A method and device for continuously providing a precursor source

Abstract

The present invention provides a device for continuously providing a precursor source, comprising: a first source bottle connected to a reaction chamber, at least one first source bottle; a second source bottle connected to the first source bottle, at least one second source bottle; the first source bottle contains a precursor source, and the precursor source contained in the second source bottle is used to provide the first source bottle, so that the first source bottle continuously transports the precursor source into the reaction chamber. The present invention also provides a method for continuously providing a precursor source. The device provided by the present invention has a simple structure and is easy to maintain and use; the precursor source can continuously enter the reaction chamber, and the ALD, CVD and other vapor deposition equipment using the device can achieve continuous production with high production capacity, meeting the requirements of large-scale industrial continuous production of vapor phase equipment.

Description

Technical Field

[0001] The present invention relates to the field of thin film deposition, and in particular to a method and a device for continuously providing a precursor source. Background Art

[0002] In gas-phase reaction equipment such as ALD (atomic layer deposition) and CAD (chemical vapor deposition), it is usually necessary to transfer the precursor source to the reaction chamber for reaction. The precursor source is generally stored in a source bottle with limited storage capacity. In continuous industrial production or R&D activities, the source bottle needs to be frequently replaced to load the precursor source. Specifically, when the precursor source in the source bottle is used up or consumed, the equipment needs to be stopped to disassemble the source bottle and replace the source bottle to load the precursor source. This method fails to achieve a continuous supply of the precursor source and the continuous operation of the process, which greatly affects the mass production performance of the equipment.

[0003] For some precursor sources that are flammable and self-ignite when exposed to air, improper operation during the removal and replacement of the source bottle may cause risks such as fire, and the operation is relatively dangerous. For precursor sources with relatively low vapor pressure, since it is often necessary to heat the precursor source to increase its saturated vapor pressure, when replacing the source bottle, it is necessary to wait for a period of time after stopping the equipment until the temperature of the source bottle drops before operating the source bottle; after the source bottle is updated, the precursor source needs to be heated to a preset temperature before the equipment can be started for the deposition process, such as heating with a heating sleeve. The precursor source takes a long time to reach the preset temperature, that is, the loading of the precursor source has strict temperature requirements.

[0004] Therefore, it is necessary to provide a device and method to solve the above problems and ensure that the precursor source can be stably and continuously provided to the reaction chamber to improve the production capacity of the ALD equipment. Summary of the invention

[0005] The purpose of the present invention is to provide a method and device for continuously providing a precursor source, which can stably and continuously provide a precursor source to a reaction chamber, effectively improve the production capacity of the equipment, and meet the requirements of large-scale industrial continuous production of vapor deposition equipment such as ALD.

[0006] To achieve the above object, the present invention provides a device for continuously providing a precursor source, comprising:

[0007] A first source bottle connected to the reaction chamber, at least one first source bottle;

[0008] A second source bottle connected to the first source bottle, the second source bottle being at least one;

[0009] The first source bottle contains a precursor source, and the precursor source contained in the second source bottle is used to provide the first source bottle, so that the first source bottle continuously transports the precursor source into the reaction chamber.

[0010] Preferably, the device for continuously providing a precursor source further comprises: a precursor source vaporization chamber for vaporizing the precursor source, the precursor source vaporization chamber being connected to the first source bottle and the reaction chamber respectively.

[0011] Preferably, the first source bottle comprises: a precursor source storage chamber and a precursor source vaporization chamber, and the precursor source vaporization chamber is connected to the reaction chamber.

[0012] Preferably, the first source bottle is provided with at least one monitoring mechanism for monitoring the remaining amount of the precursor source in the first source bottle.

[0013] Preferably, the second source bottle is mounted on a movable mechanism.

[0014] Preferably, there are at least two second source bottles, and at least one of the at least two second source bottles is connected to the first source bottle.

[0015] Preferably, the device for continuously providing a precursor source further comprises: a connecting portion connected to the first source bottle and the second source bottle respectively, and a purge mechanism for a purge pipeline is provided on the connecting portion.

[0016] Preferably, the device for continuously providing a precursor source further comprises: a first heating protection mechanism, a second heating protection mechanism and a third heating protection mechanism for providing heat to the first source bottle, the second source bottle and the connecting part respectively.

[0017] Preferably, the device for continuously providing a precursor source is applied to a CVD device, an ALD device or other vapor deposition equipment.

[0018] The present invention also provides a method for continuously providing a precursor source, comprising: a first source bottle containing the precursor source provides the precursor source to a reaction chamber; a second source bottle containing the precursor source provides the precursor source to the first source bottle, so that the first source bottle continuously transports the precursor source to the reaction chamber.

[0019] Compared with the prior art, the present invention provides a method and device for continuously providing a precursor source, and the device has a simple structure and is easy to maintain and use; the purge mechanism module in the above-mentioned connecting part arranged in the device can effectively avoid the occurrence of transmission pipeline blockage; and the setting and use of the above-mentioned three heating protection mechanisms can better ensure that the precursor source stably and continuously enters the reaction chamber for reaction, and gas phase deposition equipment such as ALD and CVD can be continuously produced with high production capacity, meeting the requirements of large-scale industrial continuous production of gas phase equipment. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 A schematic diagram of a device for continuously providing a precursor source provided by one embodiment of the present invention.

[0021] Figure 2 A schematic diagram of a device for continuously providing a precursor source provided by one embodiment of the present invention.

[0022] Figure 3 A schematic diagram of a device for continuously providing a precursor source provided by one embodiment of the present invention.

[0023] Figure 4 A schematic diagram of a device for continuously providing a precursor source provided by one embodiment of the present invention.

[0024] Figure 5 A schematic diagram of a device for continuously providing a precursor source provided by one embodiment of the present invention.

[0025] Figure 6 A schematic diagram of a device for continuously providing a precursor source provided by one embodiment of the present invention.

[0026] Figure 7 A schematic diagram of a device for continuously providing a precursor source provided by one embodiment of the present invention.

[0027] Figure 8 A schematic diagram of a device for continuously providing a precursor source provided by one embodiment of the present invention.

[0028] Fig. 9 A schematic diagram of a device for continuously providing a precursor source provided by one embodiment of the present invention.

[0029] Among them, 1. reaction chamber, 2. first source bottle, 21. precursor source storage area, 22. precursor source vaporization area, 3. second source bottle, 4. precursor source vaporization mechanism, 5. connecting part, 6. purge mechanism, 7. moving mechanism, 8. monitoring mechanism. DETAILED DESCRIPTION

[0030] The following will be combined with the accompanying drawings of the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, other embodiments obtained by technicians in this field without creative work are all within the scope of protection of the present invention.

[0031] The present invention discloses a device for continuously providing a precursor source, comprising:

[0032] A first source bottle connected to the reaction chamber, at least one first source bottle;

[0033] A second source bottle connected to the first source bottle, the second source bottle being at least one;

[0034] The first source bottle contains a precursor source, and the precursor source contained in the second source bottle is used to provide the first source bottle, so that the first source bottle continuously transports the precursor source into the reaction chamber.

[0035] There is a sample to be deposited in the reaction chamber, and the precursor source may decompose or chemically react with one or some other substances on the deposited sample after entering the reaction chamber; the precursor source can be solid, liquid or gas.

[0036] The first source bottle is provided with an outlet, and the reaction chamber is provided with an inlet corresponding to the outlet, and the precursor source placed in the first source bottle flows into the reaction chamber through the pipeline between the outlet and the inlet. That is, the first source bottle is a source bottle that directly provides the precursor source to the reaction chamber.

[0037] The second source bottle connected to the first source bottle contains the same precursor source as the first source bottle. For example, if the precursor source contained in the first source bottle A is precursor source A, then the precursor source in the second source bottle A connected to the first source bottle A is also precursor source A. This is mainly to avoid cross contamination between precursor sources. However, in some special cases, according to process requirements, the first source bottle A and the second source bottle A can contain different precursor sources.

[0038] In addition, the structure formed by the first source bottle A and the second source bottle A can be repeatedly set up multiple times so as to deposit multiple thin films in the reaction chamber. For example, the structure formed by the first source bottle A and the second source bottle A is repeated twice, that is, there are two modules of the first source bottle A and the second source bottle A, and the first source bottle B and the second source bottle B. It is assumed that the precursor sources used in these two modules are different precursor sources A and precursor sources B, respectively. The reaction process occurring in the reaction chamber includes: connecting the precursor source A and the reaction chamber to react to form a thin film A of a preset thickness; disconnecting the precursor source A, and connecting the precursor source B and the reaction chamber at the same time to react to form a thin film B of a preset thickness. If three kinds of thin films need to be deposited, then three of the above modules are set; and so on.

[0039] During the use of the equipment, the intake state of the precursor source must be kept in a relatively stable balance. Assuming that all other conditions remain unchanged, the amount of the precursor source in the first source bottle must always be maintained above the preset lower limit. For example, it has been verified that the storage volume of the precursor source A in the first source bottle A cannot be less than 1 liter or the storage height cannot be less than 20 mm (relative to the plane where the lowest point of the first source bottle is located). At this time, the lower limit is 1 liter and 20 mm. When the precursor source A reaches this lower limit, the second source bottle A corresponding to the first source bottle A is connected, and the precursor source A contained in the second source bottle A enters the first source bottle A to supplement the precursor source A in the first source bottle A. In other words, the second source bottle A is a spare source bottle for the first source bottle A. The second source bottle A and the first source bottle A are used in conjunction with each other to ensure a sufficient amount of precursor source A. The precursor source A continuously enters the reaction chamber to achieve continuous production.

[0040] The first source bottle can be connected to multiple second source bottles, for example, the first source bottle A can be correspondingly connected to the second source bottles A1, A2, A3, etc. This embodiment can flexibly replace the second source bottle, but the disadvantage is that it occupies a large space volume.

[0041] In the relative placement of the first source bottle and the second source bottle, the two can be placed vertically up and down, or horizontally in the transverse direction. Preferably, the second source bottle is above the first source bottle to utilize the gravity of the precursor source to achieve smooth flow of the precursor source of the second source bottle to the first source bottle.

[0042] Furthermore, the device for continuously providing a precursor source also includes: a gasification mechanism for gasifying the precursor source, and the gasification mechanism is respectively connected to the first source bottle and the reaction chamber.

[0043] The precursor source used for vapor deposition generally exists in a liquid or solid phase under the atmospheric environment, but reacts in the reaction chamber in the gas phase. The precursor source can be vaporized at the moment of entering the reaction chamber, but preferably, the precursor source forms a gas phase before entering the reaction chamber, so a vaporization mechanism is provided between the precursor source leaving the source bottle and entering the reaction chamber.

[0044] It is worth noting that the gasification mechanism mentioned here can also have the function of catalytic gasification. For precursor sources with low working source temperature (for example, not higher than 300 degrees Celsius), the gasification method may only be heating them; but for some precursor sources with too high working source temperature, catalytic gasification may be required in addition to heating.

[0045] Furthermore, the first source bottle includes: a precursor source storage area and a precursor source gasification area, and the precursor source gasification area is connected to the reaction chamber.

[0046] The space occupied by the precursor source is the precursor source storage area, and the space not occupied by the precursor source is defined as the precursor source vaporization area; if the first source bottle is divided into two spaces according to the above definition, and the first source bottle is placed relatively horizontally, then the upper area of ​​the first source bottle is the precursor source vaporization area, and the lower area is the precursor source storage area; if the first source bottle is divided left and right relative to the horizontal plane, then the left side is the precursor source storage area, and the right side is the precursor source vaporization area, and vice versa. The vaporization direction is generally relatively upward, and preferably, the first source bottle is divided into an upper and lower structure.

[0047] In fact, there is no obvious boundary between the precursor source storage area and the precursor source vaporization area. For a liquid precursor source, the boundary between the precursor source storage area and the precursor source vaporization area is the liquid level of the precursor source.

[0048] Furthermore, the first source bottle is provided with at least one monitoring mechanism for monitoring the remaining amount of the precursor source in the first source bottle.

[0049] The monitoring mechanism can monitor the first source bottle, even in real time, so as to replenish the precursor source in time. The monitoring mechanism can be a liquid level meter; in consideration of cost, the monitoring mechanism can be an observation window set on the first source bottle to observe the amount of the precursor source in the first source bottle. Since the data on the remaining amount of the precursor source does not need to be very accurate, the preferred monitoring mechanism in this embodiment is an observation window set on the first source bottle.

[0050] At least one observation window. When only one observation window is used, the one observation window is preferably set at a position where the lower precursor source line can be easily observed; when there are two observation windows, they are preferably set at positions where the upper precursor source line (the maximum amount of the precursor source in the first source bottle) and the lower precursor source line can be easily observed. If more than three observation windows are selected, at least two of the three or more observation windows can monitor the upper precursor source line and the lower precursor source line.

[0051] Furthermore, the second source bottle is mounted on a movable mechanism.

[0052] When the precursor source of the second source bottle is completely replenished in the non-first source bottle, the precursor source needs to be added to the second source bottle to prepare for the next replenishment of the precursor source in the first source bottle. The precursor source supplier can directly go to the work site to fill the second source bottle without moving the second source bottle, which is difficult to achieve in actual production.

[0053] During actual use, the second source bottle is movable relative to the first source bottle. That is to say, when the second source bottle is empty, the second source bottle is taken out and replaced with another second source bottle filled with a precursor source. Since the source bottle is large in volume and heavy, repeated movement is not only inconvenient to operate, but may also damage other adjacent components in the device. In this embodiment, a movable mechanism is provided, which can be used as a supporting platform for the second source bottle at the same time, or it can be independent of the second source bottle (that is, the movable mechanism is used only when the second source bottle needs to be replaced).

[0054] Furthermore, the device for continuously providing a precursor source also includes: a connecting portion connected to the first source bottle and the second source bottle respectively, and a purge mechanism for a purge pipeline is provided on the connecting portion.

[0055] After the second source bottle transfers the precursor source to the first source bottle, the valve is closed to close the connection. Precursor sources inevitably remain in the connection. The residual precursor source is adsorbed and condensed on the pipeline in the connection. If it is not completely removed, long-term accumulation will cause pipeline blockage. In this embodiment, a purge mechanism is used to purge the connection part that is transported to the precursor source each time, effectively solving the blockage problem caused by the condensation of the residual precursor source.

[0056] Furthermore, the device for continuously providing a precursor source also includes: a first heating protection mechanism, a second heating protection mechanism and a third heating protection mechanism for providing heat to the first source bottle, the second source bottle and the connecting part respectively.

[0057] During use, the precursor source in the first source bottle needs to reach temperature T1, the connection part needs to reach temperature T2, and the precursor source in the second source bottle needs to reach temperature T3; T1≥T2≥T3, T1 should make the precursor source have good volatility. T1≥T2≥T3 has two effects: one is to shorten the temperature difference of the precursor source from the second source bottle to the first source bottle; the other is to avoid condensation of the precursor source during the entire transmission process.

[0058] Preferably, there are at least two second source bottles, and at least one of the at least two second source bottles is connected to the first source bottle.

[0059] At least two second source bottles can further ensure the replenishment of the precursor source in the first source bottle; at least one second source bottle contains a precursor source; at least two second source bottles can be partially connected in series and partially connected in parallel, or at least two second source bottles are directly connected to the first source bottle. Specifically, in one embodiment, there are 5 second source bottles, namely s1, s2, s3, s4 and s5, wherein s1 and s2 are connected in series to form s12, s3, s4 and s5 are connected in series to form s345, and s12 and s345 are connected in parallel, any one of s1 and s2 is connected to the first source bottle, and any one of s3, s4 and s5 is connected to the first source bottle. In another embodiment, s1 and s2 are both connected to the first source bottle.

[0060] Preferably, the device for continuously providing a precursor source is applied to a CVD device, an ALD device or other vapor deposition equipment.

[0061] The present invention also discloses a method for continuously providing a precursor source, comprising: a first source bottle containing the precursor source provides the precursor source to a reaction chamber; a second source bottle containing the precursor source provides the precursor source to the first source bottle, so that the first source bottle continuously transports the precursor source to the reaction chamber.

[0062] Preferably, in order to ensure that the precursor source stored in the first source bottle is sufficient to be provided to the reaction chamber for action, a lower limit is preset on the first source bottle, and the amount of the precursor source needs to be ensured to be no less than the above lower limit.

[0063] More preferably, in order to prevent the amount of the precursor source in the first source bottle from being too much and causing the first source bottle to be unable to provide the precursor source to the reaction chamber, an upper shear line is preset on the first source bottle relative to the lower shear line. During the reaction, the amount of the precursor source is preferably between the preset lower shear line and the upper shear line (including the lower shear line and the upper shear line). When the precursor source in the first source bottle is reduced to the lower shear line, the precursor source in the second source bottle connected to the first source bottle is provided to the first source bottle until the precursor source in the first source bottle does not exceed the upper shear line, so that the first source bottle continuously transports the precursor source to the reaction chamber.

[0064] Considering the actual use requirements, the plane where the first source bottle is located at the lowest position relative to its placement position is defined as L est The plane where the lower insulator is located on the first source bottle is defined as D est , D est With L est The difference between them shall not be less than 20 mm.

[0065] The present invention is further described below through specific examples.

[0066] Embodiment 1

[0067] like Figure 1As shown, the device for continuously providing a precursor source in this embodiment comprises: a reaction chamber 1, a first source bottle 2 and a second source bottle 3, wherein the first source bottle 2 is connected to the reaction chamber 1 via a first pipeline, and the second source bottle 3 is connected to the first source bottle 2 via a second pipeline; a valve for controlling the precursor source in the first source bottle 2 to enter the reaction chamber 1 is provided on the first pipeline, and a valve for controlling the precursor source in the second source bottle 3 to enter the first source bottle 2 is provided on the first pipeline,

[0068] When the above-mentioned equipment is in use, the precursor source in the first source bottle 2 enters the reaction chamber 1 where the sample to be deposited is placed for reaction; the second source bottle 3 replenishes the precursor source to the first source bottle 2 to ensure that the precursor source is continuously delivered into the reaction chamber for continuous deposition on the sample to be deposited to form a thin film.

[0069] Embodiment 2

[0070] like Figure 2 As shown, the device for continuously providing a precursor source in this embodiment further includes a precursor source gasification mechanism 4 in the first embodiment, which is suitable for the scenario where the precursor source corresponding to the deposited material has poor volatility and it is difficult to meet the requirements only by heating. In addition, a carrier gas channel (not shown) can be provided on the precursor source gasification mechanism to bring the precursor source out and into the reaction chamber 1.

[0071] Embodiment 3

[0072] like Figure 3 As shown, the device for continuously providing a precursor source in this embodiment is optimized on the basis of the first embodiment. The first source bottle 2 is configured to include a precursor source storage area 21 and a precursor source vaporization area 22. The precursor source in the precursor source storage area 21 is vaporized to form a precursor source gas, and the precursor source vaporization area 22 is a space for storing the precursor source gas. The precursor source enters the reaction chamber 1 in the form of gas to react.

[0073] Embodiment 4

[0074] like Figure 4 As shown, the device for continuously providing a precursor source in this embodiment further includes a connecting portion 5 and a purge mechanism 6 on the basis of the first embodiment, and the pipeline is purged to prevent the precursor source from condensing in the pipeline and blocking the pipeline.

[0075] Embodiment 5

[0076] like Figure 5 The device shown for continuously providing precursor sources includes three different precursor sources (precursor sources A, B and C), which can deposit thin films of at least three different materials and can also be used to deposit laminated materials.

[0077] Figure 6 Another method of depositing thin films of various materials is shown.

[0078] Example 6

[0079] Figure 7 and Figure 8 The device for continuously providing a precursor source includes a moving mechanism 7 for carrying and moving the second source bottle 3 to facilitate replacement of the second source bottle 3 .

[0080] Figure 7 The second source bottle 3 is vertically arranged relative to the first source bottle 2, Figure 8 The second source bottle 3 is arranged horizontally relative to the first source bottle 2.

[0081] Example 7

[0082] Fig. 9 The device for continuously providing the precursor source shown includes a monitoring mechanism 8. In this embodiment, the monitoring mechanism 8 is configured as an observation window 81 for monitoring the upper limit of the precursor source and an observation window 82 for monitoring the lower limit of the precursor source. When the precursor source rises to the observation window 81, the addition of the precursor source to the first source bottle 2 is stopped; when the precursor source drops to the observation window 82, the precursor source needs to be added to the first source bottle 2.

[0083] In this embodiment, the lower insulator line is located at a plane 20 mm away from the lowest position of the first source bottle.

[0084] Compared with the prior art, the present invention provides a method and device for continuously providing a precursor source, and the device has a simple structure and is easy to maintain and use; the purge mechanism module in the above-mentioned connecting part arranged in the device can effectively avoid the occurrence of transmission pipeline blockage; and the setting and use of the above-mentioned three heating protection mechanisms can better ensure that the precursor source stably and continuously enters the reaction chamber for reaction, and gas phase deposition equipment such as ALD and CVD can be continuously produced with high production capacity, meeting the requirements of large-scale industrial continuous production of gas phase equipment.

[0085] The above contents are merely examples and explanations of the present invention. Those skilled in the art may make various modifications or additions to the specific embodiments described or replace them with similar methods. As long as they do not deviate from the invention or exceed the scope defined by the claims, they shall all fall within the protection scope of the present invention.

Claims

1. A device for continuously providing a precursor source, characterized in that: include: A first source bottle connected to the reaction chamber, wherein the first source bottle is at least one; a second source bottle connected to the first source bottle, wherein the second source bottle is at least one; A connecting portion connected to the first source bottle and the second source bottle respectively, wherein a purge mechanism for a purge pipeline is provided on the connecting portion; A first heating protection mechanism, a second heating protection mechanism and a third heating protection mechanism for respectively providing heat to the first source bottle, the second source bottle and the connecting portion; The first source bottle contains a precursor source, and the precursor source contained in the second source bottle is used to be provided to the first source bottle, so that the first source bottle continuously transports the precursor source into the reaction chamber; The temperature of the precursor source in the first source bottle reaches at least a first temperature T1, the temperature of the connecting part reaches at least a second temperature T2, and the temperature of the precursor source in the second source bottle reaches at least a third temperature T3; and the first temperature T1 ≥ the second temperature T2 ≥ the third temperature T3, and the first temperature T1 makes the precursor source have good volatility.

2. The device according to claim 1, characterized in that Also includes: A precursor source gasification chamber is used for gasifying a precursor source, and the precursor source gasification chamber is connected to the first source bottle and the reaction chamber respectively.

3. The device according to claim 1, characterized in that The first source bottle comprises: a precursor source storage chamber and a precursor source gasification chamber, and the precursor source gasification chamber is connected to the reaction chamber.

4. The device according to claim 1, characterized in that The first source bottle is provided with at least one monitoring mechanism for monitoring the remaining amount of the precursor source in the first source bottle.

5. The device according to claim 1, characterized in that The second source bottle is mounted on a movable mechanism.

6. The device according to claim 1, characterized in that There are at least two second source bottles, and at least one of the at least two second source bottles is connected to the first source bottle.

7. The device according to any one of claims 1 to 6, characterized in that The device is applied to CVD equipment, ALD equipment or other vapor deposition equipment.

8. A method for continuously providing a precursor source, applied to the device for continuously providing a precursor source according to claim 1, characterized in that: The first source bottle containing the precursor source provides the precursor source to the reaction chamber; the second source bottle containing the precursor source provides the precursor source to the first source bottle, so that the first source bottle continuously transports the precursor source to the reaction chamber.

Images