Solid-state precursor delivery device with microchannels and delivery method

Abstract

The present invention provides a solid precursor delivery device with a microchannel and a delivery method. A partition for carrying a solid precursor, which can be installed in a matching manner with the tray, is arranged in the tray. The partition has a partition microchannel inside, an air inlet of the partition communicating with the partition microchannel is provided on the bottom surface of the partition, and an air outlet of the partition communicating with the partition microchannel is provided on the surface of the partition. After installation, the partition has an included angle with the bottom of the tray and the bottom surface of the installed partition contacts the bottom of the tray. The air inlet of the partition communicates with the air outlet of the tray, and the air outlet of the partition communicates with the reaction cavity to form an air outlet channel, so as to increase the contact area between the solid precursor and the gas and extend the contact time to meet the application requirements.

Description

Technical Field

[0001] The present invention belongs to the technical field of integrated circuits, and relates to a solid precursor delivery device with microchannels and a delivery method. Background Art

[0002] Atomic layer deposition (ALD) technology is a type of chemical vapor deposition. Different from other chemical vapor deposition technologies, in ALD, gaseous precursors are alternately introduced into the reaction chamber, and a single atomic layer thin film covering the substrate surface is formed through chemisorption reactions on the substrate surface. This special thin film growth method endows ALD with excellent three-dimensional conformality, large-area deposition uniformity, and the ability to control film thickness with sub-atomic layer precision in high aspect ratio structures. These advantages have made ALD widely used in advanced integrated circuit processes, such as Fin-FET, GAA transistors, etc.

[0003] The ALD deposition process consists of alternately occurring self-saturating surface adsorption and chemical reactions. After the precursor reaches the surface of the deposition substrate, the precursor and the substrate will undergo chemisorption and surface reactions until it automatically terminates when the surface is saturated. The surface reaction has self-limiting properties, and continuously repeating this self-limiting reaction can form a thin film. And between precursor pulses, an inert gas is needed to effectively clean the atomic layer deposition reactor. A basic atomic layer deposition cycle includes 4 steps:

[0004] (1) Pulse the first gaseous precursor onto the substrate surface and undergo chemisorption on the surface;

[0005] (2) Introduce a cleaning gas to remove the extra unreacted precursors;

[0006] (3) Pulse the second gaseous precursor onto the substrate surface and generate the required thin film material through surface reactions;

[0007] (4) Introduce a cleaning gas to remove the by-products of the reaction.

[0008] By continuously repeating the above deposition cycle until the desired thin film thickness is obtained.

[0009] From the principle of ALD deposition, it can be seen that the ALD deposition rate is closely related to the chemisorption rate of the reactants on the substrate. If a single atomic layer covering the entire substrate surface is to be formed in one cycle, a sufficient long reactant pulse time is required to achieve saturated adsorption. At this time, the ALD growth rate reaches saturation with the increase of the pulse time, as shown in the appendix Figure 2For the same precursor, the rate of chemisorption depends on the partial pressure of the precursor. To increase the yield of the ALD process, the shorter the pulse time required for the ALD growth rate to reach saturation, the better. Therefore, it is desired that the precursor can maintain its saturated vapor pressure during multiple pulses in the deposition process. At this time, the content of the precursor carried in the pulse is the highest, and the adsorption rate on the substrate surface is also the highest, as Figure 1 (a). In actual situations, the partial pressure of the precursor depends not only on the ALD process menu but also has a close relationship with the design of the ALD precursor delivery device. If the vaporization rate of the precursor is lower than the rate at which the precursor flows out of the delivery device with the carrier gas, the partial pressure of the precursor cannot be maintained at the saturated vapor pressure, as Figure 1 (b). As the pulse time increases, the decrease in the precursor partial pressure is more obvious, as Figure 1 (c). At the same time, the shortening of the pulse interval reduces the time for the gaseous precursor in the delivery device to be replenished, which may also cause the partial pressure of the precursor to no longer be able to be maintained at the saturated vapor pressure as the number of pulses increases, as Figure 1 (d). All of the above situations will lead to an increase in the pulse time required for the deposition rate to reach saturation, and at the same time, the saturated deposition rate may decrease, thus affecting the yield of the ALD process, as Figure 2 .

[0010] ALD precursors can be classified into three types according to their physical states under normal conditions: solid, liquid, and gas. Since the precursor needs to enter the reaction chamber in the gas phase, for solid and liquid precursors, the commonly used method is to use carrier gases such as N2 to carry the precursor into the reaction chamber in the gas phase. For liquid and solid precursors, the designs of their delivery devices are quite different. The liquid precursor delivery device usually adopts the form of a Bubbler, that is, the carrier gas is directly introduced into the bottom of the liquid precursor. During the rising process of the bubbles, there is enough time for sufficient mass exchange between the carrier gas and the liquid-phase precursor, so that the partial pressure of the precursor in the bubbles reaches the saturated vapor pressure. At the same time, since the contact area between the liquid precursor and the gas above the liquid surface does not change as the precursor is consumed and the liquid level drops, the rate of replenishment of the gaseous precursor is less affected by the consumption of the precursor. In contrast, it is more difficult to stabilize the partial pressure of the gaseous precursor of the solid precursor at the saturated vapor pressure, and more factors need to be considered when designing the delivery device. The delivery device for solid precursors needs to ensure that the contact area between the solid precursor and the carrier gas is as large as possible and the contact time is as long as possible, so that the gaseous precursor carried away by the carrier gas can be quickly replenished, thus maintaining the system in a quasi-equilibrium state where the partial pressure of the precursor is close to its saturated vapor pressure during the precursor pulse time.

[0011] Most of the existing solid - state precursor delivery devices use stacked trays and place the precursors at the bottom of the trays to enable the precursors to contact the gas phase. However, the surface area through which the carrier gas flows and the residence time in this delivery device are still difficult to meet the requirements. Therefore, it is necessary to provide a solid - state precursor delivery device and a delivery method with microchannels. Summary of the Invention

[0012] In view of the above - mentioned disadvantages of the prior art, the purpose of the present invention is to provide a solid - state precursor delivery device and a delivery method with microchannels, which are used to solve the problem that the existing solid - state precursor delivery device is difficult to meet the application requirements.

[0013] To achieve the above - mentioned purpose and other related purposes, the present invention provides a solid - state precursor delivery device with microchannels, which includes a housing, a gas source hole and an exhaust hole located on the housing. The solid - state precursor delivery device further includes:

[0014] A tray disposed inside the housing, the tray includes a tray side wall and a tray bottom, the tray bottom and the tray side wall form a reaction cavity, a tray air inlet and a tray air outlet penetrating through the tray bottom are arranged on the tray bottom, the tray air inlet is connected to the gas source hole to form an air inlet channel, and the tray has a first mounting part;

[0015] A partition board, the partition board has a second mounting part, and the partition board is installed in the reaction cavity by assembling the second mounting part with the first mounting part. The partition board has a partition microchannel inside, and a partition air inlet connected to the partition microchannel is arranged on the bottom surface of the partition board, a partition air outlet connected to the partition microchannel is arranged on the surface of the partition board, and after installation, the partition board and the tray bottom form an angle, and the bottom surface of the installed partition board is in contact with the tray bottom. The partition air inlet is connected to the tray air outlet, the partition air outlet is connected to the reaction cavity, and the reaction cavity is connected to the exhaust hole to form an air outlet channel. The partition board bears the solid - state precursor.

[0016] Optionally, the range of the angle θ formed by the installed partition board and the tray bottom is 0° < θ ≤ 90°.

[0017] Optionally, the inside of the housing includes a plurality of stacked trays. The tray air inlets in the stacked trays are communicated with each other and connected to the gas source hole to form an air inlet channel. The partition microchannels in adjacent trays are communicated. The reaction cavity of the uppermost tray is connected to the exhaust hole for exhausting; the side surface of the installed partition board is in contact with the tray side wall.

[0018] Optionally, the partition air outlets located on the same partition are annularly distributed; the partition air outlets in adjacent partitions on the left and right are staggeredly arranged.

[0019] Optionally, the stacked partitions have an included angle.

[0020] Optionally, the assembly method of the first mounting portion and the second mounting portion includes snap-fit assembly. The first mounting portion is a groove and the second mounting portion is a corresponding protrusion, or the first mounting portion is a protrusion and the second mounting portion is a corresponding groove.

[0021] Optionally, the partition includes one or a combination of a flat plate and a curved plate; the partition is a metal partition with a sandblasted surface.

[0022] Optionally, it further includes a heating element, and the heating method of the heating element includes one or a combination of contact heating and radiation heating.

[0023] The present invention also provides a method for transporting a solid precursor with a microchannel, including the following steps:

[0024] Provide any one of the above solid precursor transport devices;

[0025] Place the solid precursor on the partition;

[0026] Assemble the partition on the tray and place it in the reaction cavity;

[0027] Stack and assemble the trays in the housing of the solid precursor transport device, and close the solid precursor transport device after assembly.

[0028] Optionally, the solid precursor includes a metal halide solid precursor; the method of placing the solid precursor on the partition includes a physical coating method, a sublimation crystallization method, or a chemical reaction method.

[0029] As described above, for the solid precursor transport device and transport method with a microchannel of the present invention, a partition that can be matched and installed with the tray and is used to carry the solid precursor is provided in the tray, and the partition has a partition microchannel. The bottom surface of the partition has a partition air inlet connected to the partition microchannel, and the surface of the partition has a partition air outlet connected to the partition microchannel. After installation, the partition and the bottom of the tray have an included angle and the bottom surface of the partition after installation is in contact with the bottom of the tray. The partition air inlet is connected to the tray air outlet and the partition air outlet is connected to the reaction cavity to form an air outlet channel, so as to increase the contact area between the solid precursor and the gas and extend the contact time to meet the application requirements. Description of the Drawings

[0030] Figure 1 Shown are four possible variations of the precursor partial pressure with consecutive output precursor pulses.

[0031] Figure 2 Shown is the variation of the average deposition rate per pulse of ALD with the pulse time under different pulse states.

[0032] Figure 3 Shown is a top view structural schematic diagram after the tray and the partition in Example 1 are assembled.

[0033] Figure 4 Shown as Figure 3 The cross-sectional structural schematic diagram along A-A'.

[0034] Figure 5 Shown as Figure 3 The cross-sectional structural schematic diagram along B-B' in

[0035] Figure 6 Shown is the cross-sectional structural schematic diagram of the assembled solid precursor delivery device in Example 1.

[0036] Figure 7 Shown is another top view structural schematic diagram after the tray and the partition in Example 1 are assembled.

[0037] Figure 8 Shown is yet another top view structural schematic diagram after the tray and the partition in Example 1 are assembled.

[0038] Figure 9 Shown is a top view structural schematic diagram after the tray and the partition in Example 2 are assembled.

[0039] Figure 10 Shown as Figure 9 The cross-sectional structural schematic diagram along A-A'.

[0040] Figure 11 Shown as Figure 9 The cross-sectional structural schematic diagram along B-B' in

[0041] Figure 12 Shown is the cross-sectional structural schematic diagram of the assembled solid precursor delivery device in Example 2.

[0042] Description of component labels

[0043] 110, 120 trays

[0044] 111, 121 tray air inlets

[0045] 112, 122 tray air outlets

[0046] 113, 123 reaction cavities

[0047] Partition plates 210 and 220

[0048] Partition microchannels 211 and 221

[0049] Partition air outlets 212 and 222

[0050] Housings 310 and 320

[0051] Gas source holes 311 and 321

[0052] Exhaust holes 312 and 322

[0053] Angle θ Specific implementation manners

[0054] The following uses specific specific examples to illustrate the implementation manners of the present invention. Those skilled in the art can easily understand other advantages and effects of the present invention from the content disclosed in this specification. The present invention can also be implemented or applied through other different specific implementation manners. Various details in this specification can also be modified or changed based on different viewpoints and applications without departing from the spirit of the present invention.

[0055] When detailing the embodiments of the present invention, for the convenience of description, the sectional views will be enlarged or reduced locally in a non - general proportion, and the schematic diagrams are only examples, and they should not limit the scope of protection of the present invention here.

[0056] For the convenience of description, spatial relationship terms such as "beneath", "below", "lower than", "under", "above", "on" etc. may be used here to describe the relationship between one element or feature shown in the drawings and other elements or features. It will be understood that these spatial relationship terms are intended to include other directions of the device in use or operation, in addition to the directions depicted in the drawings. And as in the context of this application, the structure where the first feature is "above" the second feature may include embodiments where the first and second features are formed in direct contact, and may also include embodiments where additional features are formed between the first and second features, that is, the first and second features may not be in direct contact.

[0057] It should be noted that the diagrams provided in this embodiment only illustrate the basic concept of the present invention schematically. Therefore, only the components related to the present invention are shown in the diagrams, rather than being drawn according to the number, shape, and size of the components in actual implementation. The type, quantity, and ratio of each component in its actual implementation can be arbitrarily changed, and the component layout type may also be more complex.

[0058] Embodiment 1

[0059] Refer to Figures 3 to 6, this embodiment provides a solid precursor delivery device with a microchannel. The solid precursor delivery device includes a housing 310, a gas source hole 311 and an exhaust hole 312 located on the housing 310. The solid precursor delivery device further includes a tray 110 and a partition 210. In this embodiment, taking the example that there are 4 trays 110 stacked from bottom to top in the housing 310, but the number of trays 110 contained in the housing 310 is not limited thereto. For example, the housing 310 may also include 1, 2 or more trays 110, and the specific number is not defined here. Among them, the tray 110 includes a tray side wall and a tray bottom. The tray bottom and the tray side wall form a reaction cavity 113. A tray air inlet 111 and a tray air outlet 112 penetrating the tray bottom 110 are provided on the tray bottom. The tray air inlets 111 in the stacked trays 110 are connected and communicate with the gas source hole 311 to form an air inlet channel, and the tray 110 has a first mounting portion (not shown); the partition 210 has a second mounting portion (not shown), and the partition 210 is installed in the reaction cavity 113 by assembling the second mounting portion with the first mounting portion. The partition 210 has a partition microchannel 211, and the bottom surface of the partition 210 has a partition air inlet (not shown) communicating with the partition microchannel 211. The surface of the partition 210 has a partition air outlet 212 communicating with the partition microchannel 211. After installation, the partition 210 and the tray bottom form an included angle θ, and the bottom surface of the installed partition 210 is in contact with the tray bottom. The partition air inlet is communicated with the tray air outlet 112, the partition air outlet 212 is communicated with the reaction cavity 113, and the reaction cavity 113 is communicated with the exhaust hole 312 to form an air outlet channel. The partition 210 carries the solid precursor.

[0060] Specifically, such as Figure 6, in this embodiment, the solid precursor delivery device internally includes 4 stacked trays 110, but the stacking number of the trays 110 is not limited to this and can be selected according to needs; the tray 110 is composed of a side wall and a bottom to form a cylindrical appearance with the reaction cavity 113, but the morphology of the tray 110 is not limited to this; in the same solid precursor delivery device, the trays 110 can adopt the same morphology or different morphologies, such as having the same side wall height, the same width or different side wall heights, different widths, etc.; an intake gas pipeline is provided at the bottom of the tray 110 to serve as the tray intake port 111, and the tray intake ports 111 in the upper and lower layers are connected to form an intake gas channel; an exhaust gas pipeline is provided at the bottom of the tray 110 to serve as the tray exhaust port 112. The partition 210 has the partition microchannel 211, the partition intake port, and the partition exhaust port 212. After the partition 210 is assembled into the reaction cavity 113, the tray exhaust port 112, the partition intake port, the partition microchannel 211, the partition exhaust port 212, and the reaction cavity 113 are connected to form an exhaust gas channel. Regarding the settings of the tray intake port 111, the tray exhaust port 112, the partition microchannel 211, the partition intake port, and the partition exhaust port 212, no excessive restrictions are made here, as long as the carrier gas can operate in each reaction cavity 113.

[0061] Among them, it is preferred that the carrier gas flows in a "bottom-up" mode, such as Figure 6 shows the flow trajectory of the carrier gas in the stacked trays 110 installed in the housing 310 in this embodiment. After the carrier gas is introduced from the top "top-down" along the tray intake port 111 into the lower region, a space communicating with the tray intake port 111, such as a pipeline, etc., can be provided at the bottom of the housing 310. The carrier gas is introduced "bottom-up" into the corresponding reaction cavities 113 of each layer of the tray 110 through the tray exhaust port 112, the partition intake port, the partition microchannel 211, and the partition exhaust port 212.

[0062] The solid precursor attached to the inner wall of the partition 210 can fully exchange substances with the gas. Finally, the carrier gas is discharged from the top. By setting the partition 210 with an included angle θ with the bottom of the tray 110, the contact area and contact time between the carrier gas and the solid precursor can be enlarged within the same space of the reaction cavity 113.

[0063] Further, according to needs, the inner wall of the tray 110 can also be attached with a solid precursor.

[0064] Among them, the adjacent two layers of the stacked trays 110 can be in direct contact, or an O-ring seal or the like can be placed between them for sealed connection; similarly, the tray air inlets 111 between adjacent upper and lower layers can also be in direct contact or an O-ring seal or the like can be placed for sealed connection.

[0065] As an example, the range of the angle θ formed between the bottom of the installed partition 210 and the tray 110 can be 0° < θ ≤ 90°.

[0066] Specifically, referring to Figure 4 , in this embodiment, the angle θ formed between the bottom of the partition 210 and the tray 110 is 90°, that is, the partition 210 is perpendicular to the bottom of the tray 110, but it is not limited thereto. In another embodiment, the partition 210 and the bottom of the tray 110 can also be inclined, that is, the angle θ can also be, for example, 30°, 45°, 60°, etc., which will not be introduced here for the time being.

[0067] As an example, the side surface of the installed partition 210 is in contact with the side wall of the tray.

[0068] Specifically, when the installed partition 210 is in contact with the side wall of the tray, the contact area between the partition 210 and the tray 110 can be increased, thereby facilitating heat transfer, especially the heating of the solid precursor delivery device in the form of contact heat transfer.

[0069] As an example, the partition air outlets 212 on the same partition 210 are annularly distributed.

[0070] Specifically, one tray air inlet 111 and multiple tray air outlets 112 can be provided on the bottom of the same tray 110, and the tray air inlet 111 can be located at the center of the tray 110. The multiple tray air outlets 112 can be located outside the tray air inlet 111 and be annularly distributed. The adjacent upper and lower tray air outlets 112 and the center of the bottom of the tray 110 can have different or the same spacing; the partition air inlets on the same partition 210 can be correspondingly arranged with the tray air outlets 112, and the partition air outlets 212 on the surface of the partition 210 can be annularly distributed, but the number, distribution, morphology, etc. of the tray air inlet 111, the tray air outlets 112, the partition air inlets, the partition microchannels 211, and the partition air outlets 212 are not limited thereto. Further, the partition air outlets 212 in the adjacent left and right partitions 210 can be staggered to extend the gas transmission path as much as possible.

[0071] As an example, the partition 210 can include one or a combination of a flat plate and a curved plate.

[0072] Specifically, referring to Figure 3 illustrates the case where the partition 210 is a flat plate. Among them, the partitions 210 in the same layer are arranged in parallel; Figure 7 illustrates another case where the partition 210 combines a curved plate and a flat plate; Figure 8 illustrates yet another case where the partition 210 is a flat plate and the partitions 210 in the same layer are parallel and cross - arranged, but not limited thereto. For example, the partition 210 can also be a corrugated plate, etc.

[0073] Among them, the distance between adjacent partitions 210 in the same layer can be less than the radius of the bottom of the tray 110. The spacing between the partitions 210 in the same layer can be the same or different. There is no excessive limitation on the morphology, quantity, and distribution of the partition 210 here, and it can be flexibly selected.

[0074] As an example, the partition 210 can be a metal partition or a metal alloy partition with a sand - blasted surface.

[0075] Specifically, for the convenience of the attachment of the solid precursor, it is preferred that the partition 210 is a partition with a sand - blasted surface, but not limited thereto. Other surface treatment methods can also be adopted to ensure that the solid precursor is adsorbed on the surface of the partition 210.

[0076] Among them, for the convenience of heat conduction, it is preferred that the material of the partition 210 is metal, such as 304 stainless steel, 316 stainless steel, etc. Of course, the material of the partition 210 can also be selected from other materials that do not react with the solid precursor being transported. The material and surface treatment method of the partition 210 can be set according to needs and are not limited here.

[0077] As an example, the assembly method of the first mounting part and the second mounting part can include snap - fit assembly. For example, the first mounting part is a groove and the second mounting part is a corresponding protrusion, or the first mounting part is a protrusion and the second mounting part is a corresponding groove.

[0078] In this embodiment, as Figure 4 and Figure 5 , grooves (not shown) can be opened on the side wall and / or the bottom of the tray 110. The partition 210 with the solid precursor attached to its surface is inserted into the groove to complete the assembly of the partition 210 and the tray 110.

[0079] Among them, the length of the groove may be the same as the height of the side wall of the tray 110, or may be less than the height of the side wall of the tray 110. The lengths of different grooves in the same tray 110 may be the same or different. Preferably, the groove is in close contact with the partition 210 to better transfer heat. The types of the first mounting portion and the second mounting portion are not limited thereto according to needs.

[0080] As an example, a heating element (not shown) may further be included, and the heating method of the heating element may include one or a combination of contact heating and radiation heating.

[0081] Specifically, a heating element may be provided outside the housing 310 of the solid precursor delivery device according to needs to meet the temperature requirements for heating the solid precursor. Among them, the heating method may include one or a combination of contact heating and radiation heating, and no excessive limitation is made here.

[0082] Embodiment 2

[0083] Refer to Figures 9 to 12 , this embodiment provides another solid precursor delivery device with a microchannel. The solid precursor delivery device includes a housing 320, a gas source hole 321 and an exhaust hole 322 located on the housing 320. The solid precursor delivery device further includes a tray 120 and a partition 220. In this embodiment, taking the housing 320 having 4 trays 120 stacked from bottom to top as an example, the number of the trays 120 contained in the housing 320 is not limited thereto. For example, the housing 320 may also include 1, 2 or more trays 120, and the specific number is not limited here. The main difference between the solid precursor delivery device in this embodiment and the solid precursor delivery device in Embodiment 1 is that: the partition 220 is inclined in the tray 120, that is, the included angle θ between the partition 220 and the bottom of the tray 120 is an acute angle, such as Figure 9 , Figure 10 , Figure 12 shown.

[0084] Specifically, such as Figures 9 to 12, the tray 120 includes a tray sidewall and a tray bottom, the tray bottom and the tray sidewall form a reaction cavity 123, a tray air inlet 121 and a tray air outlet 122 penetrating through the tray bottom 120 are arranged on the tray bottom, the tray air inlets 121 in the stacked trays 120 are communicated with each other and connected with the gas source hole 321 to form an air inlet passage, and the tray 120 has a first mounting portion; the partition 220 has a second mounting portion, and the partition 220 is mounted in the reaction cavity 123 by assembling the second mounting portion and the first mounting portion. The partition 220 has a partition microchannel 221, and a partition air inlet (not shown) communicating with the partition microchannel 221 is arranged on the bottom surface of the partition 220. A partition air outlet 222 communicating with the partition microchannel 221 is arranged on the surface of the partition 220. After installation, the partition 220 and the tray bottom form an included angle θ, and the bottom surface of the installed partition 220 is in contact with the tray bottom. The partition air inlet is communicated with the tray air outlet 122, the partition air outlet 222 is communicated with the reaction cavity 123, and the reaction cavity 123 is communicated with the exhaust hole 322 to form an air outlet passage. The partition 220 bears the solid precursor.

[0085] Only the differences between this embodiment and the first embodiment will be introduced below. The same parts as those in the first embodiment will not be elaborated here and can be referred to the first embodiment.

[0086] Such as Figure 10 , in this embodiment, the included angle θ formed by the installed partition 220 and the bottom of the tray 120 is 0° < θ < 90°, such as 30°, 45°, 60°, etc., which can be specifically set according to needs. In this embodiment, the inclined partition 220 can further extend the gas transmission path to extend the contact time between the gas and the solid precursor.

[0087] Furthermore, such as Figure 12 , the partitions 220 in the upper and lower layers can have a certain included angle, such as 15°, 30°, 45°, 60°, etc., to flexibly set the position of the partition 220, so as to further increase the gas transmission path.

[0088] Among them, the inclination directions of the partitions 220 in the same layer can be the same or different. The setting of the partition 220 can be referred to the first embodiment and will not be elaborated here.

[0089] Embodiment Three

[0090] The present application also provides a method for transporting a solid precursor with a microchannel, which may include the following steps:

[0091] Providing the above solid precursor transport device;

[0092] Place the solid precursor on the separator plate;

[0093] Assemble the separator plate on the tray and place it in the reaction cavity;

[0094] Stack and assemble the tray in the housing of the solid precursor delivery device, and close the solid precursor delivery device after the assembly is completed.

[0095] As an example, the solid precursor may include a metal halide solid precursor. Among them, the method of placing the solid precursor on the separator plate may include physical coating method, sublimation crystallization method or chemical reaction method.

[0096] Specifically, the solid precursor delivery device in this embodiment is applied to an atomic layer deposition (ALD) device, but is not limited thereto, and can also be applied to, for example, an ion implantation device.

[0097] When using solids such as metal halides as precursors for atomic layer deposition (ALD) currently, since the vapor pressure of the solid precursor is lower than that of the liquid precursor, the carrier gas carries less precursor per unit area passed through. Therefore, higher requirements are imposed on the surface area through which the carrier gas flows in the delivery device and the residence time. However, the solid precursor delivery device cannot adopt the design of a liquid precursor evaporator. In order to allow the carrier gas to better contact the precursor, a more complex internal structure is required.

[0098] In addition, as the solid precursor is gradually consumed, the volume of the precursor particles decreases, and the surface area also decreases accordingly, resulting in a decrease in the total sublimation rate of the precursor in the delivery device.

[0099] In addition, impurities are easily introduced during the loading process of the solid precursor. Therefore, the precursor loading process should be simplified as much as possible. Therefore, the delivery problem of the solid precursor can be well solved by the solid precursor delivery device in this embodiment.

[0100] In this embodiment, the solid precursor adheres to the separator plate in the solid precursor delivery device. When loading the solid precursor into the solid precursor delivery device, the separator plate with the solid precursor attached can be first inserted into the groove of the tray, and then the trays are stacked in a certain order, and finally the solid precursor delivery device is re-closed in combination with the housing.

[0101] Among them, the solid precursor can be AlCl3, HfCl4, WCl5 or other solids that do not react with the materials used in the solid precursor delivery device. The solid precursor can be attached to the partition by means such as sublimation-recrystallization, or can be generated on the partition through a chemical reaction, or the solid precursor can be attached to the surface of the partition by other means such as coating method. The attached solid precursor on the partition can be continuously distributed or island-shaped distributed. Regarding the type, attachment method, distribution morphology, etc. of the solid precursor, no excessive restrictions are made here.

[0102] The following takes the solid precursor as anhydrous AlCl3 as an example for introduction. The delivery method of the solid precursor specifically may include:

[0103] First, extract the AlCl3·6H2O containing impurities to remove the impurities therein;

[0104] Next, heat and dehydrate the purified AlCl3·6H2O in an HCl atmosphere, and at the same time sublime the dehydrated AlCl3, so that the sublimated AlCl3 recrystallizes on the surface of the partition located in the cold trap and connected to the sublimation device, thereby attaching to the partition;

[0105] Next, in a glove box isolated from moisture, take out the partition from the cold trap, assemble it in the reaction cavity of the tray in a certain arrangement manner, then stack the trays and install them in the housing. After filling is completed, close the delivery device to complete the assembly.

[0106] A heating element can be provided outside the solid precursor delivery device to meet the sublimation temperature requirement of the solid precursor. By providing a series of grooves on the side wall and / or bottom of each layer of tray for inserting the partition, the partition can be fixed in the tray and at the same time maintain good thermal contact with the tray to conduct heat and maintain the uniformity of the temperature distribution inside the delivery device. The solid precursor stored in the solid precursor delivery device is attached to the partition. The partition used can be a flat plate or a curved plate, such as other types of plates like corrugated plates, etc. to further optimize the distribution of the solid precursor on the surface of the partition and at the same time increase the contact area between the solid precursor and the gas phase. The partition in the tray can be placed vertically or inclined at a certain angle to the bottom surface of the tray, and the corresponding grooves can also be arranged vertically or inclined.

[0107] There is a channel for the carrier gas to flow through at the bottom of each layer of tray, which may include an intake channel and several outlet channels. The carrier gas entering the solid precursor delivery device from the tray intake port directly enters below the lowermost tray through the intake channel of each layer of tray, and then flows upward layer by layer through the outlet channels, and finally flows out through the tray outlet at the top of the solid precursor delivery device with the gas-phase precursor.

[0108] In order to extend the path that the carrier gas passes through in the solid precursor delivery device, the partitions between adjacent layers of trays can be arranged at an angle, and the positions of the gas outlet channels can also be staggered from each other, so as to extend the residence time of the carrier gas in the solid precursor delivery device and enable it to come into contact with the solid precursor more fully.

[0109] In specific applications, one or several preferred combinations can be found by selecting the shape, installation angle, quantity, distribution of the partitions, the quantity, pore diameter, distribution of the gas channels, the height of each layer of trays, the way of tray stacking, etc., so as to achieve the purpose of maximizing the contact time and contact area between the carrier gas and the solid precursor.

[0110] In summary, for the solid precursor delivery device and delivery method with microchannels of the present invention, the partition that can be installed in a matching manner with the tray and is used to carry the solid precursor is provided in the tray, and the partition has a partition microchannel inside. The bottom surface of the partition has a partition air inlet connected to the partition microchannel, and the surface of the partition has a partition air outlet connected to the partition microchannel. After installation, the partition has an included angle with the bottom of the tray and the bottom surface of the installed partition is in contact with the bottom of the tray. The partition air inlet is connected to the tray air outlet and the partition air outlet is connected to the reaction cavity to form an air outlet channel, thereby increasing the contact area between the solid precursor and the gas and extending the contact time to meet the application requirements.

[0111] The above embodiments are only illustrative of the principles and effects of the present invention and are not intended to limit the present invention. Any person familiar with this technology can modify or change the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or changes made by those with ordinary knowledge in the technical field without departing from the spirit and technical idea disclosed by the present invention should still be covered by the claims of the present invention.

Claims

1. A solid precursor delivery device with microchannels, comprising a housing, and a gas source hole and an exhaust hole located on the housing, characterized in that, Further comprising: A tray disposed inside the housing, the tray including a tray sidewall and a tray bottom, the tray bottom and the tray sidewall forming a reaction cavity, the tray bottom being provided with a tray air inlet and a tray air outlet penetrating the tray bottom, the tray air inlet being connected to the gas source hole to form an air inlet passage, and the tray having a first mounting portion therein; A partition, the partition having a second mounting portion, and the partition being mounted in the reaction cavity by assembling the second mounting portion with the first mounting portion. The partition has a partition microchannel therein, and the bottom surface of the partition has a partition air inlet communicating with the partition microchannel, and the surface of the partition has a partition air outlet communicating with the partition microchannel. After installation, the partition has an included angle with the tray bottom and the bottom surface of the installed partition is in contact with the tray bottom. The partition air inlet is connected to the tray air outlet and the partition air outlet is connected to the reaction cavity and the reaction cavity is connected to the exhaust hole to form an air outlet passage, and the solid precursor is carried by the partition.

2. The solid-state precursor delivery device according to claim 1, wherein: The range of the included angle θ formed between the installed partition and the tray bottom is 0° < θ ≤ 90°.

3. The solid-state precursor delivery device according to claim 1, wherein: The inside of the housing includes a plurality of stacked trays, the tray air inlets in the stacked trays are communicated with each other and connected to the gas source hole to form an air inlet passage, the partition microchannels in adjacent trays are communicated, and the reaction cavity of the uppermost tray is connected to the exhaust hole for exhausting; the side surface of the installed partition is in contact with the tray sidewall.

4. The solid-state precursor delivery device according to claim 1, wherein: The partition air outlets on the same partition are annularly distributed; the partition air outlets in the adjacent partitions on the left and right are staggeredly arranged.

5. The solid-state precursor delivery device according to claim 1, characterized in that: The stacked partitions up and down have an included angle.

6. The solid-state precursor delivery device according to claim 1, wherein: The assembly method of the first mounting portion and the second mounting portion includes snap-fit assembly, the first mounting portion is a groove and the second mounting portion is a correspondingly arranged protrusion, or the first mounting portion is a protrusion and the second mounting portion is a correspondingly arranged groove.

7. The solid-state precursor delivery device according to claim 1, wherein: The partition includes one or a combination of a flat plate and a curved plate; the partition is a metal partition with a sandblasted surface.

8. The solid-state precursor delivery device according to claim 1, wherein: Further comprising a heating element, and the heating method of the heating element includes one or a combination of contact heating and radiation heating.

9. A method for transporting a solid precursor having a microchannel, characterized in that, Including the following steps: Providing the solid precursor delivery device according to any one of claims 1 to 8; Placing the solid precursor on the partition; Assembling the partition on the tray to place it in the reaction cavity; Stacking and assembling the trays in the housing of the solid precursor delivery device, and closing the solid precursor delivery device after assembly.

10. The conveying method of the solid precursor according to claim 9, wherein: The solid precursor includes a metal halide solid precursor; the method of placing the solid precursor on the partition includes physical coating method, sublimation crystallization method or chemical reaction method.

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