Systems and techniques for monitoring precursors for semiconductor processing

Abstract

Systems and techniques for semiconductor processing are provided. In one implementation, a technique may include heating a precursor in an ampoule to a vapor state, flowing, while heating the precursor in the ampoule, a carrier gas into the ampoule for a first time period and thereby pressurizing the ampoule and creating a mixture of the precursor and the carrier gas, measuring, during the flowing, pressure data indicative of the pressure in the ampoule, determining, based on the pressure data, a starting pressure in the ampoule at the start of the first time period and an ending pressure in the ampoule at the end of the first time period, in which the starting pressure is lower than the ending pressure, and determining, based on the pressure data, the starting pressure, and the ending pressure, an amount of precursor in the mixture at the end of the first time period.

Description

Attorney Docket No.: LAM1P068WO / 11940-1WOSYSTEMS AND TECHNIQUES FOR MONITORING PRECURSORS FOR SEMICONDUCTORPROCESSINGINCORPORATION 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 claims benefit of or priority to as identified in the concurrently filed PCT Request Form is incorporated by reference herein in their entireties and for all purposes.BACKGROUND

[0002] Semiconductor manufacturing typically involves one or more processing operations to deposit and / or etch a structure on or in a semiconductor wafer (or substrate). Such processes may employ one or more vapor-phase delivery systems in which vapor-phase and sometimes gas precursors are reacted with and / or on a surface of a substrate to deposit material thereon or to remove material therefrom. Although many forms of vapor-phase delivery systems exist, they are generally configured to provide controlled gas flow and delivery of precursors, which may otherwise be in a liquid- or solid-phase at ambient temperature and atmospheric pressure conditions.

[0003] The background provided herein is for the purposes of generally presenting the context of the disclosure. Work of the presently named inventors, to the extent that it is described in this background, 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 disclosure.SUMMARY

[0004] Details of one or more implementations of the subject matter described in this specification are set forth in the accompanying drawings and the description below.Other features, aspects, and advantages will become apparent from the description, the drawings, and the claims. The following, non-limiting implementations are considered part of the disclosure; other implementations will be evident from the entirety of this disclosure and the accompanying drawings as well.

[0005] In some implementations, a method for semiconductor processing is provided. The method may include heating a precursor in an ampoule to a vapor state, flowing,Attorney Docket No.: LAM1P068WO / 11940-1WO while heating the precursor in the ampoule, a carrier gas into the ampoule for a first time period and thereby pressurizing the ampoule and creating a mixture of the precursor and the carrier gas, measuring, during the flowing, pressure data indicative of the pressure in the ampoule, determining, based on the pressure data, a starting pressure in the ampoule at the start of the first time period and an ending pressure in the ampoule at the end of the first time period, in which the starting pressure is lower than the ending pressure, and determining, based on the pressure data, the starting pressure, and the ending pressure, an amount of precursor in the mixture at the end of the first time period.

[0006] In some implementations, the method may further include determining, based on the determined amount of precursor in the mixture, a total amount of precursor in the ampoule.

[0007] In some implementations, the method may further include opening a valve along a flow path f luidica lly connecting the ampoule to a processing chamber for a second time period and thereby flowing the mixture from the ampoule to the process chamber, closing the valve at the end of the second time period, repeating, after the closing, the heating, the flowing, the measuring, the determining the starting pressure and ending pressure, the determining the amount of precursor in the mixture, the opening, and the closing, and determining, based on the determined amount of precursor in the mixture, a total amount of precursor in the ampoule after each repeating.

[0008] In some such implementations, the method may further include determining, based on total amount of precursor, whether the total amount of precursor in the ampoule is below a threshold.

[0009] In some further implementations, the method may further include issuing, based on determining that the amount of precursor in the ampoule is below the threshold, a notification.

[0010] In some further implementations, the method may further include stopping, based on determining that the amount of precursor in the ampoule is below the threshold, the processing of a substrate in the process chamber.

[0011] In some such implementations, the total amount of precursor in the ampouleAttorney Docket No.: LAM1P068WO / 11940-1WO may decrease after each repeating.

[0012] In some further such implementations, the ampoule may have the precursor and a charge volume having the mixture, the determining the total amount of precursor in the ampoule may further include determining a running total of the amount of precursor in the ampoule, the method may further include determining the charge volume in the ampoule based, at least in part, on the running total of the amount of precursor in the ampoule, and the determining the amount of precursor in the mixture at the end of the first time period may be further based on the determined charge volume.

[0013] In some such implementations, the determining the total amount of precursor in the ampoule after each repeating may further include determining a running total of the amount of precursor in the ampoule.

[0014] In some such implementations, the method may further include adjusting, based on the determined amount of precursor in the mixture, the first time period to a third time period. The performing the flowing the carrier gas during the repeating may include flowing the carrier gas into the ampoule for the third time period.

[0015] In some such implementations, the method may further include adjusting, based on the determined amount of precursor in the mixture, the second time period to a fourth time period. The opening and the closing during the repeating may include opening the valve for the fourth time period and closing the valve at the end of the fourth time period.

[0016] In some such implementations, flowing the carrier gas may be a part of a dose step in a deposition cycle of a substrate, each deposition cycle may include one repeating, and each deposition cycle may include the dose step, a purge step, a conversion step, and a purge step.

[0017] In some such implementations, the pressure data may be measured by a pressure sensor configured to measure pressure of a fluid delivery line interposed between the ampoule and the valve.

[0018] In some implementations, the pressure data may be measured by a pressure sensor of the ampoule.

[0019] In some implementations, the determining may include determining a partial pressure of the precursor in the mixture at the end of the first time period by applying aAttorney Docket No.: LAM1P068WO / 11940-1WO saturation factor to the determined about of precursor.

[0020] In some such implementations, the saturation factor may be based on empirical data.

[0021] In some implementations, the precursor may be in a solid state before vaporization.

[0022] In some implementations, the flowing may be a part of a dose step in a deposition cycle of a substrate.

[0023] In some implementations, the method may further include issuing, based on the determining, a notification.

[0024] In some implementations, the method may further include stopping, based on the determining, processing of a substrate in a process chamber.

[0025] In some implementations a semiconductor processing system is provided. The semiconductor processing system may include an ampoule having an inlet and an outlet, and configured to contain a precursor and to heat the precursor to a vapor in a headspace of the ampoule, a carrier gas source fluidically connected to the ampoule and configured to flow carrier gas to the ampoule through the inlet, and a controller having one or more processors and one or more memories that store instructions for controlling the system, the instructions are configured to cause the one or more processors to cause the ampoule to heat the precursor in the ampoule to a vapor in the headspace, the carrier gas to flow, while heating the precursor in the ampoule, into the ampoule for a first time period and thereby pressurizing the ampoule and creating a mixture of the precursor and the carrier gas, a pressure sensor to measure, during the flowing of the carrier gas to the ampoule, pressure data indicative of the pressure in the ampoule, a determination, based on the pressure data, of a starting pressure in the ampoule at the start of the first time period and an ending pressure in the ampoule at the end of the first time period, in which the starting pressure is lower than the ending pressure, and a determination, based on the pressure data, of the starting pressure, and the ending pressure, an amount of precursor in the mixture at the end of the first time period.

[0026] In some implementations, the pressure sensor may be positioned on the ampoule.

[0027] In some implementations, the pressure sensor may be positioned on a fluidAttorney Docket No.: LAM1P068WO / 11940-1WO conduit fluidically connected to the ampoule.

[0028] In some implementations, the instructions may be further configured to cause the one or more processors to cause a determination, based on the amount of precursor in the mixture determined in (d), of a total amount of precursor in the ampoule.

[0029] In some implementations, the system may further include a processing chamber having a gas distribution device and a substrate support configured to support a substrate, a flow path spanning between, and fluidically connecting the outlet of the ampoule and the gas distribution device, and a valve fluidically interposed along the flow path and configured to control flow of the mixture along the flow path. The instructions may be further configured to cause the one or more processors to cause the valve to open for a second time period and thereby flow the mixture from the ampoule to the process chamber, and the valve to close at the end of the second time period.

[0030] In some such implementations, the instructions may be further configured to cause the one or more processors to cause a repetition, after the valve is closed at the end of the second time period, the heating, the flowing, the measuring, the determining the starting pressure and ending pressure, the determining the amount of precursor in the mixture, the opening, and the closing, and a determination, based on the determined amount of precursor in the mixture, of a total amount of precursor in the ampoule after each repetition.

[0031] In some further such implementations, the instructions may be further configured to cause the one or more processors to cause a determination, based on the total amount of precursor in the ampoule after each repeating, of whether the total amount of precursor in the ampoule is below a threshold.

[0032] In some further implementations, the instructions may be further configured to cause the one or more processors to cause an issuance, based on determining that the amount of precursor in the ampoule is below the threshold, of a notification.

[0033] In some further implementations, the instructions may be further configured to cause the one or more processors to cause the processing of a substrate in the process chamber to stop, based on determining that the amount of precursor in the ampoule is below the threshold.

[0034] In some further such implementations, the total amount of precursor in theAttorney Docket No.: LAM1P068WO / 11940-1WO ampoule may decrease after each repeating, the ampoule may have the precursor and a charge volume having the mixture, the determining the total amount of precursor in the ampoule may further include determining a running total of the amount of precursor in the ampoule, the instructions may be further configured to cause the one or more processors to cause the determination of the charge volume in the ampoule based, at least in part, on the running total of the amount of precursor in the ampoule, and the determining the amount of precursor in the mixture at the end of the first time period may be further based on the determined charge volume.

[0035] In some further such implementations, the instructions may be further configured to cause the one or more processors to cause an adjustment, based on the determined amount of precursor in the mixture, of the first time period to a third time period, and flowing the carrier gas during the repeating may include flowing the carrier gas into the ampoule for the third time period.

[0036] In some further such implementations, the instructions may be further configured to cause the one or more processors to cause an adjustment, based on the determined amount of precursor in the mixture, the second time period to a fourth time period, and the opening and the closing during the repeating may include opening the valve for the fourth time period and closing the valve at the end of the fourth time period.

[0037] In some further such implementations, flowing the carrier gas may be a part of a dose step in a deposition cycle of a substrate, each deposition cycle may include one repeating, and each deposition cycle may include the dose step, a purge step, an activation step, and a purge step.

[0038] In some such implementations, the system may further include a second processing chamber having a second gas distribution device and a second substrate support configured to support a second substrate, and a second flow path spanning between, and f I uidica I ly connecting the outlet of the ampoule and the second gas distribution device. The second flow path and the flow path may overlap for an overlapping section, the valve may be f luidica lly interposed along the overlapping section and configured to control flow of the mixture along the flow path and the second flow path, and the instructions may be further configured to cause the one or moreAttorney Docket No.: LAM1P068WO / 11940-1WO processors to cause the valve to open for the second time period and thereby flow the mixture from the ampoule to the process chamber and to the second process chamber at the same time.

[0039] In some implementations, the determining may include determining a partial pressure of the precursor in the mixture at the end of the first time period by applying a saturation factor to the determined about of precursor.

[0040] In some implementations, the precursor may be in a solid state before vaporization.

[0041] In some implementations, the precursor may be in a liquid state before vaporization.

[0042] In some implementations, the flowing may be a part of a dose step in a deposition cycle of a substrate.

[0043] In some implementations, the instructions may be further configured to cause the one or more processors to cause an issuance, based on the determining, of a notification.

[0044] In some implementations, the instructions may be further configured to cause the one or more processors to cause the processing of a substrate in a process chamber to stop, based on the determining.

[0045] In some implementations, a method for semiconductor processing may be provided. The method may include (a) heating a precursor in an ampoule to a vapor state, (b) flowing, while heating the precursor in the ampoule, a carrier gas into the ampoule for a first time period and thereby pressurizing the ampoule and creating a mixture of the precursor and the carrier gas, (c) measuring, during (b), pressure data indicative of the pressure in the ampoule, (d) determining, based on the pressure data, a starting pressure in the ampoule at the start of the first time period and an ending pressure in the ampoule at the end of the first time period, in which the starting pressure is lower than the ending pressure, and (e) determining, based on the pressure data, the starting pressure, and the ending pressure, an amount of precursor in the mixture at the end of the first time period.

[0046] In some implementations, the method may further include (f) determining, based on the amount of precursor in the mixture determined in (d), a total amount ofAttorney Docket No.: LAM1P068WO / 11940-1WO precursor in the ampoule.

[0047] In some implementations, the method may further include (g) opening a valve along a flow path f luidica lly connecting the ampoule to a processing chamber for a second time period and thereby flowing the mixture from the ampoule to the process chamber, (h) closing the valve at the end of the second time period, (i) repeating, after (h), (a) through (e), (g), and (h), and (j) determining, based on the amount of precursor in the mixture determined in (d), a total amount of precursor in the ampoule after each repeating in (i).

[0048] In some such implementations, the method may further include (k) determining, based on (j), whether the total amount of precursor in the ampoule is below a threshold.

[0049] In some further such implementations, the method may further include (I) issuing, based on determining that the amount of precursor in the ampoule is below the threshold, a notification.

[0050] In some further such implementations, the method may further include (m) stopping, based on determining that the amount of precursor in the ampoule is below the threshold, the processing of a substrate in the process chamber.

[0051] In some such implementations, the total amount of precursor in the ampoule may decrease after each repeating of (i).

[0052] In some further such implementations, the ampoule may include the precursor and a charge volume having the mixture, the determining of (j) may further include determining a running total of the amount of precursor in the ampoule, the method may further include (n) determining theO charge volume in the ampoule based, at least in part, on the running total of the amount of precursor in the ampoule, and the determining of (e) may be further based on the determined charge volume.

[0053] In some such implementations, (j) may further include determining a running total of the amount of precursor in the ampoule.

[0054] In some such implementations, the method may further include (o) adjusting, based on the determined amount of precursor in the mixture in (e), the first time period to a third time period. Performing (b) during the repeating of (i) may include flowing the carrier gas into the ampoule for the third time period.Attorney Docket No.: LAM1P068WO / 11940-1WO

[0055] In some such implementations, the method may further include (p) adjusting, based on the determined amount of precursor in the mixture in (e), the second time period to a fourth time period. Performing (g) and (h) during the repeating of (i) may include opening the valve for the fourth time period and closing the valve at the end of the fourth time period.

[0056] In some such implementations, (b) may be a part of a dose step in a deposition cycle of a substrate, each deposition cycle may include one repeating of (i), and each deposition cycle may include the dose step, a purge step, an activation step, and a purge step.

[0057] In some such implementations, the pressure data may be measured by a pressure sensor configured to measure pressure of a fluid delivery line interposed between the ampoule and the valve.

[0058] In some implementations, the pressure data may be measured by a pressure sensor of the ampoule.

[0059] In some implementations, the determining in (e) may include determining a partial pressure of the precursor in the mixture at the end of the first time period by applying a saturation factor to the determined about of precursor.

[0060] In some such implementations, the saturation factor may be based on empirical data.

[0061] In some implementations, the precursor may be in a solid state before vaporization.

[0062] In some implementations, (b) may be a part of a dose step in a deposition cycle of a substrate.

[0063] In some implementations, the method may further include (p) issuing, based on the determining of (e), a notification.

[0064] In some implementations, the method may further include (q) stopping, based on the determining of (e), processing of a substrate in a process chamber.

[0065] Additional aspects will be set forth in the detailed description which follows, and, in part, will be apparent from the disclosure, or may be learned by practice of the disclosed embodiments and / or the claimed subject matter.

[0066] The foregoing general description and the following detailed description areAttorney Docket No.: LAM1P068WO / 11940-1WO illustrative and explanatory and are intended to provide further explanation of the claimed subject matter.BRIEF DESCRIPTION OF THE DRAWINGS

[0067] Various embodiments disclosed herein are illustrated by way of example, and not by way of limitation, in the figures of the accompanying drawings, in which like reference numerals refer to similar elements.

[0068] Figure 1 depicts an example semiconductor processing system according to various implementations.

[0069] Figure 2 depicts a first example pressure chart.

[0070] Figure 3 depicts a second example pressure chart.

[0071] Figure 4 depicts a first example technique according to disclosed implementations.

[0072] Figure 5 depicts a second processing technique according to disclosed implementations.

[0073] Figures 6A and 6B depict a portion of the system of Figure 1 in various configurations during processing operations.

[0074] Figure 7 depicts another processing system according to various implementations.

[0075] Figure 8 schematically illustrates a multi-station processing tool according to some embodiments.DETAILED DESCRIPTION OF SOME EMBODIMENTS

[0076] In the following description, numerous specific details are set forth in order to provide a thorough understanding of various 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 disclosed embodiments. While the disclosed embodiments will be described in conjunction with specific embodiments, it will be understood that it is not intended to limit the disclosed embodiments.

[0077] In this application, the terms "semiconductor wafer," "wafer," "substrate," "wafer substrate" and "partially fabricated integrated circuit" are used interchangeably. One of ordinary skill in the art would understand that the term "partially fabricatedAttorney Docket No.: LAM1P068WO / 11940-1WO integrated circuit" can refer to a silicon wafer during any of many stages of integrated circuit fabrication thereon. A wafer or substrate used in the semiconductor device industry typically has a diameter of 200 mm, or 300 mm, or 450 mm. In addition to semiconductor wafers, other work pieces that may take advantage of the disclosed embodiments include various articles, such as printed circuit boards, magnetic recording media, magnetic recording sensors, mirrors, optical elements, micro-mechanical devices, and the like.Introduction and Context

[0078] As previously mentioned, various semiconductor manufacturing processes, such as atomic layer deposition (ALD), atomic layer etching (ALE), chemical vapor deposition (CVD), chemical vapor etching (CVE), and the like, as well as plasma-enhanced versions of the same, may employ at least one vapor-phase delivery system in which vapor-phase and sometimes gas precursors are reacted with and / or on a surface of a substrate to deposit material thereon or remove material therefrom. Although many forms of vapor-phase delivery systems exist, they are usually configured to provide controlled gas flow, vaporization, and delivery of precursors, which may otherwise be in a liquid- or solid-phase at ambient temperature and atmospheric pressure conditions. Although the transition from a solid-phase directly to a gaseous-phase is technically a sublimation process, as used herein, terms like "vaporization" are used to refer to the transition from a solid- or liquid-phase to a gaseous-phase.

[0079] 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. This can include, for instance, pulsed CVD (pCVD), nopurge ALD (npALD), CVD, thermal ALD, plasma-enhanced ALD (PEALD). For example, 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 toAttorney Docket No.: LAM1P068WO / 11940-1WO the film-forming 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 devices 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), conversion or 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 a "RF step", and the fourth step may be referred to as a "RF purge step."

[0080] In some implementations, an ampoule may contain a precursor, such as a precursor in a solid state, and a charge volume. The precursor is heated in the ampoule which causes the precursor to transition to a vapor state, this can include sublimating from a solid phase to a gaseous or vapor phase. Carrier gas is flowed into the ampoule to create a mixture of the vapor precursor and the carrier gas, and to pressurize the ampoule. The mixture may be flowed along a flow path that spans from the ampoule to a substrate in a processing chamber. To flow the mixture from the ampoule to the substrate, a control valve along the flow path may open and thereby allow the mixture to flow out of the ampoule which causes the ampoule pressure to drop. Once the mixture is flowed out of the ampoule for the desired amount of time, the control valve closes, after which the ampoule is refilled with carrier gas while the precursor in the ampoule is concurrently heated to continue its sublimation or vaporization. Refilling the ampoule with the carrier gas again increases the ampoule pressure and the carrier gas flow may be stopped once the ampoule is at the desired pressure. The mixture of precursor and carrier gas may again be flowed to the substrate for another processing cycle. This process may be repeated for a number of cycles for one or more substrates.

[0081] As new and different precursors and chemistries are used in semiconductor manufacturing processes, new and complex challenges are presented in utilizing and delivering these chemistries to processing stations. For example, novel and emerging processes may use low vapor pressure precursors that are delivered using an ampoule where the precursor is vaporized and mixed with a carrier gas. In this flow-over-vaporAttorney Docket No.: LAM1P068WO / 11940-1WO ampoule configuration, it can be difficult to measure the amount of the low vapor pressure precursor that is flowed out of the ampoule and delivered to a substrate. In a more specific example, some low vapor pressure solid precursors may be mixed with a high partial pressure carrier gas in the ampoule such that the partial pressure of the carrier is greater than 50 times, 75 times, or 100 times the partial pressure of the precursor. In these instances, it is also difficult to measure the amount of precursor in the mixture, including quantifying the amount of precursor using the total pressure in the ampoule. Quantifying the amount of low vapor pressure precursors in a mixture can be further challenging because the ampoule precursor vaporization rate can change as a function of ampoule temperature, ampoule pressure, and / or ampoule surface area. For some solid precursors vaporized in an ampoule, the surface area of the solid precursor can change in an unpredictable manner, especially in some ampoule designs which use internal flow restrictions such as plates or tray or restricted flow orifices along the precursor delivery path.

[0082] Provided herein are new and novel systems and techniques for measuring and determining an amount of precursor that is delivered to a substrate and an amount of precursor that remains in the ampoule. These measurements and determinations can be used to alert operations personnel that the ampoule is low on precursor and a replacement is needed, to stop processing, and to detect a deviation in the ampoule. These measurements and determinations may also be used to make one or more adjustments to the system, such as carrier gas flow into an ampoule, temperature in the ampoule, valve control timing, or a combination thereof.

[0083] As provided herein, the amount of precursor delivered to the substrate may be determined by measuring pressure data indicative of the pressure in the ampoule during carrier gas flow into the ampoule and using this pressure, known process conditions, and various relationships between these values. For instance, the ideal gas law of PV = nRT may be used to determine the molar amount of precursor in the mixture of precursor and carrier gas in the ampoule.Systems and Techniques for Semiconductor Processing

[0084] According to various implementations, systems and techniques herein vaporize,Attorney Docket No.: LAM1P068WO / 11940-1WO e.g., sublimate, the precursor to a precursor vapor with an ampoule and dilute the precursor vapor with an inert carrier gas to create a mixture of the precursor vapor and carrier gas. This mixture is then flowed from the ampoule downstream to one or more process chambers and to a substrate therein. Figure 1 depicts an example semiconductor processing system. Here, the semiconductor processing system 100 which may also be referred to as the system 100, includes an ampoule 102 that is configured to have a precursor 104 (shown with cross-hatching) and heat that precursor 104 to vaporize it and create a precursor vapor in the headspace 106 of the ampoule 102. The headspace 106, which may also be considered a "charge volume," is the volume or area of the ampoule that contains vapors and gases, and not the precursor in solid or liquid state. The ampoule 102 has an inlet 108 and an outlet 110, and the inlet 108 is configured to receive carrier gas from a carrier gas source 112. In some implementations, the carrier gas may be an inert gas, such as argon or nitrogen. The carrier gas and precursor vapor in the headspace 106 of the ampoule 102 form a mixture that is flowed out of the outlet 110.

[0085] In some implementations, the mixtures provided herein have a low vapor pressure solid precursor mixed with a high partial pressure carrier gas such that the partial pressure of the carrier gas is greater than 50 times, 75 times, or 100 times the partial pressure of the precursor. As described herein, use and measurement of these mixtures is difficult, and the techniques and systems provided herein advantageously allow for more accurate measurement and use of the precursor during processing.

[0086] To control flows into and out of the ampoule 102, the system 100 also has a first valve 116 configured to control the flow of the carrier gas from the source 112 into the ampoule 102, and a second valve 118 configured to control the flow of the mixture out of the ampoule 102. The system 100 also has a processing chamber 124 f luidica lly connected to the ampoule 102 by a flow path 122 that spans from the outlet 110 of the ampoule 102 to a chamber inlet 126 of the chamber 124. The flow path 122 may have one or more fluid conduits and one or more control valves to control the flow therein. For instance, the second valve 118 is f luidica lly interposed along the flow path 122 and configured to control the flow of the mixture out of the ampoule 102. The flow of the mixture is represented by arrows 142 and as can be seen, the mixture flows from theAttorney Docket No.: LAM1P068WO / 11940-1WO outlet 110, through the second valve 118, along the flow path 122, and to the chamber inlet 126.

[0087] In the processing chamber 124 is a gas distribution device 128, such as a showerhead, f luidica lly connected to the chamber inlet and configured to flow the mixture onto a substrate 130 in the chamber 124 and directly or indirectly supported by a substrate support 132. The gas distribution device 128 may be a showerhead positioned above the substrate 130 or the substrate support 132 that is configured to flow the precursor onto the underside of the substrate 130. The substrate support 132 may be a pedestal or an electrostatic chuck ("ESC") having one or more electrodes therein and configured to apply an electrostatic clamping force on the substrate 130. As provided in more detail below, the processing chamber 124 is configured to perform deposition cycles on the substrate 130, such as ALD, pulsed CVD (pCVD), no-purge ALD (npALD), CVD, thermal ALD, or plasma-enhanced ALD (PEALD), which may include generating a plasma and / or heating the substrate 130 in order to activate the materials, such as the precursor, on the substrate 130. The system 100 also has a third valve 134 configured to control the flow of the mixture in the flow path 122 near the chamber inlet 126.

[0088] As mentioned above, the carrier gas is flowed into the ampoule 102 and the charge volume 106 where the vaporized precursor resides and where the mixture of carrier gas and precursor is formed. In some implementations, the resulting mixture has a low vapor pressure solid precursor mixed with the high partial pressure carrier gas such that the partial pressure of the carrier gas is greater than 50 times, 75 times, or 100 times the partial pressure of the precursor. During this carrier gas flow into the ampoule, the second valve 118 is closed which causes the ampoule 102 to become pressurized (see Figure 6A, discussed below). This carrier gas flow into the charge volume 106 of the ampoule 102 may be for a first time period. In some implementations, a portion 136 of the flow path 122 spanning between the outlet 110 and the second valve 118 is f luidica lly connected with the ampoule 102 and is subjected to the same pressurization as the ampoule 102. Some such instances have a pressure sensor 138 configured to measure the pressure in the portion 136 of the flow path 122. This pressure in the portion 136, which may be a fluid conduit, corresponds with, or mirrors, the pressure in the ampouleAttorney Docket No.: LAM1P068WO / 11940-1WO102 such that the measured pressure in the portion 136 is the same, or substantially the same, as the pressure in the ampoule 102. The pressure measurement of the portion 136 can therefore be used as the pressure in the ampoule 102, and may be referred to as indicating the pressure in the ampoule. In some other instances, the ampoule 102 itself may have a pressure sensor 140 configured to measure the pressure in the ampoule 102.

[0089] Once the ampoule 102 is pressurized, the mixture can be flowed to the process chamber 124 by opening the second valve 118. In some instances that have the third valve 134, this valve 134 may also be opened in order to flow the mixture to the substrate 130. The second valve 118 is opened for a second time period during which the mixture is flowed out of the ampoule 102 and into the flow path 122. As the mixture flows out of the ampoule 102, the pressure in the ampoule drops. When the second time period ends, the second valve 118 may be closed and the ampoule 102 can be pressurized again by flowing the carrier gas into the ampoule 102; this may be considered refilling the ampoule 102 with carrier gas and increasing the ampoule pressure. Similar to above, the carrier gas flow into the ampoule may be for the first time period. During and after the first and second time periods, the ampoule 102 may intermittently or continuously heat the precursor 104 so that the precursor can continue to vaporize, or sublimate. While the second valve 118 remains closed, the vaporized precursor mixes with the carrier gas flowing into the ampoule to form the mixture in the ampoule 102 charge volume 106.

[0090] Once the ampoule has been refilled with carrier gas and additional mixture formed, the mixture can again be flowed to the substrate 130 in the chamber 124 by opening the second valve 118. In some instances, the refilling of the carrier gas for the second time period may be for a set, constant amount of time. In some implementations, each discharge of the mixture in the ampoule 102 is for one deposition cycle on the substrate 130 and this discharge may be repeated for multiple cycles on the substrate 130, such as for at least 20 cycles, 50 cycles, 100 cycles, 200 cycles, 300 cycles, or more. As stated, after each discharge of the mixture, the second valve 118 is closed and the carrier gas is flowed into the ampoule 102 while the precursor 104 is, or has been, vaporized in order to create the mixture and to pressurize the ampoule. During the initial discharges and pressurizations, the overall average pressure in the ampoule increasesAttorney Docket No.: LAM1P068WO / 11940-1WO and eventually reaches a steady-state pressure regime.

[0091] The ampoule pressurization is further explained with Figures 2 and 3. Figure 2 depicts a first example pressure chart. Here, the chart illustrates pressure measurements indicative of pressure in the ampoule, with the x-axis being time and the y-axis being pressure (normalized). When discussing this illustrated pressure in Figure 2, reference is made to system 100 of Figure 1. The pressure in Figure 2 may be pressure measurements by the pressure sensor 138 on the portion 136 of the flow path 122, or by the pressure sensor 140 on the ampoule 102. In Figure 2, at time tO, the pressure is at level P5 and is being increased by flowing the carrier gas from the source 112 and into the headspace 106 (or charge volume) of the ampoule 102 while the first valve 116 is open and the second valve 118 is closed. This pressure increase may also be considered charging the ampoule. As the carrier gas flows into the ampoule charge volume 106, the carrier gas mixes with the precursor vapor and forms the mixture. The ampoule pressure continues to increase until time tl when the pressure has reached P6 and a discharge of the ampoule occurs. In some implementations, this discharge is when the second valve 118 opens and the mixture in the ampoule 102 can flow out of the ampoule 102, through the portion 136, and through the flow path 122 to the substrate 130 in the processing chamber 124. This discharge of the mixture in the ampoule may be for a dose step of one deposition cycle on the substrate. In some implementations, this discharge may occur before the dose step occurs so that the mixture can arrive at the substrate at the desired time.

[0092] The discharge of the mixture out of the ampoule occurs from time tl to time t2 and as can be seen, the pressure drops from P6 to close to P0 which may be zero, or may be a non-zero value. At time t2 the charging of the ampoule begins. For example, at time t2, the second valve 118 is closed and the carrier gas is flowed from the source 112 into the ampoule 102. Between times t2 and t3, the pressure increases at a high rate of change from close to P0 up to pressure P4. From time t3 to time t4, the pressure increases from pressure P4 to pressure P6 at a more gradual rate of change. At time t4, another discharge of the ampoule occurs, which may be another dose step of a deposition cycle. The discharging and charging illustrated in Figure 2 may be repeated for each deposition cycle on the substrate in the processing chamber. Each discharge may beAttorney Docket No.: LAM1P068WO / 11940-1WO for the dose step in each cycle and the charging occurs during other steps in the deposition cycle.

[0093] As mentioned above, during initial startup with an ampoule the pressure begins at a low level and gradually increases to a higher steady state pressure regime, which is illustrated in Figure 3 which depicts a second example pressure chart. Here, the chart illustrates pressure measurements indicative of pressure in the ampoule, with the x-axis being time and the y-axis being pressure (normalized). When discussing this illustrated pressure in Figure 3, reference is made to the system 100 of Figure 1. At time tO, the pressure is at P0, which may be zero or a low non-zero value. From time tO to time tl, the pressure is increased in the ampoule 102 by flowing the carrier gas into the charge volume 106 of the ampoule 102. The carrier gas mixes with the precursor vapor therein to form the mixture. At time tl, a discharge occurs to flow the mixture from the ampoule in the flow path 122 to the substrate 130 in the processing chamber 124. The discharge occurs from time tl to time t2, and at time t2 another charge of the ampoule begins.

[0094] From time t2 to time t3 the ampoule is charged and at time t3 another discharge occurs from time t3 to time t4 when another charge begins. The ampoule charge occurs from time t4 to time t5 and at time t5, another discharge begins. These charge and discharge cycles are repeated as illustrated in Figure 3. For example, a discharge occurs at each odd time, such as times t9, til, and tl7, and a charge begins at the very next even time, such as times tlO, tl2, and tl8. Each discharge spans from an odd time to even time, e.g., time tl3 to time tl4, and each charge spans from an even time to an odd time, e.g., time t20 to time t21. As can be seen, the overall pressure in the ampoule increases from time tO until about time tl3 when the ampoule reaches a steady state regime. From about time tl3 until after time t27, the pressure increases and decreases are at about the same levels and values, thereby indicating the steady state pressure.

[0095] The pressure measurements that indicate pressure in the ampoule can be used to determine the amount of precursor in the mixture for each discharge. In some implementations, the ideal gas law may be used along with various process conditions and assumptions to make this determination. For example, some instances may use the following equation to determine the amount of precursor in the mixture for a discharge:Attorney Docket No.: LAM1P068WO / 11940-1WO

[0097] In this equation, np doseis the number of moles of precursor per dose, or per discharge, P is the pressure at the beginning of the charge, P2is the pressure at end of the charge, Psis the saturation pressure, Vcvis the volume of the charge volume 106, or headspace 106, in the ampoule at that charge, Ruis the universal gas constant R divided by molar mass M of the precursor, and T is the temperature of ampoule during the charge. For using this equation, it is also assumed that the charge volume at the time of the charge remains constant because the change in amount is negligible during the actual charge, however, as discussed later, the charge volume changes over time due to the gradual depletion of the precursor over time.

[0098] For the pressures P and P2, some implementations determine these pressures based on the pressure measurements provided by the pressure sensors 138 and / or 140 in Figure 1. Referring back to Figure 2, it may be advantageous to use only some of the pressure measurements between times t2 and t4 because some such measurements may not be accurate indicators of pressure in the ampoule 102. For instance, when using the pressure sensor 138 on the portion 136 of the flow path 122, there may be a delay in pressure readings between the time the second valve 118 is closed and the pressure increases in the ampoule are translated to the portion 136. This behavior is illustrated in Figure 2 between times t2 and t3 when the pressure increases at a high rate which may be exponential. Because of this, in some instances, it may be advantageous to apply a linear fit to the pressure measurement data to extrapolate and determine the beginning and ending pressures P and P2.

[0099] In Figure 2, the pressure data is the solid line and is comprised of a plurality of measurement points, e.g., tens, hundreds, or thousands, and a best fit, e.g., a linear fit, may be applied to the data between times t3 and t4, or between times t2 and t4, in order to determine the pressure P at the beginning of the charge and pressure P2at the end of the charge. In this illustration, the linear fit is a dash-dot-dash line provides the beginning pressure of P3, not P4, and the ending pressure of P6. These pressures P and P2may therefore be determined based on the measurement data, and then used in the above equation to determine the amount of precursor, or moles per dose, in the mixture that is formed in the ampoule and then discharged to the substrate for one discharge,Attorney Docket No.: LAM1P068WO / 11940-1WO which may be considered one dose step or one cycle.

[0100] For the example of Figure 2, the number of moles in the mixture formed during this charge between times t2 and t4, the determined pressures are used along with the known temperature of the ampoule during this charge, the known saturation pressure, the known molar mass of the precursor (used to determine Ruwhich is the universal gas constant R divided by molar mass M of the precursor), and the known or determined volume of the charge volume at that time. Inputting these values into the above equation can determine the amount of precursor, or moles per dose, in the mixture formed between times t2 and t4. By using these pressures per occurrence of an ampoule charge, the determination is independent of the actual pressure values to any pressure fluctuations, thereby allowing its use during any of the charges illustrated in Figure 3 including the initial startup and steady state pressures.

[0101] In some implementations, a saturation factor may be applied when determining the amount of precursor in the ampoule. For example, the saturation factor, which has a value from 0 to 1, may be multiplied by the saturation pressure in order to determine the precursor partial pressure. In the above equation, this precursor partial pressure may be used and it may be represented by Pp= sy * Ps, which is the saturation factor sy multiplied by the saturation pressure Ps. In some implementations, the saturation factor may be based on measured, empirical data.

[0102] The determined amount of precursor for one discharge may be used to determine or calculate a running total of the amount of precursor used over the course of processing a plurality of substrates. For instance, referring to Figure 3, the above pressure measurements may be obtained for each charge illustrated in Figure 3, such as for the charges between times t2 and t3, times t6 and t7, times tl6 and tl7, and times t22 and t23, for instance. For each charge, the measurements are used to determine the beginning and ending pressures of that respective charge. In some instances, these pressures are determined like above using the best fit, while in other instances, the direct measurements are used. With the beginning and ending pressures of each charge, the amount of precursor in that mixture, or the number of moles of precursor in that mixture, is determined using the techniques provided herein, such as the above equation.Attorney Docket No.: LAM1P068WO / 11940-1WO

[0103] In some implementations, each of these amounts of precursor can be added together to create a running total of the amount of precursor used during the processing.For example, a first amount of precursor np lcan be determined for the charge from time tO to time tl and the dose that occurs at time tl, a second amount of precursor np 2can be determined for the charge from time t2 to time t3 and the dose that occurs at time t3, a third amount of precursor np 3can be determined for the charge from time t4 to time t5 and the dose that occurs at time t5, and this can be repeated for each charge and discharge / dose. Each determined amount of precursor is added together in a running total, such that the running total is the sum of all preceding charges. This may be represented by np,Totai= np l+ np 2+ np 3+ ■■■ np mwith each new determined amount added to the total. For instance, after the discharge that occurs at t5 the running total of used precursor is np Totai= np l+ np 2+ np 3.

[0104] In some implementations, each of these determined amounts of precursor can be used to make other determinations, such as the amount of used precursor or the volume of the headspace. For instance, each of these determined amounts of precursor can be subtracted from the initial amount of precursor in the ampoule to determine the amount of precursor remaining in the ampoule and / or the volume of the headspace 106, or charge volume 106, in the ampoule. Over the course of each charge and discharge, the amount of precursor that is created into vapor may be a negligible amount for that individual time period, but over the course of processing multiple substrates, the amount of precursor is depleted in the ampoule. As the precursor is depleted from the ampoule, the charge volume in the ampoule increases and the techniques provided herein can be used to determine the charge volume during each charge.

[0105] For example, the amount of the initial precursor in the ampoule is known and the overall volume of the ampoule is known. The initial charge volume 106, or headspace, in the ampoule can be determined by subtracting the initial volume of precursor from the total volume of the ampoule. Each determined amount of precursor in the mixture formed during the charge can then be used in various manners to determine the charge volume at that time. For instance, the determined amount of precursor can be subtracted from the charge volume, the running total of precursor flowed out of the ampoule can be subtracted from the initial charge volume, or the like.Attorney Docket No.: LAM1P068WO / 11940-1WOThis charge volume determination can be performed at each charge and used in the next determination of precursor. For example, referring back to Figure 3, the amount of precursor in the mixture formed during the charge from time tl6 to tl7 can be determined and used to determine the charge volume, or changed charge volume, for the next precursor amount determination from time tl8 to tl9. In that subsequent determination, the updated charge volume can be used. In another example, the amount of precursor in the mixture formed during the charge from time tl6 to tl7 can be determined and used with the other previous determinations to determine the running total amount of used precursor. This running total amount of precursor can be added to the initial charge volume to determine the current charge volume for the next precursor amount determination from time tl8 to tl9.

[0106] In some implementations, the amount of precursor formed during a charge may be determined in another manner, such as determining its molar mass. For example, the mass flow mole fraction of the precursor gas may be equated to the partial pressure mole fractions of the precursor gas. Doing so results in the following equation:

[0108] Here, mpis the mass of the precursor in the mixture, mcis the mass flowrate of the carrier gas, ppis the density of the precursor, pcis the density of the carrier gas, Pampis the pressure measurement of the ampoule, which may be downstream of the ampoule in the portion 136 like in Figure 1, Ppis the partial pressure of the precursor, which is the saturation factor s (a number between 0 and 1) multiplied by the saturation pressure Psof the precursor. This relationship may be used to determine the amount of precursor for each charge, similar to above. And this determined amount of precursor can be used to determine the updated charge volume and running total of precursor used during the processing.

[0109] By determining the amount of precursor used for each dose on a substrate, the amount of precursor in the ampoule can be more accurately tracked. When the ampoule has reached a desired amount of empty, e.g., within 10% of 5% of empty, or a desired amount of precursor has been used, e.g., 90% or 95% used, an alert or other action can be taken in response to determining that the amount of precursor in the ampoule has fallen below, or reached, a threshold. In some instances, an alert may be issued in variousAttorney Docket No.: LAM1P068WO / 11940-1WO forms, such as lights, text on a display, a message sent to an operator, or the like. Examples of actions taken can include stopping the processing of the substrate.

[0110] Various processing techniques may use the pressure measurements and precursor amount determinations. Figure 4 depicts a first example technique according to disclosed implementations. Here, an ampoule having an initial amount of precursor, and a charge volume may be provided. In block 401, the precursor in the ampoule is heated to a vapor state. Referring to Figure 1, this may involve providing the ampoule 102 and heating that precursor 104 contained therein to a vapor state. As mentioned above, this may include heating a solid precursor so it sublimates into the vapor state, or heating a liquid precursor to the vapor state. In block 403, carrier gas is flowed into the ampoule while the ampoule is heating the precursor. As discussed herein, and referring back to Figure 1, this may involve flowing the carrier gas from the gas source 112 into the charge volume 106 of the ampoule 102. With the second valve 118 closed, the pressure in the ampoule 102 and the portion 136 of the flow path 122 increases. The carrier gas mixes with the precursor vapor to form the mixture, as discussed above. In some implementations, the resulting mixture has a low vapor pressure solid precursor mixed with the high partial pressure carrier gas such that the partial pressure of the carrier gas is greater than 50 times, 75 times, or 100 times the partial pressure of the precursor. The carrier gas is also flowed into the ampoule for a first time period. Referring back to Figure 2, that first time period may be considered the charge, or charging, of the ampoule from time t2 to time t4. In Figure 3, the first time periods may be between each even and subsequent odd time, such as between times tlO and til, tl6 and tl7, and t22 and t23, for instance.

[0111] In block 405, pressure data indicative of the pressure in the ampoule is measured during the flowing of the carrier gas into the ampoule of block 403. As provided herein, this may include measuring the pressure in the portion 136 with the pressure sensor 138 on a conduit or a pressure sensor 140 on the ampoule 102. As mentioned above, the pressure in the portion 136 of the flow path 122, corresponds with, or mirrors, the pressure in the ampoule 102 such that the measured pressure in the portion 136 is the same, or substantially the same, as the pressure in the ampoule 102. The pressure measurement of the portion 136 may be used as the pressure in theAttorney Docket No.: LAM1P068WO / 11940-1WO ampoule, and may be referred to as indicating the pressure in the ampoule.

[0112] In block 407, after the measuring of block 405 during the charging of the ampoule in block 403, the starting pressure and the ending pressure during the first time period, e.g., during the charging of the ampoule, may be determined. This determination is based on the measured pressure, as provided above. For example, this determination may involve applying a best fit, such as a linear fit or linear regression, to the measured pressure data, such as illustrated in Figure 2 with the dash-dot-dash line. As also provided herein, the starting pressure is lower than the ending pressure.

[0113] In block 409, the amount of precursor in the mixture at the end of the time period may be determined. This determination is based on the pressure measurement data, and the starting and ending pressures of the charge, or during the first time period. The amount of precursor in the mixture may be determined in any of the ways provided herein. For example, discussed with Figure 2, the starting pressure P3 and the ending pressure P6 during the first time period from time t2 to time t4, may be determined using the np dosenumber of moles per dose techniques above, or the molar mass techniques above.

[0114] In some implementations, blocks 401, 403, and 405 may be performed at the same time, or for at least overlapping periods. Blocks 407 and 409 may be performed after blocks 401, 403, and 405.

[0115] In some implementations, optional block 411 may be performed which determines the total amount of precursor in the ampoule, as based on the determined amount of precursor in the mixture. This determination may be made in the ways provided herein, such as by determining a running total of the amount of precursor used over the course of processing with the ampoule.

[0116] As provided above, the various processing techniques may involve multiple processing cycles, such as multiple deposition cycles or multiple ALD cycles. These techniques may repeat multiple steps, such as repeating the dose step, purge step, activation step (which may also be considered a reduction or conversion step), and purge step of each cycle for multiple cycles. Referring to Figure 4, this may include repeating blocks 401 through 411 for each cycle. Figure 5 depicts a second processing technique according to disclosed implementations. Here, blocks 501 through 511 are the same asAttorney Docket No.: LAM1P068WO / 11940-1WO blocks 401 through 411 in Figure 4. Here in Figure 5, the blocks are repeated for a number of cycles, N, which may be at least 10 cycles, 20 cycles, 50 cycles, 100 cycles, 200 cycles, 300 cycles or more. After block 509 or optional block 511, block 513 may be performed in which the mixture in the ampoule may be flowed to the processing chamber by opening the second valve 118 in Figure 1 for a second time period. With this second valve 118 open, the mixture in the ampoule can flow out of the ampoule and along the flow path 122 to the substrate 130 in the processing chamber. After the second time period, the second valve 118 is closed in block 515.

[0117] After block 515, a logic check may be performed to determine whether the desired number of cycles N have been performed. If not, then another processing cycle is performed which includes performing blocks 501 through 515. If the desired number of cycles has been performed, then the process may end. Although not illustrated in Figure 5, after closing of the valve in block 515, other operations of the processing cycle may be performed. For some deposition cycles, this can include purging the processing chamber, flowing additional chemistry onto the wafer, activating the material on the substrate with heat, plasma, or both, and purging the chamber after the activating. During these other operations, block 501 through 511 may be performed. A dose step for a processing cycle may occur by flowing the mixture from the ampoule to the substrate by performing blocks 513 and 515.

[0118] To further illustrate the performance of the technique in Figure 5, Figures 6A and 6B depict a portion of the system of Figure 1 in various configurations during processing operations. In Figure 6A, the gas source 112, ampoule 102, valves 116 and 118, a section of flow path 122 along with the portion 136 of Figure 1 are shown. Here, the second valve 118 is shown in the closed position and the first valve 116 is in the open position. The carrier gas, illustrated in black arrows, is shown flowing into the charge volume 106 of the ampoule 102 with light shading indicating the mixture is formed therein. The precursor 104 is being heated, transitioning to a vapor state, and mixing with the carrier gas in the charge volume 106 to form the mixture, illustrate with white arrows. The mixture flows into the portion 136 and not through the second valve 118 or the rest of the flow path 122. With the carrier gas flowing into the ampoule, the pressure in the ampoule is increasing and Figure 6A may correspond with blocks 501 through 505Attorney Docket No.: LAM1P068WO / 11940-1WO of Figure 5. This configuration of the system 100 may also correspond with the charging of the ampoule seen between times t2 and t4 in Figure 2, for instance.

[0119] Figure 6B depicts the portion of the system in another configuration. Here, the ampoule is being discharged. Valve 116 may be closed in some instances, as shown, or open in other instances. Second valve 118 is open and the mixture is seen flowing out of the ampoule 102, through the portion 136, through the second valve 118, and along the flow path 122 towards the substrate in the processing chamber (not shown here). This Figure 6B may correspond with block 513 of Figure 5. After the second valve 118 has been open for the second time period, it may be closed as indicated in block 515 of Figure 5 and illustrated in Figure 6A.

[0120] In some implementations, the technique may include optional block 517 which determines whether the total amount of precursor is below a particular threshold or at an unacceptable level. This is described above and can include determining that the total amount is below a threshold, such as 5% of the initial amount of precursor in the ampoule at the beginning of processing. This may also include determining that the total amount is above a threshold, such as above 90% or 95% of the initial amount of precursor in the ampoule. This optional block 517 may be determined throughout the course of processing a batch of substrates because in general, multiple substrates can be processed using the initial amount of precursor in the ampoule. Nevertheless, this optional block 517 may be performed while processing each substrate.

[0121] In response to the determination of block 517, various actions may be taken. This can include generation of a notification to an operator or to a control routine in a facility, illumination of one or more lights, or the stopping of processing. In some instances, this stopping may be considered a "soft shutdown" in which the processing system stops performing further deposition steps or other procedures typically undertaken during normal processing. In some implementations, a soft shutdown will finish the current wafer processing in the chamber before further processing and in some instances, may also remove the wafers, and put module in OFFLINE mode. After that, no more wafers will be processed.

[0122] In some implementations, the techniques may determine the amount of charge volume in the ampoule as provided above. This determination may include using theAttorney Docket No.: LAM1P068WO / 11940-1WO determining amount of precursor in the mixture for the charge, the running total of total precursor in the ampoule, or both, to determine the volume of the charge volume in the ampoule. As stated above, each charge and discharge use an amount of the precursor in the mixture that is flowed out of the ampoule, which depletes or decreases the total amount of precursor in the ampoule and simultaneously increases the charge volume in the ampoule. This determined volume of the charge volume can be used in the determination of the precursor in the mixture in the next charge cycle, as provided above.

[0123] In some implementations, other actions may be performed in response to the various determinations provided herein. This may include making adjustments to process conditions to adjust the composition of the mixture or the flow of the mixture. For example, based on the determined amount of precursor in the mixture during the charge, it may be determined that amount should be adjusted. This may include flowing additional carrier gas into the ampoule which can, in some instances, decrease the amount of precursor in the mixture. This may also or alternatively include adjusting the time that the second valve 118 is open, such as having a longer or shorter does period. For instance, if the amount of precursor in the mixture is less than desired, then the second valve 118 may be opened for a longer period of time than the second time period in order to send the mixture to the substrate for a longer period of time. In another instance, the temperature of the ampoule may be increased or decreased to increase or decrease, respectively, the amount of precursor transitioning to vapor phase.

[0124] Some implementations of the systems provided herein may have one ampoule fluidically connected to only a single processing chamber or processing station, like illustrated in Figure 1. In some other implementations, the systems may have one ampoule for a plurality of processing stations which may be in the same or separate processing chambers. Figure 7 depicts another processing system according to various implementations. Here, system 700 has the same gas source and ampoule provided in Figure 1, but there is a plurality of processing stations 724A-D, represented by boxes 724A-D, fluidically connected by a plurality of flow paths 722A-D, respectively, to the ampoule. The above techniques and concepts may be equally applied to system 700. For example, the ampoule 102 is configured to flow the mixture to the four flow paths 722A-Attorney Docket No.: LAM1P068WO / 11940-1WOD and the respective processing stations. This may include opening valve 118 so the mixture can flow in the common portion 136 and then the four flow paths 722A-D at the same time. Valves 742A-D may be configured to control the flow of process chemistry to the chambers. The amount of precursor delivered to the plurality of chambers 724A-D may be determined in the same manners described above.

[0125] Further, although four flow paths and four processing stations are shown, the number of flow paths and processing stations may vary such that there are 2, 3, 4, 5, 6, 7, 8, or 10 processing stations and corresponding flow paths. This may be the case for the stations of all systems described herein.

[0126] In some embodiments, the precursor may be molybdenum halide- or oxyhalide- based or a mixture thereof, such as MOO2CI2 or M00CI4 or M0CI5, and the carrier gas may be argon or nitrogen.

[0127] In some implementations, the systems provided herein have a controller with one or more processors and one or more memories that store instructions to cause the processor to cause the system to perform various functions. For example, referring to Figure 1, system 100 has controller 123, described in more detail below, configured to control system 100. The controller 123 has a memory that includes storing instructions to cause the processor to cause the system to perform any of the techniques and functions provided herein. For instance, the controller 123 is configured to perform the technique of Figure 4 by causing the ampoule to heat the precursor in block 401, the carrier gas to flow into the ampoule 102 while the second valve 118 is closed in block 403, and the pressure data indicative of pressure in the ampoule during the flowing and heating in block 405 to be measure. The controller 123 is configured to control the heating of the ampoule 102, the operation of the valves 116 and 118, and to receive pressure data generated by pressure sensor 138 and pressure sensor 140. The controller 123 is also configured to perform any of the determinations, such as determining the starting and ending pressures in the ampoule for each charge, applying a best fit, such as a linear fit, to the pressure data of block 409, and determining the total amount of precursor in the ampoule of block 411.

[0128] Similarly, the controller is configured to perform any of the steps of the technique of Figure 5. This can include, for example, causing the ampoule to heat theAttorney Docket No.: LAM1P068WO / 11940-1WO precursor, the carrier gas to flow into the ampoule, and pressure data from the pressure sensors during blocks 501-505 to be received and measured. This also includes the various determinations of blocks 507, 509, 511, and 517, as well as the operation of the valves in blocks 513 and 515. The controller 123 is also configured to perform multiple processing cycles on the substrate.Multistation Processing Tool

[0129] Figure 8 schematically illustrates a multi-station processing tool according to some embodiments.

[0130] In some implementations, multi-station processing tool 800 can include an inbound load lock 803 and an outbound load lock 805, either or both of which may include a plasma source and / or an ultraviolet (UV) source. Robot 837, at atmospheric pressure, is configured to move wafers from a cassette loaded through pod 809 into inbound load lock 803 via an atmospheric port 811. Wafer 807 is placed by robot 837 on pedestal 813 in inbound load lock 803, atmospheric port 811 is closed, and inbound load lock 803 is pumped down. In instances in which inbound load lock 803 includes a remote plasma source, wafer 807 may be exposed to a remote plasma treatment in inbound load lock 803 prior to being introduced into processing chamber 815. Further, wafer 807 may be heated in inbound load lock 803 to, for example, remove moisture and / or adsorbed gases. Next, chamber transport port 817 to processing chamber 815 is opened, and another robot 819 places wafer 807 into the reactor on a pedestal of a first station shown in the reactor for processing. While the implementation depicted in Figure 8 includes load locks, it will be appreciated that, in some implementations, direct entry of wafer 807 into a processing station may be provided.

[0131] As seen in Figure 8, processing chamber 815 includes four process stations, numbered 1 to 4. Each process station may be considered a process module provided above. Each station has a temperature-controlled pedestal (such as temperature- controlled pedestal 821 of station 1), and gas line inlets, one or more of which may include a corresponding flow adjuster (such as flow adjuster 151) configured to match (or substantially match) flow conditions (e.g., flow conductance, flow velocity, etc.) to the gas line inlets. It will be appreciated that, in some cases, each process station may haveAttorney Docket No.: LAM1P068WO / 11940-1WO different or multiple purposes. For example, in some embodiments, a process station may be switchable between a chemical vapor deposition (CVD) and PECVD process mode. In another example, deposition operations, e.g., PECVD operations, may be performed in one station, while exposure to UV radiation for UV curing may be performed in another station. In some cases, deposition and UV curing may be performed in the same station. Further, although processing chamber 815 shown as including four stations, embodiments are not limited thereto. For example, processing chamber 815 may have any suitable number of stations, such as five or more stations, or three or less stations.

[0132] As previously mentioned, multi-station processing tool 800 may include a wafer handling system (e.g., robot 819 including spider forks 801) for transferring and / or positioning wafers within processing chamber 815. In some embodiments, the wafer handling system may transfer wafers between various process stations and / or between a process station and a load lock. It is contemplated, however, that any suitable wafer handling system may be employed, such as, for example, wafer carousels, other wafer handling robots, etc. Further, multi-station processing tool 800 may include (or otherwise be coupled to) a system controller 823 employed to control process conditions and hardware states of multi-station processing tool 800. System controller 823 may include one or more memory devices 825, one or more mass storage devices 827, and one or more processors 829. Each processor 829 may include a central processing unit (CPU) or computer, analog, and / or digital input / output connections, stepper motor controller boards, etc.

[0133] In some embodiments, system controller 823 controls each of the activities of multi-station processing tool 800. For instance, system controller 823 may execute system control software 831 stored in mass storage device 827, loaded into memory device 825, and executed by processor 829. Alternatively, control logic may be hard coded in system controller 823. Application specific integrated circuits (ASIC), programmable logic devices (e.g., field-programmable gate arrays (FPGAs)) and / or the like may be used for these purposes. In the following discussion, wherever "software" or "code" is used, functionally comparable hard coded logic may be used in its place.System control software 831 may include instructions for controlling the timing, mixture of gases, gas flow rates, flow conductance, chamber and / or station pressure, chamberAttorney Docket No.: LAM1P068WO / 11940-1WO and / or station temperature, wafer temperature, target power levels, RF power levels, substrate pedestal, chuck and / or susceptor position, and other parameters of a particular process performed by multi-station processing tool 800. Further, system control software 831 may be configured in any suitable way. For example, various process tool component subroutines or control objects may be written to control operation of the process tool components used to carry out various process tool processes. System control software 831 may be coded in any suitable computer readable programming language.

[0134] In some embodiments, system control software 831 may include input / output control (IOC) sequencing instructions for controlling the various parameters described above. Other computer software and / or programs stored on mass storage device 827 and / or memory device 825 associated with system controller 823 may be employed in some embodiments. Examples of programs or sections of programs for this purpose include a substrate positioning program, a process gas control program, a pressure control program, a heater control program, a cooler control program, and a plasma control program.

[0135] A substrate positioning program may include program code for process tool components that are used to load and orientate wafer 807 on pedestal 821 and to control the spacing between wafer 807 and other parts of multi-station processing tool 800.

[0136] A process gas control program may include code for controlling gas composition (e.g., silicon-containing gases, oxygen-containing gases, nitrogen-containing gases, dilution (or inert) gases, etc.) flow rates, flow conductances, and optionally for flowing gas into one or more process stations prior to deposition to stabilize the pressure in the process station. A pressure control program may include code for controlling the pressure in the process station by regulating, for example, a throttle valve in an exhaust system of the process station or the like.

[0137] A heater control program may include code for controlling current to one or more heating units used to heat a pedestal (e.g., pedestal 821) and / or a showerhead of processing chamber 815. Additionally or alternatively, the heater control program may control delivery of a heat transfer gas (such as helium) to a gas distributor, and, thereby,Attorney Docket No.: LAM1P068WO / 11940-1WO to wafer 807.

[0138] A cooling control program may include code for controlling a flow rate of conductive cooling fluid through a cooling unit used to extract heat from a pedestal (e.g., pedestal 821) and / or a showerhead of processing chamber 815, and, thereby, transfer such thermal energy to, for instance, a waste heat capturing, storage, recycling, and / or disposing system. The flow of the cooling fluid through the cooling unit may also extract heat from wafer 807.

[0139] A plasma control program may include code for setting RF power levels applied to the process electrodes in one or more process stations in accordance with various embodiments.

[0140] A pressure control program may include code for maintaining pressure in a reaction chamber in accordance with various embodiments.

[0141] In some embodiments, a user interface may be provided in association with system controller 823. 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.

[0142] In some embodiments, parameters adjusted by system controller 823 may relate to process conditions. Non-limiting examples include process gas composition and flow rates, temperature, pressure, plasma conditions (such as RF bias power levels), pressure, temperature, etc. These parameters may be provided to the user in the form of a recipe, which may be entered utilizing the user interface.

[0143] Signals for monitoring the process may be provided by analog and / or digital input connections of system controller 823 from various process tool sensors. The signals for controlling the process may be output on analog and / or digital output connections of multi-station process tool 800. Non-limiting examples of process tool sensors that may be monitored include mass flow controllers, pressure sensors (such as manometers), thermocouples, etc. Appropriately programmed feedback and control algorithms may be used with data from the sensors to maintain process conditions.

[0144] System controller 823 may provide program instructions for implementing one or more of the above-described processes. The program instructions may control a variety of process parameters, such as direct current (DC) power level, RF bias powerAttorney Docket No.: LAM1P068WO / 11940-1WO level, pressure, temperature, etc. The instructions may control the parameters to operate deposition of film stacks of a stress compensation layer according to various embodiments.

[0145] System controller 823 will typically include one or more memory devices and one or more processors configured to execute the instructions so that the apparatus will perform a method in accordance with some embodiments. In some instances, machine- readable media containing instructions for controlling process operations in accordance with various embodiments may be coupled to system controller 823.

[0146] In some embodiments, system controller 823 may be part of a system, which may be part of at least one of the above-described examples. Such systems may include semiconductor processing equipment, including a processing tool or tools, a chamber or chambers, a platform or platforms for processing, and / or specific processing components (e.g., a wafer pedestal, a gas flow system, a thermal management system, etc.). The systems discussed above may be integrated with electronics for controlling their operation before, during, and / or after processing of a semiconductor wafer or substrate. The electronics may be referred to as the "controller," which may control various components or subparts of the system or systems. For instance, system controller 823, depending on the processing requirements and / or the type of system, may be programmed to control any of the processes disclosed herein, including the delivery of processing gases, temperature settings (e.g., heating and / or cooling), valve operation, flow adjuster operation, light source control for radiative heating, pressure settings, vacuum settings, power settings, RF generator settings, RF matching circuit settings, frequency settings, flow rate settings, fluid delivery settings, positional and operational settings, wafer transfers into and out of a tool or chamber and other transfer tools and / or load locks connected to or interfaced with a specific system. In this manner, system controller 823 may be configured to control, among other systems, the various actuators and motors of a wafer processing system and flow adjusters of a fluid delivery system.

[0147] Broadly speaking, system controller 823 may be defined as electronics having various integrated circuits, logic, memory, and / or software that receive instructions, issue instructions, control operation, enable cleaning operations, enable endpointAttorney Docket No.: LAM1P068WO / 11940-1WO measurements, and / or the like. 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 system controller 823 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. The operational parameters may, in some embodiments, be part of a recipe defined by process engineers to accomplish one or more processing steps during the fabrication of one or more layers, materials, metals, oxides, silicon, silicon oxide, surfaces, circuits, dies of a wafer, etc.

[0148] System controller 823, 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, system controller 823 may be in the "cloud" or all or a part of a fab host computer system, which can allow for remote access of 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 or performance 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. It is to be understood that 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, system controller 823 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 aAttorney Docket No.: LAM1P068WO / 11940-1WO 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.

[0149] Without limitation, example systems may include a plasma etch chamber or module, a deposition chamber or module, a spin-rinse chamber or module, a metal plating chamber or module, a clean chamber or module, a bevel edge etch chamber or module, a physical vapor deposition (PVD) chamber or module, a chemical vapor deposition (CVD) chamber or module, an atomic layer deposition (ALD) chamber or module, an atomic layer etch (ALE) chamber or module, an ion implantation chamber or module, a track chamber or module, and / or any other semiconductor processing system that may be associated or used in the fabrication and / or manufacturing of semiconductor wafers.

[0150] As noted above, depending on the process step or steps to be performed by the tool, system controller 823 might communicate with one or more of other tool circuits or modules, other tool components, cluster tools, other tool interfaces, adjacent tools, neighboring tools, tools located throughout a factory, a main computer, another controller, and / or tools used in material transport that bring containers of wafers to and from tool locations and / or load ports in a semiconductor manufacturing factory.Additional and / or Alternative Embodiments

[0151] Unless otherwise specified, the illustrated embodiments are to be understood as providing example features of varying detail of some embodiments. Thus, unless otherwise specified, the features, components, modules, layers, films, regions, aspects, structures, etc. (hereinafter individually or collectively referred to as an "element" or "elements"), of the various illustrations may be otherwise combined, separated, interchanged, and / or rearranged without departing from the teachings of the disclosure.

[0152] The terminology used herein is for the purpose of describing some embodiments and is not intended to be limiting. As used herein, the singular forms, "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It is to be understood that the phrases "for each <item> of the one or more <items>," "each <item> of the one or more <items>," and / or the like, ifAttorney Docket No.: LAM1P068WO / 11940-1WO used herein, are inclusive of both a single-item group and multiple-item groups, i.e., the phrase "for . . . each" is used in the sense that it is used in programming languages to refer to each item of whatever population of items is referenced. For example, if the population of items referenced is a single item, then "each" would refer to only that single item (despite dictionary definitions of "each" frequently defining the term to refer to "every one of two or more things") and would not imply that there must be at least two of those items. Similarly, the term "set" or "subset" should not be viewed, in itself, as necessarily encompassing a plurality of items— it is to be understood that a set or a subset can encompass only one member or multiple members (unless the context indicates otherwise). The terms "comprises," "comprising," "includes," and / or "including," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, components, and / or groups thereof, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and / or groups thereof. It is also noted that, as used herein, the terms "substantially," "about," and other similar terms, are used as terms of approximation and not as terms of degree, and, as such, are utilized to account for inherent deviations in measured, calculated, and / or provided values that would be recognized by one of ordinary skill in the art. Accordingly, the term "substantially" as used herein, unless otherwise specified, means within 5% of a referenced value. For example, substantially perpendicular means within ±5% of parallel.

[0153] The use of cross-hatching and / or shading in the accompanying drawings is generally provided to clarify boundaries between adjacent elements. As such, neither the presence nor the absence of cross-hatching or shading conveys or indicates any preference or requirement for particular materials, material properties, dimensions, proportions, commonalities between illustrated elements, and / or any other characteristic, attribute, property, etc., of the elements, unless specified. Further, in the accompanying drawings, the size and relative sizes of elements may be exaggerated for clarity and / or descriptive purposes. As such, the sizes and relative sizes of the respective elements are not necessarily limited to the sizes and relative sizes shown in the drawings. When an embodiment may be implemented differently, a specific process order may be performed differently from the described order. For example, two consecutivelyAttorney Docket No.: LAM1P068WO / 11940-1WO described processes may be performed substantially at the same time or performed in an order opposite to the described order.

[0154] When an element, such as a layer, is referred to as being "on," "connected to," or "coupled to" another element, it may be directly on, directly connected to, or directly coupled to the other element or at least one intervening element may be present.When, however, an element is referred to as being "directly on," "directly connected to," or "directly coupled to" another element, there are no intervening elements present. Other terms and / or phrases if used herein to describe a relationship between elements should be interpreted in a like fashion, such as "between" versus "directly between," "adjacent" versus "directly adjacent," "on" versus "directly on," etc. Further, the term "connected" may refer to physical, electrical, and / or fluid connection. To this end, for the purposes of this disclosure, the phrase "fluidically connected" is used with respect to volumes, plenums, holes, etc., that may be connected to one another, either directly or via one or more intervening components or volumes, to form a fluidic connection, similar to how the phrase "electrically connected" is used with respect to components that are connected to form an electric connection. The phrase "fluidically interposed," if used, may be used to refer to a component, volume, plenum, hole, etc., that is fluidically connected with at least two other components, volumes, plenums, holes, etc., such that fluid flowing from one of those other components, volumes, plenums, holes etc., to the other or another of those components, volumes, plenums, holes, etc., would first flow through the "fluidically interposed" component before reaching that other or another of those components, volumes, plenums, holes, etc.. For example, if a pump is fluidically interposed between a reservoir and an outlet, fluid flowing from the reservoir to the outlet would first flow through the pump before reaching the outlet. The phrase "fluidically adjacent," if used, refers to placement of a fluidic element relative to another fluidic element such that no potential structures fluidically are interposed between the two elements that might potentially interrupt fluid flow between the two fluidic elements. For example, in a flow path having a first valve, a second valve, and a third valve arranged sequentially therealong, the first valve would be fluidically adjacent to the second valve, the second valve fluidically adjacent to both the first and third valves, and the third valve fluidically adjacent to the second valve.Attorney Docket No.: LAM1P068WO / 11940-1WO

[0155] For the purposes of this disclosure, "at least one of X, Y, . . and Z" and "at least one selected from the group consisting of X, Y, . . and Z" may be construed as X only, Y only, . . ., Z only, or any combination of two or more of X, Y, . . ., and Z, such as, for instance, XYZ, XYY, YZ, and ZZ. As used herein, the term "and / or" includes any and all combinations of one or more of the associated listed items.

[0156] Although the terms "first," "second," "third," etc., may be used herein to describe various elements, these elements should not be limited by these terms. These terms are used to distinguish one element from another element. Thus, a first element discussed below could be termed a second element without departing from the teachings of the disclosure. To this end, use of such identifiers, e.g., "a first element," should not be read as suggesting, implicitly or inherently, that there is necessarily another instance, e.g., "a second element." Further, the use, if any, of ordinal indicators, such as (a), (b), (c), . . ., or (1), (2), (3), . . ., or the like, in this disclosure and accompanying claims, is to be understood as not conveying any particular order or sequence, except to the extent that such an order or sequence is explicitly indicated. For example, if there are three steps labeled (i), (ii), and (iii), it is to be understood that these steps may be performed in any order (or even concurrently, if not otherwise contraindicated), unless indicated otherwise. For example, if step (ii) involves the handling of an element that is created in step (i), then step (ii) may be viewed as happening at some point after step (i). In a similar manner, if step (i) involves the handling of an element that is created in step (ii), the reverse is to be understood.

[0157] Spatially relative terms, such as "beneath," "below," "under," "lower," "above," "upper," "over," "higher," "side" (e.g., as in "sidewall"), and the like, may be used herein for descriptive purposes, and, thereby, to describe one element's spatial relationship to at least one other element as illustrated in the drawings. Spatially relative terms are intended to encompass different orientations of an apparatus in use, operation, and / or manufacture in addition to the orientation depicted in the drawings. For example, if the apparatus in the drawings is turned over, elements described as "below" or "beneath" other elements or features would then be oriented "above" or "over" the other elements or features. Thus, the term "below" can encompass both an orientation of above and below. Furthermore, the apparatus may be otherwise oriented (e.g., rotated 90 degreesAttorney Docket No.: LAM1P068WO / 11940-1WO or at other orientations), and, as such, the spatially relative descriptors used herein interpreted accordingly.

[0158] The term "between," as used herein and when used with a range of values, is to be understood, unless otherwise indicated, as being inclusive of the start and end values of that range. For example, between 1 and 5 is to be understood as inclusive of the numbers 1, 2, 3, 4, and 5, not just the numbers 2, 3, and 4.

[0159] As used herein, the phrase "operatively connected" is to be understood as referring to a state in which two components and / or systems are connected, either directly or indirectly, such that, for example, at least one component or system can control the other. For instance, a controller may be described as being operatively connected with (or to) a resistive heating unit, which is inclusive of the controller being connected with a sub-controller of the resistive heating unit that is electrically connected with a relay that is configured to controllably connect or disconnect the resistive heating unit with a power source that is capable of providing an amount of power that is able to power the resistive heating unit so as to generate a desired degree of heating. The controller itself likely will not supply such power directly to the resistive heating unit due to the current(s) involved, but it is to be understood that the controller is nonetheless operatively connected with the resistive heating unit.

[0160] As used herein, the singular forms, "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It is also to be understood that the phrases "for each <item> of the one or more <items>," "each <item> of the one or more <items>," and / or the like, if used herein, are inclusive of both a singleitem group and multiple-item groups, i.e., the phrase "for . . . each" is used in the sense that it is used in programming languages to refer to each item of whatever population of items is referenced. For example, if the population of items referenced is a single item, then "each" would refer to only that single item (despite dictionary definitions of "each" frequently defining the term to refer to "every one of two or more things") and would not imply that there must be at least two of those items. Similarly, the term "set" or "subset" should not be viewed, in itself, as necessarily encompassing a plurality of items— it is to be understood that a set or a subset can encompass only one member or multiple members (unless the context indicates otherwise). In addition, the termsAttorney Docket No.: LAM1P068WO / 11940-1WO"comprises," "comprising," "includes," and / or "including," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, components, and / or groups thereof, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and / or groups thereof.

[0161] Various embodiments are described herein with reference to sectional views, isometric views, perspective views, plan views, and / or exploded illustrations that are schematic depictions of idealized embodiments and / or intermediate structures. As such, variations from the shapes of the illustrations as a result of, for example, manufacturing techniques and / or tolerances, are to be expected. Thus, embodiments disclosed herein should not be construed as limited to the particular illustrated shapes of regions, but are to include deviations in shapes that result from, for instance, manufacturing. To this end, regions illustrated in the drawings may be schematic in nature and shapes of these regions may not reflect the actual shapes of regions of a device, and, as such, are not intended to be limiting.

[0162] Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure is a part. Terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and are not to be interpreted in an idealized or overly formal sense, unless expressly so defined herein.

[0163] As customary in the field, some embodiments are described and illustrated in the accompanying drawings in terms of functional blocks, units, and / or modules. Those skilled in the art will appreciate that these blocks, units, and / or modules are physically implemented by electronic (or optical) circuits, such as logic circuits, discrete components, microprocessors, hard-wired circuits, memory elements, wiring connections, and the like, which may be formed using semiconductor-based fabrication techniques or other manufacturing technologies. In the case of the blocks, units, and / or modules being implemented by microprocessors or other similar hardware, they may be programmed and controlled using software (e.g., microcode) to perform various functions discussed herein and may optionally be driven by firmware and / or software. ItAttorney Docket No.: LAM1P068WO / 11940-1WO is also contemplated that each block, unit, and / or module may be implemented by dedicated hardware, or as a combination of dedicated hardware to perform some functions and a processor (e.g., one or more programmed microprocessors and associated circuitry) to perform other functions. Also, each block, unit, and / or module of some embodiments may be physically separated into two or more interacting and discrete blocks, units, and / or modules without departing from the inventive concepts. Further, the blocks, units, and / or modules of some embodiments may be physically combined into more complex blocks, units, and / or modules without departing from the teachings of the disclosure.

[0164] 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. It should be noted that there are many alternative ways of implementing the processes, systems, and apparatuses of the disclosed embodiments. Accordingly, embodiments are to be considered as illustrative and not as restrictive, and embodiments are not to be limited to the details given herein.

[0165] It is to be understood that the above disclosure, while focusing on a particular example implementation or implementations, is not limited to only the discussed example, but may also apply to similar variants and mechanisms as well, and such similar variants and mechanisms are also considered to be within the scope of this disclosure. For example, the above disclosure is directed to at least, but not exclusively, the following numbered implementations.

[0166] Implementation 1: A method for semiconductor processing, the method comprising: heating a precursor in an ampoule to a vapor state; flowing, while heating the precursor in the ampoule, a carrier gas into the ampoule for a first time period and thereby pressurizing the ampoule and creating a mixture of the precursor and the carrier gas; measuring, during the flowing, pressure data indicative of the pressure in the ampoule;Attorney Docket No.: LAM1P068WO / 11940-1WO determining, based on the pressure data, a starting pressure in the ampoule at the start of the first time period and an ending pressure in the ampoule at the end of the first time period, wherein the starting pressure is lower than the ending pressure; and determining, based on the pressure data, the starting pressure, and the ending pressure, an amount of precursor in the mixture at the end of the first time period.

[0167] Implementation 2: The method of implementation 1, further comprising determining, based on the determined amount of precursor in the mixture, a total amount of precursor in the ampoule.

[0168] Implementation 3: The method of implementations 1 or 2, further comprising: opening a valve along a flow path fl uidica lly connecting the ampoule to a processing chamber for a second time period and thereby flowing the mixture from the ampoule to the process chamber; closing the valve at the end of the second time period; repeating, after the closing, the heating, the flowing, the measuring, the determining the starting pressure and ending pressure, the determining the amount of precursor in the mixture, the opening, and the closing; and determining, based on the determined amount of precursor in the mixture, a total amount of precursor in the ampoule after each repeating.

[0169] Implementation 4: The method of implementation 3, further comprising determining, based on total amount of precursor, whether the total amount of precursor in the ampoule is below a threshold.

[0170] Implementation 5: The method of implementation 4, further comprising issuing, based on determining that the amount of precursor in the ampoule is below the threshold, a notification.

[0171] Implementation 6: The method of implementation 4, further comprising stopping, based on determining that the amount of precursor in the ampoule is below the threshold, the processing of a substrate in the process chamber.

[0172] Implementation 7: The method of any one of implementations 3 to 6, wherein the total amount of precursor in the ampoule decreases after each repeating.

[0173] Implementation 8: The method of implementation 7, wherein: the ampoule comprises the precursor and a charge volume having the mixture,Attorney Docket No.: LAM1P068WO / 11940-1WO the determining the total amount of precursor in the ampoule further comprises determining a running total of the amount of precursor in the ampoule, the method further comprises determining the charge volume in the ampoule based, at least in part, on the running total of the amount of precursor in the ampoule, and the determining the amount of precursor in the mixture at the end of the first time period is further based on the determined charge volume.

[0174] Implementation 9: The method of any one of implementations 3 to 8, wherein determining the total amount of precursor in the ampoule after each repeating further comprises determining a running total of the amount of precursor in the ampoule.

[0175] Implementation 10: The method of any one of implementations 3 to 9, further comprising adjusting, based on the determined amount of precursor in the mixture, the first time period to a third time period, wherein performing the flowing the carrier gas during the repeating comprises flowing the carrier gas into the ampoule for the third time period.

[0176] Implementation 11: The method of any one of implementations 3 to 10, further comprising adjusting, based on the determined amount of precursor in the mixture, the second time period to a fourth time period, wherein the opening and the closing during the repeating comprises opening the valve for the fourth time period and closing the valve at the end of the fourth time period.

[0177] Implementation 12: The method of any one implementations 3 to 11, wherein: flowing the carrier gas is a part of a dose step in a deposition cycle of a substrate, each deposition cycle comprises one repeating, and each deposition cycle comprises the dose step, a purge step, a conversion step, and a purge step.

[0178] Implementation 13: The method of any one of implementations 3 to 12, wherein the pressure data is measured by a pressure sensor configured to measure pressure of a fluid delivery line interposed between the ampoule and the valve.

[0179] Implementation 14: The method of any one of implementations 1 to 13, wherein the pressure data is measured by a pressure sensor of the ampoule.

[0180] Implementation 15: The method of any one of implementations 1 to 14,Attorney Docket No.: LAM1P068WO / 11940-1WO wherein the determining comprises determining a partial pressure of the precursor in the mixture at the end of the first time period by applying a saturation factor to the determined about of precursor.

[0181] Implementation 16: The method of implementation 15, wherein the saturation factor is based on empirical data.

[0182] Implementation 17: The method of any one of implementations 1 to 16, wherein the precursor is in a solid state before vaporization.

[0183] Implementation 18: The method of any one of implementations 1 to 17, wherein the flowing is a part of a dose step in a deposition cycle of a substrate.

[0184] Implementation 19: The method of any one of implementations 1 to 18, further comprising issuing, based on the determining, a notification.

[0185] Implementation 20: The method of any one of implementations 1 to 19, further comprising stopping, based on the determining, processing of a substrate in a process chamber.

[0186] Implementation 21: A semiconductor processing system, comprising: an ampoule having an inlet and an outlet, and configured to contain a precursor and to heat the precursor to a vapor in a headspace of the ampoule; a carrier gas source fluidically connected to the ampoule and configured to flow carrier gas to the ampoule through the inlet; and a controller having one or more processors and one or more memories that store instructions for controlling the system, the instructions are configured to cause the one or more processors to cause: the ampoule to heat the precursor in the ampoule to a vapor in the headspace, the carrier gas to flow, while heating the precursor in the ampoule, into the ampoule for a first time period and thereby pressurizing the ampoule and creating a mixture of the precursor and the carrier gas, a pressure sensor to measure, during the flowing of the carrier gas to the ampoule, pressure data indicative of the pressure in the ampoule, a determination, based on the pressure data, of a starting pressure in the ampoule at the start of the first time period and an ending pressure in theAttorney Docket No.: LAM1P068WO / 11940-1WO ampoule at the end of the first time period, wherein the starting pressure is lower than the ending pressure, and a determination, based on the pressure data, of the starting pressure, and the ending pressure, an amount of precursor in the mixture at the end of the first time period.

[0187] Implementation 22: The system of implementation 21, wherein the pressure sensor is positioned on the ampoule.

[0188] Implementation 23: The system of implementation 21 or implementation 22, wherein the pressure sensor is positioned on a fluid conduit fluidically connected to the ampoule.

[0189] Implementation 24: The system of any one of implementations 21 to 23, wherein the instructions are further configured to cause the one or more processors to cause a determination, based on the amount of precursor in the mixture determined in (d), of a total amount of precursor in the ampoule.

[0190] Implementation 25: The system of any one of implementations 21 to 24, further comprising: a processing chamber having a gas distribution device and a substrate support configured to support a substrate; a flow path spanning between, and fluidically connecting the outlet of the ampoule and the gas distribution device; and a valve fluidically interposed along the flow path and configured to control flow of the mixture along the flow path, wherein the instructions are further configured to cause the one or more processors to cause: the valve to open for a second time period and thereby flow the mixture from the ampoule to the process chamber, and the valve to close at the end of the second time period.

[0191] Implementation 26: The system of implementation 25, wherein the instructions are further configured to cause the one or more processors to cause: a repetition, after the valve is closed at the end of the second time period, the heating, the flowing, the measuring, the determining the starting pressure and endingAttorney Docket No.: LAM1P068WO / 11940-1WO pressure, the determining the amount of precursor in the mixture, the opening, and the closing, and a determination, based on the determined amount of precursor in the mixture, of a total amount of precursor in the ampoule after each repetition.

[0192] Implementation 27: The system of implementation 26, wherein the instructions are further configured to cause the one or more processors to cause a determination, based on the total amount of precursor in the ampoule after each repeating, of whether the total amount of precursor in the ampoule is below a threshold.

[0193] Implementation 28: The system of implementation 27, wherein the instructions are further configured to cause the one or more processors to cause an issuance, based on determining that the amount of precursor in the ampoule is below the threshold, of a notification.

[0194] Implementation 29: The system of implementation 27, wherein the instructions are further configured to cause the one or more processors to cause the processing of a substrate in the process chamber to stop, based on determining that the amount of precursor in the ampoule is below the threshold.

[0195] Implementation 30: The system of implementation 26, wherein: the total amount of precursor in the ampoule decreases after each repeating, the ampoule comprises the precursor and a charge volume having the mixture, the determining the total amount of precursor in the ampoule further comprises determining a running total of the amount of precursor in the ampoule, the instructions are further configured to cause the one or more processors to cause the determination of the charge volume in the ampoule based, at least in part, on the running total of the amount of precursor in the ampoule, and the determining the amount of precursor in the mixture at the end of the first time period is further based on the determined charge volume.

[0196] Implementation 31: The system of implementation 26, wherein: the instructions are further configured to cause the one or more processors to cause an adjustment, based on the determined amount of precursor in the mixture, of the first time period to a third time period, andAttorney Docket No.: LAM1P068WO / 11940-1WO flowing the carrier gas during the repeating comprises flowing the carrier gas into the ampoule for the third time period.

[0197] Implementation 32: The system of implementation 26, wherein: the instructions are further configured to cause the one or more processors to cause an adjustment, based on the determined amount of precursor in the mixture, the second time period to a fourth time period, and the opening and the closing during the repeating comprises opening the valve for the fourth time period and closing the valve at the end of the fourth time period.

[0198] Implementation 33: The system of implementation 26, wherein: flowing the carrier gas is a part of a dose step in a deposition cycle of a substrate, each deposition cycle comprises one repeating, and each deposition cycle comprises the dose step, a purge step, an activation step, and a purge step.

[0199] Implementation 34: The system of implementation 25, further comprising: a second processing chamber having a second gas distribution device and a second substrate support configured to support a second substrate; and a second flow path spanning between, and fluidically connecting the outlet of the ampoule and the second gas distribution device, wherein: the second flow path and the flow path overlap for an overlapping section, the valve is fluidically interposed along the overlapping section and configured to control flow of the mixture along the flow path and the second flow path, and the instructions are further configured to cause the one or more processors to cause the valve to open for the second time period and thereby flow the mixture from the ampoule to the process chamber and to the second process chamber at the same time.

[0200] Implementation 35: The system of any one of implementations 21 to 34, wherein the determining comprises determining a partial pressure of the precursor in the mixture at the end of the first time period by applying a saturation factor to the determined about of precursor.

[0201] Implementation 36: The system of any one of implementations 21 to 35,Attorney Docket No.: LAM1P068WO / 11940-1WO wherein the precursor is in a solid state before vaporization.

[0202] Implementation 37: The system of any one of implementations 21 to 36, wherein the precursor is in a liquid state before vaporization.

[0203] Implementation 38: The system of any one of implementations 21 to 37, wherein the flowing is a part of a dose step in a deposition cycle of a substrate.

[0204] Implementation 39: The system of any one of implementations 21 to 38, wherein the instructions are further configured to cause the one or more processors to cause an issuance, based on the determining, of a notification.

[0205] Implementation 40: The system of any one of implementations 21 to 39, wherein the instructions are further configured to cause the one or more processors to cause the processing of a substrate in a process chamber to stop, based on the determining.

[0206] Implementation 41: A method for semiconductor processing, the method comprising:(a) heating a precursor in an ampoule to a vapor state;(b) flowing, while heating the precursor in the ampoule, a carrier gas into the ampoule for a first time period and thereby pressurizing the ampoule and creating a mixture of the precursor and the carrier gas;(c) measuring, during (b), pressure data indicative of the pressure in the ampoule;(d) determining, based on the pressure data, a starting pressure in the ampoule at the start of the first time period and an ending pressure in the ampoule at the end of the first time period, wherein the starting pressure is lower than the ending pressure; and(e) determining, based on the pressure data, the starting pressure, and the ending pressure, an amount of precursor in the mixture at the end of the first time period.

[0207] Implementation 42: The method of implementation 41, further comprising (f) determining, based on the amount of precursor in the mixture determined in (d), a total amount of precursor in the ampoule.

[0208] Implementation 43: The method of implementation 41 or 42, further comprising:Attorney Docket No.: LAM1P068WO / 11940-1WO(g) opening a valve along a flow path f luidica lly connecting the ampoule to a processing chamber for a second time period and thereby flowing the mixture from the ampoule to the process chamber;(h) closing the valve at the end of the second time period;(i) repeating, after (h), (a) through (e), (g), and (h); and(j) determining, based on the amount of precursor in the mixture determined in (d), a total amount of precursor in the ampoule after each repeating in (i).

[0209] Implementation 44: The method of implementation 43, further comprising (k) determining, based on (j), whether the total amount of precursor in the ampoule is below a threshold.

[0210] Implementation 45: The method of implementation 44, further comprising (I) issuing, based on determining that the amount of precursor in the ampoule is below the threshold, a notification.

[0211] Implementation 46: The method of implementation 44, further comprising (m) stopping, based on determining that the amount of precursor in the ampoule is below the threshold, the processing of a substrate in the process chamber.

[0212] Implementation 47: The method of implementation 43, wherein the total amount of precursor in the ampoule decreases after each repeating of (i).

[0213] Implementation 48: The method of implementation 47, wherein: the ampoule comprises the precursor and a charge volume having the mixture, the determining of (j) further comprises determining a running total of the amount of precursor in the ampoule, the method further comprises (n) determining the charge volume in the ampoule based, at least in part, on the running total of the amount of precursor in the ampoule, and the determining of (e) is further based on the determined charge volume.

[0214] Implementation 49: The method of implementation 43, wherein (j) further comprises determining a running total of the amount of precursor in the ampoule.

[0215] Implementation 50: The method of implementation 43, further comprising (o) adjusting, based on the determined amount of precursor in the mixture in (e), the first time period to a third time period, wherein performing (b) during the repeating of (i)Attorney Docket No.: LAM1P068WO / 11940-1WO comprises flowing the carrier gas into the ampoule for the third time period.

[0216] Implementation 51: The method of implementation 43, further comprising (p) adjusting, based on the determined amount of precursor in the mixture in (e), the second time period to a fourth time period, wherein performing (g) and (h) during the repeating of (i) comprises opening the valve for the fourth time period and closing the valve at the end of the fourth time period.

[0217] Implementation 52: The method of implementation 43, wherein:(b) is a part of a dose step in a deposition cycle of a substrate, each deposition cycle comprises one repeating of (i), and each deposition cycle comprises the dose step, a purge step, an activation step, and a purge step.

[0218] Implementation 53: The method of implementation 43, wherein the pressure data is measured by a pressure sensor configured to measure pressure of a fluid delivery line interposed between the ampoule and the valve.

[0219] Implementation 54: The method of any one of implementations 41 to 53, wherein the pressure data is measured by a pressure sensor of the ampoule.

[0220] Implementation 55: The method of any one of implementations 41 to 54, wherein the determining in (e) comprises determining a partial pressure of the precursor in the mixture at the end of the first time period by applying a saturation factor to the determined about of precursor.

[0221] Implementation 56: The method of implementation 55, wherein the saturation factor is based on empirical data.

[0222] Implementation 57: The method of any one of implementations 41 to 56, wherein the precursor is in a solid state before vaporization.

[0223] Implementation 58: The method of any one of implementations 41 to 57, wherein (b) is a part of a dose step in a deposition cycle of a substrate.

[0224] Implementation 59: The method of any one of implementations 41 to 58, further comprising (p) issuing, based on the determining of (e), a notification.

[0225] Implementation 60: The method of any one of implementations 41 to 59, further comprising (q) stopping, based on the determining of (e), processing of a substrate in a process chamber.

Claims

Attorney Docket No.: LAM1P068WO / 11940-1WOCLAIMSWhat is claimed is:

1. A method for semiconductor processing, the method comprising: heating a precursor in an ampoule to a vapor state; flowing, while heating the precursor in the ampoule, a carrier gas into the ampoule for a first time period and thereby pressurizing the ampoule and creating a mixture of the precursor and the carrier gas; measuring, during the flowing, pressure data indicative of the pressure in the ampoule; determining, based on the pressure data, a starting pressure in the ampoule at the start of the first time period and an ending pressure in the ampoule at the end of the first time period, wherein the starting pressure is lower than the ending pressure; and determining, based on the pressure data, the starting pressure, and the ending pressure, an amount of precursor in the mixture at the end of the first time period.

2. The method of claim 1, further comprising determining, based on the determined amount of precursor in the mixture, a total amount of precursor in the ampoule.

3. The method of claim 1, further comprising: opening a valve along a flow path fl uidica lly connecting the ampoule to a processing chamber for a second time period and thereby flowing the mixture from the ampoule to the process chamber; closing the valve at the end of the second time period; repeating, after the closing, the heating, the flowing, the measuring, the determining the starting pressure and ending pressure, the determining the amount of precursor in the mixture, the opening, and the closing; and determining, based on the determined amount of precursor in the mixture, a total amount of precursor in the ampoule after each repeating.

4. The method of claim 3, further comprising determining, based on total amount of precursor, whether the total amount of precursor in the ampoule is below a threshold.

5. The method of claim 4, further comprising issuing, based on determining that the amount of precursor in the ampoule is below the threshold, a notification.Attorney Docket No.: LAM1P068WO / 11940-1WO6. The method of claim 4, further comprising stopping, based on determining that the amount of precursor in the ampoule is below the threshold, the processing of a substrate in the process chamber.

7. The method of claim 3, wherein the total amount of precursor in the ampoule decreases after each repeating.

8. The method of claim 7, wherein: the ampoule comprises the precursor and a charge volume having the mixture, the determining the total amount of precursor in the ampoule further comprises determining a running total of the amount of precursor in the ampoule, the method further comprises determining the charge volume in the ampoule based, at least in part, on the running total of the amount of precursor in the ampoule, and the determining the amount of precursor in the mixture at the end of the first time period is further based on the determined charge volume.

9. The method of claim 3, wherein determining the total amount of precursor in the ampoule after each repeating further comprises determining a running total of the amount of precursor in the ampoule.

10. The method of claim 3, further comprising adjusting, based on the determined amount of precursor in the mixture, the first time period to a third time period, wherein performing the flowing the carrier gas during the repeating comprises flowing the carrier gas into the ampoule for the third time period.

11. The method of claim 3, further comprising adjusting, based on the determined amount of precursor in the mixture, the second time period to a fourth time period, wherein the opening and the closing during the repeating comprises opening the valve for the fourth time period and closing the valve at the end of the fourth time period.

12. The method of claim 3, wherein: flowing the carrier gas is a part of a dose step in a deposition cycle of a substrate, each deposition cycle comprises one repeating, and each deposition cycle comprises the dose step, a purge step, a conversion step, and a purge step.Attorney Docket No.: LAM1P068WO / 11940-1WO13. The method of claim 3, wherein the pressure data is measured by a pressure sensor configured to measure pressure of a fluid delivery line interposed between the ampoule and the valve.

14. The method of claim 1, wherein the pressure data is measured by a pressure sensor of the ampoule.

15. The method of claim 1, wherein the determining comprises determining a partial pressure of the precursor in the mixture at the end of the first time period by applying a saturation factor to the determined about of precursor.

16. The method of claim 1, wherein the flowing is a part of a dose step in a deposition cycle of a substrate.

17. The method of claim 1, further comprising issuing, based on the determining, a notification.

18. The method of claim 1, further comprising stopping, based on the determining, processing of a substrate in a process chamber.

19. A semiconductor processing system, comprising: an ampoule having an inlet and an outlet, and configured to contain a precursor and to heat the precursor to a vapor in a headspace of the ampoule; a carrier gas source fluidically connected to the ampoule and configured to flow carrier gas to the ampoule through the inlet; and a controller having one or more processors and one or more memories that store instructions for controlling the system, the instructions are configured to cause the one or more processors to cause: the ampoule to heat the precursor in the ampoule to a vapor in the headspace, the carrier gas to flow, while heating the precursor in the ampoule, into the ampoule for a first time period and thereby pressurizing the ampoule and creating a mixture of the precursor and the carrier gas, a pressure sensor to measure, during the flowing of the carrier gas to the ampoule, pressure data indicative of the pressure in the ampoule, a determination, based on the pressure data, of a starting pressure in the ampoule at the start of the first time period and an ending pressure in theAttorney Docket No.: LAM1P068WO / 11940-1WO ampoule at the end of the first time period, wherein the starting pressure is lower than the ending pressure, and a determination, based on the pressure data, of the starting pressure, and the ending pressure, an amount of precursor in the mixture at the end of the first time period.

20. A method for semiconductor processing, the method comprising:(a) heating a precursor in an ampoule to a vapor state;(b) flowing, while heating the precursor in the ampoule, a carrier gas into the ampoule for a first time period and thereby pressurizing the ampoule and creating a mixture of the precursor and the carrier gas;(c) measuring, during (b), pressure data indicative of the pressure in the ampoule;(d) determining, based on the pressure data, a starting pressure in the ampoule at the start of the first time period and an ending pressure in the ampoule at the end of the first time period, wherein the starting pressure is lower than the ending pressure; and (e) determining, based on the pressure data, the starting pressure, and the ending pressure, an amount of precursor in the mixture at the end of the first time period.

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