Atomic layer deposition equipment and method for two-dimensional film patterning manufacturing

Abstract

The invention relates to the field of semiconductor micro-nano manufacturing processes, in particular to atomic layer deposition equipment and method for two-dimensional film patterning manufacturing. The core of the preparation method is that a bearing platform in a deposition cavity is replaced by a multi-station rotating disc, the disc is provided with a plurality of double-layer stations in the circumferential direction, the upper layer is used for fixing a patterned mask, and the lower layer is used for fixing a deposition substrate; and an external control system drives the disc to rotate step by step, so that the stations sequentially enter a central deposition reaction area, and flexible definition of two-dimensional material film deposition of atomic deposition on the surface of the substrate and a preset pattern is realized in cooperation with alternate pulses of a precursor source. The structure supports the design of various patterning masks and multi-substrate continuous processing, and the flexibility and the process efficiency of patterned film preparation are remarkably improved.

Description

Technical Field

[0001] This invention belongs to the field of semiconductor manufacturing technology, and specifically relates to an atomic layer deposition apparatus and method for two-dimensional thin film patterning. Background Technology

[0002] Two-dimensional thin films, due to their atomic-level thickness and unique physicochemical properties, show significant potential in next-generation high-performance electronics, optoelectronic devices, and sensing. Achieving patterned deposition of thin films is a prerequisite for constructing functional micro / nano devices, and its precision and efficiency directly determine device performance and integration density.

[0003] Atomic Layer Deposition (ALD), a vapor deposition method based on self-confined surface reactions, offers advantages such as atomic-level thickness control, excellent uniformity, and high conformity, making it an ideal technology for fabricating high-quality two-dimensional thin films. However, the core function of traditional ALD equipment is to achieve the deposition of large-area uniform thin films; it lacks patterning capabilities. Current mainstream approaches to ALD patterning typically rely on two methods: one is to use a pre-fabricated patterned hard mask to cover the substrate, which needs to be removed after deposition—a cumbersome process with difficulties in mask alignment, cleaning, and reuse; the other is to perform global deposition first, then define the pattern through subsequent photolithography and etching processes, increasing process complexity and the risk of introducing contamination. This approach makes it difficult to directly fabricate patterned structures and fails to meet the demands of multi-substrate, high-efficiency mass production. Summary of the Invention

[0004] To address the aforementioned problems, this invention discloses an atomic layer deposition apparatus and method for fabricating two-dimensional thin film patterns. The apparatus includes a deposition chamber, a precursor source system, a gas path system, and a multi-station rotating disk disposed within the deposition chamber. The precursor source system provides the precursor. Within the deposition chamber, equipped with a heating device, patterned deposition and in-situ annealing processes of the thin film are sequentially completed. The core of this apparatus lies in the precise stepping rotation and positioning of the substrate and mask assembly driven by the multi-station rotating disk, allowing each station to sequentially enter the deposition zone. This achieves sequential processing of multiple substrates and flexible, efficient definition of patterns. Combined with the in-situ annealing process within the chamber, the crystal quality and performance of the thin film are effectively improved, thereby enabling controllable fabrication of two-dimensional thin film patterns.

[0005] To achieve the above objectives, the technical solution of the present invention is as follows: An atomic layer deposition apparatus for patterning two-dimensional thin films, comprising: The deposition chamber is equipped with a heating device that enables controllable heating of the interior of the chamber, providing a uniform and stable reaction environment for the patterned deposition of two-dimensional thin films; the deposition chamber is also equipped with a transition chamber for sample transfer. A precursor source system for storing precursors required for atomic layer deposition; A gas path system, which is precisely regulated by valves and flow meters, is used to deliver precursor sources and inert gases to the deposition chamber during the deposition process and to discharge reaction tail gases from the chamber. A multi-station rotating disk is disposed within the deposition chamber to fix the mask and the deposition substrate, and to allow each station to enter the deposition area sequentially by rotating, thereby achieving sequential deposition of patterned thin films.

[0006] Furthermore, it also includes external control systems and circuit systems: The external control system is used to control the switching of valves and flow meters in the gas path system, the stepping rotation of the multi-station rotary disk, and the heating program of the deposition chamber. The circuit system is used to supply power to the atomic layer deposition equipment.

[0007] Furthermore, the precursor source system includes two precursor source bottles, the material of which can be 316 stainless steel or 316L stainless steel; each precursor source bottle is equipped with an independent heating protection sleeve.

[0008] Furthermore, the deposition chamber consists of a sample deposition chamber and a transition chamber.

[0009] Furthermore, the sample deposition chamber is made of 316L stainless steel.

[0010] Furthermore, the heating temperature of the deposition chamber can be set within the range of 50 to 800 ℃.

[0011] Furthermore, the transition chamber is made of 316L stainless steel and is connected to the sample deposition chamber.

[0012] Furthermore, the multi-station rotating disk is step-controlled by the external control system.

[0013] Furthermore, each station of the multi-station rotating disk is provided with a mask plate and a base-independent mechanical clamping structure.

[0014] Furthermore, the mask is made of monocrystalline silicon, quartz, or high-temperature resistant stainless steel.

[0015] Furthermore, the gas path system is connected to a vacuum pump for evacuating the deposition chamber and discharging the reaction exhaust gas generated during the deposition process.

[0016] Secondly, the present invention also provides an atomic layer deposition method for fabricating two-dimensional thin film patterning, based on the atomic layer deposition apparatus described above, comprising the following steps: The mask and the deposition substrate are respectively loaded and fixed on the corresponding positions of the multi-station rotating disk; The deposition chamber is evacuated by a vacuum pump connected to the gas path system to achieve the required low vacuum level. An inert gas at a pressure higher than atmospheric pressure is introduced into the deposition chamber through the gas path system to perform inert gas atmosphere cleaning and remove residual gas. The circuit system supplies power to the heating device of the deposition chamber and the precursor source system, turns on the heating function, and heats the deposition chamber to a preset deposition temperature and keeps it stable. The external control system controls the valves and flow meters of the gas path system to deliver the precursor to the deposition chamber in a pulsed manner, perform atomic layer deposition on the substrate surface, and remove excess precursor and reaction byproducts by purging with inert gas. The external control system controls the multi-station rotary disk to rotate stepwise, switches stations, and repeats the above steps to sequentially deposit patterned thin films on the substrate at each station. The external control system heats the deposition chamber to perform in-situ annealing on the deposited film. After in-situ annealing, the deposition chamber is cooled under an inert gas atmosphere. Once the temperature reaches a safe level, the gas supply and heating are stopped, atmospheric pressure is restored, and the sample is removed.

[0017] Furthermore, the deposition substrate is a silicon oxide wafer, a silicon wafer, an aluminum oxide wafer, or a copper wafer.

[0018] Furthermore, the vacuum pump evacuates the deposition chamber and the gas path system to a vacuum level of 0 to 200 Pa.

[0019] Furthermore, the heating temperature of the precursor source system is 25 ~ 150℃.

[0020] Furthermore, the deposition heating temperature of the deposition chamber is 50 to 600°C.

[0021] Furthermore, the control motor of the multi-station rotating disk is a servo motor, which can realize step-by-step switching of the workstations.

[0022] Furthermore, the in-situ annealing process performed on the deposition chamber is at a temperature of 500~700℃.

[0023] The beneficial effects of this invention are as follows: 1. The present invention provides an atomic layer deposition apparatus and method for two-dimensional thin film patterning manufacturing. By integrating a multi-station rotating disk with mask and deposition substrate fixing and multi-station switching functions, combined with a precisely controlled gas path system and heating device, it realizes efficient and orderly patterned thin film deposition on multiple substrates in a single deposition chamber, which significantly improves manufacturing efficiency and pattern alignment accuracy.

[0024] 2. The present invention precisely controls the stepping rotation of the multi-station rotating disk through the external control system, so that each station enters the deposition zone sequentially. Combined with the pulse and purging process of inert gas, it ensures that the patterned deposition reaction conditions at each station are consistent, thereby greatly improving the uniformity and repeatability of film thickness and pattern morphology.

[0025] 3. By performing in-situ annealing directly within the deposition chamber, this invention avoids contamination and oxidation of the sample during transfer, effectively reduces defects within the film, optimizes the crystal quality and electrical properties of the film, and achieves integrated manufacturing of high-quality two-dimensional thin film patterning. Attached Figure Description

[0026] Figure 1 This is a schematic diagram of the device of the present invention.

[0027] Figure 2 This is a top view of the multi-station rotating disk in this invention.

[0028] List of reference numerals in the attached diagram: 1-Deposition chamber, 2-Precursor source system, 3-Gas path system, 4-Multi-position rotating disk, 5-Mask plate, 6-Deposition substrate, 7-External control system, 8-Circuit system, 9-Transition chamber. Detailed Implementation

[0029] The present invention will be further illustrated below with reference to the accompanying drawings and specific embodiments. It should be understood that the following specific embodiments are for illustrative purposes only and are not intended to limit the scope of the invention.

[0030] Example 1: like Figure 1 As shown, this specific embodiment 1 provides an atomic layer deposition apparatus for two-dimensional thin film patterning, comprising: The deposition chamber 1 consists of a sample deposition chamber and a transition chamber 9, and is made of 316L stainless steel. The sample deposition chamber integrates a heated sample stage, whose working temperature can be stably controlled within the range of 50~800℃, providing a uniform thermal environment for the deposition reaction. The transition chamber 9 is connected to the sample deposition chamber and is used for sample transfer. Precursor source system 2, which includes two independent precursor source bottles and their heating protective sleeves, for storing and providing the precursors required for the deposition process; Gas system 3, which is equipped with valves and flow meters, and has an inert gas at a pressure higher than one atmosphere, is used to precisely deliver the precursor to the patterned deposition chamber 1 in a pulse form, and to purge and discharge the exhaust gas after the reaction. A multi-station rotating disk 4 is disposed in the sample deposition chamber of the patterned deposition cavity 1, and is used to simultaneously load and fix multiple mask plates 5 and deposition substrates 6. External control system 7, which is used to coordinate and control the valves and flow rate of the gas path system 3, the heating program of the patterned deposition chamber 1, and the stepping rotation of the multi-station rotating disk 4. Circuit system 8 is used to provide power to the entire device.

[0031] In this embodiment, the precursor source system 2 includes two precursor source bottles made of 316L stainless steel, and the deposition temperature of the patterned deposition chamber 1 is set to 400 ℃. The multi-station rotating disk 4 has four double-layer stations. Each station can hold a patterned mask 5 (made of monocrystalline silicon) on the upper layer and a silicon oxide wafer deposition substrate 6 on the lower layer. The surface of the mask 5 is a hollowed-out pattern. The gas path system 3 uses high-purity nitrogen as the inert gas, and is controlled by an external control system 7 through programming to achieve an alternating cycle of precursor pulse (1 second) and nitrogen purging (60 seconds). During the deposition process, the external control system 7 drives the multi-station rotating disk 4 to rotate in steps, so that each station enters the deposition area sequentially, thereby forming a patterned thin film on the substrate in sequence.

[0032] However, it should be understood that the specific embodiments of the present invention are not limited thereto. In other specific embodiments, the number of stations of the multi-station rotating disk 4 can be 2 to 8. The material of the mask 7 can be quartz or high-temperature resistant stainless steel. The deposition substrate 6 can be a silicon wafer, aluminum oxide, or copper sheet, etc. The inert gas used in the gas path system 3 can also be argon, and the pulse and purge times can be adjusted within the range of 0.5 to 5 seconds and 30 to 180 seconds according to process requirements.

[0033] Example 2: This specific embodiment provides an atomic layer deposition method for two-dimensional thin film patterning based on the equipment of Embodiment 1, including the following steps: S1: The designed mask and the corresponding deposition substrate are respectively loaded and fixed on each station of the multi-station rotating disk; S2: Vacuum the patterned deposition chamber through the vacuum pump connected to the gas path system, so that the internal pressure drops to below 50 Pa. S3: High-purity nitrogen gas is introduced into the patterned deposition cavity to perform atmospheric cleaning, so as to remove residual air and moisture from the cavity; S4: Power the device through the circuit system, start the heating program, raise the temperature of the precursor source system to 80°C, and raise the temperature of the patterned deposition chamber to 400°C deposition temperature and keep it stable; S5: Through the external control system, the preset deposition program is started: the control gas path system pulses the first precursor (such as a metal source) into the cavity, causing it to undergo a self-limiting adsorption reaction on the exposed substrate surface, and then nitrogen is introduced for purging; then the second precursor (such as a non-metal source) is pulsed to react, and then nitrogen is purged again; thus completing one atomic layer deposition cycle. S6: After one deposition cycle is completed, the external control system drives the multi-station rotary disk to rotate one station in a step-by-step manner, so that the mask and substrate of the next station enter the deposition zone, and the deposition cycle of step S5 is repeated. S7: Repeat steps S5 and S6 in sequence until the substrates at all stations have completed the patterned thin film deposition of the predetermined number of layers; S8: After deposition is completed, the patterned deposition chamber is heated to 650 °C and held for 30 minutes in an inert gas atmosphere to perform in-situ annealing of the film. S9: After annealing, maintain an inert gas atmosphere and allow the chamber to cool naturally to a safe temperature (e.g., below 100 ℃). After restoring normal pressure, remove the sample.

[0034] This method achieves efficient and consistent patterned thin film deposition on multiple substrates within a single process chamber by sequentially switching between multi-station rotating disks, significantly improving production efficiency and pattern uniformity. In-situ annealing effectively enhances the crystallinity quality of the thin film.

[0035] Example 3: Specific embodiment 3 of this invention provides a process for preparing patterned MoS2 thin films. The deposition substrate is a 1-inch silicon oxide wafer. The precursor source system includes two source bottles: precursor source 1 is molybdenum pentachloride (MoCl5), heated to 150°C; precursor source 2 is hydrogen sulfide (H2S), used at room temperature. The set temperature of the patterned deposition chamber is 450°C. A multi-station rotating disk carries four stations, two of which use masks with micron-scale strip array patterns, and the other two use masks with dot matrix patterns, enabling the fabrication of different patterns of two-dimensional thin film materials within the same chamber.

[0036] The specific process is as follows: First, the chamber was evacuated to 20 Pa and purged with nitrogen. Then, the MoCl5 source and chamber were heated to 150 °C and 450 °C respectively and stabilized. The deposition cycle parameters were set as follows: 1 second MoCl5 pulse – 60 seconds N2 purging – 1 second H2S pulse – 60 seconds N2 purging. After each deposition cycle, the disk was rotated 90° in a stepping motion to the next station. This process was repeated 200 times.

[0037] In this process, the precursor is deposited on the substrate through the patterned window of the mask, thereby forming MoS2 thin films with strip arrays and dot array patterns corresponding to the mask on the silicon oxide wafers at each station.

[0038] After deposition, the chamber temperature was raised to 700 °C under H2S atmosphere protection for 30 minutes of in-situ annealing. This effectively compensated for sulfur vacancy defects in the MoS2 film, significantly improving the film's crystallinity and electrical properties.

[0039] It should be noted that the above content merely illustrates the technical concept of the present invention and should not be construed as limiting the scope of protection of the present invention. For those skilled in the art, various improvements and modifications can be made without departing from the principle of the present invention, and all such improvements and modifications fall within the scope of protection of the claims of the present invention.

Claims

1. An atomic layer deposition apparatus for patterning two-dimensional thin films, characterized in that, include: Deposition chamber, precursor source system, gas path system, multi-position rotating disk; The deposition chamber is equipped with a heating device, which can controllably heat the interior of the chamber to provide a uniform and stable reaction environment for the patterned deposition of two-dimensional thin films; it also includes a transition chamber for sample transfer into or out of the deposition area. The precursor source system is used to store the precursors required for atomic layer deposition and to transport the precursors to the deposition chamber via the gas path system during the deposition process. The gas path system is precisely regulated by valves and flow meters to deliver precursor sources and inert gases to the deposition chamber during the deposition process and to discharge reaction tail gases from the chamber. The multi-station rotating disk is disposed in the deposition chamber to fix the mask and the deposition substrate, and rotates to allow each station to enter the deposition area in sequence, thereby realizing the sequential deposition of patterned thin films.

2. The atomic layer deposition apparatus for two-dimensional thin film patterning according to claim 1, characterized in that, It also includes external control systems and circuit systems: The external control system is used to control the switching of valves and flow meters in the gas circuit system, as well as the stepping rotation of the multi-station rotary disk, and also includes the heating program of the deposition chamber. The circuit system is used to supply power to the atomic layer deposition equipment.

3. The atomic layer deposition apparatus for two-dimensional thin film patterning according to claim 1, characterized in that, The precursor source system includes two precursor source bottles, which are made of 316 stainless steel or 316L stainless steel; each precursor source bottle is equipped with an independent heating protection sleeve.

4. The atomic layer deposition apparatus for two-dimensional thin film patterning according to claim 1, characterized in that, The deposition chamber consists of a sample deposition chamber and a transition chamber; the sample deposition chamber is made of 316L stainless steel; the operating temperature is set within the range of 50~800 ℃; the transition chamber of the deposition chamber is also made of 316L stainless steel and is connected to the sample deposition chamber.

5. The atomic layer deposition apparatus for two-dimensional thin film patterning according to claim 1, characterized in that, The multi-station rotating disk is step-controlled by the external control system, and each station is equipped with an independent mechanical clamping structure for the mask and the substrate. The mask is made of monocrystalline silicon, quartz or high-temperature resistant stainless steel.

6. The atomic layer deposition apparatus for two-dimensional thin film patterning according to claim 1, characterized in that, The gas path system is connected to a vacuum pump, which is used to perform vacuuming operations on the deposition chamber and to discharge the reaction exhaust gas generated during the deposition process.

7. An atomic layer deposition method for patterning two-dimensional thin films, based on the atomic layer deposition apparatus as described in any one of claims 1-6, characterized in that, The atomic layer deposition equipment includes a deposition chamber, a precursor source system, a gas path system, an external control system, a circuit system, and a multi-station rotating disk, and includes the following steps: The mask and the deposition substrate are respectively loaded and fixed on the corresponding positions of the multi-station rotating disk; The deposition chamber is evacuated by a vacuum pump connected to the gas path system to achieve the required low vacuum level. An inert gas at a pressure higher than atmospheric pressure is introduced into the deposition chamber through the gas path system to perform inert gas atmosphere cleaning and remove residual gas. The power supply structure supplies power to the multi-source supply system and the multi-source co-cavity deposition cavity to activate their heating function, thereby heating and maintaining their temperature. The circuit system supplies power to the heating device of the deposition chamber and the precursor source system, turns on the heating function, and heats the deposition chamber to a preset deposition temperature and keeps it stable. The external control system controls the valves and flow meters of the gas path system to deliver the precursor to the deposition chamber in a pulsed manner, perform atomic layer deposition on the substrate surface, and remove excess precursor and reaction byproducts by purging with inert gas. The external control system controls the multi-station rotary disk to rotate stepwise, switches stations, and repeats the above steps to sequentially deposit patterned thin films on the substrate at each station. After in-situ annealing, the deposition chamber is cooled under an inert gas atmosphere. Once the temperature reaches a safe level, the gas supply and heating are stopped, atmospheric pressure is restored, and the sample is removed.

8. The atomic layer deposition method for fabricating two-dimensional thin film patterning according to claim 7, characterized in that, The deposition substrate is a silicon oxide wafer, a silicon wafer, an aluminum oxide wafer, or a copper wafer.

9. The atomic layer deposition method for fabricating two-dimensional thin film patterning according to claim 7, characterized in that, The vacuum pump evacuates the deposition chamber and the gas path system to 0~200Pa; the heating temperature of the precursor source system is 25~150℃; the heating temperature of the deposition chamber is 50~600℃; and the in-situ annealing process performed on the deposition chamber is 500~700℃.

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