Tungsten precursors and related methods

Abstract

The present invention provides a precursor comprising a tungsten precursor and a carbonaceous material. The precursor comprises less than 0.02% by weight of the carbonaceous material, based on the total weight of the precursor. A method for purifying a tungsten precursor may comprise at least one of the following steps: obtaining a source vessel containing a tungsten precursor and a carbonaceous material; separating the tungsten precursor from at least a first portion of the carbonaceous material; recovering the precursor in the collection container; or any combination thereof.

Description

Technical Field

[0001] The present disclosure relates to the field of tungsten precursors and related methods, including, for example and without limitation, purification methods and methods for verifying impurity levels. Background Art

[0002] The presence of impurities in precursors for semiconductor manufacturing can lead to defects and improper variability. Current analytical techniques for measuring impurity levels cannot detect or verify impurity levels that are low enough. Summary of the Invention

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

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

[0005] Some embodiments relate to a method for verifying a low impurity content. In some embodiments, the method includes obtaining a collection container 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 container. In some embodiments, the method includes measuring the carbon content of the precursor to verify or not verify a 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 when the low carbon content of the precursor is not verified. BRIEF DESCRIPTION OF THE DRAWINGS

[0006] By way of example only, some embodiments of the present disclosure are described herein with reference to the accompanying drawings. Referring now specifically to the drawings, it should be emphasized that the embodiments are shown by way of example and for purposes of illustrative discussion of the embodiments of the present disclosure. In this regard, the description taken in conjunction with the drawings makes it clear to those skilled in the art how the embodiments of the present disclosure may be practiced.

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

[0008] Figure 2 is a flowchart of a method for separating a carbon-containing material from a tungsten precursor according to some embodiments.

[0009] Figure 3 is a flowchart of a method for separating a carbon-containing material from a tungsten precursor according to some embodiments.

[0010] Figure 4 is a flowchart of a method for separating a carbon-containing material from a tungsten precursor according to some embodiments.

[0011] Figure 5 is a flowchart of a method for separating a carbon-containing material from a tungsten precursor according to some embodiments.

[0012] Figure 6 is a flowchart of a method for verifying the carbon content of a tungsten precursor according to some embodiments.

[0013] Figure 7 is a schematic diagram of a system for removing a carbon-containing material from a precursor according to some embodiments. DETAILED DESCRIPTION

[0014] Among the benefits and improvements already disclosed, other objects and advantages of the present disclosure will become apparent from the following description taken in conjunction with the accompanying drawings. The detailed embodiments of the present disclosure are disclosed herein; however, it should be understood that the disclosed embodiments are only illustrative of the present disclosure which can be implemented in various forms. In addition, each of the examples given with respect to the various embodiments of the present disclosure is intended to be illustrative and not restrictive.

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

[0016] Throughout this specification and the claims, unless the context clearly dictates otherwise, the following terms have the meanings explicitly associated herein. As used herein, the phrases "in one embodiment," "in an embodiment," and "in some embodiments" do not necessarily refer to the same embodiment, but may. Additionally, as used herein, the phrases "in another embodiment" and "in some other embodiments" do not necessarily refer to different embodiments, but may. All embodiments of the present disclosure are contemplated to be combinable without departing from the scope or spirit of the present disclosure.

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

[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 (WCl 5 ). In some embodiments, the tungsten precursor includes tungsten hexachloride (WCl 6 ). In some embodiments, the tungsten precursor includes WCl 5 or WCl 6One of the above. In some embodiments, at least one impurity comprises a carbon material. In some embodiments, the carbon-containing material comprises at least one of a volatile compound (e.g., a volatile carbon-containing material), a non-volatile compound (e.g., a non-volatile carbon-containing material), or any combination thereof. In some embodiments, at least one impurity comprises a chlorinated hydrocarbon. In some embodiments, the carbon-containing material comprises at least one of a hydrocarbon polymer, a haloalkane, a haloalkene, a halocycloalkane, a haloarene, or any combination thereof. In some embodiments, the carbon-containing material comprises substituents (e.g., one or more functional groups). In some embodiments, the carbon-containing material comprises a volatile carbon substance that is volatile under the conditions for evaporating the tungsten precursor. In some embodiments, the carbon-containing material comprises an entrained specific carbon substance (e.g., a substance to be captured by the filter). In some embodiments, at least one impurity comprises at least one of the following: 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-hexachloro-1,3-cyclopentadiene, trichlorocyclopentene, tetrachlorocyclopentene, pentachloronorbornene, or any combination thereof.

[0019] Based on the total weight of the precursor, the precursor may contain less than 0.05 wt% or any range or sub-range therebetween of carbon material. In some embodiments, based on the total weight of the precursor as measured by total carbon analysis using non-dispersive infrared detection, the precursor contains less than 0.02 wt%, less than 0.019 wt%, less than 0.018 wt%, less than 0.017 wt%, less than 0.016 wt%, less than 0.015 wt%, less than 0.014 wt%, less than 0.013 wt%, less than 0.012 wt%, less than 0.011 wt%, less than 0.010 wt%, less than 0.009 wt%, less than 0.008 wt%, less than 0.007 wt%, less than 0.006 wt%, less than 0.005 wt%, less than 0.004 wt%, less than 0.003 wt%, less than 0.002 wt%, less than 0.001 wt%, less than 0.0009 wt%, less than 0.0008 wt%, less than 0.0007 wt%, less than 0.0006 wt%, less than 0.0005 wt%, less than 0.0004 wt%, less than 0.0003 wt%, less than 0.0002 wt% or less than 0.0001 wt% of carbon material.

[0020] Based on the total weight of the precursor, the precursor may contain from 0.0001 wt% to 0.05 wt% or any range or sub-range therebetween of carbon material. In some embodiments, as measured by total carbon analysis using non-dispersive infrared detection, the precursor contains from 0.0001% to 0.02%, from 0.0001% to 0.019%, from 0.0001% to 0.018%, from 0.0001% to 0.017%, from 0.0001% to 0.016%, from 0.0001% to 0.015%, from 0.0001% to 0.014%, from 0.0001% to 0.013%, from 0.0001% to 0.012%, from 0.0001% to 0.011%, from 0.0001% to 0.010%, from 0.0001% to 0.009%, from 0.0001% to 0.008%, from 0.0001% to 0.007%, from 0.0001% to 0.006%, from 0.0001% to 0.005%, from 0.0001% to 0.004%, from 0.0001% to 0.003%, from 0.0001% to 0.002%, from 0.0001% to 0.001%, from 0.0002% to 0.015%, from 0.0003% to 0.015%, from 0.0004% to 0.015%, from 0.0005% to 0.015%, from 0.0006% to 0.015%, from 0.0007% to 0.015%, from 0.0008% to 0.015%, from 0.0009% to 0.015%, from 0.001% to 0.015%, from 0.0011% to 0.015%, from 0.0012% to 0.015%, from 0.0013% to 0.015%, from 0.0014% to 0.015%, from 0.0002% to 0.001%, from 0.0003% to 0.001%, from 0.0004% to 0.001%, from 0.0005% to 0.001%, from 0.0006% to 0.001%, from 0.0007% to 0.001%, from 0.0008% to 0.001%, from 0.0009% to 0.001%, from 0.0002% to 0.0009%, from 0.0002% to 0.0008%, from 0.0002% to 0.0007%, from 0.0002% to 0.0006%, from 0.0002% to 0.0005%, from 0.0002% to 0.0004%, from 0.0002% to 0.0003%, from 0.005% to 0.015%, from 0.006% to 0.015%, from 0.007% to 0.015%, from 0.008% to 0.015%, from 0.009% to 0.015%, from 0.01% to 0.015%, from 0.01% to 0.015%, from 0.012% to 0.015%, from 0.013% to 0.015%, from 0.014% to 0.015%, from 0.006% to 0.014%, from 0.006% to 0.013%, from 0.006% to 0.012%, from 0.006% to 0.011%, 0.0.06% to 0.01%, 0.006% to 0.009%, 0.006% to 0.008%, or 0.006% to 0.007%.

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

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

[0023] In step 102, in some embodiments, a source container containing a tungsten precursor and a carbon-containing material is obtained. The tungsten precursor may be present in the source container in the form of at least one of a solid, a gas / vapor, or any combination thereof. For example, in some embodiments, the tungsten precursor is present in solid form and in vapor form. In some embodiments, the solid phase of the tungsten precursor is amorphous or crystalline. In some embodiments, the tungsten precursor is present in the form of discrete crystals. The carbon-containing material may be present in the source container in the form of at least one of 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 comprises at least one of the following: 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-dichloropropionyl 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-hexachloro-1,3-cyclopentadiene, trichlorocyclopentene, tetrachlorocyclopentene, pentachloronorbornene, or any combination thereof. In some embodiments, the carbon-containing material is present in solid form and in vapor form. 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 form of discrete crystals in the source container. In some embodiments, the carbon-containing material is present within the lattice of the tungsten precursor. For example, in some embodiments, the carbon-containing material is dissolved in the lattice of the tungsten precursor.

[0024] The source container can be configured to control 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 wound around the source container. In some embodiments, a block heater having a shape that covers at least a major portion of the outer surface of the source container is employed to heat the source container. In some embodiments, a resistive heater is employed to heat the source container. In some embodiments, a lamp heater is employed to heat the source container. In some embodiments, a heat transfer fluid at an elevated temperature can be brought into contact with the outer surface of the source container to effect heating and / or cooling of the source container. In some embodiments, heating is effected by irradiating the source container with infrared or other radiant energy. In some embodiments, the collection container is cooled by a fluid, a fan, a direct thermoelectric device, or any combination thereof. It should be understood that other heating and / or cooling devices and assemblies and other configurations and arrangements of heaters and / or coolers can be employed herein without departing from the scope of the present disclosure.

[0025] The source container can be configured to control pressure. The pressure of the source container can be controlled in any suitable manner. In some embodiments, a gas inlet line is fluidly coupled to the source container. The gas inlet line can be configured to supply pressurized gas from a pressurized gas source to the source container. Control of the pressurized gas entering the source container can be effected 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 container. The vacuum line can be configured to apply a vacuum to the source container. In some embodiments, the pumping speed is controlled by a butterfly valve. It should be understood that other mechanisms for controlling the pressure of the source container can be employed herein without departing from the scope of the present disclosure.

[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 Figure 2In some embodiments, the tungsten precursor can be separated from the first portion of the carbon-containing material by applying a first condition (e.g., at least one of temperature, pressure, inert gas flow, vacuum, or any combination thereof) to the source container, thereby generating tungsten precursor vapor containing the carbon-containing material. In some embodiments, the carbon-containing material includes at least one of a first carbon-containing vapor, a first plurality of carbon-containing particles, or any combination thereof. In some embodiments, the first condition is a condition where the total pressure of the source container is lower than the true vapor pressure of the tungsten precursor for a given first temperature. In some embodiments, the first condition is a condition where the total pressure of the source container is lower than the true vapor pressure of the carbon-containing material for 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 passing the tungsten precursor vapor stream through a filter to remove at least a portion of the first plurality of carbon-containing particles. In some embodiments, the removing step includes passing the tungsten precursor vapor stream through 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 to a collection container.

[0027] The filter can include a filter or filtering medium suitable for removing carbon-containing particles from the tungsten precursor vapor. In some embodiments, the filter includes at least one of the following: wool, glass wool (e.g., glass wool made of 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 the following: perfluoroalkoxy alkane (PFA), polytetrafluoroethylene (PTFE), polypropylene, polyethylene, fibrous polymer, any copolymer thereof, or any combination thereof.

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

[0029] The collection container can be configured to control 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 strip heater is wound around the collection container. In some embodiments, a cylinder heater having a shape covering at least a major portion of the outer surface of the collection container is employed to heat the collection container. In some embodiments, a resistive heater is employed to heat the collection container. In some embodiments, a lamp heater is employed to heat the collection container. In some embodiments, a heat transfer fluid at a high temperature can be brought into contact with the outer surface of the collection container to effect heating and / or cooling of the collection container. In some embodiments, heating is effected by irradiating the collection container with infrared or other radiant energy. In some embodiments, the collection container is cooled by a fluid, a fan, a direct thermoelectric device, or any combination thereof. It should be understood that other heating and / or cooling devices and assemblies, as well as other configurations and arrangements of heaters and / or coolers, can be employed herein without departing from the scope of the present disclosure.

[0030] The collection container can be configured to control pressure. The pressure of the collection container can be controlled in any suitable manner. In some embodiments, a gas inlet line is fluidly coupled to the collection container. The gas inlet line can be configured to supply pressurized gas from a pressurized gas source to the collection container. Control of the pressurized gas entering the collection container 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 container. The vacuum line can be configured to apply a vacuum to the collection container. In some embodiments, the pumping speed is controlled by a butterfly valve. It should be understood that other mechanisms for controlling the pressure of the source container can be employed herein without departing from the scope of the present disclosure.

[0031] In step 106, the tungsten precursor is separated from at least a second portion of the carbonaceous material. As disclosed herein (e.g., in Figure 3 ), in some embodiments, the tungsten precursor can be separated from at least a second portion of the carbonaceous material by applying a second condition (e.g., at least one of temperature, pressure, inert gas flow, vacuum, or any combination thereof) to the collection container, thereby producing a tungsten precursor condensate and a second carbonaceous vapor. In some embodiments, the tungsten precursor can be separated from at least a second portion of the carbonaceous material by removing at least a portion of the second carbonaceous vapor from the collection container. In some embodiments, the second condition is a condition where the volume of the tungsten precursor condensate is greater than that of the second carbonaceous vapor. In some embodiments, when the second condition is applied, the tungsten precursor condensate contains a greater mole fraction of the tungsten precursor than the carbonaceous material.

[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., in Figure 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 container, thereby generating 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 container. In some embodiments, step 108 is performed before step 104. In some embodiments, the third condition is a condition where the total pressure of the source container is lower than the true vapor pressure of the carbon-containing material for a given third temperature. In some embodiments, the third condition is a condition where the total pressure of the source container is higher than the true vapor pressure of the tungsten precursor for 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.

[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., in Figure 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 container, thereby generating 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 container. In some embodiments, step 110 is performed after step 114, which is discussed below. In some embodiments, the fourth condition is a condition where the total pressure of the collection container is lower than the true vapor pressure of the carbon-containing material for a given fourth temperature. In some embodiments, the fourth condition is a condition where the total pressure of the collection container is higher than the true vapor pressure of the tungsten precursor for a given fourth temperature. 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.

[0034] In step 112, in some embodiments, the precursor is recovered in a collection container. In some embodiments, the precursor comprises a tungsten precursor and a carbon-containing material. In some embodiments, as measured by total carbon analysis using non-dispersive infrared detection, the precursor comprises less than 0.02 wt% of the carbon-containing material based on the total weight of the precursor. In some embodiments, the carbon-containing material comprises a chlorinated hydrocarbon. In some embodiments, the carbon-containing material comprises at least one of the following: 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-dichloropropionyl 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-hexachloro-1,3-cyclopentadiene, trichlorocyclopentene, tetrachlorocyclopentene, pentachloronorbornene, or any combination thereof.

[0035] In step 114, in some embodiments, the low carbon content of the precursor present in the collection container is verified or not verified. In some embodiments, verifying the low carbon content of the precursor present in the collection container comprises 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 container comprises removing at least a portion of the carbon-containing material from the precursor when the low carbon content is not verified. In some embodiments, the low carbon content of the precursor present in the collection container 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 container is measured by total carbon analysis using thermal conductivity detection.

[0036] Figure 2 is a flowchart of method 200 for separating a carbon-containing material from a tungsten precursor according to some embodiments. As Figure 2 shown, method 200 for separating a carbon-containing material from a tungsten precursor may comprise at least one of the following steps: step 202 of applying a first condition to a source container to generate a tungsten precursor vapor comprising a carbon-containing material; step 204 of removing a first portion of the carbon-containing material from the tungsten precursor vapor; step 206 of flowing the tungsten precursor vapor to a collection container; or any combination thereof. In some embodiments, method 200 involves separating the tungsten precursor from at least a first portion of the carbon-containing material as described above.

[0037] In step 202, in some embodiments, a first condition is applied to the source container to generate tungsten precursor vapor containing a carbonaceous material. In some embodiments, the first condition includes a first temperature of the source container. In some embodiments, the first temperature of the source container is a temperature in the range of 60 °C to 170 °C or any range or sub-range between 60 °C and 170 °C. In some embodiments, the first temperature of the source container is a temperature in the following ranges: 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 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.

[0038] In some embodiments, the first condition includes a first pressure of the source container. In some embodiments, the first pressure of the source container is a pressure in the range of 0.01 Torr to 100 Torr or any range or sub-range therebetween. In some embodiments, the first pressure of the source container is a pressure in the following ranges: 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, 0.01 Torr to 50 Torr, 0.01 Torr to 45 Torr, 0.01 Torr to 40 Torr, 0.01 Torr to 35 Torr, 0.01 Torr to 30 Torr, 0.01 Torr to 25 Torr, 0.01 Torr to 20 Torr, 0.01 Torr to 15 Torr, 0.01 Torr to 10 Torr, 0.01 Torr to 5 Torr, 0.01 Torr to 1 Torr, 0.01 Torr to 0.1 Torr, 0.1 Torr to 100 Torr, 1 Torr to 100 Torr, 5 Torr to 100 Torr, 10 Torr to 100 Torr, 15 Torr to 100 Torr, 20 Torr to 100 Torr, 25 Torr to 100 Torr, 30 Torr to 100 Torr, 35 Torr to 100 Torr, 40 Torr to 100 Torr, 45 Torr 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.

[0039] In some embodiments, the first condition is that the total pressure of the source container is lower than the true vapor pressure of the tungsten precursor for a given first temperature. In some embodiments, the first condition is that the total pressure of the source container is lower than the true vapor pressure of the carbon-containing material for a given first temperature. In some embodiments, the tungsten precursor vapor contains a carbon-containing material. In some embodiments, the carbon-containing material includes a first carbon vapor. In some embodiments, the carbon-containing material includes a first plurality of carbon particles. In some embodiments, the carbon-containing material includes at least one of a first carbon vapor, a first plurality of carbon particles, or any combination thereof.

[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, the step of removing a first portion of the carbon-containing material from the tungsten precursor vapor includes passing the tungsten precursor vapor stream through a filter to remove at least a portion of the first plurality of carbon particles. In some embodiments, the step of removing a first portion of the carbon-containing material from the tungsten precursor vapor includes passing the tungsten precursor vapor stream through an adsorbent to remove at least a portion of the first carbon vapor. In some embodiments, the step of removing a first portion of the carbon-containing material from the tungsten precursor vapor includes passing the tungsten precursor vapor stream through a filter to remove at least a portion of the first plurality of carbon particles; and passing the tungsten precursor vapor stream through an adsorbent to remove at least a portion of the first carbon vapor.

[0041] In step 206, the tungsten precursor vapor stream is directed to a collection container. In some embodiments, the tungsten precursor vapor contains a carbon-containing material. In some embodiments, the tungsten precursor vapor contains less carbon-containing material than the tungsten precursor vapor before the removal step 204.

[0042] Figure 3 Is a flowchart of a method 300 for separating a carbon-containing material from a tungsten precursor according to some embodiments. As Figure 3 shown, the method 300 for separating a carbon-containing material from a tungsten precursor may include at least one of the following steps: step 302 of applying a second condition to the collection container to produce a tungsten precursor condensate and a second carbon vapor; step 304 of removing at least a portion of the second carbon vapor from the collection container; or any combination thereof. In some embodiments, the method 300 involves separating the tungsten precursor from at least a second portion of the carbon-containing material as described above.

[0043] In step 302, in some embodiments, a second condition is applied to the collection container to produce a tungsten precursor condensate and a second carbon-containing vapor. In some embodiments, producing the tungsten precursor condensate and the second carbon-containing vapor separates the tungsten precursor from the second portion of the carbon-containing vapor. In some embodiments, the second condition includes a second temperature of the collection container. In some embodiments, the second temperature of the collection container is a temperature in the range of 10°C to 100°C or any range or sub-range therebetween. In some embodiments, the second temperature of the collection container is a temperature in the following ranges: 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 container is a temperature sufficient to condense the tungsten precursor vapor. In some embodiments, the second temperature of the collection container is a temperature sufficient to produce the second carbon-containing vapor.

[0044] In some embodiments, the second condition includes a second pressure of the collection container. In some embodiments, the second pressure of the collection container is a pressure in the range of 0.01 Torr to 100 Torr or any range or sub-range therebetween. In some embodiments, the second pressure of the collection container is a pressure in the following ranges: 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, 0.01 Torr to 50 Torr, 0.01 Torr to 45 Torr, 0.01 Torr to 40 Torr, 0.01 Torr to 35 Torr, 0.01 Torr to 30 Torr, 0.01 Torr to 25 Torr, 0.01 Torr to 20 Torr, 0.01 Torr to 15 Torr, 0.01 Torr to 10 Torr, 0.01 Torr to 5 Torr, 0.01 Torr to 1 Torr, 0.01 Torr to 0.1 Torr, 0.1 Torr to 100 Torr, 1 Torr to 100 Torr, 5 Torr to 100 Torr, 10 Torr to 100 Torr, 15 Torr to 100 Torr, 20 Torr to 100 Torr, 25 Torr to 100 Torr, 30 Torr to 100 Torr, 35 Torr to 100 Torr, 40 Torr to 100 Torr, 45 Torr 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. In some embodiments, the second pressure of the collection container is a pressure sufficient to condense the tungsten precursor vapor. In some embodiments, the second pressure of the collection container is a pressure sufficient to produce the second carbon-containing vapor.

[0045] In some embodiments, a second condition is applied to the collection container to produce a tungsten precursor condensate and a second carbonaceous vapor. In some embodiments, the second condition is a condition where the volume of the tungsten precursor condensate is greater than that of the second carbonaceous vapor. In some embodiments, the tungsten precursor condensate contains a greater amount (e.g., mole fraction, volume, or mass fraction) of the tungsten precursor condensate than the carbonaceous condensate (if any). In some embodiments, the second condition is a condition where the volume of the second carbonaceous vapor remaining evaporated is greater than that of the tungsten precursor. In some embodiments, the second condition is a condition where the second carbonaceous vapor contains the carbonaceous material present in the tungsten precursor vapor evaporated in the source container.

[0046] In step 304, in some embodiments, at least a portion of the second carbonaceous vapor is removed from the collection container. The second carbonaceous vapor can be removed via an outlet of the collection container. The outlet can be fluidly coupled to a gas discharge line, a vacuum line, or other similar lines suitable for removing the second carbonaceous vapor from the collection container.

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

[0048] In step 402, in some embodiments, a third condition is applied to the source container to produce a third carbon-containing vapor. In some embodiments, the third condition includes a third temperature of the source container. In some embodiments, the third temperature of the source container is a temperature in the range of 60°C to 170°C or any range or sub-range between 60°C and 170°C. In some embodiments, the third temperature of the source container is a temperature in the following ranges: 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 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.

[0049] In some embodiments, the third condition includes a third pressure of the source container. In some embodiments, the third pressure of the source container is a pressure in the range of 0.01 Torr to 100 Torr or any range or sub-range therebetween. In some embodiments, the third pressure of the source container is a pressure in the following ranges: 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, 0.01 Torr to 50 Torr, 0.01 Torr to 45 Torr, 0.01 Torr to 40 Torr, 0.01 Torr to 35 Torr, 0.01 Torr to 30 Torr, 0.01 Torr to 25 Torr, 0.01 Torr to 20 Torr, 0.01 Torr to 15 Torr, 0.01 Torr to 10 Torr, 0.01 Torr to 5 Torr, 0.01 Torr to 1 Torr, 0.01 Torr to 0.1 Torr, 0.1 Torr to 100 Torr, 1 Torr to 100 Torr, 5 Torr to 100 Torr, 10 Torr to 100 Torr, 15 Torr to 100 Torr, 20 Torr to 100 Torr, 25 Torr to 100 Torr, 30 Torr to 100 Torr, 35 Torr to 100 Torr, 40 Torr to 100 Torr, 45 Torr 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.

[0050] In some embodiments, the third condition is a condition where the total pressure of the source container is lower than the true vapor pressure of the carbon-containing material for a given third temperature. In some embodiments, the third condition is a condition where the total pressure of the source container is higher than the true vapor pressure of the tungsten precursor for a given third temperature. In some embodiments, the first condition is a condition that enables the evaporation of the carbon-containing material while minimizing the amount of the evaporated tungsten precursor. In some embodiments, the third condition is a condition that prevents the evaporation of the tungsten precursor. In some embodiments, when the third condition is applied, the third carbon vapor contains a carbon-containing material with a larger volume than the tungsten precursor.

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

[0052] In step 404, in some embodiments, at least a portion of the third carbon vapor is removed from the source container. The third carbon vapor may be removed via an outlet of the source container. The outlet may be fluidly coupled to a gas discharge line, a vacuum line, or other similar lines suitable for removing the third carbon vapor from the source container.

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

[0054] Figure 5 is a flowchart of method 500 for separating a carbon-containing material from a tungsten precursor according to some embodiments. According to Figure 5As shown, the method 500 for separating a carbon-containing material from a tungsten precursor may include at least one of the following steps: step 502 of applying a fourth condition to a collection container to generate a fourth carbon-containing vapor; step 504 of removing at least a portion of the fourth carbon-containing vapor from the collection container; or any combination thereof. In some embodiments, method 500 is performed after step 112 (e.g., Figure 6 ). In some embodiments, method 500 is performed after step 114 (e.g., Figure 7 ). In some embodiments, method 500 involves separating the tungsten precursor from at least a fourth portion of the carbon-containing material as described above.

[0055] In step 502, in some embodiments, a fourth condition is applied to the collection container to generate a fourth carbon-containing vapor. In some embodiments, the fourth condition includes a fourth temperature of the collection container. In some embodiments, the fourth temperature of the collection container is a temperature in the range of 60°C to 170°C or any range or sub-range between 60°C and 170°C. In some embodiments, the fourth temperature of the collection container is a temperature in the following ranges: 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 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.

[0056] In some embodiments, the fourth condition includes the fourth pressure of the collection vessel. In some embodiments, the fourth pressure of the collection vessel is a pressure within the range of 0.01 Torr to 100 Torr or within any range or sub-range therebetween. In some embodiments, the fourth pressure of the collection vessel is a pressure within the following ranges: 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, 0.01 Torr to 50 Torr, 0.01 Torr to 45 Torr, 0.01 Torr to 40 Torr, 0.01 Torr to 35 Torr, 0.01 Torr to 30 Torr, 0.01 Torr to 25 Torr, 0.01 Torr to 20 Torr, 0.01 Torr to 15 Torr, 0.01 Torr to 10 Torr, 0.01 Torr to 5 Torr, 0.01 Torr to 1 Torr, 0.01 Torr to 0.1 Torr, 0.1 Torr to 100 Torr, 1 Torr to 100 Torr, 5 Torr to 100 Torr, 10 Torr to 100 Torr, 15 Torr to 100 Torr, 20 Torr to 100 Torr, 25 Torr to 100 Torr, 30 Torr to 100 Torr, 35 Torr to 100 Torr, 40 Torr to 100 Torr, 45 Torr 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.

[0057] In some embodiments, the fourth condition is a condition where the total pressure of the collection vessel is lower than the true vapor pressure of the carbonaceous material for a given fourth temperature. In some embodiments, the fourth condition is a condition where the total pressure of the collection vessel is higher than the true vapor pressure of the tungsten precursor for a given fourth temperature. In some embodiments, the first condition is a condition that causes the carbonaceous material to evaporate while minimizing the amount of the evaporated tungsten precursor. In some embodiments, the fourth condition is a condition that prevents the tungsten precursor from evaporating. In some embodiments, when the fourth condition is applied, the fourth carbon vapor contains a greater volume of carbonaceous material than the tungsten precursor.

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

[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 may be removed via an outlet of the collection vessel. The outlet may be fluidly coupled to a gas discharge line, a vacuum line, or other similar line suitable for removing the fourth carbon-containing vapor from the collection vessel.

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

[0061] Figure 7 is a schematic diagram of a system 700 for removing carbon-containing material from a precursor according to some embodiments. According to Figure 7As shown, in some embodiments, system 700 includes a first container 702, a second container 708, a first removal unit 704, and a second removal unit 706. The first container 702 may be fluidly coupled to the second container 708. In some embodiments, the first removal unit 704 includes a filter for removing carbonaceous material from the vapor. In some embodiments, the carbonaceous material removed by the filter is a plurality of carbonaceous particles. In some embodiments, the second removal unit 706 includes an adsorbent for removing carbonaceous material from the vapor. In some embodiments, the carbonaceous material removed by the adsorbent is carbonaceous vapor. Although the second removal unit 706 is depicted as being downstream of the first removal unit 704, it should be understood that other configurations are possible, including, for example and without limitation, the second removal unit 706 being upstream of the first removal unit 704. Additionally, additional removal units (e.g., 704, 706) may be added or removed from the system without departing from the scope of the present disclosure.

[0062] Example 1

[0063] 125 mg of WCl 5 precursor was added to a tin capsule inside an air-and-moisture free glovebox. The mass of the WCl 5 precursor was measured using an analytical balance and recorded. The tin capsule containing the WCl 5 precursor was hermetically sealed inside the glovebox. The total carbon value was measured to be an average of 126 ppm using a total carbon analyzer with NDIR detection.

[0064] Example 2

[0065] 0.01 g of WCl 5 precursor was added to a tin capsule inside an air-and-moisture free glovebox. The mass of the WCl 5 precursor was measured using an analytical balance and recorded. The tin capsule containing the WCl 5 precursor was hermetically sealed inside the glovebox. The total carbon value was measured using a total carbon analyzer with NDIR detection.

[0066] Example 3

[0067] 1.5 g of WCl 5 precursor was added to a tin capsule inside an air-and-moisture free glovebox. The mass of the WCl 5 precursor was measured using an analytical balance and recorded. The tin capsule containing the WCl 5 precursor was hermetically sealed inside the glovebox. The total carbon value was measured using a total carbon analyzer with NDIR detection.

[0068] Example 4

[0069] Add 125 mg of the WCl 6 precursor to a tin capsule inside a glove box free of air and moisture. Measure the mass of the WCl 6 precursor using an analytical balance and record it. Hermetically seal the tin capsule containing the WCl 6 precursor inside the glove box. Determine using a total carbon analyzer with NDIR detection, and the total carbon value is measured to be on average 126 ppm.

[0070] Example 5

[0071] Add 0.01 g of the WCl 6 precursor to a tin capsule inside a glove box free of air and moisture. Measure the mass of the WCl 6 precursor using an analytical balance and record it. Hermetically seal the tin capsule containing the WCl 6 precursor inside the glove box. Measure the total carbon value using a total carbon analyzer with NDIR detection.

[0072] Example 6

[0073] Add 1.5 g of the WCl 6 precursor to a tin capsule inside a glove box free of air and moisture. Measure the mass of the WCl 6 precursor using an analytical balance and record it. Hermetically seal the tin capsule containing the WCl 6 precursor inside the glove box. Measure the total carbon value using a total carbon analyzer with NDIR detection.

[0074] Aspect

[0075] Various aspects are described below. It should be understood that any one or more of the features recited in the following aspects can be combined with any one or more of the other aspects.

[0076] Aspect 1. A precursor comprising:

[0077] a tungsten precursor; and

[0078] a carbon-containing material,

[0079] wherein, as measured by total carbon analysis using non-dispersive infrared detection, the precursor comprises less than 0.015 wt% of the carbon-containing material based on the total weight of the precursor.

[0080] Aspect 2. The precursor according to Aspect 1, wherein, as measured by total carbon analysis using non-dispersive infrared detection, the precursor comprises less than 0.005 wt% of the carbon-containing material based on the total weight of the precursor.

[0081] Aspect 3. The precursor according to any one of Aspects 1 to 2, wherein, as measured by total carbon analysis using non-dispersive infrared detection, the precursor contains less than 0.001% by weight of the carbon-containing material based on the total weight of the precursor.

[0082] Aspect 4. The precursor according to any one of Aspects 1 to 3, wherein, as measured by total carbon analysis using non-dispersive infrared detection, the precursor contains less than 0.0002% by weight of the carbon-containing material based on the total weight of the precursor.

[0083] Aspect 5. The precursor according to any one of Aspects 1 to 4, wherein, as measured by total carbon analysis using non-dispersive infrared detection, the precursor contains from 0.0002% to 0.001% by weight of the carbon-containing material based on the total weight of the precursor.

[0084] Aspect 6. The precursor according to any one of Aspects 1 to 5, wherein the carbon-containing material contains chlorinated hydrocarbons.

[0085] Aspect 7. The precursor according to any one of Aspects 1 to 6, wherein the carbon-containing material contains at least one of the following: 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-dichloropropionyl 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-hexachloro-1,3-cyclopentadiene, trichlorocyclopentene, tetrachlorocyclopentene, pentachloronorbornene, or any combination thereof.

[0086] Aspect 8. A method comprising:

[0087] a) obtaining a source container containing a tungsten precursor and a carbon-containing material;

[0088] b) separating at least a first portion of the tungsten precursor from the carbon-containing material, wherein the separation comprises:

[0089] applying a first condition to the source container to produce a tungsten precursor vapor containing the carbon-containing material,

[0090] 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;

[0091] removing the first portion of the carbon-containing material from the tungsten precursor vapor;

[0092] flowing the tungsten precursor vapor to a collection vessel;

[0093] c) recovering the precursor in the collection vessel.

[0094] Aspect 9. The method according to aspect 8, wherein the step of removing the first portion of the carbon-containing material from the tungsten precursor vapor comprises:

[0095] flowing the tungsten precursor vapor through a filter to remove at least a portion of the first plurality of carbon-containing particles.

[0096] Aspect 10. The method according to any one of aspects 8 to 9, wherein the step of removing the first portion of the carbon-containing material from the tungsten precursor vapor comprises:

[0097] flowing the tungsten precursor vapor through an adsorbent to remove at least a portion of the first carbon-containing vapor.

[0098] Aspect 11. The method according to any one of aspects 8 to 10, wherein the step of removing the first portion of the carbon-containing material from the tungsten precursor vapor comprises:

[0099] flowing the tungsten precursor vapor through a filter to remove at least a portion of the first plurality of carbon-containing particles;

[0100] flowing the tungsten precursor vapor through an adsorbent to remove at least a portion of the first carbon-containing vapor.

[0101] Aspect 12. The method according to any one of aspects 8 to 11, wherein the first condition is a condition that the total pressure of the source vessel is lower than the true vapor pressure of the tungsten precursor for a given first temperature.

[0102] Aspect 13. The method according to any one of aspects 8 to 12, wherein the first condition is a condition that the total pressure of the source vessel is lower than the true vapor pressure of the carbon-containing material for a given first temperature.

[0103] Aspect 14. The method according to any one of aspects 8 to 13, further comprising:

[0104] d) separating the tungsten precursor from at least a second portion of the carbon-containing material, wherein the separating step d) comprises:

[0105] Apply a second condition to the collection container to produce tungsten precursor condensates and a second carbon-containing vapor;

[0106] Remove at least a portion of the second carbon-containing vapor from the collection container.

[0107] Aspect 15. The method according to aspect 14, wherein the second condition is a condition where the volume of the tungsten precursor condensate is greater than that of the second carbon-containing vapor.

[0108] Aspect 16. The method according to aspect 14, wherein when the second condition is applied, the tungsten precursor condensate contains a greater molar fraction of the tungsten precursor than the carbon-containing material.

[0109] Aspect 17. The method according to any one of aspects 8 to 16, further comprising:

[0110] e) Separating a third portion of the tungsten precursor from the carbon-containing material, wherein the separating step e) comprises:

[0111] Apply a third condition to the source container to produce a third carbon-containing vapor; and

[0112] Remove at least a portion of the third carbon-containing vapor from the source container;

[0113] wherein the separating step e) is performed before the separating step b).

[0114] Aspect 18. The method according to aspect 17, wherein the third condition is a condition where the total pressure of the source container is lower than the true vapor pressure of the carbon-containing material for a given third temperature.

[0115] Aspect 19. The method according to aspect 17, wherein the third condition is a condition where the total pressure of the source container is higher than the true vapor pressure of the tungsten precursor for a given third temperature.

[0116] Aspect 20. The method according to aspect 17, wherein when the third condition is applied, the third carbon-containing vapor contains a greater volume of the carbon-containing material than the tungsten precursor.

[0117] Aspect 21. The method according to any one of aspects 8 to 20, further comprising:

[0118] f) Verifying the low carbon content of the precursor present in the collection container, wherein the verifying step f) comprises:

[0119] Measuring the carbon content of the precursor to verify or not verify the low carbon content of the precursor;

[0120] When the low carbon content is not verified, remove at least a portion of the carbon-containing material from the precursor.

[0121] Aspect 22. The method according to aspect 21, wherein the low-carbon content of the precursor present in the collection container is measured by total carbon analysis using non-dispersive infrared detection.

[0122] Aspect 23. The method according to aspect 21, wherein the low-carbon content of the precursor present in the collection container is measured by total carbon analysis using thermal conductivity detection.

[0123] Aspect 24. The method according to any one of aspects 8 to 23, further comprising:

[0124] g) Separating the tungsten precursor from a fourth portion of the carbon-containing material, wherein the separating step g) comprises:

[0125] Applying a fourth condition to the collection container to produce a fourth carbon-containing vapor; and

[0126] Removing at least a portion of the fourth carbon-containing vapor from the collection container.

[0127] Aspect 25. The method according to aspect 24, wherein the fourth condition is a condition where the total pressure of the collection container is lower than the true vapor pressure of the carbon-containing material for a given fourth temperature.

[0128] Aspect 26. The method according to aspect 24, wherein the fourth condition is a condition where the total pressure of the collection container is higher than the true vapor pressure of the tungsten precursor for a given fourth temperature.

[0129] Aspect 27. The method according to aspect 24, when the fourth condition is applied, the fourth carbon-containing vapor comprises a greater volume of the carbon-containing material than the tungsten precursor.

[0130] It should be understood that changes can be made in detail without departing from the scope of the present disclosure, particularly in terms of the construction materials employed, and the shape, size, and arrangement of the components. This specification and the described embodiments are examples, where the true scope and spirit of the present disclosure are indicated by the appended claims.

[0131] Aspect 28. The method according to any one of aspects 8 to 27, wherein the precursor is recovered in the collection container, and wherein, as measured by total carbon analysis using non-dispersive infrared detection, the precursor comprises less than 0.02% by weight of the carbon-containing material based on the total weight of the precursor.

Claims

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

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

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

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

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

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

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

8. The precursor according to claim 1, wherein the carbon-containing material comprises at least one of a hydrocarbon polymer (optionally substituted), a haloalkane, a haloalkene, a halocycloalkane, a haloarene, or any combination thereof.

9. The precursor according to claim 1, wherein the carbon-containing material comprises at least one of the following: 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-hexachloro-1,3-cyclopentadiene, trichlorocyclopentene, tetrachlorocyclopentene, pentachloronorbornene, or any combination thereof.

10. A method comprising: a) obtaining a source container containing a tungsten precursor and a carbon-containing material; b) separating at least a first portion of the tungsten precursor from the carbon-containing material, wherein the separation comprises: Apply a first condition to the source container to produce tungsten precursor vapor containing the carbonaceous material, wherein the carbonaceous material comprises at least one of a first carbon-containing vapor, a first plurality of carbon-containing particles, or any combination thereof; Remove the first portion of the carbonaceous material from the tungsten precursor vapor; Flow the tungsten precursor vapor to a collection container; c) Recover the precursor in the collection container.

11. The method according to claim 10, wherein the step of removing the first portion of the carbonaceous 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.

12. The method according to claim 10, wherein the step of removing the first portion of the carbonaceous material from the tungsten precursor vapor comprises: Flowing the tungsten precursor vapor through an adsorbent to remove at least a portion of the first carbon-containing vapor.

13. The method according to claim 10, wherein the step of removing the first portion of the carbonaceous 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; flowing the tungsten precursor vapor through an adsorbent to remove at least a portion of the first carbon-containing vapor.

14. The method according to claim 10, wherein the first condition is a condition in which the total pressure of the source container is lower than the true vapor pressure of the tungsten precursor for a given first temperature.

15. The method according to claim 10, wherein the first condition is a condition in which the total pressure of the source container is lower than the true vapor pressure of the carbonaceous material for a given first temperature.

16. The method according to claim 10, which further comprises: d) Separating the tungsten precursor from at least a second portion of the carbonaceous material, wherein the separating step d) comprises: Applying a second condition to the collection container 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 container.

17. The method according to claim 16, wherein the second condition is a condition in which the volume of the tungsten precursor condensate is greater than the second carbon-containing vapor.

18. The method according to claim 16, wherein when the second condition is applied, the tungsten precursor condensate comprises a greater mole fraction of the tungsten precursor than the carbonaceous material.

19. The method according to claim 10, which further comprises: e) Separating the tungsten precursor from a third portion of the carbonaceous material, wherein the separating step e) comprises: Applying a third condition to the source container to produce a third carbon-containing vapor; and Removing at least a portion of the third carbon-containing vapor from the source container; wherein the separating step e) is performed before the separating step b).

20. The method according to claim 19, wherein the third condition is a condition in which the total pressure of the source container is lower than the true vapor pressure of the carbonaceous material for a given third temperature.

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