CN219409894U - Atomic layer deposition equipment for microchannel reactor - Google Patents
Atomic layer deposition equipment for microchannel reactor Download PDFInfo
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- CN219409894U CN219409894U CN202320250796.0U CN202320250796U CN219409894U CN 219409894 U CN219409894 U CN 219409894U CN 202320250796 U CN202320250796 U CN 202320250796U CN 219409894 U CN219409894 U CN 219409894U
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Abstract
The utility model relates to the technical field of chemical reaction equipment surface treatment, and discloses atomic layer deposition equipment for a microchannel reactor, which comprises a feed pipe of the microchannel reactor and a discharge pipe of the microchannel reactor; the outlet end of the feed pipe of the microchannel reactor is used for connecting with the inlet of the microchannel reactor, and the inlet end is communicated with the outlet ends of one or more feed pipes; the feeding pipe is provided with a carrier gas inlet, and one or more reactant feed inlets are arranged between the outlet end of the feeding pipe and the carrier gas inlet; and the inlet end of the discharging pipe of the micro-channel reactor is used for being connected with the outlet of the micro-channel reactor, and the outlet end of the discharging pipe is communicated with a vacuum pump. The atomic layer deposition equipment can pertinently perform atomic layer deposition on the internal channel of the microchannel reactor, and the deposition is limited on the inner wall of the channel of the reactor, so that the atomic layer deposition equipment has the advantages of high deposition efficiency, uniform formed deposition layer and less precursor raw material waste.
Description
Technical Field
The utility model relates to the technical field of chemical reaction equipment surface treatment, in particular to atomic layer deposition equipment for a microchannel reactor.
Background
Atomic layer deposition (Atomic layer deposition, ALD), also known as atomic layer epitaxy, is a process by which substances can be plated onto a substrate surface layer by layer in the form of a monoatomic film by alternately passing pulses of a vapor phase precursor into a reactor to chemisorb and react on a deposition substrate to form a deposited film. ALD has good development prospect and wide application potential because it has high reactivity and precision, and excellent deposition uniformity and consistency, and can achieve accurate film thickness control at the atomic level.
In recent years, ALD technology has been developed in the fields of microelectronics, optoelectronics, optics, nanotechnology, micromechanical systems, energy, catalysis, biomedical applications, displays, corrosion-resistant and sealing coatings, and the like, and has shown explosive growth, and ALD equipment and ALD material markets are also undergoing rapid development and growth. While the types and amounts of materials prepared by atomic layer deposition are becoming increasingly rich, in addition to simple substances, oxides, nitrides, sulfides, fluorides, selenides, tellurides, carbides, etc., have been extended from conventional inorganic materials to polymers, organic-inorganic hybrid materials, from simple binary compounds to complex ternary, quaternary compounds and alloys, from amorphous (polycrystalline), epitaxial thin films to specific nanostructures, superlattices, nano-water patterns, metal-organic framework structures, etc.
A microchannel reactor is a three-dimensional structural element that can be used to carry out chemical reactions, fabricated in a solid matrix by means of special micromachining techniques. The micro-channel reactor takes micro-channels with small size as cores, reduces the dispersion scale of fluid, quickens the mass transfer and heat transfer rate, shortens the reaction time, simultaneously can realize the accurate control of the temperature in the reaction process, and has the advantages of high integration level, strong continuity, capability of realizing the continuous amplification of the reaction in a small space, strong anti-interference capability and the like. The micro-channel reactor has the advantages of improving the roughness of the inner surface, corrosion resistance or catalyst loading and the like due to the extremely large specific surface area if atomic layer deposition is carried out on the inner surface of the micro-channel, thereby greatly reflecting the advantages of the micro-channel reactor.
Many ALD apparatus have been reported but a vacuum chamber design is used to deposit atomic layers on substrates (plates or wafers, etc.). For example, patent CN202211109129.7 discloses an atomic layer deposition apparatus, in which a substrate sheet to be deposited is placed in a reaction chamber during operation, and then a precursor is delivered to the reaction chamber to achieve atomic layer deposition on the substrate sheet. These ALD apparatus can be used to achieve co-deposition throughout the chamber while depositing primarily on the surface of the workpiece within the chamber, but when used in a microchannel reactor, it is difficult to achieve rapid uniform deposition on the inner surfaces of the interior microchannels of the reactor.
Disclosure of Invention
In order to solve the technical problem that the existing ALD equipment is difficult to realize rapid and uniform deposition inside a microchannel reactor, the utility model provides atomic layer deposition equipment for the microchannel reactor. The device can pertinently carry out atomic layer deposition on the internal channel of the micro-channel reactor, and the deposition is limited on the inner wall of the channel of the reactor, thereby having the advantages of high deposition efficiency, uniform formed deposition layer and less precursor raw material waste.
The specific technical scheme of the utility model is as follows:
an atomic layer deposition device for a microchannel reactor comprises a feed pipe of the microchannel reactor and a discharge pipe of the microchannel reactor; the outlet end of the feed pipe of the microchannel reactor is used for connecting with the inlet of the microchannel reactor, and the inlet end is communicated with the outlet ends of one or more feed pipes; the feeding pipe is provided with a carrier gas inlet, and one or more reactant feed inlets are arranged between the outlet end of the feeding pipe and the carrier gas inlet; and the inlet end of the discharging pipe of the micro-channel reactor is used for being connected with the outlet of the micro-channel reactor, and the outlet end of the discharging pipe is communicated with a vacuum pump.
The atomic layer deposition equipment of the utility model works as follows: the precursor is introduced into a micro-channel in the micro-channel reactor through a feed pipe and a feed pipe of the micro-channel reactor by carrier gas conveying, and the precursor is attached and reacted on the inner surface of the micro-channel, so that atomic layer deposition is realized on the inner surface of the micro-channel, and redundant carrier gas and gas are discharged through a discharge pipe of the micro-channel reactor by a vacuum pump; and then introducing carrier gas and vacuumizing to remove residual precursor in the pipeline, so as to avoid pipeline blockage. When multiple precursors are needed, after each precursor is deposited, a carrier gas is introduced and vacuumized to remove the residual precursor in the pipeline, and then another precursor is introduced to avoid the formation of deposition in the pipeline to block the pipeline.
According to the utility model, the feed pipe of the micro-channel reactor and the discharge pipe of the micro-channel reactor are respectively connected with the inlet and outlet of the micro-channel reactor, so that the deposition of the whole chamber of the traditional ALD equipment can be limited in the micro-channel of the reactor, the defect that the precursor raw material is difficult to diffuse into the whole internal channel of the reactor (or slowly diffuse) when the micro-channel reactor is deposited in the traditional chamber is effectively overcome, the internal deposition efficiency and uniformity of the micro-channel reactor are greatly improved, the consumption of the precursor raw material can be reduced, and the waste is avoided.
Preferably, the atomic layer deposition apparatus includes a body chamber and a heating chamber for placing a microchannel reactor; the outlet end of the feed pipe of the micro-channel reactor and the inlet end of the discharge pipe of the micro-channel reactor are arranged in the heating cavity; the inlet end of the feed pipe of the micro-channel reactor, the outlet end of the discharge pipe of the micro-channel reactor and the feed pipe are arranged in the main body cavity.
In performing atomic layer deposition, it is often necessary to effect reaction of the precursors by heating. By utilizing the heat exchange channel in the microchannel reactor, heat exchange liquid can be introduced to heat the microchannel so as to enable the precursor to react, but the utility model focuses on that the heating mode is only suitable for atomic layer deposition with low reaction temperature (50-200 ℃). Therefore, the heating chamber is arranged in the atomic layer deposition equipment, the micro-channel reactor is arranged in the heating chamber when atomic layer deposition is carried out, and the heating in the micro-channel can be realized by utilizing the high temperature in the whole chamber, so that the heating mode can meet the atomic layer deposition requirement of high reaction temperature (up to 500 ℃), and the heating mode can be used for atomic layer deposition in the micro-channel reactor without a heat exchange channel.
In addition, since the micro-channel reactors have different specifications and the sizes of the micro-channel reactors are not fixed, the heating chamber is designed independently of the main body chamber, so that the heating chamber is convenient to be independently replaced according to the sizes of the micro-channel reactors, and the volume of the heating chamber is more adaptive.
Preferably, the reactant feed inlets are a plurality of in number, including one or more metal source feed inlets and one or more oxidation source feed inlets; the number of the feeding pipes is two, the metal source feeding port is arranged on one feeding pipe, the oxidation source feeding port is arranged on the other feeding pipe, and each feeding pipe is provided with a carrier gas inlet.
By adopting the atomic layer deposition equipment with the metal source feed inlet and the oxidation source feed inlet, metal oxides can be loaded in the microchannel reactor, and the metal oxides can play roles of improving the roughness of the inner surface of the microchannel, improving the corrosion resistance, catalyzing the reaction in the microchannel and the like. According to the utility model, the plurality of metal source feed inlets are arranged on the same feed pipe, so that the occupation of a feed pipeline to space can be reduced, and the ALD deposition process cannot be excessively influenced.
Preferably, the microchannel reactor comprises a reactor main body, and further comprises a microchannel and a heat exchange channel which are arranged in the reactor main body; two ends of the micro-channel are respectively provided with a micro-channel inlet and a micro-channel outlet; and the two ends of the heat exchange channel are respectively provided with a heat exchange liquid inlet and a heat exchange liquid outlet.
By arranging the heat exchange channel in the microchannel reactor, the atomic layer deposition requirement of low reaction temperature (50-200 ℃) can be met, and the heating mode can lead the microchannel to be heated more uniformly, thereby improving the uniformity of the deposition layer.
Preferably, the carrier gas inlet is communicated with a carrier gas inlet pipe; and the carrier gas inlet pipe is provided with a flow controller and a carrier gas inlet valve.
In the process of atomic layer deposition of a microchannel reactor, if the speed of introducing precursor raw materials into a microchannel is poorly controlled, the morphology of a deposition layer formed on the inner wall of the microchannel is difficult to control, and thus the microchannel is blocked. Therefore, the flow controller is arranged on the carrier gas inlet pipe, the speed of the precursor flowing into the micro-channel is strictly controlled by controlling the carrier gas flow rate, and the generated deposit layer is prevented from blocking the micro-channel.
Preferably, the reactant feed port is in communication with a reactant reservoir; and a reactant feeding valve is arranged between the reactant feeding hole and the reactant storage tank.
Preferably, a heat trap is arranged between the outlet end of the discharging pipe of the micro-channel reactor and the vacuum pump.
Preferably, a vacuum gauge is arranged on a branch between the outlet end of the discharging pipe of the micro-channel reactor and the vacuum pump.
Preferably, a control cabinet is arranged on the side surface of the main body chamber; the heating chamber is arranged above the main body chamber and the control cabinet.
Preferably, the feed pipe of the micro-channel reactor and/or the discharge pipe of the micro-channel reactor are/is corrugated pipes.
The size and the inlet and outlet positions of the microchannel reactor are not fixed, and if a common metal tube is used, the connecting position needs to be searched after the microchannel reactor is broken; the corrugated pipe has certain plasticity and can follow the change of the inlet and outlet positions of the microchannel reactor, thereby being more convenient to connect.
Compared with the prior art, the utility model has the following advantages:
(1) The atomic layer deposition equipment can pertinently perform atomic layer deposition on the internal channel of the microchannel reactor, and the deposition is limited on the inner wall of the channel of the reactor, so that the atomic layer deposition equipment has the advantages of high deposition efficiency, uniform formed deposition layer and less precursor raw material waste;
(2) The atomic layer deposition equipment adopts two heating modes, namely a heating mode of a heat exchange channel and a heating cavity in the microchannel reactor, wherein the heating mode can enable a deposition layer formed on the inner wall of the microchannel to be more uniform, and the heating mode can meet the atomic layer deposition requirement of high reaction temperature.
Drawings
FIG. 1 is a schematic view of an atomic layer deposition apparatus according to the present utility model;
FIG. 2 is a front view of FIG. 1;
FIG. 3 is a top view of FIG. 1;
FIG. 4 is a rear view of FIG. 1;
FIG. 5 is a flow chart of an atomic layer deposition apparatus of the present utility model;
FIG. 6 is a schematic view showing the internal structure (top view) of the microchannel reactor in application example 1;
FIG. 7 is a left side view of FIG. 6;
FIG. 8 is a schematic view showing the structure of a microchannel reactor in application example 2;
FIG. 9 is a schematic view showing the internal structure of the microchannel reactor in application example 2.
The reference numerals are: the device comprises a front chamber 1, a feeding pipe 11, a carrier gas inlet 111, a metal source feeding port 112, an oxidation source feeding port 113, a carrier gas inlet pipe 12, a flow controller 13, a carrier gas inlet valve 14, a metal source precursor storage tank 15, a metal source precursor feeding valve 16, an oxidation source storage tank 17, an oxidation source feeding valve 18, a rear chamber 2, a vacuum gauge 21, a discharging valve 22, a heat trap 23, a heating chamber 3, a control cabinet 4, a micro-channel reactor feeding pipe 5, a micro-channel reactor discharging pipe 6, a vacuum pump 7, a reactor main body 8, a micro-channel 81, a micro-channel inlet 811, a micro-channel outlet 812, a heat exchange channel 82, a heat exchange liquid inlet 821, a heat exchange liquid outlet 822 and a channel temperature measuring port 83.
Detailed Description
The utility model is further described below with reference to examples. The devices, connection structures and methods referred to in this utility model are those well known in the art, unless otherwise specified.
General examples
An atomic layer deposition device for a microchannel reactor comprises a feed pipe 5 of the microchannel reactor and a discharge pipe 6 of the microchannel reactor; the outlet end of the feed pipe 5 of the microchannel reactor is used for connecting with the inlet of the microchannel reactor, and the inlet end is communicated with the outlet ends of one or more feed pipes 11; a carrier gas inlet 111 is formed in the feeding pipe 11, and one or more reactant feed inlets are formed between the outlet end of the feeding pipe 11 and the carrier gas inlet 111; the inlet end of the discharging pipe 6 of the micro-channel reactor is used for being connected with the outlet of the micro-channel reactor, and the outlet end is communicated with the vacuum pump 7.
As one specific embodiment, the reactant feed ports are plural in number, including one or more metal source feed ports 112 and one or more oxidation source feed ports 113; the number of the feeding pipes 11 is two, the metal source feeding hole 112 is arranged on one feeding pipe 11, the oxidation source feeding hole 113 is arranged on the other feeding pipe 11, and each feeding pipe 11 is provided with a carrier gas inlet 111.
As a specific embodiment, the carrier gas inlet 111 communicates with the carrier gas inlet pipe 12; the carrier gas inlet pipe 12 is provided with a flow controller 13 and a carrier gas inlet valve 14. The reactant feed inlet is communicated with the reactant storage tank; and a reactant feeding valve is arranged between the reactant feeding hole and the reactant storage tank.
As a specific embodiment, a vacuum gauge 21 and a heat trap 23 are arranged on a branch between the outlet end of the discharging pipe 6 of the micro-channel reactor and the vacuum pump 7.
As a specific embodiment, the microchannel reactor feed pipe 5 and/or the microchannel reactor discharge pipe 6 are bellows.
As a specific embodiment, the atomic layer deposition apparatus includes a body chamber and a heating chamber 3 for placing a microchannel reactor; the outlet end of the feed pipe 5 of the micro-channel reactor and the inlet end of the discharge pipe 6 of the micro-channel reactor are arranged in the heating chamber 3; the inlet end of the feed pipe 5 of the micro-channel reactor, the outlet end of the discharge pipe 6 of the micro-channel reactor and the feed pipe 11 are arranged in the main body cavity. A control cabinet 4 is arranged on the side surface of the main body cavity; the heating chamber 3 is arranged above the main body chamber and the control cabinet 4.
As a specific embodiment, the microchannel reactor comprises a reactor body 8, and further comprises a microchannel 81 and a heat exchange channel 82 arranged in the reactor body 8; two ends of the micro-channel 81 are respectively provided with a micro-channel inlet 811 and a micro-channel outlet 812; the heat exchange channel 82 is provided with a heat exchange liquid inlet 821 and a heat exchange liquid outlet 822 at two ends respectively.
Example 1
An atomic layer deposition device for a microchannel reactor is shown in fig. 1-4, and a flow chart is shown in fig. 5. The atomic layer deposition equipment consists of a main body chamber, a heating chamber 3 and a control cabinet 4, wherein the main body chamber consists of a front chamber 1 and a rear chamber 2; the control cabinet 4 is arranged on the side surface of the main body cavity, the heating cavity 3 is detachably arranged above the main body cavity and the control cabinet 4, and the heating cavities 3 with different sizes can be replaced according to the size of the microchannel reactor.
As shown in fig. 2-4, a micro-channel reactor feed pipe 5 and a micro-channel reactor discharge pipe 6 are arranged between the main body chamber and the heating chamber 3, and the micro-channel reactor feed pipe 5 and the micro-channel reactor discharge pipe 6 are corrugated pipes. The outlet end of the feed pipe 5 of the microchannel reactor and the inlet end of the discharge pipe 6 of the microchannel reactor are positioned in the heating chamber 3 and are respectively used for connecting the inlet and the outlet of the microchannel reactor. The inlet end of the feed pipe 5 of the microchannel reactor is positioned in the front chamber 1, and the outlet end of the discharge pipe 6 of the microchannel reactor is positioned in the rear chamber 2.
As shown in fig. 2, the inlet end of the microchannel reactor feed tube 5 communicates with the outlet ends of two feed tubes 11. Each feed pipe 11 is provided with a carrier gas inlet 111; two reactant feed inlets, which are all metal source feed inlets 112, are arranged between the outlet end of one feed pipe 11 and the carrier gas inlet 111; a reactant feed port, which is an oxidation source feed port 113, is provided between the outlet end of the other feed tube 11 and the carrier gas inlet 111. A feed pipe 11 is provided in the front chamber 1.
As shown in fig. 2, each carrier gas inlet 111 communicates with the outlet of one carrier gas inlet pipe 12. A carrier gas inlet pipe 12 is provided in the front chamber 1, and its inlet communicates with the outside of the main body chamber for introducing an external carrier into the feed pipe 11. Each carrier gas inlet pipe 12 is provided with a flow controller 13 and a carrier gas inlet valve 14, and the flow controller 13 and the carrier gas inlet valve 14 are positioned in the front chamber 1.
As shown in fig. 2, a reactant feed valve is arranged between a reactant feed inlet on the feed pipe 11 and a reactant storage tank; each reactant feed port is in communication with a reactant reservoir. The reactant storage tank communicated with the metal source feed inlet 112 is a metal source precursor storage tank 15, and the reactant feed valve between the reactant storage tank and the metal source precursor storage tank is a metal source precursor feed valve 16; the reactant storage tank communicated with the oxidation source feed inlet 113 is an oxidation source storage tank 17, and the reactant feed valve between the two is an oxidation source feed valve 18. A reactant reservoir is provided in the front chamber 1.
As shown in fig. 4, the outlet end of the discharging pipe 6 of the micro-channel reactor is communicated with a vacuum pump 7, and a vacuum gauge 21 (arranged on a branch), a discharging valve 22 and a heat trap 23 are sequentially arranged between the outlet end and the vacuum pump, wherein the heat trap 23 is a heat trap. A vacuum gauge 21 and a heat sink 23 are provided in the rear chamber 2, and a vacuum pump 7 is located outside the main body chamber.
All the pipelines of the atomic layer deposition equipment are provided with heating jackets.
Example 2
This example differs from example 1 in that in this example, the reactant feed ports on the two feed pipes 11 are designed as follows: a reactant feed inlet 112 is arranged between the outlet end of one feed pipe 11 and the carrier gas inlet 111, and is a metal source feed inlet; a reactant feed port, which is an oxidation source feed port 113, is provided between the outlet end of the other feed tube 11 and the carrier gas inlet 111.
Application example 1
The microchannel reactor shown in fig. 6 and 7 was subjected to atomic layer deposition using the atomic layer deposition apparatus in example 1. The microchannel reactor in this application example is composed of a reactor main body 8 and a microchannel 81 provided in the reactor main body 8, wherein both ends of the microchannel 81 are respectively provided with a microchannel inlet 811 and a microchannel outlet 812 provided on the outer wall of the reactor main body 8.
The atomic layer deposition process in this application example is as follows:
step S1: titanium tetrachloride solution and diethyl nickel dichloride solution are respectively filled in the two metal source precursor storage tanks 15, and deionized water is filled in the oxidation source precursor storage tank 17.
Step S2: placing the microchannel reactor in the heating chamber 3, and connecting a microchannel inlet 811 and a microchannel outlet 812 with the outlet end of the microchannel reactor feed pipe 5 and the inlet end of the microchannel reactor discharge pipe 6, respectively; the temperature in the heating chamber 3 is raised to 150 ℃ by adopting an electric heating mode, and meanwhile, the temperature setting of the heating jackets at all positions of the pipeline is started.
Step S3: the nitrogen is used as carrier gas, the flow controller 13 is arranged, the carrier gas inlet valve 14 on the feeding pipe 11 where the metal source feeding hole 112 is positioned, the metal source precursor feeding valve 16 and the discharging valve 22 which are connected with a storage tank filled with titanium tetrachloride are opened, the vacuum pump 7 is opened, the titanium tetrachloride is conveyed into the micro-channel 81 through the feeding pipe 11 and the micro-channel reactor feeding pipe 5 by using the nitrogen, the vacuum pump 7 is closed for a period of time to enable the titanium tetrachloride to be deposited on the inner wall of the micro-channel, and then the vacuum pump 7 is opened to discharge redundant gas.
Step S4: the metal source precursor feed valve 16 was closed and purged with nitrogen while a vacuum was pulled.
Step S5: the carrier gas inlet valve 14 on the feeding pipe 11 where the metal source feeding port 112 is positioned is closed, the carrier gas inlet valve 14 and the oxidation source feeding valve 18 on the feeding pipe 11 where the oxidation source feeding port 113 is positioned are opened, and the oxidation source is conveyed into the micro-channel 81 through the feeding pipe 11 and the micro-channel reactor feeding pipe 5 by utilizing nitrogen gas to oxidize the titanium tetrachloride to generate titanium dioxide.
Step S6: the oxidation source feed valve 18 was closed and purged with nitrogen while a vacuum was pulled.
Step S7: the carrier gas inlet valve 14 on the feeding pipe 11 where the metal source feeding port 112 is positioned, the metal source precursor feeding valve 16 and the discharging valve 22 which are connected with a storage tank filled with diethyl nickel dichloride are opened, the diethyl nickel dichloride is conveyed into the micro-channel 81 through the feeding pipe 11 and the micro-channel reactor feeding pipe 5 by utilizing nitrogen, the vacuum pump 7 is closed for a period of time to enable the nickel dichloride to be deposited on the inner wall of the micro-channel, and then the vacuum pump 7 is opened to discharge redundant gas.
Step S8: the metal source precursor feed valve 16 was closed and purged with nitrogen while a vacuum was pulled.
Step S9: the carrier gas inlet valve 14 on the feeding pipe 11 where the metal source feeding port 112 is positioned is closed, the carrier gas inlet valve 14 and the oxidation source feeding valve 18 on the feeding pipe 11 where the oxidation source feeding port 113 is positioned are opened, and nitrogen is utilized to convey the oxidation source into the micro-channel 81 through the feeding pipe 11 and the micro-channel reactor feeding pipe 5, so that the nickel dichloride is oxidized to generate nickel oxide.
Step S10: the oxidation source feed valve 18 was closed and purged with nitrogen while a vacuum was pulled.
Step S11: repeating the steps S3-S10 for 100 cycles, and growing layer by layer.
Through the steps, tiO can be formed on the inner wall of the micro-channel 2 Deposition layer of @ NiO, observed by electron microscopy, having a thickness of about 17nm, of TiO therein 2 The @ NiO particles have an obvious core-shell structure, and NiO on the surfaces has obvious polycrystalline small particle stacking morphology.
Application example 2
The microchannel reactor shown in fig. 8 and 9 was subjected to atomic layer deposition using the atomic layer deposition apparatus in example 1. The micro-channel reactor in this application example is different from application example 1 in that in this application example, a heat exchange channel 82 and a channel temperature measurement port 83 are further provided in the reactor main body 8, two ends of the heat exchange channel 82 are respectively provided with a heat exchange liquid inlet 821 and a heat exchange liquid outlet 822 which are provided on the outer wall of the reactor main body 8, and the channel temperature measurement port 83 is provided on the outer wall of the reactor main body 8 and is communicated with the micro-channel 81.
The process of atomic layer deposition in this example of application is as follows:
step S1: trimethylaluminum is filled in a metal source precursor storage tank 15, and deionized water is filled in an oxidation source precursor storage tank 17.
Step S2: placing the microchannel reactor on a chamber table, and connecting a microchannel inlet 811 and a microchannel outlet 812 with the outlet end of the microchannel reactor feed pipe 5 and the inlet end of the microchannel reactor discharge pipe 6, respectively; the heat exchange liquid inlet and the heat exchange liquid outlet of the microchannel reactor are respectively connected to the outlet and the inlet of the heat exchange integrated machine, the temperature of the heat exchange liquid is set to be 150 ℃, and meanwhile, the temperature setting of the heating jackets at all positions of the pipeline is started.
Step S3: the nitrogen is adopted as carrier gas, the flow controller 13 is arranged, the carrier gas inlet valve 14 on the feeding pipe 11 where the metal source feeding hole 112 is positioned, the metal source precursor feeding valve 16 and the discharging valve 22 which are connected with a storage tank filled with trimethylaluminum are opened, the vacuum pump 7 is opened, the trimethylaluminum is conveyed into the micro-channel 81 through the feeding pipe 11 and the micro-channel reactor feeding pipe 5 by utilizing the nitrogen, the vacuum pump 7 is closed for a period of time to enable the trimethylaluminum to be deposited on the inner wall of the micro-channel, and then the vacuum pump 7 is opened to discharge redundant gas.
Step S4: the metal source precursor feed valve 16 was closed and purged with nitrogen while a vacuum was pulled.
Step S5: the carrier gas inlet valve 14 on the feeding pipe 11 where the metal source feeding port 112 is located is closed, the carrier gas inlet valve 14 and the oxidation source feeding valve 18 on the feeding pipe 11 where the oxidation source feeding port 113 is located are opened, and the oxidation source is conveyed into the micro-channel 81 through the feeding pipe 11 and the micro-channel reactor feeding pipe 5 by utilizing nitrogen gas to oxidize the trimethylaluminum to generate alumina.
Step S6: the oxidation source feed valve 18 was closed and purged with nitrogen while a vacuum was pulled.
Step S7: repeating the steps S3-S6 for 100 cycles, and growing layer by layer.
The foregoing description is only a preferred embodiment of the present utility model, and is not intended to limit the present utility model, and any simple modification, variation and equivalent structural transformation made according to the technical substance of the present utility model still fall within the scope of the technical solution of the present utility model.
Claims (10)
1. An atomic layer deposition device for a microchannel reactor, comprising a microchannel reactor feed pipe (5) and a microchannel reactor discharge pipe (6); the outlet end of the feed pipe (5) of the microchannel reactor is used for connecting with the inlet of the microchannel reactor, and the inlet end is communicated with the outlet ends of one or more feed pipes (11); a carrier gas inlet (111) is formed in the feeding pipe (11), and one or more reactant feed inlets are formed between the outlet end of the feeding pipe (11) and the carrier gas inlet (111); the inlet end of the discharging pipe (6) of the micro-channel reactor is used for being connected with the outlet of the micro-channel reactor, and the outlet end is communicated with the vacuum pump (7).
2. Atomic layer deposition apparatus according to claim 1, characterized in that it comprises a main body chamber and a heating chamber (3) for placing a microchannel reactor; the outlet end of the feed pipe (5) of the micro-channel reactor and the inlet end of the discharge pipe (6) of the micro-channel reactor are arranged in the heating chamber (3); the inlet end of the feed pipe (5) of the micro-channel reactor, the outlet end of the discharge pipe (6) of the micro-channel reactor and the feed pipe (11) are arranged in the main body cavity.
3. The atomic layer deposition apparatus according to claim 1, wherein the number of reactant feed ports is a plurality, including one or more metal source feed ports (112) and one or more oxidation source feed ports (113); the number of the feeding pipes (11) is two, the metal source feeding holes (112) are formed in one feeding pipe (11), the oxidation source feeding holes (113) are formed in the other feeding pipe (11), and each feeding pipe (11) is provided with a carrier gas inlet (111).
4. The atomic layer deposition apparatus according to claim 1 or 2, wherein the microchannel reactor comprises a reactor body (8), further comprising a microchannel (81) and a heat exchange channel (82) arranged within the reactor body (8); two ends of the micro-channel (81) are respectively provided with a micro-channel inlet (811) and a micro-channel outlet (812); and a heat exchange liquid inlet (821) and a heat exchange liquid outlet (822) are respectively arranged at two ends of the heat exchange channel (82).
5. The atomic layer deposition apparatus according to claim 1, wherein the carrier gas inlet port (111) communicates with a carrier gas inlet pipe (12); the carrier gas inlet pipe (12) is provided with a flow controller (13) and a carrier gas inlet valve (14).
6. The atomic layer deposition apparatus according to claim 1, wherein the reactant feed port is in communication with a reactant reservoir; and a reactant feeding valve is arranged between the reactant feeding hole and the reactant storage tank.
7. Atomic layer deposition apparatus according to claim 1, wherein a thermal trap (23) is provided between the outlet end of the microchannel reactor discharge tube (6) and the vacuum pump (7).
8. The atomic layer deposition apparatus according to claim 1, wherein a vacuum gauge (21) is arranged in the branch between the outlet end of the outlet pipe (6) of the microchannel reactor and the vacuum pump (7).
9. The atomic layer deposition apparatus according to claim 2, wherein a control cabinet (4) is provided at a side of the main body chamber; the heating chamber (3) is arranged above the main body chamber and the control cabinet (4).
10. Atomic layer deposition apparatus according to claim 1, wherein the microchannel reactor feed pipe (5) and/or the microchannel reactor discharge pipe (6) are bellows.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320250796.0U CN219409894U (en) | 2023-02-07 | 2023-02-07 | Atomic layer deposition equipment for microchannel reactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320250796.0U CN219409894U (en) | 2023-02-07 | 2023-02-07 | Atomic layer deposition equipment for microchannel reactor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN219409894U true CN219409894U (en) | 2023-07-25 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN202320250796.0U Active CN219409894U (en) | 2023-02-07 | 2023-02-07 | Atomic layer deposition equipment for microchannel reactor |
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| Country | Link |
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| CN (1) | CN219409894U (en) |
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2023
- 2023-02-07 CN CN202320250796.0U patent/CN219409894U/en active Active
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