Solid raw material container and monitoring method

Abstract

This invention provides a method for replenishing a chemical precursor container. [Solution] The method may include heating a raw material container containing a solid precursor to a predetermined temperature, sublimating a first portion of the solid precursor in the raw material container to produce a precursor gas, flowing the precursor gas through a gas line connecting the raw material container to a supply container, measuring the pressure value of the precursor gas flowing through the gas line using a first pressure sensor coupled to the gas line, and / or determining a first amount of solid precursor flowing from the raw material container to the supply container based on the pressure value. Determining the first amount of solid precursor may include inputting the measured pressure value into a predetermined function of pressure versus precursor transfer rate.

Description

Technical Field

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[0003]

[0001] The present disclosure generally relates to semiconductor processing equipment, and more specifically, to methods, systems, and apparatuses for refilling chemical precursor containers.

Background Art

[0002] Semiconductor manufacturing processes such as chemical vapor deposition (CVD) and atomic layer deposition (ALD) involve the deposition of thin films on semiconductor wafers (also referred to herein as "substrates"). During processing, the wafers are exposed to one or more precursors within a reaction chamber to deposit a thin layer of material. The precursor source is typically stored in a delivery container that can be refilled from a refill container. However, due to the structure of the reactor system and / or the arrangement of its components, it can be difficult to determine the amount of precursor transferred between containers (e.g., from the refill container to the delivery container). Therefore, methods for providing and monitoring the amount of precursor within a container (e.g., the delivery container and / or the refill container), or delivered to or from a container, can be important for process accuracy and maintenance, and / or to reduce the need to disassemble, remove, and / or service the containers from the reactor system.

Summary of the Invention

[0003] This summary of the invention is provided to introduce a selection of concepts in a simplified form. These concepts are further described in the "Detailed Description of the Invention" of the exemplary embodiments of the following disclosure. This "Summary of the Invention" is not necessarily intended to identify the key features or essential features of the claimed subject matter, nor is it intended to be used 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 raw material container containing a solid precursor, a supply container which is fluidly coupled to the raw material container via a gas line so that the precursor gas sublimated from the solid precursor can flow from the raw material container to the supply container, and / or a pressure sensor which is configured to measure the pressure of the precursor gas flowing through the gas line and is coupled to the gas line. The supply container may include a container body and / or a lid which is coupled to the container body. The lid may include a chemical inlet which is located in the central region of the lid. The reactor system may further include a heater which is in thermal communication with the lid and / or a cooling device which is in thermal communication with the base of the container body.

[0005] In various examples, the method may include heating a raw material container containing a solid precursor to a predetermined temperature, sublimating a first portion of the solid precursor in the raw material container to produce a precursor gas, flowing the precursor gas through a gas line connecting the raw material container to a destination container, measuring the pressure of the precursor gas flowing through the gas line using a first pressure sensor connected to the gas line, and / or determining a first amount of solid precursor flowing from the raw material container to the destination container based on a predetermined temperature and / or pressure value. Determining the first amount of solid precursor may include inputting the pressure value into a predetermined function. In various examples, measuring the pressure value may include a processor receiving a first pressure from a first pressure sensor, a processor receiving a second pressure from a second pressure sensor connected to the gas line, and / or a processor calculating a pressure value based on the first and second pressures.

[0006] A given function can be established by performing multiple cycles to measure pressure and / or precursor transfer. Each of these multiple cycles may include a series of steps (any one or combination thereof can be completed by the processor or by contributions from the processor). The steps may include determining the starting weight of a test material container containing a solid precursor, heating the test material container containing the solid precursor to a predetermined temperature, sublimating the test portion of the solid precursor in the test material container to produce a precursor gas, flowing the precursor gas through a test gas line connecting the test material container to a test supply container, measuring the test pressure of the precursor gas flowing through the test gas line using a test pressure sensor coupled to the test gas line, weighing the test material container after stopping the flow of precursor gas to determine a first weight, determining the amount of solid precursor to be transported by comparing the first weight with the starting weight, plotting data points on a plot of precursor transport rate against pressure based on the transport amount and test pressure, and / or repeating the cycle to receive a plurality (at least two) data points (where the first weight becomes the starting weight of the test material container for subsequent cycles). The method may further include creating a predetermined function from the plurality of data points. The predetermined function may be linear. The predetermined function may be based on the solid precursor, a predetermined temperature, and / or the volume of the test material container. The test raw material container, test supply container, test pressure sensor, and / or test gas line may be the same, similar to, or substantially identical to the raw material container, supply container, pressure sensor, and / or gas line included in the reactor system.

[0007] In various examples, the reactor system may further comprise a processor coupled to a pressure sensor and / or a tangible non-temporary computer-readable memory configured to communicate with the processor, the computer-readable memory storing instructions that cause the processor to perform an action in response to the processor's execution. The action may include heating a raw material container containing a solid precursor to a predetermined temperature, sublimating a first portion of the solid precursor in the raw material container to produce a precursor gas, flowing the precursor gas through a gas line connecting the raw material container to a destination container, measuring the pressure of the precursor gas flowing through the gas line using a pressure sensor coupled to the gas line, and / or determining a first amount of solid precursor flowing from the raw material container to the destination container based on the pressure value. The action may further comprise inputting the pressure value into a predetermined function to determine the first amount of solid precursor. The predetermined function may be based on the type of solid precursor, a predetermined temperature (e.g., a predetermined temperature to which the raw material container is heated), and / or the volume of the raw material container. In various examples, the pressure sensor may be a first pressure sensor, and the reactor system may further comprise a second pressure sensor coupled to the gas line. A first pressure sensor may be connected to a gas line adjacent to a raw material container, and a second pressure sensor may be connected to a gas line adjacent to a supply container. Measuring the pressure value may include, by the processor, receiving a first pressure from the first pressure sensor, by the processor, receiving a second pressure from the second pressure sensor, and / or by the processor, calculating a pressure value based on the first and second pressures.

[0008] A predetermined function can be established by performing multiple cycles to measure pressure and / or precursor transfer. The operation of the processor may further include performing such cycles. A cycle may include determining the starting weight of a test raw material container containing a solid precursor; heating the test raw material container containing the solid precursor to a predetermined temperature to sublimate the test portion of the solid precursor in the test raw material container and generate a precursor gas that flows through a test gas line to a test supply container; measuring the test pressure of the precursor gas flowing through the test gas line; determining a first weight of the test raw material container after stopping the flow of the precursor gas; comparing the first weight to the starting weight and determining the amount of solid precursor transferred based on the comparison of the first weight to the starting weight; and / or plotting data points on a plot of precursor transfer rate against pressure based on the amount transferred and the measured test pressure. One or more of the steps in a cycle can be repeated in subsequent cycles to receive and plot multiple data points. The first weight from a previous cycle may become the starting weight of the test raw material container for subsequent cycles. The operation may further include creating a predetermined function from multiple data points. The given function can be linear. The test raw material container, test supply container, test pressure sensor, and / or test gas line may be the same, similar to, or substantially identical to the raw material container, supply container, pressure sensor, and / or gas line included in the reactor system.

[0009] For the purpose of outlining the benefits achieved beyond this disclosure and the prior art, specific purposes and benefits of this disclosure are described above. Naturally, it should be understood that not all such purposes or benefits are necessarily achieved by any specific example of this disclosure. Therefore, it should be recognized by those skilled in the art that this disclosure may be embodied or implemented in a manner that achieves or optimizes, for example, one benefit or group of benefits as taught or suggested herein.

[0010] All of these examples are intended to be within the scope of the present disclosure disclosed herein. These examples and other examples will be readily apparent to those skilled in the art from the following “Modes for Carrying Out the Invention” of a particular example with reference to the accompanying drawings, and the present disclosure is not limited to any particular example(s) disclosed. [Brief explanation of the drawing]

[0011] [Figure 1] These are schematic diagrams of reactor systems, illustrated with various examples. [Figure 2A] This is a top perspective view of a precursor vessel for a reactor system, showing various examples. [Figure 2B] This is a top view of the precursor container in Figure 2A, showing various examples. [Figure 3A] Figures 2A and 2B show top perspective views of precursor containers, including valves, in various examples. [Figure 3B] This is a top view of the precursor container in Figure 3A, showing various examples. [Figure 4] This figure shows plots containing data points and a function of precursor transport rate against pressure, for various examples. [Figure 5] This block diagram shows methods for determining the function of precursor transport rate with respect to pressure, using various examples. [Figure 6] This block diagram shows methods for determining chemical precursor transport using various examples. [Modes for carrying out the invention]

[0012] These and other features, embodiments, and advantages disclosed herein are set forth below with reference to the drawings of a particular example, which are intended to illustrate, and not limit, the subject matter of the claims. Elements that are given the same reference numerals throughout the drawings are intended to be the same.

[0013] Please understand that the elements in the figures are illustrated for simplification and clarity, and are not necessarily drawn to actual size. For example, the relative sizes of some elements in the figures may be exaggerated relative to others to help improve understanding of the examples shown in this disclosure.

[0014] The descriptions of examples of methods, structures, devices, and systems provided below are illustrative and intended solely for illustrative purposes, and are not intended to limit the scope of this disclosure or the claims. Furthermore, the enumeration of multiple examples having the described features is not intended to exclude other examples having additional features or incorporating different combinations of the described features. For example, various examples may be described as embodiments and enumerated in dependent claims. Unless otherwise stated, examples or their components may be combined or applied separately from one another. Methods may include the disclosed steps in any preferred and / or desired order or combination.

[0015] As used herein, the term "and / or" includes any combination of one or more of the related enumerated items. Unless otherwise stated, expressions such as "at least one of" modify the entire list of elements when preceding a list of elements, and not necessarily modify any individual element of the list.

[0016] As used herein, the terms “includes,” “comprises,” “including,” and / or “comprising” identify the presence of a described feature, integer, step, process, member, component, and / or group thereof, but do not exclude the presence or addition of one or more other features, integers, steps, processes, members, components, and / or groups thereof. In this disclosure, any defined meaning does not necessarily exclude, in some examples, the ordinary, customary meaning.

[0017] As used herein, the term “substrate” may refer to one or more arbitrary substrate materials, including one or more arbitrary substrate materials on which devices, circuits, or films may be modified or formed. “Substrate” can be continuous or discontinuous, rigid or flexible, solid or porous, or a combination thereof. A substrate can be in any form, such as powder, plate, or workpiece. Examples of substrates in plate form include wafers of various shapes and sizes. A substrate may be made from semiconductor materials, including, for example, silicon, silicon germanium, silicon oxide, gallium arsenide, gallium nitride, and silicon carbide.

[0018] In some examples, “film” refers to a layer extending perpendicular to the thickness direction. In some examples, “layer” refers to a material formed on a surface that has a certain thickness and may be a synonym for film or a non-film structure. A film or layer may consist of a single film or layer having certain properties, or multiple films or layers, and the boundaries between adjacent films or layers may or may not be clear and may or may not be established based on physical, chemical, and / or any other properties, formation process or sequence, and / or function or purpose of adjacent films or layers. Layers or films may or may not be continuous. Furthermore, a single film or layer can be formed using one or more deposition cycles, and / or one or more deposition and processing cycles.

[0019] As used herein, the term “structure” may refer to a partially or completely fabricated device structure. For example, a structure may be a substrate or may include a substrate on which one or more layers and / or features are formed.

[0020] As used herein, the terms “periodic” deposition or etching process, or “periodic” deposition or etching process, may refer to a vapor deposition process in which a deposition cycle or etching cycle, typically a series of consecutive deposition or etching cycles, are carried out within a process chamber. A periodic deposition or etching process may include, for example, periodic chemical vapor deposition (CCVD) and / or atomic layer deposition (ALD) processes. A periodic deposition or etching process may include a plasma enhancement step. A periodic deposition or etching process may comprise one or more cycles including plasma activation of any combination of precursors, reactants, and / or inert gases.

[0021] In the present disclosure, any two numbers among the variables can constitute the executable range of the variable, and any range shown may include or exclude the endpoints, and all ranges and ratios disclosed herein may be combined. Additionally, in some examples, any value of the variables shown (regardless of whether they are shown with "about") may refer to an exact value or an approximate value, may also include equivalents, and may also refer to an average value, a median value, a representative value, or a majority, etc. Specifically, unless otherwise stated, references to "a", "an", and / or "the" may include one or more than one, and references to singular items may also include plural items. When referring to the components of the system discussed herein, the term "coupled" refers, as appropriate, to either a direct or an indirect coupling with other intervening elements. Unless otherwise indicated, terms such as "first", "second", etc., and / or "primary", "secondary", etc., are used herein merely as labels and are not intended to impose sequential, positional, or hierarchical requirements on the items they refer to. Further, for example, a reference to a "second" item does not require or exclude, for example, the presence of a "first" item or an item with a smaller number, and / or, for example, the presence of a "third" item or an item with a larger number. Further, for example, references to a "first" item and a "second" item do not mean that there are no intervening items, and such intervening items may exist.

[0022] Reactor systems used in ALD, CVD, and / or the like can be used for various applications, including deposition and etching of materials onto a substrate surface. The reactor system can include a precursor container (i.e., a delivery container) that can store a chemical precursor and deliver the chemical precursor from the precursor container to another component of the reactor system (e.g., a reaction chamber) for processing. The precursor container can include a solid feed container configured to contain a solid precursor (e.g., herein, "precursor container", "delivery container", and / or "solid feed container" can be used interchangeably).

[0023] The delivery container can contain a feed precursor (sometimes referred to as a "reactant", "chemical", or "chemical precursor"), which can be a solid (e.g., in powder form) or a liquid. A heater coupled to and / or in thermal communication with the delivery container (e.g., a radiant heat lamp, a resistance heater, and / or the like) can heat the delivery container to facilitate vaporization and / or sublimation of the chemical precursor within the delivery container. The delivery container can have an inlet and an outlet for a flow of carrier gas through the delivery container. The carrier gas can be inert, e.g., nitrogen, argon, or helium. Generally, the carrier gas conveys the reactant vapor (e.g., the evaporated or sublimed chemical reactant) through the container outlet and ultimately to the substrate reaction chamber. In various examples, the delivery container comprises, consists essentially of, or consists of a sublimator. Thus, whenever "solid feed container" is mentioned herein, a sublimator (e.g., a "solid feed chemical sublimator") is also clearly contemplated.

[0024] In various examples, each reaction gas can be stored in a delivery container. Reactants may be gaseous at standard pressure and temperature of approximately 1 atmosphere and room temperature. Examples of such gases include nitrogen, oxygen, hydrogen, and ammonia. In various examples, vapors of precursors that are liquid or solid at standard pressure and temperature (e.g., hafnium chloride, hafnium oxide, zirconium dioxide, etc.) are used. For some solid substances (referred herein as “solid raw material precursor,” “solid precursor,” “solid chemical reactant,” “solid reactant,” etc.), the vapor pressure at room temperature is very low, so they are typically heated and / or maintained at very low pressures to produce a sufficient amount of reactant vapor for the reaction process. Gas-phase reactants from solid or liquid substances may be useful in chemical reactions in various industries.

[0025] As described herein, one or more remote replenishment containers may be included in the reactor system to fill the delivery container with raw material precursors. As used herein, a remote replenishment container can be described as a “raw material container,” and a precursor or delivery container can be described as a “destination container” (i.e., a remote replenishment container can be a source of replenishment precursors, and a delivery container can be a destination for replenishment precursors). Conventionally, delivery containers are removed from the reactor system and replenished, which can lead to downtime and losses in wafer production. Remote replenishment containers can reduce the need to replace or replenish sublimators. Instead, remote replenishment containers can be used to automatically and / or continuously supply chemicals, such as raw material precursors, to the delivery container. A remote replenishment container system may include one or more remote replenishment containers. In various examples, remote replenishment containers may be located in a location separate from other reactor system components. For example, a remote replenishment container may be located in a separate room, across a cleanroom and / or adjacent to other reactor system components.

[0026] Figure 1 is a schematic diagram showing an exemplary reactor system 100 including a delivery container 102, and / or one or more reactors 138 and 140 including their respective reaction chambers 122 and 124. Reactors 138 and 140 may include their respective susceptors 142 and 144 for holding their respective substrates 146 and 148 during processing, and gas distribution systems 150 and 152 for distributing one or more reactants / precursors onto their respective surfaces on the substrates 146 and 148. Reactor system 100 may include a vacuum source for controlling the vacuum pressure in one or more reaction chambers 122 and 124. A reactant source may feed gas-phase reactants generated from the solid raw material delivery container 102 into a gas-phase reactor. Reactors 138 and / or 140 may be gas-phase reactors. The solid raw material delivery container 102 may include a chemical substance 114 (e.g., in solid form). Solid chemicals can include chemical reactants such as HfCl4, ZrCl4, AlCl3, TaF5, MoF5, and / or SiI4. Chemical 114 may be solid under standard conditions (i.e., room temperature and atmospheric pressure).

[0027] A carrier gas source 120 can be coupled to a delivery container 102 via a carrier gas line 136 and can hold carrier gas. The lid 130 of the delivery container 102 may include a carrier gas valve 119 for regulating the flow of carrier gas from the carrier gas source 120 to the delivery container 102. The carrier gas source 120 can 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 can be controlled by one or more control devices. Depending on when introduced into the delivery container 102, the carrier gas may help transport vaporized and / or sublimated chemical reactants to the reaction chambers 122 and / or 124 via a container outlet valve 126. A chemical delivery line 128 may include valves 132 and 134 for controlling the fluid communication of chemicals 114 and / or carrier gas from the delivery container 102 to the respective reaction chambers 122 and 124.

[0028] In various examples, the delivery container 102 may be coupled to a remote replenishment container 104 via a chemical replenishment gas line 106. The remote replenishment container 104 may be located at a distance from the delivery container 102 and / or any other components of the reactor system 100 (for example, in a different room and / or on a different plane from the delivery container 102, reaction chambers 122, 124, and / or similar).

[0029] The remote replenishment container 104 may contain replenishment chemicals 114, including precursor or source chemicals that may be solid under standard conditions (i.e., room temperature and atmospheric pressure). The chemicals 114 in the remote replenishment container 104 may be the same as the chemicals 114 in the delivery container 102. The remote replenishment container 104 can be a bulk replenishment container that has a larger chemical capacity within the housing 108 than the delivery container 102 (for example, because the remote replenishment container 104 may not be limited by dimensional constraints associated with other components of the reactor system 100). For example, the remote replenishment container 104 may have at least 1.5, 2, 3, 4, 5, 10, or 20 times the capacity of the delivery container 102.

[0030] The chemical replenishment gas line 106 can extend between the outlet valve 116 of the remote replenishment container 104 and the inlet valve 118 of the delivery container 102. The inlet valve 118 can be installed inside the lid 130 of the delivery container 102. The outlet valve 116 can be installed inside the lid 182 of the remote replenishment container 104. The outlet valve 116 and the inlet valve 118 can control the fluid communication of the chemical 114 from the remote replenishment container 104 to the delivery container 102.

[0031] The remote replenishment container 104 can be equipped to vaporize (e.g., sublimate, evaporate) the chemical 114, allowing the vaporized or sublimated chemical 114 to pass through the chemical replenishment gas line 106 to the delivery container 102. In various examples, the remote replenishment container 104 can be coupled to and / or located near a heating device 174 that is located outside the lid 182 and / or housing 108 and is in thermal communication with the lid 182 and / or housing 108. The housing 108 can be made of a thermally conductive material (e.g., stainless steel) and can be configured to transfer heat from the heating device 174 to the internal volume of the lid 182 and / or remote replenishment container 104. The heating device 174 can be configured to heat the chemical 114 to a temperature sufficient to change the phase of the chemical 114, thereby vaporizing and / or sublimating the chemical 114 and transferring it to the delivery container 102 through the chemical replenishment gas line 106. The heating device 174 may be equipped with any suitable heating device (e.g., a heater, a heating jacket, a heating block, a radial heater, and / or similar).

[0032] The remote replenishment container 104 can be configured to store the chemical 114 (for example, in a solid state) during replenishment operations. A cooling device 188 can be coupled to the bottom of the remote replenishment container 104. The cooling device 188 can cool the base portion 196 of the remote replenishment container 104 and maintain the chemical 114 in a solid state before sublimation. The cooling device 188 may include a chill plate, a cooling coil, a variable-pitch cooling coil, a cooling jacket, a cooling fan, a Peltier cooler or an integrated coolant channel for circulating coolant, or any combination thereof.

[0033] The remote replenishment container 104 can be configured to operate at a selected temperature. For example, the operating temperature may be determined based on the desired sublimation rate of the chemical precursor / reactant. In some examples, the operating temperature is in the range of about 10°C to about 500°C. The selected operating temperature may depend on the chemical being vaporized or sublimated.

[0034] The delivery container 102 can receive the chemical substance 114 in the gas phase from the remote replenishment container 104 via the chemical substance replenishment gas line 106. The chemical substance replenishment gas line 106 can be installed on the top 190 of the delivery container 102, for example, on the lid 130. In various examples, the lid 130 and the inlet valve 118 can be configured to drip and solidify the liquefied chemical substance 114 at the bottom of the delivery container 102, for example, from the inlet 184, as the chemical substance 114 is transferred to the delivery container 102.

[0035] The delivery container 102 may have any preferred structure and / or configuration for performing the functions discussed herein. Referring further to Figures 2A and 2B, the delivery container 202 is an example of the delivery container 102 (discussed with respect to Figure 1). The delivery container 202 may have a container body 278 (an example of the container body 178 of the delivery container 102) extending between an upper 290 (an example of the upper 190 of the delivery container 102) and a base 292 (an example of the base 192 of the delivery container 102). A lid 230 (an example of the lid 130 of the delivery container 102) may be coupled to the upper 290 of the container body that encloses the internal volume of the delivery container 202. A removable handle 295 may be configured to assist in transporting or moving the delivery container 202 and may be coupled to the delivery container 202 (e.g., to the container body 278 and / or the lid 230).

[0036] The lid 230 of the delivery container 202 may include a chemical inlet 218, a carrier gas inlet 219, and / or a chemical outlet 226. The chemical inlet 218 can be configured to receive chemical precursors from a remote replenishment container (for example, the chemical inlet 218 may have an inlet valve 118 coupled to a chemical inlet 218 configured to receive chemical precursors from a remote replenishment container 104). The chemical inlet 218 may be located in the central region of the lid 230 (the central region may be 10% or 20% of the center, including the center point of the lid 230). Such a location for the chemical inlet 218 allows the chemical precursors received from the remote replenishment container to enter the internal volume of the container body 278 and be distributed more evenly therein than a chemical inlet located elsewhere. The chemical outlet 226 can be configured to allow precursors to pass through it from the delivery container 202 toward the reaction chambers (e.g., reaction chambers 122 and / or 124). The carrier gas inlet 219 can be configured to allow carrier gas (e.g., from the carrier gas source 120) to enter the delivery container 202. The coupling points 254 and 256 can be configured to facilitate coupling to the valve cover 230 (e.g., as shown in Figure 3B).

[0037] Referring further to Figures 3A and 3B, the delivery container 202 may be equipped with valves coupled to each inlet within the lid 230. For example, an inlet valve 318 (an example of an inlet valve 118) can be fluid-coupled to a chemical inlet 218, an outlet valve 326 (an example of an outlet valve 126) can be fluid-coupled to a chemical outlet 226, and / or a carrier gas valve 319 (an example of a carrier gas valve 119) can be coupled to a carrier gas inlet 219. Coupling points 354 and 356 on each valve may complement coupling points 254, 256 on the lid 230 to facilitate coupling between the valve and the lid 230. The coupling points and valves on the lid 230 may be arranged linearly along and / or parallel to the axis 352.

[0038] The delivery container 102 can be thermally coupled to one or more heating devices 176 (e.g., heaters, heating jackets, heating blocks, and / or radiating heaters) and / or one or more cooling devices 186. Such heating or cooling devices can play a role in controlling or regulating the temperature of the chemical 114 during replenishment operations, material processing operations, and / or storage of the chemical 114. The cooling device 186 may comprise chill plates, cooling coils, variable-pitch cooling coils, cooling jackets, cooling fans, Peltier coolers, and / or integrated coolant channels for circulating coolant. As will be discussed in more detail herein, such heating and cooling devices 186 provide a temperature gradient within the delivery container 102.

[0039] In various examples, the heating device 176 can be coupled to and / or thermally communicate with the delivery container 102 (e.g., in the container body 178 (e.g., housing) and / or lid 130). The container body 178 and / or lid 130 can be configured to transfer heat and / or pressure from the heating device 176 to the chemical 114 (e.g., as it enters the delivery container 102 and / or so that the chemical 114 evaporates or sublimes and flows through the chemical delivery line 128). Such applied heat and / or pressure can liquefy the chemical 114 to form droplets that fall to the bottom of the delivery container 102. The base portion 192 of the delivery container 102 can be cooled by a cooling device 186 (e.g., cold plate) to a temperature lower than the chemical replenishment gas line 106, the side walls of the container body 178, and / or the lid 130 of the delivery container 102. This allows for a temperature gradient along the longitudinal axis 224 such that the highest temperature in the system is at the top 190 of the delivery container 102 and the lowest temperature in the system is at the base 192. Droplets of the chemical 114 can form as the chemical 114 enters through the lid 130 and may solidify upon contact with the bottom surface of the base 192 of the delivery container 102. During replenishment (transferring the chemical 114 from the remote replenishment container 104 to the delivery container 102), the chemical 114 may form a solid at the bottom of the delivery container 102 and may be stored at the bottom until the material processing operation. The cooling device 186 can maintain a temperature at the base 192 of the delivery container 102 sufficient to keep the chemical 114 in a solid phase.

[0040] The delivery container 102 can be configured to operate within a temperature gradient in its internal volume 180 during replenishment. For example, the operating temperature of the portion adjacent to the upper 190 may be determined based on the desired liquefaction rate of the precursor / reactant of the chemical 114. In some examples, the operating temperature is in the range of approximately 10°C to approximately 500°C. The selected operating temperature may depend on the liquefaction of the chemical upon entering the delivery container 102. Similarly, the base portion 192 of the delivery container 102 can be maintained at a lower temperature than the upper 190 to solidify the chemical 114 on the base portion 192, thereby maintaining a temperature gradient within the delivery container 102. The operating base temperature can be selected depending on the chemical being solidified. Furthermore, to prevent gaseous particles from solidifying in undesirable areas on the inside of the delivery container 102, the base portion 192 may be set to a temperature at least lower than the upper 190. In various examples, the base portion 192 is the coldest location within the internal volume 180 of the delivery container 102. Therefore, the operating temperature of the base portion 192 may be far below the melting point of the chemical substance 114.

[0041] A temperature gradient extends between the base portion 192 and the upper portion 190, including the lid 130. In various examples, the base portion 192 can be maintained below a first threshold temperature, while the upper portion 190 can be maintained above a second threshold temperature, which is higher than the first threshold temperature. In various examples, the temperature difference between the base portion 192 and the upper portion 190 can 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 in between, or can fall within any range with an endpoint therein.

[0042] In various examples, during material processing operations, the heating device 176 can be configured to heat the chemical 114 to a temperature sufficient to change the phase of the chemical 114, such as vaporizing and / or sublimating it. Once vaporized or sublimated, the chemical 114 can be delivered to reaction chambers 122 and / or 124 via the chemical delivery line 128 for substrate processing. Prior to vaporization and / or sublimation, the chemical 114 may be stored as a solid in the delivery container 102. Alternatively, the chemical 114 may be stored in the liquid phase during or after replenishment. The heating device 176 may be configured to heat the delivery container 102 to a temperature sufficient to liquefy the chemical 114.

[0043] During material processing, the delivery container 102 can be configured to operate at a selected temperature based on the desired sublimation rate of the precursor / reactant of the chemical substance 114. In some examples, the operating temperature is in the range of approximately 10°C to approximately 500°C.

[0044] The delivery container 102 can be replenished from a remote replenishment container 104. As shown in Figure 1, the reactor system 100 comprises a control unit 156 including a processor 164, a user interface 166, and / or memory 168. The processor 164 is operably connectable to the user interface 166 (for example, to receive user input and / or to provide user output through it) and is configurable to communicate with memory 168. Memory 168 includes a tangible, non-transient, machine-readable medium containing a number of program modules / instructions 172 that cause the processor 164 to perform certain operations, depending on whether they are read by and / or executed by the processor 164. Among the operations discussed herein are operations for material layer deposition methods, methods for replenishing the delivery container 102, and / or methods for determining precursor transfers. As will be understood by those skilled in the art in consideration of this disclosure, the control unit 156 may have different configurations in other examples and remain within the scope of this disclosure.

[0045] In some examples, the carrier gas source 216 may be coupled to the remote replenishment container 104 via a chemical delivery line 222, and the carrier gas may be supplied to the remote replenishment container 104. A valve 221 may control the flow of the carrier gas 220. The carrier gas 220 may assist in the transport of the sublimated chemical 114 from the remote replenishment container 104 to the delivery container 102.

[0046] In various examples, the replenishment process may be manually controlled, and / or the replenishment operation may be partially or fully automated using one or more sensors for automatic feedback controlled, for example, by a control device 156. Continuing to refer to Figure 1, the reactor system 100 may comprise one or more pressure sensors (i.e., pressure transducers, transmitters, and / or similar) coupled to the chemical replenishment gas line 106. For example, the reactor system 100 may comprise a first pressure sensor 96 located near the remote replenishment container 104 and a second pressure sensor 98 located near the delivery container 102. That is, the first pressure sensor 96 may be located closer to the replenishment container 104 than the second pressure sensor 98. The pressure sensors 96, 98 may be configured to measure the pressure in the chemical replenishment gas line 106 during the replenishment process, for example, when transferring a chemical precursor from the remote replenishment container 104 to the delivery container 102. The control unit 156 and / or processor 164 may electronically communicate with (or be operably coupled to) one or more of the pressure sensors so that the control unit 156 and / or processor 164 can receive pressure readings or data from the pressure sensors. In various examples, the chemical replenishment gas line 106 may include an accumulator, and the pressure sensors may be coupled to the accumulator to measure the pressure therein.

[0047] Based on the pressure in the chemical replenishment gas line 106 between the remote replenishment container 104 and the delivery container 102, the transfer of a certain amount of chemical precursor (e.g., solid precursor) can be determined. Thus, the amount of chemical precursor remaining in the remote replenishment container 104 can also be determined based on the pressure in the chemical replenishment gas line 106. For this purpose, a function of the precursor transfer rate (e.g., grams per unit time, such as grams / hour) to the pressure (e.g., equilibrium pressure) in the chemical replenishment gas line 106 can be predetermined. By using the predetermined function and inputting the measured pressure into the predetermined function, the amount of precursor transferred can be determined based on the measured pressure, and the corresponding amount of precursor transferred can be obtained.

[0048] Referring further to Figure 5, a method 500 for determining a function (a predetermined function) of the precursor transfer rate with respect to pressure is illustrated. To this end, the starting weight of a test raw material container (e.g., a remote replenishment container 104) can be determined (step 502). The test raw material container can be a raw material container used in the reactor system 100, or a container similar to or substantially identical to a raw material container used in the reactor system. The test raw material container is weighable with the solid chemical 114 placed inside, which may require removal from the reactor system 100. The starting weight may be determined by a processor (e.g., processor 164) and / or received by the processor from a scale used to weigh the test raw material container. In various examples, the weight of the test raw material container can be determined by tare before the chemical 114 is added to the test raw material container, thereby determining the weight of the chemical 114 in the test raw material container.

[0049] The test raw material container can be fluidly coupled to the test supply container, for example, via a test gas line. The test supply container can be a supply container used in the reactor system 100 (e.g., delivery container 102), or a container similar to or substantially identical to a supply container used in the reactor system. Similarly, the test gas line can be a gas line used in the reactor system 100 between the raw material container and the supply container (e.g., chemical replenishment gas line 106), or a gas line similar to or substantially identical to a gas line used in the reactor system. The test container can be heated to a temperature sufficient to sublimate at least a portion of the solid precursor therein to form a precursor gas (step 506) (step 504). The temperature to which the test raw material container can be heated can be a predetermined temperature (e.g., a temperature used during a replenishment event). Such heating can be completed, for example, by a heating device 174 that has thermal communication with the test raw material container (e.g., communicating with a processor). As the precursor gas is formed, it can flow through a test gas line connected to a test supply container (step 508). The processor can open one or more valves (e.g., an outlet valve 116 from the remote replenishment container 104 and / or an inlet valve 118 from the delivery container 102) to allow the precursor gas to flow between the containers. While the precursor gas is flowing through the test gas line, the pressure of the precursor gas in the test gas line can be measured (step 510). For example, pressure sensors 96 and / or 98 (e.g., in conjunction with the processor) can measure the pressure in the test gas line. The processor can receive pressure readings from the pressure sensor(s). The pressure readings can be the equilibrium pressure in the test gas line. In various examples where two or more pressure sensors (e.g., pressure sensors 96 and 98) are used, the pressure value can be calculated using multiple pressure readings (e.g., by averaging).

[0050] The flow of the precursor gas can be stopped (for example, by the processor closing an appropriate valve). Accordingly, the weight of the test material container can be determined (step 512). This may be the first weight or a new weight of the test material container after the initial weight. The test material container can be weighed (for example, by the processor) to determine its weight. To do this, the test material container may need to be removed from its position in the reactor system. The new weight of the test material container can be compared (for example, by the processor) with the initial weight of the test material container to determine the amount of solid precursor transferred from the test material container (for example, by the processor) (step 514). Based on the amount of time the gas precursor has flowed between the test material container and the test supply container, the precursor transfer rate (for example, grams per unit time, such as grams / hour) can be determined. Data points including the measured pressure and precursor transfer rate can be plotted on a plot of precursor transfer in grams per hour against pressure (equilibrium) (step 516). Steps 502-516 can be repeated in any preferred order and / or arrangement to obtain more data points to add to such a plot. For example, the first new weight determined in step 512 discussed above can be the starting weight in step 502 when repeating the steps of method 500.

[0051] As shown in plot 400 of Figure 4, four data points were obtained and plotted (for example, by utilizing the steps of Method 500). For example, data point 402 includes a pressure of approximately 20 Torre and a precursor transfer rate of approximately 37 grams / hour, data point 404 includes a pressure of approximately 32 Torre and a precursor transfer rate of approximately 90 grams / hour, data point 406 includes a pressure of approximately 34 Torre and a precursor transfer rate of approximately 85 grams / hour, and data point 408 includes a pressure of approximately 47 Torre and a precursor transfer rate of approximately 139 grams / hour (wherein used in this context, the term "approximately" means plus or minus 10 percent of the value in question). The unit of pressure can be any preferred unit of pressure (e.g., Torre, pounds per square inch, Pascal, standard atmospheric pressure (atmosphere), millimeters of mercury, etc.).

[0052] From the plotted data points (e.g., data points 402-408), a function can be created (e.g., by a processor) (step 518). For example, based on data points 402-408 in plot 400, the processor can determine a function 420. Function 420 may be a predetermined function used to estimate / predict the precursor transfer rate and / or transfer volume based on the measured pressure in the gas line between the raw material container and the destination container (e.g., pressure readings from a pressure sensor). As shown in plot 400, function 420 can be linear (i.e., the data points can be plotted substantially along line 410). That is, the relationship between pressure and precursor flow rate can be proportional.

[0053] A given function discussed herein may be specific to a particular or characteristic set of parameters (e.g., a particular chemical, a raw material container volume, a destination container volume, a container material, a temperature (e.g., a given temperature)). Thus, under the same set of parameters used to determine a given function 420, the measured pressure in the gas line between the raw material container and the destination container can be input to the function 420, and an estimated precursor transfer rate can be determined which can determine the amount of precursor transferred. For a different set of parameters (e.g., due to a different chemical, a container volume, a container material, a temperature, and / or similar), method 500 can be used to determine a given function for that set of parameters.

[0054] A method 600 for determining the amount of chemical precursor to be transferred (for example, from a raw material container to a destination container) is illustrated in Figure 6. Method 600 can utilize a predetermined function, as will be discussed herein. As an example, the raw material container may be a remote replenishment container 104, and the destination container may be a delivery container 102 of the reactor system 100 (Figure 1). The raw material container containing the solid precursor can be heated (step 602) to sublimate at least a portion of the precursor to form a precursor gas (step 604). Such heating can be completed, for example, by a heating device 174 that is in thermal communication with the raw material container. In accordance with the formation of the precursor gas, the precursor gas can be flowed through a chemical replenishment gas line 106 connected to the destination container (step 606). While the precursor gas is flowing through the chemical replenishment gas line 106, the pressure of the precursor gas in the chemical replenishment gas line 106 can be measured (step 608). For example, pressure sensors 96 and / or 98 (in conjunction with, for example, a processor) can measure the pressure in the chemical replenishment gas line 106. The processor can receive pressure readings from pressure sensors. The pressure readings can be the equilibrium pressure of the chemical replenishment gas line 106. In various examples where two or more pressure sensors (e.g., pressure sensors 96 and 98) are used, the pressure value can be calculated using multiple pressure readings (e.g., by averaging).

[0055] Based on the measured pressure, the amount of precursor transferred from the raw material container can be determined (e.g., estimated) (step 610). For example, the processor can receive the measured pressure of the gas precursor in the chemical replenishment gas line 106 (e.g., from a pressure sensor). Accordingly, the processor can input the measured pressure into a predetermined applicable function (e.g., a predetermined function 420) to determine the precursor transfer rate (its estimated value). For example, using the predetermined function 420, a precursor transfer rate of 75.45 grams / hour can be determined for a pressure measurement 30. The amount of precursor transferred from the raw material container can be determined (e.g., by the processor) from the estimated precursor transfer rate based on the time the precursor gas has flowed through the chemical replenishment gas line 106. Continuing the above example, if the precursor gas flows for 1 minute, 1.26 grams will be transferred from the raw material container.

[0056] Any or all of the steps of Method 500 or 600 can be carried out by a processor included in the respective reactor system, as required.

[0057] By utilizing the systems and methods discussed herein, it may be possible to estimate the amount of chemical precursor that has flowed from a raw material container (e.g., remote replenishment container 104) to a destination container (e.g., delivery container 102) without requiring the dismantling or separation of reactor components (e.g., to weigh the container or take other actions).

[0058] The structures and methods described herein are discussed in relation to the delivery container 102 and the remote replenishment container 104. However, it should be understood that the structures and methods described herein may be applied to any suitable container and / or any suitable container having a gas line that fluidly couples the containers for gas flow between them, and having a pressure sensor coupled to the gas line.

[0059] The examples of this disclosure described above are merely illustrative and do not limit the scope of the claimed subject matter. The present invention is defined by the appended claims and their legal equivalents. Embodiments of any equivalent are intended to be within the scope of this disclosure. In fact, various modifications of this disclosure, in addition to those shown and described herein, such as alternative useful combinations of the elements described, may be apparent to those skilled in the art from the description. Such modifications and embodiments are also intended to be within the scope of the appended claims.

Claims

1. Heating the raw material container containing the solid precursor to a predetermined temperature, The first portion of the solid precursor in the raw material container is sublimated to generate a precursor gas, The precursor gas is flowed through the gas line connecting the raw material container to the supply container, The first pressure sensor connected to the gas line measures the pressure value of the precursor gas flowing through the gas line, A method comprising determining a first amount of the solid precursor flowing from the raw material container to the supply destination container based on the pressure value.

2. The method according to claim 1, wherein determining the first amount of the solid precursor includes inputting the pressure value into a predetermined function.

3. The predetermined function is determined by performing multiple cycles, The cycle of the aforementioned multiple cycles Determining the starting weight of the test raw material container containing the solid precursor, Heating the test raw material container containing the solid precursor to the predetermined temperature, The process involves sublimating the test portion of the solid precursor in the test material container to generate the precursor gas, The precursor gas is flowed through the test gas line connecting the test raw material container to the test supply container, The test pressure of the precursor gas flowing through the test gas line is measured by a test pressure sensor connected to the test gas line, After stopping the flow of the precursor gas, the test raw material container is weighed to determine the first weight, The amount of the solid precursor to be transferred is determined by comparing the first weight with the starting weight. Based on the transfer volume and the measured test pressure, the data points are plotted on a plot of the precursor transfer rate against pressure. The method according to claim 2, comprising repeating a cycle to receive multiple data points, wherein the first weight is the starting weight of the test material container.

4. The method according to claim 3, further comprising creating the predetermined function from the plurality of data points.

5. The method according to claim 2, wherein the predetermined function is linear.

6. The method according to claim 3, wherein the predetermined function is based on the solid precursor, the predetermined temperature, and the volume of the test material container.

7. Measuring the aforementioned pressure value The processor receives the first pressure from the first pressure sensor, The processor receives a second pressure from a second pressure sensor connected to the gas line, The method according to claim 1, comprising the processor calculating the pressure value based on the first pressure and the second pressure.

8. It is a system, A raw material container containing a solid precursor, A supply container, which is fluidly coupled to the raw material container via a gas line so that the precursor gas sublimated from the solid precursor can flow from the raw material container to the supply container, A pressure sensor is configured to measure the pressure of the precursor gas flowing through the gas line, and is coupled to the gas line. A processor operably coupled to the pressure sensor, A tangible non-temporary memory configured to communicate with the aforementioned processor, In response to the execution by the aforementioned processor, the processor is instructed to: The processor and the pressure sensor measure the pressure value of the precursor gas flowing through the gas line, A system comprising: a tangible non-temporary memory, which stores instructions for the processor to perform an operation including determining a first amount of the solid precursor flowing from the raw material container to the supply container based on the pressure value.

9. The system according to claim 8, wherein determining the first amount of the solid precursor includes inputting the pressure value into a predetermined function by the processor.

10. The system according to claim 9, wherein the predetermined function is based on the type of the solid precursor, a predetermined temperature, and the volume of the raw material container.

11. The operation further includes the processor performing a plurality of cycles to establish the predetermined function, The cycle of the aforementioned multiple cycles The processor determines the starting weight of the test raw material container containing the solid precursor, The processor heats the test material container containing the solid precursor to the predetermined temperature, sublimes the test portion of the solid precursor in the test material container, and generates the precursor gas that flows through the test gas line to the test supply container. The test pressure sensor and the processor measure the test pressure of the precursor gas flowing through the test gas line, After stopping the flow of the precursor gas, the processor determines the first weight of the test raw material container. The processor compares the first weight with the starting weight, The processor determines the amount of solid precursor to be transferred based on comparing the first weight with the starting weight, The processor plots data points on a plot of precursor transfer rate against pressure, based on the transfer volume and the measured test pressure. The system according to claim 10, comprising repeating a cycle to receive and plot a plurality of data points, wherein the first weight is the starting weight of the test material container.

12. The system according to claim 11, wherein the operation further includes the processor creating the predetermined function from the plurality of data points.

13. The system according to claim 12, wherein the predetermined function is linear.

14. The system according to claim 10, wherein the operation further includes, by the processor, heating the raw material container containing the solid precursor to the predetermined temperature, sublimating the solid precursor, and generating the precursor gas that flows through the gas line.

15. The system according to claim 8, wherein the supply container comprises a container body and a lid attached to the container body.

16. The system according to claim 15, wherein the lid comprises a chemical substance inlet disposed in the central region of the lid.

17. The heater is in thermal communication with the aforementioned lid, The system according to claim 15, further comprising a cooling device that is in thermal communication with the base portion of the container body.

18. The pressure sensor is the first pressure sensor, The system further comprises a second pressure sensor connected to the gas line, The first pressure sensor is connected to the gas line that is close to the raw material container. The system according to claim 8, wherein the second pressure sensor is connected to the gas line that is close to the supply container.

19. Measuring the aforementioned pressure value The processor receives a first pressure from the first pressure sensor, The processor receives the second pressure from the second pressure sensor, The system according to claim 18, comprising the processor calculating the pressure value based on the first pressure and the second pressure.

20. It is a system, A raw material container containing a solid precursor, A supply container, which is fluidly coupled to the raw material container via a gas line so that the precursor gas formed from the solid precursor can flow from the raw material container to the supply container, Processor and A tangible non-temporary memory configured to communicate with the aforementioned processor, In response to the execution by the aforementioned processor, the processor is instructed to: A system comprising: a tangible non-temporary memory, which stores instructions for the processor to perform an operation including determining a first amount of the solid precursor flowing from the raw material container to the supply container based on the pressure value of the precursor gas in the gas line.

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