Tungsten precursors and related methods

Abstract

The precursor includes a tungsten precursor and a carbon-containing material. The precursor includes less than 0.02 wt.% of the carbon-containing material, based on the total weight of the precursor. A method for purifying a tungsten precursor can include at least one of obtaining a source container including the tungsten precursor and the carbon-containing material, separating the tungsten precursor from at least a first portion of the carbon-containing material, recovering the precursor in a collection container, or any combination thereof.

Description

[Technical Field]

[0001] FIELD OF THE DISCLOSURE

[0001] This disclosure relates to the field of tungsten precursors and related methods, including, but not limited to, purification methods, methods for verifying impurity levels, and the like. [Background technology]

[0002]

[0002] The presence of impurities in precursors used in semiconductor manufacturing results in defects and undesirable variations. Current analytical techniques for measuring impurity levels are unable to detect or verify extremely low impurity levels. Summary of the Invention

[0003] Some embodiments of the present disclosure relate to precursors. In some embodiments, the precursor comprises a tungsten precursor. In some embodiments, the precursor comprises a carbon-containing material. In some embodiments, the precursor comprises less than 0.02 wt. % of the carbon-containing material, based on the total weight of the precursor, as measured by total carbon analysis using non-dispersive infrared detection.

[0004] Some embodiments relate to a method for purifying a tungsten precursor. In some embodiments, the method includes obtaining a source vessel containing a tungsten precursor and a carbon-containing material. In some embodiments, the method includes separating the tungsten precursor from at least a first portion of the carbon-containing material. In some embodiments, separating the tungsten precursor from at least the first portion of the carbon-containing material includes applying first conditions to the source vessel to produce a tungsten precursor vapor containing at least one of a first carbon-containing vapor, a first plurality of carbon-containing particles, or any combination thereof; removing the first portion of the carbon-containing material from the tungsten precursor vapor by at least one of flowing the tungsten precursor vapor through a filter to remove at least a portion of the first plurality of carbon-containing particles; and flowing the tungsten precursor vapor over an adsorbent to remove at least a portion of the first carbon-containing vapor, or any combination thereof. In some embodiments, the method includes flowing the tungsten precursor vapor to a collection vessel. In some embodiments, the method includes separating the tungsten precursor from at least a second portion of the carbon-containing material by at least one of applying second conditions to the collection vessel to produce a tungsten precursor condensate and a second carbon-containing vapor, removing at least a portion of the second carbon-containing vapor from the collection vessel, or any combination thereof. In some embodiments, the method includes recovering the precursor in the collection vessel. In some embodiments, the method includes verifying a low carbon content of the precursor present in the collection vessel.

[0005] Some embodiments relate to a method for verifying low impurity content. In some embodiments, the method includes obtaining a collection vessel containing a precursor. In some embodiments, the precursor includes a tungsten precursor. In some embodiments, the precursor includes a carbon-containing material. In some embodiments, the method includes removing a sample of the precursor from the collection vessel. In some embodiments, the method includes measuring the carbon content of the precursor to verify or not verify the low carbon content of the precursor. In some embodiments, the method includes removing at least a portion of the carbon-containing material from the precursor if the low carbon content of the precursor is not verified.

[0006]

[0006] Certain embodiments of the present disclosure are herein described, by way of example only, with reference to the accompanying drawings. Referring now in detail to the drawings, it is emphasized that the illustrated embodiments are exemplary and are intended for illustrative discussion of embodiments of the present disclosure. In this regard, when described in conjunction with the drawings, it will become apparent to those skilled in the art how embodiments of the present disclosure may be practiced. [Brief explanation of the drawings]

[0007] [Figure 1] 7 is a flowchart of a method for purifying a tungsten precursor, according to some embodiments. [Figure 2]

[0008] 1 is a flowchart of a method for separating a carbon-containing material from a tungsten precursor, according to some embodiments. [Figure 3]

[0009] 1 is a flowchart of a method for separating a carbon-containing material from a tungsten precursor, according to some embodiments. [Figure 4]

[0010] 1 is a flowchart of a method for separating a carbon-containing material from a tungsten precursor, according to some embodiments. [Figure 5]

[0011] 1 is a flowchart of a method for separating a carbon-containing material from a tungsten precursor, according to some embodiments. [Figure 6]

[0012] 1 is a flowchart of a method for verifying the carbon content of a tungsten precursor, according to some embodiments. [Figure 7]

[0013] FIG. 1 is a schematic diagram of a system for removing carbon-containing material from a precursor, according to some embodiments. DETAILED DESCRIPTION OF THE INVENTION

[0008]

[0014] Among the benefits and improvements disclosed, other objects and advantages of the present disclosure will become apparent from the following description taken in conjunction with the accompanying drawings. While detailed embodiments of the present disclosure are disclosed herein, it should be understood that the disclosed embodiments are merely exemplary of the present disclosure, which may be embodied in various forms. Moreover, the examples given of various embodiments of the present disclosure are illustrative rather than limiting.

[0009]

[0015] All prior patents and publications referenced herein are incorporated by reference in their entirety.

[0010]

[0016] Throughout this specification and claims, the following terms have the meanings expressly associated therewith unless the context clearly dictates otherwise. As used herein, the phrases "in one embodiment," "in an embodiment," and "in some embodiments" do not necessarily refer to the same embodiment, although they may. Additionally, as used herein, the phrases "in another embodiment" and "in some other embodiments" do not necessarily refer to different embodiments, although they may. It is intended that all embodiments of the present disclosure may be combined without departing from the scope or spirit of the disclosure.

[0011]

[0017] As used herein, the term "based on" is not exclusive and allows for the use of additional unrecited factors unless the context clearly indicates otherwise. Additionally, throughout this specification, the meanings of "a," "an," and "the" include plural references. The meaning of "in" includes "in" and "on."

[0012]

[0018] Some embodiments relate to precursors. The precursor may include a tungsten precursor and at least one impurity. In some embodiments, the tungsten precursor includes tungsten pentachloride (WC15). In some embodiments, the tungsten precursor includes tungsten hexachloride (WC16). In some embodiments, the tungsten precursor includes either WC15 or WC16. In some embodiments, the at least one impurity includes a carbonaceous material. In some embodiments, the carbonaceous material includes at least one of a volatile compound (e.g., a volatile carbonaceous material), a non-volatile compound (e.g., a non-volatile carbonaceous material), or any combination thereof. In some embodiments, the at least one impurity includes a chlorinated hydrocarbon. In some embodiments, the carbonaceous material includes at least one of a hydrocarbon polymer, a haloalkane, a haloalkene, a halocycloalkane, a halo-substituted arene, or any combination thereof. In some embodiments, the carbonaceous material includes a substituent (e.g., a functional group). In some embodiments, the carbonaceous material includes a volatile carbon species that is volatile under conditions for vaporizing the tungsten precursor. In some embodiments, the carbon-containing material includes entrapped specific carbon species (eg, species that are captured by a filter).In some embodiments, the at least one impurity is selected from the group consisting of dichloromethane, phosgene, 1,1-dichloroethane, chloroform, 1,2-dichloroethane, carbon tetrachloride, tetrachloroethylene, trichloroethylene, 1,3-dichloropropane, 1,2,3-trichloropropane, 1,2-dichloropropane, 1,1,2-trichloroethane, 1,1,2-trichloropropane, 1,2,2-trichloropropane, 1,1,2,3-tetrachloropropane, 1,2,2,3-tetrachloropropane, 1,1,2,2-tetrachloroethane, 2,2-dichloropropanoyl chloride, 1,3-dichloro-1-propane The chlorochloropropane may comprise at least one of 1,3,3-trichloro-1-propene, 1,2,3-trichloro-1-propene, 1,3-dichloro-2-methylenepropane, 1,4-dichlorobutane, 1,3-dichloro-2-butene, 1,1,3,3-tetrachloro-2-methylpropane, 1,1,2,3,3-pentachloropropane, 1,3-dichlorocyclopentane, 1,1,2,2,3,3-hexachloropropane, 1,2,3,4,5,5-hexanechloro-1,3-cyclopentadiene, trichlorocyclopentene, tetrachlorocyclopentene, pentachloronorbornene, or any combination thereof.

[0013]

[0019] The precursor may contain less than 0.05% by weight of carbon material, based on the total weight of the precursor, or any range or subrange therebetween. In some embodiments, the precursor may contain less than 0.02%, less than 0.019%, less than 0.018%, less than 0.017%, less than 0.016%, less than 0.015%, less than 0.014%, less than 0.013%, less than 0.012%, less than 0.011%, less than 0.010%, less than 0.009 ... has less than 0.08%, less than 0.007%, less than 0.006%, less than 0.005%, less than 0.004%, less than 0.003%, less than 0.002%, less than 0.001%, less than 0.0009%, less than 0.0008%, less than 0.0007%, less than 0.0006%, less than 0.0005%, less than 0.0004%, less than 0.0003%, less than 0.0002%, or less than 0.0001% carbon material.

[0014]

[0020] The precursor may contain from 0.0001% to 0.05% by weight of the carbon material, based on the total weight of the precursor, or any range or subrange therebetween. In some embodiments, the precursor has a carbon content of 0.0001% to 0.02%, 0.0001% to 0.019%, 0.0001% to 0.018%, 0.0001% to 0.017%, 0.0001% to 0.016%, 0.0001% to 0.015%, 0.0001% to 0.014%, 0.0001% to 0.013%, 0.0001% to 0.012%, 0.0001% to 0.011%, 0.0001% to 0.010%, 0.0001% to 0.009%, 0.0001% to 0.016%, 0.0001% to 0.017%, 0.0001% to 0.018%, 0.0001% to 0.019 ... .008%, 0.0001%~0.007%, 0.0001%~0.006%, 0.0001%~0.005%, 0.0001%~0.004%, 0.0001%~0.003%, 0.0001%~0.002%, 0.0001%~0.001%, 0.0002%~0.015%, 0.0003%~0.015%, 0.0004%~0.015%, 0.0005%~0.015%, 0.0006%~0.015%, 0.0007%~0.015%, 0.0008%~0.015%, 0.0009%~0.015%, 0. 001%~0.015%, 0.0011%~0.015%, 0.0012%~0.015%, 0.0013%~0.015%, 0.0014%~0.015%, 0.0002%~0.001%, 0.0003%~0.001%, 0.0004%~0.001%, 0.0005%~0.001%, 0.0006%~0.001%, 0.0007%~0.001%, 0.0008%~0.001%, 0.0009%~0.001%, 0.0002%~0.0009%, 0.0002%~0.0008%, 0.0002%~ 0.0007%, 0.0002%~0.0006%, 0.0002%~0.0005%, 0.0002%~0.0004%, 0.0002%~0.0003%, 0.005%~0.015%, 0.006%~0.015%, 0.007%~0.015%, 0.008%~0.015%, 0.009%~0.015%, 0.01%~0.015%, 0.012%~0.015%, 0.013%~0.015%, 0.014%~0.015%, 0.006%~0.014%, 0.006%~0.0.013%, 0.006% to 0.012%, 0.006% to 0.011%, 0.006% to 0.01%, 0.006% to 0.009%, 0.006% to 0.008%, or 0.006% to 0.007%.

[0015]

[0021] Some embodiments relate to methods for purifying tungsten precursors. Various embodiments of methods for purifying tungsten precursors are provided herein. It will be understood that any combination of steps can be performed in any order in a method for purifying a tungsten precursor without departing from the scope of the present disclosure. Thus, the depiction of various methods and their steps in different figures is not limiting, and any combination of steps in any of the figures disclosed herein can be performed in any combination without departing from the scope of the present disclosure.

[0016]

[0022] 1 is a flowchart of a method 100 for purifying a tungsten precursor, according to some embodiments. As shown in FIG. 1, the method 100 for purifying a tungsten precursor can include at least one of the following steps: obtaining a source container containing a tungsten precursor and a carbon-containing material in step 102; separating the tungsten precursor from at least a first portion of the carbon-containing material in step 104; separating the tungsten precursor from at least a second portion of the carbon-containing material in step 106; separating the tungsten precursor from a third portion of the carbon-containing material in step 108; separating the tungsten precursor from a fourth portion of the carbon-containing material in step 110; collecting the precursor in a collection container in step 112; verifying the low carbon content of the precursor present in the collection container in step 114; or any combination thereof.

[0017]

[0023] In step 102, in some embodiments, a source vessel containing a tungsten precursor and a carbon-containing material is obtained. The tungsten precursor can be present in the source vessel in at least one of the following forms: a solid, a gas / vapor, or any combination thereof. For example, in some embodiments, the tungsten precursor exists as a solid and as a vapor. In some embodiments, the solid phase of the tungsten precursor is amorphous or crystalline. In some embodiments, the tungsten precursor exists as isolated crystals. The carbon-containing material can be present in the source vessel in at least one of the following forms: a solid, a liquid, a gas / vapor, or any combination thereof. In some embodiments, the carbon-containing material comprises at least one of a carbon-containing vapor, a plurality of carbon-containing particles, or any combination thereof. In some embodiments, the carbon-containing material comprises a volatile carbon material. In some embodiments, the carbon-containing material comprises a chlorinated hydrocarbon. In some embodiments, the carbon-containing material is selected from the group consisting of dichloromethane, phosgene, 1,1-dichloroethane, chloroform, 1,2-dichloroethane, carbon tetrachloride, tetrachloroethylene, trichloroethylene, 1,3-dichloropropane, 1,2,3-trichloropropane, 1,2-dichloropropane, 1,1,2-trichloroethane, 1,1,2-trichloropropane, 1,2,2-trichloropropane, 1,1,2,3-tetrachloropropane, 1,2,2,3-tetrachloropropane, 1,1,2,2-tetrachloroethane, 2,2-dichloropropanoyl chloride, 1,3-dichloro-1-propene , 3,3,3-trichloro-1-propene, 1,2,3-trichloro-1-propene, 1,3-dichloro-2-methylenepropane, 1,4-dichlorobutane, 1,3-dichloro-2-butene, 1,1,3,3-tetrachloro-2-methylpropane, 1,1,2,3,3-pentachloropropane, 1,3-dichlorocyclopentane, 1,1,2,2,3,3-hexachloropropane, 1,2,3,4,5,5-hexanechloro-1,3-cyclopentadiene, trichlorocyclopentene, tetrachlorocyclopentene, pentachloronorbornene, or any combination thereof. In some embodiments, the carbon-containing material is present as a solid or as a vapor.In some embodiments, the solid phase of the carbon-containing material is amorphous or crystalline. In some embodiments, the carbon-containing material is present in the source container as isolated crystals. In some embodiments, the carbon-containing material is present within the crystal lattice of the tungsten precursor. For example, in some embodiments, the carbon-containing material is dissolved in the crystal lattice of the tungsten precursor.

[0018]

[0024] The source container can be configured to control its temperature. The temperature of the source container can be controlled in any suitable manner. In some embodiments, a thermal jacket for heating and / or cooling is employed around the source container. In some embodiments, a ribbon heater is wrapped around the source container. In some embodiments, a block heater shaped to cover at least a major portion of the exterior surface of the source container is used to heat the source container. In some embodiments, a resistance heater is used to heat the source container. In some embodiments, a lamp heater is used to heat the source container. In some embodiments, a hot heat transfer fluid can be contacted with the exterior surface of the source container to heat and / or cool the source container. In some embodiments, heating is achieved by infrared or other radiant energy impinging on the source container. In some embodiments, the collection container is cooled by a fluid, a fan, a direct thermoelectric device, or any combination thereof. It will be understood that other heating and / or cooling devices and assemblies, and other configurations and arrangements of heaters and / or coolers, can be employed in the present invention without departing from the scope of this disclosure.

[0019]

[0025] The source vessel may be configured to control pressure. The pressure of the source vessel can be controlled in any suitable manner. In some embodiments, a gas inlet line is fluidly coupled to the source vessel. The gas inlet line can be configured to supply pressurized gas from a pressurized gas source to the source vessel. Control of the pressurized gas to the source vessel can be achieved by at least one of a pressure regulator, a needle valve, a mass flow controller, a downstream pressure controller, or any combination thereof. In some embodiments, the pressurized gas comprises an inert gas. In some embodiments, the inert gas comprises at least one of helium, argon, nitrogen, or any combination thereof. In some embodiments, a vacuum line is fluidly coupled to the source vessel. The vacuum line can be configured to apply a vacuum to the source vessel. In some embodiments, the pumping rate is controlled by a butterfly valve. It will be appreciated that other mechanisms for controlling the pressure of the source vessel can be employed in the present invention without departing from the scope of the present invention.

[0020]

[0026] In step 104, the tungsten precursor is separated from at least a first portion of the carbon-containing material. As disclosed herein (e.g., in FIG. 2 ), in some embodiments, the tungsten precursor can be separated from the first portion of the carbon-containing material by applying first conditions (e.g., at least one of temperature, pressure, inert gas flow, vacuum, or any combination thereof) to the source vessel to generate a tungsten precursor vapor containing the carbon-containing material. In some embodiments, the carbon-containing material comprises at least one of a carbon-containing vapor, a first plurality of carbon-containing particles, or any combination thereof. In some embodiments, the first condition is a condition in which the total pressure of the source vessel is below the true vapor pressure of the tungsten precursor for a given first temperature. In some embodiments, the first condition is a condition in which the total pressure of the source vessel is below the true vapor pressure of the carbon-containing material at a given first temperature. In some embodiments, the tungsten precursor can be separated from the first portion of the carbon-containing material by removing the first portion of the carbon-containing material from the tungsten precursor vapor. In some embodiments, the removing step includes flowing the tungsten precursor vapor through a filter to remove at least a portion of the first plurality of carbon-containing particles. In some embodiments, the removing step includes flowing the tungsten precursor vapor over an adsorbent to remove at least a portion of the first carbon-containing vapor. In some embodiments, the tungsten precursor can be separated from the first portion of the carbon-containing material by flowing the tungsten precursor vapor into a collection vessel.

[0021]

[0027] The filter may include a filter or filtration medium suitable for removing carbon-containing particles from the tungsten precursor vapor. In some embodiments, the filter includes at least one of wool, glass wool (e.g., glass wool made from at least one of quartz, glass, or borosilicate), sintered metal, fritted glass, sintered glass, resin, porous polymer, ceramic, cyclone material, electrostatic material, fibrous metal filter, or any combination thereof. In some embodiments, the filter includes at least one of perfluoroalkoxyalkane (PFA), polytetrafluoroethylene (PTFE), polypropylene, polyethylene, fibrous polymer, any copolymer thereof, or any combination thereof.

[0022]

[0028] The sorbent may comprise a material suitable for removing carbon-containing vapors from the tungsten precursor vapor. In some embodiments, the sorbent comprises an absorbent. In some embodiments, the sorbent comprises an adsorbent. In some embodiments, the sorbent comprises at least one of activated carbon, alumina, aluminosilicate, zeolite, silica, polymer, metal organic framework, alkali oxide, metal oxide, graphite felt, or any combination thereof.

[0023]

[0029] The collection container can be configured to control its temperature. The temperature of the collection container can be controlled in any suitable manner. In some embodiments, a thermal jacket for heating and / or cooling is employed around the collection container. In some embodiments, a ribbon heater is wrapped around the collection container. In some embodiments, a block heater shaped to cover at least a major portion of the exterior surface of the collection container is used to heat the collection container. In some embodiments, a resistance heater is used to heat the collection container. In some embodiments, a lamp heater is used to heat the collection container. In some embodiments, a hot heat transfer fluid can be contacted with the exterior surface of the collection container to heat and / or cool the collection container. In some embodiments, heating is achieved by infrared or other radiant energy impinging on the collection container. In some embodiments, the collection container is cooled by a fluid, a fan, a direct thermoelectric device, or any combination thereof. It will be understood that other heating and / or cooling devices and assemblies, and other configurations and arrangements of heaters and / or coolers, can be employed in the present invention without departing from the scope of this disclosure.

[0024]

[0030] The collection vessel can be configured to control pressure. The pressure of the collection vessel can be controlled in any suitable manner. In some embodiments, a gas inlet line is fluidly coupled to the collection vessel. The gas inlet line can be configured to supply pressurized gas to the collection vessel from a pressurized gas source. Control of the pressurized gas to the collection vessel can be achieved by at least one of a pressure regulator, a needle valve, a mass flow controller, a downstream pressure controller, or any combination thereof. In some embodiments, the pressurized gas comprises an inert gas. In some embodiments, the inert gas comprises at least one of helium, argon, nitrogen, or any combination thereof. In some embodiments, a vacuum line is fluidly coupled to the collection vessel. The vacuum line can be configured to apply a vacuum to the collection vessel. In some embodiments, the pumping rate is controlled by a butterfly valve. It will be appreciated that other mechanisms for controlling the pressure of the source vessel can be employed in the present invention without departing from the scope of the present invention.

[0025]

[0031] In step 106, the tungsten precursor is separated from at least a second portion of the carbon-containing material. As disclosed herein (e.g., FIG. 3 ), in some embodiments, the tungsten precursor can be separated from at least a second portion of the carbon-containing material by applying second conditions (e.g., at least one of temperature, pressure, inert gas flow, vacuum, or any combination thereof) to the collection vessel to produce a tungsten precursor condensate and a second carbon-containing vapor. In some embodiments, the tungsten precursor can be separated from at least a second portion of the carbon-containing material by removing at least a portion of the second carbon-containing vapor from the collection vessel. In some embodiments, the second conditions are conditions that result in a greater volume of tungsten precursor condensing than the second carbon-containing vapor. In some embodiments, when the second conditions are applied, the tungsten precursor condensate comprises a greater mole fraction of tungsten precursor than the carbon-containing material.

[0026]

[0032] In step 108, in some embodiments, the tungsten precursor is separated from the third portion of the carbon-containing material. As disclosed herein (e.g., FIG. 4 ), in some embodiments, the tungsten precursor can be separated from the third portion of the carbon-containing material by applying a third condition (e.g., at least one of temperature, pressure, inert gas flow, vacuum, or any combination thereof) to the source vessel to produce a third carbon-containing vapor. In some embodiments, the tungsten precursor can be separated from the third portion of the carbon-containing material by removing at least a portion of the third carbon-containing vapor from the source vessel. In some embodiments, step 108 is performed before step 104. In some embodiments, the third condition is a condition in which the total pressure of the source vessel is below the true vapor pressure of the carbon-containing material at a given third temperature. In some embodiments, the third condition is a condition in which the total pressure of the source vessel is above the true vapor pressure of the tungsten precursor at a given third temperature. In some embodiments, when the third condition is applied, the third carbon-containing vapor contains a larger volume of carbon-containing material than the tungsten precursor.

[0027]

[0033] In step 110, in some embodiments, the tungsten precursor is separated from the fourth portion of the carbon-containing material. As disclosed herein (e.g., FIG. 5 ), in some embodiments, the tungsten precursor can be separated from the fourth portion of the carbon-containing material by applying a fourth condition (e.g., at least one of temperature, pressure, inert gas flow, vacuum, or any combination thereof) to the collection vessel to produce a fourth carbon-containing vapor. In some embodiments, the tungsten precursor can be separated from the fourth portion of the carbon-containing material by removing at least a portion of the fourth carbon-containing vapor from the collection vessel. In some embodiments, step 110 is performed after step 114, described below. In some embodiments, the fourth condition is a condition in which the total pressure of the collection vessel is below the true vapor pressure of the carbon-containing material at a given fourth temperature. In some embodiments, the fourth condition is a condition in which the total pressure of the collection vessel is above the true vapor pressure of the tungsten precursor at a given fourth temperature. In some embodiments, when the fourth condition applies, the fourth carbon-containing vapor comprises a greater volume of carbon-containing material than the tungsten precursor.

[0028]

[0034] In step 112, in some embodiments, the precursor is collected in a collection vessel. In some embodiments, the precursor includes a tungsten precursor and a carbon-containing material. In some embodiments, the precursor includes less than 0.02 wt. % of the carbon-containing material, based on the total weight of the precursor, as measured by total carbon analysis using non-dispersive infrared detection. In some embodiments, the carbon-containing material includes a chlorinated hydrocarbon. In some embodiments, the carbon-containing material is selected from the group consisting of dichloromethane, phosgene, 1,1-dichloroethane, chloroform, 1,2-dichloroethane, carbon tetrachloride, tetrachloroethylene, trichloroethylene, 1,3-dichloropropane, 1,2,3-trichloropropane, 1,2-dichloropropane, 1,1,2-trichloroethane, 1,1,2-trichloropropane, 1,2,2-trichloropropane, 1,1,2,3-tetrachloropropane, 1,2,2,3-tetrachloropropane, 1,1,2,2-tetrachloroethane, 2,2-dichloropropanoyl chloride, 1,3-dichloro-1-propene , 3,3,3-trichloro-1-propene, 1,2,3-trichloro-1-propene, 1,3-dichloro-2-methylenepropane, 1,4-dichlorobutane, 1,3-dichloro-2-butene, 1,1,3,3-tetrachloro-2-methylpropane, 1,1,2,3,3-pentachloropropane, 1,3-dichlorocyclopentane, 1,1,2,2,3,3-hexachloropropane, 1,2,3,4,5,5-hexanechloro-1,3-cyclopentadiene, trichlorocyclopentene, tetrachlorocyclopentene, pentachloronorbornene, or any combination thereof.

[0029]

[0035] In step 114, in some embodiments, the low carbon content of the precursor present in the collection vessel is verified or not verified. In some embodiments, verifying the low carbon content of the precursor present in the collection vessel includes measuring the carbon content of the precursor to verify or not verify the low carbon content of the precursor. In some embodiments, verifying the low carbon content of the precursor present in the collection vessel includes: If the low carbon content is not verified, removing at least a portion of the carbon-containing material from the precursor. In some embodiments, the low carbon content of the precursor present in the collection vessel is measured by total carbon analysis using non-dispersive infrared detection. In some embodiments, the low carbon content of the precursor present in the collection vessel is measured by total carbon analysis using thermal conductivity detection.

[0030]

[0036] 2 is a flowchart of a method 200 for separating a carbon-containing material from a tungsten precursor, according to some embodiments. As shown in FIG. 2, the method 200 for separating a carbon-containing material from a tungsten precursor can include at least one of the following steps: applying first conditions to a source vessel 202 to produce a tungsten precursor vapor containing the carbon-containing material; removing a first portion of the carbon-containing material from the tungsten precursor vapor 204; flowing the tungsten precursor vapor to a collection vessel 206; or any combination thereof. In some embodiments, the method 200 relates to separating the tungsten precursor from at least a first portion of the carbon-containing material, as described above.

[0031]

[0037] In step 202, in some embodiments, first conditions are applied to the source vessel such that a tungsten precursor vapor containing a carbon-containing material is produced. In some embodiments, the first conditions include a first temperature of the source vessel. In some embodiments, the first temperature of the source vessel is in the range of 60°C to 170°C, or any range or subrange of temperatures between 60°C and 170°C. In some embodiments, the first temperature of the source vessel is in the range of 60°C to 160°C, 60°C to 150°C, 60°C to 140°C, 60°C to 130°C, 60°C to 120°C, 60°C to 110°C, 60°C to 100°C, 60°C to 90°C, 60°C to 80°C, 60°C to 70°C, 70°C to 170°C, 80°C to 170°C, 90°C to 170°C, 100°C to 180°C, 180°C to 210°C, 210°C to 220°C, 220°C to 240°C, 230°C to 250°C, 240°C to 260°C, 250°C to 280°C, 260°C to 300°C, 270°C to 310°C, 280°C to 320°C, 290°C to 330°C, 340°C to 350°C, 350°C to 360°C, 360°C to 370°C, 370°C to 380°C, 380°C to 400°C, The temperature is in the range of 0°C to 170°C, 110°C to 170°C, 120°C to 170°C, 130°C to 170°C, 140°C to 170°C, 150°C to 170°C, 160°C to 170°C, 100°C to 160°C, 120°C to 160°C, 140°C to 160°C, 120°C to 150°C, 120°C to 140°C, or 110°C to 150°C.

[0032]

[0038] In some embodiments, the first condition includes a first pressure in the source vessel. In some embodiments, the first pressure in the source vessel is a pressure in the range of 0.01 Torr to 100 Torr, or any range or subrange therebetween. In some embodiments, the first pressure in the source vessel is a pressure in the range of 0.01 Torr to 95 Torr, 0.01 Torr to 90 Torr, 0.01 Torr to 85 Torr, 0.01 Torr to 80 Torr, 0.01 Torr to 75 Torr, 0.01 Torr to 70 Torr, 0.01 Torr to 65 Torr, 0.01 Torr to 60 Torr, 0.01 Torr to 55 Torr, 0.0 1Torr~50Torr, 0.01Torr~45Torr, 0.01Torr~40Torr, 0.01Torr~35Torr, 0.01Torr~30Torr, 0.01Torr ~25Torr, 0.01Torr~20Torr, 0.01Torr~15Torr, 0.01Torr~10Torr, 0.01Torr~5Torr, 0.01Torr~1Torr , 0.01Torr~0.1Torr, 0.1Torr~100Torr, 1Torr~100Torr, 5Torr~100Torr, 10Torr~100Torr, 15Torr~1 00Torr, 20Torr~100Torr, 25Torr~100Torr, 30Torr~100Torr, 35Torr~100Torr, 40Torr~100Torr, 45T orr to 100 Torr, 50 Torr to 100 Torr, 55 Torr to 100 Torr, 60 Torr to 100 Torr, 65 Torr to 100 Torr, 70 Torr to 100 Torr, 75 Torr to 100 Torr, 80 Torr to 100 Torr, 85 Torr to 100 Torr, 90 Torr to 100 Torr, or 95 Torr to 100 Torr.

[0033]

[0039] In some embodiments, the first condition is a condition in which the total pressure of the source vessel is below the true vapor pressure of the tungsten precursor for a given first temperature. In some embodiments, the first condition is a condition in which the total pressure of the source vessel is below the true vapor pressure of the carbon-containing material at a given first temperature. In some embodiments, the tungsten precursor vapor comprises a carbon-containing material. In some embodiments, the carbon-containing material comprises a first carbon-containing vapor. In some embodiments, the carbon-containing material comprises a first plurality of carbon-containing particles. In some embodiments, the carbon-containing material comprises at least one of a first carbon-containing vapor, a first plurality of carbon-containing particles, or any combination thereof.

[0034]

[0040] In step 204, in some embodiments, a first portion of the carbon-containing material is removed from the tungsten precursor vapor. In some embodiments, removing the first portion of the carbon-containing material from the tungsten precursor vapor comprises flowing the tungsten precursor vapor through a filter to remove at least a portion of the first plurality of carbon-containing particles. In some embodiments, removing the first portion of the carbon-containing material from the tungsten precursor vapor comprises flowing the tungsten precursor vapor over an adsorbent to remove at least a portion of the first carbon-containing vapor. In some embodiments, removing the first portion of the carbon-containing material from the tungsten precursor vapor comprises flowing the tungsten precursor vapor through a filter to remove at least a portion of the first plurality of carbon-containing particles and flowing the tungsten precursor vapor over an adsorbent to remove at least a portion of the first carbon-containing vapor.

[0035]

[0041] In step 206, the tungsten precursor vapor is flowed to a collection vessel. In some embodiments, the tungsten precursor vapor includes carbon-containing materials. In some embodiments, the tungsten precursor vapor contains less carbon-containing materials than the tungsten precursor vapor prior to the removal step 204.

[0036]

[0042] 3 is a flowchart of a method 300 for separating a carbon-containing material from a tungsten precursor, according to some embodiments. As shown in FIG. 3, the method 300 for separating a carbon-containing material from a tungsten precursor can include at least one of the following steps: applying second conditions to a collection vessel 302 to produce a tungsten precursor condensate and a second carbon-containing vapor, removing at least a portion of the second carbon-containing vapor from the collection vessel 304, or any combination thereof. In some embodiments, the method 300 relates to separating the tungsten precursor from at least a second portion of the carbon-containing material, as described above.

[0037]

[0043] In step 302, in some embodiments, second conditions are applied to the collection vessel such that a tungsten precursor condensate and a second carbon-containing vapor are produced. In some embodiments, producing the tungsten precursor condensate and the second carbon-containing vapor results in the tungsten precursor being separated from a second portion of the carbon-containing vapor. In some embodiments, the second conditions include a second temperature of the collection vessel. In some embodiments, the second temperature of the collection vessel is a temperature in the range of 10° C. to 100° C., or any range or subrange therebetween. In some embodiments, the second temperature of the collection vessel is in the range of 20°C to 100°C, 30°C to 100°C, 40°C to 100°C, 50°C to 100°C, 60°C to 100°C, 70°C to 100°C, 80°C to 100°C, 90°C to 100°C, 10°C to 90°C, 10°C to 80°C, 10°C to 70°C, 10°C to 60°C, 10°C to 50°C, 10°C to 40°C, 10°C to 30°C, or 10°C to 20°C. In some embodiments, the second temperature of the collection vessel is sufficient to condense the tungsten precursor vapor. In some embodiments, the second temperature of the collection vessel is sufficient to produce a second carbon-containing vapor.

[0038]

[0044] In some embodiments, the second condition includes a second pressure in the collection vessel. In some embodiments, the second pressure in the collection vessel is a pressure in the range of 0.01 Torr to 100 Torr, or any range or subrange therebetween. In some embodiments, the second pressure in the collection vessel is a pressure in the range of 0.01 Torr to 95 Torr, 0.01 Torr to 90 Torr, 0.01 Torr to 85 Torr, 0.01 Torr to 80 Torr, 0.01 Torr to 75 Torr, 0.01 Torr to 70 Torr, 0.01 Torr to 65 Torr, 0.01 Torr to 60 Torr, 0.01 Torr to 55 Torr, 0. 01Torr~50Torr, 0.01Torr~45Torr, 0.01Torr~40Torr, 0.01Torr~35Torr, 0.01Torr~30Torr, 0.01Torr r~25Torr, 0.01Torr~20Torr, 0.01Torr~15Torr, 0.01Torr~10Torr, 0.01Torr~5Torr, 0.01Torr~1Torr , 0.01Torr~0.1Torr, 0.1Torr~100Torr, 1Torr~100Torr, 5Torr~100Torr, 10Torr~100Torr, 15Torr~1 00Torr, 20Torr~100Torr, 25Torr~100Torr, 30Torr~100Torr, 35Torr~100Torr, 40Torr~100Torr, 45T In some embodiments, the second pressure in the collection vessel is sufficient to condense the tungsten precursor vapor. In some embodiments, the second pressure in the collection vessel is sufficient to generate a second carbon-containing vapor.

[0039]

[0045] In some embodiments, second conditions are applied to the collection vessel such that a tungsten precursor condensate and a second carbon-containing vapor are produced. In some embodiments, the second conditions are conditions in which a greater volume of the tungsten precursor condenses than the second carbon-containing vapor. In some embodiments, the tungsten precursor condensate comprises a greater amount (e.g., mole fraction, volume, or mass fraction) of the tungsten precursor condensate than the carbon-containing condensate (if present). In some embodiments, the second conditions are conditions in which a greater volume of the second carbon-containing vapor remains evaporated than the tungsten precursor. In some embodiments, the second conditions are conditions in which the second carbon-containing vapor comprises carbon-containing material that was present in the vaporized tungsten precursor vapor in the source vessel.

[0040]

[0046] In step 304, in some embodiments, at least a portion of the second carbon-containing vapor is removed from the collection vessel. The second carbon-containing vapor can be removed through an outlet of the collection vessel. The outlet can be fluidly connected to a gas exhaust line, a vacuum line, or other similar line suitable for removing the second carbon-containing vapor from the collection vessel.

[0041]

[0047] 4 is a flowchart of a method 400 for separating a carbon-containing material from a tungsten precursor, according to some embodiments. As shown in FIG. 4, the method 400 for separating a carbon-containing material from a tungsten precursor can include at least one of the following steps: applying third conditions to a source vessel 402 to produce a third carbon-containing vapor, removing at least a portion of the third carbon-containing vapor from the source vessel 404, or any combination thereof. In some embodiments, the method 400 is performed before step 104 (e.g., FIG. 2). In some embodiments, the method 400 relates to separating the tungsten precursor from at least a third portion of the carbon-containing material, as described above.

[0042]

[0048] In step 402, in some embodiments, third conditions are applied to the source vessel to generate a third carbon-containing vapor. In some embodiments, the third conditions include a third temperature of the source vessel. In some embodiments, the third temperature of the source vessel is in the range of 60°C to 170°C, or any range or subrange of temperatures between 60°C and 170°C. In some embodiments, the third temperature of the source vessel is in the range of 60°C to 160°C, 60°C to 150°C, 60°C to 140°C, 60°C to 130°C, 60°C to 120°C, 60°C to 110°C, 60°C to 100°C, 60°C to 90°C, 60°C to 80°C, 60°C to 70°C, 70°C to 170°C, 80°C to 170°C, 90°C to 170°C, 100°C to 180°C, 180°C to 210°C, 210°C to 220°C, 220°C to 240°C, 230°C to 250°C, 240°C to 260°C, 250°C to 280°C, 260°C to 300°C, 270°C to 310°C, 280°C to 320°C, 290°C to 330°C, 340°C to 350°C, 350°C to 360°C, 360°C to 370°C, 370°C to 380°C, 380°C to 400°C, 390°C to 41 The temperature is in the range of 0°C to 170°C, 110°C to 170°C, 120°C to 170°C, 130°C to 170°C, 140°C to 170°C, 150°C to 170°C, 160°C to 170°C, 100°C to 160°C, 120°C to 160°C, 140°C to 160°C, 120°C to 150°C, 120°C to 140°C, or 110°C to 150°C.

[0043]

[0049] In some embodiments, the third condition includes a third pressure in the source vessel. In some embodiments, the third pressure in the source vessel is a pressure in the range of 0.01 Torr to 100 Torr, or any range or subrange therebetween. In some embodiments, the third pressure in the source vessel is a pressure in the range of 0.01 Torr to 95 Torr, 0.01 Torr to 90 Torr, 0.01 Torr to 85 Torr, 0.01 Torr to 80 Torr, 0.01 Torr to 75 Torr, 0.01 Torr to 70 Torr, 0.01 Torr to 65 Torr, 0.01 Torr to 60 Torr, 0.01 Torr to 55 Torr, 0.0 1Torr~50Torr, 0.01Torr~45Torr, 0.01Torr~40Torr, 0.01Torr~35Torr, 0.01Torr~30Torr, 0.01Torr ~25Torr, 0.01Torr~20Torr, 0.01Torr~15Torr, 0.01Torr~10Torr, 0.01Torr~5Torr, 0.01Torr~1Torr , 0.01Torr~0.1Torr, 0.1Torr~100Torr, 1Torr~100Torr, 5Torr~100Torr, 10Torr~100Torr, 15Torr~1 00Torr, 20Torr~100Torr, 25Torr~100Torr, 30Torr~100Torr, 35Torr~100Torr, 40Torr~100Torr, 45T orr to 100 Torr, 50 Torr to 100 Torr, 55 Torr to 100 Torr, 60 Torr to 100 Torr, 65 Torr to 100 Torr, 70 Torr to 100 Torr, 75 Torr to 100 Torr, 80 Torr to 100 Torr, 85 Torr to 100 Torr, 90 Torr to 100 Torr, or 95 Torr to 100 Torr.

[0044]

[0050] In some embodiments, the third condition is a condition in which the total pressure of the source vessel is below the true vapor pressure of the carbon-containing material at a given third temperature. In some embodiments, the third condition is a condition in which the total pressure of the source vessel is above the true vapor pressure of the tungsten precursor at a given third temperature. In some embodiments, the first condition is a condition in which the carbon-containing material evaporates while minimizing the amount of evaporating tungsten precursor. In some embodiments, the third condition is a condition in which the tungsten precursor does not vaporize. In some embodiments, when the third condition is applied, the third carbon-containing vapor contains a larger volume of carbon-containing material than the tungsten precursor.

[0045]

[0051] The third carbon-containing vapor may comprise a greater volume of carbon-containing material than the tungsten precursor. In some embodiments, the third carbon-containing vapor comprises less than 10%, less than 9%, less than 8%, less than 7%, less than 6%, less than 5%, less than 4%, less than 3%, less than 2%, less than 1%, less than 0.1%, or less than 0.01% by volume of the tungsten precursor, based on the total volume of the third carbon-containing vapor. In some embodiments, the third carbon-containing vapor comprises 0.01% to 10%, 0.01% to 9%, 0.01% to 8%, 0.01% to 7%, 0.01% to 6%, 0.01% to 5%, 0.01% to 4%, 0.01% to 3%, 0.01% to 2%, 0.01% to 1%, 0.01% to 0.1%, 0.1% to 10%, 1% to 10%, 2% to 10%, 3% to 10%, 4% to 10%, 5% to 10%, 6% to 10%, 7% to 10%, 8% to 10%, or 9% to 10% tungsten precursor by volume, based on the total volume of the third carbon-containing vapor.

[0046]

[0052] In step 404, in some embodiments, at least a portion of the third carbon-containing vapor is removed from the source vessel. The third carbon-containing vapor can be removed through an outlet of the source vessel. The outlet can be fluidly connected to a gas exhaust line, a vacuum line, or other similar line suitable for removing the third carbon-containing vapor from the source vessel.

[0047]

[0053] In some embodiments, the method 500 relates to separating the tungsten precursor from at least a fourth portion of the carbon-containing material, as described above.

[0048]

[0054] 5 is a flowchart of a method 500 for separating a carbon-containing material from a tungsten precursor, according to some embodiments. As shown in FIG. 5, the method 500 for separating a carbon-containing material from a tungsten precursor can include at least one of the following steps: applying fourth conditions to a source vessel 502 to produce a fourth carbon-containing vapor, removing at least a portion of the fourth carbon-containing vapor from a collection vessel 504, or any combination thereof. In some embodiments, the method 500 is performed after step 112 (e.g., FIG. 6). In some embodiments, the method 500 is performed after step 114 (e.g., FIG. 7). In some embodiments, the method 500 relates to separating the tungsten precursor from at least a fourth portion of the carbon-containing material, as described above.

[0049]

[0055] In step 502, in some embodiments, fourth conditions are applied to the collection vessel to generate a fourth carbon-containing vapor. In some embodiments, the fourth conditions include a fourth temperature of the collection vessel. In some embodiments, the fourth temperature of the collection vessel is in the range of 60°C to 170°C, or any range or subrange of temperatures between 60°C and 170°C. In some embodiments, the fourth temperature of the collection vessel is in the range of 60°C to 160°C, 60°C to 150°C, 60°C to 140°C, 60°C to 130°C, 60°C to 120°C, 60°C to 110°C, 60°C to 100°C, 60°C to 90°C, 60°C to 80°C, 60°C to 70°C, 70°C to 170°C, 80°C to 170°C, 90°C to 170°C, or 100°C. The temperature ranges are 00°C to 170°C, 110°C to 170°C, 120°C to 170°C, 130°C to 170°C, 140°C to 170°C, 150°C to 170°C, 160°C to 170°C, 100°C to 160°C, 120°C to 160°C, 140°C to 160°C, 120°C to 150°C, 120°C to 140°C, or 110°C to 150°C.

[0050]

[0056] In some embodiments, the fourth condition includes a fourth pressure in the collection vessel. In some embodiments, the fourth pressure in the collection vessel is a pressure in the range of 0.01 Torr to 100 Torr, or any range or subrange therebetween. In some embodiments, the fourth pressure in the collection vessel is a pressure in the range of 0.01 Torr to 95 Torr, 0.01 Torr to 90 Torr, 0.01 Torr to 85 Torr, 0.01 Torr to 80 Torr, 0.01 Torr to 75 Torr, 0.01 Torr to 70 Torr, 0.01 Torr to 65 Torr, 0.01 Torr to 60 Torr, 0.01 Torr to 55 Torr, 0. 01Torr~50Torr, 0.01Torr~45Torr, 0.01Torr~40Torr, 0.01Torr~35Torr, 0.01Torr~30Torr, 0.01Torr r~25Torr, 0.01Torr~20Torr, 0.01Torr~15Torr, 0.01Torr~10Torr, 0.01Torr~5Torr, 0.01Torr~1Torr , 0.01Torr~0.1Torr, 0.1Torr~100Torr, 1Torr~100Torr, 5Torr~100Torr, 10Torr~100Torr, 15Torr~1 00Torr, 20Torr~100Torr, 25Torr~100Torr, 30Torr~100Torr, 35Torr~100Torr, 40Torr~100Torr, 45T orr to 100 Torr, 50 Torr to 100 Torr, 55 Torr to 100 Torr, 60 Torr to 100 Torr, 65 Torr to 100 Torr, 70 Torr to 100 Torr, 75 Torr to 100 Torr, 80 Torr to 100 Torr, 85 Torr to 100 Torr, 90 Torr to 100 Torr, or 95 Torr to 100 Torr.

[0051]

[0057] In some embodiments, the fourth condition is a condition in which the total pressure of the collection vessel is less than the true vapor pressure of the carbon-containing material at the given fourth temperature. In some embodiments, the fourth condition is a condition in which the total pressure of the collection vessel is greater than the true vapor pressure of the tungsten precursor at the given fourth temperature. In some embodiments, the first condition is a condition in which the carbon-containing material evaporates while minimizing the amount of evaporating tungsten precursor. In some embodiments, the fourth condition is a condition in which the tungsten precursor does not evaporate. In some embodiments, when the fourth condition is applied, the fourth carbon-containing vapor contains a larger volume of carbon-containing material than the tungsten precursor.

[0052]

[0058] The fourth carbon-containing vapor may comprise a greater volume of carbon-containing material than the tungsten precursor. In some embodiments, the fourth carbon-containing vapor comprises less than 10%, less than 9%, less than 8%, less than 7%, less than 6%, less than 5%, less than 4%, less than 3%, less than 2%, less than 1%, less than 0.1%, or less than 0.01% by volume of the tungsten precursor, based on the total volume of the fourth carbon-containing vapor. In some embodiments, the fourth carbon-containing vapor comprises between 0.01% and 10%, between 0.01% and 9%, between 0.01% and 8%, between 0.01% and 7%, between 0.01% and 6%, between 0.01% and 5%, between 0.01% and 4%, between 0.01% and 3%, between 0.01% and 2%, between 0.01% and 1%, between 0.01% and 0.1%, between 0.1% and 10%, between 1% and 10%, between 2% and 10%, between 3% and 10%, between 4% and 10%, between 5% and 10%, between 6% and 10%, between 7% and 10%, between 8% and 10%, or between 9% and 10% tungsten precursor by volume, based on the total volume of the fourth carbon-containing vapor.

[0053]

[0059] In step 504, in some embodiments, at least a portion of the fourth carbon-containing vapor is removed from the collection vessel. The fourth carbon-containing vapor can be removed through an outlet of the collection vessel. The outlet can be fluidly connected to a gas exhaust line, a vacuum line, or other similar line suitable for removing the fourth carbon-containing vapor from the collection vessel.

[0054]

[0060] 6 is a flowchart of a method 600 for verifying the low impurity content of a tungsten precursor, according to some embodiments. As shown in FIG. 6 , in some embodiments, the method 600 for verifying the low impurity content of a tungsten precursor can include at least one of the following steps: measuring the carbon content of the precursor in step 602 to verify or not verify the low carbon content of the precursor; comparing the measured carbon content to a reference value in step 604 to verify or not verify the low carbon content of the precursor. If the precursor is verified to have a low carbon content, the precursor is ready for use 608. If the precursor is not verified to have a low carbon content, the method 600 includes further removing 606 at least a portion of the carbon-containing material from the precursor. In some embodiments, method 600 includes measuring the carbon content of the precursor, the measuring including applying a temperature to the collection vessel (e.g., 800°C to 2500°C, or any range or subrange therebetween), removing a sample from the collection vessel (e.g., removing a solid sample from the collection vessel (e.g., 0.01 g to 1.50 g), removing a vapor sample in the headspace above the unvaporized precursor, or any combination thereof), and analyzing the vapor sample by at least one of total carbon analysis using a non-dispersive infrared detector, total carbon analysis using a thermal conductivity detector, gas chromatography, or any combination thereof. In some embodiments, removing at least a portion of the carbon-containing material from the precursor includes repeating one or more of step 104 (e.g., including but not limited to, at least one of the steps of FIG. 2), step 106 (e.g., including but not limited to, at least one of the steps of FIG. 3), step 108 (e.g., including but not limited to, at least one of the steps of FIG. 4), step 110 (e.g., including but not limited to, at least one of the steps of FIG. 5), or any combination thereof. In some embodiments, method 600 relates to a method for verifying low carbon content of a tungsten precursor, as described above.

[0055]

[0061] FIG. 7 is a schematic diagram of a system for removing carbon-containing materials from a precursor, according to some embodiments. As shown in FIG. 7 , in some embodiments, the system 700 includes a first vessel 702, a second vessel 708, a first removal unit 704, and a second removal unit 706. The first vessel 702 can be fluidly coupled to the second vessel 708. In some embodiments, the first removal unit 704 includes a filter for removing carbon-containing materials from the vapor. In some embodiments, the carbon-containing material removed by the filter is a plurality of carbon-containing particles. In some embodiments, the second removal unit 706 includes an adsorbent for removing carbon-containing materials from the vapor. In some embodiments, the carbon-containing material removed by the adsorbent is a carbon-containing vapor. While the second removal unit 706 is illustrated downstream of the first removal unit 704, it will be understood that other configurations are possible, including, but not limited to, disposing the second removal unit 706 upstream of the first removal unit 704. Furthermore, additional removal units (eg, 704, 706) may be added or removed from the system without departing from the scope of the present disclosure.

[0056] Example 1

[0062] 125 mg of WCl5 precursor was added to a tin capsule in an air- and moisture-free glove box. The mass of the WCl5 precursor was measured and recorded using an analytical balance. The tin capsule containing the WCl5 precursor was sealed inside the glove box. Total carbon values ​​measured using a total carbon analyzer with NDIR detection averaged 126 ppm.

[0057] Example 2

[0063] 0.01 g of WCl5 precursor is added to a tin capsule in an air- and moisture-free glove box. The mass of the WCl5 precursor is measured and recorded using an analytical balance. The tin capsule containing the WCl5 precursor is sealed inside the glove box. The total carbon value is measured using a total carbon analyzer with NDIR detection.

[0058] Example 3

[0064] 1.5 g of WCl5 precursor is added to a tin capsule in an air- and moisture-free glove box. The mass of the WCl5 precursor is measured and recorded using an analytical balance. The tin capsule containing the WCl5 precursor is sealed inside the glove box. The total carbon value is measured using a total carbon analyzer with NDIR detection.

[0059] Example 4

[0065] 125 mg of WCl6 precursor is added to a tin capsule in an air- and moisture-free glove box. The mass of the WCl6 precursor is measured and recorded using an analytical balance. The tin capsule containing the WCl6 precursor is sealed inside the glove box. Total carbon values ​​measured using a total carbon analyzer with NDIR detection average 126 ppm.

[0060] Example 5

[0066] 0.01 g of WCl6 precursor is added to a tin capsule in an air- and moisture-free glove box. The mass of the WCl6 precursor is measured and recorded using an analytical balance. The tin capsule containing the WCl6 precursor is sealed inside the glove box. The total carbon value is measured using a total carbon analyzer using NDIR detection.

[0061] Example 6

[0067] 1.5 g of WCl6 precursor is added to a tin capsule in an air- and moisture-free glove box. The mass of the WCl6 precursor is measured and recorded using an analytical balance. The tin capsule containing the WCl6 precursor is sealed inside the glove box. The total carbon value is measured using a total carbon analyzer using NDIR detection.

[0062]

[0068] Aspects

[0069] Various aspects are described below, and it should be understood that any one or more of the features described in the following aspects can be combined with any one or more of the other aspects. Aspect 1 A precursor, a tungsten precursor; Carbon-containing materials and Including, A precursor comprising less than 0.015 wt. % carbon-containing material, based on the total weight of the precursor, as measured by total carbon analysis using non-dispersive infrared detection. Aspect 2 10. The precursor of embodiment 1, comprising less than 0.005 wt.% carbon-containing material, based on the total weight of the precursor, as measured by total carbon analysis using non-dispersive infrared detection. Aspect 3 3. The precursor of either aspect 1 or 2, comprising less than 0.001 wt. % carbon-containing material, based on the total weight of the precursor, as measured by total carbon analysis using non-dispersive infrared detection. Aspect 4 Aspect 4. The precursor of any one of aspects 1-3, comprising less than 0.0002 wt. % carbon-containing material, based on the total weight of the precursor, as measured by total carbon analysis using non-dispersive infrared detection. Aspect 5 5. The precursor of any one of Aspects 1-4, comprising from 0.0002% to less than 0.001% by weight of carbon-containing material, based on the total weight of the precursor, as measured by total carbon analysis using non-dispersive infrared detection. Aspect 6 The precursor of any one of Aspects 1-5, wherein the carbon-containing material comprises a chlorinated hydrocarbon. Aspect 7 The carbon-containing material may be dichloromethane, phosgene, 1,1-dichloroethane, chloroform, 1,2-dichloroethane, carbon tetrachloride, tetrachloroethylene, trichloroethylene, 1,3-dichloropropane, 1,2,3-trichloropropane, 1,2-dichloropropane, 1,1,2-trichloroethane, 1,1,2-trichloropropane, 1,2,2-trichloropropane, 1,1,2,3-tetrachloropropane, 1,2,2,3-tetrachloropropane, 1,1,2,2-tetrachloroethane, 2,2-dichloropropanoyl chloride, 1,3-dichloro-1-propene, 3,3,3-trichloro-1-propene 7. The precursor of any one of aspects 1-6, comprising at least one of 1,2,3-trichloro-1-propene, 1,3-dichloro-2-methylenepropane, 1,4-dichlorobutane, 1,3-dichloro-2-butene, 1,1,3,3-tetrachloro-2-methylpropane, 1,1,2,3,3-pentachloropropane, 1,3-dichlorocyclopentane, 1,1,2,2,3,3-hexachloropropane, 1,2,3,4,5,5-hexanechloro-1,3-cyclopentadiene, trichlorocyclopentene, tetrachlorocyclopentene, pentachloronorbornene, or any combination thereof. Aspect 8 a) obtaining a source vessel containing a tungsten precursor and a carbon-containing material; b) separating the tungsten precursor from at least a first portion of the carbon-containing material, the separating comprising: applying first conditions to a source vessel to generate a tungsten precursor vapor containing a carbon-containing material; applying, the carbon-containing material comprising at least one of a first carbon-containing vapor, a first plurality of carbon-containing particles, or any combination thereof; removing a first portion of the carbon-containing material from the tungsten precursor vapor; flowing the tungsten precursor vapor into a collection vessel and c) recovering the precursor in a collection vessel; A method comprising: Aspect 9 removing a first portion of the carbon-containing material from the tungsten precursor vapor; 9. The method of embodiment 8, comprising flowing the tungsten precursor vapor through a filter to remove at least a portion of the first plurality of carbon-containing particles. Aspect 10 removing a first portion of the carbon-containing material from the tungsten precursor vapor; 10. The method of any one of embodiments 8-9, comprising flowing the tungsten precursor vapor over an adsorbent to remove at least a portion of the first carbon-containing vapor. Aspect 11 removing a first portion of the carbon-containing material from the tungsten precursor vapor; flowing the tungsten precursor vapor through a filter to remove at least a portion of the first plurality of carbon-containing particles; 11. The method of any one of aspects 8-10, comprising flowing the tungsten precursor vapor over an adsorbent to remove at least a portion of the first carbon-containing vapor. Aspect 12 12. The method of any one of aspects 8-11, wherein the first condition is a condition in which the total pressure of the source vessel is below the true vapor pressure of the tungsten precursor for the given first temperature. Embodiment 13 The method of any one of embodiments 8 to 12, wherein the first condition is a condition in which the total pressure of the source vessel is below the true vapor pressure of the carbon-containing material at the predetermined first temperature. Aspect 14 d) separating the tungsten precursor from at least a second portion of the carbon-containing material, applying second conditions to the collection vessel to produce a tungsten precursor condensate and a second carbon-containing vapor; removing at least a portion of the second carbon-containing vapor from the collection vessel; 14. The method of any one of aspects 8 to 13, further comprising a separating step d) comprising: Aspect 15 15. The method of embodiment 14, wherein the second conditions are conditions under which a greater volume of the tungsten precursor condenses than the second carbon-containing vapor. Aspect 16 15. The method of embodiment 14, wherein, if the second condition applies, the tungsten precursor condensate comprises a greater mole fraction of tungsten precursor than the carbon-containing material. Aspect 17 e) separating the tungsten precursor from the third portion of the carbon-containing material, applying third conditions to the source vessel to produce a third carbon-containing vapor; removing at least a portion of the third carbon-containing vapor from the source vessel; e) further comprising separating the 17. The method of any one of aspects 8 to 16, wherein separating e) is performed before separating b). Aspect 18 18. The method of embodiment 17, wherein the third condition is a condition in which the total pressure of the source vessel is below the true vapor pressure of the carbon-containing material at the predetermined third temperature. Aspect 19 18. The method of embodiment 17, wherein the third condition is a condition in which the total pressure of the source vessel exceeds the true vapor pressure of the tungsten precursor at the given third temperature. Aspect 20 18. The method of embodiment 17, wherein, when the third condition applies, the third carbon-containing vapor comprises a greater volume of carbon-containing material than the tungsten precursor. Aspect 21 f) verifying a low carbon content of the precursor present in the collection vessel, wherein the verifying step f) comprises: measuring the carbon content of the precursor to verify or not verify the low carbon content of the precursor; 21. The method of any one of aspects 8-20, comprising removing at least a portion of the carbon-containing material from the precursor if low carbon content is not verified. Aspect 22 22. The method of embodiment 21, wherein the low carbon content of the precursor present in the collection vessel is measured by total carbon analysis using non-dispersive infrared detection. Aspect 23 22. The method of embodiment 21, wherein the low carbon content of the precursor present in the collection vessel is measured by total carbon analysis using thermal conductivity detection. Aspect 24 g) separating the tungsten precursor from the fourth portion of the carbon-containing material, the separating step g) comprising: applying fourth conditions to the collection vessel to produce a fourth carbon-containing vapor; removing at least a portion of the fourth carbon-containing vapor from the collection vessel; The embodiment according to any one of embodiments 8 to 23, including: Aspect 25 25. The method of embodiment 24, wherein the fourth condition is a condition in which the total pressure of the collection vessel is less than the true vapor pressure of the carbon-containing material at the predetermined fourth temperature. Aspect 26 25. The method of embodiment 24, wherein the fourth condition is a condition in which the total pressure of the collection vessel exceeds the true vapor pressure of the tungsten precursor at the given fourth temperature. Aspect 27 25. The method of embodiment 24, wherein, if the fourth condition applies, the fourth carbon-containing vapor comprises a greater volume of carbon-containing material than the tungsten precursor. It will be understood that changes may be made in details, particularly in matters of materials of construction employed and shape, size and arrangement of parts without departing from the scope of the present disclosure. The specification and described embodiments are examples, with the true scope and spirit of the present disclosure being indicated by the following claims.

[0033] Aspect 28. The method of any one of aspects 8-27, wherein the precursor comprises less than 0.02 wt. % carbon-containing material, based on the total weight of the precursor, as measured by total carbon analysis using non-dispersive infrared detection in the precursor recovered in the collection vessel.

Claims

1. A precursor, a tungsten precursor; Carbon-containing materials and Including, A precursor comprising less than 0.02 wt. % carbon-containing material, based on the total weight of the precursor, as measured by total carbon analysis using non-dispersive infrared detection.

2. 10. The precursor of claim 1, comprising less than 0.015 wt. % carbon-containing material, based on the total weight of the precursor, as measured by total carbon analysis using non-dispersive infrared detection.

3. 10. The precursor of claim 1, comprising less than 0.001 wt. % carbon-containing material, based on the total weight of the precursor, as measured by total carbon analysis using non-dispersive infrared detection.

4. 10. The precursor of claim 1, comprising less than 0.0002 wt. % carbon-containing material, based on the total weight of the precursor, as measured by total carbon analysis using non-dispersive infrared detection.

5. 10. The precursor of claim 1, comprising 0.0002 wt. % to 0.001 wt. % carbon-containing material, based on the total weight of the precursor, as measured by total carbon analysis using non-dispersive infrared detection.

6. The precursor of claim 1 , wherein the carbon-containing material comprises a chlorinated hydrocarbon.

7. The precursor of claim 1 , wherein the carbon-containing material comprises a volatile compound, a non-volatile compound, or any combination thereof.

8. 10. The precursor of claim 1, wherein the carbon-containing material comprises at least one of a hydrocarbon polymer (which may be substituted), a haloalkane, a haloalkene, a halocycloalkyl, a halo-substituted arene, or any combination thereof.

9. The carbon-containing material may be dichloromethane, phosgene, 1,1-dichloroethane, chloroform, 1,2-dichloroethane, carbon tetrachloride, tetrachloroethylene, trichloroethylene, 1,3-dichloropropane, 1,2,3-trichloropropane, 1,2-dichloropropane, 1,1,2-trichloroethane, 1,1,2-trichloropropane, 1,2,2-trichloropropane, 1,1,2,3-tetrachloropropane, 1,2,2,3-tetrachloropropane, 1,1,2,2-tetrachloroethane, 2,2-dichloropropanoyl chloride, 1,3-dichloro-1-propene, 3,3,3-trichloro 10. The precursor of claim 1, comprising at least one of 1,2,3-tetrachloro-1-propene, 1,2,3-trichloro-1-propene, 1,3-dichloro-2-methylenepropane, 1,4-dichlorobutane, 1,3-dichloro-2-butene, 1,1,3,3-tetrachloro-2-methylpropane, 1,1,2,3,3-pentachloropropane, 1,3-dichlorocyclopentane, 1,1,2,2,3,3-hexachloropropane, 1,2,3,4,5,5-hexanechloro-1,3-cyclopentadiene, trichlorocyclopentene, tetrachlorocyclopentene, pentachloronorbornene, or any combination thereof.

10. a) obtaining a source vessel containing a tungsten precursor and a carbon-containing material; b) separating the tungsten precursor from at least a first portion of the carbon-containing material, the separating comprising: applying first conditions to the source vessel to produce a tungsten precursor vapor containing a carbon-containing material; applying first conditions to a source vessel, wherein the carbon-containing material comprises at least one of a first carbon-containing vapor, a first plurality of carbon-containing particles, or any combination thereof; removing a first portion of the carbon-containing material from the tungsten precursor vapor; flowing the tungsten precursor vapor into a collection vessel and c) collecting the precursor in a collection vessel; A method comprising:

11. removing a first portion of the carbon-containing material from the tungsten precursor vapor; 11. The method of claim 10, comprising flowing the tungsten precursor vapor through a filter to remove at least a portion of the first plurality of carbon-containing particles.

12. removing a first portion of the carbon-containing material from the tungsten precursor vapor; 11. The method of claim 10, comprising flowing the tungsten precursor vapor over an adsorbent to remove at least a portion of the first carbon-containing vapor.

13. removing a first portion of the carbon-containing material from the tungsten precursor vapor; flowing the tungsten precursor vapor through a filter to remove at least a portion of the first plurality of carbon-containing particles; and flowing the tungsten precursor vapor over the adsorbent to remove at least a portion of the first carbon-containing vapor.

14. 11. The method of claim 10, wherein the first condition is a condition in which the total pressure of the source vessel is below the true vapor pressure of the tungsten precursor for a given first temperature.

15. 11. The method of claim 10, wherein the first condition is a condition in which the total pressure of the source vessel is below the true vapor pressure of the carbon-containing material for the predetermined first temperature.

16. d) separating the tungsten precursor from at least a second portion of the carbon-containing material, applying second conditions to the collection vessel to produce a tungsten precursor condensate and a second carbon-containing vapor; removing at least a portion of the second carbon-containing vapor from the collection vessel; 11. The method of claim 10, further comprising separating d) comprising:

17. 17. The method of claim 16, wherein the second conditions are conditions that result in condensation of a larger volume of the tungsten precursor than the second carbon-containing vapor.

18. 17. The method of claim 16, wherein, when the second condition applies, the tungsten precursor condensate comprises a greater mole fraction of the tungsten precursor than the carbon-containing material.

19. e) separating the tungsten precursor from the third portion of the carbon-containing material, applying third conditions to the source vessel to produce a third carbon-containing vapor; removing at least a portion of the third carbon-containing vapor from the source vessel; e) further comprising separating the 11. The method of claim 10, wherein said separating step e) occurs before separating step b).

20. 20. The method of claim 19, wherein the third condition is a condition in which the total pressure of the source vessel is less than the true vapor pressure of the carbon-containing material for the predetermined third temperature.

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