WO2022097861A1

WO2022097861A1 - Atomic layer deposition apparatus for powders

Info

Publication number: WO2022097861A1
Application number: PCT/KR2021/006187
Authority: WO
Inventors: 김재웅; 박형상
Original assignee: (주)아이작리서치
Priority date: 2020-11-09
Filing date: 2021-05-18
Publication date: 2022-05-12
Also published as: KR102570533B1; KR20220062812A

Abstract

The present invention relates to an atomic layer deposition apparatus for powders, wherein a plurality of chambers inclined with respect to the horizontal axis and connected to each other can be used to significantly increase powder processing capacity. The atomic layer deposition apparatus may comprise: chambers having a powder accommodation space that can accommodate powder and is formed inclined so that powder that has flowed in through a powder inlet can flow along an inclined surface and be discharged through a powder outlet, wherein a gas made of at least one selected from among a source gas, a purge gas, and a reaction gas is supplied to the powder; and a stirring device that is installed inside the chamber and stirs the powder.

Description

Atomic Layer Deposition Device for Powder

The present invention relates to an atomic layer deposition apparatus for powder, and more particularly, to an atomic layer deposition apparatus for powder, which can greatly increase a powder processing capacity by using a plurality of chambers inclined in a horizontal axis and connected to each other.

With the rapid development of the powder coating market such as powder catalysts, secondary battery electrodes, and fuel cell MLCC, fields that require high quality powder coating compared to conventional coatings are gradually increasing. According to this demand, powder coating using atomic layer deposition (ALD), which can produce a high-quality thin film compared to the existing wet process, is in the spotlight.

The atomic layer deposition process is a vacuum process that deposits in units of atomic layers. It has excellent step coverage characteristics and is a very advantageous method for coating a small-sized powder surface because the thickness can be adjusted in the order of several nm.

However, in the case of the conventional vertically erected fluidized bed (FB) type atomic layer deposition apparatus for powder coating, a source gas, a primary purge gas, a reaction gas and The secondary purge gas is alternately supplied to deposit an atomic layer on a small amount of powder, and although it is effective for a small-scale process of several kg or less, it is not suitable for mass production for mass production.

That is, since the conventional atomic layer deposition apparatus for powder is not suitable for mass production and rapid process according to mass production from an economic point of view, there are problems in that productivity cannot be maximized.

The present invention is intended to solve various problems including the above problems, and it is possible to greatly increase the powder processing capacity by using a plurality of chambers inclined to the horizontal axis and connected to each other, and to greatly improve the productivity by reducing the coating time. It can be connected in various forms such as a horizontal chamber assembly and a vertical chamber assembly, thereby reducing the limitation of the installation space, and improving the process characteristics by using four chambers that are individually performed by optimizing each of the four processes An object of the present invention is to provide an atomic layer deposition apparatus for powder, which can facilitate the repetition of the coating cycle in a powder circulation method, and can continuously coat a large amount of powder. However, these problems are exemplary, and the scope of the present invention is not limited thereto.

In the atomic layer deposition apparatus for powder according to the spirit of the present invention for solving the above problems, a powder receiving space in which powder can be accommodated is formed, and the powder introduced through the powder inlet is discharged to the powder outlet along the inclined surface. a chamber in which the powder accommodating space is formed to be inclined so that the powder is supplied with a gas formed by selecting at least one of a source gas, a purge gas, and a reaction gas; and a stirring device installed inside the chamber and stirring the powder.

In addition, according to the present invention, the chamber has an inclined cylindrical shape as a whole, the powder inlet is formed at the uppermost side of one side of the outer circumferential surface of the chamber, and the powder outlet is formed at the lowermost side of the other side of the outer circumferential surface of the chamber, A gas inlet may be formed in a lower circular plane, and a pumping line may be formed in an upper circular plane of the chamber.

Further, according to the present invention, the chamber has a first powder inlet through which the powder is introduced on one side of the upper side, and a first powder outlet through which the powder is discharged on the other side of the lower side, and is inclined at a first angle therein. a source gas processing chamber having a first powder accommodating space formed to be large, and supplying a source gas to the powder accommodated in the first powder accommodating space; It is connected to the first powder outlet, and a second powder inlet through which the powder is introduced is formed on one upper side, and a second powder outlet through which the powder is discharged is formed on the other side of the lower side, and is inclined at a second angle therein. a first purge process chamber having a second powder accommodating space to be used and supplying a purge gas to the powder accommodated in the second powder accommodating space; It is connected to the second powder outlet, and a third powder inlet through which the powder is introduced is formed on one upper side, and a third powder outlet through which the powder is discharged is formed on the other lower side, and is inclined at a third angle. a reaction gas processing chamber having a third powder accommodating space to be formed and supplying a reactive gas to the powder accommodated in the third powder accommodating space; and a fourth powder inlet connected to the third powder outlet, and a fourth powder inlet through which the powder is introduced is formed on one upper side, and a fourth powder outlet through which the powder is discharged at the other lower side, and inclined at a fourth angle therein. and a second purge process chamber in which a fourth powder receiving space is formed and a purge gas is supplied to the powder accommodated in the fourth powder receiving space.

In addition, according to the present invention, the source gas process chamber, the first purge process chamber, the reaction gas process chamber, and the second purge process chamber, the powder outlet of the chamber and the powder inlet of the neighboring chamber are connected to each other It may be a horizontal chamber assembly that is interlocked and connected in the front-rear direction as a whole in a line.

In addition, according to the present invention, the source gas process chamber, the first purge process chamber, the reaction gas process chamber, and the second purge process chamber, the powder outlet of the chamber and the powder inlet of the neighboring chamber are connected to each other It may be a vertical chamber assembly that is interlocked and connected by being stacked in a vertical direction in a zigzag shape as a whole.

The present invention may further include a circulation line connecting the second purge process chamber and the source gas process chamber so that at least one process cycle may be performed.

In addition, according to the present invention, the stirring device, the impeller rotated about the tilted stirring rotation shaft so as to transport the powder while mixing; and a rotating device connected to the stirring rotation shaft to rotate the impeller.

In addition, according to the present invention, the impeller may be formed by selecting at least one of a helical type, a ribbon type, a helical ribbon type, an anchor type, a turbine type, a propeller type, and combinations thereof.

Further, according to the present invention, the powder may be transferred in a downward direction in an inclined direction, and the gas may be moved in an upward manner in an inclined direction.

According to some embodiments of the present invention made as described above, it is possible to greatly increase the powder processing capacity by using a plurality of chambers inclined to the horizontal axis and connected to each other, and to greatly improve productivity by reducing the coating time, It can be connected in various forms such as a horizontal chamber assembly and a vertical chamber assembly, thereby reducing the limitation of the installation space, and by optimizing each of the four processes, it is possible to improve the process characteristics by using four chambers that are individually performed. , it is possible to facilitate the repetition of the coating cycle in a powder circulation method, and to have the effect of continuously coating a large amount of powder. Of course, the scope of the present invention is not limited by these effects.

1 is a cross-sectional view showing an atomic layer deposition apparatus for powder according to some embodiments of the present invention.

FIG. 2 is a cross-sectional view illustrating a horizontal chamber assembly of the atomic layer deposition apparatus for powder of FIG. 1 .

3 is a cross-sectional view illustrating a vertical chamber assembly of the atomic layer deposition apparatus for powder of FIG. 1 .

Hereinafter, several preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.

Examples of the present invention are provided to more completely explain the present invention to those of ordinary skill in the art, and the following examples may be modified in various other forms, and the scope of the present invention is as follows It is not limited to an Example. Rather, these embodiments are provided so as to more fully and complete the present disclosure, and to fully convey the spirit of the present invention to those skilled in the art. In addition, in the drawings, the thickness or size of each layer is exaggerated for convenience and clarity of description.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, embodiments of the present invention will be described with reference to the drawings schematically illustrating ideal embodiments of the present invention. In the drawings, variations of the illustrated shape can be envisaged, for example depending on manufacturing technology and/or tolerances. Accordingly, embodiments of the spirit of the present invention should not be construed as limited to the specific shape of the region shown in the present specification, but should include, for example, changes in shape caused by manufacturing.

1 is a cross-sectional view illustrating an atomic layer deposition apparatus 100 for powder according to some embodiments of the present invention.

First, as shown in FIG. 1 , the atomic layer deposition apparatus 100 for powder according to some embodiments of the present invention may largely include a chamber 10 and a stirring apparatus 20 .

For example, as shown in FIG. 1 , in the chamber 10 , a powder receiving space A in which the powder 1 can be accommodated is formed, and the powder 1 introduced through the powder inlet PI is formed. The powder accommodating space (A) is inclined in the horizontal direction so as to be discharged to the powder outlet (PO) along the inclined surface (CF), and the powder (1) contains at least a source gas (SG) and a purge gas (PG). , It may be a structure of a cylindrical shape inclined to a kind of sealing that supplies a gas (G) made by selecting any one of the reaction gas (RG).

However, the chamber 10 is not limited to a cylinder, and all cylindrical structures formed in a variety of shapes, such as a polygonal cylindrical shape or an elliptical cylindrical shape, may be applied.

In addition, for example, as shown in FIG. 1 , the stirring device 20 may be a device installed inside the chamber 10 and capable of stirring the powder 1 .

Accordingly, the powder 1 may be slowly transported downward by gravity while being stirred by the stirring device 20 along the inclined surface CF formed to be inclined in the transverse direction.

More specifically, for example, as shown in FIG. 1 , the powder 1 is transferred downward in an inclined direction, and the gas G is moved upward in an inclined direction so that it can be moved upward. The powder inlet PI is formed at one uppermost portion of the outer circumferential surface of the chamber 10 , and the powder outlet PO is formed at the other lowermost portion of the outer circumferential surface of the chamber 10 , and the lower circular shape of the chamber 10 . A gas inlet GI may be formed on a plane surface, and a pumping line PL may be formed on an upper circular plane of the chamber 10 .

Accordingly, the powder 1 is introduced into the powder inlet PI, which is the highest circumferential portion, and is slowly transported along the inclined surface CF while being stirred by the stirring device 20 inside the chamber 10 . It can be processed by the gas (G) rising upward as it is, and eventually can be discharged to the outside through the powder outlet (PO), which is the lowest circumferential surface portion.

Here, for example, if the inclination angle inclined to the horizontal axis is increased, the processing speed of the powder 1 can be increased, and when the inclination angle is decreased, the gas exposure time of the powder 1 can be increased, thereby increasing the processing rate. can

Accordingly, the inclination angle of the chamber 10 may be determined by being optimized according to the shape of the powder 1 or the specification of the process or environmental conditions.

In addition, for example, as shown in FIG. 1 , the stirring device 20 includes an impeller 21 and It may include a rotation device 22 connected to the stirring rotation shaft 21a to rotate the impeller 21 .

Here, the impeller 21 may be formed by selecting at least one of a helical type, a ribbon type, a helical ribbon type, an anchor type, a turbine type, a propeller type, and combinations thereof.

However, the impeller 21 may be any type of impeller installed inclined to be transported while mixing the powder 1 in addition to the drawings or mentioned types.

FIG. 2 is a cross-sectional view illustrating the horizontal chamber assembly 101 of the atomic layer deposition apparatus 100 for powder of FIG. 1 .

More specifically, for example, as shown in FIG. 2 , the chamber 10 has four chambers each responsible for a source gas process, a first purge gas process, a reaction gas process, and a second purge gas process, respectively. may include a source gas process chamber 11 , a first purge process chamber 12 , a reaction gas process chamber 13 , and a second purge process chamber 14 .

For example, as shown in FIG. 2 , in the source gas process chamber 11 , a first powder inlet PI1 into which the powder 1 is introduced is formed on one upper side, and the powder 1 is formed on the other lower side. The first powder discharge port PO1 to be discharged is formed, and a first powder receiving space A1 inclined at a first angle K1 is formed therein, and the first powder receiving space A1 is formed. It may be a chamber for supplying the source gas (SG) to the powder (1).

In addition, for example, as shown in FIG. 2 , the first purge process chamber 12 is connected to the first powder outlet PO1 and a second powder inlet through which the powder 1 is introduced at an upper side. (PI2) is formed, a second powder discharge port PO2 through which the powder 1 is discharged is formed on the other side of the lower side, and a second powder receiving space A2 is formed to be inclined at a second angle K2 therein. This may be a chamber for supplying the purge gas PG, which is an inert gas such as argon or nitrogen, to the powder 1 accommodated in the second powder accommodation space A2.

In addition, for example, as shown in FIG. 2 , the reaction gas process chamber 13 is connected to the second powder outlet PO2 and a third powder inlet through which the powder 1 is introduced at an upper side ( PI3) is formed, a third powder discharge port PO3 through which the powder 1 is discharged is formed on the other side of the lower side, and a third powder receiving space A3 is formed to be inclined at a third angle K3 therein. It may be a chamber that is formed and supplies a reaction gas RG to the powder 1 accommodated in the third powder accommodation space A3 .

In addition, for example, as shown in FIG. 2 , the second purge process chamber 14 is connected to the third powder outlet PO3 and a fourth powder inlet through which the powder 1 is introduced at an upper side. (PI4) is formed, a fourth powder discharge port PO4 through which the powder 1 is discharged is formed on the other side of the lower side, and a fourth powder receiving space A4 is formed to be inclined at a fourth angle K4 therein. is formed, and may be a chamber for supplying a purge gas PG to the powder 1 accommodated in the fourth powder receiving space A4.

More specifically, for example, the source gas process chamber 11 , the first purge process chamber 12 , the reaction gas process chamber 13 , and the second purge process chamber 14 may include The powder outlet and the powder inlet of the adjacent chamber may be connected to each other and engaged to form a horizontal chamber assembly 101 that is connected in a line as a whole in a transverse direction, that is, in a front-rear direction.

Accordingly, by repeatedly arranging the four chambers in succession to increase the number of chambers to 8, 12, 16, etc., it is possible to significantly increase the processing capacity.

In addition, although not shown, individual temperature control devices optimized for each process are installed in each chamber, so that the yield can be dramatically increased by optimizing them individually, unlike the case in which the environment for each process is the same.

In particular, if these chambers are used, even if the powder remains in any one chamber, the thickness is not increased due to the characteristics of the atomic layer deposition, so that a uniform film quality can be obtained even when the residual powder is mixed.

In addition, for example, as shown in FIG. 2 , in the atomic layer deposition apparatus 100 for powder according to some embodiments of the present invention, the second purge process chamber ( 14) and a circulation line CL connecting the source gas process chamber 11 may be further included.

Accordingly, the powder 1 is prepared by using the source gas process chamber 11 , the first purge process chamber 12 , the reaction gas process chamber 13 , and the second purge process chamber 14 . An atomic layer may be formed through one cycle consisting of a source gas process, a first purge gas process, a reactive gas process, and a second purge gas process, and a plurality of atomic layers are circulated through the chambers using the circulation line CL. A multilayer atomic layer can be formed through a cycle.

Due to this, rather than performing the source gas process, the first purge gas process, the reactive gas process, and the second purge gas process using the valve control in one chamber, the source gas process is continuously performed without a valve in four chambers, 1 Since the primary purge gas process, the reactive gas process, and the secondary purge gas process can be continuously performed, an atomic layer can be rapidly and continuously deposited on a large amount of powder.

Therefore, it is possible to greatly increase the powder processing capacity by using a plurality of chambers inclined in the horizontal axis and connected to each other, and to greatly improve productivity by reducing the coating time, and can be used in various forms such as a horizontal chamber assembly and a vertical chamber assembly. It can be connected to reduce the limitation of the installation space, to optimize each of the four processes to improve the process characteristics by using four chambers that are individually performed, and to facilitate the repetition of the coating cycle in the powder circulation method. and can continuously coat a large amount of powder.

3 is a cross-sectional view illustrating the vertical chamber assembly 102 of the atomic layer deposition apparatus 100 for powder of FIG. 1 .

As shown in FIG. 3 , the source gas process chamber 11 , the first purge process chamber 12 , and the reaction of the atomic layer deposition apparatus 100 for powder according to some embodiments of the present invention The gas process chamber 13 and the second purge process chamber 14 are vertical chambers in which the powder outlet of the chamber and the powder inlet of the neighboring chamber are connected to each other and engaged, and are stacked and connected in a zigzag shape in the vertical direction. assembly 102 .

Therefore, by changing the size of individual chambers or selecting the horizontal chamber assembly 101 or the vertical chamber assembly 102, process time, productivity, and processing capacity can be adjusted as much as desired, and each process is separated and final Equipment can be built in various forms in various places according to the purpose, for example, the horizontal chamber assembly 101 can be applied to a building with a wide and low area, and the vertical chamber assembly 101 can be applied to a building with a narrow and high area ( 102) can be applied.

Although the present invention has been described with reference to the embodiments shown in the drawings, which are merely exemplary, those skilled in the art will understand that various modifications and equivalent other embodiments are possible therefrom. Therefore, the true technical protection scope of the present invention should be determined by the technical spirit of the appended claims.

According to some embodiments of the present invention made as described above, it is possible to greatly increase the powder processing capacity by using a plurality of chambers inclined to the horizontal axis and connected to each other, and to greatly improve productivity by reducing the coating time, It can be connected in various forms such as a horizontal chamber assembly and a vertical chamber assembly, thereby reducing the limitation of the installation space, and by optimizing each of the four processes, it is possible to improve the process characteristics by using four chambers that are individually performed. , it is possible to facilitate the repetition of the coating cycle in a powder cycle manner, and to coat a large amount of powder continuously.

Claims

A powder accommodating space in which the powder can be accommodated is formed, and the powder accommodating space is inclined so that the powder introduced through the powder inlet can be discharged to the powder outlet along an inclined surface, and the powder contains at least a source gas and a purge gas. , a chamber for supplying a gas made by selecting any one of the reaction gases; and

a stirring device installed in the chamber and stirring the powder;

Including, atomic layer deposition apparatus for powder.
The method of claim 1,

The chamber has an inclined cylindrical shape as a whole,

The powder inlet is formed on one side of the uppermost part of the outer peripheral surface of the chamber,

The powder outlet is formed in the lowermost part of the other side of the outer peripheral surface of the chamber,

A gas inlet is formed in the lower circular plane of the chamber,

Atomic layer deposition apparatus for powder, in which a pumping line is formed in the upper circular plane of the chamber.
The method of claim 1,

The chamber is

A first powder inlet through which the powder is introduced is formed on one upper side, a first powder outlet through which the powder is discharged is formed on the other side of the lower side, and a first powder receiving space inclined at a first angle is formed therein. , a source gas processing chamber for supplying a source gas to the powder accommodated in the first powder receiving space;

It is connected to the first powder outlet, and a second powder inlet through which the powder is introduced is formed on one upper side, and a second powder outlet through which the powder is discharged is formed on the other side of the lower side, and is inclined at a second angle therein. a first purge process chamber having a second powder accommodating space to be used and supplying a purge gas to the powder accommodated in the second powder accommodating space;

It is connected to the second powder outlet, and a third powder inlet through which the powder is introduced is formed on one upper side, and a third powder outlet through which the powder is discharged is formed on the other side of the lower side, and is inclined at a third angle. a reaction gas processing chamber having a third powder accommodating space to be formed and supplying a reactive gas to the powder accommodated in the third powder accommodating space; and

It is connected to the third powder outlet, and a fourth powder inlet through which the powder is introduced is formed on one side of the upper side, and a fourth powder outlet through which the powder is discharged is formed on the other side of the lower side, and is inclined at a fourth angle therein. a second purge process chamber having a fourth powder accommodating space and supplying a purge gas to the powder accommodated in the fourth powder accommodating space;

Including, atomic layer deposition apparatus for powder.
4. The method of claim 3,

The source gas process chamber, the first purge process chamber, the reaction gas process chamber, and the second purge process chamber are connected to each other and meshed with a powder outlet of a chamber and a powder inlet of an adjacent chamber in a forward and backward direction as a whole. Atomic layer deposition apparatus for powder, which is a horizontal chamber assembly connected to
4. The method of claim 3,

The source gas process chamber, the first purge process chamber, the reaction gas process chamber, and the second purge process chamber are connected to each other by a powder outlet of the chamber and a powder inlet of an adjacent chamber, and are engaged with each other, and have a zigzag shape as a whole. An atomic layer deposition apparatus for powder, which is a vertical chamber assembly that is stacked and connected in the vertical direction with a furnace.
4. The method of claim 3,

a circulation line connecting the second purge process chamber and the source gas process chamber to perform at least one process cycle;

Further comprising, an atomic layer deposition apparatus for powder.
The method of claim 1,

The stirring device is

an impeller rotated about an inclined stirring rotation shaft to transport the powder while mixing; and

a rotating device connected to the stirring rotating shaft to rotate the impeller;

Including, atomic layer deposition apparatus for powder.
8. The method of claim 7,

The impeller is at least a helical type, a ribbon type, a helical ribbon type, an anchor type, a turbine type, a propeller type, and made by selecting any one or more of combinations thereof, atomic layer deposition apparatus for powder.
The method of claim 1,

The powder is conveyed in a downward-facing downward direction in an inclined direction,

The gas is moved upward in an upward direction in an inclined direction, an atomic layer deposition apparatus for powder.