Atomic layer deposition coating method and system for high aspect ratio structural device

Abstract

The invention relates to the technical field of semiconductor manufacturing, and provides an atomic layer deposition coating method and system for a high aspect ratio structural device, the system comprises a reaction cavity, a vacuum pump connected with the reaction cavity, a pressurized gas pipeline and a carrier gas pipeline; a first valve is arranged on a connecting pipeline of the reaction cavity and the vacuum pump, and a second valve is arranged on a pressurizing gas pipeline connected with the reaction cavity; a fifth valve is arranged on the carrier gas pipeline, the carrier gas pipeline is respectively connected with a first source bottle and a second source bottle which store reaction precursors, a third valve is arranged on a connecting pipeline of the first source bottle and the carrier gas pipeline, and a fourth valve is arranged on a connecting pipeline of the second source bottle and the carrier gas pipeline. By adjusting the opening and closing of the first valve and the second valve, pressurized gas enters the reaction cavity, so that the pressure of the reaction cavity is increased and reduced, and a reaction precursor quickly enters a deep hole / channel of a high aspect ratio structural device and is effectively adsorbed in the high aspect ratio structural device.

Description

Technical Field

[0001] The present application relates to the field of semiconductor manufacturing technology, and in particular to an atomic layer deposition coating method and system for high aspect ratio structural devices. Background Art

[0002] Atomic layer deposition (ALD) is a high-precision thin film deposition technology based on chemical vapor deposition (CVD). It deposits material on the surface of the substrate layer by layer in the form of a single atomic film based on chemical vapor. Specifically, two or more reaction precursor reactants are introduced into the reaction chamber one at a time and adsorbed on the substrate surface. Each reaction precursor reaches saturation adsorption on the substrate surface. In the deposition process of ALD, the reaction precursors are deposited alternately, and the chemical reaction of a new layer of atomic film is directly related to the previous layer. Only one layer of atoms is deposited each time, and the ALD reaction is self-limiting.

[0003] During the atomic layer deposition process, when the reaction precursor reaches the surface of the deposition substrate, it will be 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 precursor that is not adsorbed on the substrate surface, ensuring that the chemical reaction only occurs on the substrate surface.

[0004] With the advancement of science and technology, miniaturization is the trend of the micro-electromechanical industry. Components with high aspect ratio structures are increasingly used, and the demand is also increasing. In the semiconductor field, high aspect ratio microstructures refer to microstructures with a depth and aspect ratio greater than 10 formed on silicon wafers or other substrates through processes such as photolithography combined with etching. Usually, such structures are presented in the form of deep holes or deep grooves. The related technology uses ALD to deposit thin films on the surface of a substrate with a high aspect ratio structure. The reaction precursor cannot effectively diffuse into the interior of the high aspect ratio structure, resulting in the inability to completely fill the material into structures such as deep holes and channels, which seriously affects the working efficiency of devices with high aspect ratio structures. Summary of the invention

[0005] The present application provides an atomic layer deposition coating method and system for high aspect ratio structure devices, so as to solve the problem that the reaction precursor cannot effectively diffuse into the interior of the high aspect ratio structure when the existing atomic layer deposition performs thin film deposition on the surface of the device with a high aspect ratio structure.

[0006] In a first aspect, the present application provides an atomic layer deposition coating method for a high aspect ratio structure device, the atomic layer deposition coating method comprising: Placing a high aspect ratio structure 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 of the first reaction precursor reaches a first time; Performing a pressurization diffusion treatment on the reaction chamber, stopping the pressurization diffusion treatment when the time of the pressurization diffusion treatment reaches a second time and pumping the reaction chamber back to a low vacuum state; Introducing a second reaction precursor into the reaction chamber, and stopping the introduction of the second reaction precursor when the introduction time of the second reaction precursor reaches a third time; The reaction chamber is subjected to a pressurized diffusion treatment, and when the time of the pressurized diffusion treatment reaches a second time, the pressurized diffusion treatment is stopped and the reaction chamber is pumped back to a low vacuum state, thereby completing the coating on the surface of the high aspect ratio structure device.

[0007] The reaction chamber in the present 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, so that the pressure of the reaction chamber increases and decreases rapidly, thereby allowing the reaction precursor to quickly enter the deep holes / channels of the high aspect ratio structure device and be effectively adsorbed in the high aspect ratio structure device.

[0008] In some possible implementations, performing a pressurization diffusion process on the reaction chamber, stopping the pressurization diffusion process when the time of the pressurization diffusion process reaches a second time and pumping the reaction chamber back to a low vacuum state includes: A pressurized gas with a constant flow rate is introduced into the reaction chamber and the reaction chamber is simultaneously stopped from being evacuated, and when the time for introducing the pressurized gas or the time for stopping evacuating the reaction chamber reaches a second time, the pressurized gas is stopped from being introduced and the reaction chamber is continuously evacuated until the reaction chamber is evacuated back to a low vacuum state; or, The amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped into the reaction chamber are changed in reverse periodicity, and when the time of the reverse periodicity change reaches a second time, the reverse periodicity change is stopped and the reaction chamber is pumped back to a low vacuum state.

[0009] In some possible implementations, the reaction chamber is respectively connected to a vacuum pump and a pressurized 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 pressurized gas pipeline connected to the reaction chamber; wherein, when a constant flow of pressurized gas is introduced into the reaction chamber and the vacuum pumping of the reaction chamber is stopped at the same time, the first valve is closed and the second valve is opened, and when the pressurized gas introduction time or the vacuum pumping of the reaction chamber is stopped reaches a second time, the first valve is opened and the second valve is closed, and the vacuum pump continues to pump the reaction chamber until the reaction chamber is evacuated to a low vacuum state.

[0010] In some possible implementations, the reaction chamber is respectively connected to a vacuum pump and a pressurized gas pipeline, and a first valve and a first butterfly valve are provided on the connecting pipeline between the reaction chamber and the vacuum pump, the first butterfly valve is located between the first valve and the reaction chamber, and 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; wherein, when the amount of pressurized gas introduced into the reaction chamber and the amount of gas extracted from the reaction chamber show reverse periodic changes, the first valve and the second valve are opened, and the opening of the first butterfly valve and the opening of the second butterfly valve show reverse periodic changes, and when the time of the reverse periodic change reaches a second time, the first valve and the second valve are opened, and the opening of the first butterfly valve and the opening of the second butterfly valve stop reverse periodic changes.

[0011] In some possible implementations, the opening of the first butterfly valve and the opening of the second butterfly valve periodically change in opposite directions, including: The opening degree of the first butterfly valve changes from a preset opening degree to 0%, and then increases from 0% to the preset opening degree, and the opening degree of the second butterfly valve changes from 0% to the preset opening degree, and then decreases from the preset opening degree to 0%.

[0012] In some possible implementations, when the reaction chamber is subjected to pressurized diffusion treatment, the opening of the first butterfly valve and the opening of the second butterfly valve show continuous and synchronous reverse periodic changes. 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%.

[0013] In some possible implementations, when the time of the reverse periodic change reaches a second time, the opening of the first butterfly valve is maintained at a preset opening, the opening of the second butterfly valve is maintained at 0%, and the vacuum pump draws the reaction chamber back to a low vacuum state.

[0014] The openings of the first butterfly valve and the second butterfly valve in the present application are controllable. By simultaneously adjusting the openings of the first butterfly valve and the second butterfly valve, the reaction precursor can effectively enter the deep hole of the high aspect ratio structural device, while effectively avoiding the disadvantage of insufficient diffusion of the reaction precursor in the structure of the high aspect ratio structural device, and improving the phenomenon that the reaction precursor cannot be fully deposited in the deep hole or channel structure of the high aspect ratio structural device.

[0015] In some possible implementations, the reaction chamber is also connected to a carrier gas pipeline, a fifth valve is provided on the carrier gas pipeline, the carrier gas pipeline is respectively connected to a first source bottle and a second source bottle, the first source bottle stores a first reaction precursor, 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; 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, the fifth valve, and the second valve are closed. The valve is 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 the 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 the 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.

[0016] In some possible implementations, the reaction chamber is also connected to a carrier gas pipeline, a fifth valve is provided on the carrier gas pipeline, the carrier gas pipeline is respectively connected to a first source bottle and a second source bottle, the first source bottle stores a first reaction precursor, 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; 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 opening of the second butterfly valve are 0%; when the reaction chamber is evacuated to a low vacuum state, the third valve and the fourth valve are closed, 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, 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% The first valve, the second valve, the third valve, and the fifth valve are opened, and the fourth valve is closed, the opening of the first butterfly valve is a preset opening, and the opening 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 valve, the second valve, and the fifth valve are opened, and the third valve and the fourth valve are closed, the opening of the first butterfly valve is a preset opening, and the opening of the second butterfly valve is 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 opened, and the third valve is closed, the opening of the first butterfly valve is a preset opening, and the opening 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 valve, the second valve, and the fifth valve are opened, and the third valve and the fourth valve are closed, the opening of the first butterfly valve is a preset opening, and the opening of the second butterfly valve is 0%.

[0017] In some possible implementations, the preset opening is 70-90%.

[0018] In some possible implementations, the pressure in 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 gas flow rate of the carrier gas before passing through the fifth valve is 40~60sccm, 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 boost gas before passing through the second valve is 800~1500sccm.

[0019] In some possible implementations, the pressurized gas or carrier gas is any one of nitrogen, argon, helium, and neon.

[0020] In a second aspect, the present 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; Wherein, the atomic layer deposition coating system comprises: A reaction chamber, a vacuum pump connected to the reaction chamber, a pressurized gas pipeline, and a 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 pressurized gas pipeline connected to the reaction chamber; The carrier gas pipeline is provided with a fifth valve, and the carrier gas pipeline is respectively connected to a first source bottle and a second source bottle, the first source bottle stores a first reaction precursor, 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 is respectively connected to the first source bottle and the second source bottle storing reaction precursors, the first source bottle stores a first reaction precursor, and the second source bottle stores a second reaction precursor.

[0021] In some possible implementations, a first butterfly valve is provided on a connecting pipeline 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 openings of the first butterfly valve and the second butterfly valve are controllable.

[0022] From the above content, it can be seen that the present application provides an atomic layer deposition coating method and system for high aspect ratio structural devices, the method comprising 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 of the first reaction precursor reaches a first time; performing a pressurization diffusion treatment on the reaction chamber, stopping the pressurization diffusion treatment when the pressurization diffusion treatment time reaches a second time and evacuating the reaction chamber back to a low vacuum state; introducing a second reaction precursor into the reaction chamber, and stopping the introduction of the second reaction precursor when the introduction time of the second reaction precursor reaches a third time; performing a pressurization diffusion treatment on the reaction chamber, stopping the pressurization diffusion treatment when the pressurization diffusion treatment time reaches a second time and evacuating the reaction chamber back to a low vacuum state, thereby completing the coating on the surface of the high aspect ratio structural device. The present application increases and decreases the pressure in the reaction chamber through the coordinated control of the first valve and the second valve, or the reverse periodic change of the opening of the first butterfly valve and the second butterfly valve, so that the reaction precursor quickly or effectively enters the deep hole / channel of the high aspect ratio structure device and is adsorbed in the high aspect ratio structure device. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to more clearly illustrate the technical solution of the present application, the drawings required for use in the embodiments are briefly introduced below. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.

[0024] Figure 1 Schematic diagram of a conventional atomic layer deposition coating system; Figure 2 A schematic diagram comparing the atomic layer deposition coating method provided in this application with the atomic layer deposition method in the related art; Figure 3 Schematic diagram of an atomic layer deposition coating system for a high aspect ratio structure device provided in an embodiment of the present application Figure 1 ; Figure 4 Schematic diagram of an atomic layer deposition coating system for a high aspect ratio structure device provided in an embodiment of the present application Figure 2 ; Figure 5 A flowchart of the atomic layer deposition coating method for high aspect ratio structure devices provided in this application; Figure 6 is a cavity pressure curve diagram of the reaction cavity in Example 1 of the present application; Figure 7 This is a SEM image of the deposited sample prepared in Example 1 of the present application; Figure 8 This is an EDS spectrum analysis diagram of the deposition sample prepared in Example 1 of the present application; Fig. 9 is a cavity pressure curve diagram of the reaction cavity in Example 2 of the present application; Fig.10 This is a SEM image of the deposited sample prepared in Example 2 of the present application; Fig.11 This is an EDS spectrum analysis diagram of the deposited sample prepared in Example 2 of the present application; Fig.12 This is a cavity pressure curve diagram of the reaction cavity in Comparative Example 1 of the present application; Fig.13 This is the SEM image of the deposited sample prepared in Comparative Example 1 of the present application; Fig.14 This is an EDS spectrum analysis diagram of the deposition sample prepared in Comparative Example 1 of the present application; Fig.15 is a cavity pressure curve diagram of the reaction chamber in Example 3 of the present application; Fig.16 This is a SEM image of the deposited sample prepared in Example 3 of the present application; Fig.17 This is an EDS spectrum analysis diagram of the deposition sample prepared in Example 3 of the present application; Fig.18 is a cavity pressure curve diagram of the reaction cavity in Example 4 of the present application; Fig.19 This is a SEM image of the deposited sample prepared in Example 4 of the present application; Fig. 20 This is an EDS spectrum analysis diagram of the deposition sample prepared in Example 4 of the present application; Fig.21 This is a cavity pressure curve diagram of the reaction cavity in Comparative Example 2 of the present application; Fig. 22 This is a SEM image of the deposited sample prepared in Comparative Example 2 of the present application; Fig.23 This is an EDS spectrum analysis diagram of the deposition sample prepared in Comparative Example 2 of the present application; Fig.24 A relationship diagram between the preset opening and the filling effect of the butterfly valve in Example 2 of the present application; Fig.25 This is a relationship diagram between the preset opening and filling effect of the butterfly valve in Example 4 of the present application. DETAILED DESCRIPTION

[0025] The following embodiments are described in detail, and examples thereof are shown in the accompanying drawings. When the following description refers to the drawings, unless otherwise indicated, the same numbers in different drawings represent the same or similar elements. The embodiments described in the following embodiments do not represent all embodiments consistent with the present application.

[0026] Atomic layer deposition (ALD) is a high-precision thin film deposition technology based on chemical vapor deposition (CVD). It deposits material on the surface of the substrate layer by layer in the form of a single atomic film based on chemical vapor. Specifically, two or more reaction precursors are introduced into the reaction chamber one at a time and adsorbed on the substrate surface. Each reaction precursor reaches saturation adsorption on the substrate surface. In the deposition process of ALD, the reaction precursors are deposited alternately, and the chemical reaction of a new layer of atomic film is directly related to the previous layer. Only one layer of atoms is deposited each time, and the ALD reaction is self-limiting.

[0027] During the atomic layer deposition process, when the reaction precursor reaches the surface of the deposition substrate, it will be 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 precursor that is not adsorbed on the substrate surface, ensuring that the chemical reaction only occurs on the substrate surface.

[0028] With the advancement of science and technology, miniaturization is the trend of the MEMS industry. Components with high aspect ratio structures are increasingly used and the demand is also increasing. In related technologies, ALD process is used to deposit high aspect ratio structures. The equipment used is as follows: Figure 1 As shown, it includes a vacuum pump, a reaction chamber, a first source bottle, a second source bottle and a carrier gas pipeline. The first source bottle stores a first reaction precursor, and the second source bottle stores a second reaction precursor. The specific process of the ALD process is that the first reaction precursor and the second reaction precursor alternately enter the reaction chamber in a "pulse + purge" manner, and the reaction ends after completing a set number of cycles.

[0029] However, when the above-mentioned ALD method is used to deposit thin films on the surface of a device with a high aspect ratio structure, the first reaction precursor and the second reaction precursor cannot quickly and effectively diffuse into the high aspect ratio structure device, resulting in insufficient deposition in structures such as deep holes or grooves.

[0030] Based on this, the present application provides an atomic layer deposition coating method and system for high aspect ratio structural devices. The atomic layer deposition coating method uses a combination mode of a boost diffusion process (Boost diffuse) and an inert gas purge process, and controls the first valve and the second valve in coordination, or the opening of the first butterfly valve and the second butterfly valve is changed in reverse periodicity to increase and decrease the pressure in the reaction chamber, thereby effectively avoiding the disadvantage of insufficient diffusion of reaction precursors on the surface of high aspect ratio structural devices, and improving the phenomenon of insufficient deposition in structures such as deep holes or grooves. Figure 2 The figure shows a schematic diagram comparing the atomic layer deposition coating method provided by the present application with the atomic layer deposition method in the related art. Figure 2Figure a is the natural diffusion process of the reaction precursor in traditional ALD. Figure 2 b is the pressurized diffusion process of the reaction precursor mentioned in this application. Among them, the inert gas purging process includes pumping the reaction chamber to a low vacuum state and purging operation; Figure 2 The purge in the process refers to the purge operation, and the pulse refers to the introduction of the first reaction precursor and / or the second reaction precursor.

[0031] like Figure 3 As shown, in some embodiments, the present application provides an atomic layer deposition coating system for a high aspect ratio structure device, and the atomic layer deposition coating system is used to implement an atomic layer deposition coating method for a high aspect ratio structure device. The atomic layer deposition coating system includes: A reaction chamber, a vacuum pump connected to the reaction chamber, a pressurized gas pipeline, and a carrier gas pipeline; 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 ability of the vacuum pump to evacuate the reaction chamber, and the second valve V2 is used to control whether to introduce pressurized gas into the reaction chamber. The first valve V1 and the second valve V2 can be used to control the cavity pressure of the reaction chamber.

[0032] A fifth valve V5 is provided on the carrier gas pipeline, and the carrier gas pipeline is respectively connected to the first source bottle and the second source bottle, the first source bottle stores the first reaction precursor, the second source bottle stores the second reaction precursor, the third valve V3 is provided on the connecting pipeline between the first source bottle and the carrier gas pipeline, and the fourth valve V4 is provided on the connecting pipeline between the second source bottle and the carrier gas pipeline. Among them, the third valve V3, the fourth valve V4 and the fifth valve V5 are respectively used to control whether the first reaction precursor is introduced, whether the second reaction precursor is introduced, and whether the carrier gas is introduced.

[0033] In this embodiment, by adjusting the opening and closing of the first valve V1 and the second valve V2, the pressurized gas enters the reaction chamber, so that the pressure of the reaction chamber increases and decreases rapidly, thereby allowing the reaction precursor to quickly enter the deep holes / channels of the high aspect ratio structure device and be effectively adsorbed in the high aspect ratio structure device.

[0034] like Figure 4 As shown, in some embodiments, the present application also provides an atomic layer deposition coating system for high aspect ratio structure devices, Figure 3On the basis of the disclosed structure, 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 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 increase and decrease within the second time, so that the pressure in the reaction chamber is in dynamic change. The first butterfly valve V6 is used to control the suction volume of the vacuum pump, and the second butterfly valve V7 is used to control the inlet flow of the pressurized gas. After the reaction is completed, the airflow in the vacuum pump is effectively prevented from flowing back into the reaction chamber by closing the first valve V1, and the pressurized gas can be effectively prevented from entering the reaction chamber by closing the second valve V2.

[0035] The openings of the first butterfly valve V6 and the second butterfly valve V7 in the present application are controllable. After the reaction precursor enters the reaction chamber, the openings of the first butterfly valve V6 and the second butterfly valve V7 are changed periodically in the opposite direction to increase and decrease the pressure in the reaction chamber, so that the reaction precursor can effectively enter the deep holes of the high aspect ratio structural device, and at the same time effectively avoid the disadvantage of insufficient diffusion of the reaction precursor in the structure of the high aspect ratio structural device, and improve the phenomenon that the reaction precursor cannot be fully deposited in structures such as deep holes or channels of the high aspect ratio structural device. Figure 4 The atomic layer deposition coating system provided by the embodiment shown in the figure is simultaneously Figure 3 The atomic layer deposition coating system shown in the figure increases or decreases the pressure in the reaction chamber more slowly than in the pressurized diffusion process, but is still faster than the prior art, that is, the pressure in the reaction chamber increases more slowly and decreases more slowly.

[0036] like Figure 5 As shown, in some embodiments, the present application also provides an atomic layer deposition coating method for a high aspect ratio structure device, the method comprising: Placing a high aspect ratio structure 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 of the first reaction precursor reaches a first time; Performing a pressurization diffusion treatment on the reaction chamber, stopping the pressurization diffusion treatment when the time of the pressurization diffusion treatment reaches a second time and pumping the reaction chamber back to a low vacuum state; Introducing a second reaction precursor into the reaction chamber, and stopping the introduction of the second reaction precursor when the introduction time of the second reaction precursor reaches a third time; The reaction chamber is subjected to a pressurized diffusion treatment, and when the pressurized diffusion treatment time reaches a second time, the pressurized diffusion treatment is stopped and the reaction chamber is pumped back to a low vacuum state, thereby completing the coating on the surface of the high aspect ratio structure device.

[0037] In the atomic layer deposition coating method, performing pressurization diffusion treatment on the reaction chamber, stopping the pressurization diffusion treatment when the time of the pressurization diffusion treatment reaches a second time and pumping the reaction chamber back to a low vacuum state includes: A pressurized gas with a constant flow rate is introduced into the reaction chamber and the reaction chamber is simultaneously stopped from being evacuated. When the time for introducing the pressurized gas or the time for stopping evacuating the reaction chamber reaches a second time, the pressurized gas is stopped from being introduced and the reaction chamber is continuously evacuated until the reaction chamber is evacuated back to a low vacuum state. or, The amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped into the reaction chamber are changed in reverse periodicity. When the time of the reverse periodicity change reaches a second time, the reverse periodicity change is stopped and the reaction chamber is pumped back to a low vacuum state.

[0038] Due to the different flow rates of the pressurized gas (constant or periodically changing), the atomic layer deposition coating control process is also different. The implementation method of the atomic layer deposition coating also corresponds to atomic layer deposition coating systems of different structures, which are introduced below.

[0039] In some embodiments, the present application provides an atomic layer deposition coating method for a high aspect ratio structure device. Figure 3 In the atomic layer deposition coating system for high aspect ratio structural devices, when the high aspect ratio structural device is placed in the reaction chamber, the reaction chamber door is opened, and the vacuum pump, the first valve V1, the second valve V2, the third valve V3, the fourth valve V4, and the 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 the second valve V2, the third valve V3, and the fourth valve V4 are closed, and the vacuum pump, the first valve V1, and the fifth valve V5 are opened to evacuate the reaction chamber; when the first reaction precursor is introduced into the reaction chamber, the vacuum pump, the first valve V1, the third valve V3, and the fifth valve V5 are opened , and the second valve V2 and the fourth valve V4 are closed at the same time; when the introduction time of the first reaction precursor reaches the first time, the vacuum pump, the first valve V1, and the fifth valve V5 are opened, and the second valve V2, the third valve V3, and the fourth valve V4 are closed; when the second reaction precursor is introduced into the reaction chamber, the vacuum pump, the first valve V1, the fourth valve V4, and the fifth valve V5 are opened, and the second valve V2 and the third valve V3 are closed at the same time; when the introduction time of the second reaction precursor reaches the third time, the vacuum pump, the first valve V1, and the fifth valve V5 are opened, and the second valve V2, the third valve V3, and the fourth valve V4 are closed at the same time.

[0040] In order to facilitate a clear understanding of the functions of each valve and to facilitate distinction, the first valve V1, the second valve V2, the third valve V3, the fourth valve V4 and the fifth valve V5 are referred to as vacuum angle valve V1, booster valve V2, source valve V3, source valve V4 and carrier valve V5 respectively in the following text.

[0041] The atomic layer deposition coating method provided in this embodiment includes: S1: Place a high aspect ratio structure device in a reaction chamber, and evacuate the reaction chamber to a low vacuum state. The structure of the high aspect ratio structure device is a high aspect ratio micro-nano structure. The pressure in the reaction chamber under the low vacuum state is 1-2 torr.

[0042] The step of placing a high aspect ratio structure device in a reaction chamber and evacuating the reaction chamber to a low vacuum state includes: Placing a high aspect ratio structure device in a reaction chamber, introducing a carrier gas into the reaction chamber, and starting a vacuum pump to evacuate the reaction chamber; When the pressure in the reaction chamber reaches the preset pressure value, the first reaction precursor is introduced into the reaction chamber. The preset pressure value is 1~2torr, and the pumping speed of the vacuum pump is 500~800 m 3 / h, the flow rate of carrier gas before passing through carrier gas valve V5 is consistent with the flow rate into the reaction chamber, both of which are 40~60sccm.

[0043] Specifically, the door of the wafer loading platform in the reaction chamber is opened, and the high aspect ratio structure device is 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. It should be noted that when the carrier gas valve V5 is closed, the carrier gas in the carrier gas pipeline is pushed toward the carrier gas valve V5, and when the booster valve V2 is closed, the booster gas in the booster gas pipeline is pushed toward the booster valve V2. After the high aspect ratio structure device is placed, the door of the wafer loading platform in the reaction chamber is closed, and the vacuum pump is turned on to evacuate the reaction chamber at the same time. The 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 3 / h, the flow rate of carrier gas is the same as described above, the reaction chamber is evacuated to a low vacuum state, and the pressure value of the reaction chamber is 1~2torr. During this process, the boost valve V2 is closed, and the source valve V3 and source valve V4 are closed.

[0044] The carrier gas valve V5 and the vacuum pump are opened during vacuuming and are closed after the coating on the surface of the high aspect ratio structure device is completed.

[0045] S2: introducing a first reaction precursor into the reaction chamber, and stopping the introduction of the first reaction precursor when the introduction time of the first reaction precursor reaches a first time.

[0046] Specifically, after the reaction chamber reaches a low vacuum state, the source valve V3 is opened, and the first reaction precursor is introduced. When the introduction time of the first reaction precursor reaches the first time, the source valve V3 is closed, and the introduction of the first reaction precursor is stopped. The first time is 0.1~10s, and the source mass of the first source bottle is determined according to the actual reaction precursor. In this process, the boost valve V2 is closed, the source valve V4 is closed, the vacuum angle valve V1 is opened, and the carrier gas valve V5 is opened. Exemplarily, when the first reaction precursor is TMA (trimethylaluminum), the amount of TMA source introduced is 1~2mg, and the first time is 0.1~2s; when the first reaction precursor is Cu(acac)2 (copper acetylacetonate), the amount of Cu(acac)2 source introduced is 1~3mg, and the first time is 3~6s.

[0047] S3: introducing a constant flow of pressurized gas into the reaction chamber and stopping evacuating the reaction chamber at the same time, and when the time for introducing the pressurized gas or the time for stopping evacuating the reaction chamber reaches a second time, the introduction of the pressurized gas is stopped and the evacuation of the reaction chamber is continued until the reaction chamber is pumped back to a low vacuum state. In some embodiments, after the reaction chamber is pumped to a low vacuum state, a purging operation is also included. The inert gas purging process includes pumping the reaction chamber to a low vacuum state and a purging operation. The purging operation lasts for 5 to 10 seconds.

[0048] Among them, when a constant flow of pressurized gas is introduced into the reaction chamber and the vacuum pumping of the reaction chamber is stopped at the same time, the operation of introducing the pressurized gas and the operation of stopping the vacuum pumping of the reaction chamber are carried out simultaneously, that is, while the pressurizing valve V2 is opened, the vacuum angle valve V1 is closed, and the time for introducing the pressurized gas and the time for stopping the vacuum pumping of the reaction chamber are the same, both being the second time.

[0049] By adjusting the opening and closing of the vacuum angle valve V1 and the boost valve V2, the boost gas is allowed to enter the reaction chamber, causing the pressure in the reaction chamber to increase and decrease rapidly, thereby allowing the reaction precursor to quickly enter the deep holes / channels of the high aspect ratio structural device and be effectively adsorbed in the high aspect ratio structural device.

[0050] In this embodiment, after each reaction precursor gas is introduced, a large amount of pressurized gas is introduced, and the vacuum pump is kept in a state of continuously evacuating the reaction chamber, so that the pressure of the reaction chamber increases and decreases rapidly, so that the reaction precursor is fully diffused in the reaction chamber, and this process is called pressurized diffusion treatment; each time the reaction precursor is introduced for deposition, a pressurized diffusion treatment is performed, that is, the atomic layer deposition coating method provided in the present application includes multiple pressurized diffusion treatments. Taking the deposition of two reaction precursors as an example, the atomic layer deposition coating method includes two pressurized diffusion treatments; wherein, the first pressurized diffusion treatment specifically includes: When performing the first pressurized diffusion treatment, the boost 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 pumping of the reaction chamber reaches the second time, the boost valve V2 is closed and the vacuum angle valve V1 is opened, wherein the second time is 1 to 20 seconds. During this process, the source valve V3 and the source valve V4 remain closed, and the carrier gas valve V5 remains open. When the boost valve V2 is opened, the maximum pressure in the reaction chamber can reach 1.5 to 2.0 torr.

[0051] After closing the boost valve V2, the reaction chamber is pumped back to a low vacuum state, wherein the flow rate of the boost gas before passing through the boost valve V2 is consistent with the flow rate into the reaction chamber, both of which are 800-1500 sccm. The inert gas purge process includes pumping the reaction chamber to a low vacuum state and a purge operation. The purge operation time is 5-10 seconds.

[0052] Exemplarily, the pressurized gas or carrier gas is any one of nitrogen, argon, helium, and neon.

[0053] S4: introducing a second reaction precursor into the reaction chamber, and when the introduction time of the second reaction precursor reaches a third time, stopping the introduction of the second reaction precursor.

[0054] Specifically, when the reaction chamber reaches a low vacuum state again, the source valve V4 is opened, and the second reaction precursor is introduced. When the second reaction precursor introduction time reaches the third time, the source valve V4 is closed, and the second reaction precursor is stopped. The third time is 0.1~15s, and the source mass of the second source bottle is determined according to the actual reaction precursor. In this process, the boost valve V2 is closed, the source valve V3 is closed, the vacuum angle valve V1 is opened, and the carrier gas valve V5 is opened. Exemplarily, when the second reaction precursor is H2O (liquid), the amount of H2O introduced is 1~3mg, and the third time is 0.1~2s; when the second reaction precursor is H2 (gaseous), the amount of H2 introduced is 3~6L, and the third time is 5~15s.

[0055] S5: introducing a constant flow of pressurized gas into the reaction chamber and simultaneously stopping evacuating the reaction chamber; when the time for introducing the pressurized gas or the time for stopping evacuating the reaction chamber reaches a second time, the introduction of the pressurized gas is stopped and the evacuation of the reaction chamber is continued until the reaction chamber is returned to a low vacuum state.

[0056] After the second reaction precursor is introduced, a pressurized gas is introduced to perform a second pressurized diffusion treatment, and the second pressurized diffusion treatment specifically includes: When performing the second pressurized diffusion treatment, the booster valve V2 is opened and the vacuum angle valve V1 is closed, and the pressurized gas is introduced. When the pressurized gas introduction time or the time for stopping the vacuum pumping of the reaction chamber reaches the second time, the booster valve V2 is closed and the vacuum angle valve V1 is opened to pump the reaction chamber to a low vacuum state; wherein the second time is 1 to 20 seconds. During this process, the source valve V3 and the source valve V4 remain closed, and the carrier gas valve V5 remains open.

[0057] When the reaction chamber is evacuated to a low vacuum state, the booster valve V2, source valve V3, and source valve V4 remain closed, and the vacuum pump, vacuum angle valve V1, and carrier gas valve V5 remain open. After the reaction chamber reaches a low vacuum state, the reaction chamber is purged with an inert gas for 5 to 10 seconds.

[0058] Wherein, steps S2 to S5 constitute one deposition cycle. The number of deposition cycles is determined according to the target thickness of the required film, and steps S2 to S5 are repeated until a film of target thickness is obtained on the surface of the high aspect ratio structure device.

[0059] After the coating of the high aspect ratio structure device surface is completed, the vacuum pump is turned off, the vacuum angle valve V1 is turned off, the booster valve V2 is turned off, the source valve V3, the source valve V4, and the carrier valve V5 are turned off, and the door of the wafer loading platform in the reaction chamber is opened to take out the high aspect ratio structure device. In some embodiments, the number of deposition cycles is 100 to 200 times.

[0060] In this embodiment, each time after the reaction precursor gas is introduced, the pressurized 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 pressurized gas enters the reaction chamber, so that the pressure of the reaction chamber increases and decreases, thereby allowing the reaction precursor to quickly enter the deep holes / channels of the high aspect ratio structure device and be effectively adsorbed in the high aspect ratio structure device.

[0061] In some embodiments, the present application provides an atomic layer deposition coating method for a high aspect ratio structure device. Figure 4The atomic layer deposition coating system for high aspect ratio structure devices in the invention comprises a reaction chamber, a vacuum pump connected to the reaction chamber, a pressurized gas pipeline and a carrier gas pipeline; a vacuum angle valve V1 is provided on the connection pipeline between the reaction chamber and the vacuum pump, and a pressurized gas pipeline connected to the reaction chamber is provided with a pressurized valve V2; after the reaction is completed, the vacuum angle valve V1 is closed to effectively prevent the airflow in the vacuum pump from flowing back into the reaction chamber, and the pressurized valve V2 can effectively prevent the pressurized gas from entering the reaction chamber. A carrier gas valve V5 is provided on the carrier gas pipeline, and the carrier gas pipeline is respectively connected to a first source bottle and a second source bottle, the first source bottle stores a first reaction precursor, the second source bottle stores a second reaction precursor, a source valve V3 is provided on the connection pipeline between the first source bottle and the carrier gas pipeline, and a source valve V4 is provided on the connection pipeline between the second source bottle and the carrier gas pipeline. The source valve V3, the source valve V4 and the carrier gas valve V5 are respectively used to control whether the first reaction precursor is introduced, whether the second reaction precursor is introduced, and whether the carrier gas is introduced.

[0062] A first butterfly valve V6 is provided on the connection pipeline between the reaction chamber and the vacuum pump, and the first butterfly valve V6 is located between the vacuum angle 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 pressurized valve V2 and the reaction chamber; wherein the openings of the first butterfly valve V6 and the second butterfly valve V7 are controllable, and the openings of the first butterfly valve V6 and the second butterfly valve V7 change in reverse periodicity; the first butterfly valve V6 and the second butterfly valve V7 are used to control the pressure in the reaction chamber to increase and decrease within the second time, so that the pressure in the reaction chamber is in dynamic change. The first butterfly valve V6 is used to control the suction volume of the vacuum pump, and the second butterfly valve V7 is used to control the inflow flow of the pressurized gas.

[0063] When placing a high aspect ratio structure device in the reaction chamber, the reaction chamber door is opened, and at the same time, the vacuum pump, vacuum angle valve V1, booster valve V2, source valve V3, source valve V4 and carrier valve V5 are closed, and the opening of the first butterfly valve V6 and the opening of 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 at the same time, the vacuum pump, vacuum angle valve V1, booster valve V2, carrier valve V5 are opened, source valve V3 and source valve V4 are closed, the opening of the first butterfly valve V6 is adjusted to a preset opening, and the opening of the second butterfly valve V7 is 0%, so as to evacuate the reaction chamber to a low vacuum.

[0064] 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, booster valve V2, source valve V3, and carrier valve V5 are opened, and the source valve V4 is closed. The opening of the first butterfly valve V6 is the preset opening, and the opening 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, booster valve V2, and carrier valve V5 are opened, and the source valve V3 and source valve V4 are closed. The opening of the first butterfly valve V6 is the preset opening, and the opening of the second butterfly valve V7 is 0%; when the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped into the reaction chamber change in an inverse periodic manner, the vacuum pump, vacuum angle valve V1, booster valve V2, and carrier valve V5 are opened. , the carrier valve V5 is opened, and the source valve V3 and the source valve V4 are closed at the same time, the openings of the first butterfly valve V6 and the second butterfly valve V7 change periodically in the reverse direction, when the opening of the first butterfly valve decreases from the 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 reverse periodic change reaches the second time, the vacuum pump, the vacuum angle valve V1, the booster valve V2, and the carrier valve V5 are opened, and the source valve V3 and the source valve V4 are closed at the same time, the openings of the first butterfly valve V6 and the second butterfly valve V7 stop changing periodically in the reverse direction, and the opening of the first butterfly valve V6 is maintained at the preset opening, and the opening of the second butterfly valve V7 is maintained at 0%.

[0065] When the reaction chamber is evacuated to a low vacuum state, the vacuum pump, vacuum angle valve V1, booster valve V2, and carrier valve V5 are opened, while source valve V3 and source valve V4 are closed, the opening of the first butterfly valve V6 is a preset opening, and the opening 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, booster valve V2, source valve V4, and carrier valve V5 are opened, while source valve V3 is closed, the opening of the first butterfly valve V6 is a preset opening, and the opening 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, booster valve V2, and carrier valve V5 are opened, while source valve V3 and source valve V4 are closed, the opening of the first butterfly valve V6 is a preset opening, and the opening of the second butterfly valve V7 is 0%.

[0066] The atomic layer deposition coating method provided in this embodiment is the same as the atomic layer deposition coating method provided in the above embodiment and will not be described in detail. In order to facilitate a clear understanding of the functions of each valve and to facilitate distinction, the first butterfly valve V6 and the second butterfly valve V7 are referred to as APC butterfly valve V6 and APC butterfly valve V7 in the following text.

[0067] The atomic layer deposition coating method provided in this embodiment includes: S1': placing a high aspect ratio structure device in a reaction chamber, and evacuating the reaction chamber to a low vacuum state.

[0068] Specifically, the door of the wafer loading platform in the reaction chamber is opened, and the high aspect ratio structure device is placed. During this process, the vacuum pump, vacuum angle valve V1, booster valve V2, source valve V3, source valve V4 and carrier valve V5 are closed, and the opening of APC butterfly valve V6 and APC butterfly valve V7 are 0%. It should be noted that when carrier valve V5 is closed, the carrier gas in the carrier gas pipeline is pushed toward carrier valve V5, and when booster valve V2 is closed, the booster gas in the booster gas pipeline is pushed toward booster valve V2; after placing the high aspect ratio structure device, the door of the wafer loading platform in the reaction chamber is closed, and the vacuum pump is turned on to evacuate the reaction chamber. During this process, carrier valve V5, vacuum pump, vacuum angle valve V1 and booster valve V2 are opened, source valve V3 and source valve V4 are closed, the opening of APC butterfly valve V6 is adjusted to the preset opening, and the opening of APC butterfly valve V7 is 0%. The pumping speed of the vacuum pump is 500~800 m 3 / h, the flow rate of carrier gas before passing through carrier gas valve V5 is consistent with the flow rate into the reaction chamber, both are 40~60sccm, the reaction chamber is evacuated to a low vacuum state, the pressure value of the reaction chamber is 1~2torr, the flow rate of booster gas before passing through booster valve V2 is consistent with the flow rate into the reaction chamber, and the booster gas flow rate is 800~1500sccm.

[0069] The vacuum pump, vacuum angle valve V1, boost valve V2 and carrier gas valve V5 are opened during vacuuming and closed after the coating of the surface of the high aspect ratio structure device is completed.

[0070] S2': introducing a first reaction precursor into the reaction chamber, and stopping the introduction of the first reaction precursor when the introduction time of the first reaction precursor reaches a first time.

[0071] Specifically, after the reaction chamber reaches a low vacuum state, the source valve V3 is opened, and the first reaction precursor is introduced. When the first reaction precursor introduction time reaches the first time, the source valve V3 is closed, and the first reaction precursor is stopped. The first time is 0.1~10s, and the source mass of the first source bottle is determined according to the actual reaction precursor. In this process, the source valve V4 is closed, the opening of the APC butterfly valve V6 is the preset opening, and the opening of the APC butterfly valve V7 is 0%. Exemplarily, when the first reaction precursor is TMA (trimethylaluminum), the TMA source amount is 1~2mg, and the first time is 0.1~2s; when the first reaction precursor is Cu(acac)2 (copper acetylacetonate), the Cu(acac)2 source amount is 1~3mg, and the first time is 3~6s.

[0072] S3': the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped into the reaction chamber are changed in reverse periodicity, and when the time of the reverse periodicity reaches a second time, the reverse periodicity is stopped and the reaction chamber is pumped back to a low vacuum state.

[0073] The pressurized gas volume is the flow rate of the pressurized gas before it passes through the boost valve V2, and the suction volume is the suction volume of the vacuum pump.

[0074] When the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped into the reaction chamber change in reverse periodicity, the opening of the APC butterfly valve V6 and the opening of the APC butterfly valve V7 change in reverse periodicity. When the time of reverse periodicity changes reaches the second time, the opening of the APC butterfly valve V6 and the opening of the APC butterfly valve V7 stop changing in reverse periodicity. During this process, the source valve V3 and the source valve V4 are closed. The second time is 1 to 20 seconds.

[0075] When the opening of APC butterfly valve V6 decreases from the preset opening to 0%, and then increases from 0% to the preset opening, while the opening of APC butterfly valve V7 increases from 0% to the preset opening, and then decreases from the preset opening to 0%, it is called a reverse periodic change, and the time of a reverse periodic change is 1~20s, that is, the second time. 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 draws the reaction chamber back to a low vacuum state.

[0076] S31': The opening of the APC butterfly valve V6 and the opening of the APC butterfly valve V7 show continuous and synchronous reverse periodic changes. When the opening of the APC butterfly valve V6 decreases from a preset opening to 0%, the opening of the APC butterfly valve V7 increases from 0% to the preset opening. When the opening of the APC butterfly valve V6 increases from 0% to the preset opening, the opening of the APC butterfly valve V7 decreases from the preset opening to 0%. Exemplarily, the preset opening is 70-90%.

[0077] When the opening of APC butterfly valve V7 decreases, the flow of pressurized gas through the boost valve V2 decreases; when the opening of APC butterfly valve V7 increases, the flow of pressurized gas through the boost valve V2 increases. For example, taking the 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%.

[0078] S32': When the time of the reverse periodic change reaches the second time, the opening of the APC butterfly valve V6 is maintained at a preset opening, the opening of the APC butterfly valve V7 is maintained at 0%, and the vacuum pump draws the reaction chamber back to a low vacuum state.

[0079] Specifically, when the time of reverse periodic change reaches the second time, the opening of the APC butterfly valve V6 and the opening of the APC butterfly valve V7 stop reverse periodic change, the opening of the APC butterfly valve V6 is maintained to a preset opening, the opening of the APC butterfly valve V7 is maintained to 0%, and the reaction chamber is pumped back to a low vacuum state.

[0080] In some embodiments, after the reaction chamber is evacuated to a low vacuum state, a purging operation is further included. The inert gas purging process includes evacuating the reaction chamber to a low vacuum state and a purging operation. The purging operation is specifically purging the reaction chamber with an inert gas. The purging time is 5 to 10 seconds.

[0081] S4': introducing a second reaction precursor into the reaction chamber, and when the introduction time of the second reaction precursor reaches a third time, stopping the introduction of the second reaction precursor.

[0082] Specifically, when the vacuum pump draws the reaction chamber back to a low vacuum state, the source valve V4 is opened, and the second reaction precursor is introduced. When the second reaction precursor introduction time reaches the third time, the source valve V4 is closed, and the introduction of the second reaction precursor is stopped. The third time is 0.1-15s, and the source mass of the second source bottle is determined according to the actual reaction precursor. In this process, the source valve V3 is closed, the opening of the APC butterfly valve V6 is the preset opening, and the opening of the APC butterfly valve V7 is 0%. Exemplarily, when the second reaction precursor is H2O (liquid), the amount of H2O introduced is 1-3mg, and the third time is 0.1-2s; when the second reaction precursor is H2 (gaseous), the amount of H2 introduced is 3-6L, and the third time is 5-15s.

[0083] S5': the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped into the reaction chamber are changed in reverse periodicity, and when the time of the reverse periodicity reaches a second time, the reverse periodicity is stopped and the reaction chamber is pumped back to a low vacuum state.

[0084] When the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped into the reaction chamber change in reverse periodicity, the opening of the APC butterfly valve V6 and the opening of the APC butterfly valve V7 change in reverse periodicity continuously and synchronously. When the time of reverse periodicity changes reaches the second time, the opening of the APC butterfly valve V6 and the opening of the APC butterfly valve V7 stop changing in reverse periodicity. During this process, the source valve V3 and the source valve V4 are closed. The second time is 1 to 20 seconds.

[0085] When the time of the reverse periodic change reaches the second time, the opening of the APC butterfly valve V6 is maintained at the preset opening, the opening of the APC butterfly valve V7 is maintained at 0%, and the vacuum pump draws the reaction chamber back to a low vacuum state.

[0086] S51': The opening of the APC butterfly valve V6 and the opening of the APC butterfly valve V7 change periodically in the opposite direction. When the opening of the APC butterfly valve V6 decreases from a preset opening to 0%, the opening of the APC butterfly valve V7 increases from 0% to the preset opening. When the opening of the APC butterfly valve V6 increases from 0% to the preset opening, the opening of the APC butterfly valve V7 decreases from the preset opening to 0%. Exemplarily, the preset opening is 70-90%.

[0087] When the opening of APC butterfly valve V7 decreases, the flow of pressurized gas through boost valve V2 decreases; when the opening of APC butterfly valve V7 increases, the flow of pressurized gas through boost valve V2 increases. For example, taking the preset opening of 80% as an example, the opening range of APC butterfly valve V6 is 80% to 0%, and then from 0% to 80%; the opening range of APC butterfly valve V7 is from 0% to 80%, and then from 80% to 0%.

[0088] S52': When the time of the reverse periodic change reaches the second time, the opening of the APC butterfly valve V6 is maintained at a preset opening, the opening of the APC butterfly valve V7 is maintained at 0%, and the vacuum pump draws the reaction chamber back to a low vacuum state.

[0089] Specifically, when the time of reverse periodic change reaches the second time, the opening of APC butterfly valve V6 and the opening of APC butterfly valve V7 stop reverse periodic change, the opening of APC butterfly valve V6 is maintained to a preset opening, the opening of APC butterfly valve V7 is maintained to 0%, and the reaction chamber is pumped back to a low vacuum state. After the reaction chamber reaches the low vacuum state, the reaction chamber is also purged with inert gas for 5 to 10 seconds.

[0090] Wherein, steps S2' to S5' constitute one deposition cycle. The number of deposition cycles is determined according to the target thickness of the required film, and steps S2' to S5' are repeated until a film of target thickness is obtained on the surface of the high aspect ratio structure device.

[0091] When the coating on the surface of the high aspect ratio structure device is completed, the vacuum pump is turned off, the vacuum angle valve V1 is turned off, the booster valve V2 is turned off, the source valve V3, the source valve V4, and the carrier valve V5 are turned off, the opening of the APC butterfly valve V6 and the APC butterfly valve V7 is 0%, and the door of the wafer loading platform in the reaction chamber is opened to take out the high aspect ratio structure device. In some embodiments, the number of deposition cycles is 100 to 200 times.

[0092] The openings of the APC butterfly valve V6 and the APC butterfly valve V7 in the present application are controllable. After the reaction precursor enters the reaction chamber, the openings of the APC butterfly valve V6 and the APC butterfly valve V7 are adjusted, and the pressure in the reaction chamber increases and decreases. The openings of the APC butterfly valve V6 and the APC butterfly valve V7 are changed periodically in the opposite direction, so that the reaction precursor can effectively enter the deep holes of the high aspect ratio structural device, and at the same time, the disadvantage of insufficient diffusion of the reaction precursor in the structure of the high aspect ratio structural device is effectively avoided, and the phenomenon that the reaction precursor cannot be fully deposited in structures such as deep holes or channels of the high aspect ratio structural device is improved.

[0093] The following is a detailed explanation with reference to specific cases.

[0094] The structures of the high aspect ratio structural devices used in the following embodiments are all deep hole structures with an aspect ratio of 300:1, and the pressurized 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 of pumping the reaction chamber to a low vacuum state in the following embodiments are all the same, and the same parameters are maintained during the deposition process of the high aspect ratio structural device.

[0095] Example 1 In this embodiment, the first reaction precursor is TMA (trimethylaluminum), and the second reaction precursor is H2O. The system device used in this embodiment is connected as follows: Figure 3 As shown, the flow rate of the pressurized gas in this embodiment is constant.

[0096] (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 valve V5 are closed; after placing the high aspect ratio structure device, close the door of the wafer loading platform in the reaction chamber, and turn on the vacuum pump to evacuate the reaction chamber. At the same time, open the carrier valve V5, vacuum pump and vacuum angle valve V1, close the booster valve V2, and close the source valve V3 and source valve V4. The vacuum pump has a pumping speed of 600m 3 / h, the flow rate of carrier gas is 40sccm, the reaction chamber is evacuated to a low vacuum state, and the pressure value of the reaction chamber is 1torr. When the carrier gas valve V5 is closed, the carrier gas in the carrier gas pipeline pushes against the carrier gas valve V5, and when the booster valve V2 is closed, the booster gas in the booster gas pipeline pushes against the booster valve V2. Among them, the vacuum pump is turned on when the reaction chamber is evacuated, and is closed after the coating of the surface of the high aspect ratio structure device is completed.

[0097] (2) When the reaction chamber reaches a low vacuum state, the source valve V3 is opened to introduce the first reaction precursor. When the introduction time of the first reaction precursor reaches the first time, the source valve V3 is closed to stop introducing the first reaction precursor, wherein the first time is 0.2s, and the mass of the first source bottle is 1.5mg. During this process, the booster valve V2 is closed, the source valve V4 is closed, the vacuum angle valve V1 is opened, the carrier gas valve V5 is opened, and the vacuum pump is turned on.

[0098] (3) When performing the pressurized diffusion treatment, a constant flow of pressurized gas is introduced into the reaction chamber and the reaction chamber is stopped from being evacuated at the same time, the pressurizing valve V2 is opened, the vacuum angle valve V1 is closed, and the pressurized gas is introduced. When the pressurized gas introduction time or the time of stopping the evacuation of the reaction chamber reaches a second time, the pressurized gas is stopped, the pressurizing 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.

[0099] When the reaction chamber is evacuated to a low vacuum state, the carrier gas valve V5, the vacuum pump and the vacuum angle valve V1 are opened, at which time the booster valve V2 is closed, and the source valve V3 and the source valve V4 are closed. After the reaction chamber reaches a low vacuum state, the reaction chamber is purged with an inert gas for 8 seconds.

[0100] (4) After the purge is completed, the source valve V4 is opened to introduce the second reaction precursor. When the introduction time of the second reaction precursor reaches the third time, the source valve V4 is closed to stop introducing the second reaction precursor; wherein the third time is 0.2s, and the mass of the second source bottle is 1.5mg. During this process, the booster valve V2 is closed, the source valve V3 is closed, the vacuum pump is opened, the vacuum angle valve V1 is opened, and the carrier gas valve V5 is opened.

[0101] (5) When performing the pressurized diffusion treatment, a constant flow of pressurized gas is introduced into the reaction chamber and the reaction chamber is stopped from being evacuated at the same time, the pressurizing valve V2 is opened, the vacuum angle valve V1 is closed, and the pressurized gas is introduced. When the pressurized gas introduction time or the time of stopping the evacuation of the reaction chamber reaches a second time, the pressurized gas is stopped, the pressurizing 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.

[0102] When the reaction chamber is evacuated to a low vacuum state, the booster valve V2, source valve V3, and source valve V4 remain closed, and the vacuum pump, vacuum angle valve V1, and carrier gas valve V5 remain open. When the reaction chamber reaches a low vacuum state, the reaction chamber is also purged with an inert gas for 8 seconds.

[0103] Among them, steps (2) to (5) constitute one deposition cycle.

[0104] After 150 deposition cycles, the vacuum pump is turned off, the vacuum angle valve V1 is turned off, the boost valve V2 is turned off, the source valve V3 is turned off, the source valve V4 is turned off, and the carrier valve V5 is turned off. The door of the wafer loading platform in the reaction chamber is opened to take out the high aspect ratio structure device, on which the Al2O3 (aluminum oxide) film is deposited. Figure 6 The figure shows the pressure curve of the reaction chamber of the present 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. Figure 7 and Figure 8 shown.

[0105] Example 2 In this embodiment, the first reaction precursor is TMA, the second reaction precursor is H2O, and the system device used in this embodiment is connected as follows Figure 4 As shown, in this embodiment, the amount of pressurized gas introduced into the reaction chamber and the amount of gas extracted from the reaction chamber vary in an inverse periodic manner.

[0106] (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 valve V5 are closed, and the opening of APC butterfly valve V6 and APC butterfly valve V7 is 0%. When the carrier valve V5 is closed, the carrier gas in the carrier gas pipeline pushes toward the carrier valve V5, and when the booster valve V2 is closed, the booster gas in the booster gas pipeline pushes toward the booster valve V2.

[0107] After placing the high aspect ratio structure device, close the door of the wafer loading platform in the reaction chamber, and open the vacuum pump, vacuum angle valve V1, booster valve V2 and carrier gas valve V5 at the same time. The vacuum pump has a pumping speed of 600 m / s. 3 / h, the flow rate of carrier gas is 40sccm, and the flow rate of boost gas is 1000sccm. The reaction chamber is evacuated to a low vacuum state, and the pressure value of the reaction chamber is 1torr. At this time, source valve V3 and source valve V4 are closed, the opening of APC butterfly valve V6 is 80% (preset opening), and the opening of APC butterfly valve V7 is 0%.

[0108] The vacuum pump, vacuum angle valve V1, boost valve V2 and carrier gas valve V5 are opened during vacuuming and closed after the coating of the surface of the high aspect ratio structure device is completed.

[0109] (2) When the reaction chamber reaches a low vacuum state, the source valve V3 is opened to introduce the first reaction precursor. When the first reaction precursor introduction time reaches the first time, the source valve V3 is closed to stop introducing the first reaction precursor. The first time is 0.2s, and the source mass is 1.5mg. During this process, the source valve V4 is closed, the opening of the APC butterfly valve V6 is 80% (preset opening), and the opening of the APC butterfly valve V7 is 0%.

[0110] (3) When the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped into the reaction chamber change in reverse cyclical manner, the opening of the APC butterfly valve V6 and the opening of the APC butterfly valve V7 change in reverse cyclical manner, the opening of the APC butterfly valve V6 decreases from 80% (preset opening) to 0%, and then increases from 0% to 80% (preset opening), the opening of the APC butterfly valve V7 increases from 0% to 80% (preset opening), and then decreases from 80% (preset opening) to 0%; when the time of reverse cyclical change reaches the second time, the opening of the APC butterfly valve V6 and the opening of the APC butterfly valve V7 stop changing in reverse cyclical manner, the opening of the APC butterfly valve V6 is maintained at 80% (preset opening), the opening of the APC butterfly valve V7 is maintained at 0%, and the reaction chamber is pumped back to a low vacuum state. During this process, the source valve V3 and the source valve V4 are closed. The second time is 5s.

[0111] When the reaction chamber is evacuated to a low vacuum state, source valves V3 and V4 are closed, the opening of APC butterfly valve V6 is 80% (preset opening), and the opening of APC butterfly valve V7 is 0%. After the reaction chamber reaches a low vacuum state, the reaction chamber is purged with inert gas for 8 seconds.

[0112] (4) After the purge is completed, the source valve V4 is opened to introduce the second reaction precursor. When the introduction time of the second reaction precursor reaches the third time, the source valve V4 is closed to stop introducing the second reaction precursor. The third time is 0.2s, and the source mass is 1.5mg. During this process, the source valve V3 is closed, the opening of the APC butterfly valve V6 is 80% (preset opening), and the opening of the APC butterfly valve V7 is 0%.

[0113] (5) When the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped into the reaction chamber change in reverse cyclical manner, the openings of the APC butterfly valve V6 and the APC butterfly valve V7 change in reverse cyclical manner, the opening of the APC butterfly valve V6 decreases from 80% (preset opening) to 0%, and then increases from 0% to 80% (preset opening), the opening of the APC butterfly valve V7 increases from 0% to 80% (preset opening), and then decreases from 80% (preset opening) to 0%; when the time of reverse cyclical change reaches the second time, the openings of the APC butterfly valve V6 and the APC butterfly valve V7 stop changing in reverse cyclical manner, the opening of the APC butterfly valve V6 is maintained at 80% (preset opening), the opening of the APC butterfly valve V7 is maintained at 0%, and the reaction chamber is pumped back to a low vacuum state. During this process, the source valve V3 and the source valve V4 are closed. The second time is 5s. After the reaction chamber reaches a low vacuum state, the reaction chamber is purged with an inert gas for 8 seconds.

[0114] Among them, steps (2) to (5) constitute one deposition cycle.

[0115] After 150 deposition cycles, the vacuum pump, vacuum angle valve V1, booster valve V2, source valve V3, source valve V4, carrier valve V5 are closed, the opening of APC butterfly valve V6 and APC butterfly valve V7 is 0%, and the door of the wafer loading platform in the reaction chamber is opened to take out the high aspect ratio structure device, on which Al2O3 (aluminum oxide) film is deposited. Fig. 9 The figure shows the pressure curve of the reaction chamber of the present 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. Fig.10 and Fig.11 shown.

[0116] Comparative Example 1 In this embodiment, the first reaction precursor is TMA, the second reaction precursor is H2O, and the device used in this embodiment is Figure 1 shown.

[0117] (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, carrier 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 in the reaction chamber and turn on the vacuum pump to evacuate the reaction chamber. At the same time, turn on the vacuum pump, vacuum angle valve V1 and carrier valve V5, and close the source valve V3 and source valve V4. The vacuum pump has a pumping speed of 600 m / s. 3 / h, the flow rate of carrier gas is 40sccm, the reaction chamber is evacuated to a low vacuum state, and the pressure value of the reaction chamber is 1torr.

[0118] (2) When the reaction chamber reaches a low vacuum state, the source valve V3 is opened to introduce the first reaction precursor. When the introduction time of the first reaction precursor reaches the first time, the source valve V3 is closed to stop introducing the first reaction precursor, wherein the first time is 0.2s, and the mass of the first source bottle is 1.5mg. During this process, the source valve V4 is closed, the vacuum angle valve V1 is opened, the carrier gas valve V5 is opened, and the vacuum pump is turned on.

[0119] When the reaction chamber is evacuated to a low vacuum state, the carrier gas valve V5, the vacuum pump and the vacuum angle valve V1 are opened, and at this time, the source valve V3 and the source valve V4 are closed. When the reaction chamber reaches a low vacuum state, the reaction chamber is also purged with an inert gas for 8 seconds.

[0120] (3) After the purge is completed, the source valve V4 is opened to introduce the second reaction precursor. When the introduction time of the second reaction precursor reaches the third time, the source valve V4 is closed to stop introducing the second reaction precursor; wherein the third time is 0.2s, and the mass of the second source bottle is 1.5mg. During this process, the source valve V3 is closed, the vacuum pump is turned on, the vacuum angle valve V1 is opened, and the carrier gas valve V5 is opened.

[0121] When the reaction chamber is evacuated to a low vacuum state, the source valve V3 and the source valve V4 remain closed, and the vacuum pump, the vacuum angle valve V1, and the carrier gas valve V5 remain open. After the reaction chamber reaches a low vacuum state, the reaction chamber is purged with an inert gas for 8 seconds.

[0122] Among them, steps (2) to (3) constitute one deposition cycle.

[0123] After 150 depositions, the vacuum pump is turned off, the vacuum angle valve V1 is turned off, the source valve V3 is turned off, the source valve V4 is turned off, the carrier valve V5 is turned off, and the door of the wafer loading platform in the reaction chamber is opened to take out the high aspect ratio structure device, on which the Al2O3 (aluminum oxide) film is deposited. Fig.12 The figure shows the pressure curve of the reaction chamber of this embodiment, where t1 is the first time, t2 is the purge time, t3 is the third time, and t4 is the purge time. Fig.13 and Fig.14 shown.

[0124] Combination Figures 6 to 14 It can be seen that in Comparative Example 1, the deep hole structure of the high aspect ratio structure device is deposited using the traditional atomic layer deposition coating method. Fig.13 and Fig.14 It can be seen that with the increase of depth, Al element can no longer be detected, and Al2O3 fails to completely fill the deep hole structure of the high aspect ratio structure device. Example 1 The deposition of the deep hole structure of the high aspect ratio structure device is achieved by adjusting the opening and closing of the vacuum angle valve V1 and the boost valve V2. Figure 7 and Figure 8 It can be seen that although the Al element still cannot completely fill the deep hole structure of the high aspect ratio structure device, it is significantly improved compared with the comparative example 1. Example 2 achieves the deposition of the deep hole structure of the high aspect ratio structure device by adjusting the opening of the APC butterfly valve V6 and the APC butterfly valve V7. Fig.10 and Fig.11 It can be seen that the Al element has been completely filled into the deep hole structure of the high aspect ratio structure device, and the density is good.

[0125] Among them, the reaction parameters in Example 1 and Example 2 are the same, and the difference is that Example 2 is based on Example 1, and APC butterfly valve V6 and APC butterfly valve V7 are added. The opening of APC butterfly valve V6 and the opening of APC butterfly valve V7 are reversely periodically changed, so that the reaction precursor can effectively enter the deep hole of the high aspect ratio structure device, and at the same time effectively avoids the disadvantage 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 hole or channel structure of the high aspect ratio structure device.

[0126] Example 3 In this embodiment, the first reaction precursor is Cu(acac)2 (copper acetylacetonate), and the second reaction precursor is H2. The system device used in this embodiment is connected as follows: Figure 3 As shown, the flow rate of the pressurized gas in this embodiment is constant.

[0127] (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 valve V5 are closed; when the carrier valve V5 is closed, the carrier gas in the carrier gas pipeline is pushed toward the carrier gas valve V5, and when the booster valve V2 is closed, the pressurized gas in the booster gas pipeline is pushed toward the booster valve V2.

[0128] After placing the high aspect ratio structure device, close the door of the wafer loading platform in the reaction chamber, and start the vacuum pump to evacuate the reaction chamber. At the same time, open the carrier valve V5, vacuum pump and vacuum angle valve V1, close the booster valve V2, and close the source valve V3 and source valve V4. The vacuum pump has a pumping speed of 600 m / s. 3 / h, the flow rate of the carrier gas is 40sccm, and the reaction chamber is evacuated to a low vacuum state, and the pressure value of the reaction chamber is 1torr. Among them, the carrier gas valve V5 and the vacuum pump are opened when the reaction chamber is evacuated, and are closed after the coating of the surface of the high aspect ratio structure device is completed.

[0129] (2) When the reaction chamber reaches a low vacuum state, the source valve V3 is opened and the first reaction precursor is introduced. When the introduction time of the first reaction precursor reaches the first time, the source valve V3 is closed and the introduction of the first reaction precursor is stopped. The first time is 5s and the mass of the first source bottle is 2mg. During this process, the booster valve V2 is closed, the source valve V4 is closed, the vacuum angle valve V1 is opened, the carrier gas valve V5 is opened, and the vacuum pump is turned on.

[0130] (3) When performing the pressurized diffusion treatment, a constant flow of pressurized gas is introduced into the reaction chamber and the reaction chamber is stopped from being evacuated at the same time, the pressurizing valve V2 is opened, the vacuum angle valve V1 is closed, and the pressurized gas is introduced. When the pressurized gas introduction time or the time of stopping the evacuation of the reaction chamber reaches a second time, the pressurized gas is stopped, the pressurizing 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.

[0131] When the reaction chamber is evacuated to a low vacuum state, the carrier gas valve V5, the vacuum pump and the vacuum angle valve V1 are opened, at which time the booster valve V2 is closed, and the source valve V3 and the source valve V4 are closed. After the reaction chamber reaches a low vacuum state, the reaction chamber is purged with an inert gas for 8 seconds.

[0132] (4) After the purge is completed, the source valve V4 is opened to introduce the second reaction precursor. When the introduction time of the second reaction precursor reaches the third time, the source valve V4 is closed to stop introducing the second reaction precursor; wherein the third time is 10s, and the source volume of the second source bottle is 4.7L. During this process, the booster valve V2 is closed, the source valve V3 is closed, the vacuum pump is opened, the vacuum angle valve V1 is opened, and the carrier gas valve V5 is opened.

[0133] (5) When performing the pressurized diffusion treatment, a constant flow of pressurized gas is introduced into the reaction chamber and the reaction chamber is stopped from being evacuated at the same time, the pressurizing valve V2 is opened, the vacuum angle valve V1 is closed, and the pressurized gas is introduced. When the pressurized gas introduction time or the time of stopping the evacuation of the reaction chamber reaches a second time, the pressurized gas is stopped, the pressurizing 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.

[0134] When the reaction chamber is evacuated to a low vacuum state, the booster valve V2, source valve V3, and source valve V4 remain closed, and the vacuum pump, vacuum angle valve V1, and carrier gas valve V5 remain open. When the reaction chamber reaches a low vacuum state, the reaction chamber is also purged with an inert gas for 8 seconds.

[0135] Among them, steps (2) to (5) constitute one deposition cycle.

[0136] After 150 depositions, the vacuum pump, vacuum angle valve V1, booster valve V2, source valve V3, source valve V4, and carrier valve V5 are turned off, and the door of the wafer loading platform in the reaction chamber is opened to take out the high aspect ratio structure device on which the Cu film is deposited. Fig.15The figure shows the pressure curve of the reaction chamber of the present 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. Fig.16 and Fig.17 shown.

[0137] Example 4 In this embodiment, the first reaction precursor is Cu(acac)2 (copper acetylacetonate), and the second reaction precursor is H2. The system device used in this embodiment is connected as follows: Figure 4 As shown, in this embodiment, the amount of pressurized gas introduced into the reaction chamber and the amount of gas extracted from the reaction chamber vary in an inverse periodic manner.

[0138] (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 valve V5 are closed, and the opening of APC butterfly valve V6 and APC butterfly valve V7 is 0%. When the carrier valve V5 is closed, the carrier gas in the carrier gas pipeline pushes toward the carrier valve V5, and when the booster valve V2 is closed, the booster gas in the booster gas pipeline pushes toward the booster valve V2.

[0139] After placing the high aspect ratio structure device, close the door of the wafer loading platform in the reaction chamber, and open the vacuum pump, vacuum angle valve V1, booster valve V2 and carrier gas valve V5 at the same time. The vacuum pump has a pumping speed of 600 m / s. 3 / h, the flow rate of carrier gas is 40sccm, and the flow rate of boost gas is 1000sccm. The reaction chamber is evacuated to a low vacuum state, and the pressure value of the reaction chamber is 1torr. At this time, source valve V3 and source valve V4 are closed, the opening of APC butterfly valve V6 is 80% (preset opening), and the opening of APC butterfly valve V7 is 0%.

[0140] The vacuum pump, vacuum angle valve V1, boost valve V2 and carrier gas valve V5 are opened during vacuuming and closed after the coating of the surface of the high aspect ratio structure device is completed.

[0141] (2) When the reaction chamber reaches a low vacuum state, the source valve V3 is opened to introduce the first reaction precursor. When the first reaction precursor introduction time reaches the first time, the source valve V3 is closed to stop introducing the first reaction precursor. The first time is 5s, and the source mass is 2mg. During this process, the source valve V4 is closed, the opening of the APC butterfly valve V6 is 80% (preset opening), and the opening of the APC butterfly valve V7 is 0%.

[0142] (3) When the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped into the reaction chamber change in reverse cyclical manner, the openings of APC butterfly valve V6 and APC butterfly valve V7 change in reverse cyclical manner, the opening of APC butterfly valve V6 decreases from 80% (preset opening) to 0%, and then increases from 0% to 80% (preset opening), the opening of APC butterfly valve V7 increases from 0% to 80% (preset opening), and then decreases from 80% (preset opening) to 0%; when the time of reverse cyclical change reaches the second time, the opening of APC butterfly valve V6 and the opening of APC butterfly valve V7 stop changing in reverse cyclical manner, the opening of APC butterfly valve V6 is maintained at 80% (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. During this process, source valve V3 and source valve V4 are closed. The second time is 5s.

[0143] When the reaction chamber is evacuated to a low vacuum state, source valves V3 and V4 are closed, the opening of APC butterfly valve V6 is 80% (preset opening), and the opening of APC butterfly valve V7 is 0%. After the reaction chamber reaches a low vacuum state, the reaction chamber is purged with inert gas for 8 seconds.

[0144] (4) After the purge is completed, the source valve V4 is opened to introduce the second reaction precursor. When the introduction time of the second reaction precursor reaches the third time, the source valve V4 is closed to stop introducing the second reaction precursor. The third time is 10s, and the source volume is 4.7L. During this process, the source valve V3 is closed, the opening of the APC butterfly valve V6 is 80% (preset opening), and the opening of the APC butterfly valve V7 is 0%.

[0145] (5) When the amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped into the reaction chamber change in reverse cyclical manner, the openings of APC butterfly valves V6 and V7 change in reverse cyclical manner, the opening of APC butterfly valve V6 decreases from 80% (preset opening) to 0%, and then increases from 0% to 80% (preset opening), and the opening of APC butterfly valve V7 increases from 0% to 80% (preset opening), and then decreases from 80% (preset opening) to 0%; when the time of reverse cyclical change reaches the second time, the openings of APC butterfly valves V6 and V7 stop changing in reverse cyclical manner, the opening of APC butterfly valve V6 is maintained at 80% (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. During this process, source valves V3 and V4 are closed. The second time is 5s. After the reaction chamber reaches a low vacuum state, the reaction chamber is purged with an inert gas for 8 seconds.

[0146] Among them, steps (2) to (5) constitute one deposition cycle.

[0147] After 150 depositions, the vacuum pump is turned off, the vacuum angle valve V1 is turned off, the boost valve V2 is turned off, the source valve V3, the source valve V4, the carrier valve V5 are turned off, the opening of the APC butterfly valve V6 and the APC butterfly valve V7 are 0%, and the door of the wafer loading platform in the reaction chamber is opened to take out the high aspect ratio structure device, on which the Cu film is deposited. Fig.18 The figure shows the pressure curve of the reaction chamber of the present 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. Fig.19 and Fig. 20 shown.

[0148] Comparative Example 2 In this embodiment, the first reaction precursor is Cu(acac)2 (copper acetylacetonate), and the second reaction precursor is H2 (corresponding to source valve V4). The device used in this embodiment is as follows Figure 1 shown.

[0149] (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, carrier 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 in the reaction chamber and turn on the vacuum pump to evacuate the reaction chamber. At the same time, turn on the vacuum pump, vacuum angle valve V1 and carrier valve V5, and close the source valve V3 and source valve V4. The vacuum pump has a pumping speed of 600 m / s. 3 / h, the flow rate of carrier gas is 40sccm, the reaction chamber is evacuated to a low vacuum state, and the pressure value of the reaction chamber is 1torr.

[0150] (2) When the reaction chamber reaches a low vacuum state, the source valve V3 is opened to introduce the first reaction precursor. When the introduction time of the first reaction precursor reaches the first time, the source valve V3 is closed to stop introducing the first reaction precursor. The first time is 5s, and the mass of the first source bottle is 2mg. During this process, the source valve V4 is closed, the vacuum angle valve V1 is opened, the carrier gas valve V5 is opened, and the vacuum pump is turned on.

[0151] When the reaction chamber is evacuated to a low vacuum state, the carrier gas valve V5, the vacuum pump and the vacuum angle valve V1 are opened, and at this time, the source valve V3 and the source valve V4 are closed. After the reaction chamber reaches a low vacuum state, the reaction chamber is purged with an inert gas for 8 seconds.

[0152] (3) After the purge is completed, the source valve V4 is opened to introduce the second reaction precursor. When the introduction time of the second reaction precursor reaches the third time, the source valve V4 is closed to stop introducing the second reaction precursor; wherein the third time is 10s, and the source volume of the second source bottle is 4.7L. During this process, the source valve V3 is closed, the vacuum pump is turned on, the vacuum angle valve V1 is opened, and the carrier gas valve V5 is opened.

[0153] When the reaction chamber is evacuated to a low vacuum state, the source valve V3 and the source valve V4 remain closed, and the vacuum pump, the vacuum angle valve V1, and the carrier gas valve V5 remain open. After the reaction chamber reaches a low vacuum state, the reaction chamber is purged with an inert gas for 8 seconds.

[0154] Among them, steps (2) to (3) constitute one deposition cycle.

[0155] After 150 depositions, the vacuum pump, vacuum angle valve V1, source valve V3, source valve V4, and carrier valve V5 are turned off, and the door of the wafer loading platform in the reaction chamber is opened to take out the high aspect ratio structure device on which the Cu film is deposited. Fig.21 The figure shows the pressure curve of the reaction chamber of the present embodiment, where t1 is the first time, t2 is the purge time, t3 is the third time, and t4 is the purge time. Fig. 22 and Fig.23 shown.

[0156] Combination Figures 15 to 23 It can be seen that in Comparative Example 2, the deep hole structure of the high aspect ratio structure device is deposited using the traditional atomic layer deposition coating method. Fig. 22 and Fig.23 It can be seen that as the depth increases, the Cu element fails to completely fill the deep hole structure of the high aspect ratio structure device. Example 3 achieves deposition of the deep hole structure of the high aspect ratio structure device by adjusting the opening and closing of the vacuum angle valve V1 and the boost valve V2. Fig.16 and Fig.17 It can be seen that although the Cu element has been filled into the deep hole structure of the high aspect ratio structure device, the density is poor. Example 4 The deposition of the deep hole structure of the high aspect ratio structure device is achieved by adjusting the opening of the APC butterfly valve V6 and the APC butterfly valve V7. Fig.19 and Fig. 20 It can be seen that the Cu element has been completely filled into the deep hole structure of the high aspect ratio structure device, and the density is good.

[0157] Among them, the different openings 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, by adjusting the openings of APC butterfly valve V6 and APC butterfly valve V7, the influence of the percentage of Al element inside the high aspect ratio structure device is tested. Fig.24 The horizontal axis is the preset opening of the APC butterfly valve, and the vertical axis is the percentage of Al element (%). Fig.24 It can be seen that when the preset opening is 80%, the structural filling effect is best, and the percentage of Al atoms in the deep hole structure of the high aspect ratio structure device is greater than 90%.

[0158] Taking Example 4 as an example, the influence of the percentage of Cu element inside the high aspect ratio structure device was tested by adjusting the opening of the butterfly valve. Fig.25 The horizontal axis is the preset opening of the APC butterfly valve, and the vertical axis is the percentage of Cu element (%). Fig.25 It can be seen that when the preset opening is 80%, the structural filling effect is best, and the percentage of Cu atoms in the deep hole structure of the high aspect ratio structure device is greater than 85%.

[0159] Compared with the conventional atomic layer deposition process, the atomic layer deposition coating method for high aspect ratio structural devices provided in the present application controls the opening of APC butterfly valve V6 and APC butterfly valve V7, adjusts the opening of APC butterfly valve V6 and APC butterfly valve V7, increases and decreases the pressure in the reaction chamber, and simultaneously adjusts the opening of APC butterfly valve V6 and APC butterfly valve V7, so that the reaction precursor can effectively enter the deep hole of the high aspect ratio structural device. In this way, effective coating of the reaction precursor in the deep hole or channel structure of the high aspect ratio structural device can be achieved.

[0160] It can be seen from the above embodiments that the present application provides an atomic layer deposition coating method and system for high aspect ratio structural devices, the method comprising 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 of the first reaction precursor reaches a first time; performing a pressurization diffusion treatment on the reaction chamber, stopping the pressurization diffusion treatment when the pressurization diffusion treatment time reaches a second time and evacuating the reaction chamber back to a low vacuum state; introducing a second reaction precursor into the reaction chamber, and stopping the introduction of the second reaction precursor when the introduction time of the second reaction precursor reaches a third time; performing a pressurization diffusion treatment on the reaction chamber, stopping the pressurization diffusion treatment when the pressurization diffusion treatment time reaches a second time and evacuating the reaction chamber back to a low vacuum state, thereby completing the coating on the surface of the high aspect ratio structural device. The present application increases and decreases the pressure in the reaction chamber through the coordinated control of the first valve and the second valve, or the reverse periodic change of the opening of the first butterfly valve and the second butterfly valve, so that the reaction precursor quickly or effectively enters the deep hole / channel of the high aspect ratio structure device and is adsorbed in the high aspect ratio structure device.

[0161] Similar parts between the embodiments provided in this application can be referenced to each other. The specific implementation methods provided above are only a few examples under the general concept of this application and do not constitute a limitation on the protection scope of this application. For those skilled in the art, any other implementation methods expanded based on the scheme of this application without creative work belong to the protection scope of this application.

Claims

1. An atomic layer deposition coating method for high aspect ratio structure devices, characterized in that: The atomic layer deposition coating method for high aspect ratio structure devices comprises: Placing a high aspect ratio structure 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 of the first reaction precursor reaches a first time; Performing a pressurization diffusion treatment on the reaction chamber, stopping the pressurization diffusion treatment when the time of the pressurization diffusion treatment reaches a second time and pumping the reaction chamber back to a low vacuum state; Introducing a second reaction precursor into the reaction chamber, and stopping the introduction of the second reaction precursor when the introduction time of the second reaction precursor reaches a third time; The reaction chamber is subjected to a pressurized diffusion treatment, and when the time of the pressurized diffusion treatment reaches a second time, the pressurized diffusion treatment is stopped and the reaction chamber is pumped back to a low vacuum state, thereby completing the coating on the surface of the high aspect ratio structure device.

2. The atomic layer deposition coating method for high aspect ratio structure devices according to claim 1, characterized in that: Performing a pressurization diffusion treatment on the reaction chamber, stopping the pressurization diffusion treatment when the time of the pressurization diffusion treatment reaches a second time and pumping the reaction chamber back to a low vacuum state comprises: A pressurized gas with a constant flow rate is introduced into the reaction chamber and the reaction chamber is simultaneously stopped from being evacuated, and when the time for introducing the pressurized gas or the time for stopping evacuating the reaction chamber reaches a second time, the pressurized gas is stopped from being introduced and the reaction chamber is continuously evacuated until the reaction chamber is evacuated back to a low vacuum state; or, The amount of pressurized gas introduced into the reaction chamber and the amount of gas pumped into the reaction chamber are changed in reverse periodicity, and when the time of the reverse periodicity change reaches a second time, the reverse periodicity change is stopped and the reaction chamber is pumped back to a low vacuum state.

3. The atomic layer deposition coating method for high aspect ratio structure devices according to claim 2, characterized in that: The reaction chamber is respectively connected to a vacuum pump and a pressurized 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 pressurized gas pipeline connected to the reaction chamber; wherein, when a pressurized gas with a constant flow rate is introduced into the reaction chamber and the reaction chamber is stopped from being vacuumed, the first valve is closed and the second valve is opened, and when the pressurized gas introduction time 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 vacuum the reaction chamber until the reaction chamber is evacuated to a low vacuum state.

4. The atomic layer deposition coating method for high aspect ratio structure devices according to claim 2, characterized in that: The reaction chamber is respectively connected to a vacuum pump and a pressurized gas pipeline, and a first valve and a first butterfly valve are provided on the connecting pipeline between the reaction chamber and the vacuum pump, the first butterfly valve is located between the first valve and the reaction chamber, and 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; wherein, when the amount of pressurized gas introduced into the reaction chamber and the amount of gas extracted from the reaction chamber show reverse periodic changes, the first valve and the second valve are opened, and the opening of the first butterfly valve and the opening of the second butterfly valve show reverse periodic changes, and when the time of the reverse periodic change reaches a second time, the first valve and the second valve are opened, and the opening of the first butterfly valve and the opening of the second butterfly valve stop reverse periodic changes.

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

6. The atomic layer deposition coating method for high aspect ratio structure devices according to claim 5, characterized in that: When the reaction chamber is subjected to pressurized diffusion treatment, the opening of the first butterfly valve and the opening of the second butterfly valve present a continuous and synchronous reverse periodic change. 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 coating method for high aspect ratio structure devices according to claim 6, characterized in that: When the time of the reverse periodic change reaches a second time, the opening of the first butterfly valve is maintained at a preset opening, the opening of the second butterfly valve is maintained at 0%, and the vacuum pump draws the reaction chamber back to a low vacuum state.

8. The atomic layer deposition coating method for high aspect ratio structure devices according to claim 3, characterized in that: The reaction chamber is also connected to a carrier gas pipeline, a fifth valve is arranged on the carrier gas pipeline, the carrier gas pipeline is respectively connected to a first source bottle and a second source bottle, the first source bottle stores a first reaction precursor, the second source bottle stores a second reaction precursor, a third valve is arranged on the connecting pipeline between the first source bottle and the carrier gas pipeline, and a fourth valve is arranged on the connecting 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 a 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 a 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 coating method for high aspect ratio structure devices according to claim 4, characterized in that: The reaction chamber is also connected to a carrier gas pipeline, on which a fifth valve is arranged, and the carrier gas pipeline is respectively connected to a first source bottle and a second source bottle, wherein a first reaction precursor is stored in the first source bottle, and a second reaction precursor is stored in the second source bottle, a third valve is arranged on the connecting pipeline between the first source bottle and the carrier gas pipeline, and a fourth valve is arranged on the connecting 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 opening of the second butterfly valve are 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, and 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, The second valve, the third valve, and the fifth valve are opened, the fourth valve is closed, the opening of the first butterfly valve is a preset opening, and the opening 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 valve, the second valve, and the fifth valve are opened, the third valve and the fourth valve are closed, the opening of the first butterfly valve is a preset opening, and the opening of the second butterfly valve is 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 opened, the third valve is closed, the opening of the first butterfly valve is a preset opening, and the opening 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 valve, the second valve, and the fifth valve are opened, the third valve and the fourth valve are closed, the opening of the first butterfly valve is a preset opening, and the opening of the second butterfly valve is 0%.

10. The atomic layer deposition coating method for high aspect ratio structure devices according to claim 8, characterized in that: The pressure in the reaction chamber under low vacuum state is 1~2torr, and the pumping speed of the vacuum pump is 500~800m 3 / h, the gas flow rate of the carrier gas before passing through the fifth valve is 40~60sccm, 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 boost gas before passing through the second valve is 800~1500sccm.

11. The atomic layer deposition coating method for high aspect ratio structure devices according to claim 9, characterized in that: The pressure in the reaction chamber under low vacuum state is 1~2torr, and the pumping speed of the vacuum pump is 500~800m 3 / h, the gas flow rate of the carrier gas before passing through the fifth valve is 40~60sccm, 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 800~1500sccm, and the preset opening is 70~90%.

12. An atomic layer deposition coating system for high aspect ratio structural devices, characterized in that: Used to perform the atomic layer deposition coating method for high aspect ratio structure devices according to claim 1; Wherein, the atomic layer deposition coating system for high aspect ratio structure devices comprises: A reaction chamber, a vacuum pump connected to the reaction chamber, a pressurized gas pipeline, and a 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 pressurized gas pipeline connected to the reaction chamber; A fifth valve is provided on the carrier gas pipeline, and the carrier gas pipeline is respectively connected to a first source bottle and a second source bottle, the first source bottle stores a first reaction precursor, 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.

13. The atomic layer deposition coating system for high aspect ratio structure devices according to claim 12, characterized in that: The atomic layer deposition coating system for high aspect ratio structure devices also includes: A first butterfly valve is provided on the connecting pipeline 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 openings of the first butterfly valve and the second butterfly valve are controllable.

Images