Method and apparatus for precursor gas injection

Abstract

The present disclosure provides a gas injection system, which may include: a housing configured to accommodate a plurality of precursor storage tanks, the plurality of precursor storage tanks including one or more precursor materials; and a nozzle extending from the housing, the nozzle having a tip configured to be inserted into a sample chamber of a material processing apparatus. The precursor storage tanks are fluidly connected to the nozzle to selectively deliver one or more precursor gases into the sample chamber.

Description

[0001] Related Applications

[0002] This application claims the benefit and priority of U.S. Provisional Application No. 63 / 035,074, filed on Jun. 5, 2020, U.S. Provisional Application No. 62 / 885,795, filed on Aug. 12, 2019, and U.S. Utility Application No. 16 / 991,871, filed on Aug. 12, 2020, and the contents of these applications are hereby incorporated herein by reference in their entirety. Technical Field

[0003] The present disclosure generally relates to gas injection systems. Background Art

[0004] Among other uses, focused ion beam (FIB) systems, electron beam systems (such as scanning electron microscopes (SEM)), dual-beam FIB / SEM systems, and other laser beam-based systems are also used to deposit compounds on a sample surface by beam-induced deposition. Briefly, a precursor gas containing the desired compound or a gas composition capable of producing the desired compound through a chemical reaction is introduced into the sample chamber of the instrument, where the precursor gas undergoes decomposition or chemical reaction induced by the corresponding beam and deposits the desired compound on the sample surface. FIB, SEM, dual-beam FIB / SEM, and laser-based systems can utilize a gas injection system (GIS) to deliver the precursor gas into the sample chamber. Gas precursors are also used for gas-assisted etching (GAE) induced by ions, electrons, and laser beams.

[0005] Typically, it may be necessary to introduce different precursor gases during deposition or GAE processes. There is a need to provide a gas injection system that can handle multiple precursor gases, provide short switching times between precursors, is easy to set up, and requires minimal chemical handling. Summary of the Invention

[0006] The present disclosure relates to systems, methods, and devices related to gas injection systems. In some embodiments, a gas injection system may include: a housing configured to accommodate a plurality of precursor storage tanks, the plurality of precursor storage tanks including one or more precursor materials; and a nozzle extending from the housing, the nozzle having a tip configured to be inserted into a sample chamber of a material processing device. The precursor storage tanks are fluidly connected to the nozzle to selectively deliver one or more precursor gases into the sample chamber.

[0007] In some embodiments, the housing includes a plurality of reservoir housings configured to receive precursor reservoirs. Each reservoir housing may include an integrated valve to fluidly connect a precursor reservoir disposed within the reservoir housing to the nozzle. In some embodiments, the housing may form a vacuum envelope around the plurality of precursor reservoirs. In some embodiments, each of the plurality of reservoir housings includes one or more temperature control elements configured to operate independently of one or more heating elements associated with other reservoir housings to maintain each of the plurality of precursor reservoirs at a temperature selected for sublimating the precursor gas in the precursor gas reservoir.

[0008] In some embodiments, the plurality of precursor reservoirs are fluidly connected in series to one or more delivery lines that are in fluid communication with the nozzle and the sample chamber. In some embodiments, the system may further include a plurality of three-way valves to sequentially fluidly connect the plurality of precursor reservoirs to one or more delivery lines. In some embodiments, the one or more delivery lines are thermally controlled to prevent condensation of the precursor gas in the one or more delivery lines. In some embodiments, the one or more delivery lines are fluidly connected to one or more injection capillaries disposed in the nozzle for delivering the precursor gas into the sample chamber. The nozzle may include multiple injection capillaries for simultaneously injecting multiple precursors into the sample chamber. In some embodiments, the nozzle is configured to be maintained under a thermal gradient along the length of the nozzle. The temperature may increase towards the tip of the nozzle. In some embodiments, the nozzle and the housing are configured to form a vacuum envelope around the precursor reservoirs and the one or more delivery lines.

[0009] The present disclosure also relates to a method for delivering a plurality of precursor gases into a sample chamber of a materials processing apparatus. The method includes inserting a gas injection system into the materials processing apparatus. The gas injection system may include: a housing configured to accommodate a plurality of precursor reservoirs, the precursor reservoirs including one or more precursor materials; and a nozzle extending from the housing. The nozzle may have a tip configured to be inserted into the sample chamber, and the precursor reservoirs may be fluidly connected to the nozzle. The method further includes creating a vacuum in the housing around the plurality of precursor reservoirs, heating the plurality of gas precursor reservoirs individually to a temperature sufficient to generate one or more precursor gases from the one or more precursor materials, and selectively delivering the one or more precursor gases from the plurality of gas precursor reservoirs into the sample chamber.

[0010] In some embodiments, the method may further include heating the gas injection system to a temperature sufficient to prevent condensation of the one or more precursor gases and maintaining that temperature. In some embodiments, the nozzle is configured to be maintained under a thermal gradient along the length of the nozzle.

[0011] In some embodiments, the housing includes a plurality of reservoir housings configured to receive precursor reservoirs. Each reservoir housing may include an integrated valve to fluidly connect a precursor reservoir disposed within the reservoir housing to the nozzle. In some embodiments, the plurality of precursor reservoirs are fluidly connected in series to one or more delivery lines that are in fluid communication with the nozzle and the sample chamber. The system may further include a plurality of three-way valves to sequentially fluidly connect the plurality of precursor reservoirs to one or more delivery lines. In some embodiments, one or more of the delivery lines are thermally maintained to prevent condensation of precursor gases within the one or more delivery lines. The one or more delivery lines may be fluidly connected to one or more injection capillaries disposed within the nozzle for delivering precursor gases into the sample chamber. Description of the Drawings

[0012] Figure 1A is an exemplary embodiment of the gas injection system (GIS) of the present disclosure mounted on the main chamber of the instrument;

[0013] Figure 1B is an exemplary embodiment of the gas injection system of the present disclosure;

[0014] Figure 1C is an embodiment of the internal environment of a dual-beam FIB / SEM instrument, where the GIS is inserted and the gas release capillary is adjacent to the sample processing area;

[0015] Figure 1D is an embodiment of the internal environment of a dual-beam FIB / SEM instrument, where the GIS is retracted and the gas release capillary is kept at a safe distance from the sample processing area;

[0016] Figure 1E is an example of carbon material deposited by ion beam induced decomposition of volatile naphthalene delivered to the sample processing area by the GIS;

[0017] Figure 1F is a cross-sectional view of an example of platinum material deposited by ion beam and electron beam induced decomposition of an organometallic precursor delivered to the sample processing area by the GIS;

[0018] Figure 2 is an exemplary embodiment of the GIS body of the gas injection system of the present disclosure;

[0019] Figure 3A shows an exemplary reservoir housing with one reservoir inserted;

[0020] Figure 3B is a cross-sectional view of a reservoir suitable for the GIS system of the present disclosure;

[0021] Figure 4A and 4BShows an exemplary embodiment of a storage tank applicable to the GIS system of the present disclosure;

[0022] Figure 5A Shows an exemplary schematic diagram of a storage tank conduit system;

[0023] Figure 5B Shows an exemplary three-way valve suitable for use with the GIS system of the present disclosure;

[0024] Figure 6A Shows the cover of the GIS body with fittings for connecting a gas storage tank to a gas pipeline;

[0025] Figure 6B Shows the positions of the third storage tank with a precursor storage tank and the fourth storage tank with a precursor storage tank and a gas pipeline;

[0026] Figure 7A Shows an internal view of the GIS body of the present disclosure;

[0027] Figure 7B Shows the installation of a storage tank housing onto a PCB with an oversized hole;

[0028] Figure 8A and Figure 8B Shows an exemplary embodiment of a nozzle component;

[0029] Figure 8C-8H Shows a non-limiting example of a thermal management element of the nozzle;

[0030] Figure 8I Shows an exemplary nozzle alignment system;

[0031] Figure 9 Shows a cross-sectional view of an exemplary storage tank applicable to the GIS system of the present disclosure;

[0032] Figure 10 Shows an exemplary pneumatic actuation view of a storage tank applicable to the GIS system of the present disclosure;

[0033] Figure 11 Is an exemplary flowchart of the disclosed process;

[0034] Figure 12 Is an exemplary flowchart representing the controller state and logic flow in the ready and running states;

[0035] Figure 13 Is an exemplary flowchart representing the controller logic in the setup state;

[0036] Figure 14 Is an exemplary flowchart representing the controller logic in the service state; while

[0037] Figure 15 is an exemplary flowchart showing a user operation logic flowchart.

[0038] Although the above drawings illustrate the presently disclosed embodiments, as noted in the discussion, other embodiments are also conceivable. The present disclosure presents illustrative embodiments by way of representation and not limitation. Those skilled in the art can design many other modifications and embodiments that fall within the scope and spirit of the principles of the presently disclosed embodiments. Detailed Description

[0039] The purpose of the gas injection system (GIS) of the present disclosure is to enable the use of volatiles and improve the efficiency of sample processing by delivering a controlled amount of reactive substances for release near the sample processing area. According to some embodiments of the present disclosure, one or more chemical precursors can be delivered from a self-sealing precursor storage tank contained within an isolation envelope surrounding all internal components of the device. The flow rate and phase stability of these delivered precursors are managed by a temperature control element in thermal contact with the precursor storage tank housing through differential heating of the entire delivery path from the precursor source to the nozzle tip. The arrangement of the precursor storage tank ports, valves, common delivery lines, and evacuation ports supports continuous and efficient delivery, delivery line purging and cleaning, and continuous evacuation during idle periods.

[0040] In some embodiments, in the GIS of the present disclosure, multiple compatible precursor species can be loaded and held outside the sample chamber of the instrument through separate storage tanks at a given time, but still within the internal vacuum portion of the GIS body. Thus, the GIS of the present disclosure is capable of processing samples with different precursor species using a single gas injector, thereby eliminating the need for multiple GISs and eliminating the need for any adjustments when changing precursor materials. This makes it possible to replace an exhausted precursor storage tank on the GIS of the present disclosure without breaking into or entering the main sample chamber of an FIB, SEM, or similar instrument. In some embodiments, the GIS of the present disclosure provides continuous heating directly at the storage tank housing through thermal jackets at all points along the entire precursor flow path. By combining this continuous heating with heat measurements at the location furthest from the position of the heating element on the precursor storage tank, the integration of heating control and feedback loops can prevent downstream condensation and / or solidification of the precursor within the GIS due to cooling of the precursor. Independently heating each storage tank with chemical precursors can independently control the vapor pressure of each precursor, thus facilitating the regulation of the flow rate. In some embodiments, the design of the GIS of the present disclosure incorporates differential heating of the injection nozzle, where heaters are located near the tip and at the rear of the delivery line. This differential heating on these heating elements creates a temperature gradient along the delivery line, thereby preventing precursor condensation. Since all points along the delivery line are maintained at a temperature above the condensation temperature of the precursor material in the gas phase, this heating is beneficial for effectively removing residual precursors from within the pipe. In some embodiments, the GIS of the present disclosure has heating elements directly fixed to the precursor storage tank of the GIS to provide direct heating to the area, thereby making the heat transfer process more efficient and enabling rapid feedback control.

[0041] In some embodiments, the GIS of the present disclosure is configured to prevent precursor condensation within the delivery line and is thus suitable for precursors with low vapor pressures and precursors with significant vapor pressures, which may be in a solid, liquid, or gaseous state under ambient temperature conditions. In some embodiments, one or more temperature or thermal control elements, such as heaters, heat exchangers, heat spreaders, thermally conductive or insulating jackets, and other similar temperature control devices, are used to heat the control system to maintain the system at a desired temperature to prevent vapor condensation within the system. In some embodiments, the GIS of the present disclosure has a single nozzle that does not have segments extending at different angles and is thus capable of delivering multiple precursors without changing the position of the GIS or adjusting the ion beam or electron beam for processing the sample.

[0042] In some embodiments, the GIS of the present disclosure does not require a carrier gas for precursor delivery. The precursor flow from the storage tank to the injection capillary is facilitated by the vapor pressure of the precursor within the heated storage tank and is supported by the continuous heating of the flow path and the temperature gradient generated by differential heating along the delivery line within the nozzle. In some embodiments, the GIS of the present disclosure is configured with a three-way valve at each precursor storage tank such that when the valve is closed at the precursor storage tank, purging can be performed without additional valve actuation. The GIS of the present disclosure can also always provide a constant reverse pumping of the internal gas envelope and always provide a constant reverse pumping of the inactive portion of the gas delivery envelope while discharging into a dedicated evacuation port or the main chamber of the instrument when the precursor is not being ejected. In some embodiments, the GIS of the present disclosure is based on a continuous delivery path with three-way valves arranged in series, thereby completely eliminating the manifold and enabling rapid switching between precursors to reduce cross-contamination by continuous reverse pumping and then completely eliminating cross-contamination through a cleaning cycle with purging when necessary.

[0043] In some embodiments, the GIS of the present disclosure is configured such that all precursor species (typically in solid or liquid form) are contained within a vacuum envelope of the GIS body. In some embodiments, chemically active or inert gaseous species can also be ejected from outside the GIS housing through gas storage tanks and / or. The vacuum envelope serves as a safety enclosure for all precursors, providing isolation in the event of a leak in the precursor source and the components enclosed within the GIS body. In some embodiments, the precursor can be heated directly at the precursor storage tank and differentially heated along the gas line to the end of the nozzle to control the flow rate of precursor delivery without the need for any additional flow control devices. The continuous heating of the flow path and the thermal gradient along the delivery line of the GIS of the present disclosure can prevent condensation and / or solidification of the precursor downstream of the precursor source.

[0044] In some embodiments, the GIS of the present disclosure is configured to introduce precursor species into a sample processing space where the presence of a beam irradiation provides conditions for processing with or without the presence of additional activator chemicals. In some embodiments, the GIS of the present disclosure can be used with multiple precursor gases and in a large number of focused beam instruments.

[0045] In some embodiments, the GIS of the present disclosure provides continuous heating directly at the storage tank shell through thermal jackets at all points along the entire precursor flow path. By combining this continuous heating with heat measurements at the points furthest from the location of the heating elements on the precursor storage tank, the integration of heating control and feedback loops can prevent condensation and / or solidification of the precursor downstream within the GIS due to precursor cooling. Independent heating of each storage tank using chemical precursors enables independent control of the gas phase of each precursor, thus facilitating the regulation of flow rates. The design of the GIS of the present disclosure can incorporate differential heating of the nozzles, where heaters are located near the tip and at the rear of the delivery line. This differential heating on these heating elements creates a temperature gradient along the delivery line or conduit, thereby preventing precursor condensation. In some embodiments, all points along the delivery line are maintained at a temperature higher than that of any precursor storage tank, and this heating is beneficial for effectively removing residual precursors from within the tube. In some embodiments, the GIS of the present disclosure has heating elements directly fixed to the precursor storage tank or the storage tank shell of the GIS to provide direct heating to the area, thereby making the heat transfer process more efficient and enabling rapid feedback control. In some embodiments, this design can prevent precursor condensation within the delivery line and is thus suitable for precursors with low and significant vapor pressures, which can be solids, liquids, or gases under ambient temperature conditions.

[0046] In some embodiments, the GIS of the present disclosure does not require a carrier gas for precursor delivery. The flow of the precursor from the storage tank to the delivery line is facilitated by the vapor pressure of the precursor material within the heated storage tank and is supported by the continuous heating of the flow path and the temperature gradient generated by differential heating along the delivery line and the nozzle. The precursor material can be in solid or liquid form, or in gas form. In some embodiments, the GIS of the present disclosure is configured with a three-way valve at each precursor storage tank such that when the valve is closed at the precursor storage tank, purging can be performed without additional valve actuation. The GIS of the present disclosure can also always provide a constant reverse pumping of the internal gas envelope when the precursor is not being ejected and always provide a constant reverse pumping of the non-active part of the gas delivery envelope while discharging into a dedicated evacuation port or the main chamber of the instrument. The GIS designed according to the present disclosure is based on a continuous delivery path with three-way valves arranged in series, thereby completely eliminating the manifold and enabling rapid switching between precursors to reduce cross-contamination through continuous reverse pumping and then completely eliminating cross-contamination through a purge cycle when necessary.

[0047] All precursor species of the disclosed GIS (commonly in solid or liquid form) are contained within the vacuum envelope of the GIS body. The vacuum envelope can serve as a safety enclosure for all contained precursors, providing isolation in the event of a leak from the precursor source. In addition, the precursors are thermally controlled directly at the precursor storage tank and differentially heated along the gas line up to the nozzle tip to control the flow rate of precursor delivery without any additional flow control devices. Continuous heating of the flow path and the thermal gradient along the delivery line of the disclosed GIS can prevent condensation and / or solidification of the precursors downstream of the precursor source.

[0048] In some embodiments, the method of a gas-assisted process can include local activation of the spontaneous reaction between the precursor and the activator chemical on the sample surface, even after the beam irradiation is stopped, but the disclosed GIS is not limited to such a method of depositing or removing materials in any configuration. The precursor species can be introduced into the sample processing space, where the presence of beam irradiation provides the conditions for processing regardless of the presence of additional activator chemicals. In some embodiments, organometallic chemicals for ion beam deposition, such as methylated and / or ethylated metals (e.g., hexamethylditin), can be used to produce deposits with very low resistivity. In some embodiments, the disclosed GIS can utilize these precursors but is not limited to their use alone. Similarly, the disclosed GIS will be used in a large number of focused ion, electron, and laser beam instruments.

[0049] An exemplary embodiment of the GIS system 10 is shown in FIG. 1. In some embodiments, as Figure 1A shown, in the disclosed GIS, multiple chemically compatible precursor species are loaded into the GIS body 14 at a given time through independent storage tanks and are maintained outside the sample chamber 12 of a materials processing instrument (such as a scanning electron microscope (SEM)), a focused ion beam (FIB) instrument, a dual-beam FIB / SEM, a laser beam-based instrument, or a similar instrument), but still within the internal vacuum of the GIS body 14. Thus, the GIS of the present disclosure is capable of processing samples with different precursor species using a single gas injector that can be mounted on the sample chamber 12, eliminating the need for multiple GISs and the need for any adjustments when changing precursor materials. This allows for the replacement of an exhausted precursor storage tank on the disclosed GIS without breaking the vacuum or otherwise disturbing the environment in the main sample chamber of the FIB, SEM, or similar instrument. As Figure 1A shown, the GIS system 10 can also include electrical connectors 16 and pumping lines 18 to a controller.

[0050] The gas injection system of the present disclosure (e.g., as Figure 1B shown) is a complete multi-chemistry GIS. Figure 1BThe GIS system 10 shown in [description] includes a surrounding atmosphere portion 52 and an instrument chamber portion 54. For use, the device is installed on an instrument having an instrument chamber portion 54 housed within a sample chamber 12, and portion 52 is maintained outside the instrument, as Figure 1A shown.

[0051] The GIS system 10 also includes a GIS body 14 configured to house precursor storage tanks. In some embodiments, the GIS body 14 may have a cubic shape (aka "cube"), but may also have other shapes. The GIS body houses the internal components of the system, including multiple precursor storage tanks. Inside the sealed GIS body, chemical precursors are contained for safety and performance purposes. The sealing of the GIS body provides fail protection in the event of an accidental leak in any internal storage tank or conduit system. Since the GIS body is also maintained at a vacuum pressure, heat transfer from the storage tanks and conduit system is well isolated to achieve reliable temperature control. This vacuum insulation ensures that the GIS body remains at or near room temperature while heating the internal components. In some embodiments, the GIS body 14 is maintained under vacuum to correspond to the vacuum of the sample chamber 12. In some embodiments, the GIS body 14 is maintained under vacuum by a dedicated pump through a pumping line 18. Since the GIS housing is sealed to the sample chamber 12, the precursor storage tanks can be replaced when necessary without breaking the vacuum of the sample chamber 12 or disturbing the internal environment of the sample chamber 12.

[0052] In some embodiments, the GIS of the present disclosure has a single nozzle 20 for delivering multiple precursors from the GIS body 14. This enables the delivery of various precursors without changing the position of the GIS or without adjusting the ion beam or electron beam from an ion beam source 22 or an electron beam source 24 that processes the sample, as Figure 1C and 1D shown. Directing the precursors from a single nozzle eliminates the need to change the tip position of the nozzle 20 to direct different chemicals to the ion beam from the ion beam source 22 or the electron beam from the electron beam source 24 and the substrate material located on the sample processing area 26. Referring back to Figure 1F , the GIS system 10 may also include a nozzle adjustment knob 56 in the X direction and a nozzle adjustment knob 58 in the Y direction, which are capable of adjusting the position of the nozzle relative to the ion beam or electron beam.

[0053] During operation, the nozzle 20 of the GIS system 10 can be inserted into the sample chamber 12, and the GIS system 10 can be fixed in place using a mounting bracket 64. The nozzle 20 can move from the Figure 1D retracted position shown in [description] to the inserted position near the sample working area as shown in Figure 1C . The vacuum bellows 62 facilitates this movement while maintaining the integrity of the internal vacuum environment.

[0054] Figure 1E Shows an example of a carbon material 30, where the volatile naphthalene of the carbon material 30 transported by GIS to the sample processing area (substrate 32) is deposited by ion beam induced decomposition. Figure 1F A cross-sectional view showing an example of a platinum material 40 deposited by ion beam and a platinum material 42 deposited by electron beam induced decomposition of an organometallic precursor transported by GIS to the sample processing area. Once the device is inserted, GIS transports the precursor to the sample working area in the sample chamber for processing with a particle beam. The precursor delivery operations, including valve actuation, precursor selection, and GIS insertion, are all managed by the user through a controller and PC software.

[0055] As described above, the GIS body 14 is maintained under vacuum during the operation of the GIS system. The GIS body can be pumped down to a vacuum pressure in a variety of ways. In some embodiments, a nozzle that can reside in the sample chamber can be used. In some embodiments, when there is no active deposition of the precursor, the nozzle used to transport the precursor can also be used as an opening to evacuate the internal pipelines and volume of the GIS to the vacuum in the sample chamber. In some embodiments, one or more ports can be positioned on the GIS body, where pipelines can extend to the vacuum chamber of an external pump or instrument.

[0056] Reference Figure 2 , the GIS body 14 includes ports 80, 82 to which vacuum pipelines can be attached. The use or non-use of these ports can be configured in a variety of ways, depending on whether continuous back-pumping of the internal gas pipelines is required and which of the two pumping methods is selected. Briefly, if the GIS body 14 can be pumped into the main chamber of the SEM / FIB instrument and there is no back-pumping of the internal gas pipelines when all injection valves are closed, then the vacuum ports at the bottom of the GIS body will not be used. If the GIS body is pumped into the main chamber of the instrument and there is back-pumping of the internal gas pipelines when all injection valves are closed, then one vacuum port will be used at the bottom of the GIS body. If the GIS body is pumped through a separate vacuum pipeline and there is no back-pumping of the internal gas pipelines when all injection valves are closed, then one vacuum port will be used at the bottom of the GIS body. Finally, if the GIS body is pumped through a separate vacuum pipeline and there is back-pumping of the internal gas pipelines, then two vacuum ports will be used at the bottom of the GIS body.

[0057] As Figure 2 Further shown, a cylinder 84 is arranged on the GIS body 14, and the cylinder 84 can receive compressed gas for extending and retracting the nozzle at an adjustable speed.

[0058] The linear movement of the nozzle can be achieved with Figure 2It is controlled by the two cylinder actuators shown. In some embodiments, the air spring cylinder provides just enough force to overcome the atmospheric pressure acting on the device. This means that when the device is in its original position or when the compressed air line is damaged, the device will fully retract, thus protecting itself and other components from collision. During the operation point, the cylinder controls the extension and retraction of the nozzle at an adjustable speed. When the GIS is used for sample processing, the nozzle will be extended from the retracted position in the instrument chamber to the sample working area by the cylinder. After the GIS processing is completed, the GIS can be retracted through the same cylinder to vacate the working area around the sample and protect the instrument.

[0059] The GIS body may further include an insert linear guide 86 and a retract air spring 88 to assist the movement of the nozzle or the GIS housing relative to the instrument. The GIS body 14 also includes communication and power connection ports 89 to provide connection to a printed circuit board (PCB) that enables the electrical components of the GIS system 10 to operate. In some embodiments, fine adjustment of the insertion depth can be provided by adjusting the fixing screw 87 on the back of the air spring 88. In some embodiments, the air spring can only be compressed when its shaft is fully inserted and hard stopped. The position of the GIS body relative to the hard stop position of the air spring shaft can be adjusted by the fixing screw 87.

[0060] Reference Figure 3A and 3B , the storage tanks with chemical precursors are installed in a compact port array. In some embodiments, multiple storage tank ports 90a, 90b, 90c, 90d can be arranged on the base of the GIS body. Each port 90a, 90b, 90c, 90d may respectively include a storage tank housing 92a, 92b, 92c or 92d configured to receive the precursor storage tank 94. One or more temperature control devices 95 can be provided to evaporate the precursor. In some embodiments, the temperature control device 95 can be a resistive heater. In some embodiments, the temperature control device 95 can be a thermoelectric heat transfer element, such as a Peltier or other device. In some embodiments, the temperature control device can be located at the valve of each storage tank port. The system also includes one or more precursor flow and pumping ports 97 that fluidly connect the injection nozzle located in the sample chamber to the precursor storage tank to enable the precursor gas to be delivered into the sample chamber. The storage tank ports 90a - 90d are designed to facilitate storage tank replacement.

[0061] Figure 3B and 4A -4B provides an exemplary embodiment of a self-sealing storage tank. In some embodiments, such a storage tank assembly can be used for non-corrosive solid and liquid precursors. However, it should be noted that storage tanks with gaseous substances can also be used. As Figure 3BAs shown, the precursor storage tank includes a storage tank body 105, a storage tank base 108, and a precursor internal volume 110, which is designed to contain precursor materials. A body O-ring 107 can be provided to form a seal around the storage tank base 108. In some embodiments, the storage tank is delivered to the user together with a liquid or solid precursor material pre-loaded into the internal volume 110. The liquid or solid phase of the precursor material can be retained within the internal volume 110 by a gas-permeable barrier, which allows the gas phase of the precursor to be transferred. For example, a filter medium compatible with the precursor material can be used as the gas-permeable barrier.

[0062] In some embodiments, the storage tank 94 further includes a spring 100 held by a retaining bushing 101. When the spring 100 is compressed, the spring 100 is configured to exert pressure on a plunger 102, which in turn compresses an internal O-ring 106, effectively sealing the precursor within the internal volume 110 and the gas phase within the storage tank. When the storage tank is inserted into the storage tank housing, the plunger 102 contacts Figure 7B the storage tank valve actuator as shown. However, the storage tank remains sealed by the plunger 102 and the compressed O-ring 106. When the storage tank is fixed to the storage tank housing by one or more retaining screws, the threading acts to push the storage tank further into the storage tank housing. The storage tank valve actuator can be configured to act on the plunger 102 to overcome the force of the spring 100, moving the plunger 102 with the internal O-ring away from the storage tank body. At the same time, the O-ring contacts the bottom of the storage tank housing and is compressed by the act of fastening the storage tank to the storage tank housing, thereby forming a seal. Since the internal valve is opened by the reverse movement of the plunger and a seal is formed between the storage tank and the housing by compressing the O-ring, the gas phase of the precursor can be released into the sealed volume and reach the normally closed inlet of the three-way valve 112. The temperature of the storage tank can be set to a desired value by the action of a heater or a thermoelectric heat transfer device (e.g., arranged on the storage tank body), thereby generating the desired pressure of the gas phase of the precursor material. A control signal can be supplied to a flow control device, such as the three-way valve 112, to cause it to open and release the gas phase of the precursor material into the delivery line. The delivery line having a fluid connection to the capillary at the nozzle tip via a gas transfer tube transfers the gas phase of the precursor released from the capillary to the sample chamber.

[0063] Refer to Figure 5A , for a description of the configuration of the storage tank conduit system.

[0064] Multiple valves 112a, 112b, 112c, 112d can be provided to fluidly connect a precursor storage tank disposed in the storage tank housing ports 90a, 90b, 90c, and 90d to one or more delivery gas lines 111. The delivery gas line 111 fluidly connects the storage tank ports to a gas delivery line to deliver precursor gas to a nozzle and then to a sample chamber, and also allows for the evacuation or purging of precursor gas from within the line. By switching a series of valves 112a, 112b, 112c, 112d, the gas phase of the precursor from the precursor storage tank can flow from any one of the storage tanks into the delivery gas line 111 and downstream towards the nozzle. In some embodiments, valves 112a, 112b, 112c, 112d are three-way valves. Due to reverse pumping and / or purging through a common delivery line through a dedicated port on the GIS body or one of the storage tank ports, actuation of the three-way valve ensures either (1) the flow of precursor gas in the downstream delivery path towards the nozzle isolated from everything upstream or (2) reverse pumping of the entire delivery line and / or purging with a dedicated purge gas. In some embodiments, the delivery gas line 111 is maintained at a temperature that prevents condensation of the precursor in the delivery gas line 111. In some embodiments, at least some portions of the delivery gas line 111 include a thermally conductive sheath 113 surrounding the delivery gas line 111, which can maintain a desired temperature. Additionally or alternatively, one or more other heating or insulating elements can be employed to maintain the desired temperature of the delivery gas line 111.

[0065] Reference Figure 5B , in some embodiments, a suitable three-way valve 112 has three ports: a normally closed (NC) port 115; a switching port 116; and a normally open (NO) port. When the three-way valve is unactuated in its initial state, the NC port 115 is sealed while the NO port 117 is fluidly connected to the switching port 116. When the valve is actuated, the NO port 117 is sealed while the NC port is fluidly connected to the switching port 116, allowing the gas-phase precursor to flow downstream towards the injection capillary. When the valve is deactuated, it returns to its initial state where the NC port is sealed and the switching port is fluidly connected to the NO port in the upstream direction. Thus, in operation, the storage tank can be fluidly connected to the NC port, the delivery line for delivering the precursor downstream to the instrument can be connected to the switching port, and the upstream delivery line for exhaust / purging can be connected to the NO port. In this way, when the valve is unactuated, the common delivery gas line 111 can be reverse pumped, purged with compressed gas, or gaseous precursor can be delivered to the instrument from outside the GIS body. Additionally, the precursor storage tanks can be connected to or isolated from the delivery line by controlling the states of their respective three-way valves to deliver precursor gas to the instrument or to perform purging.

[0066] Reference Figure 6A and 6B, in some embodiments, to clean the delivery gas line 111 when switching precursor materials or as part of preventive maintenance, an additional port 120 is provided, for example, at the rear cover 122 of the GIS body to be connected to an external gas source or an exhaust pump. Inside the GIS body, the port 120 is fluidly connected to a gas storage tank 123, which can be installed within one of the gas storage tank housing ports. In some embodiments, the gas storage tank 123 can be connected to evacuate or purge the line through the last gas storage tank port. In that case, the pumping provided through port 120 first evacuates the gas storage tank and the gas storage tank housing port. When valve 112d is opened, the vacuum within the gas storage tank becomes fluidly connected and evacuates the gas lines connecting the fourth to the third, the third to the second, etc., and then pumps or purges the entire gas delivery, such as downstream of the injection capillary. Alternatively, gas can be supplied to the gas storage tank 123 through port 120. When the corresponding valve 112 is opened, the gas can purge the gas lines installed downstream of the gas storage tank ports of the gas storage tank 123. These reverse pumping and molecular scrubbing (purging) cleaning methods are fast and reliable. Compared with the traditional cleaning method of only heating and opening the nozzle, they can save a lot of time and be more effective. In some embodiments, port 120 can be used to introduce another gas precursor or reaction gas into the system during device operation.

[0067] When all valves 112a - 112d are switched to the closed position, reverse pumping for the common delivery gas line 111 is provided through a dedicated port 80 on the GIS body, which is fluidly connected to Figure 5A the exhaust / purge fitting in. As part of the purge cycle, compressed gas can be supplied through the same port to purge residual precursors from within the common delivery gas line 111. The series connection of the normally open ports of valves 112a - l12d forms a continuous path to evacuate or purge - clean the common delivery gas line 111 when switching precursor materials or as part of preventive maintenance.

[0068] It should be noted that while the precursor materials are typically evaporable solids or liquids, in some embodiments, chemically active or inert gaseous substances can also be injected through the gas storage tank and / or from outside the GIS housing. It should also be noted that in some embodiments, reverse pumping or purging of the entire gas pipeline can also be accomplished through the external port 80, which can be fluidly connected to the "exhaust / purge" fitting of the delivery gas pipeline 111. Alternatively, the exhaust / pump port can be connected to the main chamber of the instrument maintained at a vacuum pressure, or other vacuum volume. This pumping will function when all valves 112a, 112b, 112c, and 112d are closed. In some embodiments, reverse purging of the entire gas delivery system (including the piping system and gas pipelines) can be accomplished by supplying an inert or chemically inert gas to the exhaust / purge fitting when the exhaust / purge fitting is connected to the external pumping port 80.

[0069] In some embodiments, the heating process that controls the vapor pressure of the precursor is performed by temperature control means located at the valve at each storage tank port as shown Figure 3A . In some embodiments, the temperature control means is a resistive heater or a thermoelectric heat transfer element. Additionally, the system is designed such that the vaporized precursor does not condense in the gas pipeline when being delivered to the sample chamber. The temperature is measured by a sensor that can be mounted at the point on each storage tank housing 92 furthest from the heater (i.e., the top), as shown Figure 7A . By doing so, it is ensured that the entire precursor storage tank is heated to at least the measured temperature, which can be set above the sublimation point of the precursor to provide the desired vapor pressure. This, combined with the high vacuum within the GIS body, can help ensure stable vaporization and prevent condensation at or near the valve or on the back of each storage tank. In addition to utilizing the high vacuum within the GIS body to eliminate convective heat transfer, the delivery gas pipeline 111 connecting the storage tanks can be made of a resistant plastic and wrapped with a thermally conductive shield to mitigate heat loss due to radiative heat transfer in the delivery pipeline and reduce the risk of condensation in the pipeline. Naturally, the chemical substances with the lowest vaporization temperature can be placed upstream furthest from the nozzle as they may have a longer path to the nozzle. Referring to Figure 7B , a PCB mounted on the platform supporting the storage tank housing can also be provided to minimize heat transfer. The through-board channels can be large enough such that the heated components do not lose heat by conduction, and the board is laminated with a non-thermally conductive polymer (such as PEEK polymer). The storage tank housing can also be mechanically mounted by adiabatic brackets with low thermal conductivity.

[0070] Figure 7B Further shown is a storage tank valve actuator 132a disposed within the storage tank housing 92a and in communication with the three-way valve 112a. In operation, the storage tank valve actuator facilitates the fluid connection between the precursor reservoir of the storage tank and the three-way valve.

[0071] Reference Figure 8A-8I to describe the components of the nozzle 20. As described above, the nozzle 20 is connected to the GIS body to deliver precursor gas to the instrument. In some embodiments, the nozzle 20 is designed to maintain the temperature necessary to prevent vapor condensation within the nozzle. In some embodiments, the nozzle may include a set of metal tubes. Reference Figure 8A , the outer tube 131 houses the internal gas line 130, which is connected to the delivery gas line 111 to deliver precursor gas to the nozzle. In some embodiments, the internal gas line 130 is a stainless steel tube. One or more gas capillaries 136 may be provided at the end of the nozzle, in communication with the internal gas line 130 to deliver precursor gas into the sample chamber. In some embodiments, if the precursor gases can be mixed and delivered together, a single capillary may be used, while if it is desired to deliver the precursor gases separately, multiple capillaries may be used. It should also be noted that, as described above, multiple internal gas lines 130 may be employed.

[0072] In some embodiments, the temperature of the internal gas line can be maintained above the evaporation temperature of the precursor in the gas phase within the line, so that the vapor within the gas line does not condense. If multiple delivery lines are used, each line can be thermally controlled, but can be maintained at different temperatures depending on the nature of the precursor gas delivered through each gas line. In some embodiments, the internal gas line 130 may be surrounded by a thermally conductive sheath 133 to maintain the temperature of the internal gas line 130. The space between the internal gas line 130 / thermally conductive sheath 133 and the outer tube 131 may define a chamber, which may be under vacuum to remove convective heat transfer from the internal gas line 130. In some embodiments, additional insulation or heating may be added around the internal gas line 130.

[0073] Towards the end of the nozzle, the thermally conductive sheath 133 transitions to an external radiator 135 below the coupler 137, as Figure 8BAs shown. In some embodiments, the external radiator may be made of highly polished gold-plated copper. Additionally, the nozzle end of the thermally conductive sheath may be equipped with one or more heaters 134. For example, the first heater 134 may be located near the upstream end of the outer tube and may be made of thin film resistive material. In some embodiments, the heating element may be a heater, a heat exchanger, a thermally conductive sheath, or a radiator. Another heater 134 may be located downstream of the outer tube. In some embodiments, the heat dissipation difference between the nozzle heater and the heater for the storage tank housing may result in a temperature difference of several degrees, where the area of the conductive cap end is typically the hottest across the entire ejector. A slight temperature gradient, typically about 3 to 5 degrees Celsius, is beneficial for emitting thermal radiation starting from the end of the thermally conductive external radiator, thereby heating the ejection capillary and facilitating a stable flow of the gas phase without the risk of condensation at the nozzle exit. The highly polished surface of the radiator cap can also minimize radiative heat transfer to the chamber environment and the sample.

[0074] Further non-limiting examples of the thermal management elements of the nozzle are provided in Figure 8C-8E the following. Figure 8C The tip of the thermally conductive sheath protruding from the lower coupler is shown (the external radiator with the gas delivery line and the ejection capillary is not shown). Figure 8D The thermally conductive sheath / radiator is shown. The temperature control element or the thermal control element (e.g., heater 134) is wrapped around the gas line. Figure 8E The gas delivery line with the sheath is shown. An example of the heater on the thermally conductive sheath positioned within the nozzle is shown in Figure 8F-8H the following. Figure 8F The heater near the capillary end of the sheath is shown. The black substance is the heat shrink tube covering the actual heater. This end is inserted beneath the external radiator. Figure 8G The rear end of the sheath located on top of the gas delivery line, near the gas line connection point, is shown. The rear surface temperature control element (thin film resistor) is mounted. Figure 8H The rear end of the sheath with the temperature sensor attached is shown.

[0075] Refer to Figure 8I, the nozzle may be provided with alignment blocks 140 for adjusting the position of the nozzle within the sample chamber as described above. The alignment blocks may be located on the outer tube 131, and the internal gas line 130 may pass through the alignment blocks 140. The internal gas line 130 may be connected to a common gas line at the gas line connector 138. The alignment blocks 140 may include a setting rod 142 for adjusting the x-direction and a setting rod 144 for adjusting the y-direction of the nozzle. The alignment blocks may also include alignment springs 146 that bias the inner tube 138 towards the center of the alignment blocks. The extension depth can be fine-tuned by adjusting the corresponding set screws, and the overall movement has a hard stop on linear slide bearings. The controls above the lateral position of the nozzle are controlled by knobs 56 and 58 mounted on the housing. In some embodiments, the knobs drive rods into the alignment blocks 140 or the stainless-steel internal gas tube to overcome the resistance of the alignment springs 146 and move them. The rods 142, 144 interact with the inner tube at an upstream point before the O-ring connection portion of the stainless-steel internal gas tube. The force is applied away from the O-ring fulcrum, resulting in significant movement for a small change in the knob position. All-direction alignment has a typical repeatability of 5 microns. Figure 8C The upper coupler 148 of the nozzle is also shown.

[0076] Figure 9 and 10 Another embodiment of a storage tank suitable for the GIS system of the present disclosure is shown. In some embodiments, such a design may be associated with corrosive precursors (such as liquid bromine or solid iodine). Refer to Figure 9 , the storage tank for the corrosive precursor is shown within the storage tank housing. Such a storage tank 150 may have an internal structure similar to that of the Figure 3B and Figure 4A-4B shown storage tank for non-corrosive precursors. As Figure 9 shown, the liquid or solid precursor material may be placed within the internal volume of the precursor reservoir 152 and may be held there by a breathable membrane. The precursor may be sealed within the internal volume of the precursor reservoir 152 of the storage tank by a plunger O-ring 154 that is pushed towards the storage tank body 156 by a compressed internal spring 158.

[0077] The front portion of the corrosive precursor storage tank may include a spout inserted into a receiving channel within the storage tank housing. An airtight sliding seal is formed between the spout and the channel within the storage tank housing, thereby allowing the storage tank to move along the channel. The seal may be formed by an elastomeric X-O-ring 160 that is inserted into the channel within the storage tank housing and compressed between the nozzle and the channel within the storage tank seal.

[0078] Refer to Figure 10, the corrosive reservoir 150 can be positioned within the reservoir housing 168 such that its plunger 162 contacts the valve actuator pin 163. The force of one or more compressed reservoir retraction springs 164 and the internal spring of the reservoir prevent the reservoir body 156 from pushing against the valve actuator pin. As Figure 10 shown, the release of the precursor from within the reservoir 150 is achieved by the action of compressed air being injected through the compressed air inlet 170 into the expansion bellows 172. The internal pressure buildup within the bellows causes the bellows to expand in the axial direction of the reservoir. The expanding bellows can exert a force on the reservoir base 166, thereby overcoming the resistance of the reservoir retraction spring and the internal spring of the reservoir and causing the entire reservoir to move axially further into the reservoir housing 168. This axial movement can cause the valve actuator pin to cause the plunger to move away from the base of the reservoir body. This movement results in the pressure release of the plunger O-ring and the opening of the fluid connection between the internal volume of the reservoir and the reservoir housing, thereby releasing the precursor stream from the reservoir into the reservoir housing and further into the gas delivery line.

[0079] Referring Figure 11 , an exemplary process flow diagram is presented. In step 180, one or more precursor reservoirs are loaded into the gas injection system. The precursor reservoir is inserted into the reservoir housing of the GIS body. In step 182, a vacuum is formed within the GIS body to create a vacuum envelope around the reservoir. Next, the reservoir can be heated individually to evaporate the precursor material. Additionally, the system is heated to prevent condensation of the precursor gas within the system. In step 184, one or more selected valves are opened to allow the precursor gas to flow from the selected reservoir into the delivery line and into the nozzle and continue into the sample chamber. In step 186, the precursor gas or a mixture of precursor gases can be selectively delivered to the sample chamber by connecting or disconnecting various reservoirs to the delivery line. As the precursor gas is delivered to the sample chamber, the vacuum and temperature within the system are maintained. As described above, if necessary, the precursor reservoir can be switched by breaking the vacuum within the GIS body but not within the instrument. In step 188, the flow of the precursor gas is cut off and the system can be purged in step 190.

[0080] The present disclosure includes various embodiments of the above methods, systems, and components, as follows: In some embodiments, a multi-precursor gas injector installed on a FIB, SEM, or other instrument has its internal volume directly evacuated into the chamber of the instrument through a dedicated evacuation port or evacuation opening, thereby forming a vacuum envelope around all internal elements of the gas injector. In some embodiments, a storage tank containing a chemical precursor is completely enclosed within the vacuum envelope. In some embodiments, the vacuum envelope surrounding the storage tank with the precursor provides an auxiliary container for the chemical substance sealed within the storage tank. In some embodiments, the vacuum envelope surrounding the storage tank with the precursor serves as a thermal barrier to prevent heat transfer between the storage tanks and between each storage tank and other elements of the injector. In some embodiments, a storage tank containing a chemical precursor with an integrated valve remains closed during transportation and installation of the storage tank. When the storage tank is installed within the gas injector, the valve can be opened. In some embodiments, after the storage tank is installed, the integrated valve can be maintained in the open position, and the flow of the precursor from the storage tank is controlled by an additional shut-off valve in the storage tank housing or elsewhere. In some embodiments, the integrated valve within the storage tank is used to control the outflow of the precursor from the storage tank by mechanically actuating the position of the storage tank within the housing. In some embodiments, the valve integrated within the storage tank is used to control the flow of the precursor from the storage tank by mechanically actuating the valve while the storage tank remains in a fixed position within the housing. In some embodiments, the actuation of the valve position can be pneumatic, electromagnetic, electromechanical, piezoelectric, or other means. In some embodiments, the temperatures of the storage tanks, their housings, elements of the flow path, and other elements of the injector are maintained as needed at a temperature higher than, equal to, or lower than the ambient temperature to control the pressure of the precursor delivered from the storage tank and to prevent condensation of the precursor on the elements of the delivery system. In some embodiments, it can be maintained at a temperature higher than the ambient temperature by a heater in close mechanical and thermal contact with the storage tank or its housing. In some embodiments, higher than, equal to, and lower than the ambient temperature can be maintained by a heat transfer device such as a Peltier element, a heat exchanger, or other heat or temperature control / transfer elements in close mechanical and thermal contact with the storage tank or its housing. In some embodiments, the excess heat generated by the active heat transfer device is removed through close mechanical and thermal contact with the outer housing of the envelope, convective cooling, or through a heat exchanger through which a refrigerant flows. In some embodiments, inserts within the heat exchanger channels can be added to force the refrigerant to flow along the channel walls and to mix the refrigerant during flow to enhance the heat transfer efficiency within the heat exchanger. In some embodiments, it can be maintained at a temperature lower than the ambient temperature by a heat removal device in close mechanical and thermal contact with the storage tank or its housing, such as a heat exchanger through which a refrigerant flows. In some embodiments, a thermal feedback loop independently controls the temperature of all or each of a plurality of storage tanks containing chemical precursors within the same vacuum envelope. In some embodiments, the pressure of the precursor in the storage tank is regulated by controlling the temperature of the storage tank and its corresponding housing.In some embodiments, the chemical precursors are transported between storage tanks and reach the injection capillary through a piping system resistant to precursor attack. In some embodiments, the piping system for delivering chemicals is enclosed in a thermal sheath having conditions suitable for allowing the precursors to flow without condensation, decomposition, or other adverse effects on the transported materials. In some embodiments, the sheath can be rigid, such as made of aluminum, copper, or other metals with suitable thermal conductivity. In some embodiments, the sheath can be flexible or semi-flexible, such as made of copper or aluminum foil, coil fabric, mesh, tape, or heat-conductive rubber or flexible composite material with or without a metal core. In some embodiments, the temperature and thermal gradient on the sheath can be defined by the thermal conductivity of the sheath material physically connected to the temperature-controlled storage tank or housing. In some embodiments, the temperature and thermal gradient of the sheath can be controlled by independent heaters installed on the sheath along its length or at specific positions required to create a thermal gradient. The heaters of the sheath can operate at a fixed predetermined temperature or a feedback loop can be employed to control the temperature of the sheath. In some embodiments, the temperature and thermal gradient of the sheath can be generated and controlled by passing an electric current through the sheath. In some embodiments, compatible chemical precursors from different storage tanks are delivered to the instrument through a single injection capillary. In some embodiments, the connection of the compatible chemical precursors to the single injection capillary within the vacuum envelope is in series with a three-way injection valve on each precursor housing or through a parallel manifold. In some embodiments, in the manifold connection, the precursor housing can have a two-way switching valve to interrupt the precursor flow. In some embodiments, in the manifold connection, each precursor flow can be interrupted by a three-way valve. In some embodiments, when the flow of the precursor gas is interrupted, a purge gas can be injected into the manifold or the gas injection capillary to remove residual precursors. In some embodiments, the valves of the manifold and the series connection can be operated sequentially to inject multiple precursors or their mixtures through the capillary. In some embodiments, more than one capillary extending in parallel can be employed to simultaneously inject non-mixable precursors. In some embodiments, the injection capillary can release the precursor directly into the chamber of the instrument or allow the gas concentrator to create a virtual processing chamber near the sample surface. In some embodiments, the chemical precursors injected into the instrument through the delivery capillary can interact with the sample material maintained at a temperature above, equal to, or below the ambient temperature. In some embodiments, the temperature of the sample can be maintained above the ambient temperature by a resistive heater or a heat transfer device. The heat transfer device can be passive (such as a heat exchanger) or active (such as a Peltier or similar element). In some embodiments, excess heat is removed from the sample or the Peltier or other active heat transfer element that controls the sample temperature by flowing a heat transfer fluid or other medium through the internal channels of a heat exchanger in close mechanical and thermal contact with the sample or the heat transfer element.In some embodiments, the channels of the heat exchanger can include inserts that force the refrigerant to flow along the channel walls and mix the refrigerant during flow.

[0081] The following description and procedures present, as non-limiting examples, methods, systems, and apparatuses of the present disclosure.

[0082] The examples presented to aid in understanding the present disclosure should not be construed as limiting the scope of the present disclosure in any way as defined in the subsequent claims. The following embodiments are presented to provide a complete disclosure to a person of ordinary skill in the art and a description of how to make and use one embodiment of the present disclosure, and are not intended to limit the scope that the inventors regard as their invention, nor are they intended to represent that the following experiments are all or the only experiments conducted. Efforts have been made to ensure the accuracy of the numbers used (e.g., quantities, temperatures, etc.), but some experimental errors and deviations should be considered.

[0083] Example: Description of Controller States

[0084] Figure 12-15 Non-limiting embodiments of a flowchart of the system state are presented. Figure 12 Represents the controller states and logic flow in the ready and running states. Figure 13 Represents the controller logic in the setup state. Figure 14 Represents the controller logic in the service state. Figure 15 Represents the user operation logic flowchart.

[0085] As Figure 15 shown in the exemplary state flowchart, at startup, the system is in the "off" state, the GUIPC is connected to the controller, and the executable software is started. If the key is in the "setup" position when the system is powered on, the system will permanently be in the default "idle" state until the key is turned to the "run" position. Then, the system can be in a variable "idle" state. Once the system is in the "setup" mode, if the system moves to the "service" mode, the "enable" status button on the back of the controller can be pressed. In the next step, the system can be in the "service" state. If the key is switched from the "setup" state to the "run" state, the system will enter the "idle" state. Pressing the "enable" button can move the system into the "enabled" state. If all readbacks are within tolerance and the interlock is inactive for 10 seconds, the system enters the "ready" state. If one or more "inject / shutoff" buttons are open, the system enters the "run" state so that sample processing can begin.

[0086] There are various system changes that affect the system state.

[0087] 1. Uploading the executable software should reset the controller and put it into the "idle" state.

[0088] 2. The connection and disconnection of the GUIPC to and from the controller shall not cause the controller to reset, nor shall it in any way affect its operation.

[0089] 3. "Shutdown" state - power off, all injection valves closed, GIS insertion supply valve closed, GIS retracted. The controller can only switch from the "shutdown" state to the "idle" state. Enter the "shutdown" state from any other state by turning off the power of the controller.

[0090] 4. Regardless of the position of any button, key or switch, the "idle" state is entered when powered on. In the "idle" state, all injection valves are closed, the GIS is retracted, the heater and Peltier are disabled, the readback is "enabled", the GUI screen (if connected) is in read-only mode, and all buttons except the "Settings / Run" key on the front panel and the "Enable" button on the back of the controller are disabled. The controller can switch from the "idle" state to the "shutdown", "enabled" and "settings" states.

[0091] 5. Enter the "settings" state from the "idle" state by turning the "Settings / Run" key to the "Settings" position. If the key is in the "Settings" position when powered on, the controller must remain permanently in the "idle" state until the "Settings / Run" key is turned to the "Run" position. If the "Settings / Run" key is in the "Settings" position when entering the "idle" state, the key must be turned to "Run" and back to "Settings" to enter the "settings" state. In the "settings" state, the GUI functions are available in read / write mode and the setting parameters can be changed. All changes are saved to the non-volatile memory of the controller (flash memory, EPROM, etc.) and the text / configuration file on the GUIPC. All front panel buttons (except the "Settings / Run" key), valves, heaters, Peltier and insertion functions remain disabled. The controller can enter the "shutdown", "idle" and "service" states from the "settings" state.

[0092] 6. If the "Settings / Run" key is turned to the "Run" position, enter the "idle" state from the "settings" state.

[0093] 7. Enter the "Service" state from "Settings" by pressing the "Enable" button on the rear panel of the controller. If the "Enable" button has been pressed when entering the "Service" state, it must be released and pressed again to enter the "Service" state from the "Settings" state. When entering the "Service" state, the controller must read all current setting information stored in the non-volatile memory (flash memory, EPROM, etc.) of the controller. In the "Service" state, the insertion function is enabled to supply power to the heater and Peltier, and temperature feedback control is enabled. All GUI and front panel control buttons function in the "Service" state. The controller can enter the "Off" and "Idle" states from the "Service" state.

[0094] 8. In the "Service" state, interlocks and limit conditions are monitored. If an operation violates a safety condition, then (a) a GUI pop-up message should display: "The operation violates at least one safety limit and may be dangerous. Press 'Confirm' to continue the operation or 'Cancel' to return in the 'Service' state", and (b) the corresponding buttons on the controller should start flashing at a frequency of 2 Hz. Press "Confirm"

[0095] 9. Enter the "Idle" state from the "Service" state by turning the "Settings / Run" key to the "Run" position.

[0096] 10. Enter the "Enabled" state from the "Idle" state by pressing the "Enable" button on the rear panel of the controller. If the "Enable" button on the rear panel is pressed during the power-on process, it must be released and pressed again to enter the "Enabled" state from the "Idle" state. When entering the "Enabled" state, the controller must read all current setting information stored in the non-volatile memory (flash memory, EPROM, etc.) of the controller.

[0097] 11. In the "Enabled" state, the heater / Peltier is powered on, temperature and pressure readbacks are monitored, and interlock conditions are checked. As long as any enabled readback exceeds the tolerance or any enabled interlock condition is not met, the controller should remain in the "Enabled" state. In the "Enabled" state, the injection valve button on the GUI and the injection button on the front panel of the controller are disabled. In the "Enabled" state, only the retraction operation of the GIS is allowed. If the GIS is extended when the controller enters the "Enabled" state, it should remain in the extended position. The GIS can be retracted by pressing the corresponding button on the GUI or the front panel of the controller, but extension is disabled. The controller can enter the "Off", "Service", "Idle", and "Ready" states from the "Enabled" state.

[0098] 12. When at least one enabled readback exceeds the tolerance or at least one enabled interlock becomes active, transition from the "Ready" or "Running" state to the "Enabled" state. If the controller transitions from the "Running" or "Ready" state to the "Enabled" state, the GIS position does not change. If the controller transitions from the "Ready" or "Running" state to the "Enabled" state, all injection valves shall be closed and an error message corresponding to the reason for entering the "Enabled" state must be displayed.

[0099] 13. Transition from the "Enabled" state to the "Service" state by turning the "Set / Run" key to the "Set" position.

[0100] 14. When all readbacks are within the tolerance and the interlock has been inactive for at least 10 seconds, transition from the "Enabled" state to the "Ready" state.

[0101] 15. Transition from the "Ready" state to the "Service" state by turning the "Set / Run" key to the "Set" position.

[0102] 16. Transition from the "Ready" state to the "Running" state by pressing one or more "Inject / Off" buttons on the GUI or the front panel of the controller and opening the corresponding injection valves. The controller can transition from the "Running" state to the "Shutdown", "Service", "Ready", and "Enabled" states.

[0103] 17. Transition from the "Running" state to the "Service" state by turning the "Set / Run" key to the "Set" position. When transitioning from the "Running" state to the "Service" state, if any injection valve is open, then such valve shall remain open. If the GIS extends when transitioning from the "Running" state to the "Service" state, the GIS shall remain extended.

[0104] 18. Transition from the "Running" state to the "Ready" state by pressing the inject button on the GUI or the front panel of the controller and closing all injection valves.

[0105] 19. When one of the hardware limits of the temperature or pressure readback is exceeded or an abnormal hardware condition is detected, transition from the "Enabled", "Ready", or "Running" state to the "Idle" state.

[0106] Controller and GUI Behavior in the "Idle" and "Enabled" States

[0107] The following are various examples of state changes related to the "Idle" and "Enabled" states.

[0108] 1. The controller enters the "Idle" state after power-on: The controller is powered on, all injection valves are closed, the GIS is retracted, the heater / Peltier is disabled, and the readback and interlock indicators are "Enabled".

[0109] 2. When the controller is in the "Idle" state, the Set / Run key is in the "Run" position, and the GUI application is started and connected, the GUI screen is read-only: temperature, pressure, and status readback are displayed, but the control buttons on the GUI are disabled. The "Settings" function of the GUI is read-only: parameters can be read, but not modified or uploaded to the controller.

[0110] 3. When the controller is in the "Idle" state and the "Set / Run" key is in the "Run" position, all buttons on the controller are disabled.

[0111] 4. When the controller is in the "Idle" state, turning the "Set / Run" key to the "Settings" position causes the controller to enter the "Settings" state. After connecting to the GUI application, the "Settings" function of the GUI can be used for read / write: parameters can be changed and uploaded to the controller. In the "Settings" state, the injection valve button and the GIS insertion button on the GUI are disabled. Turning the Set / Run key to "Run" in the "Settings" state should close all valves, retract the GIS, and return the controller to the "Idle" state.

[0112] 5. When the controller is in the "Idle" state and the "Set / Run" key is in the "Settings" position, the physical buttons on the front panel of the controller are enabled in the "Service" state. Pressing and holding a physical button for 3 seconds or longer will cause the button to blink when released, and if the GUI is connected, a confirmation dialog box will pop up on the GUI. Regardless of the interlock and readback status, repeatedly pressing and holding the same button for 3 seconds or longer will open the corresponding valve and change the button indication on the GUI to "Open". The insertion of the GIS is also a two-stage 3-second press-and-hold operation. When a valve is open or the GIS is inserted, repeatedly pressing the same button at any time should close the valve or retract the GIS. When the controller is in the "Idle" state, turning the Set / Run key to the "Run" position should close all valves, retract the GIS, and return the controller to the "Idle" state.

[0113] 6. When the controller is in the "Idle" state and the Set / Run key is in the "Settings" position, the "Reset" button on the back of the controller is enabled. If the "Reset" button is pressed and held for 3 seconds or longer, the controller can switch to the "Service" state when the button is released.

[0114] 7. Turning the "Set / Run" key from the "Service" state to the "Run" position can switch the controller to the "Enabled" state or the "Ready" state.

[0115] 8. When the controller is in the "Service" state, the GUI buttons and the front panel controller buttons are operable in the "Service" state.

[0116] 9. When the controller is in the "Enabled" state, if the temperature and / or pressure readback exceeds the tolerance of any specific storage tank, the LED on the corresponding button of the controller shall blink, the "Temperature" and "Pressure" indicators next to the virtual buttons on the GUI shall turn red, and the "Ready" LED on the front panel of the controller shall blink. Once the temperature / pressure readback value is within the tolerance range, the LED in the corresponding button on the front panel shall turn off, and the "Temperature" and "Pressure" indicators next to the corresponding open / close buttons on the GUI shall turn green. If any other interlocks are enabled, the "Ready" LED on the front panel of the controller shall continue to blink. If all readbacks are within the tolerance range and no interlocks are enabled, the "Ready" LED turns "On" and the controller switches to the "Ready" state.

[0117] 10. If the controller is powered on and not connected to the GUI, the controller shall operate normally in the "Run" or "Setup" state using the setup information stored in the controller according to the "Setup / Run" key position and the front panel button controls. By turning the "Setup / Run" key to the "Setup" position, pressing the "Reset" button for more than 3 seconds, and waiting for the temperature and pressure readbacks of the storage tank with heating / cooling / Peltier control to enter the tolerance range, the normal operation of the controller should be able to start, and once all enabled interlocks are in the "Enabled" state, they can operate normally using the front panel buttons.

[0118] 11. If the controller loses its connection to the GUI while operating in the "Run" state, then it should continue to operate normally through the front panel button controls.

[0119] 12. If the controller loses its connection to the GUI while operating in the "Setup" state, it should close the injection valve and switch to the "Idle" state. Returning from the "Idle" state to "Enabled" is done by manually turning the Run / Setup key to the "Setup" position and pressing the "Reset" button for 3 seconds or longer. After checking that all temperature and pressure readbacks are within the tolerance range and no interlocks are enabled, return to the "Ready" state.

[0120] 13. If the GUI loses its connection to the controller, it should: (a) change the connection status message to "Lost", (b) stop drawing the graph, (c) remain operational in the view-only mode, and (d) keep checking the connection to the controller every few seconds.

[0121] 14. When the GUI software starts, it should display the connection status "Establishing" and check the connection to the controller. If there is no connection, it should display the connection status message "Lost" and remain operational in the view-only mode while checking the connection to the controller every few seconds.

[0122] 15. When the GUI software establishes a connection with the controller for the first time after the software starts, it should display the connection status "Verification", read the GIS type and setting values from the controller, and compare them with the values stored on the computer. If the GIS type and setting values are the same, the GUI should display the connection status "Connected" and operate normally. If the GIS type and setting values in the controller do not match the information stored in the PC GUI software, a message "GUI / Controller Mismatch" should be displayed and three options should be given: (a) Upload the configuration from the controller to the GUI; (b) Download the configuration from the GUI to the controller; (c) Compare the controller and GUI configurations. Options (a) and (b) should save the configurations of the controller and GUI as text files for future reference and continue, while (c) should open the two files in Notepad++ and start the "Compare" plugin.

[0123] Controller and GUI behavior in the "Ready" and "Running" states.

[0124] The following are various examples of status changes related to the "Ready" and "Running" states.

[0125] 1. In the "Ready" state, if (a) the GIS is extended, (b) the valve is closed, and (c) no other incompatible valves are open, left-clicking the GUI injection button or pressing the physical button on the front panel of the controller should open the corresponding valve. Opening the valve should (a) switch the LED in the physical button on the front panel of the controller to "On", (b) change the color of the GUI button from "Dim" to "Bright", and (c) change the word on the GUI from "Off" to "Inject".

[0126] 2. In the "Ready" state, when the injection valve is closed and the GIS is retracted, left-clicking the GUI injection button or pressing the physical injection button on the front panel of the controller should (a) pop up a dialog box containing the options (a) open the injection valve without extending the GIS, (b) extend the GIS and open the injection valve after extension, and (c) cancel the operation; (b) make the LED on the injection button and the LED on the extension button of the controller blink at a frequency of 2 Hz. Pressing the physical injection button on the front panel of the controller in this state should open the valve without extending the GIS and the pop-up dialog box should disappear, pressing the "Extend" button should extend the GIS and open the injection valve and the pop-up dialog box should disappear, pressing both buttons simultaneously should cancel the operation and the pop-up dialog box should disappear.

[0127] 3. In the "Ready" state, opening any injection valve should switch the controller from the "Ready" state to the "Inject" state.

[0128] 4. In the "Inject" state, closing all injection valves should switch the controller from the "Inject" state to the "Ready" state.

[0129] 5. In the "spray" state, a left click on the spray button of the GUI or pressing the physical button on the front panel of the controller corresponding to opening the spray valve shall close the valve. Closing the valve shall (a) switch the LED on the physical button on the front panel of the controller to "off", (b) change the color of the GUI button from "bright" to "dark", and (c) change the text of the GUI button from "spray" to "close".

[0130] 6. In the "ready" state, a left click on the "cold purge" button of the GUI shall perform a cold purge cycle. In the "spray" state, a left click on the "cold purge" button of the GUI is ignored.

[0131] 7. In the "spray" state, a left click on the "hot purge" button of the GUI shall perform a hot purge when the valve is closed. If multiple (compatible) spray valves are opened before or after pressing the "hot purge" button, the hot purge shall be performed when the last spray valve is closed, regardless of the order in which the spray valves are opened. In the "ready" state, pressing the "hot purge" button of the GUI is ignored.

[0132] 8. In the "ready" state, a left click on the "extend / retract" button of the GUI or pressing the physical "extend / retract" button on the front panel of the controller shall (a) if the GIS is retracted, extend the GIS, causing the LED on the "extend / retract" button to blink at a frequency of 0.5 Hz during extension and switch the LED to "on" when the GIS is extended, and (b) if the GIS is extended, retract the GIS, causing the LED on the "extend / retract" button to blink at a frequency of 0.5 Hz during retraction and switch the LED to "off" after the GIS is retracted.

[0133] 9. In the "spray" state, if the GIS is extended with at least one spray valve open, then a left click on the "extend / retract" button of the GUI or pressing the physical extend / retract button on the front panel of the controller shall (a) pop up a dialog with the following options: (a) retract the GIS without closing the spray valve, (b) close the spray valve first and then retract the GIS, (c) cancel the operation; (b) cause the LEDs on the physical "spray / close" buttons corresponding to the open valves and the "extend / retract" button on the front panel of the controller to blink at a frequency of 2 Hz. If the blinking "spray / close" button is pressed, the spray valve shall close, the GIS shall retract, and the dialog box shall disappear. If the blinking "extend / retract" button is pressed, the GIS shall retract without closing the spray valve, and the dialog box shall disappear. If both the blinking "spray / close" button and the blinking "extend / retract" button are pressed simultaneously, the operation shall be cancelled and the dialog box shall disappear.

[0134] 10. In the "spray" state where the GIS is retracted, pressing the GUI or the physical "extend / retract" button should extend the GIS, causing the LED on the "extend / retract" button to blink at a frequency of 0.5 Hz during extension and switching the LED to "on" when the GIS is extended.

[0135] Controller and GUI behavior in the "Settings" and "Service" states.

[0136] The following are various examples of state changes related to the "Settings" and "Service" states.

[0137] 1. When the controller is in the "Settings" or "Service" state, the front panel buttons operate in the "Service" mode: Holding a physical button for 3 seconds or longer will cause the button to blink when released and, if the GUI is connected, a confirmation dialog box will pop up on the GUI. Regardless of the interlock and readback status, repeatedly pressing and holding the same button for 3 seconds or longer will open the corresponding valve and change the button indication on the GUI to "open". The insertion of the GIS is also a two-stage 3-second press-and-hold operation. When the valve is open or the GIS is inserted, repeatedly pressing the same button for any period of time should close the valve or retract the GIS.

[0138] 2. When the controller is in the "Settings" or "Service" state and the GUI is connected, the "Settings" function of the GUI application can be used for read / write: Parameters can be changed and uploaded to the controller. In the "Settings" state, the spray valve button and the GIS insertion button on the GUI operate in the "Service" state: If the GUI button is pressed for 3 seconds or longer, releasing the button will open a pop-up dialog box to confirm opening the spray valve or extending the GIS. When the dialog is open, the corresponding button on the controller should start to blink rapidly. When confirmed, regardless of the readback and interlock, the valve should open and / or the GIS should extend; the light on the button should turn "on". When the valve is open or the GIS is inserted, repeatedly pressing the same button for any period of time should close the valve or retract the GIS; the light should return to its corresponding current state.

[0139] 3. When the controller is in the "Settings" or "Service" state, left-clicking on the "Cold Sweep" or "Hot Sweep" button on the GUI is performed in the same manner as in the "Ready" and "Spray" states.

[0140] Controller front panel button LEDs and indicators

[0141] The following are various examples of state changes related to making changes using the control panel.

[0142] 1. The Run / Service LED on the front panel is "off" in the "Idle" state, blinks at 0.5 Hz in the "Setup" and "Service" states, blinks at 1 Hz in the "Enabled" state, and is "on" in the "Ready" and "Inject" states.

[0143] 2. The "Ready" LED on the front panel blinks at 0.5 Hz in the "Idle" and "Setup" states, blinks at 1 Hz in the "Service" and "Enabled" states if one of the enabled readbacks is out of tolerance or one of the enabled interlocks is enabled, is "on" in the "Service" state if all enabled readbacks are within tolerance and no enabled interlocks are enabled, and is "on" in the "Ready" and "Inject" states.

[0144] 3. The LED in the GIS Extend / Retract button is "off" when the GIS is retracted, is "on" if the GIS is inserted, blinks at 0.5 Hz when the GIS is being inserted or retracted, blinks at 1 Hz if the GIS is in an "Error" state (i.e., neither inserted nor retracted or both inserted and retracted within a period exceeding the insertion / retraction time), and blinks at 2 Hz if an attempt is made to retract with one or more injection valves open and no confirmation is given.

[0145] 4. The LED in the "Inject / Off" button on the controller front panel is "on" when the valve is open, blinks at 0.5 Hz after holding for the first 3 seconds when opened in the "Service" or "Setup" mode, blinks at 1 Hz in the "Service" mode or "Enabled" mode if the temperature or pressure readback of the corresponding enabled tank is out of tolerance, blinks at 2 Hz if an attempt is made to open the valve in the "Ready" or "Inject" state with the GIS retracted and no confirmation is given, and is "off" at all other times.

[0146] Software Safety Features

[0147] The following are various examples of status changes related to safety features.

[0148] 1. All buttons are connected through a 100 mSec "debouncer" that will ignore button state changes shorter than 100 mSec;

[0149] 2. All interlocks are connected through a 100 mSec "debouncer" that will ignore button state changes shorter than 100 mSec;

[0150] 3. The temperature and pressure readings of the GUI graphics are "real-time" at the controller sampling rate, but tolerance compliance or non-compliance is "filtered" within 2 seconds.

[0151] 4. The "Enable" button must be in the "Released" state and then transition to the "Activated" state to switch the controller from the "Idle" state to the "Enabled" state or from the "Setup" state to the "Service" state.

[0152] 5. The "Setup" key must be in the "Run" position and transition to the "Setup" state to switch the controller from the "Idle" state to the "Setup" state, and from the "Enabled" or "Run" state to the "Service" state.

[0153] 6. All set parameters are stored in the controller. The actual parameters are read from the controller for display on the GUI.

[0154] 7. All calculations and decisions are made only within the controller; the GUI is only used as an indicator / monitor. All statuses and graphs are read from the controller for display on the GUI.

[0155] 8. The internal operations of the controller are performed in temperature and / or pressure A / D bits, with an allowable range of 0 to 1023. The conversion from bits to temperature and / or pressure units is only done in the GUI software on the PC for easy human reading.

[0156] 9. The internal operations for temperature control are performed in D / A bits, with an allowable range of 0 to 255.

[0157] Settings Function

[0158] The following describes when the controller is in the "Idle", "Enabled", "Ready", and "Inject" states, or if the GUI is disconnected from the controller, right-click on the corresponding GUI unit to open the following configuration pop-up window in read-only mode. When the controller is in the "Setup" or "Service" state and the GUI is connected to the controller, right-click on the corresponding GUI unit to open the following configuration pop-up window in read / write mode, and any changes are stored in the configuration file and uploaded to the controller.

[0159] 1. Temperature unit: K, C, F - applicable to all temperature settings and readings back; changing the unit should convert all set and read-back values.

[0160] 2. Pressure unit: Mbar, Torr, Pa - applicable to all pressure settings and readings back; changing the unit should convert all set and read-back values.

[0161] 3. Chamber vacuum HW interlock: E - Enabled; D - Disabled;

[0162] 4. Storage tank vacuum HW interlock: E - Enabled; D - Disabled;

[0163] 5. Insert HW interlock: E - Enabled; D - Disabled;

[0164] 6. Chamber Vacuum Degree Readback: A - Enabled; D - Disabled; Default is "D" (not used now)

[0165] a. Voltage - pressure gauge should be stored, and chart colors should be selectable

[0166] 7. Chamber Vacuum Degree Minimum Value: The lowest chamber vacuum degree for operation (only when readback is A)

[0167] 8. Chamber Vacuum Degree Maximum Value: The highest chamber vacuum degree for operation (only when readback is A)

[0168] 9. Nozzle Pressure Readback: A - Enabled; D - Disabled; Default is "D" (not used now)

[0169] a. Voltage - pressure gauge should be stored, and chart colors should be selectable

[0170] 10. Nozzle Pressure Minimum Value: The lowest nozzle pressure for operation (only when readback is A)

[0171] 11. Nozzle Pressure Maximum Value: The highest nozzle pressure for operation (only when readback is A)

[0172] 12. Settings for Three Kinds of Storage Tanks (H - Heating, C - Cooling, P - Peltier)

[0173] a. Minimum Readback Temperature; This is the definition of the thermistor range

[0174] b. Maximum Readback Temperature; This is the definition of the thermistor range

[0175] c. Voltage - Temperature (Thermistor Readback) Table

[0176] d. Overheat Limit: The maximum temperature for operation; This limit places the controller in the idle state and gives an error message

[0177] e. Overcool Limit: The minimum temperature for operation; This limit makes the controller enter the idle state and gives an error message

[0178] 13. Gas Settings for Four Precursors Storage Tanks:

[0179] a. Storage Tank ID - Read - only field

[0180] b. Gas: Precursors name or chemical formula "0" is disabled

[0181] c. Color: Define the color of the on - off button on the GUI and the color of the temperature chart

[0182] d. Storage Tank Type: H (Heating), C (Cooling), P (Peltier), A (Ambient)

[0183] e. Temperature Setpoint: Operating temperature

[0184] f. Temperature tolerance: Operating temperature range; default + / -1°C

[0185] g. Precursors pressure readback: A - Enabled; D - Disabled; default value is "D" (not used now)

[0186] i. Voltage-pressure gauge should be stored, and the chart color should be selectable

[0187] h. Precursors pressure minimum: The lowest nozzle pressure for operation (only when readback is A)

[0188] i. Precursors pressure maximum: The highest nozzle pressure for operation (only when readback is A)

[0189] j. Compatibility: IDs of storage tanks that can be opened simultaneously with the current storage tank

[0190] Open delay: The shortest time before the current storage tank can be opened after closing the injection valve on another storage tank; 0 seconds to 1000 seconds

[0191] l. Open purge skip delay: The shortest time to skip the open purge after closing the injection valve on another storage tank; 0 seconds to 1000 seconds

[0192] m. Open purge: Yes / No; If "Yes", a cold purge cycle is performed before opening the injection valve on the storage tank; if "No", there is no purge cycle

[0193] n. Open purge duration: 10 seconds to 1000 seconds. This setting overrides the duration in the cold purge cycle setting

[0194] o. Close purge: Hot / Cold / No; If "Hot" or "Cold", the corresponding purge cycle is performed after closing the storage tank; if "No", no purge cycle is performed

[0195] p. Close purge duration: 10 seconds to 1000 seconds. This setting overrides the duration in the hot purge cycle setting

[0196] q. Charge: Mass of the precursor charge, in grams

[0197] r. Consumption rate: Grams per second

[0198] s. "Reset" buttons for "Open time" and "Consumption" counters

[0199] 14. Stretch / Retract settings:

[0200] a. Stretch readback: 1 - Enabled high; 0 - Enabled low; D - Disabled

[0201] b. Retract readback: 1 - Enabled high; 0 - Enabled low; D - Disabled

[0202] c. Extension / retraction action timer, ranging from 1 second to 30 seconds, with a default value of 5 seconds

[0203] d. Extension cleaning duration (in seconds, "0" to disable); the time period for performing a cold cleaning cycle during GIS insertion. If both tank opening and extension cleaning are specified, the extension cleaning is performed first, followed by the tank opening cleaning

[0204] e. Retraction cleaning duration (in seconds, "0" to disable); the time period for performing a cold cleaning cycle during GIS retraction. If both tank closing cleaning and retraction cleaning are specified, the tank cleaning is performed first, followed by the retraction cleaning

[0205] 15. Nozzle settings:

[0206] a. Temperature color: Defines the color of the nozzle temperature map

[0207] b. Temperature set point: The operating temperature of the nozzle

[0208] c. Temperature tolerance: The operating temperature range; default is + / -1°C. If the nozzle temperature exceeds the tolerance, the tank valve will not open and the "Ready" indicator on the controller will flash

[0209] d. Minimum readback temperature; this is the thermistor range definition

[0210] e. Maximum readback temperature; this is the thermistor range definition

[0211] f. Voltage-temperature (thermistor readback) table

[0212] g. Overheat limit: The maximum temperature for operation; this limit places the controller in the idle state with an error message

[0213] h. Overcool limit: The minimum temperature for operation; this limit places the controller in the idle state with an error message

[0214] i. Nozzle pressure readback: A - Enabled; D - Disabled; default value is "D" (not used now)

[0215] i. The voltage-pressure table should be stored, and the chart color should be selectable

[0216] j. Nozzle pressure minimum: The lowest nozzle pressure for operation (only when the readback is A)

[0217] k. Nozzle pressure maximum: The highest nozzle pressure for operation (only when the readback is A) 16. Cold cleaning cycle settings:

[0218] a. Cleaning tank ID and type; default values are 4 and ambient

[0219] b. Delay: The time to delay opening the purge tank valve after closing the injection valve; 0 ms to 10,000 ms

[0220] c. Ejection: The time to open the purge tank injection valve during a cycle, 1 ms to 10,000 ms

[0221] d. Cycle: The time of a cycle, 1 ms to 10,000 ms. The injection valve closes after ejection until the end of the cycle. If ejection >= cycle, the injection valve remains open during the cycle.

[0222] e. Duration: The duration of the cold purge cycle after pressing the GUI button, 10 s to 1200 s

[0223] 17. Hot purge cycle settings:

[0224] a. Purge tank ID and type; default values are 4 and ambient

[0225] b. Lead: The time to delay closing the precursor injection valve before opening the purge tank injection valve for the first time, 1000 ms to 0 ms

[0226] c. Ejection: The time to open the purge tank valve during a cycle, 1 ms to 10,000 ms

[0227] d. Cycle: The time of a cycle, 1 ms to 10,000 ms. The valve closes after ejection until the end of the cycle. If ejection >= cycle, the valve remains open during the cycle

[0228] e. Duration: The duration of the hot purge cycle when pressing the GUI button, 10 s to 1200 ms

[0229] 18. Graphical and log settings:

[0230] a. The time interval for recording when one or more tank valves open. In this case, all enabled readbacks and statuses are recorded. 0.1 s, 1 s, 10 s.

[0231] b. The time interval for monitoring status changes of predefined parameters to record whether all tank valves are closed. 1 s, 10 s, 30 s

[0232] c. Readback parameter for checking when all tank valves close. Selected by radio button

[0233] d. Number of log files to retain or duration?

[0234] 19. Temperature PID settings (nozzle and each type of tank):

[0235] a. CV Est —— Voltage estimation constant

[0236] b. PID control window (0.1....5) x tolerance

[0237] c. PID update rate (milliseconds)

[0238] d. Smoothing constant (0 - not smoothed, 1 - ignore sensor)

[0239] e. I Lim —— Integration limit

[0240] f. P - Proportional gain

[0241] g. I - Integral gain

[0242] h. D - Derivative gain;

[0243] In view of the foregoing description, many modifications and alternative embodiments of the present disclosure will be apparent to those skilled in the art. Accordingly, the description should be construed as illustrative only and is for the purpose of teaching those skilled in the art the best mode for practicing the present disclosure. Without departing from the spirit of the present disclosure, details of the structure may vary widely and exclusive use of all modifications falling within the scope of the appended claims is reserved. In this specification, embodiments have been described in a manner that enables a clear and concise specification, but it is intended and will be understood that the embodiments may be combined or separated in various ways without departing from the scope of the present disclosure. It is intended to limit the present disclosure only to the extent required by the appended claims and applicable legal rules.

Claims

1. A gas injection system, comprising: a plurality of storage tank housings disposed within an outer housing and configured to receive a plurality of precursor storage tanks, the precursor storage tanks including one or more precursor materials, the plurality of storage tank housings configured to be heated such that one or more precursor gases are generated from the one or more precursor materials; a nozzle extending from the outer housing, the nozzle having an internal delivery line and a tip configured to be inserted into a sample chamber of a material processing device such that the internal delivery line of the nozzle is in fluid communication with the sample chamber; a delivery line in fluid communication with the plurality of precursor storage tanks and the internal delivery line to fluidly connect with the sample chamber, thereby delivering the one or more precursor gases generated from the one or more precursor materials to the sample chamber; a first heat conducting sheath disposed around the delivery line, the first heat conducting sheath extending from the plurality of storage tank housings to the nozzle such that the first heat conducting sheath is in thermal communication with the plurality of storage tank housings disposed within the outer housing; and a second heat conducting sheath disposed around the internal delivery line of the nozzle; the nozzle further includes an outer tube disposed around the second heat conducting sheath such that the space between the second heat conducting sheath and the outer tube defines a chamber under vacuum to remove convective heat transfer from the delivery line; the nozzle further includes an external radiator located at the tip of the nozzle, the external radiator being thermally coupled to the second heat conducting sheath; and the nozzle further includes a first heating element upstream of the outer tube and a second heating element downstream of the outer tube, the first heating element being associated with the second heat conducting sheath and the second heating element being associated with the external radiator, wherein, when the plurality of storage tank housings are heated to generate the one or more precursor gases, the heat dissipation differences of the first heating element and the second heating element of the nozzle and the plurality of storage tank housings and the heat conduction of the first heat conducting sheath and the second heat conducting sheath produce a thermal gradient along the delivery line to maintain the delivery line at a preselected temperature, thereby preventing condensation of the one or more precursor gases in the delivery line and the internal delivery line.

2. The gas injection system according to claim 1, wherein the outer housing forms a vacuum envelope around the plurality of precursor storage tanks, wherein the vacuum envelope is independent of the sample chamber to facilitate replacement of the plurality of precursor storage tanks in the outer housing while maintaining the vacuum in the sample chamber.

3. The gas injection system according to claim 1, wherein each of the plurality of storage tank housings includes an integrated valve to fluidly connect the plurality of precursor storage tanks disposed in the plurality of storage tank housings to the nozzle.

4. The gas injection system according to claim 1, wherein the plurality of precursor storage tanks are fluidly connected in series to the delivery line that is in fluid communication with the nozzle and the sample chamber.

5. The gas injection system according to claim 4 further includes a plurality of three-way valves to fluidly connect the plurality of precursor storage tanks to the delivery line in sequence.

6. The gas injection system according to claim 4, wherein the delivery line is thermally controlled to prevent condensation of the one or more precursor gases in the delivery line.

7. The gas injection system according to claim 4, wherein the delivery line is fluidly connected to one or more injection capillaries disposed in the nozzle for delivering the one or more precursor gases into the sample chamber.

8. The gas injection system according to claim 7, wherein the nozzle includes a plurality of injection capillaries for simultaneously injecting a plurality of precursors into the sample chamber.

9. The gas injection system according to claim 1, wherein each of the plurality of storage tank housings includes one or more temperature control elements configured to operate independently of one or more heating elements associated with other storage tank housings to maintain each of the plurality of precursor storage tanks at a temperature selected for sublimating the one or more precursor gases in the precursor gas storage tank.

10. The gas injection system according to claim 1, wherein the nozzle is configured to be maintained under a thermal gradient along the length of the nozzle.

11. The gas injection system according to claim 10, wherein the temperature increases towards the tip of the nozzle.

12. The gas injection system according to claim 4, wherein the nozzle and the plurality of storage tank housings are configured to form a vacuum envelope around the plurality of precursor storage tanks and the delivery line.

13. A method for delivering a plurality of precursor gases into a sample chamber of a materials processing apparatus, the method comprising: inserting a gas injection system into the materials processing apparatus, wherein the gas injection system includes: a housing configured to accommodate a plurality of precursor storage tanks containing one or more precursor materials; a nozzle extending from the housing, the nozzle having an internal delivery line and a tip configured to be inserted into the sample chamber, the plurality of precursor storage tanks being fluidly connected to the nozzle; a delivery line fluidly communicating with the plurality of precursor storage tanks and the nozzle to be fluidly connected to the sample chamber for delivering the plurality of precursor gases generated from the one or more precursor materials into the sample chamber; a first heat conducting sheath disposed around the delivery line, the first heat conducting sheath extending from the housing to the nozzle such that the first heat conducting sheath is in thermal communication with the housing, and a second heat conducting sheath disposed around the internal delivery line of the nozzle; the nozzle further includes an outer tube disposed around the second heat conducting sheath such that the space between the second heat conducting sheath and the outer tube defines a chamber under vacuum to remove convective heat transfer from the delivery line; the nozzle further includes an external radiator located at the tip of the nozzle, the external radiator being thermally coupled to the second heat conducting sheath; and The nozzle further includes a first heating element upstream of the outer tube and a second heating element downstream of the outer tube, the first heating element being associated with a second heat conducting sheath and the second heating element being associated with an external radiator. A vacuum is formed in the housing around the plurality of precursor storage tanks. The plurality of precursor storage tanks are individually heated to a temperature sufficient to generate one or more precursor gases from the one or more precursor materials; and One or more precursor gases are selectively delivered from the plurality of precursor storage tanks into the sample chamber.

14. The method according to claim 13, further comprising heating the gas injection system to and maintaining a temperature sufficient to prevent condensation of the one or more precursor gases.

15. The method according to claim 13, wherein the housing includes a plurality of storage tank housings configured to receive the plurality of precursor storage tanks.

16. The method according to claim 15, wherein each storage tank housing includes an integrated valve to fluidly connect the plurality of precursor storage tanks disposed in the storage tank housing to the nozzle.

17. The method according to claim 13, wherein the plurality of precursor storage tanks are fluidly connected in series to one or more delivery lines that are in fluid communication with the nozzle and the sample chamber.

18. The method according to claim 17, wherein the system further includes a plurality of three-way valves to sequentially fluidly connect the plurality of precursor storage tanks to the one or more delivery lines.

19. The method according to claim 18, wherein the delivery lines are thermally maintained to prevent condensation of the precursor gases in the delivery lines.

20. The method according to claim 18, wherein the delivery lines are fluidly connected to one or more injection capillaries disposed in the nozzle for delivering the plurality of precursor gases into the sample chamber.

21. The method according to claim 13, wherein the nozzle is configured to be maintained under a thermal gradient along the length of the nozzle.

22. The gas injection system according to claim 1, wherein the nozzle includes an internal delivery line such that the internal delivery line of the nozzle is in fluid communication with the delivery lines and the sample chamber.

23. The gas injection system according to claim 22, further comprising a second heat conducting sheath disposed around the internal delivery line of the nozzle.

24. The gas injection system according to claim 1, wherein the delivery lines include a single delivery line such that the plurality of precursor storage tanks are fluidly connected in series to the single delivery line to selectively deliver one or more precursor gases generated from the one or more precursor materials into the sample chamber.

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