Multifunctional atomic layer deposition device compatible with powder coating

Abstract

The utility model discloses a multifunctional atomic layer deposition device compatible with powder coating, which belongs to the technical field of thin film deposition, and is characterized in that a cavity cover of a planar reaction cavity is redesigned, and a hole is formed in the cavity cover to be connected with a vacuum magnetofluid device; the vacuum magnetofluid device is arranged in the cavity cover, and the powder containers of different specifications are arranged in the cavity cover and connected with the vacuum magnetofluid device, so that the device can meet the requirement for large-size sample film deposition and can also meet the requirement for powder coating of different types of powder samples, the application scene of atomic layer deposition equipment is greatly widened, and the scientific research cost is reduced.

Description

Technical Field

[0001] The utility model relates to a multifunctional atomic layer deposition device compatible with powder coating, belonging to the technical field of thin film deposition. Background Art

[0002] Atomic layer deposition (ALD) technology is a technology for preparing ultra-thin films. It alternately introduces different chemical vapor precursors on the surface of a substrate and deposits materials layer by layer on the substrate through chemical reactions. This process is based on the principles of surface self-limiting and self-saturating adsorption reactions, that is, each reaction step forms a single molecular layer on the substrate surface. When the surface active sites are completely occupied, additional precursors will not be adsorbed, thus achieving precise control of the film thickness. The films prepared based on atomic layer deposition technology have excellent three-dimensional conformal properties, large-area uniformity, etc., are suitable for depositing films on the surface of complex high aspect ratio substrates, and can also ensure precise sub-monolayer film thickness control. Therefore, atomic layer deposition technology is widely used in the fields of microelectronics, energy, information, catalysis, etc.

[0003] Powder atomic layer deposition (PALD) technology is an advanced surface coating technology that can precisely construct ultra-thin nano-coatings or active components on the surface of powder particles. This technology is different from traditional surface modification methods. It can achieve atomic or molecular level control precision, and the coating has good conformal properties.

[0004] Considering that the currently reported thermal ALD equipment deposits films by placing samples in the reaction chamber and depositing the required films on static samples, while powder samples cannot be directly placed in the reaction chamber, so the demand for uniformly coating the surface of powder samples cannot be met; most of the reported powder-type ALD equipment uses fluidized beds or rotation methods to coat powders, and its reaction chamber can only be used to place powder samples, so the demand for film deposition on larger-sized samples by scientific research workers cannot be taken into account. In order to meet the film deposition requirements of powder samples and larger-sized samples, research and development institutions often need to purchase two ALD devices, which will greatly increase the research and development costs. Content of the Utility Model

[0005] In order to solve the above problems, the utility model provides a multifunctional atomic layer deposition device compatible with powder coating. By redesigning the cavity cover of the planar reaction chamber, holes are opened in the newly designed cavity cover and connected to a vacuum magnetohydrodynamic device. Different specifications of powder containers are arranged inside the cavity cover and connected to the vacuum magnetohydrodynamic device. The outside of the cavity cover drives the magnetohydrodynamic fluid to rotate through an electromagnetic coupling driver, so as to ensure that the powder container can rotate in a vacuum state; heating devices are equipped on the top and the annular wall of the cavity cover, so as to ensure the uniformity of the temperature field in the whole cavity.

[0006] In one embodiment, different mesh sieves with different mesh numbers are arranged at both ends of the powder container according to the particle size of the powder sample. In practical applications, they can be disassembled and replaced to meet the coating requirements of powder samples with different particle sizes, and to prevent the powder from overflowing from both ends during rotation. During the experimental process, the gas-phase precursor source diffuses into the powder container through the mesh sieve holes at both ends, fully contacts and reacts with the surface of the powder sample. After the reaction is complete, the by-products generated by the reaction and the excess gas-phase precursor source are cleaned by washing and purging.

[0007] If a large-area planar sample needs to be deposited, simply remove the powder container, place the large-area planar sample in the center of the cavity base, close the cavity cover, evacuate to vacuum, and then the coating process can be carried out according to the experimental process.

[0008] Advantages of the present utility model:

[0009] The multifunctional atomic layer deposition device compatible with powder coating provided by the present utility model, through the re-design of the cavity cover of the planar reaction cavity, opens holes in the cavity cover and connects with the vacuum magnetic fluid device, and different specifications of powder containers are arranged inside the cavity cover and connected with the vacuum magnetic fluid device, so that the device can not only meet the requirements of thin film deposition of large-size samples, but also meet the powder coating requirements of different types of powder samples, greatly broadening the application scenarios of atomic layer deposition equipment and reducing the scientific research cost. Description of the drawings

[0010] Figure 1 It is a schematic diagram of the multifunctional atomic layer deposition device compatible with powder coating provided by the present utility model;

[0011] Figure 2 It is a schematic diagram of the composition of the powder cavity;

[0012] Among them, 1 - powder container, 2 - cavity cover, 3 - heating device, 4 - vacuum magnetic fluid device, 5 - electromagnetic coupling driver, 6 - cavity base, 7 - precursor and carrier gas inlet, 8 - by-product and carrier gas outlet, 9 - handle, 10 - connecting component; 11 - cylinder body, 12 - left pressing plate, 13 - left mesh sieve, 14 - right pressing plate of the container, 15 - right mesh sieve. Detailed implementation manners

[0013] The following is a specific description of the present utility model.

[0014] Example 1

[0015] As Figure 1As shown in the figure, the multifunctional atomic layer deposition device compatible with powder coating provided by the present utility model includes: a powder container 1, a cavity cover 2, and a cavity base 6. The cavity cover 2 and the cavity base 6 are connected by a connecting component 10. Among them, the cavity cover 2 is a lid with a raised edge around it, and through holes are provided on the raised edge, and a vacuum magnetic fluid device 4 is installed at the through holes to achieve dynamic sealing inside the cavity; the powder container 1 is located inside the cavity cover 2 and is connected to an external electromagnetic coupling driver 5 through the through holes to achieve self-rotation, so that the powder sample can fully contact and react with the gas-phase precursor.

[0016] A precursor and carrier gas inlet 7 and a by-product and carrier gas outlet 8 are provided on the cavity base 6.

[0017] In one implementation, heating devices are also provided on the cavity cover 2 and the cavity base 6 to achieve heat treatment during the deposition process. Figure 1 Only the heating device 3 provided on the cavity cover 2 is shown as an example.

[0018] The connecting component 10 is a cavity hinge and is configured with a locking mechanism to stop after the cavity cover 2 is opened at any angle. For easy opening and closing, a handle 9 is also provided on the cavity cover 2.

[0019] The powder container 1 includes a cylinder body 11, a left pressing plate 12, a left screen 13, a right pressing plate 14, and a right screen 15. The left pressing plate 12 and the right pressing plate 14 are annular structures, and the left screen 13 and the right screen 15 are respectively embedded therein and fixed at both ends of the cylinder body 11. Since the particle sizes of the powder samples are diverse, in order to adapt to powder samples with different particle sizes and densities, both ends of the powder container 2 designed in this application can be disassembled and replaced. Different meshes of screens (including the left screen 13 and the right screen 15) can be selected according to the powder particle size. During the experimental process, the screens can prevent the powder samples from overflowing during rotation. The gas-phase precursor source diffuses into the powder container 1 through the screen holes at both ends, fully contacts and reacts with the surface of the powder sample. After the reaction is complete, the by-products and excess gas-phase precursor source generated by the reaction are cleaned by washing and purging.

[0020] No improvements have been made to other conventional components in the atomic layer deposition process in this application, so they are not shown in the drawings, such as the precursor source pipeline, the vacuum pumping pipeline, the ALD valve, and the controller, etc.

[0021] The above device can not only meet the requirements for depositing thin films on large-size samples, but also meet the requirements for powder coating of different types of powder samples. For example, the process of depositing a 30-nm Al2O3 thin film on an 8-inch wafer is as follows:

[0022] Set the deposition temperature of the cavity base and the cavity cover to 200 °C, the temperature of the precursor source pipeline and the ALD valve to 120 °C, and the temperature of the exhaust pipeline to 150 °C. After preheating for 45 minutes, fill the reaction cavity with gas to one atmosphere. Open the cavity cover 2, place an 8-inch wafer at the center of the cavity base 6, close the cavity cover 2 and evacuate. Set the alumina process parameters. Trimethylaluminum is used as the aluminum source for a 50-millisecond pulse and cleaned for 20 seconds; ultrapure water is used as the water source for a 50-millisecond pulse and cleaned for 25 seconds; high-purity nitrogen is used as the carrier gas with a carrier gas flow rate of 20 sccm; the number of cycles is 300 cycles. Click to start coating and start the automatic operation of the alumina process. After the process is completed, stop evacuating and fill the cavity with gas to one atmosphere. Open the cavity cover and take out the sample.

[0023] Another example is the process of coating an approximately 10 nm alumina thin film on a 10-gram silicon oxide powder sample (with a diameter of about 3 microns) as follows:

[0024] Weigh approximately 10 grams of silicon oxide powder and place it in a 20-ml powder container 1. Select a sieve with an appropriate mesh size.

[0025] At room temperature, fill the reaction cavity with gas to one atmosphere. Open the cavity cover 2, install the powder container 1 containing the sample on the electromagnetic coupling driver 5, close the cavity cover 2 and evacuate.

[0026] Set the deposition temperature of the cavity base 6 and the cavity cover 2 to 200 °C, the temperature of the precursor source pipeline and the ALD valve to 120 °C, and the temperature of the exhaust pipeline to 150 °C. After preheating for 45 minutes, set the rotation speed of the electromagnetic coupling driver 5 to 120 revolutions per minute. Set the alumina process parameters. Trimethylaluminum is used as the aluminum source for a 500-millisecond pulse and exposed in the cavity for 20 seconds to allow the gaseous aluminum source to fully contact and react with the powder, then cleaned for 50 seconds to clean up the remaining aluminum source and by-products generated by the reaction; ultrapure water is used as the water source for a 500-millisecond pulse and exposed in the cavity for 20 seconds to allow the gaseous water vapor to fully contact and react with the powder, then cleaned for 50 seconds to clean up the remaining water vapor and by-products generated by the reaction; high-purity nitrogen is used as the carrier gas with a carrier gas flow rate of 50 sccm; the number of cycles is 100 cycles. Click to start coating and start the automatic operation of the alumina process. After the process is completed, set the rotation speed of the electromagnetic coupling driver to 0, stop evacuating and fill the cavity with gas to one atmosphere. Open the cavity cover, remove the powder container 1, and take out the silicon oxide powder on which the deposition has been completed from the powder container 1.

[0027] The working principle of the present utility model:

[0028] When depositing a large-sized sample (such as 8 inches), place the sample on the cavity base, close the cavity cover and evacuate, set the deposition temperature of the base heater and the cavity cover heater, and perform thin film deposition according to the ALD process formula.

[0029] When depositing a thin film on a powder sample, first weigh about 10 grams of the powder and place it in a powder container. Install the powder container on the electromagnetic coupling driver on the chamber lid, close the chamber lid and evacuate the chamber. Set the deposition temperatures of the base heater and the chamber lid heater, and set the rotation speed of the electromagnetic coupling driver (adjustable from 0.1 to 1000 revolutions per minute). Set the ALD process recipe to perform the thin film process deposition.

[0030] Although the present utility model has been disclosed above with preferred embodiments, it is not intended to limit the present utility model. Anyone familiar with this technology can make various modifications and decorations without departing from the spirit and scope of the present utility model. Therefore, the protection scope of the present utility model should be defined by the claims.

Claims

1. A multifunctional atomic layer deposition device compatible with powder coating, characterized in that: The multifunctional atomic layer deposition device comprises a powder container (1), a chamber cover (2) and a chamber base (6), wherein the chamber cover (2) and the chamber base (6) are connected via a connecting component (10); the chamber cover (2) is provided with a through hole, and a vacuum magnetic fluid device (4) is installed at the through hole to achieve dynamic sealing inside the chamber; the powder container (1) is a detachable component, located inside the chamber cover (2), and connected to an external electromagnetic coupling driver (5) via the through hole to achieve self-rotation.

2. The multifunctional atomic layer deposition device compatible with powder coating according to claim 1, characterized in that: The powder container (1) comprises a barrel (11), a left pressure plate (12), a left mesh screen (13), a right pressure plate (14) and a right mesh screen (15); the left pressure plate (12) and the right pressure plate (14) are annular structures, the left mesh screen (13) and the right mesh screen (15) are respectively embedded therein and fixed to the two ends of the barrel (11) by a detachable device.

3. The multifunctional atomic layer deposition device compatible with powder coating according to claim 2, characterized in that: The powder container (1) is provided with a left mesh screen (13) and a right mesh screen (15) of various mesh sizes.

4. The multifunctional atomic layer deposition device compatible with powder coating according to claim 1, characterized in that: The cavity cover (2) is a cover with a raised edge around it, and the through hole is opened on the raised edge.

5. The multifunctional atomic layer deposition device compatible with powder coating according to claim 1, characterized in that: A heating device is also provided on the cavity cover (2) and / or the cavity base (6).

6. The multifunctional atomic layer deposition device compatible with powder coating according to claim 1, characterized in that: The chamber base (6) is provided with a precursor and carrier gas inlet (7) and a by-product and carrier gas outlet (8).

7. The multifunctional atomic layer deposition device compatible with powder coating according to claim 1, characterized in that: The connecting component (10) is a cavity hinge and is provided with a locking mechanism so that the cavity cover (2) stops after opening to any angle.

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