Reactant delivery system and reactor system including the same
The remote solid feed reactant delivery system addresses the challenge of reactant replenishment in vapor deposition reactors by using bulk fill containers and controlled interconnecting lines to maintain continuous reactant supply, improving processing efficiency.
Patent Information
- Application Number
- JP2024228982
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-01-03
- Filing Date
- 2024-12-25
- Publication Date
- 2025-07-15
AI Technical Summary
Current solid source reactant delivery systems for vapor deposition reactors face challenges in quickly and effectively replenishing reactants without significant downtime, leading to inefficiencies in semiconductor processing.
A remote solid feed reactant delivery system with bulk fill containers and interconnecting lines, including a line heater to maintain reactant vaporization and a gas panel with valves for seamless switching, allowing continuous reactant supply without interrupting the reactor operation.
The system enables uninterrupted reactant delivery, reducing downtime and improving throughput in semiconductor processing by allowing remote refilling of reactants, thus enhancing the efficiency of vapor deposition reactors.
Smart Images

Figure 2025106222000001_ABST
Abstract
Description
Technical Field
[0001] (Cross - Reference to Related Applications) This application is a continuation - in - part application claiming priority to U.S. Patent Application No. 18 / 074,629, filed on December 5, 2022, entitled "REMOTE SOLID SOURCE REACTANT DELIVERY SYSTEMS FOR VAPOR DEPOSITION REACTORS", which is a non - provisional application of U.S. Provisional Patent Application No. 63 / 265,139, filed on December 8, 2021, entitled "REMOTE SOLID SOURCE REACTANT DELIVERY SYSTEMS FOR VAPOR DEPOSITION REACTORS", and claims the priority and benefit thereof, all of which are hereby incorporated by reference in their entirety.
[0002] This application generally relates to systems and methods including or associated with semiconductor processing equipment, and more specifically to solid source reactant delivery systems for vapor deposition reactors.
Background Art
[0003] Solid source reactant delivery systems can be used to deliver reactant vapor to a vapor deposition reactor including a deposition reaction chamber. A solid source reactant delivery system can include a container that can contain a solid source reactant to be vaporized. During operation of the vapor deposition reactor, the solid source reactant can be vaporized by a carrier gas, transported, or drawn into the reaction chamber alone as vapor, and the reactant can participate in a chemical reaction to deposit a material on a substrate. When the reactant vaporizes, it depletes and may need to be refilled or replenished. However, currently, there are certain limitations regarding methods that can quickly and effectively replenish the solid source reactant while reducing the downtime of the vapor deposition reactor. Therefore, improved reactant delivery systems, reactor systems including the reactant delivery systems, and methods of using them are desired.
[0004] Any consideration of the problems and solutions described in this section is included in this disclosure only for the purpose of providing context for the disclosure, and should not be taken as an admission that any or all of the considerations were known at the time the invention was made.
Prior Art Documents
Patent Documents
[0005]
Patent Document 1
Patent Document 2
Patent Document 3
Summary of the Invention
Problems to be Solved by the Invention
[0006] A solid source reactant delivery system and method for a vapor deposition reactor are disclosed. In some embodiments, the solid source reactant delivery system includes a first bulk fill container remote from the vapor deposition reactor. The first bulk fill container can be configured to hold a first solid source chemical reactant therein. The first bulk fill container can include a first fluid outlet configured to pass a first vaporized chemical reactant out of the first container body. The delivery system can further include a second bulk fill container remote from the vapor deposition reactor and configured to hold a second solid source chemical reactant therein. The second bulk fill container can include a second fluid outlet configured to pass a second vaporized chemical reactant out of the second container body. The delivery system can include interconnecting lines fluidly connecting the vapor deposition reactor to each of the first and second bulk fill containers. The vapor deposition reactor can be separated from both of the first and second bulk fill containers by at least a minimum distance. The delivery system can further include a line heater configured to heat at least a portion of the interconnecting lines to at least a minimum line temperature. The delivery system can include a gas panel including valves. The gas panel can be disposed between the interconnecting lines and each of the first and second bulk fill containers. The valves can be configured to selectively flow a first vaporized chemical reactant from the first fluid outlet and a second vaporized chemical reactant from the second fluid outlet through the interconnecting lines.
[0007] According to additional embodiments of the present disclosure, an exemplary reactant delivery system includes a first container, a first housing surrounding the first container, a second container, a conduit fluidly coupled to the second container and the first container, and a flow control device within the conduit for controlling the amount of vapor of a solid feed reactant moving from the second container to the first container. According to examples of these embodiments, the first container includes a first container inlet and a first container outlet. The first container can form part of a reactor system and can be configured to hold a solid feed reactant. According to further examples, the second container is external to the first housing. The second container can be configured to hold a solid feed reactant. The second container may be remote from the reactor system. According to further examples, the pressure within the first housing is less than the ambient pressure external to the first housing. According to still further examples, the reactant delivery system further includes a valve plate within the first housing. The valve plate can include one or more valves fluidly coupled to the first container outlet. According to further examples, the reactant delivery system includes a pressure transducer for measuring the pressure within the conduit. According to still further examples, the reactant delivery system includes a second housing surrounding the second container. In such cases, the pressure within the second housing may be greater than the pressure within the first housing. The exemplary reactant delivery system also includes a controller. The controller can be configured to control the temperature of the first container and the temperature of the second container. For example, the controller can be configured to adjust the temperature of the bottom portion of the first container to be lower than the temperature of the upper portion of the first container. Additionally or alternatively, the controller can be configured to automatically heat the second container when the amount of reactant within the first container falls below a threshold amount.
[0008] According to still further embodiments of the present disclosure, the reactant delivery system includes a first container, a second container, a third container, a conduit, and a flow control device. According to an example of the present disclosure, the first container includes a first container inlet and a first container outlet. The first container can form part of a reactor system and can be configured to hold a solid raw material reactant. The second and third containers are also configured to hold a solid raw material reactant. The flow control device can be configured to control the amount of vapor of the solid raw material reactant moving from the third container to one or more of the first container or the second container. The first container outlet and / or the second container outlet can be fluidly coupled to one or more reaction chambers (e.g., an inlet to the reaction chamber).
[0009] According to still further examples, the reactor system includes one or more process modules and a reactant delivery system such as the reactant delivery system described herein. By way of example, the reactant delivery system can include a first container, a second container, a third container, a conduit, and a flow control device. The first container can include a first container inlet and a first container outlet, the first container forms part of the reactor system and is configured to hold a solid raw material reactant. The second container can include a second container outlet. The second container can be configured to hold a solid raw material reactant. The third container can include a third container outlet, the third container can be remote from the reactor system, and can be configured to hold a solid raw material reactant. The conduit can fluidly couple the third container outlet to the first container inlet and / or the second container inlet. The flow control device can be disposed within the conduit and can control the amount of vapor of the solid raw material reactant moving from the third container to one or more of the first container or the second container. The second container outlet can be fluidly coupled to one or more of the process modules (e.g., each).
[0010] This is provided only as an example and should not be regarded as limiting the present disclosure in any way. Other embodiments are described below in conjunction with the related drawings.
[0011] These and other aspects of the present disclosure will be readily apparent to those skilled in the art from the description herein, the appended claims, and the drawings which are intended to illustrate and not limit the invention.
Brief Description of the Drawings
[0012]
Figure 1
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[0013] It will be understood that the elements in the figures are illustrated for simplicity and clarity and are not necessarily drawn to scale. For example, the dimensions of some of the elements in the figures may be exaggerated relative to other elements to assist in improving the understanding of the illustrated embodiments of the present disclosure.
Modes for Carrying Out the Invention
[0014] If there are headings provided in this specification, they are for convenience only and do not necessarily affect the scope or meaning of the claimed invention. This specification describes systems and related methodologies for delivering gaseous reactant substances from solid raw material reactants. Such systems and methodologies are suitable for use, for example, in large volume deposition modules.
[0015] The following detailed description describes specific specific embodiments to assist in understanding the scope of the claims. However, the invention may be practiced in many different embodiments and ways as defined and covered by the claims.
[0016] The reaction process may include various processes, including deposition processes such as chemical vapor deposition (CVD) and atomic layer deposition (ALD), vapor etching processes, and other processes in the semiconductor industry for forming and patterning thin films of materials on substrates such as silicon wafers. In a deposition process, reactant vapors (including "precursor gases") of different chemical substances of reactants are delivered to one or more substrates within a reaction chamber. In some cases, the reaction chamber comprises only a single substrate supported on a substrate holder (such as a susceptor), and the substrate and substrate holder are maintained at a desired process temperature. In other instances, the reaction chamber may hold two, three or more substrates to be processed.
[0017] In a typical CVD process, one or more reactive reactant vapors react with each other and / or with the substrate to form a thin film on the substrate, and the growth rate is generally related to the temperature and the amount of reactant gas. In some variations, the energy driving the deposition reactants is supplied in whole or in part by a plasma. The production of electronic devices such as semiconductor devices may include a plurality of reactant steps in which gaseous reactants are provided to the reaction chamber, for example, one or more steps in which precursors are provided to a deposition process and / or one or more etching steps.
[0018] During the reactant supply process, gaseous (e.g., vaporized) reactants are delivered into the deposition reaction chamber of a vapor deposition reactor. The reactants may be solid raw materials that are vaporized by a sublimator such as a solid raw material sublimator before being introduced into the reaction chamber. The sublimator can heat the solid raw material chemical reactant (which may be referred to herein as a solid raw material reactant or simply a reactant) to exceed the minimum sublimation temperature at which the sublimator is configured to vaporize the solid raw material chemical reactant. The minimum sublimation temperature may depend on the type of solid raw material reactant.
[0019] Another known process for forming a thin film on a substrate is ALD. In many applications, ALD uses the liquid and / or solid raw material chemicals described herein. ALD is a type of vapor deposition that deposits a film generally through a self-saturating reaction carried out in cycles. The thickness of the film is generally determined by the number of cycles carried out. In the ALD process, gaseous reactants are supplied alternately and / or repeatedly to a substrate or wafer to form a thin film of material on the wafer. One reactant adsorbs on the wafer through a self-controlled process. Subsequently, different pulsed reactants react with the adsorbed material to form a single molecular layer of the desired material. For example, decomposition may occur through the interaction between adsorbed species and with appropriately selected reagents in a ligand exchange or gettering reaction. In some ALD reactions, only a single molecular layer of just one molecule is formed per cycle. Thicker films are produced through repeated growth cycles until the target thickness is achieved.
[0020] In some ALD reactions, the reactive reactants are kept separately in the gas phase by intervening a removal process while exposing the substrate to different reactants. For example, in a time - divided ALD process, the reactants are provided to a stationary substrate in pulses and typically separated by purge and / or evacuation phases. In a space - divided ALD process, the substrate moves through zones having different reactants, and in some processes, both aspects of space - divided ALD and time - divided ALD can be combined. One skilled in the art will understand that some variations or hybrid processes can enable a reaction like CVD to some extent, either by selection of deposition conditions outside the normal ALD parameter window and / or by allowing some overlap between reactive reactants during exposure to the substrate.
[0021] Delivery of the vaporized solid - state source reactant from the sublimator to the deposition reaction chamber can be controlled by a delivery mechanism that delivers the reactant vapor. In some embodiments, the sublimator may be disposed within the deposition reactor, for example, near one or more deposition reaction chambers. This can provide more rapid delivery of the reactant vapor to the reaction chamber. However, this arrangement may require a significant amount of downtime for the reactor while the sublimator is being refilled with the solid - state source reactant.
[0022] To address this issue, in some embodiments, the sublimator can be disposed remotely from the deposition reactor. This remoteness or separation can provide greater flexibility with respect to space and thus can reduce space constraints. Further, using the remote delivery system described herein allows the sublimator to be refilled without significantly interrupting or with significantly reduced interruption of semiconductor processing. Instead, according to an example of the present disclosure, the sublimator can be refilled during operation of the reactor, and this refill may not significantly affect the processing of the substrate. Therefore, the remote delivery system can improve the throughput of semiconductor processing.
[0023] A sublimator can generally refer to any receptacle or container that vaporizes reactants such as solid starting reactant materials. The sublimator can include a housing or body that contains the solid starting reactant material. The sublimator can include one or more bulk filling containers. For example, a remote sublimator can include a plurality of bulk filling containers disposed within a housing. Other arrangements are possible.
[0024] A solid starting reactant delivery system can include one or more of a solid and / or liquid filling container (or feedstock container) and a heater (such as a radiant heat lamp, a resistance heater, and / or the like). The filling container can be heated, for example, using a resistive cable and / or rod heater, within a vacuum enclosure. The filling container can contain a chemical reactant (which may also be referred to as a “chemical precursor” or “feedstock precursor”), which can be a solid (e.g., in powder form) or a liquid. The heater heats the container and promotes vaporization and / or sublimation of the reactant material within the container.
[0025] The container can have an inlet and an outlet for the flow of a carrier gas such as a noble gas (e.g., N2, Ar, He, etc.) through the container. Generally, the carrier gas carries the reactant vapor (e.g., the evaporated or sublimed chemical reactant) along with it through the container outlet and ultimately to the reaction chamber. Typically, the container includes a isolation valve to fluidically isolate the contents of the container from the outside. The isolation valve may be disposed on or near the lid of the filling container.
[0026] The filling containers of some embodiments comprise, consist essentially of, or consist of a sublimator. That is, whenever “feedstock container” or “filling container” is referred to herein, a sublimator (such as a “solid starting chemical sublimator”) is also explicitly contemplated.
[0027] In some applications, the reactant gas is stored in gaseous form in a reactant-filled container. In such applications, the reactant is often gaseous at standard pressure and temperature of about 1 atmosphere and room temperature. Examples of such gases include nitrogen, oxygen, hydrogen, and ammonia. However, in some cases, the vapor of a chemical reactant (a "precursor") that is a solid at standard pressure and standard temperature (e.g., hafnium chloride, hafnium oxide, zirconium dioxide, and the like) is used. For some chemical reactants, the vapor pressure at room temperature is very low, so it is typically heated and / or held at a very low pressure to produce a sufficient amount of reactant vapor for the reaction process. After vaporization (e.g., sublimation or evaporation), by keeping the gaseous reactant above the vaporization temperature across the processing system, unwanted condensation in valves, filters, conduits, and other components associated with the delivery of the gaseous reactant to the reaction chamber can be prevented. Such gaseous reactants from natural solids or liquids are useful in chemical reactions in a variety of other industries.
[0028] The reactant-filled container is equipped with a gas line extending from an inlet and an outlet, a isolation valve on the line, and a fitting on the valve, and the fitting is configured to connect to a gas flow line to the reactor. For example, the interconnecting line may connect the sublimator and / or other parts of the delivery system to the reactor. Often, some additional heaters are provided to heat the various valves and gas flow lines between the reactant-filled container or sublimator and the reactor to prevent the reactant vapor from condensing and depositing on such components. Thus, the gas transport components between the filled container and the reaction chamber may be referred to as a "hot zone" where the temperature is maintained higher than the vaporization / condensation / sublimation temperature of the reactant. The temperature required to vaporize the reactant may be different from the temperature required to avoid condensation in lines, valves, etc. Thus, the acceptable temperature range may be different from the temperature range in the sublimator, in the gas line (e.g., interconnecting line), or in another element, as will be described in more detail below.
[0029] The remote filling container can directly deliver the vaporized reactant to the reaction chamber. However, in some embodiments, the remote filling container may be configured to fill the reactant filling container within the reactor with the chemical reactants described herein. The container may include an "intermediate filling" container, a "transfer fill" container, or a "bulk" container or the like (for the sake of brevity, the intermediate filling container or the transfer fill container may be referred to herein simply as a "filling container"). Examples of some transfer fill containers are disclosed in Patent Document 1 titled "FILL VESSELS AND CONNECTORS FOR CHEMICAL SUBLIMATORS", filed on September 3, 2020, which application is hereby incorporated by reference in its entirety for all purposes.
[0030] When the chemical reactant is depleted and needs to be replaced, it is common practice to replace the entire filling container with a new container full of the chemical reactant. Replacing the filling container requires shutting off the associated valves, disconnecting and physically removing the filling container, placing the new filling container in the appropriate location, and connecting the fittings of the new filling container to the remaining substrate processing apparatus. Often, this process also involves disassembling various thermocouples, line heaters, clamps, and the like. These processes can be somewhat laborious and time-consuming.
[0031] The delivery system described herein having a refill container can advantageously reduce the need to replace or refill sublimators within the reactor. Instead, the refill container can be used to automatically and / or continuously supply chemical reactants to the reactor system. Additionally or alternatively, the flow may be pulsed. The refill chamber system can include one or more refill containers. Further, a refill container according to an embodiment herein can be disposed near, adjacent to, or within the reactor. As described above, since the refill container need not be removed from the reactor system for refilling, the refill container can achieve the advantages (such as a relatively short flow path) of being disposed proximal to or within the reactor system without the labor and downtime associated with refilling. Additional features are described herein with reference to various configurations.
[0032] FIG. 1 schematically illustrates an exemplary remote solid feed reactant delivery system 100 according to some configurations. The remote solid feed reactant delivery system 100 can include a vapor deposition reactor 102, a plurality of bulk refill containers 108, 112, and an interconnect line 140 fluidly connecting the plurality of bulk refill containers 108, 112 to the vapor deposition reactor 102.
[0033] The vapor deposition reactor 102 can include one or more vapor deposition reaction chambers 104. Each vapor deposition reaction chamber 104 can include one or more substrate supports 106. The substrate support 106 can be configured to receive a substrate therein and, as described above, to allow reactant gas to pass thereover.
[0034] Each of the bulk filling containers 108, 112 can include a corresponding container body 116, 120, a container lid 124, 128, and fluid outlets 126, 130 configured to pass the vaporized chemical reactant out of the corresponding container body 116, 120 and toward the interconnecting line 140. The bulk filling containers 108, 112 can each be configured to hold a solid raw material chemical inside. In some embodiments, the first bulk filling container 108 can be configured to hold the same chemical reactant as the second bulk filling container 112. However, in some embodiments, each may hold a different chemical reactant.
[0035] Generally, each of the bulk filling containers 108, 112 can include a solid chemical reactant, but can also be a liquid chemical reactant. The terms "solid raw material precursor" and "solid raw material chemical reactant" may generally be used interchangeably and have their customary and ordinary meaning in the art in light of this disclosure. These terms refer to raw material chemicals that are solid under standard conditions (i.e., room temperature and atmospheric pressure).
[0036] Each of the container lids 124, 128 is adapted to be mechanically attached to the top of the corresponding container body 116, 120. This may be done using one or more of attachment devices (e.g., bolts, screws, etc.). In certain embodiments, the container lids 124, 128 and the container bodies 116, 120 are hermetically and mechanically attached. The container bodies 116, 120 can be shaped to reduce the footprint and hold a significant amount of chemical reactant inside (see below).
[0037] Each of the bulk filling containers 108, 112 can include corresponding container heaters 132, 136 configured to heat the corresponding bulk filling containers 108, 112. The first container heater 132 and the second container heater 136 can operate independently of each other. Thereby, it may be possible to allow the operation of one of the container heaters 132, 136, and the other heater may be temporarily turned off and / or the other corresponding bulk filling containers 108, 112 are replaced or refilled. As shown in FIG. 1, the container heaters 132, 136 can be disposed below the corresponding bulk filling containers 108, 112. However, other configurations are possible. For example, the container heaters 132, 136 can be disposed within the corresponding container bodies 116, 120. The heater can include a heating pad, a heating rod, a heating jacket, a heating blade, a heating lamp, or other heaters.
[0038] One or more of the bulk filling containers 108, 112 can be at least partially housed within a housing 152. The housing 152 can include a metal housing. The housing 152 may be insulated to prevent or reduce the flow of heat from the housing. Thereby, the possibility of condensation occurring within one or more lines or valves of the remote solid reactant delivery system 100 can be reduced. The housing 152 can function as a central repository for holding chemical reactants and an intuitive central point for accessing and refilling the chemical reactants.
[0039] The interior of the housing or cabinet 152 can be maintained at a reduced pressure (e.g., 1 mTorr to 10 Torr, and often about 500 mTorr). This reduced pressure can promote radiative heating of the bulk fill containers 108, 112 within the housing 152 and / or thermally isolate the containers from each other to encourage a more uniform temperature field. In other variations, the housing 152 does not include a vent and includes a convection enhancement device (e.g., a fan, crossflow, etc.). A reflector sheet can be provided that is configured to surround components within the housing 152 and reflect radiant heat generated by the heating devices 132, 156 to the components positioned within the housing 152. The reflector sheet can be provided on the inner walls of the housing 152 as well as the ceiling and floor of the housing.
[0040] The remote solid source reactant delivery system 100 can include a gas panel 148 that includes one or more valves for passing through and / or controlling the flow of vapor between the bulk fill containers 108, 112 and the deposition reactor 102. The gas panel 148 may be disposed between the interconnect lines 140 and each of the bulk fill containers 108, 112. Additionally or alternatively, the deposition reactor 102 can include a reactor gas panel 172 that includes one or more corresponding valves configured to control the flow of gas into the deposition reaction chamber 104. The reactor gas panel 172 can direct the flow of vaporized reactants to one or more deposition reaction chambers of the deposition reactor 102.
[0041] The flow from the bulk fill containers 108, 112 to the vapor deposition reactor 102 via the interconnect line 140 may not be simultaneous from each of the bulk fill containers 108, 112, but instead may be switchable such that the flow to the vapor deposition reactor 102 can be switched exclusively from the first bulk fill container 108, exclusively to the second bulk fill container 112, and vice versa. Each of the one or more valves of the gas panel 148 can be configured to switch the flow of the vaporized chemical reactant through the interconnect line 140 from the flow exiting the first fluid outlet 126 to the flow exiting the second fluid outlet 130. By being switchable, the vapor deposition reactor 102 may be allowed to receive a non-interrupted flow of reactants. Thus, when it is necessary to refill the first bulk fill container 108 with chemical reactants, the gas panel 148 can be seamlessly switched (e.g., via one or more valves) such that the flow comes from the second bulk fill container 112. This seamless transition may be referred to as a "hot swap" of the gas flow.
[0042] To avoid condensation of reactants within vessels, valves, lines, etc., the vaporized reactants are maintained generally above a threshold temperature. Accordingly, the line supplying the vaporized reactants to the vapor deposition reactor 102 is generally heated. To effect the above-described hot swap, each of the bulk fill vessels 108, 112 may need to be heated to at least a minimum vessel temperature to vaporize the chemical reactants. In some embodiments, the temperature inside each of the bulk fill vessels 108, 112 is substantially the same. The minimum vessel temperature may depend on the chemical substances held within the corresponding bulk fill vessels 108, 112 and the associated pressure. Additionally or alternatively, the minimum vessel temperature may depend at least in part on the flow rate of vapor out of the bulk fill vessels 108, 112. For example, the minimum vessel temperature may be about 85 °C, about 90 °C, about 95 °C, about 100 °C, about 105 °C, about 110 °C, about 115 °C, about 120 °C, about 125 °C, about 130 °C, about 135 °C, about 140 °C, about 145 °C, about 150 °C, about 155 °C, about 160 °C, about 165 °C, about 170 °C, about 175 °C, about 180 °C, any value therebetween, or within any range having endpoints therewithin. For example, the minimum vessel temperature may be about 105 °C to about 155 °C, and in some embodiments, is about 135 °C at a vapor pressure of about 150 Torr and a flow rate of about 100 sccm. Other temperatures and pressures may be achieved by the hardware designs disclosed herein. A vessel temperature of about 135 °C to about 150 °C appears to be an effective range for generally maintaining the vaporized chemical reactants at standard pressure and flow rate without consuming excessive energy.
[0043] The interconnect line 140 may be heated by a line heater 144 of the remote solid reactant delivery system 100. The line heater 144 can be any type of heater known in the art, such as a heating jacket that at least partially surrounds the interconnect line 140. The line heater 144 may be configured to heat at least a portion of the interconnect line 140 to at least a minimum line temperature. The line heater 144 may be configured to insulate a portion of the interconnect line 140 from temperature changes when a temperature above the minimum line temperature is achieved. The minimum line temperature may generally be higher than the minimum vessel temperature and may depend on the chemical substances held within the corresponding bulk fill containers 108, 112, the associated pressure within the interconnect line 140, and / or the flow rate of the vapor from the bulk fill containers 108, 112. For example, the minimum line temperature may be about 115 °C, about 120 °C, about 125 °C, about 130 °C, about 135 °C, about 140 °C, about 145 °C, about 150 °C, about 155 °C, about 160 °C, about 165 °C, about 170 °C, about 175 °C, about 180 °C, about 185 °C, about 190 °C, about 195 °C, about 200 °C, about 205 °C, about 210 °C, about 215 °C, any value between these, or within any range having endpoints therein. For example, the minimum line temperature may be about 140 °C to about 190 °C and in some embodiments is about 155 °C at a vapor pressure of about 120 Torr and a flow rate of 100 sccm. A line temperature of about 140 °C to about 190 °C appears to be an effective range for generally maintaining the vaporized chemical reactants at standard pressure and flow rate without consuming excessive energy.
[0044] In some embodiments, the housing 152 includes a housing heater 156. The housing heater 156 may be disposed near, adjacent to, and / or within the housing 152. The housing heater 156 may be configured to heat the housing 152 to at least a minimum housing temperature. The minimum housing temperature may be lower than the minimum vessel temperature and / or the minimum line temperature.
[0045] In some embodiments, the remote solid - state reactant delivery system 100 includes a flow controller 160 or a flow meter configured to alter the flux of the vaporized chemical reactant through the interconnect line 140. The flow controller 160 can be in fluid communication with the interconnect line 140 and / or the flow controller 160 may monitor the flow of vapor through the interconnect line 140. The flow controller 160 can measure the flow rate of the vapor. The monitoring may be updated repeatedly (e.g., periodically), such as over regular intervals. The flow controller 160 may be coupled to a flow control valve (e.g., a needle valve, a throttle valve, etc.) that can control the flux of the vaporized chemical reactant through the interconnect line 140. The flow controller 160 can receive a signal (e.g., from a flow control sensor within the interconnect line 140) that the amount of flux through the interconnect line 140 is too high or too low. The flow controller 160 can then send a signal to the flow control valve to decrease or increase the flux of the vapor through the interconnect line 140.
[0046] The remote solid - state reactant delivery system 100 can include a vessel controller 164 configured to track the amount of chemical reactant within the bulk fill vessels 108, 112. The vessel controller 164 can include one or more sensors configured to identify the amount of reactant in each of the bulk fill vessels 108, 112. Additionally or alternatively, the vessel controller 164 can be configured to receive an indication when one or more of the bulk fill vessels 108, 112 hold a chemical amount outside of a threshold amount of reactant. For example, the vessel controller 164 may obtain from one or more sensors a signal indicating that the amount of solid - state reactant chemical within the first bulk fill vessel 108 is below a minimum threshold amount. In response to the signal, the vessel controller 164 may instruct one or more valves of the gas panel 148 to switch the flow of the vaporized chemical reactant through the interconnect line from the flow from the first fluid outlet to the flow from the second fluid outlet.
[0047] In some embodiments, the container controller 164 can transmit to the user interface a notification that the amount of chemical substance in one or more of the bulk filling containers 108, 112 is outside a threshold amount. The threshold amount can be a maximum threshold (e.g., a signal is generated when the amount exceeds the maximum threshold) or a minimum threshold (e.g., a signal is generated when the amount is below the minimum threshold). The container controller 164 can communicate with the housing 152 and / or any elements therein via the container controller connection 168. The container controller connection 168 can be a wired connection or a wireless connection.
[0048] The housing 152 and / or one or more of the bulk filling containers 108, 112 may be disposed remotely from the vapor deposition reactor 102. By disposing remotely, more flexibility can be provided in the location where the bulk filling containers 108, 112 are placed. Additionally or alternatively, this can allow at least one of the bulk filling containers 108, 112 to have a sufficient amount of chemical reactant therein to reduce the amount of time required to refill the amount of chemical reactant within the housing 152 for delivery to the vapor deposition reactor 102. In some embodiments, the interconnecting line 140 separates the vapor deposition reactor 102 from the housing 152 and / or the bulk filling containers 108, 112 by a minimum distance. The minimum distance may be partially determined by the chemical reactant, flow rate, and / or pressure within the interconnecting line 140. The minimum distance may be about 3 m, about 5 m, about 8 m, about 10 m, about 15 m, about 18 m, about 20 m, about 25 m, about 30 m, about 35 m, about 40 m, any value between these, or within any range having endpoints therein. For example, in some embodiments, the minimum distance is about 15 m. In some embodiments, the total separation distance is about 30 m.
[0049] The ratio of the height of each of the bulk filling containers 108, 112 to its width / diameter can be such that the installation area of the remote solid raw material reactant delivery system 100 is reduced. The ratio of height to width is greater than about 1, greater than about 1.5, greater than about 2, greater than about 3, greater than about 4, greater than about 5, greater than about 6, greater than any value between these, or within any range having endpoints therein. For example, in some embodiments, the ratio of height to width is about 1.54. In some embodiments, the height of the bulk filling containers 108, 112 is about 85 cm and the width is about 55 cm. Each of the bulk filling containers 108, 112 can be configured to hold a substantial amount of solid raw material chemical reactant. This ability to hold so much chemical reactant can reduce the need to refill each bulk filling container, thereby reducing the likelihood of errors in refilling and reducing human intervention. Each of the bulk filling containers 108, 112 can be configured to hold about 16 L of chemical reactant inside. Based on the chemical, each of the bulk filling containers 108, 112 can hold at least 18 kg of chemical reactant. For example, it may be advantageous to minimize the volume or installation area that the bulk filling containers 108, 112 will require so that they can be placed in more locations if needed. A compact container assembly can reduce such an installation area. In certain embodiments, each of the bulk filling containers 108, 112 is about 2000 cm 2 ~ about 3500 cm 2 and can have an area (e.g., where the corresponding bulk filling containers 108, 112 are disposed).
[0050] Each of the container lids 124, 128 may include a corresponding carrier gas inlet (not shown) that can permit a flow of carrier gas therethrough. The carrier gas inlet can include a corresponding valve that may be included in the gas panel 148. The carrier gas can combine with the chemical substances sublimated or evaporated within the bulk fill containers 108, 112. Next, the effluent from the bulk fill containers 108, 112 includes the carrier gas and the reactant gas vaporized from within the bulk fill containers 108, 112. In some embodiments, the interior of the bulk fill containers 108, 112 is configured to include a headspace after being filled with the chemical reactants. The headspace can be in fluid communication with the corresponding carrier gas inlet and / or fluid outlets 126, 130 and can be configured for sublimation of the chemical reactants by the fluid (e.g., carrier gas) within the headspace.
[0051] As described above, it is preferred to use an inert or noble gas as the carrier gas for the vaporized chemical reactants. A noble gas (e.g., nitrogen, argon, helium, or the like) may be supplied to the bulk fill containers 108, 112 through the corresponding carrier gas inlet. It will be understood that additional valves and / or other fluid control elements not shown may be included.
[0052] The effluent (e.g., carrier gas + vaporized chemical substance) can pass through fluid outlets 126, 130, through gas panel 148 and interconnect line 140, and move to deposition reactor 102. In some embodiments, each of fluid outlets 126, 130 comprises a corresponding filter (not shown in FIG. 1) configured to prevent the passage of particulate matter therethrough. The filter can serve to ensure that particulate matter does not pass into deposition reactor 102 (e.g., within deposition reaction chamber 104). In some embodiments, interconnect line 140 connects directly to deposition reaction chamber 104. Additional information regarding exemplary solid precursor chemical sublimators and / or their fluid engineering can be found in Patent Document 2, issued on March 20, 2012, entitled "PRECURSOR DELIVERY SYSTEM", which application is hereby incorporated by reference in its entirety for all purposes. It will be understood that additional valves and / or other fluid elements not shown may be included. Bulk fill containers 108, 112 can have additional or alternative features disclosed in Patent Document 3, filed on September 30, 2016, entitled "REACTANT VAPORIZER AND RELATED SYSTEMS AND METHODS", which application is hereby incorporated by reference in its entirety for all purposes.
[0053] Figure 2 schematically shows another exemplary remote solid - state reactant delivery system 200 according to one embodiment. The remote solid - state reactant delivery system 200 can include a plurality of bulk - filled containers 208, 212 within a housing 252, and a vapor deposition reactor 202. The vapor deposition reactor 202 can include a substrate handling chamber 210 and one or more housing modules 204a, 204b, 204c, 204d. As shown, an interconnect line 240 can directly connect the housing 252 (or any element therein) to the one or more housing modules 204a, 204b, 204c, 204d. In some embodiments, the interconnect line 240 can indirectly connect the housing modules 204a, 204b, 204c, 204d via an intermediate solid - state sublimator (not shown). Additionally or alternatively, a reactor gas panel (not shown) on the vapor deposition reactor 202 can direct the gas flow from the interconnect line 240 towards the one or more housing modules 204a, 204b, 204c, 204d. Thus, the bulk - filled containers 208, 212 can supply the vaporized chemical reactants received from the housing 252 to the plurality of housing modules 204a, 204b, 204c, 204d from a distance via the interconnect line 240. As shown, each of the housing modules 204a, 204b, 204c, 204d can include one or more vapor deposition reactors 206a, 206b. The interconnect line 240 is shown connecting only one of the housing modules 204a, 204b, 204c, 204d, but any combination of the housing modules 204a, 204b, 204c, 204d can receive the vaporized reactants via the reactor gas panel.
[0054] The remote solid - state reactant delivery system 200 can include one or more features of the remote solid - state reactant delivery system 100 described above. However, to avoid unnecessary repetition, the details are not repeated here. For example, the bulk - filled containers 208, 212 can include one or more features of the bulk - filled containers 108, 112 described above.
[0055] Figure 3 shows an exemplary method 300 for delivering vaporized chemical reactants to a deposition reactor (e.g., deposition reactor 102, deposition reactor 202) according to some configurations. At block 304, method 300 includes storing a solid-source chemical reactant within first and second container bodies (e.g., container bodies 116, 120) of respective first and second bulk-fill containers (e.g., bulk-fill containers 108, 112, bulk-fill containers 208, 212). At block 308, method 300 includes heating each of the first and second container bodies to at least a minimum container temperature. The minimum container temperature is configured to vaporize the solid-source chemical reactant into a vaporized chemical reactant within the bulk-fill container. As described above, the minimum container temperature may be at least partially based on the solid-source chemical and the pressure within the bulk-fill container. At block 312, an interconnect line (e.g., interconnect line 140, interconnect line 240) may be heated. The interconnect line can fluidly connect the deposition reactor to each of the first and second container bodies. At block 316, method 300 can include passing a vaporized chemical reactant from the first container body through the interconnect line to the deposition reactor. In some embodiments, method 300 includes switching a valve from a first orientation to a second orientation. This switching can change the source of the vaporized chemical reactant flow. For example, in the first orientation, the first container body may be in fluid communication with the deposition reactor, and in the second orientation, the second container body may be in fluid communication with the deposition reactor. Each of the bulk-fill containers may be heated to at least the minimum container temperature to vaporize the chemical reactant. Thus, the containers can be configured to perform the hot swap described above. A container controller (e.g., container controller 164) can be configured to effect the switching and / or maintain a continuous flow of reactant passed to the deposition reactor. At block 320, the vaporized chemical reactant may be passed from the second container body through the interconnect line to the deposition reactor.This switchability and / or use of two bulk fill containers allows for reducing interruptions in the flow of vaporized chemical reactants from one container to the vapor deposition reactor, and thus can improve the vapor deposition of the substrate and / or improve throughput.
[0056] (Exemplary embodiments) The following are a series of non-limiting examples of the above-described embodiments.
[0057] In a first embodiment, a remote solid feed reactant delivery system for a vapor deposition reactor includes a first bulk fill container that is remote from the vapor deposition reactor and configured to hold a first solid feed chemical reactant therein, the first bulk fill container including a first fluid outlet configured to pass a first vaporized chemical reactant out of the first container body; a second bulk fill container that is remote from the vapor deposition reactor and configured to hold a second solid feed chemical reactant therein, the second bulk fill container including a second fluid outlet configured to pass a second vaporized chemical reactant out of the second container body; an interconnecting line fluidly connecting the vapor deposition reactor to each of the first and second bulk fill containers, the vapor deposition reactor being separated from both the first and second bulk fill containers by at least a minimum distance; a line heater configured to heat at least a portion of the interconnecting line to at least a minimum line temperature; and a gas panel including valves, the gas panel being disposed between the interconnecting line and each of the first and second bulk fill containers, the valves being configured to selectively flow a first vaporized chemical reactant from the first fluid outlet and a second vaporized chemical reactant from the second fluid outlet through the interconnecting line.
[0058] In a second embodiment, the delivery system of Example 1, wherein the valves are configured to continuously and / or pulsingly flow at least one of the first vaporized chemical reactant or the second vaporized chemical reactant through the interconnecting line to the vapor deposition reactor.
[0059] In the third embodiment, the delivery system of Example 2, where the minimum line temperature is from about 140°C to about 190°C.
[0060] In the fourth embodiment, the delivery system of any one of Examples 1 to 3, where the line heater comprises a heating jacket configured to at least partially surround a portion of the interconnecting line.
[0061] In the fifth embodiment, the delivery system of any one of Examples 1 to 4, where each of the first and second bulk filling containers comprises a corresponding container heater configured to heat the interior of the respective first and second bulk filling containers to at least the minimum container temperature.
[0062] In the sixth embodiment, the delivery system of Example 5, where the minimum container temperature is from about 105°C to about 155°C.
[0063] In the seventh embodiment, the delivery system of any one of Examples 1 to 6, where the interconnecting line fluidly connects the vapor deposition reactor to each of the first and second bulk filling containers.
[0064] In the eighth embodiment, the delivery system of any one of Examples 1 to 7, further comprising a housing that encloses the first and second bulk filling containers.
[0065] In the ninth embodiment, the delivery system of any one of Examples 1 to 8, where each of the first and second bulk filling containers is configured to hold at least 15 kg of the first and second solid raw material chemical reactants, respectively.
[0066] In the tenth embodiment, the delivery system of any one of Examples 1 to 9, further comprising a flow controller in fluid communication with the interconnecting line, the flow controller being configured to vary the flux of the vaporized chemical reactant passing through the interconnecting line.
[0067] In the 11th embodiment, a container controller is further provided, which is configured to receive a signal indicating that the volume of the solid raw material chemical reactant in the first bulk filling container is below a minimum threshold amount, and to instruct the valve to stop the flow of the first vaporized chemical reactant through the interconnecting line and start the flow of the second chemical reactant through the interconnecting line. The delivery system according to any one of Embodiments 1 to 10.
[0068] In the 12th embodiment, each of the first and second fluid outlets is provided with a corresponding valve configured to control the flow of gas passing therethrough. The delivery system according to any one of Embodiments 1 to 11.
[0069] In the 13th embodiment, the minimum distance is about 15 m. The delivery system according to any one of Embodiments 1 to 12.
[0070] In the 14th embodiment, a delivery system includes a plurality of bulk filling containers, each comprising a container body configured to hold a first solid raw material chemical reactant therein, a lid having a first fluid outlet configured to allow a first vaporized chemical reactant to pass therethrough outside the first container body, and a container heater configured to heat the interior of the container body to at least a container temperature of about 105°C to about 155°C; an interconnecting line fluidly connecting the vapor deposition reactor to each of the bulk filling containers, wherein the vapor deposition reactor is separated from each of the bulk filling containers by at least a minimum distance of at least 5 m; and a line heater configured to heat at least a portion of the interconnecting line to at least a line temperature of, for example, about 140°C to about 190°C.
[0071] In the 15th embodiment, the delivery system according to Embodiment 14 further includes a second bulk filling container, the second bulk filling container comprising a second container body configured to hold a second solid raw material chemical reactant therein, and a second lid including a second fluid outlet configured to allow a second vaporized chemical reactant to pass therethrough outside the second container body.
[0072] In the 16th embodiment, a second bulk filling container is further provided, and the second bulk filling container is provided with a valve disposed between the interconnection line and each of the first and second bulk filling containers, and the valve is configured to selectively flow the first vaporized chemical reactant and the second vaporized chemical reactant through the interconnection line. The delivery system of Example 14 or 15.
[0073] In the 17th embodiment, a method for delivering a vaporized chemical reactant to a vapor deposition reactor, the method comprising storing a solid raw material chemical reactant in the first and second container bodies of the respective first and second bulk filling containers; heating each of the first and second container bodies to at least a minimum container temperature at which the solid raw material chemical reactant is vaporized; heating the interconnection line fluidly to at least a minimum line temperature, wherein the interconnection line connects the vapor deposition reactor to each of the first and second container bodies; moving the vaporized chemical reactant from the first container body to the vapor deposition reactor via the interconnection line; and passing the vaporized chemical reactant from the second container body to the vapor deposition reactor via the interconnection line.
[0074] In the 18th embodiment, the method of Example 17 further includes switching the valve from a first orientation to a second orientation, wherein in the first orientation, the first container body is in fluid communication with the vapor deposition reactor, and in the second orientation, the second container body is in fluid communication with the vapor deposition reactor.
[0075] In the 19th embodiment, the method of Example 17 or 18, wherein the minimum container temperature is about 105°C to about 155°C.
[0076] In the 20th embodiment, the method of any one of Examples 17 to 19, wherein the minimum line temperature is about 140°C to about 190°C.
[0077] Turning again to the drawings, FIG. 4 illustrates a delivery system 400 according to an additional embodiment of the present disclosure. In the illustrated embodiment, the reactant delivery system 400 includes a first container 402 that forms part of a reactor system 408, a first housing 412 that surrounds the first container 402, a second container 414 that is external to the first housing 412 and remote from the reactor system 408, a conduit 420 fluidly coupled to the first container 402 and the second container 414, and a flow control device 422. As will be described in more detail below, the second container 414 can be used to refill the first container 402. When the reactant (e.g., solid feedstock chemical reactant 410) is depleted from the first container 402, the reactant can be replenished from the reactant (e.g., solid feedstock chemical reactant 418) within the second container 414. When the reactant within the second container is depleted, or once depleted, the second container 414 can be replaced or refilled with relatively little interruption to the operation of the reactor system 408.
[0078] The first container 402 is configured to hold a solid raw material reactant. The first container 402 includes a first container lid 409, a first container body 405, a first container inlet 404, and a first container outlet 406. The first container 402 can also include a noble gas inlet 407 for receiving the carrier gas described herein. The configuration of the first container 402 may be similar to the configuration of the bulk filling containers 108, 112 described above. However, in some cases, since the first container 402 forms part of the reactor system 408 or is mounted on the reactor system 408, the first container 402 may have a smaller configuration and / or a smaller installation area compared to the installation areas of the bulk filling containers 108, 112. For example, the ratio of the height of the first container 402 to its width / diameter can be greater than about 0.5, greater than about 0.75, greater than about 0.95, greater than about 1, greater than about 1.25, greater than about 1.5, greater than about 2, greater than any value therebetween, or within any range having endpoints therein. For example, in some embodiments, the ratio of height to width is about 0.95 or about 1.25. In some embodiments, the height of the first container 402 is about 15 cm or about 25 cm, and the width is about 15 cm or about 25 cm. The first container 402 can be configured to contain from about 20 to about 30 kg of the reactant. The reactant can be any suitable solid raw material reactant such as molybdenum or tungsten halide or oxyhalide.
[0079] The first container 402 can be within a first housing 412. The first housing can be the same as or similar to the housing 152 described above. The pressure within the first housing may be below ambient pressure. For example, the pressure within the first housing 412 can be as described above in connection with the housing 152, or can be from about 10 Torr to about 20 Torr, or from about 1 Torr to less than atmospheric pressure.
[0080] The second container 414 is configured to hold the solid raw material chemical reactant 418. The second container 414 may be similar to the bulk refill containers 108, 112 described above. For example, the second container can include a second container lid 413, a second container body 415, and a second container outlet 416. The second container can also include a second container inlet 417 configured to receive the noble gas or inert gas described herein. The second container 414 can be configured with the dimensions and capacities described above in relation to the bulk refill containers 108, 112. By way of example, the second container 414 can be configured to hold from about 20 kg to about 80 kg or about 50 kg of the solid raw material chemical reactant 418.
[0081] As an illustration, the second container 414 can be held within a second housing 436 that surrounds the second container 414. According to an embodiment of the present disclosure, the pressure within the second housing 436 is greater than the pressure within the first housing 412. For example, the pressure within the second housing can be from about 1 Torr to less than atmospheric pressure, or from about 1 Torr to about 750 Torr. In some cases, the pressure within the second housing can be from about 1 to about 100 Torr below atmospheric pressure or ambient pressure. The second housing 436 can be at the fab level, adjacent to the reactor system 408, or remote from the reactor system 408 as described above in relation to the remote solid raw material reactant delivery system 100. For example, the second housing 436 and / or the second container 414 can be at a minimum distance from the reactor system 408 and / or the first container 402 (as described above). The pressure within the second container can be, for example, from about 2 Torr to about 10 Torr.
[0082] The second container 414 can be heated using the container heater 432. The container heater 432 may be the same as or similar to the container heater 132 described above. An additional heater 435 can be used to heat the second container lid 413 and / or the valve plate 434. The container heater 432 and / or the additional heater 435 may be the same as or similar to the container heaters 132, 136 and the other heaters described above.
[0083] The flow of reactants from the second container 414 to the first container 402 can be controlled using the valve plate 434. The valve plate 434 can include one or more valves fluidly coupled to the second container inlet 417 to control the flow of carrier gas into the second container 414 and / or the flow of vaporized reactants to the first container 402. The valve plate 434 can be located within the second housing 436. As illustrated, the valve plate 434 can be disposed between the second container outlet 416 and the first container inlet 404. The valve plate 434 can be heated as described above in connection with the system 100. For example, the valve plate 434 can be heated to a temperature above the sublimation or condensation temperature of the reactants. As a specific example, when the reactant is molybdenum chloride, the valve plate 434 can be heated to a temperature of about 150°C.
[0084] The conduit 420 fluidly couples the second container outlet 416 and the first container inlet 404. The conduit may be the same as or similar to the above-described interconnecting line 140. Further, the conduit 420 can be heated using a line heater 421 that may be the same as or similar to the above-described line heater 144. The line heater 421 can be configured to heat the conduit 420 to a temperature higher than the temperature of the second container 414 in relation to a controller 438 described below. For example, the temperature of the conduit 420 may be 10°C, 15°C, 20°C, 30°C, or 50°C higher than the temperature of the second container 414. According to an embodiment of the present disclosure, the conduit 420 can be heated such that a temperature gradient is formed between a first end 423 of the conduit coupled to the second container 414 and a second end 425 coupled to the first container 402. The temperature gradient can be 5°C, 10°C, 15°C, 20°C, 30°C, or 50°C, or any temperature therebetween.
[0085] The flow control device 422 can include any suitable flow control device such as the above-described flow control device / flow controller 160. As illustrated, the flow control device 422 is within the conduit 420 and can control and / or meter the amount of vapor of the solid raw material chemical reactant 418 moving from the second container 414 to the first container 402. By way of example, the flow control device 422 can be or include one or more of a mass flow controller and a mass flow meter.
[0086] The reactant delivery system 400 can further include a valve plate 428 that may be the same as or similar to the gas panel 148 described above. The valve plate 428 can include one or more valves fluidly coupled to the first container outlet 406 to control the flow of vapor through and / or between the second container 414 and the first container 402 and / or between the first container 402 and the vapor deposition reactor, which may be the same as or similar to the vapor deposition reactor 102. Additionally or alternatively, the valve plate 428 can include valves for controlling the flow of carrier gas through the first container inlet 404 and / or inlet 407. The valve plate 428 can be located within the first housing 412. As illustrated, the valve plate 428 can be disposed between the first container inlet 404 and the vapor deposition reactor. Additionally or alternatively, the vapor deposition reactor can include a reactor gas panel, such as the reactor gas panel 172, that includes one or more corresponding valves configured to control the flow of gas into the vapor deposition chamber. As described above, the reactor gas panel can direct the flow of vaporized reactants to one or more vapor deposition chambers of the vapor deposition reactor.
[0087] One or more heaters 430 can be used to heat the valve plate 428. The one or more heaters 430 may be the same as or similar to the heaters described above. For example, the one or more heaters 430 can be, or can include, a radiant heater capable of maintaining a thermal gradient from the top 401 to the bottom 403 of the first container. Additionally or alternatively, the one or more heaters 430 can be configured to heat the valve plate to a temperature higher than the sublimation or condensation temperature of the reactant. According to an embodiment of the present disclosure, the one or more heaters 430 heat the valve plate 428 to a temperature higher than the temperature at which the heater 435 heats the valve plate 434 and / or the temperature of the first container 402. By way of example, the one or more heaters 435 can heat the valve plate 434 to a temperature that exceeds the temperature of the first valve plate 434 and / or the temperature of the first container 402 by 10°C, 15°C, 20°C, 30°C, or 50°C.
[0088] The reactant delivery system 400 can also include one or more heaters 433, such as a heater jacket, to heat the side wall of the first container 402. Additionally or alternatively, the reactant delivery system 400 can include one or more heaters 431, such as a heater jacket, to heat the side wall of the second container 414.
[0089] As illustrated, the reactant delivery system 400 can further include a vessel cooling device 426 for actively or passively cooling the bottom of the first container 402. Cooling the bottom of the first container 402 can facilitate filling the first container 402 from the bottom up. For example, the cooling device 426 can cool the temperature of the bottom of the first container 402 to a temperature less than 10°C, 15°C, 20°C, 30°C, or 50°C, or even less than the temperature of the top of the first container 402. According to an embodiment of the present disclosure, the cooling device 426 includes a fluid cooling device, a conventional cooling device, a thermoelectric device, and / or a heat sink.
[0090] The reactant delivery system 400 can further include a pressure transducer 424. The pressure transducer 424 can include any suitable pressure measurement device, such as a heated capacitance manometer, for measuring the pressure within conduit 420. The pressure transducer 424 and / or the flow control device 422 can be used to measure the amount of reactant transferred from the second container 414 to the first container 402.
[0091] The reactant delivery system 400 can further include a controller 438 for controlling various devices and functions of the reactant delivery system 400 and / or the reactor system 408. The controller 438 can be configured using closed-loop control to control the amount and / or rate of transfer of material transferred from the second container 414 into the first container 402. The amount of reactant consumed or replenished can be measured at any location downstream of the second container 414. For example, the controller can receive, as an input for closed-loop control, an input of the amount of reactant delivered to the accumulator or to the reaction chamber.
[0092] The controller 438 can be configured to independently control the temperature of the first vessel 402 and the temperature of the second vessel 414. In some cases, the controller 438 can be further configured to adjust the temperature of the bottom 403 of the first vessel to be lower than the temperature of the top 401 of the first vessel, for example, to facilitate filling the first vessel 402 from the second vessel 414. In some cases, the controller 438 is configured to automatically heat the second vessel 414 to stop the flow of reactants from the second vessel 414 to the first vessel 402 when the amount of reactants in the first vessel 402 falls below a threshold amount and / or when a threshold amount of reactants is in the first vessel, i.e., when the first vessel 402 is filled to a desired level. Additionally or alternatively, the controller 438 is configured to change the temperature gradient between the top 401 and the bottom 403 of the first vessel (e.g., by controlling one or more heaters 430 and / or cooling devices 426) to maintain a desired temperature gradient (e.g., 5 °C, 10 °C, 15 °C, 20 °C, 30 °C, or greater than 50 °C) from the top 401 to the bottom 403 of the first vessel, particularly during the filling process.
[0093] FIG. 5 illustrates another reactor delivery system 500 suitable for use with a reactor system 502 according to a further embodiment of the present disclosure. In this case, the delivery system 500 includes a first vessel 504, a second vessel 512, a third vessel 520, a conduit 526 fluidly coupling the third vessel to the second vessel 512 and / or the first vessel 504, and a flow control device 530 within the conduit 526 that controls the amount of vapor of a solid feed reactant 524 moving from the third vessel 520 to one or more of the first vessel 504 or the second vessel 512. In this case, the first vessel 504 can be a primary delivery vessel, the second vessel 512 can be a support vessel, and the third vessel 520 can be a remote filling vessel. The delivery system 500 can be used to reduce the downtime associated with filling the reactant vessels and can allow for continuous operation of the reactor system or module without stopping the operation to refill the reactant vessels.
[0094] The first container 504 may be identical to the first container 402 described above in connection with FIG. 4. The first container 504 can include a first container lid 503 and a first container body 505. As illustrated, the first container 504 can form part of a reactor system 502. As described above, the first container is configured to contain reactants 510. The first container includes a first container inlet 507, a first container outlet 509, and can include a carrier gas inlet 511. The first container inlet 507 can be coupled to the outlet 521 of the third container 520. As illustrated, the first container outlet 509 is fluidly coupled to one or more reaction chambers RC1, RC2.
[0095] The second container 512 may also be the same as or similar to the first container 402. In some cases, the second container 512 can have a volume smaller than that of the first container 504 (e.g., about 50 v%, 60 v%, 75 v%, 80 v%, or any range therebetween).
[0096] The second container 512 includes a second container lid 527, a second container body 513, a second container outlet 514, and a second container inlet 515. The second container 512 is configured to hold the solid feed reactant 516. The second container inlet 515 can be coupled to the outlet 521 of the third container. The second container 512 can include a second inlet 517 coupled to a carrier gas. The second container outlet 514 is fluidly coupled to one or more reaction chambers RC1, RC2.
[0097] The first container 504 and the second container 512 can be within a first housing 519. The first housing 519 can be controlled to a desired pressure, such as the pressure described above in connection with the first housing 412.
[0098] The third container 520 may be the same as or similar to the second container 414 described above. The third container 520 is preferably remotely located from the reactor system 502 and can be configured to hold the solid feed reactant 524. The third container 520 can include a third container lid 523 and a third container body 525, which may be the same as or similar to the container body and lid described above. The third container 520 can be enclosed within a second housing 552 that may be the same as or similar to the second housing 436 described above. The second housing 552 can have an internal pressure as described above in relation to the second housing 436.
[0099] The reactant delivery system 500 can include heaters 508, 548, and 550, heater jackets 549, 553, line heater 551, and / or cooling devices 546, 547, which may be the same as or similar to the heaters and cooling devices described above in relation to FIG. 4. Further, the reactant delivery system 500 can include one or more valve plates as described above.
[0100] The conduit 526 may be the same as or similar to the conduit 420. As described above, the conduit 526 fluidly couples the third container outlet 521 to the first container inlet 507 and / or the second container inlet 515. The reactant delivery system 500 can also include a line heater, such as the heater 551, to maintain the conduit at a desired temperature or desired gradient, as described above.
[0101] The flow control device 530 can be located within the conduit 526. The flow control device 530 can be configured to cooperate with the controller 556 to control the amount of vapor of the solid feed reactant moving from the third container 520 to one or more of the first container 504 or the second container 512.
[0102] The reactant delivery system 500 can also include a pressure transducer 558. The pressure transducer 558 can include any suitable pressure measurement device such as the device described above in connection with the pressure transducer 424. The pressure transducer 558 and / or the flow control device 530 can be used to measure the amount of reactant transferred from the third container 520 to the first container 504 and / or the second container 512.
[0103] The reactant delivery system 500 can also include a separation valve 532. The separation valve 532 can be used when switching the third container 520 for a new container.
[0104] The reactor system 502 can also include a reactor gas panel 542, which can direct the flow of vaporized reactants to one or more vapor deposition reaction chambers RC1, RC2 of the vapor deposition reactor system 502. RC1 and RC2 can each have respective inlets 538, 540. The reactor gas panel 542 can be fluidly coupled to the first container 504 and the second container 512 via lines 544 and valves 534, 536.
[0105] The reactor gas panel 542 can be the same as or similar to the reactor gas panel 172 described above. The reaction chambers RC1 and RC2 can form part of a process module 554. The reactor system 502 can include one, two, three, four, or more process modules, each of which is fluidly coupled to the third container 520.
[0106] Controller 556 may be similar to the above-described controller 438. Generally, controller 556 can be configured to independently control the temperature of the first container 504, the temperature of the second container 512, and the temperature of the third container 520 to provide a desired flow of reactants from the third container 520 to the first container 504 and / or the second container 512. For example, controller 556 can be configured to automatically increase the temperature of the second container 512 and / or the third container 520 when the amount of reactant 510 in the first container 504 falls below a threshold amount. Additionally or alternatively, controller 556 can be configured to automatically increase the temperature of the third container 520 when the amount of reactant 516 in the second container 512 falls below a threshold amount.
[0107] FIG. 6 illustrates a reactor system 600 according to a further additional embodiment of the present disclosure. Reactor system 600 includes one or more process modules 602, 604, 606, 608, and a reactant delivery system 610.
[0108] Process modules 602-608 can include any suitable process modules such as the process modules described herein. Exemplary process modules 602-608 can include a first reaction chamber RC1, a second reaction chamber RC2, a reactor gas panel 646, and a first container 612, as illustrated in relation to process module 602. Reaction chambers RC1 and RC2, reactor gas panel 646, and first container 612 can be as described above in relation to FIG. 5, for example.
[0109] Reactant delivery system 610 includes a first container 612, a second container 620, a third container 652, and a flow control device 656. According to an embodiment of the present disclosure, each process module 602-608 includes a first container. The second container 620 and / or the third container 652 can be fluidly coupled to one, two, three, four or more process modules.
[0110] The first container 612 is configured to contain a solid raw material reactant 618. The first container 612 can include a first container lid 611 and a first container body 613. The first container 612 includes a first container inlet 615, a first container outlet 617, and another first container inlet 619, which may be the same as or similar to the first container inlets and outlets described above. For example, the first container inlet 615 can receive reactants from the third container 652. The first container inlet 619 can receive a carrier gas. The first container outlet 617 provides the vaporized reactants to line 616, delivering the reactants to the reactor gas panel 646 and ultimately to one or more reaction chambers RC1, RC2. The first container 612 can be included within a first housing 647 that may be the same as or similar to the first housing 519 described above in connection with FIG. 5.
[0111] The second container 620 can be configured to contain a reactant 630 and may be the same as or similar to the second container 414 described above in connection with FIG. 4. As illustrated, the second container 620 may be remote (e.g., by a minimum distance) from one or more of the reactor system 600 and / or the process modules 602 - 608.
[0112] The second container 620 includes a second container lid 625, a second container body 621, and a second container outlet 622. The second container 620 can also include another inlet 623 for receiving the carrier gas described above. The second container outlet 622 or a plurality of second container outlets (e.g., outlets 624 - 628) can be fluidly coupled to each of one or more process modules. The second container 620 can be included within a second housing 634 that may be the same as or similar to the second housing 436 described above. The pressure within the second housing 634 can be as described above in connection with the second housing 436.
[0113] The third container 652 may be the same as or similar to the third container 520 described above in connection with FIG. 5. The third container 652 can include a third container lid 657, a third container body 653, and a third container outlet 654, and can include a third container inlet 655 for receiving a carrier gas. As illustrated, the third container 652 can be configured to hold a solid raw material reactant 660. The third container 652 may be remotely located from the reactor system 600, for example, by the minimum distance described herein. The third container 652 may be enclosed within a third housing 662 that may be the same as or similar to the housing 552 discussed above.
[0114] The conduit 614 fluidly couples the third container outlet 654 to the first container inlet 615.
[0115] The flow control device 656 is within the conduit 614 and can control the amount of vapor of the solid raw material reactant moving from the third container 652 to one or more of the process modules 602-608.
[0116] The reactor gas panel 646 and the reaction chambers RC1, RC2 can be as described above. Similarly, the heaters 632, 633, 658, 659 and the cooling device 670 may be the same as or similar to the heaters and cooling devices described above.
[0117] The reactor system 600 can also include a controller 672. As described above, the controller 672 can be configured to independently control the temperature of the first vessel 612, the temperature of the second vessel 620, and the temperature of the third vessel 652. In particular, the controller 672 can be configured to control the temperature of the first vessel 612 with the temperature gradient described above. Additionally or alternatively, the controller 672 can be configured to automatically heat or cool the vessels to provide the desired reactant transfer as described herein. For example, the controller 672 can automatically increase the temperature of the third vessel 652 when the amount of reactant in the first vessel 612 falls below a threshold amount, such as to fill the first vessel as described above. Additionally or alternatively, the controller 672 can automatically increase the temperature of the second vessel 620 when the amount of reactant in the first vessel 612 falls below a threshold amount, such as to continue to provide reactant to one or more of the process modules 602-608 while the first vessel is being filled.
[0118] (Other Considerations) In the foregoing specification, the invention has been described with reference to specific embodiments thereof. However, it will be apparent that various modifications and changes can be made thereto without departing from the broader spirit and scope of the invention. Accordingly, the specification and drawings are to be regarded in an illustrative rather than a restrictive sense.
[0119] In fact, each of the systems and methods of the present disclosure has several innovative aspects, and it will be understood that no single one of these innovative aspects is solely responsible for or required for the desirable attributes disclosed herein. The various features and processes described herein can be used independently of each other or combined in various ways. All possible combinations and sub-combinations are intended to be within the scope of the present disclosure.
[0120] The specific features described herein in connection with separate embodiments may also be implemented in combination in a single embodiment. Conversely, the various features described in connection with a single embodiment may also be implemented separately, or in any suitable sub-combination, in a plurality of embodiments. Further, features may be described herein as functioning in a particular combination and may initially be claimed as such, but one or more features from the claimed combination may, optionally, be excluded from the combination and the claimed combination may be directed to a sub-combination or variation of a sub-combination. Neither a single feature nor a group of features is necessary or indispensable to all embodiments.
[0121] Conditional language used herein, such as in particular "can", "could", "might", "may", "for example" and the like, is generally intended to convey that a particular embodiment includes a particular feature, element and / or step, but other embodiments do not, unless otherwise specified or understood within the context in use. Thus, such conditional language is generally not intended to suggest that a feature, element, and / or step is required in any way in one or more embodiments, or that one or more embodiments necessarily include logic for determining whether these features, elements and / or steps are included in or implemented in any particular embodiment, regardless of the author's input or instructions. "Comprising", "including", "having" and the like are synonyms and are used in an inclusive, open-ended fashion and do not exclude additional elements, features, acts, operations, etc. Also, since the term "or" is used in an inclusive sense (and not in an exclusive sense), for example when used to concatenate a list of elements, the term "or" means one, some, or all of the elements in the list. Additionally, the articles "a", "an", and "the" used in this application and the appended claims should be construed to mean "one or more" or "at least one" unless otherwise specified. Similarly, operations may be depicted in the drawings in a particular order, but such operations need not be performed in the particular order or sequential order shown to achieve the desired result, and it should be recognized that not all of the operations illustrated need to be performed. Further, the drawings may schematically depict another exemplary process in the form of a flowchart. However, other operations not depicted may be incorporated into the exemplary methods and processes schematically illustrated. For example, one or more additional operations may be performed before, after, simultaneously with, or between any of the operations illustrated. Further, in other embodiments, the operations may be rearranged or reordered. In certain situations, multitasking and parallel processing may be advantageous.Furthermore, the separation of the various system components in the embodiments described herein should not be understood as requiring such separation in all embodiments, and it should be understood that the described components and systems may generally be integrated together into a single product or packaged into multiple products. Further, other embodiments are within the scope of the following claims. In some cases, the acts recited in the claims may be performed in a different order and still achieve desirable results.
[0122] Accordingly, the claims are not intended to be limited to the embodiments shown herein but rather to be in the broadest scope consistent with the disclosure, the principles and features disclosed herein. For example, many of the examples within the disclosure are provided with respect to supplying vapor from a solid source for supply to a deposition chamber for semiconductor manufacturing, but certain embodiments described herein may be practiced in a variety of other applications and / or numerous other situations.
Claims
Claim 1 A reactant delivery system comprising: a first container having a first container inlet and a first container outlet, the first container forming part of a reactor system and configured to hold a solid raw material reactant; a first housing surrounding the first container; a second container having a second container outlet, the second container being external to the first housing and remote from the reactor system, the second container being configured to hold the solid raw material reactant; a conduit fluidly coupled to the second container outlet and the first container inlet; a flow control device in the conduit for controlling the amount of vapor of the solid raw material reactant moving from the second container to the first container; and the reactant delivery system, wherein the pressure within the first housing is less than the ambient pressure external to the first housing. Claim 2 The reactant delivery system according to claim 1, further comprising a valve plate within the first housing, the valve plate comprising one or more valves fluidly coupled to the first container outlet. Claim 3 The reactant delivery system according to claim 1, further comprising a pressure transducer for measuring the pressure within the conduit. Claim 4 The reactant delivery system according to claim 1, wherein the flow control device comprises one or more of a mass flow controller and a mass flow meter. Claim 5 The reactant delivery system according to claim 1, wherein the pressure within the first housing is between 1 Torr and less than atmospheric pressure, or between 10 Torr and 20 Torr. Claim 6 The reactant delivery system according to claim 1, further comprising a second housing surrounding the second container, wherein the pressure within the second housing is greater than the pressure within the first housing. Claim 7 The reactant delivery system according to claim 1, further comprising a controller for controlling the temperature of the first container and the temperature of the second container. Claim 8 The reactant delivery system according to claim 7, wherein the controller is configured to adjust the temperature of the bottom portion of the first container to be lower than the temperature of the upper portion of the first container. Claim 9 The reactant delivery system according to claim 7, wherein the controller is configured to automatically heat the second container when the amount of reactant within the first container falls below a threshold amount. Claim 10 A reactant delivery system, comprising: A first container having a first container inlet and a first container outlet, wherein the first container forms part of a reactor system and is configured to hold a solid raw material reactant; a first container; A second container having a second container outlet and a second container inlet, wherein the second container is configured to hold the solid raw material reactant; a second container; A third container having a third container outlet, which is remote from the reactor system and is configured to hold the solid raw material reactant; a third container; A conduit fluidly coupling the third container outlet to the first container inlet and to the second container inlet; A flow control device in the conduit for controlling the amount of vapor of the solid raw material reactant moving from the third container to one or more of the first container or the second container; A reactant delivery system, wherein the first container outlet and the second container outlet are fluidly coupled to a reaction chamber.
11. The reactant delivery system according to claim 10, further comprising a heater for heating the conduit.
12. The reactant delivery system according to claim 10, wherein the first container and the second container are enclosed within a first housing.
13. The reactant delivery system according to claim 10, wherein the third container is enclosed within a second housing.
14. The reactant delivery system according to claim 10, further comprising a controller configured to independently control the temperature of the first container, the temperature of the second container, and the temperature of the third container.
15. The reactant delivery system according to claim 14, wherein the controller is configured to automatically increase the temperature of the second container when the amount of reactant in the first container falls below a threshold amount.
16. The reactant delivery system according to claim 10, wherein the first container is within a first housing, the second container is within a second housing, and the third container is within a third housing.
17. The reactant delivery system according to claim 10, wherein the second container is remote from the reactor system.
18. A reactor system, comprising: One or more process modules; and A reactant delivery system, wherein the reactant delivery system is... A first container having a first container inlet and a first container outlet, the first container forming part of the reactor system and being configured to hold a solid raw material reactant, the first container; A second container having a second container outlet, the second container being configured to hold the solid raw material reactant, the second container; A third container having a third container outlet, the third container being remote from the reactor system and being configured to hold the solid raw material reactant, the third container; A conduit fluidly coupling the third container outlet to the first container inlet; A flow control device in the conduit for controlling the amount of vapor of the solid raw material reactant moving from the third container to the one or more process modules; and A reactor system in which the second container outlet is fluidly coupled to each of the one or more process modules. **Claim 19** The reactor system according to claim 18, further comprising a controller configured to independently control the temperature of the first container, the temperature of the second container, and the temperature of the third container. **Claim 20** The reactor system according to claim 19, wherein the controller is configured to automatically increase the temperature of the third container when the amount of reactant in the first container falls below a threshold amount.
Citation Information
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