Remote solids refill chamber

Abstract

Various examples of the present disclosure relate to methods, systems, and apparatus for coupling a transport container disposed at a first location on a substrate processing platform to a remote refill container disposed at a second location remote from the substrate processing platform, storing a chemical in the remote refill container in a first phase, the method includes receiving a chemical substance in a remote refill container, changing the chemical substance in the remote refill container to a second phase, transferring the chemical substance in the second phase to a delivery container, maintaining a temperature gradient within an interior volume of the delivery container, and returning the chemical substance to the first phase within the interior volume.

Description

Technical Field

[0001] The present disclosure relates generally to semiconductor processing equipment and, more particularly, to methods, systems, and apparatus for refilling chemical precursor delivery containers. Background Art

[0002] Semiconductor manufacturing processes such as chemical vapor deposition (CVD) and atomic layer deposition (ALD) involve depositing thin films on semiconductor wafers (also referred to herein as "substrates"). During processing, the wafer is exposed to one or more precursors in a reaction chamber to deposit a thin layer of material. The precursor sources are typically stored in delivery containers on the processing tool and transported from the delivery containers to the reaction chamber. In order to reduce the need for maintenance and replacement of delivery containers, delivery containers are becoming larger. However, even large delivery containers will eventually become empty and need to be replaced, which requires downtime and may affect quality or safety. Such systems have been generally accepted for their intended purposes.

[0003] However, there remains a need for improved methods, systems, and apparatus to reduce the need for maintenance and replacement of delivery containers. The present disclosure provides a solution to this need. Summary of the invention

[0004] This summary is provided to introduce some concepts in a simplified form. These concepts are further described in detail in the detailed description of the example embodiments disclosed below. This summary is not intended to identify 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.

[0005] Various embodiments of the present disclosure relate to methods, systems, and apparatus for coupling a transport container disposed at a first location on a substrate processing platform to a remote refill container disposed at a second location remote from the substrate processing platform, storing chemicals in a first phase in the remote refill container, changing the chemicals in the remote refill container to a second phase, transferring the chemicals in the second phase to the transport container, maintaining a temperature gradient within an interior volume of the transport container, and returning the chemicals to the first phase within the interior volume.

[0006] According to various examples of the present disclosure, the first phase may be a solid and the second phase may be a gas, and wherein maintaining the temperature gradient further comprises controlling a heating device disposed at a top of the transport container or controlling a cooling device disposed at a bottom of the transport container or a combination thereof in response to sensor data received from one or more temperature sensors inside the transport container, and solidifying the chemical substance within the internal volume at least on a bottom surface of the transport container.

[0007] In some examples, controlling a heating device disposed at a top portion of the transport container or controlling a cooling device disposed at a bottom portion of the transport container, or a combination thereof, can be further based on a comparison of the sensor data with a curve corresponding to the transport container, the curve identifying a predetermined first temperature and a first threshold temperature range for at least a top portion of the transport container and a predetermined second temperature and a second threshold temperature range for at least a bottom portion of the transport container.

[0008] In various examples, the first temperature may be higher than the second temperature. According to various examples of the present disclosure, the first temperature may be higher than the sublimation temperature of the chemical substance, and the second temperature may be lower than the condensation temperature of the chemical substance. Maintaining the temperature gradient may further include maintaining the top of the transport container at a first temperature higher than the phase transition temperature of the chemical substance, maintaining the bottom of the transport container at a second temperature lower than the phase transition temperature of the chemical substance, and providing a thermal barrier between the top of the transport container and the bottom of the transport container.

[0009] According to various examples of the present disclosure, maintaining the temperature gradient further comprises providing a thermal barrier between the top of the transport container and the bottom of the transport container. In some embodiments, the thermal barrier may be disposed in a lower half of the transport container relative to a longitudinal axis extending from the top surface of the transport container to the bottom surface of the transport container. Alternatively, the thermal barrier may be disposed in an upper half of the transport container relative to a longitudinal axis extending from the top surface of the transport container to the bottom surface of the transport container.

[0010] According to various examples of the present disclosure, maintaining the temperature gradient further includes dissipating heat through the chemical substance via a thermally conductive cooling member thermally coupled to the base of the transport container after the chemical substance on the bottom surface of the transport container is solidified.

[0011] According to various examples of the present disclosure, maintaining the temperature gradient further includes storing in the controller memory a first temperature and a first threshold temperature range corresponding to at least the top of the transport container, storing in the controller memory a second temperature and a second threshold temperature range corresponding to at least the bottom of the transport container, wherein the first temperature may be higher than the second temperature, detecting a third temperature within the interior volume of the transport container, and adjusting the heating device or the cooling device in response to the detection. Detecting the third temperature may further include detecting that the third temperature at the top surface of the solidified chemical on the bottom surface of the transport container may be higher than the threshold temperature, and adjusting the cooling device to a fourth temperature lower than the second temperature in response to the detection.

[0012] According to a further example of the present disclosure, a substrate processing system is disclosed, comprising: a transport container, disposed at a first position on a substrate processing platform; a remote refill container, fluidically connected to the transport container via a chemical transport pipeline, the remote refill container being disposed at a second position away from the substrate processing platform; a heating device thermally connected to a top surface of the transport container, a cooling device thermally connected to a bottom surface of the transport container, a thermal barrier disposed between the top surface and the bottom surface, a sensor located within an internal volume of the transport container, and a controller coupled to the sensor, the heating device, and the cooling device, the controller being configured to control the heating device and the cooling device in response to the sensor so as to maintain a temperature gradient within the transport container.

[0013] The substrate processing system can also include one or more cooling members thermally coupled to the base of the transport container. In some examples, the one or more cooling members include rods, fins, or piles, or a combination thereof.

[0014] According to another example of the present disclosure, the thermal barrier can be a vacuum portion within the wall of the transport container. The thermal barrier can be disposed in the upper half of the transport container relative to the longitudinal axis. Alternatively, the thermal barrier can be disposed in the lower half of the transport container relative to the longitudinal axis.

[0015] In some examples, the heating device includes a heater, a heating jacket, a heating block, or a radial heater, or a combination thereof. In other examples, the cooling device includes a cooling coil, an integrated cooling channel, a cooling member, a cooling jacket, or a cold plate, or a combination thereof. According to yet another example of the present disclosure, the substrate processing system includes a plurality of sensors, wherein data from each of the plurality of sensors includes associated position data. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] These and other features, aspects, and advantages of the present invention disclosed herein are described below with reference to the accompanying drawings of specific embodiments, which are intended to illustrate rather than to limit the present invention.

[0017] Figure 1 is a schematic diagram illustrating an example substrate processing system including a transport container disposed on a substrate processing platform;

[0018] Figure 2 It shows Figure 1 A schematic diagram of an example refill subassembly of a substrate handling system depicted in;

[0019] Figure 3 It is shown as Figure 1 A schematic diagram of an example delivery container is shown;

[0020] Figure 4 Shows Figure 1 The example delivery container shown includes a heating device and a cooling device;

[0021] Figure 5 is a schematic diagram illustrating an example bulk refill process;

[0022] Fig. 6A It is shown Figure 1 A schematic diagram of an example transport vessel depicted in , including a heat transfer member;

[0023] Figure 6B It is shown Figure 1 A schematic diagram of a side view of an example delivery container depicted in;

[0024] Figure 7 is a schematic diagram illustrating an example bulk refill process;

[0025] Figure 8 It shows Figure 1 A schematic diagram of an example delivery container depicted in , including a heat transfer member coupled to a base;

[0026] Fig. 9 is a flow chart illustrating an example solid source refill process;

[0027] Fig.10 is a flow chart illustrating an example solid source refill process;

[0028] Fig.11 is a flow chart illustrating an example solid source refill process;

[0029] Fig.12 is a flow chart illustrating an example solid source refill process; and

[0030] Fig.13 is a flow chart illustrating an example solid source refill process.

[0031] It should be understood that the elements in the drawings are shown for simplicity and clarity and are not necessarily drawn to scale. For example, the relative sizes of some elements in the drawings may be enlarged relative to other elements to help improve the understanding of the illustrated embodiments of the present disclosure. DETAILED DESCRIPTION

[0032] Although certain embodiments and examples are disclosed below, it will be appreciated by those skilled in the art that the present invention extends beyond the specifically disclosed embodiments and / or uses of the present invention and their obvious modifications and equivalents. Therefore, it is intended that the scope of the disclosed invention should not be limited by the specifically disclosed embodiments described below.

[0033] As used herein, the term "substrate" may refer to any one or more underlying materials, including any one or more underlying materials that may be modified or on which a device, circuit, or film may be formed. A "substrate" may be continuous or non-continuous; rigid or flexible; solid or porous; and combinations thereof. A substrate may be in any form, such as a powder, a plate, or a workpiece. A plate-like substrate may include wafers of various shapes and sizes. A substrate may be made of semiconductor materials, including, for example, silicon, silicon germanium, silicon oxide, gallium arsenide, gallium nitride, and silicon carbide.

[0034] The continuous substrate may extend beyond the boundaries of the processing chamber in which the deposition process occurs. In some processes, the continuous substrate may be moved through the processing chamber so that the process continues until the end of the substrate is reached. The continuous substrate may be provided by a continuous substrate feeding system to allow the continuous substrate to be manufactured and output in any suitable form.

[0035] Non-limiting examples of continuous substrates may include sheets, nonwoven films, rolls, foils, meshes, flexible materials, bundles of continuous filaments or fibers (eg, ceramic fibers or polymer fibers).The continuous substrate may also include a carrier or sheet on which a non-continuous substrate is mounted.

[0036] The illustrations presented herein are not intended to be actual views of any particular material, structure, or device but are merely idealized representations used to describe embodiments of the present disclosure.

[0037] The specific embodiments shown and described are illustrations of the present invention and its best mode and are not intended to limit the scope of these aspects and implementations in any way. In fact, for the sake of brevity, the traditional manufacturing, connection, preparation and other functional aspects of the system may not be described in detail. In addition, the connecting lines shown in the various figures are intended to represent exemplary functional relationships and / or physical connections between various elements. Many alternative or additional functional relationships or physical connections may exist in actual systems, and / or may not exist in some embodiments.

[0038] The chemical reactant or solid source delivery system may include a delivery container and a heater (e.g., a radiant heat lamp, a resistive heater, etc.). The delivery container includes a source precursor (also referred to as a "chemical substance" or "chemical precursor"), and may be solid (e.g., in powder form) or liquid. The heater heats the delivery container to promote evaporation and / or sublimation of the reactants in the container. The delivery container may have an inlet and an outlet for a carrier gas to flow through the container. The carrier gas may be inert, such as nitrogen, argon, or helium. Typically, the carrier gas transports the reactant vapor (e.g., evaporated or sublimated chemical reactant) with it through the container outlet and ultimately reaches the substrate reaction chamber. The container typically includes an isolation valve for isolating the contents of the container from the fluid outside the container. One isolation valve may be disposed upstream of the container inlet, and another isolation valve may be disposed downstream of the container outlet. The delivery container of some embodiments includes a sublimator (consisting of or substantially consisting of it). Similarly, wherever a "delivery container" is mentioned, a sublimator (e.g., a "solid source chemical substance sublimator") is also explicitly considered.

[0039] Chemical vapor deposition (CVD) is a known process in the semiconductor industry for forming a thin film of material on a substrate such as a silicon wafer. In CVD, reactant vapors (including "precursor gases") of different reactant chemical substances are transported to one or more substrates in a reaction chamber. In many cases, the reaction chamber only includes a single substrate supported on a substrate holder (e.g., a pedestal), and the substrate and substrate holder are maintained at a desired processing temperature. In a typical CVD process, the reactant vapors that react with each other react with each other to form a thin film on the substrate, and the growth rate is related to the temperature and the amount of the reactant gas.

[0040] In some applications, the reactant gas is stored in a reactant delivery container. In such applications, the reactant is generally gaseous at standard pressure and about 1 atmosphere and room temperature. Examples of such gases include nitrogen, oxygen, hydrogen and ammonia. However, in some cases, a vapor of a source chemical substance ("precursor") that is liquid or solid at standard pressure and temperature is used (e.g., hafnium chloride (HfCl4), hafnium oxide (HfO2), zirconium dioxide (ZrO2), zirconium (IV) chloride (ZrCl4), aluminum chloride (AlCl3), tantalum pentafluoride (TaF5), molybdenum pentafluoride (MoF5), silicon tetraiodide (SiI4), molybdenum pentachloride (MoCl5), molybdenum dichloride (MoO2Cl2), tungsten pentachloride (WCl5) etc. or a combination thereof). For some solid materials (referred to herein as "solid source precursors", "solid chemical reactants" or "solid reactants"), the vapor pressure at room temperature is very low, so that they are usually heated and / or maintained at very low pressures to produce a sufficient amount of reactant vapor for the reaction process. Once vaporized (e.g., sublimed or evaporated), maintaining the vapor-phase reactants at or above the vaporization temperature through a processing system can prevent undesirable condensation from occurring in valves, filters, conduits, and other components associated with transporting the vapor-phase reactants between locations (e.g., from a transport vessel to a reaction chamber). Vapor-phase reactants from such natural solid or liquid materials can be used in chemical reactions in a variety of other industries.

[0041] Atomic layer deposition (ALD) is another known process for forming a thin film on a substrate. In many applications, ALD uses solid and / or liquid source chemicals as described herein. ALD is a vapor deposition in which a thin film is accumulated by a self-saturated reaction that is performed in cycles. The thickness of the film is determined by the number of cycles performed. In the ALD process, gaseous reactants are alternately and / or repeatedly supplied to a substrate or wafer to form a thin film of material on the wafer. A reactant is adsorbed on the wafer in a self-limiting process. Different, subsequent pulses of reactants react with the adsorbed material to form a monolayer of the desired material. Decomposition can occur through mutual reactions between adsorbed substances and with appropriately selected reagents, such as in ligand exchange or gettering reactions. In some ALD reactions, only one molecular monolayer is formed per cycle. Thicker films are produced by repeated growth cycles until the target thickness is reached. In some ALD reactions, the reactants that react with each other are kept separate in the gas phase, and removal processes are inserted between substrates exposed to different reactants.

[0042] Traditionally, the size of the delivery container is limited due to the limited available space on the substrate processing platform. When exhausted, the delivery container is removed and refilled, which may result in downtime and loss of wafer production. A remote refill container can be coupled to the delivery container to refill the delivery container on the substrate processing platform (or "tool"). The remote refill container can reduce the need to replace or refill the sublimator. On the contrary, the remote refill container can be used to automatically and / or continuously supply chemicals, such as source precursors, to the delivery container. Therefore, the volume of the remote refill container is not limited by the size of the container set on the substrate processing platform. In some examples, the remote refill container can be set at a position spaced apart from the tool. For example, the remote refill container can be located in another room of the substrate processing platform, through the clean room of the substrate processing platform, adjacent to the substrate processing platform or in a sub-factory. For the purposes of this disclosure, a "sub-factory" is an area below the substrate processing platform. In some examples, it can be built in the floor of the clean room, in a building floor lower than the level at which the substrate processing platform is set, or can include the lower part of the substrate processing platform. A plurality of remote refill containers can be included for filling the delivery container with the source precursor described herein.

[0043] Remote refilling container and / or delivery container can be provided with gas pipeline extending from inlet and outlet, isolation valve on pipeline and fittings on valve, and fittings are configured to be connected to gas flow pipeline of remaining substrate processing platform. It is desirable to provide multiple additional heaters for heating various valves and gas flow pipelines between reactant delivery container and reaction chamber to prevent reactant liquid or vapor from solidifying or condensing and being deposited on these parts. Therefore, gas and / or liquid delivery components between remote refilling container, delivery container and reaction chamber can be maintained at a temperature higher than the evaporation / condensation / sublimation temperature of reactant.

[0044] Furthermore, in order to efficiently refill the delivery container, it is advantageous to refill the container in a controlled manner by deposition or condensation. To control deposition, the temperature of the deposition chemical precursors can be controlled to reduce or prevent condensation or plugging of input (or output) lines that are attached to the delivery container cap, allowing fluid communication to the reactor and the "outside" world. Furthermore, bottom-up filling, or filling from the bottom and interior sidewalls of the delivery container, can achieve close filling on the delivery container.

[0045] Figure 11 is a schematic diagram showing an example substrate processing system 100, which includes a delivery container 102 disposed on a substrate processing platform 110. The substrate processing platform 110 includes one or more reactors 138 and 140, and the reactors 138 and 140 include respective reaction chambers 122 and 124. The reactors 138 and 140 include respective pedestals 142 and 144 to hold respective substrates 146 and 148 during processing. The substrate processing platform 110 includes gas distribution systems 150 and 152 to distribute one or more reactants to the respective surfaces of the substrates 146 and 148. The substrate processing platform 110 may include a vacuum source (not shown) for controlling the vacuum pressure in the one or more reaction chambers 122 and 124. The reactant source may supply the gas phase reactant generated from the solid precursor source delivery container 102 to the gas phase reactor. The reaction chambers 138 and / or 140 may be gas phase reactors. The solid source delivery container 102 may contain a chemical substance 114, which includes a chemical reactant, such as a source chemical substance or precursor, including but not limited to HfCl4, HfO2, ZrO2, ZrCl4, AlCl3, TaF5, MoF5, SiI4, MoCl5, MoO2Cl2, WCl5, etc. or a combination thereof. The chemical substance 114 may be a solid under standard conditions (i.e., room temperature and atmospheric pressure). A carrier gas source 120 may be coupled to the delivery container 102 via a chemical delivery line 136 and may contain a carrier gas. The carrier gas source 120 may be fluidly coupled to the reaction chambers 122 and 124 via a chemical delivery line 154 and valves 158 and 160. When introduced into the delivery container 102, the carrier gas 198 helps to transport the evaporated and / or sublimated reactants, such as the chemical substance 114, to the collector 101 via the container outlet valve 126 via the chemical delivery line 105. Chemicals 114 may exit valve 107 from collector 101 and be delivered to reaction chambers 122 and / or 124 for substrate processing via chemical delivery line 128. Collector 101 may regulate the flow of chemical 114 gas and may maintain a consistent pressure and flow throughout the substrate processing process. Chemical delivery line 128 may include valves 132 and 134 for controlling fluid communication of chemicals 114 and / or carrier gas from delivery container 102 to respective reaction chambers 122 and 124. Inlet and outlet valves on substrate processing platform 110 may be controlled by one or more controllers (e.g., controller 156).

[0046] In one example, the transport container 102 can be coupled to a remote refill container 104 via a chemical delivery line 106. The remote refill container 104 can be located laterally remote from, above, or below the transport container 102 and / or the substrate processing platform 110, such as in a sub-fab below the substrate processing platform 110.

[0047] The remote refill container 104 may contain a refill chemical 114. The remote refill container 104 may be a bulk refill container that may have a greater chemical capacity within the housing 108 than the delivery container 102 because it may not be subject to size limitations associated with the substrate processing platform 110. For example, the remote refill container 104 may have at least 1.5 times, 2 times, 3 times, 4 times, 5 times, 10 times, or 20 times the capacity of the delivery container 102. Other capacities are possible, and claimed subject matter is not limited in this regard.

[0048] The chemical delivery line 106 may extend between an outlet valve 116 of the remote refill container 104 and an inlet valve 118 of the delivery container 102. The inlet valve 118 may be disposed in a cap 130 of the delivery container 102. The outlet valve 116 may be disposed in a cap 182 of the remote refill container 104. The outlet valve 116 and the inlet valve 118 may control fluid communication of the chemical 114 from the remote refill container 104 to the delivery container 102.

[0049] The remote refill container 104 can be configured to vaporize (e.g., sublimate, evaporate) the chemical 114, and can subsequently transfer the evaporated or sublimated chemical 114 to the delivery container 102 via the chemical delivery line 106. In one example, the remote refill container 104 can be proximate to a heating device 174. The heating device 174 can be in thermal communication with the cap 182 and / or the housing 108, and can be disposed on the exterior of the remote refill container 104 or on the interior of the cap 182 and / or the 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 interior volume of the cap 182 and / or the remote refill 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, e.g., evaporate and / or sublimate the chemical 114, so as to transfer the chemical 114 to the delivery container 102 via the chemical delivery line 106. Heating device 174 may include any of a variety of heating devices, such as a heater, a heating jacket, a heating block, and / or a radiant heater or the like known to those skilled in the art, although the claimed subject matter is not limited in this regard.

[0050] The remote refill container 104 can be configured to store the chemical 114 between refill operations. A cooling device 188 can be coupled to the bottom of the remote refill container 104. The cooling device 188 can cool the bottom surface 196 to maintain the chemical 114 in solid form before sublimation. The cooling device 188 can include a cooling plate, a cooling coil, a cooling jacket, a cooling fan, a Peltier cooler, a cooling member, or an integrated coolant channel for circulating a coolant, etc., or any combination thereof.

[0051] The remote refill container 104 can be configured to operate at a selected temperature. For example, the operating temperature can be determined based on the expected 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, or in the range of about 50°C to about 400°C, or in the range of about 75°C to about 300°C, or in the range of about 100°C to about 250°C. Other temperature ranges are also possible, and the claimed subject matter is not limited thereto.

[0052] The delivery container 102 can receive the chemical 114 in a vapor phase from the remote refill container 104 via the chemical delivery line 106. The chemical delivery line 106 can be disposed at the top 190 of the delivery container 102, such as in the cover 130. In one example, the cover 130 and the inlet valve 118 can be configured to maintain a temperature above the vaporization temperature of the chemical 114 when the chemical 114 enters the delivery container 102 to prevent the chemical 114 from condensing in the delivery container components, such as the cover 130, the valve 184 and / or 118, or the chemical delivery line 106, etc. or any combination thereof.

[0053] The transport container 102 can be thermally coupled to one or more heating devices 176 for heating the chemical 114 and maintaining the chemical 114 in a gas phase at the top 190 of the transport container 102. The heating device 176 can include a heater, a heating jacket, a heating block, a heating fin, and / or a radial heater, etc. or a combination thereof. The heating device 176 can be disposed at the top 190 of the transport container 102, such as within the cover 130 and / or outside the transport container 102. Such a heating device 176 is used to control or regulate the temperature of the chemical 114 during refilling operations, material handling operations, and storage of the chemical 114.

[0054] The bottom 192 of the transport container 102 can be thermally coupled to one or more cooling devices 186 for cooling the chemical 114 at the bottom 192 of the transport container 102. The cooling device 186 can include a cooling plate, a cooling coil, a variable pitch cooling coil, a cooling jacket, a cooling member (e.g., cooling rods and / or heat sinks (see FIGS. 6 and 8 )), a cooling fan, a Peltier cooler, or an integrated coolant channel for circulating a coolant, the like, or any combination thereof.

[0055] As will be discussed in more detail, such heating device 176 and cooling device 186 provide a temperature gradient within the transport container 102 (see Figure 3 Element 324 in).

[0056] In one example, the inner sidewall 178 and / or the lid 130 can be configured to transfer heat from the heating device 176 to the chemical 114 before the chemical 114 enters the transport container 102 to maintain a temperature above the condensation point of the chemical 114. This applied heat and / or pressure can maintain the chemical 114 in a vapor phase. As the chemical 114 cools, it may condense at the bottom surface 196 and / or the inner sidewall 178 below the thermal barrier 109.

[0057] The temperature of the bottom 192 of the transport container 102 can be cooled by the cooling device 186 (e.g., a cold plate) to a lower temperature than the input chemical delivery line 106, the interior sidewall 178 above the thermal barrier 109 (discussed in more detail below), or the cover 130 of the transport container 102. This provides a cooling effect along the longitudinal axis 224 (see FIG. Figure 2 ), where the highest temperature in the system may be at the top 190 of the transport container 102, and the lowest temperature in the system may be at the base 111. The chemical 114 solidifies when it comes into contact with the bottom inner surface 196 of the base 111 of the transport container 102. During refilling, the chemical 114 will form a solid at the bottom of the transport container 102 and can be stored there until material processing operations. The cooling device 186 can maintain a temperature at the bottom 192 of the transport container 102 sufficient to keep the chemical 114 in a solid phase.

[0058] In the transport container 102, the thermal barrier 109 can insulate the top 190 of the transport container 102 from the bottom 192. This can help the top 190 of the transport container 102 maintain a higher temperature than the bottom 192. The thermal barrier 109 can enhance the temperature gradient extending from the top 190 to the bottom 192 of the transport container 102. This can promote the deposition of the chemical 114 on the interior sidewall 115 below the thermal barrier 109 and the bottom surface 196 of the transport container 102.

[0059] In one example, the thermal barrier 109 can be disposed circumferentially around the transport container 102 between the top 190 and the bottom 192. The thermal barrier 109 can be formed by a variety of methods. For example, the thermal barrier 109 can include a ring of insulating material embedded in the interior sidewall 178. It can be embedded by any of a variety of methods known to those skilled in the art, such as by welding, brazing, bonding, airtight fastening, etc. or a combination thereof.

[0060] In one example, the thermal barrier 109 can be comprised of an insulating layer disposed within the inner sidewall 178 of the container. The sidewall can be double-walled with a hollow portion or space between the inner and outer walls. The thermal barrier 109 can be a double-walled portion filled with an insulating material or a vacuum. The insulating material can be a variety of materials, such as ceramic fiber, high temperature insulating wool, and / or foam insulation (e.g., polystyrene, polyurethane, or polyisocyanurate). The length L of the thermal barrier 109 on the longitudinal axis of the transport container 102 is tb This may vary depending on various factors, such as the desired temperature range within the transport container 102, the chemical nature of the chemical 114 to be stored, the materials used in the transport container 102 and the insulation within the thermal barrier 109, and / or other similar factors.

[0061] The thermal barrier 109 can prevent heat from dissipating from the top 190 of the delivery vessel 102 to better maintain the temperature at the top 190 above the condensation temperature of the chemical 114. This can reduce or prevent condensation of the chemical 114, thereby reducing or preventing blockage of components such as the chemical delivery line 106, valves 118, 126, and 184, or a combination thereof.

[0062] During the refill operation (such as Figure 5-Figure 8 ), the transport container 102 can be configured to operate with a temperature gradient within the internal volume 180. For example, the operating temperature near the top 190 can be determined based on the desired condensation rate of the chemical 114. In some examples, the operating temperature is in the range of about 10°C to about 500°C, or in the range of about 50°C to about 400°C, or in the range of about 75°C to about 300°C, or in the range of about 100°C to about 250°C. The selected operating temperature may depend on the vaporization temperature of the chemical 114. Similarly, the base 111 of the transport container 102 can be maintained at a lower temperature than the top 190 to solidify the chemical 114 on the base 111 and maintain the temperature gradient within the transport container 102. The selected operating base temperature can also depend on the chemical to be solidified. In addition, in order to prevent gaseous particles from solidifying in unwanted areas on the interior of the transport container 102, the bottom 192 can be set to a temperature that is at least cooler than the top 190. In one example, the base 111 is the coldest location in the internal volume 180 of the transport container 102. Therefore, the operating temperature of the base 111 may be much lower than the condensation point of the chemical 114 .

[0063] In one example, the temperature gradient can extend between the base 111 and the cover 130. In one example, the bottom 192 can be maintained at or below the first threshold temperature, while the top 190 can be maintained at or above the second threshold temperature, which is higher than the first threshold temperature. For example, the base 111 and the cover 130 can be maintained at a temperature difference (e.g., the difference between the first threshold temperature and the second threshold temperature). In one example, the temperature difference between the base 111 and the cover 130 can be at least about 1°C, about 5°C, about 10°C, about 20°C, about 30°C, about 40°C, about 50°C, about 60°C, about 70°C, about 80°C, or about 160°C, or any value therebetween, or fall within any range having endpoints therein. Other temperature differences are possible, and the claimed subject matter is not limited thereto.

[0064] In one example, the temperature gradient can be set along the longitudinal axis 224 (see Figure 2 ), which axial distance is about 1 inch, about 3 inches, about 6 inches, about 9 inches, about 12 inches, about 15 inches, about 18 inches, about 21 inches, about 24 inches, about 27 inches, about 30 inches, about 32 inches, about 34 inches, about 36 inches, about 64 inches, or about 128 inches, or any value therebetween, or falling within any range having endpoints therein. The gradient can be stepped or linear. Other gradient sizes are possible, and the claimed subject matter is not limited thereto.

[0065] In one example, during a material processing operation, 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 to evaporate and / or sublimate the chemical 114. Once evaporated or sublimated, the chemical 114 can be transported to the reaction chamber 122 and / or 124 for substrate processing as previously described. Prior to evaporation and / or sublimation, the chemical 114 can be stored as a solid in the delivery container 102.

[0066] During material processing, the delivery container 102 can be configured to operate at a selected temperature based on the desired sublimation rate of the chemical substance 114 precursor / reactant. In some examples, the operating temperature is in the range of about 10° C. to about 500° C., or in the range of about 50° C. to about 400° C., or in the range of about 75° C. to about 300° C., or in the range of about 100° C. to about 250° C. Other temperature ranges are possible, and the claimed subject matter is not limited thereto.

[0067] Once the chemical 114 is depleted, the delivery container 102 may be refilled from the remote refill container 104. It is not necessary to completely deplete the chemical 114 in the delivery container 102 before refilling from the remote refill container 104.

[0068] In the illustrated example, the controller 156 includes a device interface 162, a processor 164, a user interface 166, and a memory 168. The device interface 162 connects the processor 164 to a wired or wireless link 170. The processor 164 can be operably connected to the user interface 166 (e.g., receiving user input and / or providing user output through the user interface 166), and can be arranged to communicate with the memory 168. The memory 168 includes a non-transitory machine-readable medium having recorded thereon a plurality of program modules 172, which contain instructions that, when read by the processor 164, cause the processor 164 to perform certain operations. As described below, these operations include operations of a material layer deposition method and a method for refilling the delivery container 102 (e.g., Figure 5-6A and Figure 7-13 In view of this disclosure, those skilled in the art will appreciate that the controller 156 may have a different arrangement in other examples and still be within the scope of the present disclosure.

[0069] Figure 2 It shows Figure 1 Schematic diagram of an example refill subassembly 200 of a substrate processing system 100 is depicted in FIG. The refill subassembly 200 includes a delivery container 102 coupled to a remote refill container 104 via a chemical delivery line 106. The remote refill container 104 can be configured to maintain a temperature gradient along a longitudinal axis 202 to store the chemical 114 (e.g., a precursor) in a solid state before the chemical 114 (e.g., a precursor) sublimates or evaporates. The base 204 of the remote refill container 104 can be at a relatively low temperature (e.g., to maintain the precursor as a solid). The cover 182 can reach a relatively high temperature to facilitate transfer to the delivery container 102. Such a temperature is sufficient to at least cause the chemical 114 to enter a vapor phase and minimize condensation in downstream flow path components, such as the chemical delivery line 106, the cover 182, the outlet valve 116, and the inlet valve 118.

[0070] In some examples, carrier gas source 216 can be coupled to remote refill container 104 via chemical delivery line 222 and can supply carrier gas 220 to remote refill container 104. Valve 218 can control the flow of carrier gas 220. Carrier gas 220 can facilitate the transfer of sublimated chemical 114 from remote refill container 104 to delivery container 102.

[0071] In one example, heaters 206 and 208 can be coupled to the chemical delivery line 106 to maintain a "transfer temperature," which can be a vaporization temperature to prevent condensation during transport. Such a vaporization temperature can be above a phase change temperature (e.g., a sublimation temperature) of the chemical 114. The heaters 206 and 208 can include heating jackets or other heating devices known to those skilled in the art, although the claimed subject matter is not limited thereto. The heaters 206 and 208 can be wrapped, coiled, surrounded, or otherwise disposed about the chemical delivery line 106. The chemical delivery line 106 can have few angles or corners to prevent condensation. Valves, connection points, and / or other interruptions in the chemical delivery line 106 can be minimized to the extent that they can offset any condensation in the chemical delivery line 106 due to the remote refill container 104 being remote (i.e., spaced apart) from the substrate processing platform 110 (see Figure 1 ) setting resulting in a higher risk of condensation.

[0072] In one example, one or more spare remote refill containers 290 may be co-located with the remote refill container 104 to reduce the downtime required to replace the remote refill container 104 when the remote refill container 104 is depleted. When the remote refill container 104 needs to be replaced, the spare remote refill container 290 may be quickly coupled to the delivery container 102 via the chemical delivery line 106 (or via a different chemical delivery line) to avoid downtime waiting for the remote refill container 104 to be removed and replaced. Alternatively, the spare remote refill container 290 may be coupled to the remote refill container 104 to refill the container 104 at other suitable idle times, such as between refill operations or between upstream events requiring downtime on the substrate processing platform 110.

[0073] In one example, the refilling process may be manually controlled and / or the refilling operation may be partially or fully automated using various sensors for automatic feedback control via the controller 156. For example, the sensor 210 may be disposed near or within the interior volume 180 of the delivery container 102, the sensor 212 may be disposed within or near the chemical delivery line 106, and the sensor 214 may be disposed near or within the interior volume 220 of the remote refill container 104. The sensors 210, 212, and 214 may monitor various physical phenomena, such as acoustics, vibrations, chemicals, moisture, flow, light, pressure, force, density, temperature, and / or presence, etc., or any combination thereof. The sensors 210, 212, and / or 214 may, for example, monitor a temperature gradient in the delivery container 102 and / or monitor the temperature of the chemical 114 disposed in at least one of the chemical delivery line 106, the delivery container 102, or the remote refill container 104, or a combination thereof. Sensors 210, 212, and / or 214 may alternatively or additionally monitor the temperature of or within chemical delivery line 106, delivery container 102, and / or remote refill container 104, or a combination thereof. Sensors 210, 212, and / or 214 may generate sensor data based on the monitoring and send the sensor data to controller 156 (see Figure 1 ) to adjust the monitored equipment to change the monitored parameter (e.g., temperature). For example, controller 156 may adjust one or more heating devices 174, 176, 206, and / or 208 and / or cooling devices 186 and 188, or a combination thereof, based on sensor data. In some embodiments, the electronics and / or computer elements used to control one or more of reaction chamber 122, reaction chamber 124, delivery container 102, and / or remote refill container 104 may be found elsewhere in the system. For example, a central controller may control two devices in one or more chambers themselves, as well as control valves connected to various containers and any associated heating devices. One or more valves may be used to control the flow of gases throughout substrate processing system 100.

[0074] Figure 3 1 is a schematic diagram showing an example transport container 102 and a cover 130 coupled to the top of the transport container 102, as shown in FIG. Figure 1 shown.

[0075] Temperature gradient 324 may include a first temperature in top portion 190, a second temperature in upper middle portion 302, a third temperature in lower middle portion 304, and a fourth temperature in bottom portion 192. An ideal temperature gradient for a refill operation of delivery container 102 with chemical 114 would include having a temperature above thermal barrier 109 that is above the condensation temperature of chemical 114 and below the condensation temperature of chemical 114 below thermal barrier 109. For example, the first temperature and the second temperature would be the same, above the condensation temperature of chemical 114 and above the third temperature and the fourth temperature. In such an ideal system, the third temperature and the fourth temperature would be the same, below the condensation temperature and below the first and second temperatures.

[0076] However, in an actual system, the temperature gradient 324 may gradually cool from the highest temperature in the top portion 190 to the lowest temperature in the bottom portion 192. The first temperature may be higher than the second temperature. The first and second temperatures may both be higher than the condensation temperature of the chemical 114 to protect the components of the transport container 102. The third temperature may be higher than the fourth temperature, both may be lower than the condensation temperature of the chemical 114, and both may be lower than the first and second temperatures.

[0077] The temperature gradient 324 may be maintained by a feedback mechanism including the controller 156. The sensor array 312 may include one or more sensors 210, 306, 308, and / or 310 disposed within the interior volume 180 of the transport container 102. The sensors 210, 306, 308, and / or 310 may monitor a variety of physical phenomena, such as acoustics, vibrations, chemicals, moisture, flow, light, pressure, force, density, temperature, and / or presence, etc. or any combination thereof. The sensors 210, 306, 308, and / or 310 may be positioned at selected locations of the transport container 102 along the temperature gradient 324 to correlate temperature data (or other data) with the location along the temperature gradient 324. For example, the sensor 210 may be disposed within the top portion 190, the sensor 306 may be disposed within the upper middle portion 302, the sensor 308 may be disposed within the lower middle portion 304, and the sensor 310 may be disposed within the bottom portion 192. At least one of the sensors 210, 306, 308, and / or 310 can monitor a physical phenomenon (e.g., obtain a temperature reading) and / or transmit sensor data (including, for example, data related to the measured / monitored physical phenomenon, a sensor identification, position data, etc., or a combination thereof) to the controller 156. In one example, the position data can be stored in the memory 168 in a table associated with a sensor identification associated with a sensor location within the volume 180 of the transport container 102.

[0078] In one example, controller 156 may control heating device 176 and / or cooling device 186 based on data from sensors 210, 306, 308, and / or 310 to maintain temperature gradient 324. Temperature gradient 324 may be based on a temperature-programmed time curve. Temperature gradient 324 may be maintained in a variety of other ways and based on various sensor data and / or stored time curves and temperature parameters, and the claimed subject matter is not limited in this regard.

[0079] Figure 4 An example transport container 102 is shown that includes a heating device 176 and a cooling device 186. In one example, a temperature gradient 324 extends from a first temperature above the condensation temperature of the chemical 114 at the top 190 to a second temperature below the condensation temperature of the chemical 114 near the bottom 192 of the transport container 102. The chemical 114 may be transferred to the transport container 102 in a vapor phase from a remote refill container 104. It may be desirable for the chemical 114 to first condense at the coldest location at a bottom surface 414 in the transport container 102, which may be cooled by the cooling device 186. This first condensed portion may serve as a nucleation point for further solidification of the chemical 114 entering the transport container 102. The cover 130 may be maintained at an elevated temperature to prevent the chemical 114 from condensing at locations such as the inlet valve 118, the outlet valve 126, and / or the chemical delivery line 106 (see FIG. 1 ). Figure 1 ) components. Therefore, it is desirable to maintain a temperature gradient 324 to promote solidification of the chemical 114 on the cooled interior surface 414 and prevent the chemical 114 from solidifying in and around the cover 130. Depending on the effectiveness and location of the thermal barrier 109, the temperature gradient 324 can change suddenly or gradually from a highest temperature at the top 190 of the transport container 102 to a lowest temperature at the bottom 192. The heating device 176 and the cooling device 186 can be coupled to the controller 156, and the controller 156 can be configured to control the heating device 176 and the cooling device 186 in response to the sensors 210, 306, 308, and / or 310 of the sensor array 312 to maintain the temperature gradient 324.

[0080] In one example, the cooling device 186 may include any of a variety of cooling mechanisms, such as a cooling coil 402, an integrated cooling channel 404, a cooling member 406, a cooling jacket 408, a cold plate 410, etc. or a combination thereof. The controller 156 may control various functions of the cooling device 186 (e.g., device temperature, coolant temperature, coolant flow) to maintain the temperature gradient 324.

[0081] In one example, the cooling coil 402 can be disposed on a portion of the outer surface 412 near the bottom 192 or at any level of the transport container 102. The cooling coil 402 can help maintain the temperature gradient 324 by keeping the bottom 192 cool to below a threshold temperature (e.g., the condensation temperature of the chemical substance 114). The cooling coil 402 can be hollow to allow a coolant to flow therethrough. The coolant can be any of a variety of coolants known to those skilled in the art, such as water, deionized water, ethylene glycol / water solution, and dielectric fluid, etc., or a combination thereof. The cooling coil 402 can be formed of a variety of thermally conductive materials, including but not limited to stainless steel, aluminum, copper, etc., or a combination thereof.

[0082] In one example, the integrated cooling channel 404 can be formed (e.g., machined, etched, and / or 3D printed) at any level into the inner sidewall 178 of the transport container 102. The integrated cooling channel 404 can help maintain the temperature gradient 324 by keeping the bottom 192 cool to below the threshold temperature. The integrated cooling channel 404 can be hollow to allow a coolant to flow therethrough. The coolant can be any of a variety of coolants known to those skilled in the art, such as water, deionized water, ethylene glycol / water solution, and dielectric fluid, or a combination thereof. The integrated cooling channel 404 may also include a conduit disposed in the cooling channel 404 formed by a thermally conductive material.

[0083] In one example, the cooling member 406 can be coupled to the bottom surface 414. Figure 2 As discussed, the cooling member 406 can help maintain the temperature gradient 324 by dissipating heat from the solid chemical 114 formed during the refill operation on the surface 414. Such cooling by the solid block can facilitate cooling of the top surface of the solid chemical 114 below the threshold temperature. The cooling member 406 can be formed of a thermally conductive material, such as stainless steel, aluminum, copper, etc., or a combination thereof.

[0084] In one embodiment, the cooling jacket 408 may be disposed on a portion of the outer surface 412 near the bottom 192 or at any level of the transport vessel 102. The cooling jacket 408 may be a housing including an integrated cooling conduit 420. The cooling jacket 408 may help maintain the temperature gradient 324 by keeping the bottom 192 cool to below the threshold temperature. The cooling conduit 420 may be hollow to allow a coolant to flow therethrough. The coolant may be any of a variety of coolants known to those skilled in the art, such as water, deionized water, ethylene glycol / water solution, and dielectric fluid, or the like, or a combination thereof.

[0085] In one example, a cold plate 410 can be disposed on the bottom surface 416 of the transport container 102. The cold plate 410 can be a flat metal plate made of a material with high thermal conductivity, such as aluminum. The cold plate 410 can help maintain the temperature gradient 324 by keeping the bottom 192 cool below a threshold temperature by dissipating heat from the bottom surface 416. The cold plate 410 can have integrated cooling channels and / or embedded cooling conduits to allow coolant to flow therethrough to remove additional heat from the bottom surface 414.

[0086] In one example, the heating device 176 may include any of a variety of heating mechanisms, such as a heating block 418, a heating jacket 420, a resistive heater 422, a hot plate 424, a heating lamp 426, etc. or a combination thereof. The controller 156 may control various functions of the heating device 176 (e.g., device temperature, brightness, temperature change) to maintain the temperature gradient 324.

[0087] In one example, the heating jacket 420 can be thermally coupled to and disposed on a portion of the outer surface 412 near the top 190 of the delivery container 102. The heating jacket 420 can be thermally coupled to and disposed on a portion of the outer surface 412 near the top 190 of the delivery container 102. The heating jacket 420 can be thermally coupled to and disposed on a portion of the outer surface 412 near the top 190 of the delivery container 102. Figure 1 ), etc., or a combination thereof, to a threshold temperature (e.g., the condensation temperature of the chemical 114) to help maintain the temperature gradient 324. The heating jacket 420 may include a housing with an integrated heating element 428. The integrated heating element 428 may be a conduit through which a heating fluid may flow, or may be a resistive heating device.

[0088] In one example, a resistive heater 422 can be thermally coupled to the delivery container 102 within the top 190 and / or the lid 130. The resistive heater 422 can help maintain the temperature gradient 324 by heating components near the top 190 (e.g., the lid 130, valves 118, 184, and / or 126, the chemical delivery line 106, etc., or a combination thereof) above a threshold temperature.

[0089] In one example, a heat plate 424 can be thermally coupled to the delivery container 102 within the top 190 and / or the lid 130. The heat plate 424 can help maintain the temperature gradient 324 by heating components near the top 190 (e.g., the lid 130, valves 118, 184, and / or 126, the chemical delivery line 106, etc., or a combination thereof) above a threshold temperature.

[0090] In one example, heat lamps 426 can be thermally coupled to the delivery container 102 within the top 190 and / or the lid 130. The heat lamps 426 can help maintain the temperature gradient 324 by heating components near the top 190 (e.g., the lid 130, valves 118, 184, and / or 126, the chemical delivery line 106, etc., or a combination thereof) above a threshold temperature.

[0091] Figure 5 is a schematic diagram illustrating an example batch refilling process 500. In one example, the transport container 102 can be heated by any of a variety of heating devices in the top 190 (as described above with reference to Figure 1-4 Detailed description), and can be actively cooled by any of a variety of cooling devices (such as those described above with reference to Figure 1-4 Detailed description). A thermal barrier 109 may be disposed within the transport container 102 to thermally isolate the actively cooled bottom portion 192 from the heated top portion 190. Such thermal isolation may be used to promote condensation of the chemical 114 in the actively cooled region of the transport container 102 after the chemical 114 exits the heated components (e.g., the lid 130, valve 184, and / or chemical line 106) in the top portion 190 in gaseous form.

[0092] As schematically shown in stage 502, the batch refill process 500 begins with the chemical 114 entering the interior volume 180 of the delivery container 102 in gaseous form. The chemical 114 flows into the interior volume 180 via the heated chemical line 106 through the heated cover 130. As the chemical 114 continues to flow into the delivery container 102, the chemical 114 begins to condense and deposit on the bottom 192. At stage 504, the chemical 114 begins to accumulate at the base 111 within the interior volume 180 of the delivery container 102. The driving force is the vapor pressure increment between the pure component vp at 150°C and the vp at 130°C. In an example, there may be no external pumping to drive the flow of the chemical 114. Instead, the driving force may be a pressure gradient to drive the transfer of gas from the remote refill container 104 to the delivery container 102, the pressure gradient being generated by the condensation of the chemical 114 within the delivery container 102. The pressure gradient generated by the phase change of the chemical 114 from gas to solid can drive the gas from the refill container 104 to the delivery container 102.

[0093] The thermal barrier 109 is disposed near the bottom 192 of the transport container 102. In one example, the thermal barrier 109 can be composed of a thermal insulation layer disposed within the inner sidewall 178. The sidewall can be double-walled with a hollow portion 622 (e.g., a space) between the inner wall 624 and the outer wall 626. The thermal barrier 109 can be a double-walled portion filled with an insulating material or a vacuum.

[0094] The example temperatures provided herein are for illustration purposes only and are not intended to limit the claimed subject matter. A representative temperature is that of the chemical substance 114 having a condensation temperature of approximately 150°C.

[0095] In one example, the temperature gradient 510 extends in the longitudinal direction along the length of the transport container 102 from a higher temperature T1 (eg, about 170° C.) at the top 190 to a lower temperature T2 (eg, about 130° C.) at the bottom 192 .

[0096] In an example system, the thermal barrier 109 may not completely isolate the bottom 192, so the temperature may gradually decrease longitudinally from the top 190 toward the bottom 192. For example, the temperature T3 may be between the temperature T1 and the temperature T2 (e.g., about 160°C), and the temperature T4 may be between the temperature T3 and the temperature T2 (e.g., about 150°C). However, the temperatures T3 and T4 may still be above the phase change temperature of the chemical 114. This can reduce blockages in the cover 130, the valve 184, and / or the chemical line 106. In addition, it can reduce condensation on the interior sidewall 178 in the top 190. Heat is dissipated from the heated top 190 of the transport container 102 to the cooled bottom 192. When in contact with a surface at or below the phase change temperature and / or when the ambient atmosphere is at or below the phase change temperature, the chemical 114 can cool to its phase change temperature, causing it to condense.

[0097] At stage 506, as the chemical 114 continues to condense within the transport container 102, the solid chemical 114 may accumulate higher in the middle portion forming the vertical column 512, rather than being evenly packed on the surface 526, due to the temperature distribution within the transport container 102. The interior sidewall 178 may be hotter than the bottom 192 due to heat dissipation from the heated components in the top 190 through the transport container 102. Therefore, the temperature of the interior sidewall 178 at or above the thermal barrier 109 may be higher than the phase change temperature of the chemical 114, and therefore the chemical 114 will not condense on the interior sidewall 178 at or above the thermal barrier 109. Dashed arrows 518 and 520 point in the direction of heat dissipation through the sidewall 178.

[0098] Heat is also dissipated from the surface 526 to the base 111 through the chemical 114. Dashed arrows 522 and 524 point in the direction of heat dissipation through the solidifying chemical 114. Heat dissipation through the chemical 114 may be slower than heat dissipation through the interior sidewalls 178. As the condensation thickness grows, heat transfer through the chemical 114 will become increasingly difficult, and the sublimated heat cannot be easily vented. At this point, the temperature within the vertical column 512 and / or at the surface 526 may reach the temperature of the interior sidewalls 178, rather than the temperature of the cooler base 111, causing the condensation of the chemical 114 to slow or stop, and the vertical column 512 to stop growing. The height of the vertical column 512 at which condensation can stop depends on the thermal conductivity of the chemical 114.

[0099] Moving to stage 508, in one example, lowering the base 111 temperature can lower the temperature of the chemical 114 surface 526 and restart (or further enable) condensation of the chemical 114 in the vertical column 512. Continuing with the example temperature above, when condensation stops, the surface 526 can reach about 150°C. For example, lowering the base 111 temperature from about 130°C to about 110°C can cool the surface 526 (and the inner sidewall 178) and can restart condensation, allowing the vertical column 512 to reach a new height. As the temperature of the base 111 decreases, the resulting cooling can extend through the inner sidewall 178 of the delivery container 102 into the lid 130, valves 184 and 118, and / or the chemical delivery line 106. These and other components may become clogged. In some examples, due to the increased heat capacity of the growing solid, it is not necessary to reduce the base temperature by increasing the heat flux to maintain a cooler temperature.

[0100] Fig. 6A An example delivery container 102 is shown that includes a heat transfer member 602 coupled to a base 111. The powdered chemical 114 may have a lower thermal conductivity than the material from which the delivery container 102 is made, such as stainless steel. In one example, one or more heat transfer members 602 may be coupled to the base 111 to increase thermal conductivity through the chemical 114. The heat transfer members 602 may provide a shorter path for heat diffusion through the powdered chemical 114 to cool the surface 526. The heat transfer members 602 may be connected around a common member base 610 configured to be coupled to the base 111. Alternatively, the heat transfer members 602 may be separate members that are each connected to the base 111 (see also Figure 8 ). The heat transfer member 602 may include fins, round rods, polygonal piles, etc. or any one or combination of various heat transfer devices known to those skilled in the art. Contrast arrow 604 indicates the direction of heat transfer from the chemical substance 114 to the heat transfer member 602. Arrow 606 indicates the direction of heat transfer from the top of the heat transfer member 602 to the base 111 longitudinally along the heat transfer member 602.

[0101] Figure 6B A side view of an example transport container 102 is shown. The thermal barrier 109 may be disposed circumferentially, forming an annular ring 620 around the transport container 102 between the top 190 and the bottom 192 .

[0102] Figure 7 An example bulk refill process 700 is shown.

[0103] The example temperatures provided herein are for illustration purposes only and are not intended to limit the claimed subject matter. A representative temperature is that of the chemical substance 114 having a condensation temperature of approximately 150°C.

[0104] In one example, the thermal barrier 726 can be placed on the top 190 of the transport container 102. As described above, the transport container can be heated by any of a variety of heating devices in the top 190 (such as those described above with reference to Figure 1-4 Detailed description), and can be actively cooled by any of a variety of cooling devices (such as those described above with reference to Figure 1-4 Detailed description).

[0105] Additionally, to facilitate condensation of chemical 114 in actively cooled regions of transport container 102 , thermal barrier 726 may be disposed at top 190 of transport container 102 .

[0106] As schematically shown in stage 702, the batch refill process 700 begins with the chemical 114 entering the interior volume 180 of the delivery container 102 in gaseous form. The chemical 114 flows into the interior volume 180 through the heated lid 130 via the heated chemical line 106. As the chemical 114 continues to flow into the delivery container 102, the chemical 114 begins to deposit at the base 111 and the interior sidewall 178.

[0107] At stage 704, chemical substance 114 begins to accumulate at base 111 and on interior wall 178 within interior volume 180 of transport container 102. Thermal barrier 726 is disposed near top 190 of transport container 102. Temperature gradient 710 extends in a longitudinal direction along the length of transport container 102 from a higher temperature T1 (e.g., about 170° C.) at top 190 to a lower temperature T2 (e.g., about 130° C.) at bottom 192.

[0108] In one example, the thermal barrier 726 may not completely isolate the area below the thermal barrier 726. Instead, the temperature may gradually decrease longitudinally from the top 190 toward the bottom 192, thereby generating a temperature gradient 710. The temperature T5 may be between the temperature T1 and the temperature T2 (e.g., about 150°C), the temperature T4 may be between the temperature T5 and the temperature T3 (e.g., about 140°C), and as the gradient 710 moves longitudinally away from the thermal barrier 720, the temperature T3 may be closer to the temperature T2 (e.g., about 130°C). The temperatures T5, T4, and T3 may all be below the condensation temperature of the chemical 114, which helps the chemical 114 condense at the sidewall 178 and the bottom surface 196.

[0109] At stage 706, as the chemical 114 continues to condense within the transport container 102, solid chemical 114 may accumulate on the sidewalls 178 and from the bottom surface 196. As heat beneath the thermal barrier 726 is dissipated through the transport container 102 to the cooled bottom 192, the interior sidewalls 178 may be at or below the condensation temperature of the chemical 114. Arrows 722 and 724 point in the direction of heat dissipation through the interior sidewalls 178.

[0110] Heat is also dissipated from surface 730 to base 111 through chemical 114. Dashed arrows 726 and 728 point in the direction of heat dissipation through solidifying chemical 114. The condensation rate and thickness of chemical 114 near bottom 192 and lower interior sidewall 178 will be greater than the condensation rate and thickness of chemical 114 closer to thermal barrier 726, which will grow slower and thinner than solidifying chemical 114 in the lower portion of transport container 102 at any point in time. Chemical 114 can have a maximum fill height in transport container 102 that is directly related to the height at which the thermal barrier is placed. Thus, the fill height of transport container 102 with thermal barrier 726 is higher than the fill height of transport container 102 with thermal barrier 109 (see FIG. 109 ). Figure 5 ). Although the heat dissipation through the chemical 114 may slow as the condensation thickness grows, heat transfer through the chemical 114 will become increasingly difficult. At this point, the surface 730 may reach a temperature close to or above the condensation temperature of the chemical 114, causing the condensation of the chemical 114 to slow or stop, and the solid chemical 114 stops filling the delivery container 102.

[0111] Moving to stage 708, in one example, lowering the base 111 temperature can lower the temperature of the chemical 114 surface 730 and restart (or further enable) condensation of the chemical 114 within the container 102. Continuing with the above example temperature, the surface 730 can approach 150°C when condensation slows or stops. Lowering the base 111 temperature, for example from about 130°C to about 110°C, can cool the surface 730 and can restart condensation, allowing the solidified chemical 114 volume to reach a new height. As the temperature of the base 111 decreases, the resulting cooling can extend through the sidewall 178 of the delivery container 102 into the lid 130, valves 184 and 118, and / or the chemical delivery line 106. As the temperature drops, these and other components may become clogged due to condensation.

[0112] Figure 8 An example transport container 102 including a heat transfer member 802 coupled to a base 111 is shown. The thermal conductivity of the powdered chemical 114 may be lower than the material of which the transport container 102 is made, such as stainless steel. In an example, one or more heat transfer members 802 may be coupled to the base 111 to improve the thermal conductivity through the chemical 114. The heat transfer member 802 may provide a shorter path for heat diffusion through the powdered chemical 114 to cool the surface 730. The heat transfer members 802 may be separate members that are each connected to the base 111. Alternatively, the members 802 may be connected around a common member base (not shown) configured to be coupled to the base 111. The heat transfer member 802 may include fins, round rods, polygonal piles, etc. or any one or combination of various heat transfer devices known to those skilled in the art. Contrast arrow 804 indicates the direction of heat transfer from the chemical 114 to the heat transfer member 802. Arrow 806 indicates the direction of heat transfer from the top of the heat transfer member 802 to the base 111 along the longitudinal direction of the heat transfer member 802. The heat transfer member 802 may be made of various heat conductive materials, such as stainless steel, aluminum, titanium and / or tungsten, etc., or a combination thereof.

[0113] Fig. 9 is a flow chart generally depicting an embodiment of a solid source refill process 900. Reference will be made to Figure 1-2 Process 900 is described. Process 900 may be controlled by controller 156. Process 900 may begin at block 902, where a transport container 102 (see Figure 1 ) may be coupled to a remote refill container 104. The transport container 102 may be disposed at a first location on the substrate processing platform 110, and the remote refill container 104 may be disposed at a second location away from the substrate processing platform 110. In an example, the first location may be separated from the second location by a distance of about 1 foot to about 20 feet, 20 feet to about 100 feet, 100 feet to about 200 feet, or 200 feet to about 500 feet. Other distances are possible, and the claimed subject matter is not limited thereto.

[0114] The transport container 102 may be coupled to the remote refill container 104 via a chemical delivery line 106. The process 900 may move to block 904, where a chemical 114 (e.g., a precursor) may be stored in a first phase in the remote refill container. In one example, the first phase may be a solid phase. In another example, the first phase may be a liquid or a gas. At block 906, the phase of the chemical 114 may be changed to a second phase by the action of one or more components of the remote refill container 104. Such an action may include heating and / or pressurizing the chemical 114. In one example, the first phase and the second phase are different. The process 900 may move to block 908, where the chemical 114 may be transferred to the transport container 102 in the second phase to refill the transport container 102 with the chemical 114. The chemical 114 may be transferred from the remote refill container 104 to the transport container 102 by opening the chemical delivery line 106, wherein the opened chemical delivery line 106 places the remote refill container 104 in fluid communication with the transport container. At block 910, a temperature gradient within the transport container 102 may be maintained. In one example, the controller 156 may be coupled to the heating device 176, the cooling device 186, and one or more sensors disposed within the interior volume 180. The controller 156 may be configured to control the temperature of the heating device 176 and / or the cooling device 186 in response to sensor data received from one or more sensors (e.g., sensors 210, 306, 308, and / or 310). At block 912, the chemical 114 may be deposited on at least the bottom surface 414 (see FIG. 4 ) of the transport container 102. Figure 4 ) returns to the first phase (e.g., solidification) within the internal volume 180.

[0115] One or more of the actions described in blocks 902, 904, 906, 908, 910, and / or 912 may be performed simultaneously and / or sequentially. After refilling is complete, the chemical 114 may be transferred to other components in fluid communication with the delivery container 102, such as the collector 101 or the reaction chambers 138 and / or 140, to process one or more substrates 146 and / or 148.

[0116] Fig.10 is a flowchart depicting an example process 1000 of Fig. 9 An example embodiment of a solid source refill process 900 is shown. In one example, reference is made to Figure 1-9 Process 1000 is described. Process 1000 may be controlled by controller 156. Process 1000 may begin at block 1002, where a transport container 102 (see Figure 1) may be coupled to the remote refill container 104 at the top 190 via the chemical delivery line 106. The delivery container 102 may be disposed at a first location on the substrate processing platform 110, and the remote refill container 104 may be disposed at a second location remote from the substrate processing platform 110. The process 1000 may continue at block 1004, where a solid chemical 114 (e.g., a precursor) may be stored in the remote refill container 104 in a solid phase at a first temperature below a condensation temperature of the chemical 114. At block 1006, the chemical 114 may sublime within the remote refill container 104 at a second temperature above the condensation temperature by exposing the chemical 114 to heat and / or pressure to convert the solid into a gas.

[0117] In one example, block 910 (see Fig. 9 ) “Maintaining a temperature gradient within the transport container” may include box 1008, box 1010 and / or box 1012.

[0118] At block 1008, the controller 156 may generate a temperature signal in response to one or more temperature sensors 210, 306, 308, and / or 310 (see FIG. 1004 ) within the transport container 102. Figure 3 ) receives sensor data to control the heating device 176 to heat the top 190 of the transport container 102 to maintain the temperature gradient 324. In one example, the heating device 176 can be controlled based on a comparison of the sensor data with a temperature gradient curve corresponding to the transport container 102 stored in the memory 168, the temperature gradient curve identifying at least a predetermined first temperature and / or a first threshold temperature range of the top 190. Maintaining the temperature gradient 324 (see Figure 3 ) may also include maintaining the top 190 at approximately the first temperature.

[0119] At block 1010, the controller 156 may cool the bottom 192 of the transport container 102 by controlling the cooling device 186 in response to sensor data received from one or more temperature sensors 210, 306, 308, and / or 310 within the transport container 102 to maintain the temperature gradient 324. In one example, controlling the cooling device 186 may be based on a comparison of the sensor data with a temperature gradient profile stored in the memory 168 corresponding to the transport container 102, the temperature gradient profile identifying at least a predetermined second temperature and / or a second threshold temperature range for the bottom 192. Maintaining the temperature gradient 324 may also include maintaining the bottom 192 at approximately the second temperature.

[0120] In one example, the first temperature may be higher than the second temperature. For example, the first temperature may be higher than the sublimation temperature of the chemical substance 114 , and the second temperature may be lower than the condensation temperature of the chemical substance 114 .

[0121] At block 1012, maintaining the temperature gradient 324 also includes maintaining the temperature gradient 324 at the top surface 113 and the bottom surface 196 of the transport container 102 (see Figure 1 ) provide a thermal barrier 109 between the top and bottom surfaces of the transport container 102. In one example, the location of the thermal barrier 109 can affect the manner in which the chemical 114 solidifies within the transport container 102. The thermal barrier 109 can be disposed in the upper or lower half of the transport container relative to a longitudinal axis extending from the top surface to the bottom surface of the transport container 102.

[0122] At block 1016 , the chemical 114 may be transferred in a vapor phase to the top 190 of the delivery container 102 to refill the delivery container 102 .

[0123] At block 1014, the sublimated chemical 114 may be transferred to the remote refill container 102 to the transport container 102. At block 1016, the chemical 114 solidifies and accumulates on the bottom surface 196 within the interior volume 180 of the transport container 102. At block 1018, the controller 156 may determine whether the refilling of the transport container 102 is complete, such as whether the chemical 114 solid has grown to a predetermined height. The controller 156 may maintain a temperature gradient within the interior volume 180 of the transport container 102 to promote the growth of the solid mass of the chemical 114, such as by maintaining the temperature of the bottom surface 196 below the condensation temperature of the chemical 114. The process 1000 may continuously return to block 1006 until the transport container 102 is refilled. Blocks 1006-1018 may be performed simultaneously during the filling process. After the refilling of the transport container 102 with the chemical 114 is completed, the process 1000 moves to block 1020. At block 1020, the solidified chemical 114 may be stored in the delivery container 102 until used in a material processing operation. Blocks 1002-1020 may be performed simultaneously or sequentially.

[0124] Fig.11 is a flow chart illustrating an example process 1100, which is an example stage of the solid source refill process 900 at box 910 (see Fig. 9 ). The process 1100 may be controlled by the controller 156. Figure 1-9 Process 1100 is described.

[0125] At block 1008, the controller 156 may control the heating device 176 to heat the top 190 of the transport container 102. At block 1010, the controller 156 may maintain the temperature gradient 324 by cooling the bottom 192 of the transport container 102. At block 1012, the top surface 113 and the bottom surface 196 (see FIG. 104 ) of the transport container 102 may be cooled. Figure 1 ) between the heat barrier 109. In block 1102, heat can be cooled by the heat conductive cooling member 406 (see Figure 4 ) is dissipated through solid chemical 114.

[0126] Fig.12 is a flow chart illustrating an example process 1200 of Fig. 9 The example stage of the solid source refill process 900 at block 910 is shown. In one example, reference is made to Figure 1-9 Process 1200 is described. Process 1200 may be controlled by controller 156 .

[0127] At block 1008, the heating device 176 may be controlled by the controller 156 to heat the top 190 of the transport container 102. At block 1010, the controller 156 may maintain the temperature gradient 324 by cooling the bottom 192 of the transport container 102. At block 1012, the top surface 113 and the bottom surface 196 (see FIG. 104 ) of the transport container 102 may be cooled. Figure 1 ) provide a thermal barrier 109 between the top 190 of the transport container 102. At block 1202, a first temperature and / or a first threshold temperature range corresponding to the top 190 of the transport container 102 can be stored in the memory 168. The first temperature can be above the sublimation temperature of the chemical 114. In one example, the controller 156 can monitor the sensor data as described above to determine whether a selected location (e.g., the top 190) within the transport container 102 is within a first threshold temperature range of the first temperature. At block 1204, a second temperature and / or a second threshold temperature range corresponding to the bottom 192 of the transport container 102 can be stored in the memory 168. The second temperature can be equal to or below the sublimation temperature of the chemical 114. In one example, the controller 156 can monitor the sensor data as described above to determine whether a selected location (e.g., the bottom 192) within the transport container 102 is within a second threshold temperature range of the second temperature.

[0128] At block 1206, a third temperature may be detected within the interior volume of transport container 102. The detection may be performed by sensors 210, 306, 308, and / or 310. If the temperature data from sensors 210, 306, 308, and / or 310 indicates that the temperature of a selected location (e.g., top 190 and / or bottom 192) is outside of an identified temperature range (e.g., first and / or second threshold temperature ranges), controller 156 may take action at block 1208, where controller 156 may adjust heating device 176 or cooling device 186 in response to the detection.

[0129] Fig.13 is a flowchart depicting an example process 1000 of Fig. 9 An example embodiment of a solid source refill process 900 is shown. In one example, reference is made to Figure 1-9 Process 1000 is described. Process 1300 may be controlled by controller 156 .

[0130] At block 1008, the heating device 176 may be controlled by the controller 156 to maintain the temperature gradient 324 by heating the top 190 of the transport container 102. At block 1010, the controller 156 may maintain the temperature gradient 324 by cooling the bottom 192 of the transport container 102. At block 1012, a thermal barrier 109 may be provided between the top surface 113 and the bottom surface 196 of the transport container 102. At block 1302, a first temperature and / or a first threshold temperature range corresponding to the surface 526 of the solidified chemical 114 may be stored in the memory 168. At block 1304, a second temperature may be detected on the surface 526 of the solidified chemical 114. The detection may be performed by the sensor 210, 306, 308, and / or 310, etc. If temperature data from sensors 210, 306, 308 and / or 310, etc. indicates that the temperature at surface 526 is outside of an identified temperature range (e.g., a first threshold temperature range), controller 156 may take action at box 1306, where controller 156 may adjust cooling device 186 to a lower temperature to reduce the temperature of surface 526, thereby restarting condensation of chemical 114, which may have ceased due to the increase in temperature at surface 526.

[0131] It should be understood that the configuration and / or method described herein are exemplary in nature, and these specific embodiments or examples should not be considered restrictive, because many variations are possible. The specific routine or method described herein can represent one or more of any number of processing strategies. Therefore, the various actions shown can be performed in the order shown, in other orders, or omitted in some cases.

[0132] The headings provided herein, if any, are for convenience only and do not necessarily affect the scope or meaning of the apparatus and methods disclosed herein.

Claims

1. A method comprising: coupling a delivery container disposed at a first location on the substrate processing platform to a remote refill container disposed at a second location remote from the substrate processing platform; storing the chemical in a first phase in a remote refill container; changing the chemical in the remote refill container to a second phase; transferring the chemical in the second phase to a transfer vessel; maintaining a temperature gradient within the interior volume of the transport vessel; and The chemical species are returned to the first phase within the interior volume.

2. The method according to claim 1, wherein: The first phase is a solid, the second phase is a gas, and wherein maintaining the temperature gradient further comprises: In response to sensor data received from one or more temperature sensors inside the transport container, controlling a heating device disposed at the top of the transport container or controlling a cooling device disposed at the bottom of the transport container, or a combination thereof; and The chemical within the interior volume is solidified at least on a bottom surface of the delivery container.

3. The method according to claim 2, wherein: The controlling of a heating device disposed at the top of the transport container or the controlling of a cooling device disposed at the bottom of the transport container or a combination thereof is also based on a comparison of the sensor data with a curve corresponding to the transport container, the curve identifying a predetermined first temperature and a first threshold temperature range of at least the top of the transport container and a predetermined second temperature and a second threshold temperature range of at least the bottom of the transport container.

4. The method according to claim 3, wherein: The first temperature is higher than the second temperature.

5. The method according to claim 3, wherein: The first temperature is higher than a sublimation temperature of the chemical substance, and the second temperature is lower than a condensation temperature of the chemical substance.

6. The method according to claim 1, wherein: Maintaining the temperature gradient also includes: maintaining a top portion of the transport container at a first temperature above a phase transition temperature of the chemical substance and maintaining a bottom portion of the transport container at a second temperature below the phase transition temperature of the chemical substance; and A thermal barrier is provided between the top of the transport container and the bottom of the transport container.

7. The method according to claim 1, wherein: Maintaining the temperature gradient also includes providing a thermal barrier between the top of the transport container and the bottom of the transport container.

8. The method according to claim 7, wherein: The thermal barrier is disposed in a lower half of the transport container relative to a longitudinal axis extending from a top surface of the transport container to a bottom surface of the transport container.

9. The method according to claim 7, wherein: The thermal barrier is disposed in an upper half of the transport container relative to a longitudinal axis extending from a top surface of the transport container to a bottom surface of the transport container.

10. The method according to claim 1, wherein: Maintaining the temperature gradient also includes dissipating heat through the chemical substance after the chemical substance on the bottom surface of the transport container solidifies via a thermally conductive cooling member thermally coupled to the base of the transport container.

11. The method according to claim 1, wherein: Maintaining the temperature gradient also includes: storing in a controller memory a first temperature and a first threshold temperature range corresponding to at least a top portion of a transport container; storing in a controller memory a second temperature and a second threshold temperature range corresponding to at least a bottom portion of the transport container, wherein the first temperature is greater than the second temperature; detecting a third temperature within the interior volume of the transport container; and In response to the detection, the heating device or the cooling device is adjusted.

12. The method according to claim 11, wherein: Detecting the third temperature further includes: detecting a third temperature at a top surface of the solidified chemistry on a bottom surface of the delivery container that is greater than a threshold temperature; and In response to detecting, the cooling device is adjusted to a fourth temperature that is lower than the second temperature.

13. A substrate processing system comprising: A delivery container disposed at a first position on the substrate processing platform; a remote refill container in fluid communication with the delivery container via a chemical delivery line, the remote refill container being disposed at a second location remote from the substrate processing platform; a heating device in thermal communication with the top surface of the transport container; a cooling device in thermal communication with the bottom surface of the transport container; a thermal barrier disposed between the top surface and the bottom surface; a sensor positioned within the interior volume of the delivery container; as well as A controller coupled to the sensor, the heating device, and the cooling device is configured to control the heating device and the cooling device in response to the sensor so as to maintain a temperature gradient within the transport container.

14. The substrate processing system of claim 13, further comprising one or more cooling members thermally coupled to a base of the transport container.

15. The substrate processing system according to claim 14, wherein: The one or more cooling members include rods, fins or piles or a combination thereof.

16. The substrate processing system according to claim 13, wherein: The thermal barrier is a vacuum section within the walls of the transport container.

17. The substrate processing system according to claim 13, wherein: The thermal barrier is disposed in an upper half of the transport container relative to the longitudinal axis.

18. The substrate processing system according to claim 13, wherein: The thermal barrier is disposed in a lower half of the transport container relative to the longitudinal axis.

19. The substrate processing system according to claim 13, wherein: The heating device includes a heater, a heating jacket, a heating block or a radial heater or a combination thereof.

20. The substrate processing system according to claim 13, wherein: The cooling device includes a cooling coil, an integrated cooling channel, a cooling member, a cooling jacket or a cold plate or a combination thereof.

21. The substrate processing system of claim 13, further comprising a plurality of sensors, wherein the data from each of the plurality of sensors includes associated position data.

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