Ampoule containing solid precursor for atomic layer deposition processes

Abstract

An ampoule of a substrate processing system includes an enclosure for containing a solid precursor and a control valve arrangement including a plurality of control valves, including at least an outlet valve disposed between the enclosure and a substrate processing chamber. The substrate processing system is configured to cause at least a portion of the solid precursor to sublimate, and to deliver resulting gaseous precursor chemicals, through at least the outlet valve, to the substrate processing chamber. Each of the plurality of control valves has a cyclic lifetime of at least thirty million cycles.

Description

AMPOULE CONTAINING SOLID PRECURSOR FOR ATOMIC LAYER DEPOSITION PROCESSESINCORPORATION BY REFERENCE

[0001] A PCT Request Form is filed concurrently with this specification as part of the present application. Each application that the present application claim benefit of or priority to as identified in the concurrently filed PCT Request Form is incorporated by reference herein in its entirety and for all purposes.BACKGROUND

[0002] Semiconductor manufacturing typically involves one or more processes to deposit and pattern a structure on a wafer. For example, in some semiconductor manufacturing processes a film is created on a semiconductor wafer by flowing a vaporized precursor onto the wafer and then activating a reaction on the substrate surface. In one such process, atomic layer deposition (“ALD”), one or more vaporized precursors are flowed from an ampoule onto a semiconductor wafer as part of one or more “dose” steps during an ALD cycle. The precursor material may be containerized as a solid in an ampoule that is configured to deliver to the wafer, as needed, vapor sublimated from the solid. A control valve arrangement may be provided to cyclically deliver desired quantities of the vapor.

[0003] The background description provided herein is for the purposes of generally presenting the context of the disclosure. Work of the presently named inventors, to the extent it is described in this background section, as well as aspects of the description that may not otherwise qualify as prior art at the time of filing, are neither expressly nor impliedly admitted as prior art against the present disclosure.SUMMARY

[0004] Techniques, in a substrate processing system, for controlling delivery of precursor chemicals from an ampoule enclosing a solid precursor, where the ampoule is fluidically coupled with a processing chamber through a control valve arrangement and the substrate processing system is configured to cause at least a portion of the solid precursor to sublimate, and to deliver resulting gaseous precursor chemicals, through the control valve arrangement, to the processing chamber are disclosed.

[0005] According to some embodiments, an apparatus includes an ampoule of a substrate processing system, the ampoule including an enclosure for containing a solid precursor and acontrol valve arrangement including a plurality of control valves, the plurality of control valves including at least an outlet valve disposed between the enclosure and a substrate processing chamber. The substrate processing system is configured to cause at least a portion of the solid precursor to sublimate, and to deliver resulting gaseous precursor chemicals, through at least the outlet valve, to the substrate processing chamber and each of the plurality of control valves has a cyclic lifetime of at least thirty million cycles.

[0006] In some examples, at least one of the plurality of control valves may have a cyclic lifetime of at least forty million cycles.

[0007] In some examples, each of the control valves may have an actuation response time no greater than 40 milliseconds. In some examples, at least one of the plurality of control valves may have an actuation response time no greater than 20 milliseconds.

[0008] In some examples, each of the control valves may have an actuation response time uncertainty of + / - 5 milliseconds or less. In some examples, at least one of the plurality of control valves may have an actuation response time uncertainty of + / - 3 milliseconds or less.

[0009] In some examples, the outlet valve may be configured to control flow of the resulting gaseous precursor chemicals from the enclosure to the processing chamber. In some examples, the plurality of control valves may include an inlet valve for controlling flow of a carrier gas into the enclosure. In some examples, the plurality of control valves may include a bypass valve for controlling flow of the carrier gas to the processing chamber, an upstream side of the bypass valve being fluidically coupled with an upstream side of the inlet valve and a downstream side of the bypass valve being fluidically coupled to a downstream side of the outlet valve. In some examples, each of the plurality of control valves may be coupled with a common manifold block, the manifold block providing a fluidic coupling of (a) the upstream side of the inlet valve with the upstream side of the bypass valve and (b) the downstream side of the outlet valve with the downstream side of the bypass valve. In some examples, the manifold block is configured to provide a fluidic coupling of: (c) a supply of the carrier gas with the upstream side of the inlet valve; (d) a downstream side of the inlet valve and an inlet port of the enclosure; (e) an outlet port of the enclosure and an upstream side of the outlet valve; and (f) the downstream side of the outlet valve with the substrate processing chamber. In some examples, the manifold block may be configured to provide a surface mount interface for each of the plurality of control valves. In some examples, the surface mount interface includes a C-ring seal.

[0010] According to some implementations, a substrate processing system includes a substrate processing chamber, a source of a carrier gas, and two or more ampoules, configured to be installed in the system, fluidically coupled with and disposed between the substrate processingchamber and the source of the carrier gas. Each ampoule includes an enclosure for containing a solid precursor and a control valve arrangement including a plurality of control valves, the plurality of control valves including at least an outlet valve disposed between the enclosure and the substrate processing chamber and an inlet valve disposed between the enclosure and the source of the carrier gas. The substrate processing system is configured to cause at least a portion of the solid precursor to sublimate, and to cause the carrier gas to deliver resulting gaseous precursor chemicals, through at least the outlet valve, to the substrate processing chamber. Each of the plurality of control valves has a cyclic lifetime of at least thirty million cycles and each of the two or more ampoules has a respective enclosure of a different size and provides a substantially identical coupling interface with the system, and is configured to be interchanged without altering other aspects of the substrate processing system.

[0011] In some examples, at least one of the plurality of control valves may have a cyclic lifetime of at least forty million cycles.

[0012] In some examples, each of the control valves may have an actuation response time no greater than 40 milliseconds. In some examples, at least one of the plurality of control valves may have an actuation response time no greater than 20 milliseconds.

[0013] In some examples, each of the control valves may have an actuation response time uncertainty of + / - 5 milliseconds or less. In some examples, at least one of the plurality of control valves may have an actuation response time uncertainty of + / - 3 milliseconds or less.

[0014] In some examples, the outlet valve may be configured to control flow of the resulting gaseous precursor chemicals from the enclosure to the processing chamber. In some examples, the plurality of control valves may include an inlet valve for controlling flow of a carrier gas into the enclosure. In some examples, the plurality of control valves may include a bypass valve for controlling flow of the carrier gas to the processing chamber, an upstream side of the bypass valve being fluidically coupled with an upstream side of the inlet valve and a downstream side of the bypass valve being fluidically coupled to a downstream side of the outlet valve. In some examples, each of the plurality of control valves may be coupled with a common manifold block, the manifold block providing a fluidic coupling of (a) the upstream side of the inlet valve with the upstream side of the bypass valve and (b) the downstream side of the outlet valve with the downstream side of the bypass valve. In some examples, the manifold block may be configured to provide a fluidic coupling of: (c) a supply of the carrier gas with the upstream side of the inlet valve; (d) a downstream side of the inlet valve and an inlet port of the enclosure; (e) an outlet port of the enclosure and an upstream side of the outlet valve; and (f) the downstream side of the outlet valve with the substrate processing chamber. In some examples,the manifold block may be configured to provide a surface mount interface for each of the plurality of control valves. In some examples, the surface mount interface may include a C- ring seal.

[0015] According to some implementations, a substrate processing system includes a substrate processing chamber, a source of a carrier gas and two or more ampoules, configured to be installed in the system, fluidically coupled with and disposed between the substrate processing chamber and the source of the carrier gas. Each ampoule includes an enclosure for containing a solid precursor; and a control valve arrangement including a plurality of control valves, the plurality of control valves including at least an outlet valve disposed between the enclosure and the substrate processing chamber and an inlet valve disposed between the enclosure and the source of the carrier gas. The substrate processing system is configured to cause at least a portion of the solid precursor to sublimate, and to cause the carrier gas to deliver resulting gaseous precursor chemicals, through at least the outlet valve, to the substrate processing chamber, each of the plurality of control valves has a cyclic lifetime of at least thirty million cycles; and at least one of the two or more ampoules includes control valves fabricated from stainless steel and at least one of the two or ampoules includes control valves fabricated from a UNS N06022 alloy and each of the ampoules is configured to be interchanged without altering other aspects of the substrate processing system.

[0016] According to some implementations, a substrate processing system includes a substrate processing chamber, a source of a carrier gas, a controller, and an ampoule, configured to be installed in the system, fluidically coupled with and disposed between the substrate processing chamber and the source of the carrier gas. Each ampoule includes an enclosure for containing a solid precursor and a control valve arrangement including a plurality of control valves, plurality of control valves including at least an outlet valve disposed between the enclosure and the substrate processing chamber and an inlet valve disposed between the enclosure and the source of the carrier gas. The substrate processing system is configured to cause at least a portion of the solid precursor to sublimate, and to cause the carrier gas to deliver resulting gaseous precursor chemicals, through at least the outlet valve, to the substrate processing chamber. Each of the plurality of control valves includes a respective piston for opening and closing the valve and a respective proximity sensor communicatively coupled with the controller and configured to output to the controller a position of the respective piston. The controller is configured to control a timing sequence of opening and closing the control valves, determine, from the output of each respective sensor, an actuation time of the respective control valve; and adjust the timing sequence based on the determined actuation time.

[0017] According to some implementations, a method of operating a substrate processing system including a substrate processing chamber, a source of a carrier gas, a controller, and an ampoule, including a control valve arrangement, fluidically coupled with and disposed between the substrate processing chamber and the source of the carrier gas, the method including: controlling, with the controller, a timing sequence of opening and closing control valves within the control valve arrangement; receiving an output of a respective proximity sensor of each control valve, the output being representative of a respective valve piston position; determining, from the output of each respective sensor, an actuation time of the respective control valve; and, adjusting the timing sequence based on the determined actuation time.

[0018] These and other features of the disclosed embodiments will be described in detail below with reference to the associated drawings.BRIEF DESCRIPTION OF DRAWINGS

[0019] Figure 1 Figure 1 depicts a schematic representation of an example precursor delivery system, according to some implementations.

[0020] Figure 2 shows features of an ampoule, including an enclosure and a control valve arrangement.

[0021] Figure 3 illustrates an implementation in which a control valve arrangement is arranged as a valve cluster.

[0022] Figure 4 shows an example of a valve according to some implementations.

[0023] Figure 5 shows a further example of a control valve arrangement.

[0024] Figure 6 shows a further example of an ampoule including a control valve arrangement and an enclosure.

[0025] Figure ? shows a further example of an ampoule including a control valve arrangement and a relatively large enclosure.

[0026] Figure 8 shows a further example of an ampoule including a control valve arrangement and a relatively small enclosure.

[0027] Figure 9 shows a process flow diagram, according to some implementations.DETAILED DESCRIPTION

[0028] In the following description, numerous specific details are set forth to provide a thorough understanding of the presented embodiments. The disclosed embodiments may be practiced without some or all of these specific details. In other instances, well-known process operations have not been described in detail to not unnecessarily obscure the disclosedembodiments. While the disclosed embodiments will be described in conjunction with the specific embodiments, it will be understood that it is not intended to limit the disclosed embodiments.

[0029] The subscripts “x” and “y” are used throughout the disclosure to denote a number greater than zero that forms a stable compound. However, it should be noted that the lack of an “x” or other subscript (e.g., in titanium nitride (TiN) or titanium oxynitride (TiON)) does not imply a particular atomic ratio.

[0030] Described herein are techniques controlling delivery of a gas including gaseous sublimated precursor chemicals to a processing chamber from an ampoule storing a solid precursor. The techniques may find particular utility for semiconductor fabrication processes which use an atomic layer deposition (“ALD”) technique for film deposition. Some implementations of depositing a thin film on a semiconductor wafer may involve a cyclical process that may include two half reactions on the wafer surface. The first half reaction may include adsorption of one or more precursors on the surface of the wafer and the second half reaction may include the conversion of the adsorbed precursor(s) into a film or layer.

[0031] ALD is a film forming technique which is well-suited to the deposition of conformal films due to the fact that a single cycle of ALD only deposits a single thin layer of material, the thickness being limited by the amount of one or more film precursor reactants which may adsorb onto the substrate surface (i.e., forming an adsorption-limited layer) prior to the filmforming chemical reaction itself. Multiple “ALD cycles” may then be used to build up a film of the desired thickness, and since each layer is thin and conformal, the resulting film substantially conforms to the shape of the underlying device structure. In certain implementations, each ALD cycle includes the following steps (1) exposure of the substrate surface to a first precursor, (2) purge of the reaction chamber in which the substrate is located, (3), activation of a reaction of the substrate surface, typically with a plasma and / or a second precursor, and (4) purge of the reaction chamber in which the substrate is located. The first step listed herein may be referred to as a “dose step,” the second step may be referred to as a “purge step,” the third step may be referred to as an “RF step”, and the fourth step may be referred to as an “RF purge step.”

[0032] Some implementations of semiconductor processing that use a precursor may include hardware, and may implement methods, to deliver the precursor to the processing chamber. In certain implementations of semiconductor processing, a solid precursor contained in an ampoule may be sublimated (vaporized) before being transported to and / or deposited on a semiconductor wafer. A carrier gas, which may be an inert gas (such as argon), a non-inert gas(such as oxygen), or a non-inert gas mixture (such as oxygen and argon), may flow through the ampoule to carry sublimated precursor chemicals to a semiconductor processing chamber. Carrier gas may be either “pushed” (where gas is forced through the lines) or “pulled” (where gas is pulled through the lines, possibly via a vacuum) through the ampoule to carry the evaporated precursor. Throughout this disclosure, the term “precursor” may be used to describe precursor in both solid and vapor states.

[0033] Figure 1 depicts a schematic representation of an example precursor delivery system. In the illustrated example, a precursor delivery system 100 includes a flow controller 102, an ampoule 1000, and a processing chamber 128 that are connected to a series of pipes and valves and through which fluid, e.g. liquid and / or gas, may flow, generally in the direction shown in Figure 1 by arrows. Accordingly, for example, the flow controller 102 may be considered upstream from the ampoule 1000 which in turn is upstream from the process chamber 128. In Figure 1 and subsequent drawings, a gas line and / or pipe of the example precursor delivery system 100 is depicted as a line while a valve is depicted as a “bowtie” (i.e., two opposing triangles). A closed valve will be shaded, whereas an open valve will be unshaded. Thus, for example all the valves in Figure 1 are shown as open.

[0034] The flow controller 102 is connected downstream from valve 106 and upstream from the rest of the system. A carrier (or “push”) gas, or other fluid, may flow into the system through valve 106 and then through flow controller 102. In some implementations, the flow controller 102 controls the flow of the push gas or other fluid. Flow controller 102 is upstream from valve 108, which is upstream from the ampoule 1000. As illustrated, the ampoule 1000 includes an enclosure 1100, in which solid precursor is contained, and a control valve arrangement 1200, described in more detail hereinbelow.

[0035] The carrier gas, together with sublimated precursor chemicals exits the ampoule 1000 via flow path 118 to a semiconductor processing chamber 128. It will be appreciated that there may be other components disposed between the ampoule 1000 and the process chamber (e.g., additional control valves, a mixing assembly, and / or other apparatus that have been omitted for clarity of illustration). In the illustrated example, a controller 160 is communicatively coupled with the ampoule 1000 and may be configured to send actuation commands (e.g., valve open / valve close) to the control valve arrangement 1200 and / or to receive data therefrom (e.g., temperature, valve piston position or other data).

[0036] The controller 160 will typically include one or more memory devices and one or more processors. A processor may include a CPU or computer, analog and / or digital input / output connections, stepper motor controller boards, etc.

[0037] There may be a user interface associated with the controller 160. The user interface may include a display screen, graphical software displays of the apparatus and / or process conditions, and user input devices such as pointing devices, keyboards, touch screens, microphones, etc.

[0038] System control logic may be configured in any suitable way. In general, the logic can be designed or configured in hardware and / or software. The instructions for controlling the drive circuitry may be hard coded or provided as software. The instructions may be provided by “programming.” Such programming is understood to include logic of any form, including hard coded logic in digital signal processors, application-specific integrated circuits, and other devices which have specific algorithms implemented as hardware. Programming is also understood to include software or firmware instructions that may be executed on a general- purpose processor. System control software may be coded in any suitable computer readable programming language.

[0039] The computer program code may be written in any conventional computer readable programming language: for example, assembly language, C, C++, Pascal, Fortran, or others. Compiled object code or script is executed by the processor to perform the tasks identified in the program. Also as indicated, the program code may be hard coded.

[0040] Signals for monitoring the process may be provided by analog and / or digital input connections of the controller 160.

[0041] Broadly speaking, the controller 160 may be defined as electronics having various integrated circuits, logic, memory, and / or software that receive instructions, issue instructions, and control operations. The integrated circuits may include chips in the form of firmware that store program instructions, digital signal processors (DSPs), chips defined as application specific integrated circuits (ASICs), and / or one or more microprocessors, or microcontrollers that execute program instructions (e.g., software). Program instructions may be instructions communicated to the controller in the form of various individual settings (or program files), defining operational parameters for carrying out a particular process on or for a semiconductor wafer or to a system.

[0042] The controller 160, in some implementations, may be a part of or coupled to a computer that is integrated with, coupled to the system, otherwise networked to the system, or a combination thereof. For example, the controller 160 may be in the “cloud” or all or a part of a fabrication host computer system, which can allow for remote access of the wafer processing. The computer may enable remote access to the system to monitor current progress of fabrication operations, examine a history of past fabrication operations, examine trends orperformance metrics from a plurality of fabrication operations, to change parameters of current processing, to set processing steps to follow a current processing, or to start a new process. In some examples, a remote computer (e.g. a server) can provide process recipes to a system over a network, which may include a local network or the Internet. The remote computer may include a user interface that enables entry or programming of parameters and / or settings, which are then communicated to the system from the remote computer. In some examples, the controller receives instructions in the form of data, which specify parameters for each of the processing steps to be performed during one or more operations. The parameters may be specific to the type of process to be performed and the type of tool that the controller is configured to interface with or control. Thus, as described above, the controller may be distributed, such as by including one or more discrete controllers that are networked together and working towards a common purpose, such as the processes and controls described herein. An example of a distributed controller for such purposes would be one or more integrated circuits on a chamber in communication with one or more integrated circuits located remotely (such as at the platform level or as part of a remote computer) that combine to control a process on the chamber.

[0001] Figure 2 shows features of the ampoule 1000, including the enclosure 1100 and the control valve arrangement 1200. In the illustrated example, the enclosure 1100 is configured to store a supply of solid precursor 1104. A solid precursor may be desirable for certain applications. For example, conductive lines in semiconductor memory devices increasingly use molybdenum (Mo) and precursors for molybdenum deposition may preferably be containerized within the ampoule 102 in a solid state. Examples include molybdenum chloride (MoClx), molybdenum oxychloride (MoOyXz), and certain molybdenum organometallic compounds. Molybdenum chloride precursors are given by the formula MoClx, where x is 2, 3, 4, 5, or 6, and include molybdenum dichloride (M0CI2), molybdenum trichloride (M0CI3), molybdenum tetrachloride (M0CI4), molybdenum pentachloride (M0CI5), and molybdenum hexachloride (MoCle). In some embodiments, M0CI5 or Mode are used. In addition to MoClxprecursors, in other embodiments, other molybdenum halide precursors may be used. Molybdenum halide precursors are given by the formula MoXz, where X is a halogen (fluorine (F), chlorine (Cl), bromine (Br), or iodine (I)) and z is 2, 3, 4, 5, or 6. In some embodiments, a non-fluorine- containing MoXzprecursor is used to prevent fluorine etch or incorporation. In some embodiments, a non-bromine-containing and / or a non-iodine-containing MoXzprecursor is used to prevent etch or bromine or iodine incorporation.

[0002] Molybdenum oxyhalide precursors are given by the formula MoOyXz, where X is ahalogen (fluorine (F), chlorine (Cl), bromine (Br), or iodine (I)), and y and z are numbers greater than 0 such that MoOyXzforms a stable compound. Examples of molybdenum oxyhalides include molybdenum dichloride dioxide (MOO2CI2), molybdenum tetrachloride oxide (MoOCU), molybdenum tetrafluoride oxide (M00F4), molybdenum dibromide dioxide (MoCEBn), and the molybdenum iodides MOO2I, and MO4O11I. It should be understood that as used herein the term molybdenum oxyhalide precursor may refer to a molybdenum oxyhalide precursor as described above or a molybdenum-containing oxyhalide precursor that includes molybdenum, oxygen, a halide and one or more other elements. In some embodiments, molybdenum oxyhalide or molybdenum-containing oxyhalides may include multiple different halogens (e.g., F and Cl and / or I and / or Br, etc.).

[0043] In some implementations, the ampoule enclosure 110 may have a volume of between about 0.5-15 liters. The ampoule 1000 may typically be pre-loaded with the solid precursor 1104, which is consumed over time, as a result of the solid precursor 1104 being sublimated and the resulting gaseous precursor chemicals in region 1103 being delivered, with the carrier gas, to the processing chamber 128.

[0044] In the illustrated example, control valve arrangement 1200 includes an inlet valve 1202, an outlet valve 1206, and a bypass valve 1204, so arranged as to control whether or not the gaseous precursor chemicals flow to the processing chamber. For example, when inlet valve 1202 and outlet valve 1206 are both open and bypass valve 1204 is closed, as shown in Detail A, gaseous precursor chemicals from region 1103 may be caused by the carrier gas to flow to the processing chamber. Contrariwise, as shown in Detail B, when inlet valve 1202 and outlet valve 1206 are both closed and bypass valve 1204 is open, only carrier gas flows to the processing chamber. In the absence of the presently disclosed techniques, the control valve arrangement for a solid precursor ampoule enclosure may conventionally use relatively inexpensive valves because, when the solid precursor is depleted (that may occur after normal operation for as little as 1-12 months), the ampoule may be discarded and replaced with a new pre-loaded ampoule enclosure and control valve arrangement.

[0045] At least for ALD processing, however, the inlet valve 1202, the outlet valve 1206, and the bypass valve 1204 (collectively, the “control valves”) may be expected to undergo a large number of open / close cycles during the life of the ampoule 1000. Indeed, the present disclosure contemplates that each valve should be configured to have a cyclic lifetime (e.g., a life expectation as demonstrated by tests of samples and / or analysis) of at least 30-50 million cycles. In some implementations, one or more of the control valves may be configured to have a cyclic lifetime of at least 40 million cycles. Moreover, at least some ALD processingprocedures require precise control of the timing and quantity of precursor chemical delivery. Advantageously, therefore, the control valves may be configured to have fast actuation times, and the actuation times are preferably highly repeatable. For example, each control valve may be configured to have an actuation response time (e.g., a duration required for transitioning from an open condition to a closed condition or a from closed condition to an open condition) of less than 40 milliseconds (msec) or, more preferably, less than 20 msec and / or an actuation response time uncertainty no greater than about + / - 5 msec, or, more preferably, less than + / - 3 msec.

[0046] In some implementations, as illustrated in Figure 3, a control valve arrangement may be arranged as a valve cluster. In the illustrated example, valve cluster 300 includes the inlet valve 1202, the bypass valve 1204 and the outlet valve 1206, flow paths 311, 313, 315 and 317, and couplings 301, 303, 305 and 307. A first coupling 301 may be configured to engage with and provide a fluidic path to a source of carrier gas (not illustrated), either directly or through a gas line or pipe (not illustrated). The carrier gas is distributed through first flow path 311 to respective upstream sides (entrances) of inlet valve 1202 and bypass valve 1204.

[0047] When inlet valve 1202 is open and bypass valve 1204 is closed, the carrier gas will exit a downstream side of inlet valve 1202 through second flow path 313 and reach second coupling 303. The second coupling 303 may be configured to engage with and provide a fluidic path to an inlet port of region 1103 of the ampoule enclosure 1100, either directly or through a gas line or pipe (not illustrated). The carrier gas entering region 1103 may cause gaseous precursor chemicals from region 1103 to exit the ampoule enclosure 1100 through an outlet port of region 1103. Third coupling 305 may be configured to engage with and provide a fluidic path from the outlet port, either directly or through a gas line or pipe (not illustrated), to third flow path 315. The carrier gas and gaseous precursor chemicals flow through (opened) outlet valve 1206 and through fourth flow path 317 to fourth coupling 307. The fourth coupling 307 may be configured to engage with and provide a fluidic path to a substrate processing chamber (not illustrated), either directly or through a gas line or pipe (not illustrated). As a result, the outlet valve 1206 is configured to control flow of gaseous precursor chemicals from the enclosure to the processing chamber.

[0048] When the bypass valve 1204 is open and the inlet valve 1202 and the outlet valve 1206 are closed, the carrier gas will simply flow to the substrate processing chamber, without entering region 1103, through the first coupling 301, the first flow path 311, the bypass valve 1204, the fourth flow path 317 and the fourth coupling 307.

[0049] Figure 4 shows an example of a valve 400 contemplated by the present disclosure. Asmay be observed, the valve 400 has a longitudinal axis 430 orthogonal to a mounting interface surface 441 of a base 440.

[0050] Figure 5 shows a further example of a control valve arrangement. In the illustrated example, depicted in elevation view (Detail C) and isometric view (Detail D) a control valve arrangement 500 is configured such that each of the plurality of control valves (i.e., each of inlet valve 502, bypass valve 504 and outlet valve 506) is coupled with a common manifold block 550. The manifold block 550 may provide a fluidic coupling of an upstream side of the inlet valve 502 with an upstream side of the bypass valve504 (i.e., a flow path corresponding to the first flow path 311 of Figure 3). The manifold block 550 may also provide a fluidic coupling of a downstream side of the outlet valve 506 with a downstream side of the bypass valve 504 (i.e., a flow path corresponding to the fourth flow path 317 of Figure 3).

[0051] In addition, in the illustrated example, the control valve arrangement 500 may be configured to provide a fluidic coupling, including first coupling 501, of a supply of the carrier gas with the upstream side of the inlet valve 502. Similarly, the control valve arrangement 500 may be configured to provide a fluidic coupling, including second coupling 503 of a downstream side of the inlet valve 502 and an inlet port of the enclosure; to provide a fluidic coupling, including third coupling 505 of an outlet port of the enclosure and an upstream side of the outlet valve 506; and to provide a fluidic coupling, including fourth coupling 507 of the downstream side of the outlet valve 506 with the substrate processing chamber.

[0052] It may be observed that a longitudinal axis 530 of, for example, outlet valve 506 is generally orthogonal to a longitudinal axis 535 of, for example, coupling 503. The manifold block 550 may in some instances be an integral block of, for example, metal and may be configured to have internal flow paths formed by machining processes. Alternatively, or in addition, flow paths may be formed, at least in part, by an additive manufacturing process. In some implementations, the manifold block 550 may be configured to provide a surface mount interface for one or more of the inlet valve 502, the bypass valve 504 and the outlet valve 506. The surface mount interface may include a metal C-ring seal (e.g., a circular sealing member having a C-shaped cross section configured to elastically deform and thereby provide a spring force against adjoining sealing surfaces), in some implementations.

[0053] Figure 6 shows a further example of an ampoule including a control valve arrangement and an enclosure. In the illustrated example an elevation view of an ampoule 6000 is shown, including control valve arrangement 500 and the enclosure 1100. It will be appreciated that, in the illustrated example, a mechanical and fluidic connection may be established between second coupling 503 and an inlet port 1163 of the enclosure 1100. Similarly a mechanical andfluidic connection may be established between third coupling 505 and an outlet port 1165 of the enclosure 1100.

[0054] As indicated hereinabove, the present disclosure contemplates control valve arrangements incorporating high performance valves such that each valve should be configured to have a cyclic lifetime of at least 30-50 million cycles and, in some implementations, an actuation response time of less than 50 msec and / or an actuation response time uncertainty no greater than about + / - 5 msec. At least the outlet valve must also be compatible with high temperature fluids, up to 200°C, for example. Suitable control valves are available from Fujikin of America in Fremont, California, for example.

[0055] In some implementations, valve components may be primarily stainless steel (e.g., SAE grade 316L stainless steel). However, for some use cases, the gaseous precursor chemicals are highly corrosive. For such use cases, valve components are preferably fabricated from an austenitic, nickel-chromium-molybdenum-tungsten alloy such as those having the universal designation UNS N06022, for example. INCONEL®, available from the Special Metals Corporation group of companies and HASTELLOY®, available from Haynes International Inc. are examples of suitable materials for these applications.

[0056] The ampoules contemplated by the present disclosure are intended for use in semiconductor processing systems that are complex multipurpose machines capable of being configured to perform a variety of processes. In some instances, a selected process or production cycle may require a “large” ampoule enclosure (on the order of 12-15 liters volume, for example), but in other processes a “small” ampoule enclosure (on the order of 0.5-3 liters volume, for example) may be preferred. Because the machines are expensive, operational downtime is to be minimized, and the ampoules are preferably configured to be interchangeable or amenable to being “swapped out” in an efficient manner.

[0057] Accordingly, in some implementations, each of two ampoules may have a respective enclosure of a different size, but may still provide a substantially identical coupling interface with the system, and may be configured to be interchanged without altering other aspects of the substrate processing system. Referring now to Figure 7 and Figure 8, for example, it may be observed that ampoule 7000 of Figure 7 includes a “large” enclosure, whereas ampoule 8000 of Figure 8 includes a “small” enclosure. Notwithstanding that difference, the coupling interface with the system for the two ampoules is substantially identical as a result, for example of dimensions di and d2 being identical. Similarly, in the illustrated example, dimensions hi and hi may be identical.

[0058] Alternatively, or in addition, a first ampoule may include control valves fabricated fromstainless steel and a second ampoule may include control valves fabricated from a UNS N06022 alloy and each of the ampoules may be configured to be interchanged without altering other aspects of the substrate processing system.

[0059] As indicated hereinabove, the control valves of the present disclosure, in some implementations, may be configured to have an actuation response time of less than 20-50 msec and an actuation response time uncertainty no greater than about + / - 5 msec. Although these values, representing the precision with which flow control may be effectuated, are considerably improved with respect to the prior art of valves used in solid precursor ampoules, a still further improvement in flow control precision may be desirable. For example, valve-to-valve variation in actuation time, and variation of actuation time with operating temperature, may result in greater than desired uncertainty as to when flow of the gaseous precursor will start and stop in response to corresponding open and close commands that may be issued by a controller.

[0060] Accordingly, in some implementations, where each control valve has a respective piston for opening and closing a respective control valve, each control valve may also include a respective proximity sensor communicatively coupled with a controller (e.g., controller 160 of Figure 1) and may be configured to output to the controller a position of the respective piston. The controller, then, may be configured to: (a) control a timing sequence of opening and closing the control valves; (b) determine, from the output of each respective sensor, an actuation time of the respective control valve; and (c) adjust the timing sequence based on the determined (actual) actuation time. As a result, even small variations in actuation timing from a desired timing may be further reduced.

[0061] Referring now to Fig. 9, a method 900 for operating a substrate processing system will be described. As indicated above, the substrate processing system may include a substrate processing chamber, a source of a carrier gas, a processor, and an ampoule, including a control valve arrangement, fluidically coupled with and disposed between the substrate processing chamber and the source of the carrier gas.

[0062] At block 970, in the illustrated example, a timing sequence of opening and closing control valves within the control valve arrangement is controlled.

[0063] At block 975, an output of a respective proximity sensor of each control valve is received, the output being representative of a respective valve piston position.

[0064] At block 980, from the output of each respective sensor, an actuation time of the respective control valve is determined.

[0065] At block 985, the timing sequence may be adjusted based on the determined actuation time.Conclusion

[0066] Although the foregoing embodiments have been described in some detail for purposes of clarity of understanding, it will be apparent that certain changes and modifications may be practiced within the scope of the appended claims. Embodiments disclosed herein may be practiced without some or all of these specific details. In other instances, well-known process operations have not been described in detail to not unnecessarily obscure the disclosed embodiments. Further, while the disclosed embodiments will be described in conjunction with specific embodiments, it will be understood that the specific embodiments are not intended to limit the disclosed embodiments. It should be noted that there are many alternative ways of implementing the processes, systems, and apparatus of the present embodiments. Accordingly, the present embodiments are to be considered as illustrative and not restrictive, and the embodiments are not to be limited to the details given herein.

Claims

CLAIMSWhat is claimed is:

1. An apparatus comprising: an ampoule of a substrate processing system, wherein the ampoule comprises: an enclosure for containing a solid precursor; and a control valve arrangement comprising a plurality of control valves, wherein the control valve arrangement comprises at least an outlet valve disposed between the enclosure and a substrate processing chamber, wherein: the substrate processing system is configured to cause at least a portion of the solid precursor to sublimate, and to deliver resulting gaseous precursor chemicals through the at least the outlet valve, to the substrate processing chamber; and each of the plurality of control valves has a cyclic lifetime of at least thirty million cycles.

2. The apparatus of claim 1, wherein at least one of the plurality of control valves has a cyclic lifetime of at least forty million cycles.

3. The apparatus of claim 1, wherein each of the control valves has an actuation response time no greater than 40 milliseconds.

4. The apparatus of claim 3, wherein at least one of the plurality of control valves has an actuation response time no greater than 20 milliseconds.

5. The apparatus of claim 1, wherein each of the control valves has an actuation response time uncertainty of + / - 5 milliseconds or less.

6. The apparatus of claim 5, wherein at least one of the plurality of control valves has an actuation response time uncertainty of + / - 3 milliseconds or less.

7. The apparatus of claim 1, wherein the outlet valve is configured to control flow of the resulting gaseous precursor chemicals from the enclosure to the processing chamber.

8. The apparatus of claim 7, wherein the plurality of control valves comprises an inlet valve for controlling flow of a carrier gas into the enclosure.

9. The apparatus of claim 8, wherein the plurality of control valves comprises a bypass valve for controlling flow of the carrier gas to the processing chamber, an upstream side of the bypass valve being fluidically coupled with an upstream side of the inlet valve and a downstream side of the bypass valve being fluidically coupled to a downstream side of the outlet valve.

10. The apparatus of claim 9, wherein each of the plurality of control valves is coupled with a common manifold block, the manifold block providing a fluidic coupling of (a) the upstream side of the inlet valve with the upstream side of the bypass valve and (b) the downstream side of the outlet valve with the downstream side of the bypass valve.

11. The apparatus of claim 10, wherein the manifold block is configured to provide a fluidic coupling of:(c) a supply of the carrier gas with the upstream side of the inlet valve;(d) a downstream side of the inlet valve and an inlet port of the enclosure;(e) an outlet port of the enclosure and an upstream side of the outlet valve; and(f) the downstream side of the outlet valve with the substrate processing chamber.

12. The apparatus of claim 10, wherein the manifold block is configured to provide a surface mount interface for each of the plurality of control valves.

13. A substrate processing system comprising: a substrate processing chamber; a source of a carrier gas; and two or more ampoules, configured to be installed in the system, fluidically coupled with and disposed between the substrate processing chamber and the source of the carrier gas, wherein each ampoule comprises: an enclosure for containing a solid precursor; and a control valve arrangement comprising a plurality of control valves, wherein the control valve arrangement comprises at least an outlet valve disposed between the enclosure and the substrate processing chamber and an inlet valve disposed between the enclosure andthe source of the carrier gas, wherein: the substrate processing system is configured to cause at least a portion of the solid precursor to sublimate, and to cause the carrier gas to deliver resulting gaseous precursor chemicals through the at least the outlet valve, to the substrate processing chamber; each of the plurality of control valves has a cyclic lifetime of at least thirty million cycles; and each of the two or more ampoules has a respective enclosure of a different size, and provides a substantially identical coupling interface with the system, and is configured to be interchanged without altering other aspects of the substrate processing system.

14. The substrate processing system of claim 13, wherein at least one of the plurality of control valves has a cyclic lifetime of at least forty million cycles.

15. The substrate processing system of claim 13, wherein each of the control valves has an actuation response time no greater than 40 milliseconds.

16. The substrate processing system of claim 15, wherein at least one of the plurality of control valves has an actuation response time no greater than 20 milliseconds.

17. The substrate processing system of claim 13, wherein each of the control valves has an actuation response time uncertainty of + / - 5 milliseconds or less.

18. The substrate processing system of claim 17, wherein at least one of the plurality of control valves has an actuation response time uncertainty of + / - 3 milliseconds or less.

19. The substrate processing system of claim 13, wherein the outlet valve is configured to control flow of the resulting gaseous precursor chemicals from the enclosure to the processing chamber.

20. The substrate processing system of claim 19, wherein the plurality of control valves comprises an inlet valve for controlling flow of a carrier gas into the enclosure.

21. The substrate processing system of claim 20, wherein the plurality of control valves comprises a bypass valve for controlling flow of the carrier gas to the processingchamber, an upstream side of the bypass valve being fluidically coupled with an upstream side of the inlet valve and a downstream side of the bypass valve being fluidically coupled to a downstream side of the outlet valve.

22. The substrate processing system of claim 21, wherein each of the plurality of control valves is coupled with a common manifold block, the manifold block providing a fluidic coupling of (a) the upstream side of the inlet valve with the upstream side of the bypass valve and (b) the downstream side of the outlet valve with the downstream side of the bypass valve.

23. The substrate processing system of claim 22, wherein the manifold block is configured to provide a fluidic coupling of:(c) a supply of the carrier gas with the upstream side of the inlet valve;(d) a downstream side of the inlet valve and an inlet port of the enclosure;(e) an outlet port of the enclosure and an upstream side of the outlet valve; and(f) the downstream side of the outlet valve with the substrate processing chamber.

24. The substrate processing system of claim 22, wherein the manifold block is configured to provide a surface mount interface for each of the plurality of control valves.

25. A substrate processing system comprising: a substrate processing chamber; a source of a carrier gas; and two or more ampoules, configured to be installed in the system, fluidically coupled with and disposed between the substrate processing chamber and the source of the carrier gas, wherein each ampoule comprises: an enclosure for containing a solid precursor; and a control valve arrangement including a plurality of control valves, including at least an outlet valve disposed between the enclosure and the substrate processing chamber and an inlet valve disposed between the enclosure and the source of the carrier gas, wherein: the substrate processing system is configured to cause at least a portion of the solid precursor to sublimate, and to cause the carrier gas to deliver resulting gaseous precursor chemicals through the at least the outlet valve, to the substrate processing chamber; each of the plurality of control valves has a cyclic lifetime of at least thirty millioncycles; and at least one of the two or more ampoules comprises control valves fabricated from stainless steel and at least one of the two or ampoules comprises control valves fabricated from a UNS N06022 alloy and each of the ampoules is configured to be interchanged without altering other aspects of the substrate processing system.

26. A substrate processing system comprising: a substrate processing chamber; a source of a carrier gas; a controller; and an ampoule, configured to be installed in the system, fluidically coupled with and disposed between the substrate processing chamber and the source of the carrier gas, wherein each ampoule comprises: an enclosure for containing a solid precursor; and a control valve arrangement including a plurality of control valves, including at least an outlet valve disposed between the enclosure and the substrate processing chamber and an inlet valve disposed between the enclosure and the source of the carrier gas, wherein: the substrate processing system is configured to cause at least a portion of the solid precursor to sublimate, and to cause the carrier gas to deliver resulting gaseous precursor chemicals, through at least the outlet valve, to the substrate processing chamber; each of the plurality of control valves comprises a respective piston for opening and closing the valve and a respective proximity sensor communicatively coupled with the controller and configured to output to the controller a position of the respective piston; and the controller is configured to: control a timing sequence of opening and closing the control valves; determine, from the output of each respective sensor, an actuation time of the respective control valve; and adjust the timing sequence based on the determined actuation time.

27. A method of operating a substrate processing system, the substrate processing system comprising a substrate processing chamber, a source of a carrier gas, a controller, and an ampoule, including a control valve arrangement, fluidically coupled with and disposed between the substrate processing chamber and the source of the carrier gas, the method comprising:controlling, with the controller, a timing sequence of opening and closing control valves within the control valve arrangement; receiving an output of a respective proximity sensor of each control valve, the output being representative of a respective valve piston position; determining, from the output of each respective sensor, an actuation time of the respective control valve; and adjusting the timing sequence based on the determined actuation time.

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