Liquefied gas electrolyte container device and dispensing method

Abstract

Methods and structures for dispensing a liquefied gas electrolyte (LGE) from a liquefied gas electrolyte (LGE) container are disclosed. The LGE includes a liquefied gas solvent having a vapor pressure of 100 kPa or more at a temperature of 293.15 K and a salt. The LGE vessel includes a temperature sensor for detecting a temperature of the liquefied gas electrolyte within the LGE vessel. The temperature of the LGE container is controlled using a temperature control element and a processor connected to the temperature sensor and the temperature control element. The LGE is transferred from the container to a secondary container through a valve. The method comprises the steps of: (a) opening the valve to allow the LGE to flow from the LGE container into the secondary container; (b) reading a reading from the temperature sensor; (c) heating the LGE container to maintain the temperature of the LGE container within a predetermined temperature or temperature range as a function of the temperature readings.

Description

1.0 Cross-Reference to Related Applications

[0001] This application claims priority to U.S. Provisional Application No. 63 / 391,220, filed on July 21, 2022, entitled “LIQUEFIED GAS ELECTROLYTE CONTAINER APPARATUS AND DISPENSING METHOD”. This application is incorporated herein by reference in its entirety.

[0002] This application is related to the following applications and patents, each of which is incorporated herein by reference in its entirety: US10608284, granted on March 31, 2020; US10988143, granted on May 4, 2021; US10784532, granted on September 22, 2020; PCT / US19 / 032413, filed on May 15, 2019; PCT / US20 / 26086, filed on April 1, 2020; US11088396, granted on October 8, 2021 ; US11049668 granted on June 29, 2021; US10873070 granted on December 22, 2020; US application 63 / 195592 filed on June 1, 2021; US ​​application 16 / 666155 filed on October 28, 2019; US application 17 / 326093 filed on May 20, 2021; US ​​application 63 / 306396 filed on February 3, 2022; and US application 63 / 328480 filed on April 7, 2022. 2.0 Statement Regarding Federally Sponsored Research and Development

[0003] none. Technical Field

[0004] Embodiments of the present invention are directed to apparatus and methods for bulk delivery of liquefied gas solvents for preparing electrochemical energy storage devices. Background Art

[0005] The preparation of liquefied gas electrolytes (LGE) requires an accurate and efficient flow control mechanism. Temperature monitoring of the LGE container allows for efficient and precise flow control during the preparation process. Flow control is typically achieved using an electronic mass flow controller (MFC). However, MFCs are not typically configured in the flow system to utilize temperature feedback from either the source or receiving container.

[0006] If the temperature of the LGE container increases during LGE preparation, backpressure exceeding the MFC operating window may negatively affect the flow rate or accuracy of the MFC. These effects may affect the performance of electrochemical devices fabricated using liquefied gas solvents.

[0007] The prior art has demonstrated that the quality and composition of the electrolyte has a significant impact on the performance of an electrochemical device. Deviations in electrolyte quality can negatively impact the performance of an electrochemical device. For example, too little electrolyte may not fully utilize all of the electrode capacity within the device. In addition, too much electrolyte can reduce the energy density of the electrochemical device by increasing mass. Similarly, deviations in electrolyte composition can also negatively impact the performance of an electrochemical device. For example, an inexact ratio of one electrolyte component to another electrolyte component may not fully utilize all of the electrode capacity within the device.

[0008] Therefore, it is necessary to prepare electrochemical devices with precise electrolyte quality and composition to match a specified energy density. It is necessary to have an apparatus and method that utilizes temperature feedback to improve the accuracy and efficiency in the LGE preparation process. Summary of the invention

[0009] A method and structure for filling a container with a liquefied gas solvent having a vapor pressure higher than atmospheric pressure (100 kPa) at room temperature 293.15 K is disclosed. The method includes providing a filling device having a mass flow controller (MFC), a liquefied gas solvent source connected to the MFC, and a container connected to the MFC, wherein the container includes salt and a temperature sensor to detect the temperature of the liquefied gas electrolyte present in the container. A processor connected to the MFC and the temperature sensor is used to receive a temperature reading from the temperature sensor and start a flow rate on the MFC. The flow rate is adjusted to keep the temperature reading from the temperature sensor below a predetermined maximum temperature. The liquefied gas solvent is mixed with the salt in the container to form a liquefied gas electrolyte.

[0010] The method may include pre-loading the non-salt components into the container.

[0011] The method may include setting a predetermined maximum temperature for the temperature sensor and adjusting the flow rate through the MFC to maintain the temperature reading below the predetermined maximum temperature.

[0012] A method and structure for dispensing a liquefied gas electrolyte from a LGE container is disclosed. The LGE includes a liquefied gas solvent having a vapor pressure greater than 100 kPa at a temperature of 293.15 K and a salt. The container includes a temperature sensor to detect the temperature of the liquefied gas electrolyte within the liquefied gas electrolyte container. The container temperature is controlled using a temperature control element and a processor connected to the temperature sensor and the temperature control element. The LGE is transferred from the container to a secondary container through a valve. The method includes the following steps: (a) opening a valve to allow the liquefied gas electrolyte to flow from the liquefied gas electrolyte container to the secondary container; (b) reading a reading from the temperature sensor; (c) based on the temperature reading, heating the liquefied gas electrolyte container to maintain the temperature of the liquefied gas electrolyte container at a predetermined temperature or within a temperature range.

[0013] The method may include a secondary container that is an electrochemical device. The device may include an electrochemical device such as a battery or a capacitor.

[0014] The method may include the predetermined temperature range of the container being 303.15K + / - 2K. Similarly, the method may include the predetermined temperature range of the secondary container being 293.15K + / - 5K.

[0015] Other aspects, alternatives and variations that are obvious to those skilled in the art are also disclosed herein and are specifically contemplated as being a part of the present invention. The present invention is set forth only in the claims allowed by the Patent Office in this or related applications, and the following summary description of certain embodiments does not in any way limit, define or otherwise determine the scope of legal protection. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 is a block diagram illustrating one embodiment of an apparatus for delivering a liquefied gas solvent to a container.

[0017] Figure 2 is a block diagram illustrating one embodiment of an apparatus for delivering a liquefied gas solvent to a container, including additional pressure and flow control components.

[0018] Figure 3 is a block diagram illustrating one embodiment of an apparatus for delivering a liquefied gas solvent to a container, wherein the liquefied gas source and / or the gas delivery line is temperature controlled.

[0019] Figure 4 is a block diagram illustrating one embodiment of an apparatus for delivering a liquefied gas solvent to a container, wherein the gas line between the valve and the container is temperature controlled.

[0020] Figure 5 is a block diagram illustrating one embodiment of an apparatus for delivering a liquefied gas solvent to a container, wherein the gas line between the source gas cylinder and the mass flow controller is temperature controlled.

[0021] Figure 6 is a block diagram illustrating one embodiment of an apparatus for delivering a liquefied gas solvent to a container, wherein a heat exchanger is used to cool the gas entering the container.

[0022] Figure 7 is a block diagram illustrating one embodiment of an apparatus for delivering a liquefied gas solvent to a container, wherein two or more liquefied gas solvent sources are connected in parallel to the container.

[0023] Figure 8is a block diagram illustrating one embodiment of an apparatus for dispensing liquefied gas electrolyte to a secondary container.

[0024] Fig. 9 is a block diagram illustrating one embodiment of an apparatus for dispensing liquefied gas electrolyte to a secondary container, including a loading volume.

[0025] Fig.10 is a block diagram illustrating one embodiment of an apparatus for dispensing liquefied gas electrolyte to a secondary container, wherein a heat sink is used to cool the secondary container.

[0026] Fig.11 is a block diagram illustrating one embodiment of an apparatus for dispensing liquefied gas electrolyte to a secondary container, wherein a liquid mass flow controller is used to control the liquefied gas flow rate.

[0027] Fig.12 is a block diagram illustrating one embodiment of an apparatus for dispensing liquefied gas electrolyte to a secondary container, wherein the liquefied gas electrolyte is dispensed through a dip tube.

[0028] Fig.13 is a block diagram illustrating one embodiment of an apparatus for dispensing liquefied gas electrolyte to a secondary container, wherein a temperature controlled reservoir is filled prior to the secondary container.

[0029] Fig.14 is shown with Fig.10 A block diagram of one embodiment of a similar apparatus for dispensing liquefied gas electrolyte to a secondary container wherein the valve is a mass flow controller connected to a processor. DETAILED DESCRIPTION

[0030] Reference is made herein to some specific embodiments of the present invention, including any best mode contemplated by the inventors for carrying out the present invention. Examples of these specific embodiments are shown in the accompanying drawings. Although the present invention has been described in conjunction with these specific embodiments, it should be understood that they are not intended to limit the present invention to the embodiments described or shown. On the contrary, they are intended to cover alternatives, modifications and equivalents that may be included in the spirit and scope of the present invention as defined by the appended claims.

[0031] In the following description, many specific details are set forth in order to provide a thorough understanding of the present invention. Specific example embodiments of the present invention may be implemented without some or all of these specific details. In other cases, process operations well known to those skilled in the art are not described in detail to avoid unnecessarily obscuring the present invention. Various techniques and mechanisms of the present invention are sometimes described in singular form for clarity. However, it should be noted that, unless otherwise stated, some embodiments include multiple iterations or multiple mechanisms of a technique. Similarly, in some embodiments, the various steps of the methods shown and described herein are not necessarily performed in the order indicated, or not performed at all. Therefore, some implementations of the methods discussed herein may include more or fewer steps than the steps shown or described. In addition, the techniques and mechanisms of the present invention sometimes describe connections, relationships, or communications between two or more entities. It should be noted that a connection or relationship between entities does not necessarily mean a direct, unimpeded connection, because various other entities or processes may reside between or occur between any two entities. Therefore, unless otherwise stated, the indicated connection does not necessarily mean a direct, unimpeded connection.

[0032] The following list of example features corresponds to the drawings for ease of reference, wherein like reference numerals indicate corresponding features throughout the specification and drawings: 1- Source cylinder 2- Pipeline 3-Mass flow controller 4-Container 5- Salt 6-Liquid gas electrolyte 7-Temperature sensor 8-Processor 9- Radiator 10-Isolation valve 11- Downstream isolation valve 12-Container Isolation Valve 13- Waste volume 14-Pressure sensor 15-Evacuation valve 16-Vacuum pump 17-Temperature control element 18-Temperature control element 19-Temperature control element 20-Heat exchanger 21-Gas transmission pipeline 22.1 - Liquefied gas source 22.1 22.x- Parallel liquefied gas source 23.1-Gas delivery pipeline 23.x-Parallel gas delivery pipelines 24-Secondary Container 25-Temperature control element 26- Loading capacity 27-Loading volume isolation valve 28-Temperature sensor 29-Radiator 30-Temperature sensor 31-Liquid Mass Flow Controller 32-Isolation valve 33-Immersion tube 34-Isolation valve 35- Storage 36-Temperature sensor 37-Isolation valve 38-Isolation valve 39-Temperature control element The proposed new method for preparing LGE uses a container with a temperature sensor to detect the temperature of the liquefied gas electrolyte in the container. The proposed LGE preparation device includes a liquefied gas solvent source, a flow controller, a container containing salt, a temperature sensor for detecting the temperature of LGE, and a processor connected to both the temperature sensor and the flow controller. During the LGE preparation process, a mass flow controller is used to control the flow rate of the liquefied gas solvent, and the flow rate is set by the processor connected to the flow controller. The processor is also connected to a temperature sensor, which monitors the temperature of the LGE during the liquefied gas solvent filling step.

[0033] In some embodiments, the container may initially be cooled to a temperature below that of the liquefied gas solvent source. As the liquefied gas solvent fills the container, a large amount of heat may be released into the container and cause the temperature of the LGE to increase. If the LGE temperature increases, the vapor pressure within the container may exceed the back pressure limit of the mass flow controller and compromise the MFC accuracy.

[0034] To reduce the rate of heating caused by the liquefied gas solvent fill, the processor can reduce the MFC flow rate. The processor can use temperature feedback from the temperature sensor and adjust the MFC flow rate to ensure that the back pressure on the MFC does not exceed the limit. The processor can optimize the MFC flow rate during the liquefied gas solvent fill to minimize the time required to prepare the LGE.

[0035] Example Implementation The following are 4 non-limiting examples showing various embodiments of the invention. Figure 1One such embodiment is shown in . In apparatus 100-1, liquefied gas is supplied by a liquefied gas solvent source 1 (shown as a gas cylinder in the present disclosure). The liquefied gas solvent may include one or more of the following; fluoromethane, difluoromethane, trifluoromethane, fluoroethane, tetrafluoroethane, pentafluoroethane, 1,1-difluoroethane, 1,2-difluoroethane, 1,1,1-trifluoroethane, 1,1,2-trifluoroethane, 1,1,1,2-tetrafluoroethane, 1,1,2,2-tetrafluoroethane, pentafluoroethane, chloromethane, chloroethane, thionyl fluoride, thionyl chlorofluoride, phosphoryl fluoride, phosphoryl chlorofluoride, sulfuryl fluoride, sulfuryl chlorofluoride, 1-fluoropropane, 2-fluoropropane, 1,1 In some embodiments, the components of the gas delivery device are connected by pipes or pipelines of variable size. In some embodiments, the outer diameter of the pipe can be 1 / 16 inch, 1 / 8 inch, 1 / 4 inch, 1 / 2 inch, 1 / 2 inch, 1 / 2 inch, 1 / 3 inch, 2 / 4 inch, 2 / 6 inch, 3 / 8 inch, 4 / 5 inch, 5 / 6 inch, 6 / 7 inch, 7 / 8 inch, 8 / 9 inch, 9 / 10 inch, 10 / 11 inch, 11 / 12 inch, 12 / 13 inch, 13 / 14 inch, 14 / 15 inch, 15 / 16 inch, 16 / 17 inch, 17 / 18 inch, 18 / 19 inch, 19 / 20 inch, 20 / 21 inch, 21 / 22 inch, 22 / 23 inch, 23 / 24 inch, 24 / 25 inch, 25 / 26 inch, 26 / 27 inch, 27 / 28 inch, 28 / 29 inch, 29 / 30 inch, 30 / 31 inch, 31 / 32 inch, 32 / 33 inch, 33 / 34 inch, 33 / 35 inch, 33 / 36 inch, 33 / 37 inch, 33 / 38 inch, 33 / 39 inch, 34 ... In some embodiments, the pipe size may be 1 / 8, 1 / 4, 1 / 2, 1, 2, or larger of a nominal pipe size.

[0036] The vapor of the liquefied gas solvent is transmitted through a mass flow controller (MFC) 3. MFC3 may include, but is not limited to, a thermal flow controller or a Coriolis flow controller. MFC3 has an upstream pressure P1 and a downstream pressure P2. A sufficient pressure difference between P1 and P2 is necessary for the precise operation of MFC3 described herein. The upstream pressure P1 is the working pressure of MFC3. The downstream pressure P2 is about 15 pounds per square inch less than P1. In a preferred embodiment, the pressure difference P1-P2 may be greater than 0.1psi, preferably greater than 1psi, and more preferably greater than 10psi. The vapor of the liquefied gas solvent is transferred to a container 4 through MFC3, where it is mixed with a salt 5 to form a liquefied gas electrolyte 6. Container 4 may be any suitable metal, ceramic or plastic device capable of accommodating a liquefied gas electrolyte having a vapor pressure greater than atmospheric pressure (100kPa) at a temperature of 293.15K. Container 4 may be of any size suitable for accommodating LGE. In some embodiments, container 4 may be greater than 1 cubic centimeter, greater than 10 cubic centimeters, greater than 100 cubic centimeters, greater than 1,000 cubic centimeters, greater than 10,000 cubic centimeters, greater than 100,000 cubic centimeters, or greater than 1,000,000 cubic centimeters. The salt 5 may include lithium bis(trifluoromethanesulfonyl)imide (LiTFSI), lithium hexafluorophosphate (LiPF6), lithium perchlorate (LiClO4), lithium hexafluoroarsenate (LiAsF6), lithium tetrachloroaluminate (LiAlCl4), lithium tetragalloaluminate, lithium bis(oxalato)borate (LiBOB), lithium hexafluorostannate, lithium difluoro(oxalato)borate (LiDFOB), lithium bis(fluorosulfonyl)imide (LiFSI), lithium aluminum fluoride (LiAlF3), lithium nitrate (LiNO3), lithium chloroaluminate, lithium tetrafluoroborate (LiBF4), lithium tetrachloroaluminate, lithium difluorophosphate, lithium tetrafluoro(oxalato)phosphate, lithium difluorobis(oxalato)phosphate, lithium borate, lithium oxalate, lithium thiocyanate, lithium tetrachlorogallate, lithium chloride, lithium bromide, lithium iodide, lithium carbonate, lithium fluoride, lithium oxide, lithium hydroxide, lithium nitride, lithium superoxide, lithium azide, lithium trioxide (lithium hydroxide), lithium trioxide (lithium trioxide ... deltate), dilithium squarate, lithium pentasquarate dihydrate, dilithium rhodonate, lithium oxalate, dilithium ketomalonate, lithium diketosuccinate or any corresponding salts, wherein the positively charged lithium cation replaces sodium or magnesium or any combination thereof.Other useful salts include salts with positively charged cations such as tetramethylammonium, tetraethylammonium, tetrapropylammonium, tetrabutylammonium, triethylmethylammonium, spiro-(1,1′)-bispyrrolidinium, 1,1-dimethylpyrrolidinium and 1,1-diethylpyrrolidinium, N,N-diethyl-N-methyl-N(2-methoxyethyl)ammonium, N,N-diethyl-N-methyl-N-propylammonium, N,N-dimethyl-N-ethyl-N-(3-methoxypropyl)ammonium, N,N- dimethyl-N-ethyl-N-benzylammonium, N,N-dimethyl-N-ethyl-N-phenylethylammonium, N-ethyl-N,N-dimethyl-N-(2-methoxyethyl)ammonium, N-tributyl-N-methylammonium, N-trimethyl-N-hexylammonium, N-trimethyl-N-butylammonium, N-trimethyl-N-propylammonium, 1,3-dimethylimidazolium, 1-(4-sulfobutyl)-3-methylimidazolium, 1-allyl-3H-imidazolium, 1-butyl-3-methyl imidazolium, 1-ethyl-3-methylimidazolium, 1-hexyl-3-methylimidazolium, 1-octyl-3-methylimidazolium, 3-methyl-1-propylimidazolium, H-3-methylimidazolium, trihexyl (tetradecyl) phosphonium, N-butyl-N-methylpiperidinium, N-propyl-N-methylpiperidinium, 1-butyl-1-methylpyrrolidinium, 1-methyl-1-(2-methoxyethyl)pyrrolidinium, 1-methyl-1-(3-methoxypropyl)pyrrolidinium, 1-Methyl-1-octylpyrrolidinium, 1-methyl-1-pentylpyrrolidinium or N-methylpyrrolidinium is paired with negatively charged anions such as acetate, bis(fluorosulfonyl)imide, bis(oxalato)borate, bis(trifluoromethanesulfonyl)imide, bromide, chloride, dicyanamide, diethyl phosphate, hexafluorophosphate, hydrogen sulfate, iodide, methanesulfonate, methylphosphonate, tetrachloroaluminate, tetrafluoroborate and trifluoromethanesulfonate, combinations thereof and isomers thereof.

[0037] The temperature of the LGE is detected using a temperature sensor 7. The temperature sensor 7 may be enclosed in any suitable feedthrough housing such as a dip tube. The temperature sensor 7 may be any sensor capable of having a wide dynamic range, such as a thermocouple. In some embodiments, the temperature sensor 7 may be a resistive sensor, a semiconductor sensor, or a thermistor. The temperature sensor 7 is connected to a processor 8. The processor 8 provides an initial flow rate setting on the MFC 3 and continuously monitors the flow rate during the liquefied gas solvent filling process. The processor 8 also monitors the temperature of the LGE through the temperature sensor 7 and adjusts the flow rate of the MFC 3 if the temperature of the LGE 8 rises above a predetermined maximum temperature. A person skilled in the art will recognize that the predetermined maximum temperature will be associated with a specific vapor pressure of the LGE 8. The vapor pressure of the LGE 8 may be the same as the downstream pressure P2. Therefore, the predetermined maximum temperature of the LGE 8 may correspond to a predetermined pressure difference P1-P2 as described above. The container 4 may be in contact with a heat sink 9 connected and regulated by the processor 8. A person skilled in the art will recognize that keeping the container 4 at a temperature lower than the source 1 will allow the liquefied gas solvent to condense into the container 4. The heat sink 9 can be connected to a refrigeration unit so that the container 4 can be cooled below room temperature. The container 4 can be cooled to below 50 degrees Celsius, preferably below 25 degrees Celsius, more preferably below 0 degrees Celsius, and even more preferably below -20 degrees Celsius. The heat sink 9 may include a thermally conductive material in contact with the container 4. The heat sink 9 may be, but is not limited to, a solid container, a metal sand bed, a liquid bath, an ice bath, a dry ice bath, or a gas stream. The refrigeration unit may be, but is not limited to, a circulating cooler, a Peltier cooler, or a refrigerant gas. The container 4 may also be precooled to below the temperature of the liquefied gas solvent source 1 so that the liquefied gas can be condensed into the container 4. In a preferred embodiment of the present invention, the temperature of the container 4 is maintained below the temperature of the liquefied gas solvent source 1.

[0038] Figure 2 Another embodiment of the present invention is shown. In the device 100-2, the liquefied gas solvent is supplied by the liquefied gas solvent source 1. The vapor of the liquefied gas solvent is transmitted through the upstream isolation valve 10, the mass flow controller 3, the downstream isolation valve 11 and the container isolation valve 12. The pipe section between the downstream isolation valve 11 and the container isolation valve 12 is defined as the waste volume 13, which has a pressure sensor 14 connected to the processor 8 to monitor the pressure. A person skilled in the art will recognize that the pressure monitor can be used to calculate the vapor density in the waste volume 13. When the liquefied gas solvent is delivered to the container 4, the vapor mass in the waste volume 13 can be calculated and taken into account. When the container 4 is full, the container isolation valve 12 is closed and the waste volume 13 is evacuated by the evacuation valve 15 and the pump 16. Considering the waste volume 13 can improve the accuracy of the delivery of the liquefied gas solvent to the container 4.

[0039] Another embodiment of the present invention is as Figure 3As shown. In device 100-3, the temperature of liquefied gas solvent source 1, isolation valve 10, pipeline 2 and MFC3 is controlled by temperature control element 17, which can be connected to processor 8 and can also include temperature sensor. In one embodiment, the temperature deviation between liquefied gas solvent source 1 and gas delivery pipeline is less than 10 degrees Celsius, preferably less than 5 degrees Celsius, more preferably less than 1 degree Celsius, and even more preferably less than 0.1 degrees Celsius. The temperature can be controlled to be higher than room temperature. The temperature can be controlled between -30 degrees Celsius and 100 degrees Celsius, preferably between 0 degrees Celsius and 50 degrees Celsius, more preferably between 20 degrees Celsius and 30 degrees Celsius. The processor can control the temperature control element 17 to keep the temperature change within + / -2.0 degrees Celsius during the filling process, more preferably within 0.5 degrees Celsius. When the liquefied gas solvent source 1 delivers gas during the filling process, it cools down, and the change in gas temperature may affect the accuracy of MFC3. The inaccuracies of the MFC 3 can be minimized by maintaining a near constant temperature during the filling process using a temperature control element 17. Those skilled in the art recognize that the temperature of the liquefied gas solvent source 1 can be adjusted to provide adequate vapor pressure and flow rate. The temperature control element 17 can be, but is not limited to, a heating blanket, a heating belt, a heating rope, or a heat regulating housing.

[0040] Figure 4 Another embodiment of the present invention is shown. In device 100-4, a temperature control element 18 (which can be connected to processor 8 and can further include a temperature sensor) is used to control the temperature of the downstream side of valve 11 (which is also the waste volume). The temperature can be controlled between -30 degrees Celsius and 100 degrees Celsius, preferably between 0 degrees Celsius and 50 degrees Celsius, and more preferably between 20 degrees Celsius and 30 degrees Celsius. The temperature control element 18 can be, but is not limited to, a heating blanket, a heating belt, a heating rope, or a heat regulating housing. The temperature control element 18 (through the processor 8) can keep the temperature variation within the waste volume within + / -2.0 degrees Celsius, more preferably within 0.5 degrees Celsius. The temperature control element 18 can be set to a preset temperature, and the set temperature and the pressure reading from the pressure sensor 14 can be used to determine the gas mass in the waste volume. This method can further improve the accuracy of the liquefied gas solvent delivery to the container 4.

[0041] Another embodiment of the present invention is as Figure 5As shown. In the device 100-5, the temperature of the isolation valve 10 and the pipeline 2 between the liquefied gas solvent source 1 and the MFC 3 is controlled by a temperature control element 19 (which can be connected to the processor 8 and can further include a temperature sensor). A person skilled in the art will recognize that the temperature between the gas outlet of the liquefied gas solvent source 1 and the MFC 3 can be adjusted to be higher than the temperature of the liquefied gas solvent source 1 to prevent condensation of the liquefied gas. The temperature control element 19 can be, but is not limited to, a heating blanket, a heating belt, a heating rope, or a heat regulating housing.

[0042] Figure 6 Another embodiment of the present invention is shown. In apparatus 100-6, there is a heat exchanger 20 upstream of container 4. Heat exchanger 20 cools the gas entering container 4. The heat exchanger can cool the gas to less than 50 degrees Celsius, less than 20 degrees Celsius, less than 0 degrees Celsius, less than minus 20 degrees Celsius, less than minus 40 degrees Celsius, or less than minus 60 degrees Celsius. The gas condenses above container 4 and flows into container 4 to mix with salt 5 and form LGE 6. One of ordinary skill in the art will recognize that the use of heat exchanger 20 can improve the collection of condensed liquefied gas solvent in container 4.

[0043] Figure 7 Another embodiment of the present invention is shown. Apparatus 100-7 includes two or more parallel gas delivery lines for supplying a liquefied gas solvent to container 4. Liquefied gas source 1 is connected to gas delivery line 21, liquefied gas source 22.1 is connected to gas delivery line 23.1, and both gas delivery lines 21 and 23.1 deliver gas to container 4. This embodiment can be extended to any number of liquefied gas sources and gas delivery lines (shown as liquefied gas sources 22.x and gas delivery lines 23.x, both of which are connected to container 4 and deliver gas to container 4). The gas delivery line can include components in any of the above embodiments for delivering an accurate mass of liquefied gas solvent at a desired flow rate. Different gases can be delivered to container 4 simultaneously or continuously.

[0044] Figure 8Another embodiment of the present invention is shown. In device 100-8, container 4, container isolation valve 12, liquefied gas electrolyte 6 and temperature sensor 7 are used to distribute LGE 6 into secondary container 24. Secondary container 24 can be any suitable metal, ceramic or plastic device capable of containing a liquefied gas electrolyte having a vapor pressure higher than atmospheric pressure (100 kPa) at a temperature of 293.15K. Secondary container 24 can be an electrochemical device such as a battery or capacitor. When container isolation valve 12 is opened, LGE 6 flows from container 4 to secondary container 24. Processor 8 monitors temperature sensor 7 and controls temperature control element 25. Those skilled in the art will recognize that during the filling process, the volume of liquid in container 4 decreases during the filling process, which causes LGE 6 to evaporate into the head space of container 4. This evaporation process removes heat from the surrounding of LGE 6 and may reduce the temperature of LGE 6. If the temperature of LGE 6 decreases, the density of LGE may change and reduce the accuracy of the mass of LGE transferred to secondary container 19. If the temperature of LGE decreases, the head space vapor pressure of LGE may also decrease. The device can use the pressure difference between the container 4 and the secondary container 24 to promote LGE transfer. If the headspace vapor pressure decreases, the LGE transfer efficiency may decrease. Therefore, the temperature control element 25 is used to provide heat to the container 4 to maintain a constant temperature. The temperature can be controlled between -30 degrees Celsius and 100 degrees Celsius, preferably between 20 degrees Celsius and 50 degrees Celsius, and more preferably between 30 degrees Celsius and 40 degrees Celsius. The temperature control element 25 can be, but is not limited to, a heating blanket, a heating belt, a heating rope, or a heat regulating shell. The temperature control element 25 can maintain the temperature variation within the container within + / -2.0 degrees Celsius, and more preferably within 0.5 degrees Celsius.

[0045] Fig. 9Another embodiment of the present invention is shown. In device 100-9, container 4 dispenses LGE 6 into an intermediate container, referred to as loading volume 26. When container isolation valve 12 is opened, LGE 6 is transferred from container 4 to loading volume 26. During this step, isolation valve 27 is closed, and LGE 6 completely fills loading volume 26. Isolation valve 12 is then closed. In a subsequent step, loading volume isolation valve 27 is opened, and loading volume 26 dispenses LGE 6 into secondary container 24. Loading volume 26 can be any suitable metal, ceramic, or plastic device capable of containing a liquefied gas electrolyte having a vapor pressure above atmospheric pressure (100 kPa) at a temperature of 293.15 K. Loading volume 26 can be configured as a predetermined volume to dispense an accurate mass of LGE 6 into secondary container 24. A temperature sensor 28 is connected to loading volume 26 and processor 8 to monitor the temperature. One of ordinary skill in the art will recognize that both the container 4 and the load volume 26 should be maintained at the same temperature to provide a uniform density within the LGE 6. It is known that in order to deliver an accurate mass of LGE 6 to the secondary container 24, it may be desirable for the LGE 6 to have a uniform density. Therefore, a temperature control element 25 is used to maintain a constant uniform temperature in the container 4 and the load volume 26. The temperature may be controlled between -30 degrees Celsius and 100 degrees Celsius, preferably between 20 degrees Celsius and 50 degrees Celsius, and more preferably between 30 degrees Celsius and 40 degrees Celsius. The temperature control element 25 may be, but is not limited to, a heating blanket, a heating tape, a heating rope, or a thermally regulated housing. The temperature control element 25 may maintain temperature variations within the container within + / - 2.0 degrees Celsius, and more preferably within 0.5 degrees Celsius.

[0046] The pressure differential may facilitate the flow of LGE 6 from the loading volume 26 into the secondary container 24. The secondary container 24 may initially be evacuated to a pressure of less than 14.7 psi at room temperature of 293.15 K. When the loading volume isolation valve 27 is opened, the LGE 6 will be dispensed into the secondary container 24 and partially evaporated in the secondary container head space. To achieve efficient flow of the LGE 6 into the secondary container 24, the loading volume 26 may be heated to a temperature higher than that of the secondary container 24, such that the vapor pressure within the loading volume 26 is always higher than the vapor pressure in the secondary container 24. In one embodiment, the temperature difference between the loading volume 26 and the secondary container 24 is greater than 1 degree Celsius, preferably greater than 5 degrees Celsius, and more preferably greater than 10 degrees Celsius.

[0047] Fig.10Another embodiment of the present invention is shown. In device 100-10, secondary container 24 has a heat sink 29 and a temperature sensor 30, both of which are connected to processor 8. Heat sink 29 can be used to remove heat from secondary container 24 as secondary container 24 fills with LGE 6, so that secondary container 24 maintains a constant temperature during the filling process of LGE 6. Heat sink 29 can be used to maintain a temperature difference between the load volume 26 and secondary container 24 as described above. Temperature sensor 30 can be connected to processor 8 so that processor 8 can monitor the temperature difference between the load volume 26 and secondary container 24 and adjust the heat sink as needed.

[0048] Fig.11 Another embodiment of the present invention is shown. In the apparatus 100-11, the LGE 6 is transferred from the container 4 to the secondary container 24 using a liquid mass flow controller 31. The liquid mass flow controller 31 can be a thermal type, a Coriolis type, a magnetic induction type, or a vortex type. The liquid mass flow controller 31 can be connected to the processor 8 so that a predetermined mass of LGE 6 can be input to the processor 8 and automatically dispensed using the liquid mass flow controller 31.

[0049] Fig.12Another embodiment of the present invention is shown. In apparatus 100-12, the apparatus is oriented so that the vessel isolation valve 32 is located above the vessel 4, and a dip tube 33 extends from the vessel isolation valve 32 to the LGE 6. The LGE 6 is transferred to the secondary vessel 24 through the dip tube 33, the vessel isolation valve 32, and the valve 34. The LGE 6 can be transferred from the vessel 4 to the secondary vessel 24 using the pressure difference between the two vessels. Therefore, the temperature control element 35 is used to maintain a constant, uniform temperature within the vessel 4, and the heat sink 36 is used to remove heat from the secondary vessel 24. The secondary vessel 24 can initially be evacuated to a pressure of less than 15 psia at room temperature of 293.15K. The processor 8 can receive the temperature measurement from the temperature sensor 7 and adjust the temperature control element 20 so that the temperature of the vessel 4 and the LGE 6 is maintained at a predetermined set point. The processor can also adjust the heat sink 29 based on the reading of the temperature sensor 30. One of ordinary skill in the art will recognize that a higher temperature of the container 4 than the secondary container 24 will result in a higher pressure in the container 4 than in the secondary container 24 and facilitate the flow of the LGE 6 from the container 4 into the secondary container 24. The temperature of the container 4 may be controlled between -30 degrees Celsius and 100 degrees Celsius, preferably between 20 degrees Celsius and 50 degrees Celsius, and more preferably between 30 degrees Celsius and 40 degrees Celsius. The temperature control element 20 may be, but is not limited to, a heating blanket, a heating tape, a heating cord, or a heat regulating enclosure. The temperature control element 20 may maintain the temperature variation within the container within + / -2.0 degrees Celsius, and more preferably within 0.5 degrees Celsius. The heat sink 29 on the secondary container 24 may be connected to a refrigeration unit so that the secondary container 24 may be cooled to room temperature or lower. The secondary container 24 may be cooled to less than 50 degrees Celsius, preferably less than 25 degrees Celsius, and more preferably less than 20 degrees Celsius. The heat sink 29 may include a thermally conductive material in contact with the secondary container 24. The heat sink 29 can be, but is not limited to, a solid container, a metal sand bed, a liquid bath, an ice bath, a dry ice bath, or an air flow. The refrigeration unit can be, but is not limited to, a circulating cooler, a Peltier cooler, or a refrigerant gas. In one embodiment, the temperature difference between the container 4 and the secondary container 24 is greater than 1 degree Celsius, preferably greater than 5 degrees Celsius, and more preferably greater than 10 degrees Celsius. In a preferred embodiment of the present invention, the temperature of the secondary container 24 is maintained at close to room temperature, i.e., 20 degrees Celsius. The temperature of the secondary container 24 can be monitored by a temperature sensor 30 connected to the processor 8.

[0050] Fig.13Another embodiment of the present invention is shown. In device 100-13, the device includes a reservoir 35 with a temperature sensor 36, a valve 37 isolating the reservoir from a conduit connected to valve 12 and container 4, a load volume 26 with a temperature sensor 28, a valve 38 isolating the reservoir 38 from the load volume 26, and a temperature control element 39. LGE 6 from container 4 is filled into the reservoir 35 using a method similar to that described above. The temperature of the reservoir 35 and the load volume 26 is maintained below the temperature of the container 4 to facilitate the flow of LGE 6 under the pressure difference. The temperature control element 39, the temperature sensor 28, and the temperature sensor 36 are connected to the processor 8 to maintain the temperature below the temperature of the temperature sensor 7. In a preferred embodiment, the temperature difference is greater than 1 degree Celsius, greater than 5 degrees Celsius, or greater than 10 degrees Celsius. In a preferred embodiment, the temperature of the reservoir 35 and the load volume 26 is controlled between -30 degrees Celsius and 100 degrees Celsius, preferably between 20 degrees Celsius and 50 degrees Celsius, and more preferably between 30 degrees Celsius and 40 degrees Celsius. The temperature control element 39 can be, but is not limited to, a heating blanket, a heating tape, a heating cord, or a thermally regulated enclosure. The temperature control element 39 can maintain the temperature variation within the container within + / - 2.0 degrees Celsius, and more preferably within 0.5 degrees Celsius. The reservoir 35 can improve the accuracy of the LGE 6 delivery to the secondary container 24 by allowing the LGE 6 to reach thermal equilibrium before delivery to the secondary container 24.

[0051] Fig.14 Another embodiment of the present invention is shown. Device 100-14 and Fig.13 The illustrated device 100-13 is similar except that valves 37, 38, 27, and 32 are mass flow controllers connected to processor 8. In this device 100-14, processor 8 can activate the mass flow controllers of valves 32, 37, and 38 to regulate the flow between container 4 and reservoir 35. Similarly, the processor can activate the mass flow controllers of valves 37, 38, and 27 to regulate the flow between reservoir 35 and secondary container 24. The flow regulation can be used in conjunction with temperature control elements 20 and 39 and heat sink 29 to maintain an optimal temperature for filling reservoir 35 and / or filling secondary container 24.

[0052] Although exemplary embodiments and applications of the present invention have been described herein, including applications as described above and shown in the included example figures, the present invention is not limited to these exemplary embodiments and applications, nor is it limited to the operation of the exemplary embodiments and applications or the manner described herein. In fact, it will be appreciated by those skilled in the art that many variations and modifications of the exemplary embodiments are possible. The present invention may include any device, structure, method, or function as long as the resulting device, system, or method falls within the scope of one of the claims allowed by the Patent Office based on this patent application or any related patent application.

Claims

1. A device for dispensing a liquefied gas electrolyte, the device comprising: a liquefied gas electrolyte container containing a liquefied gas electrolyte, the liquefied gas electrolyte containing a liquefied gas solvent and a salt, the liquefied gas solvent having a vapor pressure of 100 kPa or more at a temperature of 293.15 K; a temperature sensor for detecting the temperature of the liquefied gas electrolyte in the liquefied gas electrolyte container; temperature control elements for heating liquefied gas electrolyte containers; a valve connected to the liquefied gas electrolyte container and the secondary container; A processor connected to the temperature sensor and the temperature control element, the processor being adapted to perform the following steps: a. Receive temperature readings from temperature sensors; b. Activating a temperature control element based on the temperature reading to maintain the temperature of the liquefied gas electrolyte container within a predetermined temperature or temperature range.

2. The apparatus of claim 1, wherein the valve is a mass flow controller connected to the processor, and wherein the processor is adapted to activate the mass flow controller to regulate the flow of the liquefied gas electrolyte from the liquefied gas electrolyte container to the secondary container.

3. The device of claim 1, wherein the secondary container is an electrochemical device.

4. The device of claim 3, wherein the electrochemical device is a battery or a capacitor.

5. The apparatus of claim 1, wherein the predetermined temperature range is 303.15K + / - 2K.

6. A device for dispensing a liquefied gas electrolyte, the device comprising: a liquefied gas electrolyte container containing a liquefied gas electrolyte, the liquefied gas electrolyte containing a liquefied gas solvent and a salt, the liquefied gas solvent having a vapor pressure of 100 kPa or more at a temperature of 293.15 K; a first temperature sensor, for detecting the temperature of the liquefied gas electrolyte in the liquefied gas electrolyte container; a first temperature control element for heating the liquefied gas electrolyte container; a first valve connected to the liquefied gas electrolyte container and the reservoir; a second temperature sensor for detecting the temperature of the liquefied gas electrolyte in the reservoir; a second temperature control element for heating the reservoir; a second valve connected to the reservoir and the secondary container; a processor connected to the first and second temperature sensors and the first and second temperature control elements, the processor being adapted to perform the following steps: a. Receiving temperature readings from a first temperature sensor and a second temperature sensor; b. starting a first temperature control element based on a temperature reading from a first temperature sensor to maintain the temperature of the liquefied gas electrolyte container at a predetermined temperature or temperature range; c. activating a second temperature control element based on the temperature reading from the second temperature sensor to maintain the temperature of the reservoir within a second predetermined temperature or temperature range.

7. The apparatus of claim 6, wherein the first valve is a mass flow controller connected to the processor, and wherein the processor is adapted to activate the mass flow controller to regulate the flow of liquefied gas electrolyte from the liquefied gas electrolyte container to the reservoir.

8. The apparatus of claim 6, wherein the second valve is a mass flow controller connected to the processor, and wherein the processor is adapted to activate the mass flow controller to regulate the flow of the liquefied gas electrolyte from the reservoir to the secondary container.

9. The device of claim 6, wherein the secondary container is an electrochemical device.

10. The device of claim 9, wherein the electrochemical device is a battery or a capacitor.

11. The apparatus of claim 6, wherein the first predetermined temperature range is 313.15K + / - 2K.

12. The apparatus of claim 6, wherein the second predetermined temperature range is 303.15K + / - 2K.

13. The apparatus according to claim 6, further comprising: a third temperature sensor for detecting the temperature of the liquefied gas electrolyte in the secondary container; a radiator for cooling the secondary container; The processor is connected to the third temperature sensor and the heat sink and is adapted to perform the following steps: The heat sink is activated based on the temperature reading from the third temperature sensor to maintain the temperature of the secondary container within a third predetermined temperature or temperature range.

14. The apparatus of claim 7, wherein the third predetermined temperature range is 293.15K + / - 5K.

15. A method of dispensing a liquefied gas electrolyte from a liquefied gas electrolyte container to a secondary container through a valve, the liquefied gas electrolyte comprising a liquefied gas solvent and a salt, the liquefied gas solvent having a vapor pressure above 100 kPa at a temperature of 293.15 K, wherein the liquefied gas electrolyte container comprises a temperature sensor to detect the temperature of the liquefied gas electrolyte in the liquefied gas electrolyte container, the method comprising: a. Open the valve to allow the liquefied gas electrolyte to flow from the liquefied gas electrolyte container into the secondary container; b. Read the temperature sensor; c. Based on the temperature reading, heating the liquefied gas electrolyte container to maintain the temperature of the liquefied gas electrolyte container within a predetermined temperature or temperature range.

16. The method of claim 15, wherein the secondary container is an electrochemical device.

17. The method of claim 16, wherein the electrochemical device is a battery or a capacitor.

18. The method of claim 15, wherein the predetermined temperature range is 303.15K + / - 2K.

19. The method according to claim 15, wherein the secondary container comprises a second temperature sensor and a heat sink, the second temperature sensor is used to detect the temperature of the liquefied gas electrolyte in the secondary container, and the heat sink is used to cool the secondary container, the method further comprising: d. Reading from the second temperature sensor; e. Cooling the secondary container to maintain the temperature of the secondary container within a second predetermined temperature or temperature range based on the temperature reading from the second sensor.

20. The method of claim 19, wherein the predetermined temperature range is 293.15K + / - 5K.

21. The method of claim 15, wherein the secondary container comprises a reservoir, the reservoir comprises a second temperature sensor and a second temperature control element, the second temperature sensor detecting a temperature of the liquefied gas electrolyte in the reservoir, the method further comprising: d. Reading from the second temperature sensor; e. Activating a second temperature control element based on the temperature reading from the second temperature sensor to maintain the temperature of the reservoir within a second predetermined temperature or temperature range.

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