Patent ID: 12187619

DETAILED DESCRIPTION

For the purpose of promoting an understanding of the principles of the present disclosure, reference will now be made to the embodiments illustrated in the drawings and specific language will be used to describe the same. It will, nevertheless, be understood that no limitation of the scope of the disclosure is thereby intended; any alterations and further modifications of the described or illustrated embodiments, and any further applications of the principles of the disclosure as illustrated therein are contemplated as would normally occur to one skilled in the art to which the disclosure relates. All limitations of scope should be determined in accordance with and as expressed in the claims.

Whether a term is capitalized is not considered definitive or limiting of the meaning of a term. As used in this document, a capitalized term shall have the same meaning as an uncapitalized term, unless the context of the usage specifically indicates that a more restrictive meaning for the capitalized term is intended. However, the capitalization or lack thereof within the remainder of this document is not intended to be necessarily limiting unless the context clearly indicates that such limitation is intended.

Overview

I. Definitions

“Anhydrous hydrogen fluoride” or “AHF” as used herein refers to a colorless toxic gas (under standard environment conditions) with a sharp odor, at room temperature exists predominantly in the form of H2F2 dimer. AHF is a colorless, mobile, volatile liquid at temperatures below 19.9° C. degrees. AHF is miscible with water in any proportion with the formation of hydrofluoric acid. AHF reacts with water, which results in an azeotropic mixture with a concentration of 35.4% HF. AHF reacts with water molecules in the air to form HF gas, among other products, and thus AHF and HF are used interchangeably in this present disclosure.

“Corrosion” as used herein refers to the disintegration of a material due to chemical reactions with its surroundings.

“Fuel salt” as used herein refers a molten salt containing fissionable fuel and optionally other components. The fissionable fuel may be, for example, uranium, plutonium, or thorium.

“High purity” as used herein refers to a purity greater than about 85%, more particularly, greater than about 90%, about 92%, about 93%, about 94%, about 95%, about 96%, about 97%, about 98%, about 99% or about 100%, in each case with respect to a particular contaminant.

“Hydroflourination” as used herein is a process that involves sparging of a molten salt with both hydrogen and hydrogen-fluoride to remove trace impurities such as oxygen and moisture.

“Hydrogen fluoride” or “HF” as used herein refers to a colorless, corrosive gas or liquid made up of a hydrogen atom and a fluorine atom. When hydrogen fluoride is dissolved in water, it is referred to as hydrofluoric acid.

“Medical isotope” as used herein refers to metal, a metal-like, or non-metal isotope appropriate for use in medical contexts such as use in imaging or therapeutic use and includes clinical research and preclinical applications. In some embodiments, a medical isotope is or includes a radioactive isotope, i.e., a radioisotope. Molybdenum-99 (Mo-99) is one representative, non-limiting example.

“Molten salt” as used herein refers to a salt which is solid at standard temperature and pressure but enters the liquid phase due to elevated temperature. Molten salts have applications in waste oxidation, catalytic coal gasification, concentrated solar power, and advanced nuclear reactors.

“On-demand” refers to production as needed or whenever required.

“Oxidizing agent” or “oxidizer” refers to a substance that has the ability to oxidize other substances, i.e., to accept their electrons. Common oxidizing agents are oxygen, hydrogen peroxide and the halogens.

“Oxidize” or “oxidizing” as used herein refers to undergoing, or causing to undergo, a reaction in which electrons are lost to another species.

“Purification” as used herein refers to the act or process of removing physical impurities, i.e., clarification, refinement.

“Redox potential” as used herein refers to an intrinsic property of all electrically conductive solutions, such as ionic molten salts, which indicates the tendency for that solution and all dissolved constituents to undergo an oxidation or reduction reaction. The redox potential is solely determined by that solution's chemical composition.

“Sodium bifluoride” as used herein refers to an inorganic compound with the formula NaHF2. It is a salt of sodium cation (Na+) and bifluoride anion (HF2−). It is a white, water-soluble solid that decomposes upon heating.

“Vapor etching” as used herein refers to a process used in sacrificial layers are isotropically etched using gaseous acids such as HF.

“Vessel” as used herein may refer to a hollow container.

II. Vessel

Disclosed herein are various examples related to systems and methods for hydrogen fluoride gas generation. In one embodiment of the present disclosure, an anhydrous hydrogen fluoride generator vessel (also referred to herein as the “AHF generator vessel”) is provided. Vessels configured according to various embodiments of the present disclosure may include a container assembly, one or more shelves, and a center pipe or a center pipe assembly.

In many embodiments, the container assembly may include a base and a wall forming a cavity. The container assembly may include a lid assembly that may be removably coupled to the wall, and one or more feet. The lid assembly may include a lid, and a top adapter coupled to the cavity.

In several embodiments, the center pipe assembly may include a base adapter, a center pipe, and a bottom adapter. The base adapter may be mechanically coupled to the base and the center pipe. The center pipe may be fluidically coupled to the base adapter so that fluids, liquids or gases, may flow into the cavity. The center pipe may include one or more perforations. The bottom adapter may include an elbow or other inlet for fluid flow through the bottom adapter, into the center pipe, and out the perforations of the center pipe into the cavity. A plate may be coupled to an end of the center pipe.

In various embodiments, the one or more shelves may include shelf supports for supporting any of the one or more shelves. For example, a first one of shelves may be supported by the base adapter, a second one of the shelves may be supported by a shelf support that is removably fastened to the first one of the shelves, and so forth. In some examples, each of the one or more shelves may extend radially away from the center pipe toward an outer edge of the respective one of the one or more shelves. The one or more shelves may be adapted for loading sodium bifluoride into the cavity.

In an example operation, sodium bifluoride may be loaded onto the shelves which are positioned perpendicular to the center pipe of the center pipe assembly. The use of a plurality of shelves may allow for increased surface area of the sodium bifluoride and efficient production of the hydrogen fluoride gas. The shelves containing the sodium bifluoride may be placed in the cavity formed by the base and the wall of the container assembly. The lid of the lid assembly may be removably coupled to the wall. Trace-heating wrapped around a main body of the container may provide the heat to thermally degrade the sodium bifluoride into HF and sodium fluoride (NaF). A source for a carrier gas such as Argon (Ar) may be coupled to the elbow or inlet to provide the carrier gas. Examples disclosed herein may allow the carrier has to move the generated HF out of the cavity towards the downstream application, e.g., purification of fluoride salts. The center pipe assembly may allow argon to enter and flow through the perforations in the center pipe over each of the shelves and eventually out of the cavity through the top adapter.

III. Method

Disclosed are methods for generating AHF gas on demand. The methods disclosed herein advantageously prevent the need for transport and storage of AHF gas and thereby offer certain safety advantages. In several embodiments, AHF may react with the moisture in the air to form HF, and thus, AHF and HF may be used interchangeably when AHF mixes with air.

In a first aspect, a method is disclosed for generating AHF gas on-demand, including (i) providing solid sodium bifluoride in a vessel disclosed herein; and (ii) heating the solid sodium bifluoride at a suitable temperature and/or for a suitable period of time to generate a quantity of AHF gas.

The AHF gas produced by the method above may be used for any suitable purpose. In one embodiment, the AHF gas is used for purifying molten salts. In another embodiment, the AHF gas is used for vapor etching and more particularly, for removing films from substrate materials.

In certain embodiments, the AHF gas so-produced is used for conditioning (e.g., pre-conditioning or re-conditioning) of molten salts. Molten salts, sometimes referred to as salt melts, are a family of products used for a wide range of applications including high-temperature process heating, heat treating and annealing of steel, and thermal storage in solar thermal power plants. In one embodiment, the method disclosed herein is suitable for use in conditioning (e.g., pre-conditioning, re-conditioning) molten salts for use in molten salts reactors (MSR).

In certain embodiments, the methods disclosed herein are used to condition molten fluoride salts. Molten salt fluorides as coolants offer good transport properties, strong irradiation resistance, high thermal stability and boiling points. They share some advantages with liquid metal coolants like reactor operation at low pressure. This constitutes a significant safety and cost advantage.

Molten salts are known to contain impurities. These impurities come from various sources; some are inherently part of the raw salt (e.g., complexed water, even when the salt is considered anhydrous), some are introduced into the salt during processing (e.g., absorbed from the atmosphere), and some result from processes utilizing the salt (e.g., corrosion processes).

Representative, non-limiting impurities that may be found in molten salts conditioned according to the methods disclosed herein include oxides and hydroxides formed in the salt by its main constituents during contact with H2O and O2 in air, as well as metal impurities (e.g., chromium, iron and nickel) and non-metal impurities (e.g., sulfides and phosphates). Such impurities tend to accelerate corrosion of structural materials (e.g., structural alloys), for example the reactor vessel and heat exchangers within a molten salt reactor. Mitigating this corrosion is critical for the design, life cycle and economics of molten salt systems. Moreover, when such impurities reach a critical concentration, they impact thermophysical properties of the molten salt, including the heat capacity, thermal conductivity and latent heat of the salts.

In particular, moisture is a source of oxygen, which drives hydrolysis of salt and results in the formation of hydrofluoric acid in fluoride salt and hydrochloric acid in chloride salts. These acids react with alloying elements within the molten salt system, increasing corrosion. The moisture may be introduced during processing or inherent to the salt, i.e., complexed water present in an “anhydrous” molten salt.

In another particular embodiment, the impurity is oxide (O2−). Oxide ion reacts with alloying elements (e.g., chromium) and destabilizes the protective layer on metal surfaces. Oxide ions also increases basicity of melt and the solubility increases solubility of alloying elements within the molten salt system.

In another embodiment, the impurity is iron (Fe). FeF2 in fluoride salts may react with and leach chromium from the alloy within the molten salt system.

In another embodiment, the impurity is nickel (Ni). NiF2in fluoride salts may react with and leach chromium from the alloy.

In one embodiment, the impurity is chromium (Cr).

In one aspect, a method is disclosed for conditioning (e.g., pre-conditioning, re-conditioning) molten salts, including (i) providing a quantity of molten salts; (ii) providing solid sodium bifluoride in a vessel disclosed herein; (iii) heating the solid sodium bifluoride at a suitable temperature and/or for a suitable period of time to generate a quantity of hydrogen fluoride (HF) gas; and (iv) exposing the molten salts to the HF gas for a suitable time, thereby pre-conditioning the molten salts. In certain embodiments, the method does not include exposing the molten salt to anhydrous hydrogen fluoride gas.

In another aspect, a method is disclosed for reducing oxidizing contaminants in molten salts, including (i) providing a quantity of molten salts; (ii) providing solid sodium bifluoride in a vessel disclosed herein; (iii) heating the solid sodium bifluoride at a suitable temperature and/or for a suitable period of time to generate a quantity of hydrogen fluoride (HF) gas; and (iv) exposing the molten salts to the HF gas for a suitable time, thereby reducing oxidizing contaminants present in the molten salts. In certain embodiments, the method does not include exposing the molten salt to anhydrous hydrogen fluoride gas.

In a further aspect, a method is disclosed for purifying molten salts, including (i) providing a quantity of molten salts; (ii) providing solid sodium bifluoride in a vessel disclosed herein; (iii) heating the solid sodium bifluoride at a suitable temperature and/or for a suitable period of time to generate a quantity of hydrogen fluoride (HF) gas; and (iv) exposing the molten salts to the HF gas for a suitable time, thereby purifying the molten salts. In certain embodiments, the method does not include exposing the molten salt to anhydrous hydrogen fluoride gas.

In a still further aspect, a method is disclosed for mitigating corrosion in a molten salt system, including (i) providing a quantity of molten salts; (ii) providing solid sodium bifluoride in a suitable vessel; (iii) heating the solid sodium bifluoride at a suitable temperature and/or for a suitable period of time to generate a quantity of hydrogen fluoride (HF) gas; (iv) exposing molten salts to the HF gas for a suitable time, and (v) utilizing the molten salts in the molten salt system, wherein corrosion of the molten salt system is mitigated relative to a molten salt system using molten salts not processed by steps (i)-(iv). In certain embodiments, the method does not include exposing the molten salt to anhydrous hydrogen fluoride gas.

In a further embodiment, a method is disclosed for controlling redox potential in a molten salts system, including (i) providing a quantity of molten salts; (ii)) providing solid sodium bifluoride in a suitable vessel; (iii) heating the solid sodium bifluoride at a suitable temperature and/or for a suitable period of time to generate a quantity of hydrogen fluoride (HF) gas; (iv) exposing molten salts to the HF gas for a suitable time; and (v) utilizing the molten salts in the molten salt system, wherein the redox potential is controlled relative to a molten salt system using molten salts not processed by steps (i)-(iv). In a particular embodiment, the redox potential is kept within mildly reducing conditions. In certain embodiments, the method does not include exposing the molten salt to anhydrous hydrogen fluoride gas.

In the methods disclosed above, the molten salt system may be any suitable molten salt system. In certain embodiments, the molten salt system is a molten salt nuclear reactor. Molten salt nuclear reactors operate at high temperatures, for example between about 400 to about 800° C., and frequently between 700 and about 800° C., and offer increased efficiency and safety compared to conventional reactors. In one embodiment, the molten salt system is a liquid fueled non-power molten salt reactor.

In another embodiment, a method is disclosed for controlling corrosion of a structural alloy, including (i) providing a quantity of molten salts; (ii) providing solid sodium bifluoride in a suitable vessel; (iii) heating the solid sodium bifluoride at a suitable temperature and/or for a suitable period of time to generate a quantity of hydrogen fluoride (HF) gas; (iv) exposing molten salts to the HF gas for a suitable time, and (v) contacting the structural alloy with the molten salt, wherein corrosion of the molten salt system is mitigated relative to a molten salt system using molten salts not processed by steps (i)-(iv).

In one embodiment, the structural alloy is selected from nickel, chromium or iron. In a particular embodiment, the structural alloy is stainless steel.

In the methods disclosed above, the molten salt may be any suitable molten salt or combination thereof. Representative, non-limiting examples of molten salts include molten halide, molten nitrate, molten carbonate, molten sulfate, molten hydroxide or molten oxide.

In one embodiment, the molten salt is a fluoride molten salt. In a particular embodiment, the molten salt is a lithium-based fluoride molten salt and more particularly, a lithium-based fluoride molten salt selected from LiF, LiF—BeF2 (also known as Flibe), LiF—NaF—KF (also known as FLiNaK), LiF—NaF—BeF2, LiF—NaF—ZrF4, LiF—NaF—ZrF4 and LiF—ZrF4.

In the methods disclosed above, the molten salt prior to treatment does not meet the level of purity necessary to prevent considerable corrosion. Industrial source purity of a fluoride salt may be as high as 99.99% (trace metal) but this does not include the presence of water and therefore does not fully describe the corrosivity of the salt

In certain embodiments, the methods disclosed herein includes one or more additional steps. In one embodiment, the method further including mixing the HF gas with hydrogen gas before the molten salts are exposed to the HF gas in (iv).

The suitable temperature in (iii) may vary. In certain embodiments, the temperature is between about and 90 and 140° C., more particularly, about 100-130° C. and even more particularly, about 120° C. degrees.

The suitable time in (iii) may vary. In certain embodiments, the suitable time is between about and about 12 and about 48 hours; more particularly, about 16 and about 36 hours, or even more particularly, about 18 and 24 hours. In one embodiment, the suitable time is about 24 hours. The suitable time may be, for example, about 18, about 20, about 22, about 24 or about 26 hours.

The suitable time in (iv) may vary. In certain embodiments, the suitable time is between about 12 and about 48 hours; more particularly, about 16 and about 36 hours, or even more particularly, about 18 and 24 hours. In one embodiment, the suitable time is about 24 hours. The suitable time may be, for example, about 18, about 20, about 22, about 24 or about 26 hours.

The degree to which oxidizing contaminants are reduced may vary. In certain embodiments, the impurities are reduced by about 10% to about 99%, more particularly, about 10%, about 20%, about 30%, about 40%, about 50%, about 60%, about 70%, about 80%, about 85%, about 90%, about 95% or about 95% or more compared to the molten salt not conditioned by the disclosed method.

In a particular embodiment, the oxide level is reduced by the method to disclosed herein to about 200 ppm or less, about 180 ppm or less, about 160 ppm or less, about 140 ppm or less, about 120 ppm or less, about 100 ppm or less, about 80 ppm or less, about 60 ppm, about 40 ppm or less or about 20 ppm or less.

In one embodiment, the total oxygen content in molten salts is reduced below about 80 ppm. In certain embodiments, the total oxygen content is reduced below about 75 ppm, about 70 ppm, about 65 ppm, about 60 ppm, about 55 ppm, about 50 ppm, about 45 ppm, about 40 ppm, about 35 ppm, about 30 ppm, about 25 ppm, about 20 ppm, about 15 ppm or about 10 ppm or less.

The degree of purification may vary. In certain embodiments, the impurities are reduced by about 10% to about 99%, more particularly, about 10%, about 20%, about 30%, about 40%, about 50%, about 60%, about 70%, about 80%, about 85%, about 90%, about 95% or about 95% or more compared to the molten salt not conditioned by the disclosed method.

The degree of mitigation may vary. In a particular embodiment, the 10% to about 99%, more particularly, about 10%, about 20%, about 30%, about 40%, about 50%, about 60%, about 70%, 80%, about 85%, about 90%, about 95% or about 95% or more compared to the molten salt not conditioned by the disclosed method.

In one embodiment, the reduction in corrosion may vary. In a particular embodiment, the method produces a reduction in corrosion of about 10% or more and more particularly, about 10%, about 20%, about 30%, about 40%, about 50%, about 60%, about 70%, 80%, about 85%, about 90%, about 95% or about 95% or more compared to the molten salt not preconditioned by the disclosed method.

In one embodiment, the method produces a reduction in corrosion rate compared to molten salts not preconditioned according to the disclosed method. In a particular embodiment, the method produces a reduction in corrosion rate of about 10% or more. More particularly, about 10%, about 20%, about 30%, about 40%, about 50%, about 60%, about 70%, 80%, about 85%, about 90%, about 95% or about 95% or more compared to the molten salt not preconditioned by the disclosed method.

In one embodiment, the corrosion rate is less than about 0.25 mg/cm{circumflex over ( )}2 over 1000 hrs, in a flowing loop.

Corrosion may be tested in any suitable manner. In one embodiment, coupons of the structural alloy (e.g., stainless steel) are exposed to the pre-conditioned (cleaned) salt in a flowing loop. In another embodiment, a coupon of the structural alloy is immersed in a pre-conditioned salt for a specified time.

In one embodiment, the corrosion test simulates the reactor cooling circuit by thermal convection loop. Tested material is shaped into tubing and joined to form a loop with one vertical leg heated and the second vertical leg cooled. Natural convection then ensures molten salt circulation in the loop, so that the motion of the corrosive medium and temperature gradients are included in the test layout.

In certain embodiments, the vessels and methods described herein can be used to generate gases other than hydrogen fluoride, for example other hazardous and/or corrosive gases. In one embodiment, a vessel for generation of a hazardous or corrosive gas includes: a container assembly, including: a wall with a first end and a second end, and a base connected to the first end of the wall, forming a cavity; one or more shelves adapted to be placed in the cavity; a center pipe assembly; and a lid assembly adapted to be removably coupled to the second end of the wall. In one embodiment, a method for producing on-demand hazardous or corrosive gas includes: loading precursor substance onto one or more shelves of a vessel for generation of a hazardous or corrosive gas as described herein; heating the vessel to a temperature at which the precursor substance hydrolyzes or degrades to form the hazardous or corrosive gas; and providing a carrier gas to flow through the vessel, wherein the carrier gas causes the hazardous or corrosive gas to flow out of the vessel.

EXEMPLARY EMBODIMENTS

Referring now to the figures, for the purposes of example and explanation of the fundamental processes and components of the disclosed systems and methods, reference is made toFIG.1, which illustrates an exemplary, high-level overview100of one embodiment of the AHF generator vessel102. As will be understood and appreciated, the exemplary, high-level overview100shown inFIG.1represents merely one approach or embodiment of the present system, and other aspects are used according to various embodiments of the present system.

As shown inFIG.1, a side perspective view of an exemplary AHF generator vessel100is shown, according to one embodiment of the present disclosure. In various embodiments, the AHF generator vessel100may be in fluid connection with a system so that the AHF produced in the AHF generator vessel100may flow out of the AHF generator vessel100and to an apparatus in which the AHF is utilized.

In multiple embodiments, the vessel100may include a container assembly102, one or more shelves104, and a center pipe assembly106. In many embodiments, the container assembly102may include a container base108having a top surface130and a bottom surface132, a container wall110, a flange112, and a lid assembly116. In some embodiments, the base108and wall110connect to form a cavity, and the one or more shelves104and center pipe assembly106are positioned within the cavity. In one or more embodiments, the wall110and the flange112connect at an end opposite the connection of the base108and wall110. In at least one embodiment, the container assembly102may include one or more feet114connected to the bottom surface132of the base108. In many embodiments, each of the components in the container assembly102and the center pipe assembly106, and each of the one or more shelves104, are made of stainless steel or another corrosion-resistant material, such as copper, bronze, brass, titanium, galvanized steel, or alloys thereof.

In several embodiments, the container assembly102may include a lid assembly116that may be removably coupled to the flange112at the opposite end of the vessel100from the container base108. In certain embodiments, the lid assembly116may include a lid118having a top surface134and a bottom surface136(bottom surface136shown inFIG.6B), and a top adapter120mechanically coupled to the top surface134of the lid118and fluidly coupled to the cavity. In one embodiment, the top adapter120may include a fluid outlet121(including, but not limited to, an elbow or other outlet device) for fluid flow from the cavity through the top adapter120and out the fluid outlet121. In many embodiments, the fluid outlet121may be in fluid connection with piping (not shown inFIG.1) so that the AHF/carrier gas mixture may flow to a second apparatus within the system to be utilized. In at least one embodiment, the lid assembly116may also include a gasket119. In one or more embodiments, the gasket119may be positioned in between the bottom surface136of the lid118and the flange112. In many embodiments, the lid assembly may be removably coupled to the flange112via one or more bolts138and an equal number of one or more nuts140. In some embodiments, the lid116, the gasket119, and the flange112may each define one or more openings (not shown inFIG.1) so that each of the one or more bolts138may pass through an opening of the one or more openings in the lid116, the gasket119, and the flange112, and the one or more nuts140mechanically couples to the one or more bolts138. In one embodiment, the lid assembly116coupled to the flange112ensures that the AHF/carrier gas mixture only flows through the top adapter120and does not leak out of the vessel100at any other point.

In several embodiments, the center pipe assembly106may include a base adapter122, a center pipe124, and a bottom adapter126. In one embodiment, the center pipe124may include one or more perforations128. In some embodiments, the base adapter122may be mechanically coupled to the top surface130of the base108and the center pipe124. In at least one embodiment, the bottom adapter126may be mechanically coupled to the bottom surface132of the base108and may also be mechanically coupled to a fluid inlet127(including, but not limited to, an elbow or other inlet device) for fluid flow through the bottom adapter126. In many embodiments, fluid inlet127, the bottom adapter126, base adapter122, and center pipe124may be fluidically coupled, so that the fluid may flow into the fluid inlet127, through the bottom adapter126, through the base adapter122, into the center pipe124, and out the perforations128of the center pipe124and into the cavity.

In various embodiments, each of the one or more shelves104may include a shelf base204that includes a bottom surface208and a top surface206(the shelf base202, bottom surface208, and top surface206shown inFIG.2), and each of the one or more shelves104may define an opening212(as shown inFIG.2) so that the center pipe124may extend through the opening212of each of the one or more shelves104, so that the one or more shelves104are stacked upon each other and around the center pipe124. In many embodiments, each of the one or more shelves104may include one or more shelf supports142to support the one or more shelves104.

In an example operation, in at least one embodiment, sodium bifluoride (NaHF2) may be loaded onto the one or more shelves104, which are positioned perpendicular to the center pipe124of the center pipe assembly106. Continuing with the example, in many embodiments, the use of one or more shelves104may allow for increased surface area of the sodium bifluoride, which allows for a more efficient production of hydrogen fluoride gas. In some embodiments, the one or more shelves104containing the sodium bifluoride may be placed in the cavity formed by the base108and the wall110of the container assembly102, and the lid118of the lid assembly116may be removably coupled to the wall110or flange112. In several embodiments, external heaters (e.g., trace heating wrapped around the vessel100) (external heaters not shown) may provide heat to thermally degrade the sodium bifluoride into HF gas and sodium fluoride (NaF). In many embodiments, a source for a carrier gas, such as Argon (Ar) or other inert gases, may be coupled to bottom adapter126at the elbow or inlet to provide the carrier gas into the cavity. In one or more embodiments, the flow of the carrier gas into the cavity via the center pipe assembly106may allow the carrier gas to flow over each of the one or more shelves104and cause the generated HF gas to flow out of the cavity with the carrier gas via the top adapter120and continue flowing towards a downstream application, e.g., purification of fluoride salts.

Turning now toFIGS.2A,2B, and2C, a perspective view, a front view, and a side view of an exemplary salt shelf202of the one or more shelves104are shown, according to one embodiment of the present disclosure. In several embodiments, each shelf202of the one or more shelves104may include a shelf base204having a top surface206, a bottom surface208, a raised outer edge211, and a raised inner edge210, and may define an opening212at the center of the shelf base204. In at least one embodiment, the shelf base204is circular, and the opening212is circular, though the shelf base204and/or the opening212may be any other shape. In many embodiments, the raised outer edge211protrudes from the top surface206of the shelf base204to create an outer rim on the top surface206of the shelf base204. In one or more embodiments, the raised inner edge210is the edge of the opening212and protrudes upwards from the top surface206of the shelf base204to create an inner rim on the top surface206of the shelf base204. In at least one embodiment, the raised outer edge211and raised inner edge210lessens the risk of the sodium bifluoride placed onto the top surface206of the shelf base204to fall off while each shelf202is being placed in the cavity.

In several embodiments, the shelf202also includes one or more shelf supports142. In a particular embodiment, the shelf202includes three shelf supports142, though the shelf202may include any number of shelf supports142. In one or more embodiments, each shelf support142aof the one or more shelf supports142includes a top end214protruding upwards from the top surface206of the shelf base204and a bottom end216protruding downwards from the bottom surface208of the shelf base204. In at least one embodiment, the top end214is fastened to the bottom end216. In another embodiment, the top end214and the bottom end216form a single body. In certain embodiments, the shelf base204may define one or more shelf support openings (not shown in the figures) so that the top end214may fasten or mechanically couple to the bottom end216through a shelf support opening in the shelf base204. In another embodiment, if the shelf support142ais a single body, the shelf support142amay fit through the shelf support opening and be fastened to the shelf base204. In some embodiments, the shelf support openings may be arranged so that each shelf support opening is an equal distance apart from the adjacent shelf support openings around the shelf base204. For example, in one embodiment, if there are three shelf support openings, then each shelf support opening may be 120° away from the adjacent shelf support openings (i.e., a shelf support opening located at 0°, 120°, and 240° around the shelf base204). In at least one embodiment, there may be any number of shelf support openings, and, preferably, the shelf base204defines three shelf support openings.

In many embodiments, the top end214includes a flat end surface to provide consistent support to the shelf202above. In some embodiments, the height of each shelf support142ais larger than the height of the raised outer edge211and the raised inner edge210(the raised outer edge211and the raised inner edge210may have the same height or different heights), so that the one or more shelf supports142of a first shelf202awill be contacted by the bottom surface208of a second shelf202bbeing placed on top of the first shelf202ainstead of the inner edge210and/or outer edge211of the first shelf202a.

For example, in one embodiment, a first shelf202aof the one or more shelves104may be placed into the cavity, around the center pipe124(i.e., the center pipe124extends through the opening212of the first shelf202a) and moved down the length of the center pipe124until the bottom surface208of the first shelf202ais in contact with a surface of the base adapter122(i.e., the first shelf202ais supported by the base adapter122). Continuing with the example, in one embodiment, a second shelf202bof the one or more shelves104may be placed into the cavity, around the center pipe124, and moved down the length of the center pipe124until the bottom surface208of the second shelf202bin in contact with and supported by the one or more shelf supports142of the first shelf202a. Still continuing with the example, in one embodiment, a third shelf202cmay be placed upon and supported by the one or more shelf supports142of the second shelf202b, a fourth shelf202dmay be placed upon and supported by the one or more shelf supports142of the third shelf202c, and so on.

In certain embodiments, any number of shelves202may be placed utilized in the vessel100. In a preferred embodiment, the vessel100may contain six shelves202. In some embodiments, each shelf202of the one or more shelves104may be positioned perpendicular to and extend radially away from the center pipe124toward the outer edge211of the respective shelf202. In many embodiments, sodium bifluoride may be loaded onto each shelf202of the one or more shelves104, preferably in between the inner edge210and outer edge211of each shelf202, and each shelf202of the one or more shelves104placed into the cavity with the center pipe124extending through the opening212of each shelf202of the one or more shelves104.

In multiple embodiments, each shelf202is made of stainless steel, though it may be made of other corrosion resistant materials, such as copper, titanium, galvanized steel, or alloys thereof. In at least one embodiment, the shelf base204may have an outer diameter that is smaller than the inner diameter of the container wall110. In many embodiments, the opening212may have a diameter that is larger than the outer diameter of the center pipe124so the center pipe124can fit through the opening212. In one or more embodiments, shelf base204may have a certain thickness (i.e., the distance between the top surface206and the bottom surface208of the shelf base204).

Turning now toFIG.3, an exemplary center pipe124and base adapter122are shown, according to one embodiment of the present disclosure. In various embodiments, the center pipe124and the base adapter122are fluidically connected, meaning that fluid can flow from the base adapter122to the center pipe124. In many embodiments, the center pipe124includes a first end302, a second end304, a main expanse of pipe306between the first end302and second end304, and an outer surface305. In at least one embodiment, the center pipe124defines an opening at the first end302that extends from the first end302to the second end304, such that the center pipe124is substantially hollow, which allows the carrier gas to flow through the center pipe124. In some embodiments, an end plate308is fastened to the second end304such that the carrier gas cannot flow out of the second end304of the center pipe124. In certain embodiments, the end plate308may be fastened to the second end304via welding and/or fasteners. In an alternative embodiment, the end plate308may be an end cap that mechanically couples to the second end304or may be a plug that plugs the opening at the second end304. In one embodiment, the center pipe124is cylindrical and the opening that extends from the first end302to the second end304is circular, though the center pipe124and the opening may be any shape. In a preferred embodiment, the center pipe124is shaped and sized so that the center pipe124can fit inside of and extend through the opening212of each shelf202of the one or more shelves104.

In several embodiments, the base adapter122includes a first end310and a second end312. In many embodiments, the base adapter122defines an opening at the first end310and the second end312and that extends through the base adapter122between the first end310and the second end312, such that the base adapter122is hollow and includes an inner surface. In one or more embodiments, the first end310of the base adapter122is attached to the top surface130of the container base108. In some embodiments, the first end310may be attached to the top surface130of the base308via welding, fasteners, or other connection devices.

In multiple embodiments, the second end312of the base adapter122is mechanically coupled or fastened to the first end302of the center pipe124, such that the opening at the second end312of the base adapter122and the opening at the first end302of the center pipe124are fluidically connected. In one or more embodiments, the first end302of the center pipe124may be mechanically coupled to the second end312of the base adapter122. In one embodiment, for example, as shown inFIG.3, the first end302of the center pipe124may have screw threading314around the outer surface305, and the inner surface of the second end312of the base adapter122may have screw threading, such that the first end302of the center pipe124may screw into the opening at the second end312of the base adapter122and couple to the screw threading on the inner surface of the base adapter122. In other embodiments, the first end302of the center pipe124may be welded to the second end312of the base adapter122, or may be connected via fasteners or otherwise mechanically coupled together. In one embodiment, the center pipe124has an outer diameter that is smaller than the diameter of the opening at the second end312of the base adapter122.

In an alternative embodiment, the base adapter122may have an outer diameter that is smaller than the opening at the first end302of the center pipe124. In this alternative embodiment, the center pipe124may have an inner surface that has screw threads, and the base adapter122may have an outer surface that has screw threads around it. Continuing with this alternative embodiment, the inner surface of the first end302of the center pipe124screws onto the outer surface of the second end312of the base adapter122such that the second end312of the base adapter122extends into and is substantially covered by the first end302of the center pipe124.

In various embodiments, the main expanse306of the center pipe124includes the one or more perforations128. In many embodiments, the one or more perforations128are openings defined by the main expanse306extend from the hollow interior of the center pipe124to the outer surface305, so that the carrier gas can flow from the interior of the center pipe124to the one or more shelves104. In one or more embodiments, the one or more perforations128may arranged in one or more rows316at certain intervals along the length of the main expanse306, wherein each perforation128awithin a row316ahas a center point that is the same length from the first end302of the center pipe124and the same length from the second end304of the center pipe124as each of the other perforations128awithin the row316a. In other embodiments, the one or more perforations128may be arranged in other patterns, or may be arranged in a random order, depending on the design needs of the vessel100. In some embodiments, each row316amay include any number of perforations128aaround the circumference of the center pipe124(or perimeter of the center pipe124if the center pipe124is not cylindrical). In one embodiment, each row316aof the one or more rows316may contain the same number of perforations128a. In many embodiments, each perforation128aof the one or more perforations128may have a substantially identical diameter, though in an alternative embodiment, the diameters of each perforation128aof the one or more perforations128may not be substantially identical. In a preferred embodiment, the main expanse306of the center pipe124includes six rows316a, and each of the six rows316aincludes eight perforations128a. In the preferred embodiment, the eight perforations128amay be defined at around the circumference of the center pipe124at 0°, 45°, 90°, 135°, 180°, 225°, 270°, and 315° such that the eight perforations128aare separated at a defined interval (i.e., each perforation128ais 45° from the two perforations128abeside it). In other embodiments, if a row316aincludes a different number of perforations128a, then the perforations128amay be separated at a different defined interval (e.g., 4 perforations128amay be separated at 90° intervals around the center pipe124).

In several embodiments, the center pipe124and base adapter122are made of stainless steel or any other non-corrosive metal, such as copper, galvanized steel, titanium, or any alloys thereof. In at least one embodiment, the center pipe124may have a certain length may include any number of one or more perforations128along the length of the center pipe124. In some embodiments, the rows316may be separated by any distance, depending on the design needs of the vessel100and how many shelves202are placed in the vessel100. In a preferred embodiment, the rows316are spaced evenly apart from each other.

Turning now toFIG.4, an exemplary center pipe assembly106and one or more shelves104are shown, according to one embodiment of the present disclosure. As discussed herein, the center pipe assembly106includes the fluid inlet127, the bottom adapter126, the base adapter122, and the center pipe124, each component fluidically connected to the others. In many embodiments, fluid, such as the carrier gas, may flow into the fluid inlet127, through the bottom adapter126, through the base adapter122, through the center pipe124and may flow out of the center pipe124via the one or more perforations128and into the cavity.

In several embodiments, the fluid inlet127may include a first end402and a second end404, and each of the first end402and the second end404may define an opening that extends from the first end402to the second end404so that fluid can flow into and through the first end402to and out of the second end404. In some embodiments, the first end402may be designed so that the first end402can fluidically connect to a fluid source, via piping or other similar devices.

In at least one embodiment, the bottom adapter126includes a first end406and a second end408. In many embodiments, the bottom adapter126defines an opening at the first end406and the second end408and that extends through the bottom adapter126between the first end406and the second end408, such that the bottom adapter126is hollow and includes an inner surface. In one or more embodiments, the second end408of the bottom adapter126is attached to the bottom surface132of the container base108. In some embodiments, the second end408may be attached to the bottom surface132of the base308via welding, fasteners, or other connection devices.

In multiple embodiments, the first end406of the bottom adapter126is mechanically coupled or fastened to the second end404of the fluid inlet127, such that the opening at the first end406of the bottom adapter126and the opening at the second end404of the fluid inlet127are fluidically connected. In one or more embodiments, the second end404of the fluid inlet127may be mechanically coupled to the first end406of the bottom adapter126. In one embodiment, for example, as shown inFIG.4, the second end404of the fluid inlet127may have screw threading314around the outer surface, and the inner surface of the first end406of the bottom adapter126may have screw threading, such that the second end404of the fluid inlet127may screw into the opening at the first end406of the bottom adapter126and couple to the screw threading on the inner surface of the bottom adapter126. In other embodiments, the second end404of the fluid inlet127may be welded to the first end406of the bottom adapter126, or may be connected via fasteners or otherwise mechanically coupled together. In one embodiment, the fluid inlet127has an outer diameter that is smaller than the diameter of the opening at the first end406of the bottom adapter126.

In an alternative embodiment, the bottom adapter126may have an outer diameter that is smaller than the opening at the second end404of the fluid inlet127. In this alternative embodiment, the fluid inlet127may have an inner surface that has screw threads, and the bottom adapter126may have an outer surface that has screw threads around it. Continuing with this alternative embodiment, the inner surface of the second end404of the fluid inlet127screws onto the outer surface of the first end406of the bottom adapter126such that the first end406of the bottom adapter126extends into and is substantially covered by the second end404of the fluid inlet127.

In one or more embodiments, as described further in relation to the description ofFIG.5B, the container base108defines an opening through which fluid may pass through. In at least one embodiment, the opening at the second end408of the bottom adapter126is in fluid connection with the opening in the container base108at the bottom surface132of the container base108, and the opening at the second end310of the base adapter122is in fluid connection with the opening in the container base at the top surface130of the container base108, such that a fluid may pass through the bottom adapter126, through the opening in the container base108, and into the base adapter122(and then into the center pipe124).

As seen inFIG.4, the one or more shelves104are aligned on top of each other so that the shelf supports142of one shelf202do not come in contact with the shelf supports of another shelf202.

Turning now toFIGS.5A and5B, an exemplary container assembly102is shown, according to one embodiment of the present disclosure. In various embodiments, the container assembly102includes the container base108, the container wall110, the flange112, and the one or more feet114. In at least one embodiment, the container base108may be circular, such that the container base109extends radially away from a center opening502(as seen inFIG.5B) toward an outer edge504. In other embodiments, the container base108may be any other shape, to fit the design needs of the vessel100. In many embodiments, the container wall110includes a first end506, a second end508, and a main wall expanse510between the first end506and the second end508. In some embodiments, the container wall110is cylindrical and has an outer diameter that is equal to an outer diameter of the base108. In other embodiments, the container wall110may be shaped in such a way that a horizontal cross-section of the container wall110is the same shape as the base108. In certain embodiments, the first end506and the second end508each define a cavity opening702(seeFIG.7B) that extends from the first end506through the main wall expanse510and through the second end508, creating a hollow interior. In several embodiments, the first end506of the wall110is connected to the base108along the outer edge504, creating a cavity. In one embodiment, the first end506of the wall110is connected to the top surface130of the base108via welding, fasteners, or other connection devices.

In multiple embodiments, the flange112includes a flange body511, an outer edge512, an inner edge514, a top surface516and a bottom surface518. In many embodiments, the inner edge514of the flange112may define a cavity opening520that is the same shape as the second end508of the container wall110and has a diameter (i.e., the diameter of the inner edge514) that is the same as the inner diameter of the second end508of the container wall. In some embodiments, the flange body511is the expanse between the inner edge514and the outer edge512of the flange112. In one or more embodiments, the outer edge512and the inner edge514may be the same shape or different shapes. In a preferred embodiment, the outer edge512and the inner edge514are circular, and the diameter of the circle defined by the outer edge512is larger than the circle defined by the inner edge514. In several embodiments, the bottom surface518of the flange112is connected to the second end508of the container wall110. In some embodiments, the portion of the flange body511proximate to the inner edge514on the bottom surface518may be welded or otherwise fastened or connected to the second end508of the container wall110, such that another portion of the flange body511and the outer edge512are outside the cavity.

In various embodiments, the flange body511may define one or more flange openings522that extend from the top surface516of the flange112through the bottom surface518of the flange112, and are used to removably couple the lid assembly116to the container assembly102. In many embodiments, each flange opening522aof the one or more flange openings522may be spaced an equal distance apart around the flange body511. For example, in certain embodiments, if the flange body511has eight flange openings522a, the eight flange openings522amay be located 45° apart around the flange body511(i.e., one flange opening522alocated at the point defined at 0°, 45°, 90°, 135°, 180°, 225°, 270°, and 315° around the circular flange body511). In one embodiment, each flange opening522amay be circular, though each may be any other shape so that a connection device, such as a screw or bolt, or other similar device, may pass through the flange opening522a. In some embodiments, the number of flange openings522amay be the same as the number of openings in the gasket119and the number of openings in the lid118, and the one or more flange openings522, the openings in the gasket119, and the openings in the lid118may all be arranged so that a bolt140(or other connection device or fastener) can pass through one opening in the lid118, one opening in the gasket119, and one flange opening522a, and a nut138be attached to the bolt140to couple the lid118, the gasket119, and the flange112together. In one or more embodiments, the flange body511may include 4 to 24 flange openings522a, though it may include more or less depending on the design needs of the vessel100. In a preferred embodiment, the flange body511may include 16 flange openings522a(thus, the 16 flange openings522aare located 22.5° apart around the flange body511).

In several embodiments, the one or more feet114may each include a first end524that is connected to the bottom surface132of the container base208, and a second end526that is in contact with an exterior surface to support the vessel100, and a foot body528in between the first end524and the second end526. In many embodiments, the first end524may be connected to the bottom surface132of the container base via welding, fasteners, or other connection devices or methods. In some embodiments, each of the one or more feet114may include a height (defined as the length between the first end524and the second end526) that is greater than the height or length of the bottom adapter126and the fluid inlet127together, so that there is enough space under the container base108to connect the bottom adapter126and the fluid inlet127to the center pipe assembly106.

Turning toFIGS.6A and6B, an exemplary lid118and top adapter120are shown, according to one example of the present disclosure. In several embodiments, the lid118defines a center opening602that extends from the bottom surface136through the top surface134to allow fluid to flow out of the cavity. In at least one embodiment, the lid118may be circular, extending radially from the center opening602to an edge606. In other embodiments, the lid118may be any other shape depending on the design needs of the vessel100. In some embodiments, the lid118may define one or more lid openings604that are utilized for mechanically coupling the lid118to the flange112. In certain embodiments, the one or more lid openings604may be arranged substantially identically to the flange openings522so that the lid openings604and the flange openings522align. In one embodiment, each lid opening604aof the one or more lid openings604may be circular or any other shape so that a bolt140can extend through the lid opening604a. In at least one embodiment, each lid opening604aof the one or more lid openings604may be an equal distance apart from the adjacent lid openings604aaround the lid118. For example, in certain embodiments, if the lid118has eight lid openings604a, the eight lid openings604amay be located 45° apart around the lid118(i.e., one lid opening604alocated at the point defined at 0°, 45°, 90°, 135°, 180°, 225°, 270°, and 315° around the circular lid118). In certain embodiments, each lid opening604ais the same distance away from the center opening602, which distance is greater than the radius of the cavity opening520, so the one or more lid openings604are exterior to the cavity. In at least one embodiment, the lid118may have a diameter that is substantially equal to the outer diameter of the flange112and the outer diameter of the gasket119.

In multiple embodiments, the lid118may include 4 to 24 lid openings604a, and preferably, 16 lid openings604a.

In one or more embodiments, the top adapter120includes a first end608and a second end610. In many embodiments, the top adapter120defines a circular opening at the first end608and the second end510and that extends through the top adapter120between the first end608and the second end610, such that the top adapter120is hollow and includes an inner surface. In one or more embodiments, the first end608of the top adapter120is attached to the top surface134of the lid118. In some embodiments, the first end608may be attached to the top surface134of the lid118via welding, fasteners, or other connection devices.

In multiple embodiments, the second end610of the top adapter120is mechanically coupled or fastened to a first end of the fluid outlet121, such that the opening at the second end610of the top adapter120and the opening at the first end of the fluid outlet121are fluidically connected. In one embodiment, for example, the first end of the fluid outlet121may have screw threading around the outer surface of the fluid outlet121, and the inner surface of the second end610of the top adapter120may have screw threading, such that the first end of the fluid outlet121may screw into the opening at the second end610of the top adapter120and couple to the screw threading on the inner surface of the top adapter120. In other embodiments, the first end of the fluid outlet121may be welded to the second end610of the top adapter120, or may be connected via fasteners or otherwise mechanically coupled together. In one embodiment, the fluid outlet has an outer diameter that is smaller than the diameter of the opening at the second end610of the top adapter120.

In an alternative embodiment, the top adapter120may have an outer diameter that is smaller than the opening at the first end of the fluid inlet121. In this alternative embodiment, the fluid outlet121may have an inner surface that has screw threads, and the top adapter120may have an outer surface that has screw threads around it. Continuing with this alternative embodiment, the inner surface of the first end of the fluid outlet121screws onto the outer surface of the second end610of the top adapter120such that the second end610of the top adapter120extends into and is substantially covered by the first end of the fluid outlet121.

Turning now toFIGS.7A and7B, side and top views of an exemplary embodiment of the container wall110are shown, according to one embodiment of the present disclosure. In many embodiments, the container wall110includes a first end506, a second end508, and a main wall expanse510between the first end506and the second end508. In some embodiments, the container wall110is cylindrical and has an outer diameter that is equal to an outer diameter of the base108. In other embodiments, the container wall110may be shaped in such a way that a horizontal cross-section of the container wall110is the same shape as the base108. In certain embodiments, the first end506and the second end508each define a container opening702(as shown inFIG.7B) that extends from the first end506through the main wall expanse510and through the second end508, creating a hollow interior.

In many embodiments, the hollow container wall110includes an interior surface704and an exterior surface706. In one or more embodiments, the container wall110has a certain thickness between the interior surface704and the exterior surface706. In at least one embodiment, the container wall110has a certain height between the first end506and the second end508.

Now turning toFIG.8, a side and front view of an exemplary gasket119are shown, according to one embodiment of the present disclosure. In various embodiments, the gasket119is made of polytetrafluoroethylene or another material suitable for the needs of a gasket. In at least one embodiment, the gasket119is positioned between the lid118and the flange112so that the HF/carrier gas fluid only flows through the center opening602of the lid118and does not leak through any other point or component the lid assembly116. In several embodiments, the gasket119includes a gasket body802, an outer edge804, an inner edge806, a top surface808and a bottom surface810. In many embodiments, the inner edge806of the gasket119may define an inner opening812that is the substantially the same shape as the second end508of the container wall110and has an inner diameter (i.e., the diameter of the inner edge806) that is the substantially the same as the inner diameter of the second end508of the container wall110. In some embodiments, the gasket body802is the expanse between the inner edge806and the outer edge804of the gasket119. In one or more embodiments, the outer edge804and the inner edge806may be the same shape or different shapes. In a preferred embodiment, the outer edge804and the inner edge806are circular, and the diameter of the circle defined by the outer edge804is larger than the circle defined by the inner edge806. In several embodiments, the bottom surface810of the gasket119is connected to the top surface516of the flange112. In some embodiments, the top surface808of the gasket119is connected to the bottom surface136of the lid118. In

In various embodiments, the gasket body802may define one or more gasket openings814that extend from the top surface804of the gasket119through the bottom surface806of the gasket119, and are used to removably couple the lid assembly116to the container assembly102, with the gasket119in between the flange112and the lid118. In many embodiments, each gasket opening814aof the one or more gasket openings814may be spaced an equal distance apart around the gasket body802. For example, in certain embodiments, if the gasket body802has eight gasket openings814a, the eight gasket openings814amay be located 45° apart around the gasket body802(i.e., one gasket opening814alocated at the point defined at 0°, 45°, 90°, 135°, 180°, 225°, 270°, and 315° around the circular gasket body802). In one embodiment, each gasket opening814amay be circular, though each may be any other shape so that a connection device, such as a screw or bolt, or other similar device, may pass through the gasket opening814a. In some embodiments, the number of gasket openings814amay be the same as the number of flange openings522aand the number of lid openings604a, and the one or more gasket openings814, the one or more flange openings522, and the one or more lid openings604may all be arranged so that a bolt140(or other connection device or fastener) can pass through one lid opening604ain the lid118, one gasket opening814ain the gasket119, and one flange opening522a, and a nut138be attached to the bolt140to couple the lid118, the gasket119, and the flange112together. In one or more embodiments, the gasket body802may include 4 to 24 gasket openings814a, though it may include more or less depending on the design needs of the vessel100. In a preferred embodiment, the gasket body802may include 16 gasket openings814a(thus, the 16 gasket openings814aare located 22.5° apart around the gasket body814).

Turning now toFIGS.9A and9B, a front view and side view of an exemplary flange112are shown, according to one embodiment of the present disclosure. In several embodiments, as shown in theFIGS.9A and9Band as previously described, the flange112includes the outer edge512, the inner edge514, and a flange body511in between the inner edge514and outer edge512, and also includes the top surface516of the flange112and the bottom surface518of the flange112. In one embodiment, the flange112defines the cavity opening520, and also defines one or more flange openings522within the flange body511.

Turning now toFIG.10, shown is a top view of an exemplary lid118that is fastened, according to one embodiment of the present disclosure. In various embodiments, the fastened lid118includes one or more bolts140extending through each of the one or more lid openings604. In at least one embodiment, the fluid outlet121is shown attached to the top adapter120(not shown inFIG.10).

Turning now toFIG.11, shown is a side view of an exemplary fastened vessel100, according to one embodiment of the present disclosure. In many embodiments, when the vessel100is fastened, the lid assembly116(the flange, the gasket119, and the lid118) are removably coupled together via one or more bolts140and one or more nuts138, or other connectors or fasteners. As shown inFIG.11, in several embodiments, the each of the one or more bolts140are positioned so that each extends through one lid opening604a, one gasket opening814a, and one flange opening522a, and one or more nuts138are attached to the portion of the one or more bolts140protruding therefrom to connect and seal (except for the center opening602in the lid118) the lid assembly116onto the container assembly102.

Turning now toFIG.12, a perspective view of an alternative exemplary HF generator vessel1200is shown, according to one embodiment of the present disclosure. In many embodiments, the function of the vessel1200is the same as the vessel100, namely, to produce HF gas from sodium bifluoride undergoing thermal degradation while being fluidly connected to a system that immediately use the produced HF gas.

In various embodiments, the vessel1200includes a container assembly1202, a lid assembly1204, and a shelf assembly1500(as shown inFIG.15). In one or more embodiments, the container assembly1202includes a container wall1206, a container base1208, a fluid inlet1212, a center pipe1302(as shown inFIG.13), and a fluid outlet1214that defines a fluid outlet opening1216. In at least one embodiment, the lid assembly1204may include a lid1210and a lid connector1224. In many embodiments, the shelf assembly1500may include one or more shelves1502(as shown inFIG.15), one or more support rods1602(as shown inFIG.16), a support rod base1902(as shown inFIG.19), a shelf assembly lid1218having a top surface1226and a bottom surface, one or more nuts1222, and a handle1220.

In many embodiments, the shelf assembly1500may be placed inside the container assembly1202, and the lid assembly1204may thereafter be removably coupled. In one or more embodiments, the lid1210may be connected to the lid connector1224to prevent leaks out of the vessel1200. In some embodiments, the lid1210may be connected to the lid connector1224by screwing onto the lid connector1224, by snapping onto lid connector1224, by bolting or fastening the lid110to the lid connector1224, or by any other means of connecting the lid1210to the lid connector1224

In several embodiments, the vessel1200may be assembled and fluidly connected so that a carrier gas (e.g., Argon), may be pumped into the fluid inlet1212, through the center pipe1302, and out of the fluid outlet1214via the outlet opening1216.

Turning now toFIGS.13A and13B, a perspective and a side view of an exemplary container assembly1202is shown, according to one embodiment of the present disclosure. In multiple embodiments, the container assembly1202includes a container wall1206that has a bottom end1306and a top end1308, and a main expanse1310therebetween, and also includes a container base1208with a bottom surface1314and a top surface1402(seeFIG.14). In one or more embodiments, the bottom end1306of the container wall1206is connected to the top surface1402of the base1208. In at least one embodiment, the top end1308of container wall1206defines an opening that extends through the main expanse1310and to the top surface1402of the container base1208, forming a vessel cavity1304. In many embodiments, the top end1308of the container wall1206connects to the lid connector1224. In certain embodiments, the fluid inlet1212defines an inlet opening1312that allows fluid to enter the vessel1200.

In several embodiments, the center pipe1302protrudes upwards from substantially the center of the top surface1402of the container base1208into the cavity1304, such that when the shelf assembly1500is placed into the cavity1304, the center pipe1302extends through the one or more shelves1502of the shelf assembly1500via a center pipe opening1804(as shown inFIG.18) in each of the one or more shelves1502.

In multiple embodiments, the fluid outlet1214protrudes out from the main expanse1310of the container wall1206and includes a first end1316, a second end1318, and a main body1320therebetween. In many embodiments, the first end1316defines the opening1216that extends from the first end through the main body1320, but does not extend through the second end1318, such that the fluid outlet1214is substantially hollow. In some embodiments, the container wall1206defines a side wall opening enclosed by the fluid outlet1214such that the vessel cavity1304and the hollow fluid outlet1214are fluidly connected. In one embodiment, piping or some other components may be fluidly connected with the fluid outlet1214via the fluid outlet opening1216so that the HF gas may flow downstream to an application that utilizes the HF gas.

Turning now toFIG.14, a perspective view of an exemplary container assembly1202without the container wall1206is shown, according to one embodiment of the present disclosure. In various embodiments, the container assembly1202includes the center pipe1302. In one or more embodiments, the center pipe1302includes a first end1404, a second end1406, a center pipe body1408therebetween the first end1404and the second end1406, one or more perforations1410extending through the center pipe body1408through to an interior surface1604(as shown inFIG.16) of the center pipe1302, and an end cap1412connected to the second end1406. In one or more embodiments, the first end1404of the center pipe1302defines an opening that extends through the first end, through the pipe body1408, and through the second end1406. In certain embodiments, the end cap1412covers the opening at the second end1404of the center pipe1302so that the carrier gas is forced through the one or more perforations1410. In many embodiments, the fluid inlet1212is fluidly connected to the center pipe1302through the base1208(i.e., the top surface1402defines an opening (not shown) and the bottom surface1314defines an opening (not shown) and there extends a fluid pathway therebetween, where the opening in the top surface1402is fluidly connected to the interior of the center pipe1302at the first end1404).

In several embodiments, the one or more perforations1410may be evenly spaced apart around the circumference of the center pipe1302and along the length of the center pipe1302. In at least one embodiment, the carrier gas may exit the center pipe1302through the one or more perforations1410and into the cavity1304. In many embodiments, each of the one or more perforations1410may have a substantially identical diameter, though in an alternative embodiment, the diameters of each of the one or more perforations1410may not be substantially identical.

Turning now toFIG.15, a perspective view of an exemplary shelf assembly1500is shown, according to one embodiment of the present disclosure. In various embodiments, the shelf assembly1500includes the support rod base1902connected to one or more support rods1602, and one or more shelves1502stacked on top of one another with the one or more support rods1602extending through the stacked one or more shelves1502. In several embodiments, before stacking the one or more shelves1502, sodium bifluoride is loaded onto each of the one or more shelves1502. In many embodiments, by placing a shelf1502aon top of another shelf1502acreates a notched opening1504afor the carrier gas to flow out from the shelf1502aand into the fluid outlet1214. In at least one embodiment, the one or more shelves1502stacked on top of one another defines one or more notched openings1504.

In many embodiments, once a certain number of one or more shelves1502are stacked on top of one another, the shelf assembly lid1218is placed on top of the top-most shelf1502a, with the one or more support rods1602extending through the shelf assembly lid1218, and one or more nuts1222are fastened to each of the one or more support rods1602on the top surface1226of the shelf assembly lid1218.

In some embodiments, the handle1220may be utilized to place the shelf assembly1500into the cavity1304of the container assembly1202. In certain embodiments, the shelf assembly1500is positioned over and around the center pipe1302. In one embodiment, the shelf assembly1500is also placed over and around an internal heating element.

Turning now toFIG.16andFIG.17, a cross-sectional perspective view and a cross-sectional side view of an alternative exemplary vessel1200is shown, according to one embodiment of the present disclosure. As shown inFIG.16, in many embodiments, the shelf assembly1500is placed into the cavity1304of the container assembly1202around the center pipe1302. In at least one embodiment, as shown inFIG.17, the one or more support rods1602extend through each of the one or more shelves1502and through the shelf assembly lid1218, and connect to a support rod base1902at one end and to one or more nuts1222at the other end of the one or more support rods1602. In one or more embodiments, the center pipe1302includes the interior surface1604of the hollow center pipe1302.

In various embodiments, as shown inFIG.17, each of the one or more perforations1410align with each of the one or more shelves1502so that the carrier gas flows out of each of the one or more perforations and over each of the one or more shelves1502, and the flow of the carrier gas causes the produced HF gas to flow to the fluid outlet1214and out of the fluid outlet opening1216. In one or more embodiments, the fluid inlet1212may be fluidly connected to the center pipe1302via a space1702defined between the top surface1402of the base1208and a bottom surface of the one or more shelves1502. In at least one embodiment, the bottommost perforations1410defined by the center pipe1302may allow fluid to enter into the interior of the center pipe1302from the space1702.

Turning now toFIG.18, a perspective view of an exemplary shelf1502aof the one or more shelves1502is shown, according to one embodiment of the present disclosure. In multiple embodiments, the shelf1502ainclude a shelf base1802having a top surface1818and a bottom surface (not shown in the figures) and a raised outer edge1806that protrudes up from the top surface1818of the shelf base1802. In at least one embodiment, the shelf base1802defines a center pipe opening1804that extends from the top surface1818through the bottom surface, and a raised inner edge1808that surrounds the center pipe opening1804protrudes up from the top surface1818of the shelf base1802. In some embodiments, the center pipe opening1804has a diameter that is greater than the diameter of the center pipe1302. In many embodiments, the outer edge1806may include a notched portion1816that does not protrude as high from the top surface1818of the shelf base1802as the remaining portion of the raised outer edge1806. In one embodiment, the outer edge1806may have a diameter that is smaller than the diameter of the cavity1304so that the shelf assembly1500may be placed inside the cavity1304.

In several embodiments, the shelf base1802defines one or more support rod openings1812that extend from the top surface1818through to the bottom surface of the shelf base1802so that the one or more support rods1602may extend through the one or more support rod openings1812. In one embodiment, the one or more support rod openings1812include a diameter that is greater than the diameter of the one or more support rods1602. In at least one embodiment, the shelf base1802also includes one or more raised support rod edges1810that protrude up from the top surface1818of the shelf base1802and surround the one or more support rod openings1812.

In some embodiments, the raised inner edge1808may not protrude as high from the top surface1818of the shelf base1802as the raised outer edge1806(except the raised inner edge1808may protrude as high from the top surface1818as the notched portion1816protrudes), so as to not block the one or more perforations1410or the carrier gas from exiting the one or more perforations and flowing over the one or more shelves1502.

In one or more embodiments, the shelf base1802may also define a heating element opening1814that extends from the top surface1818through to the bottom surface of the shelf base1802. In one embodiment, the shelf base1802may also include a raised heating element edge around the heating element opening1814that protrudes up from the top surface1818of the shelf base1802. In at least one embodiment, an internal heating device may extend through the heating element opening1814, and may provide the heat necessary for the sodium bifluoride to thermally degrade into HF gas.

Turning now toFIG.19, a perspective view of an exemplary support rod base1902and one or more support rods1602is shown, according to one embodiment of the present disclosure. In various embodiments, each of the one or more support rods1602may have a first end1904and a second end1906. In one or more embodiments, the first end1904of each of the one or more support rods1602may be connected to the support rod base1902(e.g., via welding, screwing, or some other connection device or method). In certain embodiments, the second end1906of each of the support rods1602may have a threaded exterior surface1908such that the second end1906of each of the support rods1602may be removably coupled with one or more nuts1222.

In several embodiments, to assemble the one or more shelves1502onto the one or more support rods1602and support rod base1902, the one or more support rods1602may be placed through the one or more support rod openings1812of a first shelf1502aloaded with sodium bifluoride, and the first shelf1502amay be placed on and supported by the support rod base1902. In many embodiments, the one or more support rods1602may be placed through the support rod openings1812of a second shelf1502athat is loaded with sodium bifluoride, and the second shelf1502amay be placed on top of the first shelf1502a. In some embodiments, the bottom surface of the shelf base1802of the second shelf1502ais in contact with and supported by the raised outer edge1806(except for the notched portion1816) of the first shelf1502a. In certain embodiments, the bottom surface of the shelf base1802of the second shelf1502aand the notched portion1816of the raised outer edge1806of the first shelf1502adefine a notched opening1504afor the first shelf1502aso that the carrier gas can flow over the first shelf1502aand into the fluid outlet1214via the notched opening1504aof the first shelf1502a. In some embodiments, any number of shelves1502may be added onto the one or more support rods1602. In certain embodiments, the center pipe opening1804, the one or more support rod openings1812, and the heating element opening1814of each shelf1502ain the shelf assembly1500may be aligned such that each of the components (the center pipe1302, the one or more support rods1602, and the heating device) extending through each of their respective openings may extend through each respective opening without obstruction due to misalignment of said openings.

Now turning toFIG.20, a perspective view of an exemplary shelf assembly lid1218is shown, according to one embodiment of the present disclosure. In many embodiments, the shelf assembly lid1218defines one or more shelf assembly lid openings2002that extend from the top surface1226through to the bottom surface (not shown in the figures) of the shelf assembly lid1218. In some embodiments, the second end1906of each of the one or more support rods1602may extend through the one or more shelf assembly lid openings2002, such that the one or more nuts1222may be connected to the screw threads1908at the second end1906of each of the one or more support rods1602. In one embodiment, when the one or more support rods1602are connected to the shelf assembly lid1218via the one or more nuts1222, the one or more shelves1502are secured to the shelf assembly lid1218and the shelf assembly1500is assembled and may be moved via the handle1220.

In many embodiments, the shelf assembly1500is placed into the cavity1304such that the center pipe1302extends through each of the one or more shelves via the center pipe openings1804. In at least one embodiment, the support rod base1902contacts the top surface1402of the container base1208when fully positioned in the container assembly1202. Thereafter, in some embodiments, the lid assembly1204is coupled. In one or more embodiments, the internal heating device may provide the necessary heat to the sodium bifluoride such that it thermally degrades into HF gas. In an alternate embodiment, the necessary heat may be provided by external heating devices, as described herein, instead of or in addition to the internal heating devices.

In various embodiments, the carrier gas may flow or be pumped into the fluid inlet1212via the inlet opening1312, through the space1702and into the center pipe1302. In other embodiments, the fluid inlet1212may be directly fluidly connected to the center pipe1302. In many embodiments, the carrier gas may exit the center pipe1302via the one or more perforations1410and flow over the one or more shelves1502, causing the produced HF gas to flow to the fluid outlet1214and out of the vessel1200via the fluid outlet opening1216.

Turning now toFIG.21, an exemplary purification vessel2100is shown, according to one embodiment of the present disclosure. In various embodiments, once the HF gas (or HF gas/carrier gas mixture) is produced, the HF gas can be pumped (or otherwise caused to move to) the purification vessel2100. In many embodiments, the purification vessel2100may include a salt transfer line2102, a salt loading pipe2104, an exhaust line2106, and a sparger2108. In at least one embodiment, the HF gas goes through the sparger2108and into the purification vessel2100. In some embodiments, the purification vessel2100may utilize HF to remove metal oxides and metal sulfides from molten salt fuel medium of a molten salt reactor. However, the HF may be utilized in any way after production with the vessel100or vessel1200.

Turning now toFIG.22, shown is a flowchart of an exemplary hydrofluorination system2200, according to one embodiment of the present disclosure. In several embodiments, the system2200includes the HF generator vessel100(or vessel1200) and the purification vessel2100. In one or more embodiments, the vessel100receives carrier gas (argon or “Ar”) from a carrier gas source, to carry the HF gas from the vessel100to the purification vessel2100. In certain embodiments, hydrogen gas (H2) is provided and mixes with the HF gas in the sparger2108line. In one embodiment, once the HF gas is utilized in the sparger2108, the HF gas is pumped through the exhaust line2106and to at least one carboy used to collect the exhaust gas.

Turning now toFIG.23, a graph showing the temperature over time in an exemplary HF generator vessel is shown, according to one embodiment of the present disclosure. In several embodiments, the thermal degradation of the sodium bifluoride into HF and sodium fluoride (NaF) occurs at about 120° C. In at least one embodiment, the carrier gas flow rate was about 800 milliliters per minute (Ar gas). As seen inFIG.23, the temperature inside the vessel100reached about 120° C. in about two hours, while the temperature of the heat wrap on the outside of the vessel100had an average temperature of about 160° C. after two hours, and both internal and external temperatures remained substantially constant thereafter.

Turning toFIG.24, a perspective view of an exemplary flow path of a carrier gas flowing through an exemplary HF generator vessel100is shown, according to one body of the present disclosure. In several embodiments, the carrier gas flows through the fluid inlet127and through the center pipe assembly106before flowing out of the one or more perforations128of the center pipe124. The carrier gas then flows over the one or more shelves104, and the flow of the carrier gas causes the produced HF to flow along the same flow path as the carrier gas over the raised outer edge211of each of the one or more shelves104and up out of the center opening602of the lid118and out of the fluid outlet121. As shown inFIG.24, the flow of the carrier gas out of each of the one or more perforations128of an exemplary center pipe124and over the one or more shelves104is substantially equal.

Turning now toFIG.25, a graph of the amount of AHF produced over time in an exemplary HF generator vessel100at a certain carrier gas flow rate is shown, according to one embodiment of the present disclosure. In at least one embodiment, the carrier gas flow rate was about 800 milliliters per minute (Ar gas). In one embodiment, the vessel100and method produced about 0.5-0.6 moles HF per mole of sodium bifluoride (NaHF2) over about 1500 minutes.

In an example, according to one embodiment, if 9.2 moles of sodium bifluoride (568 grams) are loaded into the vessel100, the HF production may be about 0.00326 mol HF per minute delivery rate, at about 730 milliliters per minute flow rate and about 120° C. in the vessel100. Continuing with the example, if there are six shelves202in the vessel100, each shelf has about 95 grams of sodium bifluoride loaded onto it, and with the 730 milliliter per minute flow rate and the 120° C. in the vessel100, the vessel100should generate a gas ratio of about ten H2 to one HF for the hydrofluorination process.

Turning now toFIG.26, an exemplary method2600for producing anhydrous hydrogen fluoride gas in an exemplary HF generator vessel100(or vessel1200) is described, according to one embodiment of the present disclosure. In various embodiments, the vessel100is utilized during the exemplary method2600. In one or more embodiments, the method2600produces HF via the vessel100(or vessel1200) by thermally degrading sodium bifluoride into HF gas and NaF.

In many embodiments, to start method2600, at step2602, sodium bifluoride is placed onto the one or more shelves104(or one or more shelves1502). In at least one embodiment, the sodium bifluoride is granular to create more surface area for the thermal degradation reaction to occur. In some embodiments, the amount of sodium bifluoride placed into each of the one or more shelves104(or one or more shelves1502) may fill each of the one or more shelves104(or one or more shelves1502) to the top of the height of the raised outer edge211(or to the height of notched edge1816). In another embodiment, the amount of sodium bifluoride placed into each of the one or more shelves104(or one or more shelves1502) may only be about 1-2 millimeters deep. In certain embodiments, for the vessel100, each of the one or more shelves104is placed onto the center pipe124and onto the shelf supports142of the shelf below. In some embodiments, for the vessel1200, each of the one or more shelves1502is placed on the one or more support rods1602(i.e., the one or more support rods1602extend through the one or more shelf assembly lid openings2002) and is placed on top of the outer edge1806of the shelf1502abelow.

In several embodiments, at optional step2603, the shelf assembly lid1226is fastened onto the support rods1602. In at least one embodiment, the shelf assembly lid1226is fastened to the support rods via the nuts1222screwing onto the second end1906of each of the support rods1602after the second end1906of each of the support rods1602have extended through the shelf lid openings2002. In many embodiments, the handle1220may be utilized to place the shelf assembly1500onto the center pipe1302.

In various embodiments, at step2604, the lid assembly116(or lid assembly1204) is closed and fastened. In many embodiments, for the vessel100, each of the lid118, gasket119, and flange112are aligned so that the one or more bolts140will go through the openings of each component, and a nut138is placed onto each bolt140once the bolt140is placed through the three openings. In some embodiments, for vessel1200, the lid1210is connected to the lid connector1224. In many embodiments, the lid assembly116(or lid assembly1204) may also be fastened via other connector devices.

In several embodiments, at step2606, the vessel100(or vessel1200) is rapidly heated via heat sources so that the sodium bifluoride inside the vessel100(or vessel1200) will get to a temperature at which it will degrade into HF (about 120° C.). In some embodiments, for vessel100, the heat source is external to the vessel100, and the external heat source may be heat tracing tape in combination with insulation to keep the heat inside the vessel; however, any other external heat source may be applicable to cause the vessel100to reach the necessary temperature. In certain embodiments, for vessel1200, the heat source is internal to the vessel1200, and the internal heat source may radiate heat inside the vessel1200to cause the vessel1200to reach the necessary temperature.

In many embodiments, at step2608, carrier gas is pumped through the vessel100(or vessel1200) as described herein to cause any produced HF to flow out of the vessel100(or vessel1200) at the fluid outlet121(or fluid outlet1216). In some embodiments, the carrier gas may be pumped into the vessel100(or vessel1200) before the temperature inside the vessel100(or vessel1200) has reached the temperature to cause the sodium bifluoride to degrade into HF and NaF.

In multiple embodiments, at step2610, the HF gas produced at step2608may be utilized immediately for any commercial use. For example, in one embodiment, the HF gas may be pumped from the vessel100(or vessel1200) to a purification vessel2100to condition molten salts (such as, but not limited to, molten fluoride salts) to reduce the concentration of one or more impurities (such as, but not limited to, H2O, sulfur, H+, OH−, or any combination thereof) in the molten salt. In some embodiments, the conditioned molten salts may be utilized in a liquid fuel molten salt reactor, as the rate of corrosion of molten salt reactors is reduced compared to molten salt reactors that do not use pre-conditioned molten salts. In at least one embodiment, the molten salts may be pre-conditioned with the HF gas before use, and may be reconditioned after being used (i.e., the salts became contaminated during use).

In other embodiments, the HF gas may be utilized to reduce oxidizing contaminants in molten salt by exposing the molten salt to the HF for a certain amount of time. In another embodiment, the HF gas may be utilized for vapor etching (i.e., removing films from substrate materials).

CONCLUSION

Aspects, features, and benefits of the systems, methods, processes, formulations, apparatuses, and products discussed herein will become apparent from the information disclosed in the exhibits and the other applications as incorporated by reference. Variations and modifications to the disclosed systems and methods may be effected without departing from the spirit and scope of the novel concepts of the disclosure.

It will, nevertheless, be understood that no limitation of the scope of the disclosure is intended by the information disclosed in the exhibits or the applications incorporated by reference; any alterations and further modifications of the described or illustrated embodiments, and any further applications of the principles of the disclosure as illustrated therein are contemplated as would normally occur to one skilled in the art to which the disclosure relates.

The foregoing description of the exemplary embodiments has been presented only for the purposes of illustration and description and is not intended to be exhaustive or to limit the inventions to the precise forms disclosed. Many modifications and variations are possible in light of the above teaching.

The embodiments were chosen and described in order to explain the principles of the inventions and their practical application so as to enable others skilled in the art to utilize the inventions and various embodiments and with various modifications as are suited to the particular use contemplated. Alternative embodiments will become apparent to those skilled in the art to which the present inventions pertain without departing from their spirit and scope. Accordingly, the scope of the present inventions is defined by the appended claims rather than the foregoing description and the exemplary embodiments described therein.

While various aspects have been described in the context of a preferred embodiment, additional aspects, features, and methodologies of the claimed inventions will be readily discernible from the description herein, by those of ordinary skill in the art. Many embodiments and adaptations of the disclosure and claimed inventions other than those herein described, as well as many variations, modifications, and equivalent arrangements and methodologies, will be apparent from or reasonably suggested by the disclosure and the foregoing description thereof, without departing from the substance or scope of the claims. Furthermore, any sequence(s) and/or temporal order of steps of various processes described and claimed herein are those considered to be the best mode contemplated for carrying out the claimed inventions. It should also be understood that, although steps of various processes may be shown and described as being in a preferred sequence or temporal order, the steps of any such processes are not limited to being carried out in any particular sequence or order, absent a specific indication of such to achieve a particular intended result. In most cases, the steps of such processes may be carried out in a variety of different sequences and orders, while still falling within the scope of the claimed inventions. In addition, some steps may be carried out simultaneously, contemporaneously, or in synchronization with other steps.

The embodiments were chosen and described in order to explain the principles of the claimed inventions and their practical application so as to enable others skilled in the art to utilize the inventions and various embodiments and with various modifications as are suited to the particular use contemplated. Alternative embodiments will become apparent to those skilled in the art to which the claimed inventions pertain without departing from their spirit and scope. Accordingly, the scope of the claimed inventions is defined by the appended claims rather than the foregoing description and the exemplary embodiments described therein.