Method to reduce particle generation in gas delivery systems for semiconductor processing

Abstract

Disclosed herein is a process gas delivery apparatus comprising a precursor ampoule and a gas delivery testing module. The testing module comprises a manifold having one or more gas distribution ports extending from an inlet to the manifold. The one or more gas distribution ports of the manifold are configured to couple to at least one test component; The inlet to the manifold is coupled to the precursor ampoule. An outlet of the manifold has a transparent portion. An optical particle detector comprising a light source is optically coupled to a photodetector through an optical path passing through the transparent portion of the outlet of the manifold.

Description

METHOD TO REDUCE PARTICLE GENERATION IN GAS DELIVERY SYSTEMS FOR SEMICONDUCTOR PROCESSINGCLAIM FOR PRORITY

[0001] This application claims priority to U.S. Provisional Patent Application No.63 / 790,454, filed on April 17, 2025, titled “METHOD TO REDUCE PARTICLE GENERATION IN GAS DELIVERY SYSTEMS FOR SEMICONDUCTOR PROCESSING,” which is incorporated by reference in its entirety for all purposes. Each of these applications is hereby incorporated by reference in its entirety for all purposes.BACKGROUND

[0002] Substrate processing for etch and deposition form a backbone of the semiconductor industry. Process gases containing deposition precursors are generally preconditioned prior to introduction into process vacuum sy stems. Deposition precursors are vapors of materials that are heated to vaporization temperatures. Such materials are liquids or solids at room temperature. In many implementations, such vapors are entrained in inert carrier gases and may be mixed with reactive gases and delivered to a network of gas delivery components. While gas delivery7lines can be heated to prevent in-situ particle generation that may include re-condensation of vapors entrained in a carrier gas stream, some nucleation within the gas delivery system may still occur, particularly where abrupt pressure changes or velocity changes occur. Such abrupt changes in pressure and gas velocity may occur in interior paths within gas handling or conditioning components in a gas delivery system. In other instances, back mixing of precursor and reactive gases due to plumbing layout inadequacies can engender gas-phase or surface reactions on interior walls of gas delivery components, where these reactions are intended to occur on a production wafer surface or after in the gas phase after gases have passed out of a showerhead in the process chamber. Another cause of in-situ particle generation may be that interior wall surfaces comprise reactive materials and / or have droplet or crystal nucleation sites, which can also catalyze reactions between precursor vapor and reactive gases in the gas stream. Many of these sites exhibit hydrophilicity, having high surface energies that may act as incipient particle nuclei. For example, liquid droplets may grow at these sites, or chemical reactions may occur to form solid particles, causing liquid and solid particles to eventually enter the gas stream to be carried into a process chamber. Accumulation of solid and / or liquid particles may also occur in gas lines or components, eventually clogging these. Particles that enter the processDocket No.: 12124-1WOchamber may travel through a showerhead to deposit on wafers, which may cause significate defects in deposited films.

[0003] One way process engineers may attempt to correct these problems is to modify their gas deli very systems for a process tool in a systematic manner to mitigate in-situ particle formation. Modifications may include substituting gas handling and conditioning components in the gas delivery system to determine whether internal path designs or surface treatments of some components may be less prone to droplet formation than others. Such experimental approaches to process optimization are necessary but can consume many hours of the engineers’ time and equipment time when a process tool normally dedicated to high-volume manufacturing is used as a testing system. A more streamlined approach to gas delivery' system optimization is needed.BRIEF DESCRIPTION OF DRAWINGS

[0004] Material described herein is illustrated by way of example and not by way of limitation in accompanying figures. For simplicity and clarity of illustration, elements illustrated in figures are not necessarily drawn to scale. For example, dimensions of some elements may be exaggerated relative to other elements for clarity. Also, various physical features may be represented in their simplified forms and geometries for clarity of discussion, but it is nevertheless to be understood that practical implementations may approximate the illustrations. For example, smooth surfaces and square intersections may be drawn in disregard of finite roughness, comer-rounding, and imperfect angular intersections characteristic of structures formed by nanofabrication techniques. Further, where considered appropriate, reference labels have been repeated among figures to indicate corresponding or analogous elements.

[0005] Fig. 1 illustrates a first portion of a piping and instrumentation diagram (P&I D) for an example of a gas delivery test module, in accordance with at least one implementation.

[0006] Fig. 2 illustrates a piping and instrumentation diagram (P&I D) for another example of a gas delivery test module, in accordance with at least one implementation.

[0007] Fig. 3 illustrates a cross-sectional view of a particle detection system, in accordance with at least one implementation.

[0008] Fig. 4A illustrates a piping and instrumentation diagram (P&I D) for a stand-alone gas delivery system comprising a gas delivery test module and particle detection and a measurement system coupled to the gas delivery test module and dummy vacuum chamber, in accordance with at least one implementation.Docket No.: 12124-1WO

[0009] Fig. 4B illustrates a piping and instrumentation diagram (P&ID) for a semiconductor processing system comprising a particle detection and measuring system installed at a process gas inlet to a showerhead within the semiconductor processing system to continuously monitor particle formation in the process gas delivery system, in accordance with at least one implementation.

[0010] Fig. 5 illustrates a flowchart of an exemplary’ method for operating a gas delivery system, in accordance with at least one implementation.DETAILED DESCRIPTION

[0011] Here, the same reference numbers or other reference designators are used in the drawings to designate the same or similar (either by function and / or structure) features.

[0012] Fig. 1 illustrates a piping and instrumentation diagram (P&I D) for a gas delivery component evaluation assembly 100, in accordance with at least one implementation. Gas deliver}' component evaluation assembly 100 may be implemented as part of a larger process gas delivery system, as will be shown in Fig. 4A. In at least one example, gas delivery component evaluation assembly 100 comprises a test manifold 102, which may be implemented as a subassembly of gas deliver}’ component evaluation assembly 100.

[0013] In at least one implementation, test manifold 102 comprises an inlet line 104 and an outlet line 106. In at least one implementation, a mixing tee 108 may be a part of outlet line 106. Mixing tee 108 may enable attachment of a second gas line, such as gas line 110. to mix additional gases with gases entering through inlet line 106 and having passed through a test component 112, coupled to inlet line 104 and outlet line 106 via port 105 and port 107, respectively. For example, mixing tee 108 is coupled to an external gas source (not shown), allowing mixing of an auxiliary gas. such as an inert gas or a reactive gas, with a precursorbearing gas that has passed through test component 112. An exemplary use of test manifold 102 can be the determination of the propensity of test component 112 (e.g., a valve) to encourage development of particulates in the gas stream. The evaluation may be performed with the addition of an auxiliary gas entering through gas line 110. In at least one implementation, test manifold 102 may be installed as a self-contained module within a larger gas delivery system for the purpose of evaluating gas conditioning or handling components. For example, test manifold 102 may be implemented as a modular gas box that is connected to one or more other modular gas boxes in a larger gas delivery system, such as gas delivery component evaluation assembly 100.Docket No.: 12124-1WO

[0014] It is noted that some gas lines may be heated, as indicated by the hatched sheaths that surround the heated lines. Test component 112 may be any type of gas handling or gas conditioning component that is typically part of a gas delivery system box. Such hardware may include valves, mixers, gas line sections, orifices, charge volumes, etc., through which process gases may flow. Here, test component 112 may be substituted by similar components of different design or materials, including surface coatings, to evaluate their propensity to generate particles. Test component 112 may comprise two or more separate components connected in series. While one test component is shown in the figure, multiple test components may be connected in parallel between inlet line 104 and outlet line 106, for example as shown in Fig. 2. In some implementations, test component 112 can be heated. This propensity for particle generation can be either direct or indirect, whereby particles may be generated in the component itself, or the component may contribute to the generation of particles either upstream or dow nstream of the component, elsewhere in the gas box.

[0015] In at least one implementation, gas delivery component evaluation assembly 100 further comprises subassemblies that include a precursor ampoule 114, a particle detection and measurement system 121 and a test chamber 126. These subassemblies of gas delivery component evaluation assembly 100 are described presently. In at least one implementation, inlet line 104 is coupled to precursor ampoule 114. A carrier gas may be introduced into precursor ampoule 114 by gas line 116 to entrain vapors of a precursor substance to carry the precursor into inlet line 104. The carrier gas may be an inert gas, such as nitrogen, argon, helium, or air (if oxygen is not reactive to the precursor at the temperature and pressure of the gas). Precursor ampoule 114 may be heated to evaporate precursor material contained within, while passage of the carrier gas through gas line 116 entrains the vapors of the precursor, as noted. A valve 118 may be included at the entrance of inlet line 104 to bypass test manifold 102 when not in use.

[0016] Implementation of test manifold 102 can enable a variety of test components 112 to be readily evaluated for particle formation propensities, including gas line sections for evaluation of interior wall materials and conditions. Such interior wall materials may include hydrophobic coatings, for example. In some examples, particles may be present in outlet line 106 after precursor gas passes through test component 112 or may form in outlet line 106 spontaneously or after mixing with an auxiliary gas introduced into mixing tee 108.

[0017] In at least one implementation, an observation assembly 120 is coupled in an inline manner to outlet line 106. Particles, if present, may be transported through outlet line 106 and through observation assembly 120. In at least one implementation, observationDocket No.: 12124-1WOassembly 120 may comprise a portion of an optically transparent portion of outlet line 106, as shown. For example, observation assembly 120 may comprise a transparent tube that is coupled in-line with outlet line 106, as described below. In other implementations, observation assembly 120 may comprise a flat viewport attached to anon-transparent wall of outlet line 106. Observation assembly 120 may enable visual observation of gases travelling through, and / or an optical window for detecting and measuring particles formed in the gas stream, as is described below.

[0018] In at least one implementation, observation assembly 120 may be part of a particle detection and measurement system 121, where the particle detection and measurement system 121 comprises a light source 122 and photodetector 124. In at least one example, observation assembly 120 may comprise a quartz or fused silica tube or optical window mounted on a metal tube. Other materials may be employed, such as optical glasses, polymers such as polycarbonates, acrylic, and other polymers of suitable characteristics. The interior surface of observation assembly 120 may be treated with a coating or have a surface finish that does not contribute to particle generation.

[0019] An optical path may be formed between light source 122 and photodetector 124, shown by the dashed line extending between the two components. Light source 122 and photodetector 124 are optically coupled by the optical path, which extends through observation assembly 120. As will be shown below, photodetector 124 may be positioned at various angles with respect to the optical axis. Photodetector 124 may sample light scattered by particles entrained in the gas flowing through observation assembly 120. Particle concentration and particle size (e.g., an average) may be deduced from the light signal recorded by photodetector 124 measured at one or more angles with respect to the optical axis.

[0020] In at least one implementation, test chamber 126 is coupled to outlet line 106 downstream of observation assembly 120. In at least one implementation, test chamber 126 is a small vacuum chamber (e.g., having a volume under 5 liters) and may be implemented as a dummy chamber for facilitating connection of a high vacuum pump to gas deliverycomponent evaluation assembly 100. For example, test chamber 126 may have a volume of 1 to 5 liters. Test chamber 126 may provide a means to couple a vacuum system to test manifold 102 for applying vacuum to test manifold 102 for testing components under realistic vacuum levels.

[0021] Fig. 2 illustrates a piping and instrumentation diagram (P&I D) for a gas delivery component evaluation assembly 200, in accordance w ith at least one implementation. GasDocket No.: 12124-1WOdeliver}' component evaluation assembly 200 is substantially equivalent to gas deliver}' component evaluation assembly 100 shown in Fig. 1. In at least one example, gas delivery component evaluation assembly 200 comprises test manifold 201, which is substantially equivalent to test manifold 102 shown in Fig. 1. Test manifold 201 comprises an inlet line 202 and an outlet line 204. Both inlet line 202 and outlet line 204 are configured to attach multiple test components in parallel between inlet line 202 and outlet line 204. Multiple test components, here represented by test components 206, 208, and 210, are coupled to inlet line 202 via ports 212 and to outlet line 204 via ports 214. In at least one implementation, valves 216 and 218 may be located at ports 212 and 214, respectively. Valves 216 and 218 may control flow of gases into and out of test components 206, 208, and 210. Individual valves 216 and / or 218 may be implemented in any combination to isolate or exclude any one of test components 206, 208, or 210. Test components 206, 208, or 210 may be tested in any combination, including evaluating all test components 206, 208, and 210 simultaneously, or evaluating only a subset of test components 206-210. In at least one example, inlet line 202 and outlet line 204 may be heated. While three test components 206, 208, and 210 are shown in Fig. 2, it should be appreciated that a greater or fewer number of test components (e.g., two, etc.) may be included in the gas delivery component evaluation assembly 200.

[0022] As show n in Fig.2, test components 206-210 are connected in parallel fashion for testing separately or in combination. Multiple test components may be connected to manifold 201 in strictly parallel fashion or in a series-parallel fashion. Test components 206. 208, and 210 may be tested in any combination simultaneously or separately.

[0023] Fig. 3 illustrates a cross-sectional view of particle detection and measurement system 121, in accordance with at least one implementation. An optical path 302 extends between light source 122 and photodetector 124. Light source 122 may be a light emitting diode (LED) outputting non-coherent light or a laser source. Optical path 302 extends through a transparent portion of observation assembly 120, for example, through a tubular wall. In at least one example, photodetector 124 may be positioned at an angle 0 relative to the optical axis 304 of light source 122. Angle 9 may range between 0 degrees to 90 degrees. Photodetector 124 may be positioned off-axis with respect to the optical axis 304 to capture light scattered by particles that may be present within optical path 302. The angle (0) of light scattered may be related to particle size. For example, particles having a minimum diameter of 20 nm may be detected in this manner. Data from photodetector 124 may be output as anDocket No.: 12124-1WOanalog voltage that is read by a computing system. Correlations of photodetector signal and position to particle size and concentration may be empirically determined.

[0024] In at least one implementation, photodetector 124 may be rotated about transparent portion of observation assembly 120 on a goniometer or similar instrument to desired angles for measurement of angle-dependent scattered light luminosity or power intensity from particles transiting through observation assembly 120.

[0025] Fig. 4A illustrates a piping and instrumentation diagram (P&I D) for a gas delivery system 400 comprising gas delivery component evaluation assembly 100 or 200 coupled to a network of gas lines, as well as an external vacuum source. Boundaries of gas delivery component evaluation assembly 100 or 200 are delineated by the dashed box to distinguish it from the other components of gas delivery system 400. In some implementations, test manifold 102 or 201 may be contained in a gas box as a stand-alone module that may be integrated into a larger system such as gas delivery' component evaluation assembly 100 or 200. Here, test manifolds 102 or 201 may retain modularity' byremaining within a separate gas box that is connected to a larger system, such as gas deliverycomponent evaluation assembly 100 or 200, as shown in Fig.4A.

[0026] In some implementations, gas delivery- component evaluation assembly 100 or 200 may also be contained within a gas box. In some implementations, gas deliverycomponent evaluation assembly 100 or 200 may be integrated with gas delivery system 400, which also may be contained within one or more gas boxes. In some implementations, gas delivery system 400 comprises facility- gases, including gas supplies 402 and 404 coupled to gas lines 406 and 408, respectively. For example, gas line 406 is coupled to a gas line 116 of precursor ampoule 114, whereas gas line 408 is coupled directly- to test manifold 102 (or test manifold 201) through gas line 110 and mixing tee 108 within test manifold 102 or 201 to provide one or more auxiliary gases. In at least one implementation, the gas handling components of gas delivery system 400 may be configured within a single gas box or within multiple gas boxes. For example, in some implementations, test manifold 102 may be self-contained within a modular stand-alone gas box and coupled to gas delivery system 400 as shown, which may be contained in a separate gas box. In other implementations, test manifold 102 may be integrated within gas delivery system 400 and not be contained in a separate gas box.

[0027] In at least one implementation, gas supply 402 may provide facility (house) gases that may include nitrogen, argon, air, helium, and other suitable gases for precursor vapor carrier gases. Such gases may serve as carrier gases for transporting precursor vapors fromDocket No.: 12124-1WOprecursor ampoule 114. Gas supply 404 may provide house reactive gases that may include oxygen, water vapor, hydrogen, ammonia, hydrazine, hydrocarbons, and other suitable gases that may serve to react with precursor vapors homogeneously or heterogeneously, above specific temperatures, etc. All components of gas deliver}' system 400 have been described above in regard to Figs. 1 and 2.

[0028] Facility gases may be preconditioned prior to entering gas delivery component evaluation assembly 100 (200). For example, gas pressure and flow rate may be controlled by adjustment of mass flow controller 410 and 416 for gas supply 402 and gas supply 404. In some implementations, filters 417 and 419 may be placed indine with gas supply 402 and gas supply 404, respectively. Pressures may be monitored by pressure transducers 413 and 415, respectively. The foregoing gas handling and conditioning components may be included in a gas box that is part of gas delivery system 400, and may be separate from or inclusive of gas delivery component evaluation assembly 100 (or 200).

[0029] Test chamber 126 is shown coupled to vacuum pump 418 for pumping down gas test manifold 102 to high vacuum levels for evaluation of test components, such as test components 112, 206, 208, or 210. Vacuum pump 418 may be a turbo pump, for example. As noted above, test chamber 126 may be optionally included separately as an external component accompanying gas delivery' component evaluation assembly.

[0030] Fig. 4B illustrates a piping and instrumentation diagram (P&I D) for a semiconductor processing system 420, in accordance with at least one implementation. In at least one example, semiconductor processing system 420 comprises particle detection and measurement system 121 installed at a process gas inlet for process deposition chamber 422 coupled to a showerhead 426 within process deposition chamber 422, for continuous monitoring of particle formation in the process gas delivery system comprising gas box 424. Here, semiconductor processing system 420 includes gas delivery' system 400, contained within gas box 424. In an example, process deposition chamber 422 is a full-sized vacuum process chamber (e.g., greater than 100 liters) that is employed in semiconductor manufacture. As shown in the example of Fig. 4B, process deposition chamber 422 receives conditioned process gases from gas box 424. In at least one implementation, gas box 424 comprises gas handling and gas conditioning components that are shown for gas deliver}' system 400. In the illustrative example, gas box 424 is connected to facility gases, such as gas supplies 402 and 404. These connections may be made via gas lines 406 and 408 (see Fig.4A).Docket No.: 12124-1WO

[0031] Gas supply 404 may be a house gas supply providing air, oxygen, nitrogen, argon, or helium. In at least one implementation, gas box 424 is connected to precursor ampoule 114, which may be connected to gas supply 402 via gas line 406. Gas supply 402 may also be a house gas supply, providing house nitrogen, helium, or argon serving as inert carrier gases. For semiconductor wafer processing, process deposition chamber 422 comprises a showerhead 426 and a pedestal 428 below showerhead 426. Showerhead 426 enables deposition of vaporized precursor molecules over a wafer to create solid films. Exhaust gases may exit process deposition chamber 422 through a foreline 421 coupled to process deposition chamber 422 and to vacuum pump 418.

[0032] Process gases containing precursor vapor entrained in an inert carrier gas, such as nitrogen or argon, may be conditioned in gas box 424 in a similar fashion as is described for gas delivery component evaluation assembly 100 or 200. In at least one implementation, a particle detection and measurement system 121 is coupled to line 430 in an in-line configuration, attached between gas box 424 and process deposition chamber 422. In at least one implementation, process gases exiting gas box 424 are routed to showerhead 426 through particle detection and measurement system 121. Here, particle detection and measurement system 121 is substantially the same as described above (e.g., see Fig. 3 and accompanying description).

[0033] In addition to light source 122 and photodetector 124, particle detection and measurement system 121 comprises observation assembly 120 (denoted by the cross-hatched region), which may be a transparent tube of the same or different diameter as the nontransparent portion of line 430. Process gases flowing to showerhead 426 pass through observation assembly 120 and may be continuously monitored for presence of particles by particle detection and measurement system 121. For example, particles may form in gas handling and conditioning components of gas box 424. Particle detection and measurement system 121 may be permanently installed between gas box 424 and process deposition chamber 422 for continuously monitoring process gas streams fed to showerhead 426. Any particles introduced in this manner may contaminate films that are produced by CVD or PECVD, or cause plugging or clogging of orifices of showerhead 426. Particles small enough to pass through orifices of showerhead 426 and enter process deposition chamber may also deposit on surfaces within process deposition chamber 422, causing undesirable buildup of solid film material on chamber surfaces or on surfaces of chamber components such as pedestal 428 that may require frequent cleaning.Docket No.: 12124-1WO

[0034] Frequent downtime of process chambers such as process deposition chamber 422 can be costly, therefore monitoring process gases on a continuous basis for particle formation can be cost effective. Here, particle detection and measurement system 121 may be used as an early warning system to detect particles in the process gas stream that may not have existed prior to a certain process change, process gas composition or temperature changes as well as possible component failure, for example.

[0035] Fig. 5 illustrates a flowchart 500 of an exemplary method for operating a gas delivery system, such as gas delivery system 400, in accordance with at least one implementation. In describing the method, references are made to gas delivery component evaluation assembly 100 or 200, and gas delivery system 400.

[0036] At operation 502. a test component (e.g.. test component 112) is attached to a test module, such as gas delivery' component evaluation assembly 100 or 200. The test component may be a gas handling or gas conditioning device, such as a valve, a gauge, a section of gas line for testing hydrophobic interior coatings, an orifice, a mixing tee, or a charge volume. The test component may be a surface mount component or an in-line component. In some implementations, the test component may be a candidate component for a gas delivery system to be used for supply ing process gases to a wafer processing tool. Here, the test module may provide a platform for testing and qualifying / rejecting the component in a mock tool. In this manner, a production process tool may not need to be taken away from production for testing trials, thus may not need to be taken offline to perform component qualifying tasks. The test component may be attached to the test manifold (e.g., gas delivery component evaluation assembly 100 or 200) by coupling the component to ports (e.g., port 105 and 107) of the inlet (e.g., inlet line 104) and the outlet (e.g., outlet line 106). The ports may employ swage-type engagements for in-line connections or may employ surface-mount style engagements. Gas pressures and flow rates may be adjusted by mass flow controller (e.g., mass flow controller 410 and / or 416) adjustments. Temperatures may be adjustable for precursor and gas lines as well by adjustment of heating tapes or other hearing means surrounding gas lines and other permanent components. Base-line vacuum may be set by initiating vacuum pump 418 to pump the system down to the base-line vacuum level.

[0037] At operation 504, a process gas flow is initiated into the gas delivery test system. The process gas may emanate from an auxiliary7gas source, such as auxiliary7gas supply 402, and comprise an inert gas, such as nitrogen or argon flowing into precursor ampoule 114. Such gases can be carrier gases entraining vapors formed within ampoule 114. The gas flow may be started after the system has been pumped down to a base vacuum level by vacuumDocket No.: 12124-1WOpump 418. The auxiliary (carrier) gas or gases may be scrubbed while passing through filter 419, and its flow rate set by a mass flow controller (mass flow controller 410) on the gas line.

[0038] In addition to delivery of a earner, a reactive gas may flow to a dow nstream mixer (e.g., mixing tee 108) on gas delivery test module, where the reactive gas may mix and react with precursor. At this stage, particles may begin to nucleate in the gas phase or on interior walls of gas lines by surface reactions of precursor with reactive wall sites or with reactive gases at reactive wall sites in the gas lines themselves. Here, a hydrophobic coating such as a polymer or graphene may optionally be included on interior surfaces of gas lines and other permanent components to passivate such reactive sites for heterogeneous particle nucleation, or to provide a hydrophobic coating (e.g., graphene) on the interior surfaces to prevent droplet growth by incipient droplets formed homogeneously.

[0039] At operation 506, particles may be detected by shining light through a transparent portion (e.g., observation assembly 120) of the outlet line (e.g., outlet line 106) of the test module. Here, a light source such as light source 122 may be an LED source or laser (LED or crystal laser) positioned such that a beam of light may pass through the transparent portion and be detected by a photodetector (e.g., photodetector 124) on the opposite side. The photodetector may be off axis with respect to the optical axis (e.g., optical axis 304) of the light source to detect light scattered by particles transiting through the transparent portion. The angle of the photodetector with respect to the optical axis of the light source may be positioned at an optimal angle, for example, or at various angles to measure scattered light intensity or power. The angle of measurement may be correlated with particle size and concentration.

[0040] In some instances, well-known methods and devices are shown in block diagram form, rather than in detail, to avoid obscuring at least one implementation. Reference throughout this specification to “an implementation,” '‘one implementation,” '‘in at least one implementation,” or ’‘some implementations” means that a particular feature, structure, function, or characteristic described in connection with implementation is included in at least one implementation. Thus, appearances of phrase “in an implementation,” “in at least one implementation,” or “in one implementation,” or “some implementations” in various places throughout this specification are not necessarily referring to same implementation of disclosure. Furthermore, particular features, structures, functions, or characteristics may be combined in any suitable manner in one or more implementations. For example, a first implementation may be combined with a second implementation anywhere particularDocket No.: 12124-1WOfeatures, structures, functions, or characteristics associated with two implementations are not mutually exclusive.

[0041] As used in herein, singular forms “a,”£'an,” and '‘the” are intended to include plural forms as well, unless context clearly indicates otherwise. It will also be understood that term “and / or’ as used herein refers to and encompasses all possible combinations of one or more of associated listed items.

[0042] Here, “coupled” and “connected,” along with their derivatives, may be used herein to describe functional or structural relationships between components. These terms are not intended as synonyms for each other. Rather, in particular implementations, “connected” may be used to indicate that two or more elements are in direct physical, optical, or electrical contact with each other. “Coupled” may be used to indicate that two or more elements are in either direct or indirect (with other intervening elements between them) physical, electrical, or in magnetic contact with each other, and / or that two or more elements co-operate or interact with each other (e.g., as in a cause an effect relationship). Coupled may also have the meaning of non-mechanical contact or connection. Coupling may also have the meaning of thermal connectivity, where one object may be a heat source and another object may be a heat sink, either in thermal equilibrium with each other or subj ect to a common conductive, convective, or radiative heat flow between them; electrically coupled, where objects may be connected electrically in an electric or electronic circuit and a current flow may be induced by application of a voltage between the electrically interconnected objects or by an electric field between mechanically coupled or isolated objects; magnetically, where two mechanically coupled or isolated objects mutually share a common magnetic field flux; and fluidically, where objects such as vessels and conduits may share a common gas or liquid fluid that is static or flowing.

[0043] Here, “over,” “under,” “between,” and “on” as used herein refer to a relative position of one component or material with respect to other components or materials where such physical relationships are noteworthy. For example, in context of materials, one material or material disposed over or under another may be directly in contact or may have one or more intervening materials. Moreover, one material disposed between two materials may be directly in contact with two layers or may have one or more intervening layers. In contrast, a first material “on” a second material is in direct contact with that second material / material. Similar distinctions are to be made in context of component assemblies. As used throughout this description, and in claims, a list of items joined by term "at least one of’ or “one or more of’ can mean any combination of listed terms.Docket No.: 12124-1WO

[0044] Here, “adjacent” generally refers to a position of a thing being next to (e.g., immediately next to or close to with one or more things between them) or adjoining another thing (e.g., abutting it).

[0045] Unless otherwise specified in explicit context of their use, terms “substantially equal,” “about equal,” and “approximately equal” mean that there is no more than incidental variation between two things so described. Such variation is typically no more than + / -10% of a predetermined target value.

[0046] Here, “left,” “right,” “front,” “back,” “top,” “bottom,” “over,” “under,” and similar terms are used for descriptive purposes and not necessarily for describing permanent relative positions. For example, terms “over,” “under,” “front side,” “back side,” “top,” “bottom,” “over.” “under,” and “on” as used herein refer to a relative position of one component, structure, or material with respect to other referenced components, structures, or materials within a device, where such physical relationships are noteworthy. These terms are employed herein for descriptive purposes only and predominantly within context of a device z-axis and therefore may be relative to an orientation of a device. Hence, a first material “over” a second material in context of a figure provided herein may also be “under” second material if device is oriented upside-down relative to context of figure provided. Similar distinctions are to be made in context of component assemblies.

[0047] Here, a device that is “configured to” perform a task or function may be configured (e.g., programmed and / or hardwired) at a time of manufacturing by a manufacturer to perform the function. In at least one example, the device may be configurable (or reconfigurable) by a user after manufacturing to perform the function and / or other additional or alternative functions. In at least one example, the configuring may be through firmware and / or software programming of the device, through a construction and / or layout of hardware components and interconnections of the device, or a combination thereof.

[0048] Here, “between” may be employed in context of z-axis, x-axis, ory-axis of a device. A material that is between tw o other materials may be in contact with one or both of those materials. In another example, a material that is between two or other material may be separated from both of other two materials by one or more intervening materials. A material “between” two other materials may therefore be in contact with either of other two materials. In another example, a material “between” tw o other materials may be coupled to other tw o materials through an intervening material. A device that is between two other devices may be directly connected to one or both of those devices. In another example, a device that isDocket No.: 12124-1WObetween two other devices may be separated from both of other two devices by one or more intervening devices.

[0049] Here, '‘vacuum chamber’’ may generally refer to a vacuum chamber configured to enable semiconductor processing, such as film deposition to be carried out in a vacuum environment conditioned for such processing. In at least one implementation, the process vacuum chamber is equipped with a showerhead, pedestal and other equipment designed for semiconductor processing.

[0050] Here, “showerhead” may generally refer to a process gas distribution device that has a resemblance in appearance and function to a showerhead in a bathroom shower. In at least one implementation, the showerhead comprises a plurality of exit holes for distribution of a process gas in an even manner, generally over a semiconductor substrate within a process chamber.

[0051] Here, “process gas” may generally refer to a gas mixture containing reactive vapors and other gaseous substances, sometimes diluted by an inert carrier gas, which is employed for semiconductor processing. In at least one implementation, a process gas may comprise a nitrogen or argon carrier gas having a precursor vapor that will react in the gas phase or heterogeneously on a wafer surface to form a solid thin film.

[0052] Here, “gas delivery' apparatus” or “process gas delivery' apparatus” may generally refer to a network of piping or tubing coupled together such that process gases are distributed in a predetermined way by gas delivery components, such as filters, pressure regulators, valves, gas manifolds, etc.

[0053] Here, “mass flow controller” may generally refer to a gas handling component that maintains a constant gas flow rate of a gas flowing in a gas line regardless of changes in upstream and downstream pressures in the gas line.

[0054] Here, '‘mixing tee” may generally refer to a device configured as a conduit having an inlet and a side port or orifice, where two gases or liquids may' enter and mix in a portion of the mixing tee that may be engineered for efficient mixing, where the mixture may exit the mixing tee through an exit port or orifice.

[0055] Here, “precursor ampoule” may generally refer to a cannister or other suitable vessel for storage of a precursor material within a gas delivery apparatus. The precursor material may be in a liquid or solid state. Multiple precursor vessels may be included in a process gas delivery sy stem. In this disclosure, multiple precursor vessels are part of the multichannel chemistry delivery assembly described herein. Here, “manifold” may generally refer to a type of gas transport line that has multiple inlet and outlet ports.Docket No.: 12124-1WO

[0056] Here, “manifold’' may refer to a portion of a gas deliver}' apparatus that is configured for attaching one or more candidate gas handling and conditioning components, such as valves, orifices, gauges, conduit, charge volumes, etc., that are to be evaluated for their overall effects on the dynamics of the gas delivery apparatus that may cause particle formation.

[0057] Here, “outlet” may generally refer to a port on the manifold where gases exit the manifold.

[0058] Here, “inlet” may generally refer to a port on the manifold where gases enter the manifold.

[0059] Here, “gas distribution port” may generally refer to an orifice in the manifold configured for attachment of other gas handling components.

[0060] Here, “gas flow path” may generally refer to a path for gas flow within a gas delivery apparatus that is defined by a combination of gas lines or conduits and gas handling components that are in series or parallel.

[0061] Here, “hydrophobic” may generally refer to a property’ of lack of affinity for water. In some examples a coating of material is applied to a component to make the component repel water. It is a property of a substance or component that repels water.

[0062] Here, “hydrophobic coating” may generally refer to a coating on the interior surfaces of a gas handling component that has a low surface energy, where water or other polar liquid does not wet the hydrophobic coating. For example, the contact angle of a drop on a hydrophobic surface is 90 degrees or more, etc.

[0063] Here, “transparent portion” may generally refer to a section or portion of the outlet of the manifold that is optically transparent to allow an optical path for light from a light source to pass through the transparent section to a photodetector. The transparent portion may be a transparent component of an observation assembly of the manifold outlet allows observation of a gas flow passing through the outlet for presence of entrained particles. It may include a transparent tubular section of the outlet line of the test manifold, that may be connected in line with the outlet line of the test manifold.

[0064] Here, “light source” may generally refer to a source of light for the purposes of optical detection, such as a LED (light emitting diode) that may be configured as a noncoherent light source or as a laser (e.g., coherent) light source.

[0065] Here, “non-coherent light source” may generally refer to a light source that is not generated by stimulated emission as would be a laser source. The light photons are not in phase with one another.Docket No.: 12124-1WO

[0066] Here, “laser” may generally refer to a light source that uses stimulated emission to generate a coherent light beam, whereby emitted photons in the beam are in phase with one another.

[0067] Here, “optical path” may generally refer to a path that light follows from a source to a detector. The optical path may follow a straight line of sight to the photodetector, or may follow a bent path, where the light may deviate from a straight line by light scattering.

[0068] Here, “optical axis” may generally refer to an axis that passes through the center of an output lens of a light source and is normal thereto. The optical axis may be part or all the optical path

[0069] Here, “photodetector” may generally refer to a device that can respond to light impinging on a receiving portion of the photodetector. The response may be an analog signal that is generated by interaction of the light with the receiving portion. For example, a photodetector may be a photodiode or a phototransistor, where a current and voltage is generated, sometimes detected as a change in resistivity, by the interaction of light impinging on a semiconductive region of the photodetector.

[0070] Here, “optical particle detector” may generally refer to a device or component that includes a light source optically coupled to a photodetector through an optical path. An optical particle detector may detect light being received by it by generating an analog or a digital signal indicating detection of the light.

[0071] Here, “carrier gas” may generally refer to an inert or reactive gas for diluting and transporting reactive gases or precursor vapors.

[0072] Here, “process gas” may generally refer to a gas that is used in semiconductor processing, which may comprise a carrier gas, a reactive gas, or a gas containing a precursor vapor.

[0073] Here, “facility gas” may generally refer to one or more gases that are supplied by an infrastructure of a manufacturing facility or a laboratory facility. These gases may typically be non-specialty gases such as oxygen, argon, or nitrogen and are generally available for general use within the facility’, not necessarily exclusively for semiconductor processing.

[0074] Here, “facility gas source” may generally refer to a supplier of one or more facility gases. The supplier can be an infrastructure of a manufacturing facility or a laboratory facility.

[0075] Here, “particle” may generally refer to microscopic and sub-microscopic liquid droplets or crystallites, or a combination of both.Docket No.: 12124-1WO

[0076] Here, “entrained particle'’ may generally refer to a particle entrained in a gas flow.

[0077] Here, “gas box” may generally refer to an enclosure holding a gas delivery apparatus comprising one or more gas conditioning blocks, where multiple gases are handled and distributed within the process gas delivery apparatus.

[0078] Here, “test” may generally refer to a gas handling component that is a device under test, and may be attached to the manifold in an experimental or operational gas delivery apparatus.

[0079] Here, “charge volume” may generally refer to a vessel holding a material, such as a precursor.

[0080] Structures of various examples described herein can also be described as method(s) of forming those structures or apparatuses, and method(s) of operation of these structures or apparatuses. The following examples are provided that illustrate the various examples of the disclosure. The examples can be combined with other examples. As such, various examples can be combined with other examples without changing the scope of the invention.

[0081] Example 1 is a process gas delivery apparatus comprising a precursor ampoule; and a gas delivery testing module, comprising a manifold having one or more gas distribution ports extending from an inlet to the manifold, wherein the inlet to the manifold is coupled to the precursor ampoule; an outlet of the manifold having a transparent portion, wherein the one or more gas distribution ports of the manifold are configured to couple to at least one test component; and an optical particle detector comprising a light source optically coupled to a photodetector through an optical path, wherein the optical path passes through the transparent portion of the outlet of the manifold.

[0082] Example 2 is a process gas delivery apparatus as in any of the examples, in particular example 1, wherein the transparent portion of the outlet of the manifold is coupled to a vacuum chamber.

[0083] Example 3 is a process gas delivery' apparatus as in any of the examples, in particular example 1, wherein the at least one test component is a test valve, a test orifice, a test mixing tee, or a test charge volume.

[0084] Example 4 is a process gas delivery apparatus as in any of the examples, in particular example 1, wherein a first facility7gas source is coupled to the precursor ampoule, wherein a second facility gas source is coupled to a mixing tee within the gas delivery testing module, wherein the mixing tee is coupled to the outlet of the manifold.Docket No.: 12124-1WO

[0085] Example 5 is a process gas deliver}' apparatus as in any of the examples, in particular example 1, wherein the light source of the optical particle detector is a laser.

[0086] Example 6 is a process gas delivery apparatus as in any of the examples, in particular example 1, wherein the photodetector is configured to measure light scattered by a plurality7of entrained particles within the transparent portion at one or more angles relative to an optical axis of the light source, wherein the optical axis of the light source passes through the transparent portion.

[0087] Example 7 is a process gas delivery apparatus as in any of the examples, in particular example 6, wherein the optical particle detector is configured to detect some entrained particles of the plurality of entrained particles having a minimum diameter of 20 nm.

[0088] Example 8 is a process gas delivery apparatus as in any of the examples, in particular example 2, wherein the vacuum chamber has an interior volume of 2 liters or less.

[0089] Example 9 is a process gas delivery' apparatus as in any of the examples, in particular example 1, wherein one or more interior surfaces of the inlet and the outlet of the manifold are hydrophobic.

[0090] Example 10 is a process gas delivery' apparatus as in any of the examples, in particular example 9, wherein the one or more interior surfaces of the manifold are coated with a hydrophobic coating.

[0091] Example 11 is a system, comprising: a gas delivery testing module, comprising: a manifold having one or more gas distribution ports extending from an inlet to the manifold, wherein the inlet to the manifold is coupled to a precursor ampoule; an outlet of the manifold having a transparent portion, wherein the one or more gas distribution ports of the manifold are configured to couple to at least one test component; and an optical particle detector comprising a light source optically coupled to a photodetector through an optical path, wherein the optical path passes through the transparent portion of the outlet of the manifold; a precursor ampoule coupled to the inlet of the manifold; and a vacuum chamber coupled to the outlet of the manifold.

[0092] Example 12 is a system as in any of the examples, in particular example 11, wherein the precursor ampoule is coupled to a first facility gas source.

[0093] Example 13 is a system as in any of the examples, in particular example 11, wherein the manifold comprises a mixing tee coupled to the outlet of the manifold, wherein a second facility gas source is coupled to the mixing tee.Docket No.: 12124-1WO

[0094] Example 14 is a system as in any of the examples, in particular example 11, wherein the vacuum chamber has a volume of 2 liters or less.

[0095] Example 15 is a system as in any of the examples, in particular example 11, wherein the vacuum chamber has a volume of 100 liters or greater.

[0096] Example 16 is a method for operating a gas treatment testing module, comprising: attaching a test component in a gas delivery testing module, wherein the gas delivery testing module comprises: a manifold having one or more gas distribution ports extending from an inlet to the manifold, wherein the inlet to the manifold is coupled to a precursor ampoule; an outlet of the manifold having a transparent portion, wherein the one or more gas distribution ports of the manifold are configured to couple to at least one test component; and an optical particle detector comprising a light source optically coupled to a photodetector through an optical path, wherein the optical path passes through the transparent portion of the outlet of the manifold; flowing a gas comprising a precursor through the test component within the gas delivery testing module as part of a gas flow path; and detecting a presence of particles formed in the manifold.

[0097] Example 17 is a method as in any of the examples, in particular example 16, wherein detecting the presence of particles formed in the transparent portion of the outlet of the manifold comprises positioning the photodetector about the transparent portion to capture scattered light from the light source at a plurality of angles relative to an optical axis of the light source.

[0098] Example 18 is a method as in any of the examples, in particular example 16, wherein flowing the gas comprising the precursor through the test component comprises flowing a first facility' gas through the precursor ampoule, wherein the precursor is vaporized to a precursor vapor by the first facility gas and flowing the precursor vapor and the first facility gas through the test component.

[0099] Example 19 is a method as in any of the examples, in particular example 18, wherein flowing the gas comprising the precursor through the outlet of the manifold further comprises flowing the gas comprising the precursor through a mixing tee within the gas delivery testing module and mixing a second facility gas with the gas comprising the precursor.

[0100] Example 20 is a method as in any of the examples, in particular example 16, wherein detecting the presence of the particles formed in the transparent portion of the outlet of the manifold comprises detecting scattered light from the particles within the transparentDocket No.: 12124-1WOportion, wherein the scattered light is detected at one or more angles relative to an optical axis of the light source.

[0101] Example 21 is a method as in any of the examples, in particular example 20, wherein detecting scattered light from particles with the transparent portion comprises moving the photodetector about the transparent portion to capture light scattered at the one or more angles relative to the optical axis of the light source.

Claims

Docket No.: 12124-1WOCLAIMSWhat is claimed is:

1. A process gas delivery apparatus comprising:a precursor ampoule;a manifold having one or more gas distribution ports extending from an inlet to the manifold, wherein the inlet to the manifold is coupled to the precursor ampoule;an outlet of the manifold having a transparent portion, wherein the one or more gas distribution ports of the manifold are configured to couple to at least one test component; andan optical particle detector comprising a light source optically coupled to a photodetector through an optical path, wherein the optical path passes through the transparent portion of the outlet of the manifold.

2. The process gas delivery apparatus of claim 1. wherein the transparent portion of the outlet of the manifold is coupled to a vacuum chamber.

3. The process gas delivery' apparatus of claim 1, wherein the at least one test component is a test valve, a test orifice, a test mixing tee, or a test charge volume.

4. The process gas delivery apparatus of claim 1 , wherein a first facility gas source is coupled to the precursor ampoule, wherein a second facility gas source is coupled to a mixing tee within the manifold, and wherein the mixing tee is coupled to the outlet of the manifold.

5. The process gas delivery apparatus of claim 1, wherein the light source of the optical particle detector is a laser or a non-coherent light source.

6. The process gas delivery apparatus of claim 1. wherein the photodetector is configured to measure light scattered by a plurality of entrained particles within the transparent portion at one or more angles relative to an optical axis of the light source, and wherein the optical axis of the light source passes through the transparent portion.Docket No.: 12124-1WO7. The process gas delivery apparatus of claim 6, wherein the optical particle detector is configured to detect entrained particles of the plurality of entrained particles having a minimum diameter of 20 nm.

8. The process gas delivery apparatus of claim 2, wherein the vacuum chamber has an interior volume of 2 liters or less.

9. The process gas delivery apparatus of claim 1, wherein one or more interior surfaces of the inlet and the outlet of the manifold are hydrophobic.

10. The process gas delivery apparatus of claim 9. wherein the one or more interior surfaces of the manifold are coated with a hydrophobic coating.

11. A system comprising:a process gas delivery apparatus, comprising:a manifold having one or more gas distribution ports extending from an inlet to the manifold, wherein the inlet to the manifold is coupled to a precursor ampoule;an outlet of the manifold having a transparent portion, wherein the one or more gas distribution ports of the manifold are configured to couple to at least one test component; andan optical particle detector comprising a light source optically coupled to a photodetector through an optical path, wherein the optical path passes through the transparent portion of the outlet of the manifold; and a vacuum chamber coupled to the outlet of the manifold.

12. The system of claim 11, wherein the precursor ampoule is coupled to a facility7gas source.

13. The system of claim 11, wherein the manifold comprises a mixing tee coupled to the outlet of the manifold, w herein a second facility7gas source is coupled to the mixing tee.

14. The system of claim 11, wherein the vacuum chamber has a volume of 5 liters or less.Docket No.: 12124-1WO15. The system of claim 11, wherein the vacuum chamber has a volume of 100 liters or greater.

16. A method for operating a gas treatment testing module, comprising:attaching a test component in a gas delivery testing module, wherein the gas delivery testing module comprises:a manifold having one or more gas distribution ports extending from an inlet to the manifold, wherein the inlet to the manifold is coupled to a precursor ampoule;an outlet of the manifold having a transparent portion, wherein the one or more gas distribution ports of the manifold are configured to couple to at least one test component; andan optical particle detector comprising a light source optically coupled to a photodetector through an optical path, wherein the optical path passes through the transparent portion of the outlet of the manifold; flowing a gas comprising a precursor through the test component within the gas delivery testing module as part of a gas flow path; anddetecting a presence of particles formed in the manifold.

17. The method of claim 16. wherein detecting the presence of particles formed in the transparent portion of the outlet of the manifold comprises positioning the photodetector about the transparent portion to capture scattered light from the light source at a plurality of angles relative to an optical axis of the light source.

18. The method of claim 16, wherein flowing the gas comprising the precursor through the test component comprises flowing a first facility' gas through the precursor ampoule, and wherein the precursor is vaporized to a precursor vapor by the first facility' gas and flowing the precursor vapor and the first facility gas through the test component.

19. The method of claim 18, wherein flowing the gas comprising the precursor through the outlet of the manifold further comprises flowing the gas comprising the precursor through a mixing tee within the gas delivery testing module and mixing a second facility gas with the gas comprising the precursor.Docket No.: 12124-1WO20. The method of claim 16, wherein detecting the presence of the particles formed in the transparent portion of the outlet of the manifold comprises detecting scattered light from the particles within the transparent portion, and wherein the scattered light is detected at one or more angles relative to an optical axis of the light source.

21. The method of claim 20, wherein detecting the scattered light from the particles with the transparent portion comprises moving the photodetector about the transparent portion to capture light scattered at the one or more angles relative to the optical axis of the light source.

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