Charge container and connector for chemical sublimator

Abstract

To provide a solid source chemical intermediate filling container.SOLUTION: The charging vessel 100 can comprise a proximal end, a distal end, and a base 112 disposed at the proximal end configured to hold the solid source chemical reactant therein. The intermediate fill container can further comprise a lid 120 at the distal end comprising the second thermal conductor. The lid may comprise a chemical inlet, a carrier gas inlet, and a chemical outlet. The filled container may further comprise an intermediate layer arranged between the base and the lid. The intermediate layer may comprise an insulator configured to reduce heat flow between the base and the lid.SELECTED DRAWING: Figure 1

Description

[Technical Field]

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS All applications claiming foreign or domestic priority are identified in the Application Data Sheet filed with this application and are hereby incorporated by reference under 37 CFR 1.57.

[0002] A typical solid or liquid source reactant delivery system includes a solid or liquid source container and a heater. The container can contain a chemical reactant to be vaporized. A carrier gas travels through a passage within the container, carrying the vaporized and / or sublimated chemical reactant through a container outlet and ultimately to a substrate reaction chamber.

[0003] TECHNICAL FIELD This application relates generally to systems and methods involving semiconductor processing equipment, and more particularly to evaporation systems for chemical vapor delivery. Summary of the Invention

[0004] Some embodiments include a solid source chemical intermediate fill vessel comprising a proximal end, a distal end, and a base disposed at the proximal end configured to hold a solid source chemical reactant therein. The base can comprise a first thermal conductor. The base can be configured to be maintained at or below a first threshold temperature. The intermediate fill vessel can further comprise a lid at the distal end comprising a second thermal conductor. The lid can be configured to be maintained at or above a second threshold temperature greater than the first threshold temperature. The lid can comprise a chemical inlet configured to receive sublimated or vaporized chemical reactant therethrough into the base. The lid can comprise a carrier gas inlet configured to receive a carrier gas flow therethrough, and the lid can comprise a chemical outlet configured to pass sublimated or vaporized chemical reactant from the lid. The fill vessel can further comprise an intermediate layer disposed between the base and the lid. The intermediate layer comprises or consists of an insulator configured to reduce heat flow between the base and the lid.

[0005] The details of one or more embodiments of the subject matter described herein are set forth in the accompanying drawings and the description herein. Other features, aspects, and advantages will become apparent from the description, drawings, and claims. Neither this summary nor the following detailed description is intended to define or limit the scope of the inventive subject matter. [Brief explanation of the drawings]

[0006] These and other aspects of the present disclosure will become readily apparent to those skilled in the art in view of the description herein, the appended claims, and the drawings which illustrate, but do not limit, the invention.

[0007] [Figure 1] FIG. 1 shows a schematic example of a filled container according to several configurations.

[0008] [Figure 2] FIG. 2 shows a side view of an example of a filled container.

[0009] [Figure 3] FIG. 3 shows a perspective view of the filled container of FIG.

[0010] [Figure 4] FIG. 4 shows a side view of an example of a fill chamber system.

[0011] [Figure 5] FIG. 5 shows a cross-sectional perspective view of the fill chamber system shown in FIG.

[0012] [Figure 6] FIG. 6 shows an example of a solid source chemistry system including a charge vessel, a solid source chemical sublimator, a chemical supply, and a carrier gas supply. DETAILED DESCRIPTION OF THE INVENTION

[0013] The headings provided herein, if any, are for convenience only and do not necessarily affect the scope or meaning of the claimed invention. This specification describes a system and related methods for delivering vaporized or sublimated reactants into a high-volume deposition module.

[0014] The following detailed description sets forth specific embodiments to aid in understanding the claims, but the invention can be practiced in many different embodiments and ways, as defined and covered by the claims.

[0015] A chemical reactant or solid source delivery system can include a solid or liquid source container and a heater (e.g., radiant heat lamp, resistance heater, and / or the like). The container contains a source precursor (sometimes referred to as a "chemical precursor"), which can be solid (e.g., in powder form) or liquid. The heater heats the container to promote vaporization and / or evaporation of the reactants within the container. The container can have an inlet and an outlet for the flow of a carrier gas (e.g., N2) through the container. The carrier gas can be inert, such as nitrogen, argon, or helium. Typically, the carrier gas carries the reactant vapor (e.g., vaporized or sublimated chemical reactant) through the container's outlet and ultimately to the substrate reaction chamber. Typically, the container includes an isolation valve for fluidly isolating the contents of the container from the exterior of the container. One isolation valve can be located upstream of the container's inlet, and another isolation valve can be located downstream of the container's outlet. In some embodiments, the source container includes, consists essentially of, or consists of a sublimator. That is, whenever a "source vessel" is referred to herein, a sublimator (eg, a "solid source chemical sublimator") is also expressly intended.

[0016] Chemical vapor deposition (CVD) is a known process in the semiconductor industry for forming thin films of materials on substrates, such as silicon wafers. In CVD, reactant vapors (including "precursor gases") of different reactant chemicals are supplied to one or more substrates in a reaction chamber. Often, the reaction chamber contains only a single substrate supported on a substrate holder (e.g., a susceptor), and the substrate and substrate holder are maintained at a desired process temperature. In a typical CVD process, mutually reactive reactant vapors react with each other to form a thin film on the substrate, with the growth rate related to the temperature and the amount of reactant gas. In some variations, the energy driving the deposition reactants is provided in whole or in part by a plasma.

[0017] In some applications, reactant gases are stored in gaseous form in reactant source vessels. In such applications, reactants are often gases at standard pressure and temperature, approximately 1 atmosphere and room temperature. Examples of such gases include nitrogen, oxygen, hydrogen, and ammonia. However, in some cases, vapors of source chemicals ("precursors") that are liquids or solids (e.g., hafnium chloride, hafnium oxide, zirconium dioxide, etc.) at standard pressure and temperature are used. Some solid materials (referred to herein as "solid source precursors," "solid chemical reactants," or "solid reactants") have very low vapor pressures at room temperature, so they are typically heated and / or maintained at very low pressures to generate sufficient reactant vapor for the reaction process. After vaporization (e.g., sublimation or evaporation), maintaining the vapor-phase reactant above its vaporization temperature throughout the processing system prevents undesired condensation in valves, filters, conduits, and other components associated with delivering the vapor-phase reactant to the reaction chamber. Vapor-phase reactants from such naturally occurring solid or liquid materials are useful for chemical reactions in a variety of other industries.

[0018] Atomic layer deposition (ALD) is another known process for forming thin films on substrates. In many applications, ALD uses solid and / or liquid source chemicals, as described herein. ALD is a type of vapor deposition that deposits films through self-saturating reactions performed in cycles. The thickness of the film is determined by the number of cycles performed. In an ALD process, gaseous reactants are sequentially and / or repeatedly delivered to a substrate or wafer to form a thin film of material on the wafer. One reactant adsorbs on the wafer in a self-limiting process. A different pulse of reactant then reacts with the adsorbed material to form a monolayer of the desired material. Decomposition may occur through interactions between adsorbed species and with appropriately selected reagents, such as ligand exchange or gettering reactions. In some ALD reactions, as little as a monolayer of one molecule is formed per cycle. Thicker films are produced through repeated growth cycles until the target thickness is achieved.

[0019] In some ALD reactions, mutually reactive reactants are kept separate in the gas phase by intervening removal processes between substrate exposures to different reactants. For example, in time-resolved ALD processes, reactants are delivered in pulses to a stationary substrate and are typically separated by purge or evacuation phases. In space-resolved ALD processes, the substrate moves through zones of different reactants. Some processes can combine aspects of both space-resolved and time-resolved ALD. Those skilled in the art will appreciate that some variants or hybrid processes allow for some degree of CVD-like reaction, either by selection of deposition conditions outside the normal ALD parameter window and / or by allowing some overlap between mutually reactive reactants during substrate exposure.

[0020] Reactant source vessels typically have gas lines extending from inlets and outlets, isolation valves on the lines, and fittings on the valves that are configured to connect to the gas flow lines of the rest of the substrate processing equipment. It is often desirable to provide several additional heaters to heat the various valves and gas flow lines between the reactant source vessels and the reaction chamber to prevent reactant vapors from condensing and depositing on such components. Thus, the gas delivery components between the source vessels and the reaction chamber are sometimes referred to as a "hot zone" where the temperature is maintained above the vaporization / condensation / sublimation temperature of the reactants.

[0021] As described herein, various vessels may be included for filling reactant source vessels with source precursors. The vessels may include “intermediate fill” vessels or “transfill” vessels (for simplicity, intermediate fill vessels or transfill vessels may be referred to herein simply as “fill vessels”). Traditionally, source vessels are removed from reactor systems and refilled, which can lead to downtime and lost wafer production. Transfill vessels can advantageously reduce the need to replace or refill sublimators. Instead, transfill vessels can be used to automatically and / or continuously supply source precursors to the reactor system. A fill chamber system can include one or more transfill vessels. Furthermore, transfill vessels according to embodiments herein can be located near, adjacent to, or within the reactor system. Proximity of the transfill vessel to the reactor system can reduce the need for long piping, reduce the possibility of condensation in the piping, and / or reduce the need for unnecessary fluidic elements. However, because the transfill vessel does not need to be removed from the reactor system for refilling, the transfill vessel can achieve the advantages of being located proximal to or internal to the reactor system (such as a relatively short flow path) without the labor and downtime associated with refilling. Further features are described herein with reference to various configurations.

[0022] Another advantage of the various transfill vessels described herein relates to the temperature gradient achievable within the transfill vessel. Generally, chemical precursors may be contained (e.g., stored) in a solid state within the transfill vessel or may be sublimated or vaporized for delivery to another location (e.g., a deposition module or reaction chamber). In some configurations, a carrier gas can be used to transport the vaporized chemical precursor from the transfill vessel to another location (e.g., a deposition module or reaction chamber). Thus, the base of the transfill vessel is preferably at a relatively low temperature (e.g., to maintain the precursor as a solid), and the lid of the transfill vessel is preferably at a relatively high temperature (e.g., to promote the precursor to enter the vapor phase so that it can be delivered to another location while minimizing condensation on valves and downstream flow paths). As described herein, an intermediate layer can help maintain a temperature gradient within the transfill vessel. The intermediate layer can include an insulating material that reduces and / or inhibits thermal communication between the lid and the base.

[0023] FIG. 1 schematically illustrates an example of a filling vessel 100 according to some configurations. The filling vessel 100 can contain chemical reactants, such as solid or liquid source precursors. “Solid source precursor” has its customary and ordinary meaning in the art, in light of the present disclosure. It refers to a source chemical that is solid under standard conditions (i.e., room temperature and atmospheric pressure). In some embodiments, the filling vessel 100 can include a base 112, a lid 120, and a mid-section 116. The filling vessel 100 can define a vessel axis extending in a proximal direction 104 and a distal direction 108. The vessel axis can be oriented in an “up” and “down” direction with reference to FIG. 1. As shown, the base 112 is disposed proximal to the mid-section 116 and the lid 120. As described herein, FIG. 1 should not be construed as limiting the number of elements that the filling vessel 100 can include. The mid-section 116 can be disposed between the base 112 and the lid 120. In some embodiments, the lid 120 is configured to be mechanically attached to the middle section 116. This can be done using one or more attachment means (e.g., bolts, screws, etc.). In particular embodiments, the lid 120 and / or the base 112 are mechanically attached to the middle section 116 in an airtight manner. In some embodiments, the base 112 is removably secured onto the middle section 116.

[0024] The intermediate section 116 may be disposed between the base and the lid. The intermediate section 116 may be disposed in contact with both the base 112 and the lid 120. The intermediate section 116 may comprise an insulator configured to reduce and / or inhibit heat flow between the base 112 and the lid 120. The intermediate section 116 may comprise one or more separate chambers. The one or more chambers may contain a vacuum. The intermediate section 116 may be configured to maintain a temperature gradient between the base 112 and the lid 120 such that the base 112 is maintained at or below a first threshold temperature and the lid 120 is maintained at or above a second threshold temperature that is greater than the first threshold temperature. For example, the base 112 and the lid 120 may be maintained at a temperature difference (e.g., a difference between the second threshold temperature and the first threshold temperature). For example, the temperature difference between the base and the lid can be at least about 1°C, about 2°C, about 3°C, about 4°C, about 5°C, about 6°C, about 7°C, about 8°C, about 9°C, about 10°C, about 11°C, about 12°C, about 13°C, about 14°C, about 15°C, about 18°C, about 20°C, about 25°C, about 30°C, any value therebetween, or any range having endpoints therein, e.g., about 1°C to about 5°C, about 1°C to about 10°C, about 1°C to about 15°C, about 1°C to about 20°C, about 1°C to about 25°C, about 5°C to about 10°C, about 5°C to about 15°C, about 5°C to about 20°C, about 5°C to about 25°C, about 10°C to about 15°C, about 10°C to about 20°C, or about 10°C to about 25°C. The slope can be disposed over a distance (e.g., axial distance) of about 1 inch, about 2 inches, 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 33 inches, about 36 inches, any value therebetween, or any range having endpoints therein, such as about 3 inches to about 9 inches, about 3 inches to about 12 inches, about 3 inches to about 24 inches, about 3 inches to about 36 inches, about 9 inches to about 12 inches, about 9 inches to about 24 inches, about 9 inches to about 36 inches, about 12 inches to about 24 inches, about 12 inches to about 36 inches, or about 24 inches to about 36 inches.

[0025] Filling vessel 100 may include one or more heating and / or cooling elements (not shown). The cooling element (e.g., a water cooler or cooling plate) may be positioned near a proximal portion of base 112. Additionally or alternatively, a heating element (e.g., a heating rod, heating filament, heating plate, and / or heating fins) may be positioned at or near a distal portion of lid 120. Thus, intermediate section 116 may be able to reduce and / or inhibit heat flow between an actively heated portion (e.g., lid 120) and an actively cooled portion (e.g., base 112) of filling vessel 100. The use of heating and / or cooling elements can provide more precise control of the temperature gradient and / or temperature. In some examples, the cooling element is positioned proximal to base 112. One or more cooling elements may be positioned adjacent to (e.g., in contact with) base 112. Additionally or alternatively, one or more heating elements may be positioned distal to lid 120. The cooling element may include a fluid cooling element (e.g., water-cooled, air-cooled, etc.). The heating element may include a heating rod, a heating filament, a heating plate, a heating fin, or any other type of heating element. The one or more heating elements may be configured to heat the lid 120 and / or one or more valves via radiation. In some examples, the heating element may heat the lid 120 via conduction.

[0026] The ratio of the height of the lid 120 to the mid-section 116 may be such that a temperature gradient is positioned a favorable distance from one or more valves of the lid 120 to keep those valves at a sufficiently high temperature (e.g., above a second threshold temperature) to minimize condensation within the valves of the lid 120. The ratio of the lid height to the mid-section height may be greater than about 1, greater than about 1.5, greater than about 2, greater than about 3, greater than about 4, greater than about 5, greater than about 6, or any value therebetween, or within any range having endpoints therein. The mid-section 116 may comprise a ceramic, metal, or other structural material.

[0027] For example, it may be advantageous to minimize the volume or footprint that a fill vessel 100 would require so that it can be placed within a reactor system. A compact vessel assembly can reduce such footprint. In certain embodiments, each fill vessel 100 has a volume of about 40 cm 2 ~150cm 2 The filling container 100 may have an area (eg, where the filling container 100 is located).

[0028] The middle section 116 may include one or more exhaust sections configured to prevent heat flow therethrough. For example, the middle section 116 may include multiple spaced apart exhaust sections. The filling vessel 100 may include one or more vacuum pumps (not shown) for evacuating the exhaust sections. In some configurations, the vacuum pumps are positioned between the exhaust sections of the filling vessel 100.

[0029] Lid 120 may include one or more inlets and / or outlets. The inlets and / or outlets may include corresponding valves. As shown in FIG. 1 , lid 120 may include chemical inlet 124, carrier gas inlet 128, and chemical outlet 132. Chemical inlet 124 may be configured to receive a chemical therethrough. The chemical may be in a sublimated or vaporized form (e.g., in combination with a carrier gas) when entering filling vessel 100 (e.g., from a larger bulk filling vessel).

[0030] The carrier gas inlet 128 can allow the flow of carrier gas therethrough. The carrier gas inlet 128 can include a valve coupled to the carrier gas inlet 128 of the filling vessel 100. The carrier gas can combine with the chemical that has sublimated or vaporized within the filling vessel 100. The effluent from the filling vessel 100 then includes the carrier gas and the reactant gas that has vaporized from the interior of the filling vessel 100. In some embodiments, the interior of the filling vessel 100 is configured to include a headspace after being filled with chemical reactants. The headspace can be in fluid communication with the chemical inlet 124, the carrier gas inlet 128, and / or the chemical outlet 132 and can be configured for sublimation of the chemical reactants by a fluid (e.g., a carrier gas) within the headspace. Thus, the headspace can provide a fail-safe so that the chemical reactants can continue to sublimate or vaporize even if one or more of the inlets / outlets are clogged.

[0031] An inert or inert gas is preferably used as a carrier gas for the vaporized precursor. An inert gas (e.g., nitrogen, argon, helium, etc.) may be supplied to the filling vessel 100 through a carrier gas inlet 128. In some embodiments, different inert gases may be used for various processes and systems described herein. It will be understood that additional valves and / or other fluid control elements not shown may be included.

[0032] The effluent (e.g., carrier gas plus vaporized chemical) can pass through chemical outlet 132. Chemical outlet 132 can be in communication with a reaction chamber or deposition module and / or another fill vessel. In some configurations, chemical outlet 132 is configured to route the vaporized chemical (e.g., along with a carrier gas) to a reaction chamber or deposition module, for example, in preparation for a downstream chemical reaction. One or more of chemical inlet 124, carrier gas inlet 128, and chemical outlet 132 can include corresponding valves configured to control gas flow therethrough. Further information regarding solid source chemical sublimators and / or their fluidics is described in U.S. Patent No. 8,137,462, entitled "PRECURSOR DELIVERY SYSTEM," issued March 20, 2012, the entire contents of which are incorporated herein by reference for all purposes. It is understood that other valves and / or other fluidic elements not shown can be included. Certain configurations can include other valves and other fluidic elements not shown.

[0033] In certain configurations, the base 112 is configured to hold a solid source chemical. The base 112 may include a substantially flat surface for holding a chemical reactant, although other shapes and variations are possible. The filling vessel 100 may define an interior, such as the space between the interior of the walls, the space between the ceiling of the filling vessel 100 and the floor of the base 112, etc. In some embodiments, the interior is configured to contain a chemical reactant, such as a solid source chemical. The filling vessel 100, or portions thereof, may be formed in a variety of ways. For example, the filling vessel 100 may include two or more sides stacked and / or attached to one another.

[0034] In some embodiments, the height of the filled container 100 assembly can range from approximately 25 cm to 120 cm. In some embodiments, the height can range from approximately 50 cm to 100 cm, and in some embodiments, is approximately 60 cm (approximately 24 inches). In some embodiments, the width (e.g., diameter) of the filled container 100 can range from approximately 20 cm to 50 cm. In some embodiments, the width of the filled container 100 can range from approximately 30 cm to 40 cm, and in certain embodiments, is approximately 38 cm (approximately 15 inches). In some embodiments, the container 104 can have a height:diameter aspect ratio ranging from approximately 1 to 4. In some embodiments, the container is approximately cylindrical in shape, although other shapes are possible. That is, in some embodiments, the housing 110 comprises, consists essentially of, or consists of a cylindrical shape. In some embodiments, the mass of the (unfilled) filled container 100 in various embodiments described herein can range from approximately 10 kg to 50 kg. In some embodiments, the mass of a filled charging vessel 100 can range from approximately 35 kg to 85 kg. A smaller mass vessel can be more easily transported, but a larger mass allows for a larger reactant volume, requiring fewer refills and allowing for longer charging of the sublimator.

[0035] 2-3 illustrate another example of a filling vessel 200 according to some embodiments. FIG. 2 illustrates a side view of the example filling vessel 200. The filling vessel 200 may include a base 212, a mid-section 216, and a lid 220. FIG. 3 illustrates a perspective view of the filling vessel 200. As shown, the filling vessel 200 includes a chemical inlet 224, a carrier gas inlet 228, and a chemical outlet 232. Each of the chemical inlet 224, the carrier gas inlet 228, and the chemical outlet 232 includes a corresponding valve for controlling gas flow therethrough. The filling vessel 200 may include the features described herein with respect to the filling vessel 100 described herein. Corresponding elements may also have similar functionality.

[0036] 3 includes a plurality of insulating chambers 236. Each insulating chamber 236 may include an insulator, such as a vacuum interior, to prevent heat flow therethrough. Additionally or alternatively, the insulating chambers 236 may include an insulating material.

[0037] Filling vessel 200 can comprise separate lid 220 and base 212 sidewalls (as shown) or can be formed from a single structure. Lid 220 may have a circular or rectangular cross-sectional shape, although other shapes are suitable. In some embodiments, lid 220 and / or base 212 are fluid-tightly sealed with middle section 216 such that gas cannot substantially enter and / or exit filling vessel 200. Chemical reactants can be contained within filling vessel 200.

[0038] The illustrated fill vessel 200 may be coupled (directly or indirectly) to a deposition module that is particularly suited for delivering gas-phase reactants for use in one or more gas-phase reaction chambers. The gas-phase reactants may be used for chemical vapor deposition (CVD) or atomic layer deposition (ALD). In some embodiments, a control processor and programming stored on a computer-readable medium are included, and the systems and methods of the embodiments disclosed herein are configured to perform ALD. In certain embodiments, a control processor and programming stored on a computer-readable medium are included, and the embodiments disclosed herein are configured to perform CVD.

[0039] 4-5 illustrate an example of a filling chamber system 300 including a filling vessel 200 therein. FIG. 4 illustrates a side view of the example filling chamber system 300. The filling chamber system 300 may include a filling chamber housing 310. The filling vessel 200 may be disposed within the filling chamber housing 310. The filling chamber housing 310 may be configured to reduce thermal communication with any elements outside the filling chamber system 300. The filling chamber housing 310 may be substantially hollow and may have the exterior shape of a rectangular prism or cylinder. The filling chamber system 300 may include a heating element 320 and / or a cooling element 330. The heating element 320 may be disposed distal to the filling vessel 200. The heating element 320 may have one or more heating element functions described herein. The cooling element 330 may be disposed proximal to the filling vessel 200. In some embodiments, the cooling element 330 is water-cooled. The cooling element 330 may be disposed adjacent to (eg, in contact with) the base 212 .

[0040] FIG. 5 shows a cross-sectional perspective view of the fill chamber system 300 shown in FIG. 4 . The heating element 320 can include a partial loop, but can also be a filament. The cooling element 330 can also be a cooling plate. The fill chamber system 300 can include additional elements, such as valves, inlets, outlets, heating elements, cooling elements, support structures, and / or other elements. For example, in some embodiments, the fill vessel 200 can be associated with one or more controllers (not shown), which can be configured to direct a system (such as a reactor system) to perform ALD, as described in more detail herein. In some embodiments, the one or more controllers include a processor and memory programmed to direct a system (such as a reactor system) to perform ALD. The one or more controllers can be configured to control all heaters in the deposition module, pumps, valves to the pumps for pressure control, robotic controls for substrate processing, and / or valves controlling vapor flow, including carrier flow to and from the fill vessel 200.

[0041] In some embodiments, the filling vessel 200 may include one or more heating elements. In some embodiments, one or more of the heating elements may be positioned vertically adjacent to or vertically proximate to the filling vessel 200. In some embodiments, the one or more heating elements are configured to heat the sublimator 100 via conduction. In certain embodiments, a heater plate may be positioned laterally of the lid 220. In certain embodiments, a heater may be positioned distal to the housing 110. In some embodiments, one or more valves may be conductively and / or radiatively heated. The filling vessel 200 may be placed in a cabinet (e.g., the filling chamber housing 310) configured to be airtight so that it can be evacuated to a low pressure, e.g., 0.1 Torr to 20 Torr, e.g., about 5 Torr, thus promoting efficient radiative heating that minimizes conductive or convective losses to the atmosphere within the cabinet. In some configurations, the filling vessel 200 may be placed within a higher pressure, such as 100 Torr, 200 Torr, 300 Torr, 500 Torr, or atmospheric pressure. Other pressures are possible. In some embodiments, a solid source assembly (as disclosed herein) can be operated at a target vacuum pressure. In some embodiments, the target vacuum pressure can be in the range of about 0.5 Torr to 20 Torr, for example, 5 Torr. In certain embodiments, the vacuum pressure within the solid source assembly can be regulated using one or more pressure controllers.

[0042] FIG. 6 shows an example of a solid source chemistry system 400 including a filling vessel 100, a chemical source vessel 450, and a carrier gas source 440. The chemical source vessel 450 can be connected to the filling vessel 100 via a chemical delivery line 404. The chemical source vessel 450 can comprise a larger chemical source vessel, such as a bulk filling vessel. The chemical source vessel (e.g., a bulk filling vessel) can be a vessel similar to the filling vessel 100, but the source vessel can have a larger chemical volume within its housing 402, e.g., at least 1.5, 2, 3, 4, 5, 10, or 20 times the volume of the filling vessel 100. The carrier gas source 440 can include a carrier gas source, such as those described herein. The chemical source vessel 450 can deliver chemicals therein to the filling vessel 100 via the chemical delivery line 404. The chemicals can be vaporized (e.g., sublimated, evaporated) before passing through the chemical delivery line 404.

[0043] Chemical outlet 132 can deliver vaporized chemical (e.g., along with a carrier gas) through reaction flow path 434 to a reaction (e.g., a reaction chamber). Filling vessel 100 can have additional or alternative features, for example, as disclosed in U.S. Patent Application Publication No. 2018 / 0094350, filed September 30, 2016, and entitled "REACTANT VAPORIZER AND RELATED SYSTEMS AND METHODS," which is incorporated herein by reference in its entirety for all purposes.

[0044] In some embodiments, the electronics and / or computer elements used in controlling one or more reaction chambers and / or one or more charge vessels (e.g., charge vessel 100, charge vessel 200) may be located elsewhere in the system. For example, a central controller may control the valves connecting the various vessels and any associated heaters, as well as the equipment in the one or more chambers themselves. One or more valves may be used to control the flow of gases throughout the solid source chemistry system 400. [Example]

[0045] Below are a series of non-limiting examples of the above-described embodiments.

[0046] In a first embodiment, a solid source chemical intermediate fill vessel comprises a proximal end, a distal end, and a base at the proximal end configured to hold a solid source chemical reactant therein, the base comprising a first thermal conductor and configured to be maintained at or below a first threshold temperature, and a lid at the distal end comprising a second thermal conductor and configured to be maintained at or above a second threshold temperature that is greater than the first threshold temperature, the lid comprising a chemical inlet configured to receive vaporized chemical reactant at the base, a carrier gas inlet configured to receive a flow of carrier gas therethrough, a chemical outlet configured to deliver vaporized chemical reactant from the lid, and an intermediate layer comprising an insulator configured to reduce heat flow between the base and the lid.

[0047] In a second embodiment, the intermediate layer is an intermediate filled container as described in embodiment 1, comprising one or more chambers each containing a vacuum.

[0048] In a third embodiment, the intermediate filled container according to any one of the first and second embodiments is provided, wherein the intermediate layer is disposed in contact with both the base and the lid.

[0049] In a fourth embodiment, the intermediate filling vessel of any of the first to third embodiments further comprises a cooling element configured to maintain the base at or below the first threshold temperature.

[0050] In a fifth embodiment, the intermediate filled vessel of embodiment 4 is configured such that the cooling element comprises a water cooling element thermally coupled to the base.

[0051] A sixth embodiment is an intermediate-filled container according to any one of embodiments 1 to 5, wherein the first threshold temperature is about 135°C.

[0052] A seventh embodiment is an intermediate-filled container according to any one of embodiments 1 to 6, wherein the second threshold temperature is about 145°C.

[0053] In an eighth embodiment, the intermediate filled container of any of embodiments 1-7 further comprises a heating element configured to maintain the lid at or above the first threshold temperature.

[0054] In a ninth embodiment, the intermediate filled container of any of embodiments 1-8, wherein the cooling element comprises a water cooling element thermally coupled to the base.

[0055] In a tenth embodiment, the intermediate filled container of embodiment 9 is provided, wherein the heating element comprises a rod or plate configured to heat the lid via radiation.

[0056] In an eleventh embodiment, the intermediate filling vessel of any of embodiments 1-10, wherein the chemical inlet, carrier gas inlet, and chemical outlet each include a corresponding valve configured to control gas flow therethrough.

[0057] In a twelfth embodiment, the intermediate filling vessel of any of embodiments 1-11, wherein the chemical outlet comprises a filter configured to prevent the passage of particulate matter therethrough.

[0058] In a thirteenth embodiment, the intermediate filled vessel of example 12, wherein the porosity of the filter is configured to prevent passage therethrough of reactants below the second threshold temperature and to allow passage therethrough of reactants above the second threshold temperature.

[0059] In a fourteenth embodiment, the intermediate-filled container according to any one of embodiments 12 to 13 is configured such that the filter comprises at least one of ceramic and metal.

[0060] A fifteenth embodiment is an intermediate filled container according to any one of embodiments 1 to 14, wherein the ratio of the height of the base to the height of the lid is greater than about four.

[0061] In a sixteenth embodiment, the intermediate filled container of any of embodiments 1 to 15 is configured such that the intermediate layer maintains a temperature gradient between the lid and the base of at least 10°C.

[0062] A seventeenth embodiment is an intermediate-filled container according to any one of embodiments 1 to 16, wherein the ratio of the height of the lid to the height of the intermediate layer is greater than about 2.

[0063] In an eighteenth embodiment, the intermediate filled container according to any one of the first to seventeenth embodiments has a cross section of the base that includes at least two flat edges.

[0064] A nineteenth embodiment is the intermediate-filled container of any one of embodiments 1 to 18, wherein the intermediate layer comprises ceramic or metal.

[0065] In a twentieth embodiment, the intermediate filling vessel is the intermediate filling vessel of any of embodiments 1-19, wherein the intermediate filling vessel is sized for in-situ placement in a solid feedstock chemical reaction chamber.

[0066] In a 21st embodiment, the intermediate-filled container is the intermediate-filled container according to any one of embodiments 1 to 19, wherein the intermediate-filled container in an unfilled state has a mass of about 10 kg to 50 kg.

[0067] In a 22nd embodiment, a solid source chemical system includes an intermediate solid source chemical vessel of any of embodiments 1-21; and a solid source chemical sublimator in fluid communication with the intermediate vessel, wherein the solid source chemical sublimator includes a housing having an interior space and an interior surface facing the interior space; and a filter having a first end and a second end, the filter having porosity configured to restrict passage of a solid chemical reactant therethrough, the filter being shaped and positioned to define a flow path surrounding the filter in a space between the filter and the interior surface.

[0068] In a 23rd embodiment, a method for providing a vaporized chemical reactant to a reaction chamber includes continuously flowing the vaporized chemical reactant into a chemical inlet of an intermediate filling vessel described in any of embodiments 1 to 21, wherein the lid is maintained at a higher temperature than the base, whereby the vaporized chemical reactant condenses at the base; sublimating the condensed chemical reactant at the base; and flowing the sublimated chemical reactant through the outlet into the reaction chamber.

[0069] Other Considerations In the foregoing specification, the invention has been described with reference to specific embodiments thereof. It will, however, be apparent that various modifications and changes can be made thereto without departing from the broader spirit and scope of the invention. The specification and drawings are, therefore, to be regarded in an illustrative rather than a restrictive sense.

[0070] Indeed, it will be understood that the systems and methods of the present disclosure each have several innovative aspects, no single aspect of which is solely responsible for or required for the desirable attributes disclosed herein. The various features and processes described herein can be used independently of one another or can be combined in various ways. All possible combinations and subcombinations are intended to be within the scope of the present disclosure.

[0071] Certain features described herein in the context of separate embodiments may also be implemented in combination in a single embodiment. Conversely, various features described in the context of a single embodiment may also be implemented in multiple embodiments separately or in any suitable subcombination. Furthermore, while features may be described herein as functioning in a particular combination and initially claimed as such, one or more features from the claimed combination may optionally be deleted from the combination, and the claimed combination may be directed to a subcombination or a variation of the subcombination. No single feature or group of features is necessary or essential to every embodiment.

[0072] It will be understood that conditional language used herein, such as, among others, "can," "could," "might," "may," "for example," and the like, is generally intended to convey that certain embodiments include certain features, elements, and / or steps, while other embodiments do not, unless otherwise indicated or understood within the context of use. Thus, such conditional language is generally not intended to suggest that features, elements, and / or steps are somehow required in one or more embodiments, or that one or more embodiments necessarily include logic for determining whether those features, elements, and / or steps are included in or performed in any particular embodiment, with or without authorial input or direction. The terms "comprise," "include," "have," and the like are synonymous and are used in an inclusive, open-ended manner and do not exclude additional elements, features, steps, operations, etc. Additionally, the term "or" is used in an inclusive sense (and not an exclusive sense), so that, for example, when used to connect a list of elements, the term "or" may refer to one, some, or all of the elements in the list. Furthermore, the articles "a," "an," and "the," as used in this application and the appended claims, should be construed to mean "one or more" or "at least one," unless otherwise specified. Similarly, while operations may be depicted in the figures in a particular order, it should be recognized that such operations need not be performed in the particular order or sequential order shown, or that all illustrated operations be performed to achieve a desired result. Furthermore, the figures may generally depict another exemplary process in the form of a flowchart. However, other operations not shown may be incorporated into the generally illustrated exemplary methods and processes. For example, one or more additional operations may be performed before, after, simultaneously with, or between any of the illustrated operations. Furthermore, operations may be rearranged or reordered in alternative embodiments. Multitasking and parallel processing may be advantageous in certain situations.Furthermore, the separation of various system components in the embodiments described herein should not be understood as requiring such separation in all embodiments, and it will be understood that the described components and systems may generally be integrated together in a single product or packaged into multiple products (e.g., a filter insert with a housing and a base and an ingredient container). Furthermore, other embodiments are within the scope of the following claims. In some cases, the steps recited in the claims may be performed in a different order to achieve still more desirable results.

[0073] Thus, the scope of the claims is not intended to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with this disclosure and the principles and features disclosed herein. For example, while many examples within this disclosure are provided with respect to providing vapor from a solid source for delivery to a deposition chamber for semiconductor manufacturing, the specific embodiments described herein can be implemented in a wide variety of other applications and / or in numerous other contexts.

Claims

1. 1. A solid source chemical intermediate filling vessel comprising: a proximal end; a distal end; and a base at the proximal end configured to hold a solid source chemical reactant therein, the base comprising a first thermal conductor and configured to be maintained at or below a first threshold temperature; a lid at the distal end comprising a second thermal conductor and configured to be maintained at or above a second threshold temperature greater than the first threshold temperature; a chemical inlet configured to receive a vaporized chemical reactant within the base; a carrier gas inlet configured to receive a carrier gas flow therethrough; a lid including a chemical outlet configured to pass vaporized chemical reactant through the lid; an intermediate layer disposed between the base and the lid, the intermediate layer comprising an insulator configured to reduce heat flow between the base and the lid.

2. 10. The intermediate filled vessel of claim 1, wherein the intermediate layer comprises one or more chambers each containing a vacuum.

3. The intermediate filled container of claim 1 , wherein the intermediate layer is positioned in contact with both the base and the lid.

4. The intermediate filling vessel of claim 1 , further comprising a cooling element configured to maintain the base at or below the first threshold temperature.

5. The intermediate fill vessel of claim 4 , wherein the cooling element comprises a water cooling element thermally coupled to the base.

6. 10. The intermediate filled vessel of claim 1, wherein the first threshold temperature is about 135°C.

7. 10. The intermediate filled vessel of claim 1, wherein the second threshold temperature is about 145°C.

8. The intermediate filling vessel of claim 1 , further comprising a heating element configured to maintain the lid at or above the first threshold temperature.

9. The intermediate filled vessel of claim 1 , wherein the cooling element comprises a water cooling element thermally coupled to the base.

10. 10. The intermediate filled vessel of claim 9, wherein the heating element comprises a rod or plate configured to heat the lid via radiation.

11. 10. The intermediate filling vessel of claim 1, wherein the chemical inlet, the carrier gas inlet, and the chemical outlet each include a corresponding valve configured to control gas flow therethrough.

12. 10. The intermediate filling vessel of claim 1, wherein the chemical outlet comprises a filter configured to prevent the passage of particulate matter therethrough.

13. 13. The intermediate filling vessel of claim 12, wherein the porosity of the filter is configured to prevent passage therethrough of the reactants below the second threshold temperature and to allow passage therethrough of the reactants at or above the second threshold temperature.

14. 10. The intermediate filling vessel of claim 1, wherein the filter comprises at least one of a ceramic or a metal.

15. 10. The intermediate filled container of claim 1, wherein the ratio of the height of the base to the height of the lid is greater than about 4.

16. 10. The intermediate filled container of claim 1, wherein the intermediate layer is configured to maintain a temperature gradient between the lid and the base of at least 10 degrees Celsius.

17. 10. The intermediate filled container of claim 1, wherein the ratio of the height of the lid to the height of the intermediate layer is greater than about 2.

18. 10. The intermediate filled container of claim 1, wherein the cross section of the base comprises at least two flat edges.

19. The intermediate filled vessel of claim 1 , wherein the intermediate layer comprises a ceramic or a metal.

20. 10. The intermediate filling vessel of claim 1, wherein the intermediate filling vessel is sized for in-situ placement in a solid feedstock chemical reaction chamber.

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