a film of the target thickness is obtained on the surface of a high aspect ratio structure device.

[0113] After the coating on the surface of the high aspect ratio structure device is completed, the vacuum pump, vacuum valve V1, booster valve V2, source valve V3, source valve V4, and carrier gas valve V5 are turned off. The wafer loading platform door in the reaction chamber is then opened to remove the high aspect ratio structure device. In some embodiments, the deposition cycle is 100 to 200 times.

[0114] In this embodiment, after each introduction of the reaction precursor gas, a booster gas is introduced, and the vacuum pump is stopped from continuously evacuating the reaction chamber. By adjusting the opening and closing of the vacuum angle valve V1 and the booster valve V2, the booster gas enters the reaction chamber, causing the pressure in the reaction chamber to increase or decrease. This allows the reaction precursor to quickly enter the deep holes / channels of the high aspect ratio structure device and be effectively adsorbed within the high aspect ratio structure device.

[0115] In some embodiments, this application provides an atomic layer deposition (ALD) method for high aspect ratio (HAR) structural devices. This embodiment corresponds to the ALD system for HAR structural devices shown in Figure 4. The ALD system includes a reaction chamber, a vacuum pump connected to the reaction chamber, a pressurized gas pipeline, and a carrier gas pipeline. A vacuum valve V1 is provided on the pipeline connecting the reaction chamber and the vacuum pump, and a pressurized valve V2 is provided on the pressurized gas pipeline connected to the reaction chamber. After the reaction is completed, the vacuum valve V1 closes to effectively prevent the gas flow from the vacuum pump from flowing back into the reaction chamber, and the pressurized valve V2 effectively prevents the pressurized gas from entering the reaction chamber. A carrier gas valve V5 is provided on the carrier gas pipeline, which is connected to a first source bottle and a second source bottle. The first source bottle stores a first reaction precursor, and the second source bottle stores a second reaction precursor. A source valve V3 is provided on the pipeline connecting the first source bottle and the carrier gas pipeline, and a source valve V4 is provided on the pipeline connecting the second source bottle and the carrier gas pipeline. Among them, source valve V3, source valve V4 and carrier gas valve V5 are used to control whether the first reaction precursor is introduced, whether the second reaction precursor is introduced, and whether the carrier gas is introduced, respectively.

[0116] A first butterfly valve V6 is installed on the connecting pipeline between the reaction chamber and the vacuum pump, located between the vacuum angle valve V1 and the reaction chamber. A second butterfly valve V7 is installed on the pressurized gas pipeline connected to the reaction chamber, located between the pressurization valve V2 and the reaction chamber. The opening degrees of the first butterfly valve V6 and the second butterfly valve V7 are controllable, and their opening degrees change in opposite periods. The first butterfly valve V6 and the second butterfly valve V7 are used to control the pressure in the reaction chamber to rise and fall within a second time interval, so that the pressure in the reaction chamber is dynamically changing. The first butterfly valve V6 is used to control the pumping volume of the vacuum pump, and the second butterfly valve V7 is used to control the flow rate of the pressurized gas.

[0117] When the high aspect ratio structure device is placed in the reaction chamber, the reaction chamber door is opened, and the vacuum pump, vacuum angle valve V1, booster valve V2, source valve V3, source valve V4, and carrier gas valve V5 are closed. The opening degree of the first butterfly valve V6 and the second butterfly valve V7 are 0%. After the high aspect ratio structure device is placed in the reaction chamber, the reaction chamber door is closed, and the vacuum pump, vacuum angle valve V1, booster valve V2, and carrier gas valve V5 are opened, while the source valves V3 and V4 are closed. The opening degree of the first butterfly valve V6 is adjusted to the preset opening degree, and the opening degree of the second butterfly valve V7 is 0%, so as to evacuate the reaction chamber to a low vacuum.

[0118] When the reaction chamber reaches a low vacuum state, the first reaction precursor is introduced into the reaction chamber. At this time, the vacuum pump, vacuum angle valve V1, pressure boosting valve V2, source valve V3, and carrier gas valve V5 are opened, while the source valve V4 is closed. The opening degree of the first butterfly valve V6 is the preset opening degree, and the opening degree of the second butterfly valve V7 is 0%. When the introduction time of the first reaction precursor reaches the first time, the vacuum pump, vacuum angle valve V1, pressure boosting valve V2, and carrier gas valve V5 are opened, while the source valves V3 and V4 are closed. The opening degree of the first butterfly valve V6 is the preset opening degree, and the opening degree of the second butterfly valve V7 is 0%. When the amount of pressurized gas introduced into the reaction chamber changes periodically in the opposite direction to the amount of gas pumped out of the reaction chamber, the vacuum pump, vacuum angle valve V1, and pressure boosting valve V5 are opened. Carrier gas valve V5 opens, while source valves V3 and V4 close. The openings of the first butterfly valve V6 and the second butterfly valve V7 change in an anti-cyclical manner. When the opening of the first butterfly valve decreases from a preset opening to 0%, and then increases from 0% to the preset opening, the opening of the second butterfly valve increases from 0% to the preset opening, and then decreases from the preset opening to 0%. When the time of the anti-cyclical change reaches the second time, the vacuum pump, vacuum angle valve V1, booster valve V2, and carrier gas valve V5 open, while source valves V3 and V4 close. The anti-cyclical changes in the openings of the first butterfly valve V6 and the second butterfly valve V7 stop, and the opening of the first butterfly valve V6 remains at the preset opening, while the opening of the second butterfly valve V7 remains at 0%.

[0119] When the reaction chamber is evacuated to a low vacuum state, the vacuum pump, vacuum angle valve V1, pressure boosting valve V2, and carrier gas valve V5 are opened, while source valves V3 and V4 are closed. The opening degree of the first butterfly valve V6 is the preset opening degree, and the opening degree of the second butterfly valve V7 is 0%. When the second reaction precursor is introduced into the reaction chamber, the vacuum pump, vacuum angle valve V1, pressure boosting valve V2, source valve V4, and carrier gas valve V5 are opened, while source valve V3 is closed. The opening degree of the first butterfly valve V6 is the preset opening degree, and the opening degree of the second butterfly valve V7 is 0%. When the introduction time of the second reaction precursor reaches the third time, the vacuum pump, vacuum angle valve V1, pressure boosting valve V2, and carrier gas valve V5 are opened, while source valves V3 and V4 are closed. The opening degree of the first butterfly valve V6 is the preset opening degree, and the opening degree of the second butterfly valve V7 is 0%.

[0120] The atomic layer deposition (ALD) coating method provided in this embodiment is the same as that provided in the above embodiments, and will not be repeated for the same content. For ease of understanding and differentiation of the functions of each valve, the first butterfly valve V6 and the second butterfly valve V7 will be referred to as APC butterfly valve V6 and APC butterfly valve V7 respectively in the following text.

[0121] The atomic layer deposition method provided in this embodiment includes:

[0122] S1': Place the high aspect ratio structure device inside the reaction chamber and evacuate the reaction chamber to a low vacuum state.

[0123] Specifically, the wafer loading platform door inside the reaction chamber is opened, and high aspect ratio structural devices are placed. During this process, the vacuum pump, vacuum angle valve V1, booster valve V2, source valve V3, source valve V4, and carrier gas valve V5 are closed. The opening degrees of APC butterfly valve V6 and APC butterfly valve V7 are 0%. It should be noted that when carrier gas valve V5 is closed, the carrier gas in the carrier gas pipeline pushes against carrier gas valve V5; when booster valve V2 is closed, the booster gas in the booster gas pipeline pushes against booster valve V2. After the high aspect ratio structural devices are placed, the wafer loading platform door inside the reaction chamber is closed, and the vacuum pump is turned on to evacuate the reaction chamber. During this process, carrier gas valve V5, vacuum pump, vacuum angle valve V1, and booster valve V2 are opened, source valves V3 and V4 are closed, the opening degree of APC butterfly valve V6 is adjusted to the preset opening degree, and the opening degree of APC butterfly valve V7 is 0%. The pumping speed of the vacuum pump is 500-800 m / s. 3 / h, the flow rate of the carrier gas before the carrier gas valve V5 is the same as the flow rate into the reaction chamber, both being 40-60 sccm. The reaction chamber is evacuated to a low vacuum state, and the pressure value of the reaction chamber is 1-2 torr. The flow rate of the booster gas before the booster valve V2 is the same as the flow rate into the reaction chamber, and the booster gas flow rate is 800-1500 sccm.

[0124] The vacuum pump, vacuum angle valve V1, pressure boosting valve V2, and carrier gas valve V5 are opened during vacuuming and closed after the coating of the high aspect ratio structure device surface is completed.

[0125] S2': Introduce the first reaction precursor into the reaction chamber, and stop introducing the first reaction precursor when the introduction time of the first reaction precursor reaches the first time.

[0126] Specifically, after the reaction chamber reaches a low vacuum state, source valve V3 opens to introduce the first reaction precursor. When the introduction time of the first reaction precursor reaches a first time, source valve V3 closes to stop the introduction of the first reaction precursor. The first time is 0.1–10 s. The mass of the first source bottle is determined according to the actual reaction precursor. During this process, source valve V4 is closed, the opening degree of APC butterfly valve V6 is the preset opening degree, and the opening degree of APC butterfly valve V7 is 0%. For example, when the first reaction precursor is TMA (trimethylaluminum), the TMA introduction amount is 1–2 mg, and the first time is 0.1–2 s; when the first reaction precursor is Cu(acac)2 (copper acetylacetonate), the Cu(acac)2 introduction amount is 1–3 mg, and the first time is 3–6 s.

[0127] S3': The amount of pressurized gas introduced into the reaction chamber changes in an anti-periodic manner with the amount of gas pumped out of the reaction chamber. When the time of the anti-periodic change reaches the second time, the anti-periodic change is stopped and the reaction chamber is pumped back to a low vacuum state.

[0128] Among them, the pressurized gas volume is the flow rate of the pressurized gas before passing through the pressurization valve V2, and the pumping volume is the pumping volume of the vacuum pump.

[0129] When the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped out of the reaction chamber change in an anti-cyclical manner, the opening degrees of APC butterfly valve V6 and APC butterfly valve V7 also change in an anti-cyclical manner. When the time of this anti-cyclical change reaches a second time interval, the opening degrees of APC butterfly valve V6 and APC butterfly valve V7 cease their anti-cyclical changes. During this process, source valves V3 and V4 are closed. The second time interval is 1–20 seconds.

[0130] When the opening of APC butterfly valve V6 decreases from the preset opening to 0%, and then increases back to the preset opening, simultaneously, the opening of APC butterfly valve V7 increases from 0% to the preset opening, and then decreases back to 0%. This is called one reverse periodic change, and the time for one reverse periodic change is 1-20 seconds, i.e., the second time interval. When the time for the reverse periodic change reaches the second time interval, the opening of APC butterfly valve V6 remains at the preset opening, and the opening of APC butterfly valve V7 remains at 0%. The vacuum pump then returns the reaction chamber to a low vacuum state.

[0131] S31': The opening degree of APC butterfly valve V6 and the opening degree of APC butterfly valve V7 change in a continuous and synchronous reverse periodic manner. When the opening degree of APC butterfly valve V6 decreases from the preset opening degree to 0%, the opening degree of APC butterfly valve V7 increases from 0% to the preset opening degree. When the opening degree of APC butterfly valve V6 increases from 0% to the preset opening degree, the opening degree of APC butterfly valve V7 decreases from the preset opening degree to 0%. For example, the preset opening degree is 70-90%.

[0132] When the opening of APC butterfly valve V7 decreases, the flow rate of pressurized gas after passing through pressurization valve V2 decreases; when the opening of APC butterfly valve V7 increases, the flow rate of pressurized gas after passing through pressurization valve V2 increases. For example, taking a preset opening of 80% as an example, the opening of APC butterfly valve V6 decreases from 80% to 0%, and then increases from 0% to 80%; the opening of APC butterfly valve V7 increases from 0% to 80%, and then decreases from 80% to 0%.

[0133] S32': When the time of the reverse periodic change reaches the second time, the opening of APC butterfly valve V6 is maintained at the preset opening, the opening of APC butterfly valve V7 is maintained at 0%, and the vacuum pump draws the reaction chamber back to a low vacuum state.

[0134] Specifically, when the time of the reverse periodic change reaches the second time, the opening of APC butterfly valve V6 and the opening of APC butterfly valve V7 stop changing in the reverse periodic manner, the opening of APC butterfly valve V6 is maintained at the preset opening, the opening of APC butterfly valve V7 is maintained at 0%, and the reaction chamber is pumped back to a low vacuum state.

[0135] In some embodiments, after the reaction chamber is evacuated to a low vacuum state, a purging operation is also included. The inert gas purging process includes evacuating the reaction chamber to a low vacuum state and then purging. Specifically, the purging operation involves purging the reaction chamber with inert gas. The purging time is 5–10 seconds.

[0136] S4': Introduce the second reaction precursor into the reaction chamber, and stop introducing the second reaction precursor when the introduction time of the second reaction precursor reaches the third time.

[0137] Specifically, after the vacuum pump returns the reaction chamber to a low vacuum state, source valve V4 opens, introducing the second reaction precursor. When the second reaction precursor has been introduced for a third time period (0.1–15 s), source valve V4 closes, stopping the introduction of the second reaction precursor. The mass of the second source bottle is determined based on the actual reaction precursor. During this process, source valve V3 is closed, the APC butterfly valve V6 is at a preset opening, and the APC butterfly valve V7 is at 0%. For example, when the second reaction precursor is H2O (liquid), the H2O input is 1–3 mg, and the third time period is 0.1–2 s; when the second reaction precursor is H2 (gaseous), the H2 input is 3–6 L, and the third time period is 5–15 s.

[0138] S5': The amount of pressurized gas introduced into the reaction chamber changes in an anti-periodic manner with the amount of gas pumped out of the reaction chamber. When the time of the anti-periodic change reaches the second time, the anti-periodic change is stopped and the reaction chamber is pumped back to a low vacuum state.

[0139] When the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped out of the reaction chamber change in an anti-periodic pattern, the opening degrees of APC butterfly valve V6 and APC butterfly valve V7 change continuously and synchronously in an anti-periodic pattern. When the time of this anti-periodic change reaches a second time interval, the opening degrees of APC butterfly valve V6 and APC butterfly valve V7 cease their anti-periodic changes. During this process, source valves V3 and V4 are closed. The second time interval is 1–20 seconds.

[0140] When the time of the reverse periodic change reaches the second time, the opening of APC butterfly valve V6 remains at the preset opening, the opening of APC butterfly valve V7 remains at 0%, and the vacuum pump returns the reaction chamber to a low vacuum state.

[0141] S51': The opening degree of APC butterfly valve V6 changes in an inverse periodic manner with the opening degree of APC butterfly valve V7. When the opening degree of APC butterfly valve V6 decreases from the preset opening degree to 0%, the opening degree of APC butterfly valve V7 increases from 0% to the preset opening degree. When the opening degree of APC butterfly valve V6 increases from 0% to the preset opening degree, the opening degree of APC butterfly valve V7 decreases from the preset opening degree to 0%. For example, the preset opening degree is 70-90%.

[0142] When the opening degree of APC butterfly valve V7 decreases, the flow rate of pressurized gas after passing through pressurization valve V2 decreases; when the opening degree of APC butterfly valve V7 increases, the flow rate of pressurized gas after passing through pressurization valve V2 increases. For example, taking a preset opening degree of 80% as an example, the opening degree of APC butterfly valve V6 changes from 80% to 0%, and then from 0% to 80%; the opening degree of APC butterfly valve V7 changes from 0% to 80%, and then from 80% to 0%.

[0143] S52': When the time of the reverse periodic change reaches the second time, the opening of APC butterfly valve V6 is maintained at the preset opening, the opening of APC butterfly valve V7 is maintained at 0%, and the vacuum pump draws the reaction chamber back to a low vacuum state.

[0144] Specifically, when the time for the reverse periodic change reaches the second time interval, the opening degrees of APC butterfly valve V6 and APC butterfly valve V7 cease their reverse periodic changes. The opening degree of APC butterfly valve V6 is maintained at the preset opening degree, and the opening degree of APC butterfly valve V7 is maintained at 0%. Simultaneously, the reaction chamber is evacuated to a low vacuum state. After the reaction chamber reaches the low vacuum state, it is further purged with inert gas for 5–10 seconds.

[0145] Steps S2' to S5' constitute one deposition cycle. The number of deposition cycles is determined based on the target thickness of the desired film, and steps S2' to S5' are repeated until a film of the target thickness is obtained on the surface of a high aspect ratio structure device.

[0146] When the deposition on the surface of the high aspect ratio structure device is completed, the vacuum pump, vacuum valve V1, booster valve V2, source valve V3, source valve V4, and carrier gas valve V5 are turned off. The opening degree of APC butterfly valves V6 and V7 is 0%. The wafer loading platform door in the reaction chamber is opened to remove the high aspect ratio structure device. In some embodiments, the number of deposition cycles is 100 to 200.

[0147] In this application, the opening degrees of APC butterfly valves V6 and V7 are controllable. After the reaction precursor enters the reaction chamber, adjusting the opening degrees of APC butterfly valves V6 and V7 increases and decreases the pressure inside the reaction chamber. By making reverse periodic changes in the opening degrees of APC butterfly valves V6 and V7, the reaction precursor can effectively enter the deep holes of high aspect ratio structural devices. At the same time, it effectively avoids the drawback of insufficient diffusion of the reaction precursor in the structure of high aspect ratio structural devices, and improves the phenomenon that the reaction precursor cannot be fully deposited in the deep holes or channels of high aspect ratio structural devices.

[0148] The following detailed explanation will be provided with specific examples.

[0149] The high aspect ratio structures used in the following embodiments are all deep-hole structures with an aspect ratio of 300:1. The pressurizing gas or carrier gas used in the following embodiments is any one of nitrogen, argon, helium, and neon. The pumping speed of the vacuum pump, the flow rate of the carrier gas, and the pressure value for evacuating the reaction chamber to a low vacuum state are all the same in the following embodiments, and these parameters are maintained at the same level during the deposition process of the high aspect ratio structures.

[0150] Example 1

[0151] In this embodiment, the first reaction precursor is TMA (trimethylaluminum), and the second reaction precursor is H2O. The system device connection used in this embodiment is shown in Figure 3. In this embodiment, the flow rate of the pressurized gas is constant.

[0152] (1) Open the door of the wafer loading platform inside the reaction chamber and place the high aspect ratio structure device. During this process, the vacuum pump, vacuum angle valve V1, booster valve V2, source valve V3, source valve V4, and carrier gas valve V5 are closed. After placing the high aspect ratio structure device, close the door of the wafer loading platform inside the reaction chamber and simultaneously turn on the vacuum pump to evacuate the reaction chamber. At the same time, open the carrier gas valve V5, the vacuum pump, and the vacuum angle valve V1, close the booster valve V2, and close the source valves V3 and V4. The pumping speed of the vacuum pump is 600 m / s. 3The carrier gas flow rate is 40 sccm / h, evacuating the reaction chamber to a low vacuum state, with a pressure of 1 torr. When carrier gas valve V5 is closed, the carrier gas in the carrier gas pipeline pushes against carrier gas valve V5; when pressure booster valve V2 is closed, the pressure booster gas in the pressure booster gas pipeline pushes against pressure booster valve V2. The vacuum pump is turned on during the evacuation operation of the reaction chamber and remains on until the coating of the high aspect ratio structure device surface is completed, after which it is turned off.

[0153] (2) When the reaction chamber reaches a low vacuum state, source valve V3 opens and the first reaction precursor is introduced. When the introduction time of the first reaction precursor reaches the first time interval, source valve V3 closes and the introduction of the first reaction precursor stops. The first time interval is 0.2s, and the mass of the first source bottle is 1.5mg. During this process, pressure boosting valve V2 is closed, source valve V4 is closed, vacuum angle valve V1 is open, carrier gas valve V5 is open, and vacuum pump is turned on.

[0154] (3) During the pressurized diffusion process, when a constant flow of pressurized gas is introduced into the reaction chamber while the vacuum in the reaction chamber is simultaneously stopped, the pressurization valve V2 is opened and the vacuum angle valve V1 is closed, and the pressurized gas is introduced. When the time for the pressurized gas to be introduced or the time for stopping the vacuum in the reaction chamber reaches the second time, the pressurized gas is stopped, the pressurization valve V2 is closed, and the vacuum angle valve V1 is opened to evacuate the reaction chamber to a low vacuum state; wherein, the second time is 5s, and the flow rate of the pressurized gas is 1000sccm. During this process, the source valves V3 and V4 remain closed, and the carrier gas valve V5 remains open.

[0155] When the reaction chamber is evacuated to a low vacuum state, the carrier gas valve V5, vacuum pump, and vacuum angle valve V1 are opened. At this time, the booster valve V2 is closed, and the source valves V3 and V4 are closed. After the reaction chamber reaches a low vacuum state, it is also purged with inert gas for 8 seconds.

[0156] (4) After purging, source valve V4 is opened to introduce the second reaction precursor. When the second reaction precursor has been introduced for a third time period, source valve V4 is closed to stop the introduction of the second reaction precursor. The third time period is 0.2s, and the mass of the second source bottle is 1.5mg. During this process, pressure boosting valve V2 is closed, source valve V3 is closed, vacuum pump is turned on, vacuum angle valve V1 is opened, and carrier gas valve V5 is opened.

[0157] (5) During the pressurized diffusion process, when a constant flow of pressurized gas is introduced into the reaction chamber while the vacuum in the reaction chamber is simultaneously stopped, the pressurization valve V2 is opened and the vacuum angle valve V1 is closed, and the pressurized gas is introduced. When the time for the pressurized gas to be introduced or the time for stopping the vacuum in the reaction chamber reaches a second time, the pressurized gas is stopped, the pressurization valve V2 is closed, and the vacuum angle valve V1 is opened to evacuate the reaction chamber to a low vacuum state; wherein, the second time is 5s, and the flow rate of the pressurized gas is 1000sccm. During this process, the source valves V3 and V4 remain closed, and the carrier gas valve V5 remains open.

[0158] When the reaction chamber is evacuated to a low vacuum state, the booster valve V2, source valve V3, and source valve V4 remain closed, while the vacuum pump, vacuum angle valve V1, and carrier gas valve V5 remain open. Once the reaction chamber reaches a low vacuum state, it is also purged with inert gas for 8 seconds.

[0159] Steps (2) to (5) constitute one deposition cycle.

[0160] After 150 deposition cycles, the vacuum pump, vacuum valve V1, booster valve V2, source valve V3, source valve V4, and carrier gas valve V5 were shut off. The wafer loading platform door in the reaction chamber was opened, and the high aspect ratio device was removed. An Al2O3 (alumina) thin film was deposited on this high aspect ratio device. Figure 6 shows the chamber pressure curve of the reaction chamber in this embodiment, where t1 is the first time, t2 is the second time, t3 is the purge time, t4 is the third time, t5 is the second time, and t6 is the purge time. SEM and EDS energy dispersive spectroscopy analyses were performed on the high aspect ratio device, as shown in Figures 7 and 8.

[0161] Example 2

[0162] In this embodiment, the first reaction precursor is TMA and the second reaction precursor is H2O. The system device connection used in this embodiment is shown in Figure 4. In this embodiment, the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped out of the reaction chamber change in opposite periodicity.

[0163] (1) Open the door of the wafer loading platform in the reaction chamber and place the high aspect ratio structure device. During this process, the vacuum pump, vacuum angle valve V1, booster valve V2, source valve V3, source valve V4 and carrier gas valve V5 are closed, and the opening degree of APC butterfly valve V6 and APC butterfly valve V7 is 0%. When the carrier gas valve V5 is closed, the carrier gas in the carrier gas pipeline pushes against the carrier gas valve V5. When the booster valve V2 is closed, the booster gas in the booster gas pipeline pushes against the booster valve V2.

[0164] After placing the high aspect ratio structural components, close the door of the wafer loading platform inside the reaction chamber. Simultaneously, open the vacuum pump, vacuum angle valve V1, pressure boosting valve V2, and carrier gas valve V5. The vacuum pump speed is 600 m / s. 3 The carrier gas flow rate is 40 sccm / h, and the booster gas flow rate is 1000 sccm. The reaction chamber is evacuated to a low vacuum state, and the pressure value of the reaction chamber is 1 torr. At this time, source valves V3 and V4 are closed, the opening degree of APC butterfly valve V6 is 80% (preset opening degree), and the opening degree of APC butterfly valve V7 is 0%.

[0165] The vacuum pump, vacuum angle valve V1, pressure boosting valve V2, and carrier gas valve V5 are opened during vacuuming and closed after the coating of the high aspect ratio structure device surface is completed.

[0166] (2) When the reaction chamber reaches a low vacuum state, source valve V3 opens, introducing the first reaction precursor. When the first reaction precursor has been introduced for a first time, source valve V3 closes, stopping the introduction of the first reaction precursor. The first time is 0.2s, and the introduced mass is 1.5mg. During this process, source valve V4 is closed, the opening degree of APC butterfly valve V6 is 80% (preset opening degree), and the opening degree of APC butterfly valve V7 is 0%.

[0167] (3) When the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped into the reaction chamber change in opposite periods, the openings of APC butterfly valve V6 and APC butterfly valve V7 also change in opposite periods. The opening of APC butterfly valve V6 decreases from 80% (preset opening) to 0%, then increases from 0% to 80% (preset opening), while the opening of APC butterfly valve V7 increases from 0% to 80% (preset opening), then decreases from 80% (preset opening) to 0%. When the time of the opposite periodic change reaches the second time, the openings of APC butterfly valve V6 and APC butterfly valve V7 stop changing in opposite periods. The opening of APC butterfly valve V6 is maintained at 80% (preset opening), and the opening of APC butterfly valve V7 is maintained at 0%. At the same time, the reaction chamber is pumped back to a low vacuum state. During this process, source valves V3 and V4 are closed. The second time is 5 seconds.

[0168] When the reaction chamber is evacuated to a low vacuum state, source valves V3 and V4 are closed, APC butterfly valve V6 is opened to 80% (preset opening), and APC butterfly valve V7 is opened to 0%. After the reaction chamber reaches a low vacuum state, it is also purged with inert gas for 8 seconds.

[0169] (4) After purging, source valve V4 opens to introduce the second reaction precursor. When the second reaction precursor has been introduced for a third time period (0.2 s), source valve V4 closes to stop the introduction of the second reaction precursor. The introduced precursor mass is 1.5 mg. During this process, source valve V3 is closed, APC butterfly valve V6 is open at 80% (preset opening), and APC butterfly valve V7 is open at 0%.

[0170] (5) When the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped into the reaction chamber change in opposite periods, the openings of APC butterfly valves V6 and V7 also change in opposite periods. The opening of APC butterfly valve V6 decreases from 80% (preset opening) to 0%, then increases from 0% to 80% (preset opening), while the opening of APC butterfly valve V7 increases from 0% to 80% (preset opening), then decreases from 80% (preset opening) to 0%. When the time of this reverse periodic change reaches the second time interval, the reverse periodic changes of APC butterfly valves V6 and V7 cease. The opening of APC butterfly valve V6 is maintained at 80% (preset opening), and the opening of APC butterfly valve V7 is maintained at 0%. Simultaneously, the reaction chamber is pumped back to a low vacuum state. During this process, source valves V3 and V4 are closed. The second time interval is 5 seconds. After the reaction chamber reaches a low vacuum state, it is purged with inert gas for 8 seconds.

[0171] Steps (2) to (5) constitute one deposition cycle.

[0172] After 150 deposition cycles, the vacuum pump, vacuum valve V1, booster valve V2, source valves V3 and V4, and carrier gas valve V5 were shut off. The openings of APC butterfly valves V6 and V7 were set to 0%. The wafer loading platform door in the reaction chamber was opened, and the high aspect ratio structure device was removed. An Al2O3 (alumina) thin film was deposited on this high aspect ratio structure device. Figure 9 shows the chamber pressure curve of the reaction chamber in this embodiment, where t1 is the first time, t2 is the second time, t3 is the purge time, t4 is the third time, t5 is the second time, and t6 is the purge time. SEM and EDS energy dispersive spectroscopy analyses were performed on the high aspect ratio structure device, as shown in Figures 10 and 11.

[0173] Comparative Example 1

[0174] In this embodiment, the first reaction precursor is TMA, the second reaction precursor is H2O, and the apparatus used in this embodiment is shown in Figure 1.

[0175] (1) Open the door of the wafer loading platform inside the reaction chamber and place the high aspect ratio structure device. During this process, the vacuum pump, vacuum angle valve V1, carrier gas valve V5, source valve V3, and source valve V4 are closed. After placing the high aspect ratio structure device, close the door of the wafer loading platform inside the reaction chamber and simultaneously turn on the vacuum pump to evacuate the reaction chamber. At the same time, open the vacuum pump, vacuum angle valve V1, and carrier gas valve V5, and close source valves V3 and V4. The pumping speed of the vacuum pump is 600 m / s. 3 / h, the carrier gas flow rate is 40sccm, the reaction chamber is evacuated to a low vacuum state, and the pressure value of the reaction chamber is 1torr.

[0176] (2) When the reaction chamber reaches a low vacuum state, source valve V3 opens and the first reaction precursor is introduced. When the introduction time of the first reaction precursor reaches the first time interval, source valve V3 closes and the introduction of the first reaction precursor stops. The first time interval is 0.2s, and the mass of the first source bottle is 1.5mg. During this process, source valve V4 is closed, vacuum angle valve V1 is open, carrier gas valve V5 is open, and vacuum pump is turned on.

[0177] When the reaction chamber is evacuated to a low vacuum state, carrier gas valve V5, vacuum pump, and vacuum angle valve V1 are opened, while source valves V3 and V4 are closed. Once the reaction chamber reaches a low vacuum state, it is also purged with inert gas for 8 seconds.

[0178] (3) After purging, source valve V4 is opened to introduce the second reaction precursor. When the second reaction precursor is introduced for a third time period, source valve V4 is closed to stop the introduction of the second reaction precursor. The third time period is 0.2s, and the mass of the second source bottle is 1.5mg. During this process, source valve V3 is closed, vacuum pump is turned on, vacuum angle valve V1 is opened, and carrier gas valve V5 is opened.

[0179] When the reaction chamber is evacuated to a low vacuum state, source valves V3 and V4 remain closed, while the vacuum pump, vacuum angle valve V1, and carrier gas valve V5 remain open. After the reaction chamber reaches a low vacuum state, it is also purged with inert gas for 8 seconds.

[0180] Steps (2) to (3) constitute one deposition cycle.

[0181] After 150 deposition cycles, the vacuum pump, vacuum valve V1, source valve V3, source valve V4, and carrier gas valve V5 were shut off. The wafer loading platform door in the reaction chamber was opened, and the high aspect ratio device was removed. An Al2O3 (alumina) thin film was deposited on this high aspect ratio device. Figure 12 shows the chamber pressure curve of the reaction chamber in this embodiment, where t1 is the first time, t2 is the purge time, t3 is the third time, and t4 is the purge time. SEM and EDS energy dispersive spectroscopy analysis of the device are shown in Figures 13 and 14.

[0182] Referring to Figures 6 to 14, Comparative Example 1 uses a traditional atomic layer deposition (ALD) method to deposit the deep-hole structure of a high aspect ratio device. Figures 13 and 14 show that as the depth increases, Al elements are no longer detectable, indicating that Al₂O₃ fails to completely fill the deep-hole structure. Example 1 achieves the deposition of the deep-hole structure of a high aspect ratio device by adjusting the opening and closing of vacuum valve V1 and pressure valve V2. Figures 7 and 8 show that although Al elements still fail to completely fill the deep-hole structure, it is a significant improvement compared to Comparative Example 1. Example 2 achieves the deposition of the deep-hole structure of a high aspect ratio device by adjusting the opening of APC butterfly valves V6 and V7. Figures 10 and 11 show that Al elements have completely filled the deep-hole structure of the high aspect ratio device, and the density is good.

[0183] In both Examples 1 and 2, the reaction parameters are the same. The difference is that Example 2, based on Example 1, adds APC butterfly valves V6 and V7. The openings of APC butterfly valves V6 and V7 change in opposite directions periodically, which allows the reaction precursor to effectively enter the deep holes of the high aspect ratio structure device. At the same time, it effectively avoids the drawback of insufficient diffusion of the reaction precursor in the structure of the high aspect ratio structure device, and improves the phenomenon that the reaction precursor cannot be fully deposited in the deep holes or channels of the high aspect ratio structure device.

[0184] Example 3

[0185] In this embodiment, the first reaction precursor is Cu(acac)2 (copper acetylacetone), and the second reaction precursor is H2. The system device connection used in this embodiment is shown in Figure 3. In this embodiment, the flow rate of the pressurized gas is constant.

[0186] (1) Open the door of the wafer loading platform in the reaction chamber and place the high aspect ratio structure device. During this process, the vacuum pump, vacuum angle valve V1, pressure boosting valve V2, source valve V3, source valve V4 and carrier gas valve V5 are closed. When the carrier gas valve V5 is closed, the carrier gas in the carrier gas pipeline pushes against the carrier gas valve V5. When the pressure boosting valve V2 is closed, the pressure boosting gas in the pressure boosting gas pipeline pushes against the pressure boosting valve V2.

[0187] After placing the high aspect ratio structural components, close the door of the wafer loading platform inside the reaction chamber. Simultaneously, start the vacuum pump to evacuate the reaction chamber, and open the carrier gas valve V5, vacuum pump, and vacuum angle valve V1. Close the booster valve V2, and close the source valves V3 and V4. The vacuum pump's pumping speed is 600 m / s. 3 The carrier gas flow rate is 40 sccm / h, and the reaction chamber is evacuated to a low vacuum state with a pressure of 1 torr. The carrier gas valve V5 and the vacuum pump are opened during the evacuation operation and closed after the coating of the high aspect ratio structure device surface is completed.

[0188] (2) When the reaction chamber reaches a low vacuum state, source valve V3 opens and the first reaction precursor is introduced. When the introduction time of the first reaction precursor reaches the first time interval, source valve V3 closes and the introduction of the first reaction precursor stops. The first time interval is 5 seconds, and the mass of the first source bottle is 2 mg. During this process, pressure boosting valve V2 is closed, source valve V4 is closed, vacuum angle valve V1 is open, carrier gas valve V5 is open, and vacuum pump is turned on.

[0189] (3) During the pressurized diffusion process, when a constant flow of pressurized gas is introduced into the reaction chamber while the vacuum in the reaction chamber is simultaneously stopped, the pressurization valve V2 is opened and the vacuum angle valve V1 is closed, and the pressurized gas is introduced. When the time for the pressurized gas to be introduced or the time for stopping the vacuum in the reaction chamber reaches the second time, the pressurized gas is stopped, the pressurization valve V2 is closed, and the vacuum angle valve V1 is opened to evacuate the reaction chamber to a low vacuum state; wherein, the second time is 5s, and the flow rate of the pressurized gas is 1000sccm. During this process, the source valves V3 and V4 remain closed, and the carrier gas valve V5 remains open.

[0190] When the reaction chamber is evacuated to a low vacuum state, the carrier gas valve V5, vacuum pump, and vacuum angle valve V1 are opened. At this time, the booster valve V2 is closed, and the source valves V3 and V4 are closed. After the reaction chamber reaches a low vacuum state, it is also purged with inert gas for 8 seconds.

[0191] (4) After purging, source valve V4 is opened to introduce the second reaction precursor. When the second reaction precursor has been introduced for a third time period, source valve V4 is closed to stop the introduction of the second reaction precursor. The third time period is 10 seconds, and the source flow rate of the second source bottle is 4.7 L. During this process, pressure boosting valve V2 is closed, source valve V3 is closed, vacuum pump is turned on, vacuum angle valve V1 is opened, and carrier gas valve V5 is opened.

[0192] (5) During the pressurized diffusion process, when a constant flow of pressurized gas is introduced into the reaction chamber while the vacuum in the reaction chamber is simultaneously stopped, the pressurization valve V2 is opened and the vacuum angle valve V1 is closed, and the pressurized gas is introduced. When the time for the pressurized gas to be introduced or the time for stopping the vacuum in the reaction chamber reaches a second time, the pressurized gas is stopped, the pressurization valve V2 is closed, and the vacuum angle valve V1 is opened to evacuate the reaction chamber to a low vacuum state; wherein, the second time is 5s, and the flow rate of the pressurized gas is 1000sccm. During this process, the source valves V3 and V4 remain closed, and the carrier gas valve V5 remains open.

[0193] When the reaction chamber is evacuated to a low vacuum state, the booster valve V2, source valve V3, and source valve V4 remain closed, while the vacuum pump, vacuum angle valve V1, and carrier gas valve V5 remain open. Once the reaction chamber reaches a low vacuum state, it is also purged with inert gas for 8 seconds.

[0194] Steps (2) to (5) constitute one deposition cycle.

[0195] After 150 deposition cycles, the vacuum pump, vacuum valve V1, pressure booster valve V2, source valves V3 and V4, and carrier gas valve V5 were shut off. The wafer loading platform door in the reaction chamber was opened to remove the high aspect ratio structure device, which has a Cu thin film deposited on it. Figure 15 shows the chamber pressure curve of the reaction chamber in this embodiment, where t1 is the first time, t2 is the second time, t3 is the purge time, t4 is the third time, t5 is the second time, and t6 is the purge time. SEM and EDS energy dispersive spectroscopy analyses were performed on the high aspect ratio structure device, as shown in Figures 16 and 17.

[0196] Example 4

[0197] In this embodiment, the first reaction precursor is Cu(acac)2 (copper acetylacetone), and the second reaction precursor is H2. The system device connection used in this embodiment is shown in Figure 4. In this embodiment, the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped out of the reaction chamber change in opposite periodicity.

[0198] (1) Open the door of the wafer loading platform in the reaction chamber and place the high aspect ratio structure device. During this process, the vacuum pump, vacuum angle valve V1, booster valve V2, source valve V3, source valve V4 and carrier gas valve V5 are closed, and the opening degree of APC butterfly valve V6 and APC butterfly valve V7 is 0%. When the carrier gas valve V5 is closed, the carrier gas in the carrier gas pipeline pushes against the carrier gas valve V5. When the booster valve V2 is closed, the booster gas in the booster gas pipeline pushes against the booster valve V2.

[0199] After placing the high aspect ratio structural components, close the door of the wafer loading platform inside the reaction chamber. Simultaneously, open the vacuum pump, vacuum angle valve V1, pressure boosting valve V2, and carrier gas valve V5. The vacuum pump speed is 600 m / s. 3 The carrier gas flow rate is 40 sccm / h, and the booster gas flow rate is 1000 sccm. The reaction chamber is evacuated to a low vacuum state, and the pressure value of the reaction chamber is 1 torr. At this time, source valves V3 and V4 are closed, the opening degree of APC butterfly valve V6 is 80% (preset opening degree), and the opening degree of APC butterfly valve V7 is 0%.

[0200] The vacuum pump, vacuum angle valve V1, pressure boosting valve V2, and carrier gas valve V5 are opened during vacuuming and closed after the coating of the high aspect ratio structure device surface is completed.

[0201] (2) When the reaction chamber reaches a low vacuum state, source valve V3 opens to introduce the first reaction precursor. When the introduction time of the first reaction precursor reaches the first time, source valve V3 closes to stop the introduction of the first reaction precursor. The first time is 5 seconds, and the introduced mass is 2 mg. During this process, source valve V4 is closed, the opening degree of APC butterfly valve V6 is 80% (preset opening degree), and the opening degree of APC butterfly valve V7 is 0%.

[0202] (3) When the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped into the reaction chamber change in opposite periods, the openings of APC butterfly valves V6 and V7 also change in opposite periods. The opening of APC butterfly valve V6 decreases from 80% (preset opening) to 0%, then increases from 0% to 80% (preset opening), while the opening of APC butterfly valve V7 increases from 0% to 80% (preset opening), then decreases from 80% (preset opening) to 0%. When the time of this reverse periodic change reaches the second time interval, the reverse periodic changes of APC butterfly valves V6 and V7 cease. The opening of APC butterfly valve V6 is maintained at 80% (preset opening), and the opening of APC butterfly valve V7 is maintained at 0%. Simultaneously, the reaction chamber is pumped back to a low vacuum state. During this process, source valves V3 and V4 are closed. The second time interval is 5 seconds.

[0203] When the reaction chamber is evacuated to a low vacuum state, source valves V3 and V4 are closed, APC butterfly valve V6 is opened to 80% (preset opening), and APC butterfly valve V7 is opened to 0%. After the reaction chamber reaches a low vacuum state, it is also purged with inert gas for 8 seconds.

[0204] (4) After purging, source valve V4 opens to introduce the second reaction precursor. When the second reaction precursor has been introduced for a third time period (10 seconds), source valve V4 closes to stop the introduction of the second reaction precursor. The feed rate is 4.7 L. During this process, source valve V3 is closed, APC butterfly valve V6 is opened at 80% (preset opening), and APC butterfly valve V7 is opened at 0%.

[0205] (5) When the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped into the reaction chamber change in opposite periods, the openings of APC butterfly valves V6 and V7 change in opposite periods. The opening of APC butterfly valve V6 decreases from 80% (preset opening) to 0%, then increases from 0% to 80% (preset opening), while the opening of APC butterfly valve V7 increases from 0% to 80% (preset opening), then decreases from 80% (preset opening) to 0%. When the time of the opposite periodic change reaches the second time, the openings of APC butterfly valves V6 and V7 stop changing in opposite periods. The opening of APC butterfly valve V6 is maintained at 80% (preset opening), and the opening of APC butterfly valve V7 is maintained at 0%. At the same time, the reaction chamber is pumped back to a low vacuum state. During this process, source valves V3 and V4 are closed. The second time is 5 seconds. After the reaction chamber reaches a low vacuum state, it is purged with inert gas for 8 seconds.

[0206] Steps (2) to (5) constitute one deposition cycle.

[0207] After 150 deposition cycles, the vacuum pump, vacuum valve V1, booster valve V2, source valves V3 and V4, and carrier gas valve V5 were shut off. The openings of APC butterfly valves V6 and V7 were set to 0%. The wafer loading platform door in the reaction chamber was opened to retrieve the high aspect ratio structure device, which had a Cu thin film deposited on it. Figure 18 shows the chamber pressure curve of this embodiment, where t1 is the first time, t2 is the second time, t3 is the purge time, t4 is the third time, t5 is the second time, and t6 is the purge time. SEM and EDS energy dispersive spectroscopy analyses were performed on the high aspect ratio structure device, as shown in Figures 19 and 20.

[0208] Comparative Example 2

[0209] In this embodiment, the first reaction precursor is Cu(acac)2 (copper acetylacetone), and the second reaction precursor is H2 (corresponding to source valve V4). The apparatus used in this embodiment is shown in Figure 1.

[0210] (1) Open the door of the wafer loading platform inside the reaction chamber and place the high aspect ratio structure device. During this process, the vacuum pump, vacuum angle valve V1, carrier gas valve V5, source valve V3, and source valve V4 are closed. After placing the high aspect ratio structure device, close the door of the wafer loading platform inside the reaction chamber and simultaneously turn on the vacuum pump to evacuate the reaction chamber. At the same time, open the vacuum pump, vacuum angle valve V1, and carrier gas valve V5, and close source valves V3 and V4. The pumping speed of the vacuum pump is 600 m / s. 3 / h, the carrier gas flow rate is 40sccm, the reaction chamber is evacuated to a low vacuum state, and the pressure value of the reaction chamber is 1torr.

[0211] (2) When the reaction chamber reaches a low vacuum state, source valve V3 opens and the first reaction precursor is introduced. When the introduction time of the first reaction precursor reaches the first time interval, source valve V3 closes and the introduction of the first reaction precursor stops. The first time interval is 5 seconds, and the mass of the first source bottle is 2 mg. During this process, source valve V4 closes, vacuum angle valve V1 opens, carrier gas valve V5 opens, and vacuum pump is turned on.

[0212] When the reaction chamber is evacuated to a low vacuum state, carrier gas valve V5, vacuum pump, and vacuum angle valve V1 are opened, while source valves V3 and V4 are closed. After the reaction chamber reaches a low vacuum state, it is also purged with inert gas for 8 seconds.

[0213] (3) After purging, source valve V4 is opened to introduce the second reaction precursor. When the second reaction precursor is introduced for a third time period, source valve V4 is closed to stop the introduction of the second reaction precursor. The third time period is 10 seconds, and the source flow rate of the second source bottle is 4.7 L. During this process, source valve V3 is closed, vacuum pump is turned on, vacuum angle valve V1 is opened, and carrier gas valve V5 is opened.

[0214] When the reaction chamber is evacuated to a low vacuum state, source valves V3 and V4 remain closed, while the vacuum pump, vacuum angle valve V1, and carrier gas valve V5 remain open. After the reaction chamber reaches a low vacuum state, it is also purged with inert gas for 8 seconds.

[0215] Steps (2) to (3) constitute one deposition cycle.

[0216] After 150 deposition cycles, the vacuum pump, vacuum valve V1, source valves V3 and V4, and carrier gas valve V5 were shut off. The wafer loading platform door in the reaction chamber was opened, and the high aspect ratio structure device, on which a Cu thin film was deposited, was removed. Figure 21 shows the chamber pressure curve of the reaction chamber in this embodiment, where t1 is the first time, t2 is the purge time, t3 is the third time, and t4 is the purge time. SEM and EDS energy dispersive spectroscopy analyses were performed on the high aspect ratio structure device, as shown in Figures 22 and 23.

[0217] Referring to Figures 15 to 23, in Comparative Example 2, a traditional atomic layer deposition (ALD) method was used to deposit the deep-hole structure of a high aspect ratio device. Figures 22 and 23 show that, with increasing depth, Cu elements failed to completely fill the deep-hole structure. In Example 3, the deposition of the deep-hole structure of the high aspect ratio device was achieved by adjusting the opening and closing of vacuum valve V1 and pressure valve V2. Figures 16 and 17 show that although Cu elements filled the deep-hole structure, the density was poor. In Example 4, the deposition of the deep-hole structure of the high aspect ratio device was achieved by adjusting the opening of APC butterfly valves V6 and V7. Figures 19 and 20 show that Cu elements completely filled the deep-hole structure, and the density was good.

[0218] Among them, the different opening degrees of APC butterfly valve V6 and APC butterfly valve V7 have different filling effects on high aspect ratio structures. Taking Example 2 as an example, the influence of adjusting the opening degree of APC butterfly valve V6 and APC butterfly valve V7 on the percentage of Al element inside the high aspect ratio structure device was tested. In Figure 24, the horizontal axis represents the preset opening degree of APC butterfly valve, and the vertical axis represents the percentage of Al element (%). It can be seen from Figure 24 that when the preset opening degree is 80%, the structural filling effect is the best, and the percentage of Al atoms in the deep hole structure of the high aspect ratio structure device is greater than 90%.

[0219] Taking Example 4 as an example, the effect of adjusting the opening degree of the butterfly valve on the percentage of Cu elements inside the high aspect ratio structure device was tested. In Figure 25, the horizontal axis represents the preset opening degree of the APC butterfly valve, and the vertical axis represents the percentage of Cu elements (%). It can be seen from Figure 25 that when the preset opening degree is 80%, the structure filling effect is the best, and the percentage of Cu atoms in the deep hole structure of the high aspect ratio structure device is greater than 85%.

[0220] Compared to conventional atomic layer deposition processes, the atomic layer deposition coating method for high aspect ratio structural devices provided in this application controls the opening of APC butterfly valves V6 and V7, and adjusts the opening of APC butterfly valves V6 and V7 to increase and decrease the pressure in the reaction chamber. By simultaneously adjusting the opening of APC butterfly valves V6 and V7, the reaction precursor can effectively enter the deep holes of the high aspect ratio structural devices. In this way, effective coating of the reaction precursor in deep holes or channels of high aspect ratio structural devices can be achieved.

[0221] As can be seen from the above embodiments, this application provides an atomic layer deposition method and system for high aspect ratio structural devices. The method includes placing the high aspect ratio structural device in a reaction chamber and evacuating the reaction chamber to a low vacuum state; introducing a first reaction precursor into the reaction chamber and stopping the introduction of the first reaction precursor when the introduction time reaches a first time; performing a pressure diffusion treatment on the reaction chamber and stopping the pressure diffusion treatment and evacuating the reaction chamber back to a low vacuum state when the pressure diffusion treatment time reaches a second time; introducing a second reaction precursor into the reaction chamber and stopping the introduction of the second reaction precursor when the introduction time reaches a third time; performing a pressure diffusion treatment on the reaction chamber and stopping the pressure diffusion treatment and evacuating the reaction chamber back to a low vacuum state when the pressure diffusion treatment time reaches a second time, thereby completing the deposition on the surface of the high aspect ratio structural device. This application controls the reaction chamber by coordinating the first and second valves, or by making reverse periodic changes in the opening of the first and second butterfly valves, so as to increase and decrease the pressure in the reaction chamber, thereby enabling the reaction precursor to quickly or effectively enter the deep holes / channels of the high aspect ratio structure device and be adsorbed into the high aspect ratio structure device.

[0222] Similar parts between the embodiments provided in this application can be referred to mutually. The specific implementation methods provided above are only a few examples under the overall concept of this application and do not constitute a limitation on the scope of protection of this application. For those skilled in the art, any other implementation methods extended from the solution of this application without creative effort shall fall within the scope of protection of this application.

Claims

1. An atomic layer deposition method for high aspect ratio devices, wherein, The atomic layer deposition method for high aspect ratio structure devices includes: A high aspect ratio structure device is placed inside the reaction chamber, and the reaction chamber is evacuated to a low vacuum state; A first reaction precursor is introduced into the reaction chamber, and the introduction of the first reaction precursor is stopped when the introduction time of the first reaction precursor reaches a first time. The reaction chamber is subjected to pressurized diffusion treatment. When the pressurized diffusion treatment time reaches the second time, the pressurized diffusion treatment is stopped and the reaction chamber is pumped back to a low vacuum state. A second reaction precursor is introduced into the reaction chamber, and the introduction of the second reaction precursor is stopped when the introduction time of the second reaction precursor reaches a third time. The reaction chamber is subjected to a pressurized diffusion process. When the pressurized diffusion process reaches a second time, the pressurized diffusion process is stopped and the reaction chamber is pumped back to a low vacuum state to complete the coating on the surface of the high aspect ratio structure device.

2. The atomic layer deposition method for high aspect ratio structure devices according to claim 1, wherein, Performing pressurized diffusion treatment on the reaction chamber, stopping the pressurized diffusion treatment when the time of the pressurized diffusion treatment reaches a second time, and pumping the reaction chamber back to a low vacuum state includes: A constant flow rate of pressurized gas is introduced into the reaction chamber while the vacuuming of the reaction chamber is stopped. When the time for introducing the pressurized gas or the time for stopping the vacuuming of the reaction chamber reaches a second time, the introduction of the pressurized gas is stopped and the vacuuming of the reaction chamber continues until the reaction chamber is returned to a low vacuum state. or, The amount of pressurized gas introduced into the reaction chamber is made to change in an anti-periodic manner with the amount of gas pumped out of the reaction chamber. When the time of the anti-periodic change reaches a second time, the anti-periodic change is stopped and the reaction chamber is pumped back to a low vacuum state.

3. The atomic layer deposition method for high aspect ratio structure devices according to claim 2, wherein, The reaction chamber is connected to a vacuum pump and a pressurized gas pipeline. A first valve is provided on the pipeline connecting the reaction chamber and the vacuum pump, and a second valve is provided on the pressurized gas pipeline connected to the reaction chamber. When a constant flow of pressurized gas is introduced into the reaction chamber and the vacuuming of the reaction chamber is stopped, the first valve is closed and the second valve is opened. When the time for introducing pressurized gas or the time for stopping the vacuuming of the reaction chamber reaches a second time, the first valve is opened and the second valve is closed, and the vacuum pump continues to evacuate the reaction chamber until the reaction chamber reaches a low vacuum state.

4. The atomic layer deposition method for high aspect ratio structure devices according to claim 2, wherein, The reaction chamber is connected to a vacuum pump and a pressurized gas pipeline. A first valve and a first butterfly valve are provided on the pipeline connecting the reaction chamber and the vacuum pump. The first butterfly valve is located between the first valve and the reaction chamber. A second valve and a second butterfly valve are provided on the pressurized gas pipeline connected to the reaction chamber. The second butterfly valve is located between the second valve and the reaction chamber. When the amount of pressurized gas introduced into the reaction chamber changes in an anti-periodic manner with the amount of gas pumped into the reaction chamber, the first valve and the second valve open. The opening degree of the first butterfly valve changes in an anti-periodic manner with the opening degree of the second butterfly valve. When the time of the anti-periodic change reaches a second time, the first valve and the second valve open, and the anti-periodic change in the opening degree of the first butterfly valve and the second butterfly valve stops.

5. The atomic layer deposition method for high aspect ratio structure devices according to claim 4, wherein, The opening degree of the first butterfly valve and the opening degree of the second butterfly valve change in opposite directions periodically, including: The opening degree of the first butterfly valve decreases from a preset opening degree to 0%, and then increases from 0% to the preset opening degree; the opening degree of the second butterfly valve increases from 0% to the preset opening degree, and then decreases from the preset opening degree to 0%.

6. The atomic layer deposition method for high aspect ratio structure devices according to claim 5, wherein, During the pressurization and diffusion process in the reaction chamber, the opening of the first butterfly valve and the opening of the second butterfly valve change in a continuous and synchronous reverse periodic manner. When the opening of the first butterfly valve decreases from a preset opening to 0%, the opening of the second butterfly valve increases from 0% to the preset opening. When the opening of the first butterfly valve increases from 0% to the preset opening, the opening of the second butterfly valve decreases from the preset opening to 0%.

7. The atomic layer deposition method for high aspect ratio structure devices according to claim 6, wherein, When the time of the reverse periodic change reaches the second time, the opening of the first butterfly valve remains at a preset opening, the opening of the second butterfly valve remains at 0%, and the vacuum pump draws the reaction chamber back to a low vacuum state.

8. The atomic layer deposition method for high aspect ratio structure devices according to claim 3, wherein, The reaction chamber is also connected to a carrier gas pipeline, which is equipped with a fifth valve. The carrier gas pipeline is connected to a first source bottle and a second source bottle. The first source bottle stores a first reaction precursor, and the second source bottle stores a second reaction precursor. A third valve is installed on the connection pipeline between the first source bottle and the carrier gas pipeline, and a fourth valve is installed on the connection pipeline between the second source bottle and the carrier gas pipeline. When a high aspect ratio structure device is placed in the reaction chamber, the vacuum pump, the first valve, the second valve, the third valve, the fourth valve, and the fifth valve are closed. When the reaction chamber is evacuated to a low vacuum state, the second valve, the third valve, and the fourth valve are closed, and the vacuum pump, the first valve, and the fifth valve are opened. When the first reaction precursor is introduced into the reaction chamber, the vacuum pump, the first valve, the third valve, and the fifth valve are opened, and the second valve and the fourth valve are closed. When the introduction time of the first reaction precursor reaches a first time, the vacuum pump, the first valve, and the fifth valve are opened, and the second valve, the third valve, and the fourth valve are closed. When the second reaction precursor is introduced into the reaction chamber, the vacuum pump, the first valve, the fourth valve, and the fifth valve are opened, and the second valve and the third valve are closed. When the introduction time of the second reaction precursor reaches a third time, the vacuum pump, the first valve, and the fifth valve are opened, and the second valve, the third valve, and the fourth valve are closed.

9. The atomic layer deposition method for high aspect ratio structure devices according to claim 4, wherein, The reaction chamber is also connected to a carrier gas pipeline, which is equipped with a fifth valve. The carrier gas pipeline is connected to a first source bottle and a second source bottle. The first source bottle stores a first reaction precursor, and the second source bottle stores a second reaction precursor. A third valve is installed on the connection pipeline between the first source bottle and the carrier gas pipeline, and a fourth valve is installed on the connection pipeline between the second source bottle and the carrier gas pipeline. When a high aspect ratio structure device is placed in the reaction chamber, the vacuum pump, the first valve, the second valve, the third valve, the fourth valve, and the fifth valve are closed, and the opening of the first butterfly valve and the second butterfly valve is 0%. When the reaction chamber is evacuated to a low vacuum state, the third valve and the fourth valve are closed, and the vacuum pump, the first valve, the second valve, and the fifth valve are opened. The opening of the first butterfly valve is adjusted to a preset opening, and the opening of the second butterfly valve is 0%. When the first reaction precursor is introduced into the reaction chamber, the vacuum pump, the first valve, and the fifth valve are closed. The second, third, and fifth valves are open, the fourth valve is closed, the first butterfly valve is at a preset opening degree, and the second butterfly valve is at 0%. When the introduction time of the first reaction precursor reaches the first time, the vacuum pump, the first valve, the second valve, and the fifth valve are open, the third valve and the fourth valve are closed, the first butterfly valve is at the preset opening degree, and the second butterfly valve is at 0%. When the second reaction precursor is introduced into the reaction chamber, the vacuum pump, the first valve, the second valve, the fourth valve, and the fifth valve are open, the third valve is closed, the first butterfly valve is at the preset opening degree, and the second butterfly valve is at 0%. When the introduction time of the second reaction precursor reaches the third time, the vacuum pump, the first valve, the second valve, and the fifth valve are open, the third valve and the fourth valve are closed, the first butterfly valve is at the preset opening degree, and the second butterfly valve is at 0%.

10. The atomic layer deposition method for high aspect ratio structure devices according to claim 8, wherein, Under low vacuum conditions, the pressure inside the reaction chamber is 1–2 torr, and the pumping speed of the vacuum pump is 500–800 m / s. 3 / h, the flow rate of the carrier gas before passing through the fifth valve is 40-60 sccm, the first time is 0.1-10s, the second time is 1-20s, the third time is 0.1-15s, and the flow rate of the pressurized gas before passing through the second valve is 800-1500 sccm.

11. The atomic layer deposition method for high aspect ratio structure devices according to claim 9, wherein, Under low vacuum conditions, the pressure inside the reaction chamber is 1–2 torr, and the pumping speed of the vacuum pump is 500–800 m / s. 3 / h, the flow rate of the carrier gas before passing through the fifth valve is 40-60 sccm, the first time is 0.1-10s, the second time is 1-20s, the third time is 0.1-15s, the flow rate of the pressurized gas before passing through the second valve is 800-1500 sccm, and the preset opening degree is 70-90%.

12. An atomic layer deposition system for high aspect ratio devices, wherein, Used to perform the atomic layer deposition coating method for high aspect ratio structure devices as described in claim 1; The atomic layer deposition coating system for high aspect ratio structure devices includes: The reaction chamber, the vacuum pump connected to the reaction chamber, the pressurized gas pipeline, and the carrier gas pipeline; A first valve is provided on the connecting pipeline between the reaction chamber and the vacuum pump, and a second valve is provided on the pressurizing gas pipeline connected to the reaction chamber; A fifth valve is provided on the carrier gas pipeline. The carrier gas pipeline is connected to a first source bottle and a second source bottle respectively. The first source bottle stores a first reaction precursor, and the second source bottle stores a second reaction precursor. A third valve is provided on the connection pipeline between the first source bottle and the carrier gas pipeline, and a fourth valve is provided on the connection pipeline between the second source bottle and the carrier gas pipeline.

13. The atomic layer deposition coating system for high aspect ratio structure devices according to claim 12, wherein, The atomic layer deposition coating system for high aspect ratio structure devices also includes: A first butterfly valve is provided on the connecting pipe between the reaction chamber and the vacuum pump, and the first butterfly valve is located between the first valve and the reaction chamber. A second butterfly valve is provided on the pressurized gas pipeline connected to the reaction chamber, and the second butterfly valve is located between the second valve and the reaction chamber; wherein the opening degree of the first butterfly valve and the second butterfly valve is controllable.

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