Precursor container system and method

Abstract

A method can include heating a source container including a solid precursor to a predetermined temperature; in response to heating the source container, sublimating or vaporizing a first portion of the solid precursor in the source container to produce a precursor gas, thereby increasing a headspace volume in the interior space to a second volume; flowing the precursor gas out of the source container; and / or in response to sublimating or vaporizing the first portion of the non-gaseous precursor, moving a movable bottom to decrease the headspace volume toward the first volume.

Description

Technical Field

[0001] This disclosure generally relates to systems and methods for gas phase processing. More specifically, this disclosure relates to methods and systems for delivering precursors to a gas phase reactor system. Background Technology

[0002] Semiconductor manufacturing processes such as chemical vapor deposition (CVD) and atomic layer deposition (ALD) may involve depositing thin films on a semiconductor wafer (also referred to herein as a “substrate”). During processing, the wafer is exposed to one or more precursors in a reaction chamber to deposit a thin layer of material. The precursors may be stored in a delivery or source container from which they are delivered to the reaction chamber for processing. As precursors are added to or removed from the source container, the unoccupied volume within the source container can be altered, which can change the conditions within the source container (e.g., temperature and / or pressure). This change can lead to undesirable variations in precursor delivery (e.g., the rate at which precursors are delivered to the reaction chamber) during processing. Summary of the Invention

[0003] This invention is provided to introduce some concepts in a simplified form. These concepts are further described in detail in the following detailed description of exemplary embodiments of this disclosure. This invention is not intended to necessarily identify key or essential features of the claimed subject matter, nor is it intended to limit the scope of the claimed subject matter.

[0004] Systems and methods relating to reactor systems are disclosed. In various examples, the reactor system may include a source container comprising a non-gaseous (e.g., solid or liquid) precursor; a reaction chamber fluidly coupled to the source container via a gas line such that a precursor gas sublimated or vaporized from the non-gaseous precursor may flow from the source container to the reaction chamber; and / or a pressure sensor coupled to the gas line and / or the source container, configured to measure the pressure of the precursor gas flowing through or within the gas line and / or the source container.

[0005] In various examples, one method may include: heating a source container to a predetermined temperature, wherein the source container includes a movable bottom and a wall system, the wall system at least partially defining an interior space in which a non-gaseous precursor is disposed, wherein the interior space includes a headspace volume having a first volume above the precursor; in response to heating the source container, causing a first portion of the non-gaseous precursor in the source container to sublimate and / or vaporize to generate a precursor gas, thereby increasing the headspace volume in the interior space to a second volume; allowing the precursor gas to flow out of the source container; and / or moving the movable bottom in response to the sublimation or vaporization of the first portion of the non-gaseous precursor to reduce the headspace volume toward the first volume. Moving the movable bottom may occur substantially simultaneously with at least one of (a) sublimation or vaporization of the first portion of the non-gaseous precursor or (b) allowing the precursor gas to flow out of the source container. The method may further include maintaining the headspace volume at a substantially constant volume. The method may also include adding more non-gaseous precursors to the source container, thereby reducing the headspace volume in the internal space; and / or lowering the movable bottom to increase the headspace volume toward the first volume. In various examples, moving the movable bottom may include applying pressure to the movable bottom in response to precursor gas outflow from the source container. The movable bottom may include a telescopic structure, wherein moving the movable bottom includes deploying the telescopic structure into a second volume when precursor gas flows out of the source container; and / or lowering / folding the telescopic structure when non-gaseous precursors are added to the source container. The movable bottom may be configured to move between a raised position and a lowered position.

[0006] In various examples, the method may include adding a non-gaseous precursor to the interior space of a source container, wherein the source container includes a movable bottom and a wall system that at least partially defines the interior space, wherein the interior space includes a headspace volume having a first volume above the non-gaseous precursor. In response to the addition of the non-gaseous precursor, the headspace volume in the interior space may decrease to a second volume. The method may also include moving the movable bottom to increase the headspace volume in response to adding the non-gaseous precursor to the interior space. The method may further include maintaining the headspace volume at a substantially constant level. The method may also include monitoring the headspace volume in the interior space by a processor; and / or detecting a change in the headspace volume in the interior space by a processor in response to the addition of the non-gaseous precursor to the interior space. Moving the movable bottom may be in response to detecting a change in the headspace volume. The method may also include removing a portion of the non-gaseous precursor from the interior space of the source container, thereby increasing the headspace volume in the interior space; and / or moving the movable bottom in response to the increase in headspace volume.

[0007] In various examples, a method may include adding a non-gaseous precursor to the interior space of a source container, wherein the source container includes a movable bottom and a wall system that at least partially defines the interior space, wherein the interior space includes a headspace volume having a first volume above the non-gaseous precursor; moving the movable bottom, wherein the non-gaseous precursor is disposed on the movable bottom; and / or agitating the non-gaseous precursor. The method may further include distributing the non-gaseous precursor at least partially on the movable bottom in response to agitation of the non-gaseous precursor. The method may further include sublimating and / or vaporizing a first portion of the non-gaseous precursor in the source container to generate a precursor gas; causing the precursor gas to flow out of the source container in response to the sublimation or vaporization of the first portion of the non-gaseous precursor, thereby causing an increase in the headspace volume in the interior space; and / or moving the movable bottom to decrease the headspace volume in response to the flow of the precursor gas out of the source container.

[0008] For the purpose of outlining this disclosure and the advantages achieved relative to the prior art, certain objects and advantages of this disclosure have been described above. It should be understood, of course, that not all of these objects or advantages may necessarily be achieved according to any particular example of this disclosure. Therefore, for example, those skilled in the art will recognize that this disclosure may be embodied or implemented in a manner that achieves or optimizes one or more advantages as taught or suggested herein.

[0009] All these examples are intended to fall within the scope of the disclosure herein. These and other examples will become apparent to those skilled in the art from the following detailed description of some examples with reference to the accompanying drawings, and this disclosure is not limited to any particular example disclosed. Attached Figure Description

[0010] A more complete understanding of the present technology can be obtained by referring to the specific embodiments when considered in conjunction with the following illustrative drawings. In the following drawings, the same reference numerals refer to similar elements and steps throughout all the drawings.

[0011] Figure 1A These are schematic diagrams of reactor systems based on various examples.

[0012] Figure 1B It is based on various examples Figure 1A A schematic diagram of the source vessel of the reactor system.

[0013] Figure 2 Representative examples of source containers with movable bottoms are shown, based on various examples.

[0014] Figure 3A The movable bottom of the source container in its fully contracted position is shown representatively according to various examples.

[0015] Figure 3B The movable bottom of the source container in the first intermediate position is shown representatively according to various examples.

[0016] Figure 3C The movable bottom of the source container in the second intermediate position is shown representatively according to various examples.

[0017] Figure 3D The movable bottom of the source container in the third intermediate position is shown representatively according to various examples.

[0018] Figure 3E The movable bottom of the source container in its fully expanded position is shown representatively according to various examples.

[0019] Figure 4 Methods including a source container, which includes a movable bottom, are described according to various examples.

[0020] Figure 5 Methods for agitating non-gaseous precursors in a source container are described according to various examples.

[0021] It should be understood that the elements in the accompanying drawings are shown for simplicity and clarity and are not necessarily drawn to scale. For example, the relative dimensions of some elements in the drawings may be exaggerated relative to other elements to aid in understanding the examples shown in this disclosure. Detailed Implementation

[0022] The descriptions of the methods, structures, devices, and systems provided below are merely exemplary and intended for illustrative purposes only. The following descriptions are not intended to limit the scope of this disclosure or the claims. Furthermore, the recitation of multiple examples having the described features is not intended to exclude other examples having additional features or other examples containing different combinations of the described features. For example, various examples are set forth as embodiments and may be recited in the dependent claims. Unless otherwise stated, examples or components thereof may be combined or may be applied separately from each other. Methods may include the disclosed steps (including mixed / combined steps from methods depicted in individual figures) in any suitable and / or desired order or combination.

[0023] As used herein, the term “and / or” includes any and all combinations of one or more of the associated listed items. Unless otherwise stated, expressions such as “at least one of…” modify the entire column of elements when following an element in the column, and not necessarily a single element in that column.

[0024] As used herein, the terms “includes,” “comprises,” “including,” and / or “comprising” specify the presence of the stated feature, integer, step, process, component, part, and / or group thereof, but do not exclude the presence or addition of one or more other features, integers, steps, processes, components, parts, and / or groups thereof. In some examples within this disclosure, the meaning of any definition does not necessarily exclude its common and customary meaning.

[0025] As used herein, the term "substrate" can refer to any one or more underlying materials, including any one or more underlying materials that can be modified or on which devices, circuits, or films can be formed. A "substrate" can be continuous or discontinuous; rigid or flexible; solid or porous; and combinations thereof. A substrate can be in any form, such as powder, plate, or workpiece. Plate-type substrates can include wafers of various shapes and sizes. Substrates can be made of semiconductor materials, including, for example, silicon, silicon germanium, silicon oxide, gallium arsenide, gallium nitride, and silicon carbide.

[0026] In some examples, "membrane" refers to a layer extending in a direction perpendicular to the thickness direction. In some examples, "layer" refers to a material of a certain thickness formed on a surface, and can be synonymous with membrane or non-membrane structures. A membrane or layer can consist of discrete single membranes or layers or multiple membranes or layers with certain properties, and the boundaries between adjacent membranes or layers may or may not be clear, and can be established based on or not based on the physical, chemical and / or any other properties, formation process or sequence, and / or function or purpose of adjacent membranes or layers. A layer or membrane can be continuous or discontinuous. Furthermore, a single membrane or layer can be formed using one or more deposition cycles and / or one or more deposition and processing cycles.

[0027] As used herein, the term "structure" can refer to a device structure that is partially or fully fabricated. For example, a structure can be a substrate or a substrate having one or more layers and / or features formed thereon.

[0028] In this disclosure, any two numbers of a variable may constitute a feasible range of the variable, and any range indicated may include or exclude endpoints, and may combine all ranges and ratio limits disclosed herein. Furthermore, any value of the indicated variable (whether or not it is indicated by “about”) may refer to an exact value or an approximate value and include equivalents, and in some examples may refer to the mean, median, representative value, multi-value, etc. Unless otherwise specified, references to “a,” “an,” and / or “the” may include one or more, and references to singular items may also include plural items. When referring to components of the system discussed herein, the term “connection” means a direct connection or an indirect connection with other intermediate elements, as appropriate. Unless otherwise stated, the terms “first,” “second,” etc., and / or “primary,” “secondary,” etc., are used herein merely as labels and are not intended to impose any order, position, or hierarchy requirements on the items referred to by these terms. Furthermore, references to items such as “second” do not require or exclude the existence of items such as “first” or lower numbered items and / or items such as “third” or higher numbered items. Furthermore, references to items such as "first" and "second" do not imply the absence of intermediate items, and such intermediate items may exist.

[0029] Reactor systems for ALD, CVD, etc., can be used in a variety of applications, including depositing and etching materials on substrate surfaces. A reactor system may include a precursor container (i.e., a delivery container or a source container) in which chemical precursors can be stored and transported from the container to another component of the reactor system (e.g., a reaction chamber) for processing. A precursor container may include a source container configured to contain solid or liquid (i.e., non-gaseous) precursors (“precursor container,” “delivery container,” and / or “source container” are used interchangeably herein).

[0030] The source container may include a source precursor (which may also be referred to as a "reactant," "chemical," or "chemical precursor"), which may be a solid (e.g., in powder form) (which may also be referred to as a "solid precursor") or a liquid. As used herein, a "non-gaseous precursor" may be a precursor that does not sublimate or vaporize, and is therefore in solid or liquid form. A heater (e.g., a radiant heater, resistance heater, etc.) coupled to and / or in thermal communication with the source container may heat the source container to facilitate the vaporization and / or sublimation of the chemical precursor in the source container. The source container may include any suitable shape or size, such as rectangular, square, and / or cylindrical. The source container may have an inlet and an outlet for allowing a carrier gas to flow through the source container. The carrier gas may be inert, such as nitrogen, argon, or helium. Typically, the carrier gas carries the reactant vapor (i.e., the precursor gas) (e.g., the vaporized or sublimated chemical reactant) along with it through the container outlet and ultimately to the reaction chamber. In various examples, the source container includes, is substantially composed of, or is composed of, a sublimator and / or a vaporizer. Therefore, wherever “solid source container” is mentioned in this document, sublimators (e.g., “solid source chemical sublimator”) and / or vaporizers are also envisioned.

[0031] In various examples, each chemical reactant can be stored in a source container. For some solid substances (referred to herein as "solid source precursors," "solid precursors," "solid chemical reactants," "solid reactants," etc.), the vapor pressure at room temperature is very low, so they are typically heated and / or kept at very low pressures to produce sufficient quantities of reactant vapor for the reaction process. Gas-phase reactants (i.e., precursor gases) from solid or liquid substances can be used in chemical reactions in a variety of industries.

[0032] In various examples, the source container may include a movable bottom. The movable bottom may define the lower boundary of the internal space of the source container. The movable bottom may move up and down (or in any other suitable direction) or translate, thereby changing the volume of the internal space in which chemical precursors may be placed. In various examples, the movable bottom may include a movable platform that moves up and down (e.g., it is curved, substantially flat, or any other suitable configuration). The movable bottom may move between a lower position and an elevated position, and / or move to an intermediate position between the lower and elevated positions. In various examples, the movable bottom may include a telescopic structure (e.g., including concentric portions that can slide / fold into or unfold from itself). For the telescopic structure, the lower position may be a contracted or folded position, and the elevated position may be an unfolded position.

[0033] In various examples, the movable bottom can be manually, mechanically, or electromechanically controlled or facilitated, and / or can be partially or fully automated, for example, using one or more sensors controlled by a controller and / or processor for automatic feedback. In various examples, the reactor system may include one or more pressure sensors (i.e., pressure transducers, transmitters, etc.). The pressure sensors can be configured to measure pressure within the source container and / or gas lines, for example, in response to the sublimation or vaporization of a chemical precursor in the source container, through which the precursor gas travels between components of the reactor system (e.g., between the source container and the reaction chamber). In various examples, the controller and / or processor can communicate electronically (or be operatively coupled) to one or more pressure sensors, such that the controller and / or processor can receive pressure readings or data from the pressure sensors and / or various other components of the system to perform various functions, operations, movements, etc.

[0034] Figure 1A This is a schematic diagram illustrating an example reactor system 100, which includes a source container 102 and / or one or more reactors 138 and 140, each reactor including a corresponding reaction chamber 122 and 124. Reactors 138 and 140 may include corresponding bases 142 and 144 to hold corresponding substrates 146 and 148 during processing, and gas distribution systems 150 and 152 to distribute one or more reactants / precursors onto the corresponding surfaces of substrates 146 and 148. Reactor system 100 may include a vacuum source for controlling the vacuum pressure in one or more of the reaction chambers 122 and 124. The reactant source may feed gaseous reactants generated from the source container 102, which includes non-gaseous precursors, into the gas-phase reactor. Reactors 138 and / or 140 may be gas-phase reactors. Source container 102 may contain a solid precursor 114 (e.g., in a solid state). Solid chemicals may include chemical reactants, including, for example, HfCl4, ZrCl4, AlCl3, TaF5, MoF5, and / or SiI4. Solid precursor 114 may be solid under standard conditions (e.g., room temperature and atmospheric pressure). It should be understood that systems and methods involving solid precursors within a source container and their sublimation into gaseous precursors can also be applied to liquid precursors within a source container and their vaporization into gaseous precursors.

[0035] A carrier gas source 120 may be coupled to a source container 102 via a carrier gas line 136 and may contain a carrier gas. A cover 130 of the source container 102 may include a carrier gas valve 119 or have a carrier gas valve attached thereto to regulate the flow of carrier gas from the carrier gas source 120 into the source container 102. The carrier gas source 120 may be fluidly coupled to reaction chambers 122 and 124 via a gas line 154 and valves 158 and 160. In various examples, valves 158 and 160 may be controlled by one or more controllers. In response to being introduced into the source container 102, the carrier gas may assist in delivering vaporized and / or sublimated chemical reactants through the container outlet valve 126 to reaction chambers 122 and / or 124. The chemical delivery line 128 may include valves 132 and 134 for controlling fluid communication of the solid precursor 114 (gas phase) and / or the carrier gas from the source container 102 to the respective reaction chambers 122 and 124.

[0036] Source container 102 may be thermally coupled to one or more heating devices 176 (e.g., heaters, heating jackets, heating blocks, and / or radial heaters) and / or one or more cooling devices 186. Such heating or cooling devices can be used to control or regulate the temperature of the solid precursor 114 during refilling operations, material processing operations, and / or storage. Cooling devices 186 may include cooling plates, cooling coils, variable pitch cooling coils, cooling jackets, cooling fans, Peltier coolers, and / or integrated coolant channels for circulating coolant. As discussed in more detail herein, such heating devices 176 and cooling devices 186 can provide a temperature gradient within source container 102.

[0037] In various examples, heating device 176 may be coupled to and / or in thermal communication with source container 102 (e.g., at wall system 178 (e.g., container body or shell) and / or lid 130). Wall system 178 and / or lid 130 may be configured to transfer heat and / or pressure from heating device 176 to solid precursor 114 (e.g., to vaporize or sublimate solid precursor 114 to flow through chemical delivery line 128). Removable bottom 192 may be cooled by cooling device 186 (e.g., cold plate) to a lower temperature than the sidewalls of wall system 178 and / or lid 130 of source container 102. This can provide a temperature gradient along longitudinal axis 194, where the highest temperature in the system may be located at the top portion 190 of source container 102, while the lowest temperature in the system may be located at or near the movable bottom 192.

[0038] A temperature gradient extends between the movable bottom 192 and the top portion 190, including the cover 130. In various examples, the movable bottom 192 may be maintained at or below a first threshold temperature, while the top portion 190 may be maintained at or above a second threshold temperature. In various examples, the temperature difference between the movable bottom 192 and the top portion 190 may be at least about 1°C, about 5°C, about 10°C, about 20°C, about 40°C, about 80°C, or about 160°C, or any value between these, or fall within any range with endpoints.

[0039] In various examples, during material handling operations, heating device 176 can be configured to heat solid precursor 114 to a temperature sufficient to change the phase of solid precursor 114, for example, to liquefy and / or sublimate solid precursor 114 (and / or vaporize liquid precursor in source container 102). Once vaporized or sublimated into a gaseous precursor, the gaseous precursor can be delivered via chemical delivery line 128 to reaction chambers 122 and / or 124 for substrate treatment. Solid precursor 114 can be stored as a solid in source container 102 prior to vaporization and / or sublimation. Alternatively, solid precursor 114 can be stored in a liquid phase (as a liquid precursor). Heating device 176 can be configured to heat source container 102 to a temperature sufficient to vaporize or sublimate the solid or liquid precursor in source container 102.

[0040] Reactor system 100 may include controller 156, which includes processor 164, user interface 166, and / or memory 168. Processor 164 may be operatively connected to user interface 166 (e.g., to receive user input and / or provide user output therethrough) and may be configured to communicate with memory 168. Memory 168 includes a tangible, non-transitory machine-readable medium thereon storing a plurality of program modules / instructions 172 that cause processor 164 to perform certain operations in response to reading and / or execution by processor 164. These operations include operations of material layer deposition methods, methods for refilling source container 102, methods for determining precursor transfer, and / or methods for moving movable bottom 192, as discussed herein. As those skilled in the art will understand in light of this disclosure, controller 156 may have different arrangements or configurations in other examples, and remain within the scope of this disclosure.

[0041] Continue to refer to Figure 1AThe reactor system 100 may include one or more pressure sensors 97, 98 (i.e., pressure transducers, transmitters, etc.). Pressure sensor 97 may be coupled to source container 102 and / or configured to measure pressure within source container 102. Pressure sensor 98 may be coupled to chemical delivery line 128 and / or configured to measure pressure within chemical delivery line 128. For example, pressure sensor 97 may detect pressure during the vaporization and / or sublimation of a non-gaseous precursor in source container 102, and / or in response to the pressure of a non-gaseous precursor added to source container 102 or a gaseous precursor flowing out of source container 102. In various examples, pressure sensors 97, 98 may sense pressure automatically, partially automatically, or manually and / or detect changes in pressure. In some examples, the processor may detect changes in the amount of solid precursor 114. In some examples, the processor may receive pressure readings or data from pressure sensor 97. In response, the processor may determine or detect changes in the volume of internal space 180 (e.g., headspace volume as discussed herein).

[0042] Figure 1B This is a schematic diagram of a source container 102 according to various examples. The source container 102 includes a wall system 178 that at least partially defines an interior space 180. The source container 102 may also include a movable bottom 192, which may at least partially define the interior space 180. The movable bottom 192 may be used as the lower boundary of the interior space 180, which includes non-gaseous precursors.

[0043] A non-gaseous precursor may be disposed within the internal space 180 (e.g., a solid precursor 114). The portion of the internal space 180 above the non-gaseous precursor is the headspace volume 188. The headspace volume 188 may vary with the amount of non-gaseous precursor. For example, the headspace volume 188 may become larger as the non-gaseous precursor vaporizes and / or sublimates, or it may become smaller as the non-gaseous precursor is added to the source container 102.

[0044] In response to a change in headspace volume 188, the movable bottom 192 can move to different locations. For example, pressure sensors 97 and / or 98 can detect the pressure within source container 102 and / or chemical delivery line 128 and transmit the pressure data to controller 156 (e.g., to processor 164). Controller 156 can receive the pressure data and determine the pressure change within source container 102 and / or chemical delivery line 128 based on the received pressure data. Based on the pressure data and / or the determined pressure change, controller 156 can determine the change in headspace volume 188, and in response, controller 156 can command the movable bottom 192 to move to compensate for the increase or decrease in headspace volume 188. Thus, the objective could be to keep headspace volume 188 as consistent as possible (e.g., substantially constant). The movable bottom 192 can be moved in any suitable manner, such as via a motor 195 operably coupled to the movable bottom 192 (e.g., mechanical and / or electromechanical movement), via gas injection below the movable bottom 192 such that the pressure below determines the position of the movable bottom 192 between a lower position and a raised position, and / or similar means.

[0045] Figure 2 Source container 200 (an example of source container 102) is shown according to various examples. Source container 200 may include wall system 278 (an example of wall system 178) that at least partially defines interior space 212 (an example of interior space 180). Source container 200 may also include a movable bottom 292 (an example of movable bottom 192). Movable bottom 292 may at least partially define interior space 212. In various examples, the location of the movable bottom may determine the amount of space provided by interior space 212 that can accommodate or include non-gaseous precursors.

[0046] The source container may include a connection portion 215 (e.g., as part of or coupled to wall system 278). The source container 200 may include a carrier gas inlet 219 (e.g., included in the connection portion 215). The carrier gas inlet 219 (an example of a carrier gas inlet controlled by carrier gas valve 119) may be fluidly coupled to a carrier gas source (e.g., carrier gas source 120) and may be configured to allow carrier gas flow through it and into the source container 200. For example, carrier gas valve 217 may regulate the flow of carrier gas through carrier gas inlet 219 and into the interior space 212. The source container 200 may include a container outlet 226 (e.g., included in the connection portion 215). The container outlet 226 (an example of a container outlet controlled by container outlet valve 126) may be fluidly coupled between the interior space 212 of the source container 200 and the reaction chamber, such that gaseous precursors (and / or carrier gas) may flow from the interior space 212 through container outlet 226 and to a next destination within the reactor system (e.g., the reaction chamber).

[0047] A non-gaseous precursor (e.g., solid precursor 214) may be disposed within the internal space 212 of the source container 200. Solid precursor 214 may be disposed on a movable bottom 292. The volume above the non-gaseous precursor within the internal space 212 may be a headspace volume 288 (an example of headspace volume 188). Therefore, headspace volume 288 may change in response to vaporization and / or sublimation of the non-gaseous precursor within the source container 200, and / or in response to the addition of more non-gaseous precursor into the internal space 212.

[0048] The movable bottom 292 can be moved to change the headspace volume 288. For example, the movable bottom 292 can be moved to maintain the headspace volume 288 at a substantially constant volume (e.g., increasing or decreasing in response to the addition or removal of a non-gaseous precursor). Therefore, the movable bottom 292 can move between positions such as 204, 206, 208, and / or 210. The movable bottom 292 may include a telescopic structure. Thus, position 204 can be a fully folded or retracted position (i.e., a lower position), positions 206 and 208 can be intermediate positions, and / or position 210 can be a fully extended position (i.e., an elevated position).

[0049] In various examples, pressure sensor 297 may be (e.g., physically, electronically, operatively, etc.) coupled to source container 200 and may be configured to measure or detect pressure within source container 200 (and / or internal space 212). Pressure within source container 200 may be monitored, for example, via pressure sensor 297 and / or a controller (e.g., controller 156). Based on pressure data received from pressure sensor 297, controller (and / or processor therein) may determine headspace volume 288 when a non-gaseous precursor is added to or removed from internal space 212, and may monitor headspace volume 288 and its changes. In various examples, processor may automatically detect changes in headspace volume 288. In various examples, based on pressure from pressure sensor 297 and / or detected changes in headspace volume 288, processor may determine and / or detect changes in the amount of solid precursor 214 in internal space 212.

[0050] The movable bottom 292 can be configured to move in response to a change in pressure or non-gaseous precursor quantity detected by the controller and / or processor within the source container 200. For example, in response to the processor detecting an increase in headspace volume 288 (e.g., due to the sublimation of solid precursor 214 and / or the outflow of gaseous precursor from the source container 200 via container outlet 226), the controller / processor can command the movable bottom 292 to move to a position above its current position to reduce headspace volume 288 (e.g., from position 204 to position 206). The movable bottom 292 can move accordingly. As another example, in response to the processor detecting a decrease in headspace volume 288 (e.g., due to the addition of solid precursor 214 to the source container 200), the controller and / or processor can command the movable bottom 292 to move to a position below its current position to increase headspace volume 288 (e.g., from position 206 to position 204). The movable bottom 292 can move accordingly. In various examples, the controller and / or processor can determine changes in pressure and / or the amount of non-gaseous precursor in source container 200 in real time or near real time (e.g., within less than 1, 3, 5, 10, or 30 seconds), and in response, the movable bottom 292 can move substantially simultaneously. That is, the movable bottom can be configured to move substantially simultaneously with the sublimation or vaporization of the non-gaseous precursor and / or with the gaseous precursor flowing out of source container 200 (generated by the vaporization or sublimation of the non-gaseous precursor). Thus, in various examples, the movable bottom can maintain a substantially constant headspace volume 288, which can minimize and / or prevent fluctuations in parameters (e.g., pressure and / or temperature) within source container 200 that could lead to changes in processing (e.g., changes in the rate and / or amount of precursor delivery to the reaction chamber).

[0051] As discussed herein, the movable bottom 292 can be raised or lowered in any suitable manner, for example, via a motor (e.g., motor 195) and / or via hydraulic pressure or pressure (via liquid or gas). In various examples, source container 200 may include an expansion gas system 280. The expansion gas system 280 may include an expansion gas inlet 289 and an expansion gas outlet 286. The expansion gas inlet 289 may be fluidly coupled to a gas source (e.g., a non-reactive or inert and / or atmospheric gas source). The gas source may supply gas to source container 200 to cause the movable bottom 292 to expand or rise. To raise the movable bottom 292, expansion gas may flow through the expansion gas inlet 289, increasing the pressure below the movable bottom 292, thereby raising the movable bottom 292 to a higher position. To lower the movable bottom 292, expansion gas disposed below the movable bottom 292 may be released via the expansion gas outlet 286, thereby reducing the pressure below the movable bottom 292, thus lowering the movable bottom 292 to a lower position.

[0052] Figures 3A-3E A source container 300 is representatively shown, comprising a movable bottom 392 and a container base 378. A wall system may be coupled to the base 378 to at least partially define the internal space of the source container 300 (e.g., utilizing the movable bottom 392). The movable bottom 392 may include a telescopic structure 312. The telescopic structure may include multiple nested segments that can fold / retract together and / or be arranged side-by-side to lower the movable bottom 392 and / or unfold to raise the movable bottom 392. In various examples, the movable bottom 392 may be configured to unfold or fold (i.e., raise or lower) between multiple different locations 302, 304, 306, 308, and / or 310.

[0053] Position 302 can be a fully retracted / folded position (lower or lowest position), positions 304, 306, and / or 308 can be intermediate positions, and / or position 310 can be a fully extended position (raised position). That is to say, Figure 3A The fully retracted / folded position 302 (lower or lowest position) of the movable bottom 392 of the source container 300 is shown representatively. Figure 3B The image represents the middle position 304 of the movable bottom 392 of the source container 300. The middle position 304 can be a position higher than the folded position 302. Figure 3C The image shows a representative example of the middle position 306 of the movable bottom 392 of the source container 300. The middle position 306 can be a position higher than positions 304 and 302. Figure 3D The image shows a representative view of the middle position 308 of the movable bottom 392 of the source container 300. The middle position 308 is a higher position than positions 306, 304, and 302. Figure 3E The image represents the deployed position 310 (raised or highest position) of the movable bottom 392 of the source container 300. The deployed position 310 is a higher position than positions 308, 306, 304, and 302. The movable bottom 392 may contain and / or support a solid precursor 314 within the source container 300 (the movable bottom 392 may also be used to contain and raise / lower a liquid precursor).

[0054] In various examples, during operation, a first portion of the solid precursor 314 (the internal space of source container 300 is surrounded by a wall system) can sublimate to generate a precursor gas (e.g., in response to heating the source container). In response to the sublimation of the solid precursor 314, the headspace volume (e.g., headspace volume 288 of source container 200) increases (because there is less solid precursor 314 present, and therefore more space above the solid precursor 314 in source container 300). In response to the increase in headspace volume 188, the movable bottom 392 can be moved to a different location (e.g., a higher location). For example, the movable bottom 392 can be moved from a lower location (e.g., location 302) to a higher location (e.g., one or more of locations 304, 306, 308, and / or 310) to reduce the headspace volume (e.g., to maintain the headspace volume at a substantially constant level).

[0055] In various examples, a solid precursor 314 can be added to the source container 300, which can reduce the headspace volume in the internal space. In response, the movable bottom 392 can be lowered to a lower position to increase the headspace volume (e.g., to maintain the headspace volume at a substantially constant level). "Substantially constant" can mean within 10% or 20% of the headspace volume before and after adding or removing a non-gaseous precursor from the source container.

[0056] refer to Figure 2 and Figure 4 The diagram illustrates a method 400 utilizing a source container 200 including a movable bottom 292. The source container 200 may include a non-gaseous precursor disposed therein, resting on the movable bottom 292. The non-gaseous precursor may be a solid or liquid precursor (e.g., solid precursor 214). The source container 200 including the non-gaseous precursor may be heated (step 402). In response, at least a portion of the non-gaseous precursor may sublimate or vaporize (step 404) (i.e., a portion of the non-gaseous precursor may become a gaseous precursor). This heating may be achieved, for example, by a heating device in thermal communication with the source container 200 (e.g., [other device]). Figure 1BThis is accomplished by the heating device 174 in the source container 200. In response to the formation of the precursor gas, the precursor gas can flow out of the source container 200 (step 406) (e.g., through the container outlet 226 toward the reaction chamber). Sublimation and / or vaporization of the non-gaseous precursor can cause an increase in the headspace volume 288 above the non-gaseous precursor. In response, the movable bottom 192 can be moved (step 408). For example, a pressure sensor 297 (e.g., in conjunction with a processor) can measure the pressure in the source container 200 (or its internal space 212). The processor can receive pressure readings from the pressure sensor 297. Based on the pressure readings, the processor can determine the headspace volume 288, the change in the headspace volume 288, and / or the reduction in the amount of the non-gaseous precursor. In response to determining that the headspace volume in the source container 200 has increased, and / or the amount of the non-gaseous precursor has decreased, the processor can command or otherwise move the movable bottom 292 to reduce the headspace volume. Thus, the movable bottom 292 can be moved to a higher position. For example, if the movable bottom 292 starts in the lower position 204, the movable bottom 292 can be moved to the middle position 206 or 208.

[0057] The movable bottom 292 can be moved in any suitable manner, such as by a motor and / or by applying pressure below the movable bottom 292 to deploy a telescopic structure. In various examples, the movement of the movable bottom 192 can be manually controlled and / or the movement can be partially or fully automated, for example using one or more sensors controlled by controller 156 for automatic feedback.

[0058] In response to the movement of the movable bottom 292, the headspace volume 288 can be maintained (step 410), for example, at a substantially constant level. For example, in response to pressure sensor 297 sending pressure data and the processor detecting a pressure change in the source container 200, the movable bottom can move to maintain a substantially identical headspace volume in the source container 200.

[0059] In various examples, a non-gaseous precursor may be added to source container 200 (step 412). For example, when the non-gaseous precursor in source container 200 is depleted, source container 200 may be refilled with more non-gaseous precursor. This may be accomplished via a refilling process of a refill source container in fluid communication with source container 200. In response to the additional non-gaseous precursor, the headspace volume 288 in source container 200 may decrease. In response, movable bottom 292 may be moved (step 414), for example, to increase headspace volume 288. Thus, the headspace volume may be maintained (step 416) at a desired and / or substantially constant level.

[0060] In various examples, the movement of the movable bottom 292 in response to the sublimation and / or vaporization (and departure from source container 200) of the non-gaseous precursor and / or in response to the addition of the non-gaseous precursor to source container 200 can occur substantially simultaneously with this change in the non-gaseous precursor. For example, headspace volume 288 can be monitored (step 418). Headspace volume 288 can be monitored by any suitable method, such as by a processor receiving data from any suitable sensor, such as a pressure sensor 297 that detects the pressure in source container 200, a sensor that detects the weight of the non-gaseous precursor in source container 200, etc. Sensor data can be sent to a processor, and the processor can calculate and / or detect changes in headspace volume (step 420) (e.g., based on sensor data). In response to the detection of a change in headspace volume 288, the movable bottom 292 can move, as discussed herein.

[0061] For further reference Figure 5 A method 500 for agitating a non-gaseous precursor (e.g., solid precursor 214) may include adding the non-gaseous precursor to a source container 200 (step 502). A movable bottom 292 may be moved (step 504) to agitate the non-gaseous precursor (step 506). The movable bottom 292 may be moved before, during, and / or after the addition of the non-gaseous precursor to the source container 200. To agitate the non-gaseous precursor, the movable bottom 292 may be moved in any suitable manner, such as being pulsated (e.g., moving up and down or left and right a short distance over a short period of time, similar to vibration), vibrating, etc. In response to such agitation, the non-gaseous precursor may be distributed within the source container 200 (step 508) (e.g., within the internal space 212, above the movable bottom 292, or across / along the movable bottom 292), etc. Such agitation can provide various benefits, such as mixing non-gaseous precursors (e.g., maintaining the mixing of compounds and / or phases), preventing agglomeration, and / or exposing a larger surface area (e.g., the surface area of ​​powders to promote sublimation).

[0062] Any or all steps of methods 400 and / or 500 may be performed and / or facilitated by a controller and / or processor included in the respective reactor system.

[0063] Using the systems and methods discussed herein, a movable bottom in a source container can be moved in response to the addition or removal (or conversion to gas) of a non-gaseous precursor in the source container without disassembling or separating reactor components (e.g., weighing the container or taking other measures) or significantly affecting the concentration, pressure, temperature and / or any other parameters in the source container.

[0064] This article discusses the structures and methods for source containers. It should be understood that the structures and methods discussed herein can be applied to any suitable container configured to contain chemicals (e.g., non-gaseous precursors), such as remote refill containers (e.g., source containers configured to refill their fluid connections) and / or the like.

[0065] The examples given above in this disclosure do not limit the scope of the claimed subject matter, as they are merely examples. The invention is defined by the appended claims and their legal equivalents. Any equivalent embodiments are intended to fall within the scope of this disclosure. In fact, various modifications to this disclosure, such as alternative useful combinations of the described elements, in addition to those shown and described herein, will become apparent to those skilled in the art from the description. These modifications and embodiments are also intended to fall within the scope of the appended claims.

Claims

1. A method comprising: A source container is heated to a predetermined temperature, wherein the source container includes a movable bottom and a wall system, the wall system at least partially defining an interior space in which a non-gaseous precursor is disposed, wherein the interior space includes a headspace volume having a first volume above the non-gaseous precursor; In response to heating the source container, a first portion of the non-gaseous precursor in the source container is sublimated or vaporized to generate a precursor gas, thereby increasing the headspace volume in the interior space to a second volume. The precursor gas is allowed to flow out of the source container; and The movable bottom moves in response to the sublimation or vaporization of the first portion of the non-gaseous precursor to reduce the headspace volume toward the first volume.

2. The method according to claim 1, wherein, Moving the movable bottom includes applying pressure to the movable bottom in response to causing the precursor gas to flow out of the source container.

3. The method according to claim 1, wherein, The movable bottom includes a telescopic structure, wherein moving the movable bottom includes unfolding the telescopic structure into the second volume when the precursor gas flows out of the source container.

4. The method according to claim 1, wherein, The movement of the movable bottom occurs substantially simultaneously with at least one of the following: The sublimation or vaporization of the first portion of the non-gaseous precursor, or The precursor gas is then allowed to flow out of the source container.

5. The method of claim 4, further comprising maintaining the headspace volume at a substantially constant volume.

6. The method of claim 1, further comprising adding more of the non-gaseous precursor to the source container, thereby reducing the headspace volume in the interior space.

7. The method of claim 6, further comprising lowering the movable bottom to increase the headspace volume toward the first volume.

8. The method according to claim 7, wherein, The movable bottom includes a telescopic structure, wherein lowering the movable bottom and adding more of the non-gaseous precursor occur substantially simultaneously.

9. The method according to claim 1, wherein, The movable bottom is configured to move between an elevated position and a lowered position.

10. A method comprising: A non-gaseous precursor is added to the interior space of a source container, wherein the source container includes a movable bottom and a wall system that at least partially defines the interior space, wherein the interior space includes a headspace volume having a first volume above the non-gaseous precursor. Wherein, the headspace volume in the internal space decreases to a second volume in response to the addition of the non-gaseous precursor; and In response to the addition of the non-gaseous precursor to the interior space, the movable bottom is moved to increase the headspace volume.

11. The method of claim 10, further comprising maintaining the headspace volume at a substantially constant level.

12. The method of claim 10, further comprising monitoring the headspace volume in the internal space via a processor.

13. The method of claim 12, further comprising: In response to the addition of the non-gaseous precursor to the internal space, the processor detects the change in the headspace volume within the internal space. The movement of the movable bottom is in response to the detection of a change in the headspace volume.

14. The method of claim 10, further comprising removing a portion of the non-gaseous precursor from the interior space of the source container, thereby increasing the headspace volume in the interior space.

15. The method of claim 14, further comprising moving the movable bottom in response to an increase in the headspace volume.

16. A method comprising: Add a non-gaseous precursor to the interior space of a source container, wherein the source container includes a movable bottom and a wall system that at least partially defines the interior space, wherein the interior space includes a headspace volume having a first volume above the non-gaseous precursor; The movable bottom is moved, wherein the non-gaseous precursor is disposed on the movable bottom; and The non-gaseous precursor is agitated.

17. The method of claim 16, further comprising, in response to the agitation of the non-gaseous precursor, distributing the non-gaseous precursor at least partially onto the movable bottom.

18. The method of claim 16, further comprising sublimating or vaporizing a first portion of the non-gaseous precursor in the source container to generate a precursor gas.

19. The method of claim 18, further comprising causing the precursor gas to flow out of the source container in response to the sublimation or vaporization of the first portion of the non-gaseous precursor, thereby resulting in an increase in the headspace volume in the interior space.

20. The method of claim 19, further comprising moving the movable bottom to reduce the headspace volume in response to the precursor gas flowing out of the source container.

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