US20180194625A1 - Gas-Loading and Packaging Method and Apparatus - Google Patents
Gas-Loading and Packaging Method and Apparatus Download PDFInfo
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- US20180194625A1 US20180194625A1 US15/891,416 US201815891416A US2018194625A1 US 20180194625 A1 US20180194625 A1 US 20180194625A1 US 201815891416 A US201815891416 A US 201815891416A US 2018194625 A1 US2018194625 A1 US 2018194625A1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
- C01B3/0026—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof of one single metal or a rare earth metal; Treatment thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
- C01B3/08—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents with metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/02—Preparation of oxygen
- C01B13/0222—Preparation of oxygen from organic compounds
- C01B13/0225—Peroxy compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/04—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids
- H01M8/04082—Arrangements for control of reactant parameters, e.g. pressure or concentration
- H01M8/04089—Arrangements for control of reactant parameters, e.g. pressure or concentration of gaseous reactants
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/04—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids
- H01M8/04082—Arrangements for control of reactant parameters, e.g. pressure or concentration
- H01M8/04089—Arrangements for control of reactant parameters, e.g. pressure or concentration of gaseous reactants
- H01M8/04119—Arrangements for control of reactant parameters, e.g. pressure or concentration of gaseous reactants with simultaneous supply or evacuation of electrolyte; Humidifying or dehumidifying
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/06—Combination of fuel cells with means for production of reactants or for treatment of residues
- H01M8/0606—Combination of fuel cells with means for production of reactants or for treatment of residues with means for production of gaseous reactants
- H01M8/0612—Combination of fuel cells with means for production of reactants or for treatment of residues with means for production of gaseous reactants from carbon-containing material
- H01M8/0643—Gasification of solid fuel
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
- C01B3/10—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents by reaction of water vapour with metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/04—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids
- H01M8/04082—Arrangements for control of reactant parameters, e.g. pressure or concentration
- H01M8/04201—Reactant storage and supply, e.g. means for feeding, pipes
- H01M8/04216—Reactant storage and supply, e.g. means for feeding, pipes characterised by the choice for a specific material, e.g. carbon, hydride, absorbent
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
-
- Y02E60/362—
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Definitions
- the present disclosure relates generally to alternative energy technologies and, more particularly, to methods and apparatus for gas-loading and packaging solid materials for use in hydrogen fuel cells and low-energy nuclear reactions (LENRs).
- LNRs low-energy nuclear reactions
- the loading of hydrogen (or its isotopes) into a solid material is an important technology for hydrogen fuel cells and low energy nuclear reactors.
- a hydrogen loading ratio in palladium above 0.8 is widely believed to be a necessary condition to produce a LENR.
- High loading of hydrogen into a fuel cell compatible material increases the life of the fuel cell.
- the loading of methane into metal-organic frameworks is an important, emerging technology to increase the storage capacity of this fuel source. In each of these scenarios, the loading process must be controllable, quantifiable and sustainable to be repeatable and production-worthy.
- the amount of hydrogen loaded into a solid material can be quantified by measuring an increase in a sample's mass or a decrease in pressure of a fixed quantity of gas in the presence of the material.
- Measuring the pressure decrease in a fixed quantity of gas suffers from one major source of error.
- the gas may adsorb on all surfaces present in addition to the material of interest.
- the existing technologies do not allow for the hydrogen load to be sustained after quantification. For high purity, homogeneous materials this does not necessarily present a problem because sample of the same material may be used in other processes.
- sample-to-sample variability can be considerable creating a need to characterize materials for fuel cell or LENR use.
- the present disclosure describes a method and apparatus for loading a solid material with a gas and packaging the solid material in a sealed container.
- the solid material is placed in a chamber with a controlled environment.
- the environment may be a vacuum, hydrogen or one of its isotopes, or any other gas of interest.
- the loading of a gas into or onto a solid material is quantified by measuring the solid material's increase in mass.
- the loaded material is transferred to a second chamber where it is packaged while maintaining the loading gas atmosphere and pressure.
- FIG. 1 is a schematic diagram illustrating a system for gas-loading and packaging a solid material.
- FIGS. 2A-2C illustrate an intake process during which the sample loading chamber of the gas-loading and packaging system is evacuated and then pressurized.
- FIGS. 2D and 2E illustrate a first transfer process during which the solid material is transferred from the sample loading chamber to a process chamber of the gas-loading and packaging system.
- FIG. 2F illustrates a gas-loading process during which the solid material is loaded with hydrogen gas in the process chamber.
- FIGS. 2G and 2H illustrate a second transfer process during which the solid material is transferred from the process chamber to a packaging chamber gas-loading and packaging system.
- FIGS. 2I and 2J illustrate the packaging process during which the solid material is packaged into a sealed container.
- FIG. 3 illustrates an exemplary controller for controlling the gas loading and packaging system
- FIGS. 4A and 4B illustrate an exemplary method for gas-loading and packaging a solid material.
- FIG. 1 illustrates an exemplary gas-loading and packaging system 10 according to one exemplary embodiment.
- the main function of the gas-loading and packaging system 10 is to load a solid material used in a hydrogen fuel cell or LENR with gas and package the solid material.
- the gas may comprise a hydrogen gas or other gas.
- hydrogen gas includes all gaseous isotopes of hydrogen including deuterium and tritium.
- the solid material may, for example, comprise palladium, a nickel alloy, platinum, or other metal.
- the solid material is loaded with gas by exposing the solid material to the gas under high pressure. When the solid material is exposed to gas under pressure, the gas absorbs into or adsorbs onto the solid material. After the solid material is loaded with gas, the gas atmosphere and high pressure are maintained while the solid material is packaged in a sealed container that is capable of retaining the high pressure gas.
- the main functional components of the gas-loading and packaging system 10 comprise a gas source 12 , rough/backing pump 15 , turbo-molecular pump 17 , sample loading chamber 20 , process chamber 40 , and packaging chamber 60 .
- the gas source 12 connects via gas supply line 14 to the sample loading chamber 20 , process chamber 40 , and packaging chamber 60 .
- Control valves 22 , 42 , and 62 control the flow of gas from the gas source 12 into the sample loading chamber 20 , process chamber 40 , and packaging chamber 60 respectively.
- the rough/backing pump 15 connects via vacuum line 16 to the sample loading chamber 20 , process chamber 40 , and packaging chamber 60 .
- Control valves 24 , 44 , and 66 connect/disconnect the sample loading chamber 20 , process chamber 40 , and packaging chamber 60 respectively from the rough/backing pump 15 .
- the turbo-molecular pump 17 connects via vacuum line 18 to the sample loading chamber 20 , process chamber 40 , and packaging chamber 60 .
- Control valves 26 , 46 , and 64 connect/disconnect the sample loading chamber 20 , process chamber 40 , and packaging chamber 60 respectively from the turbo-molecular pump 17 .
- the sample loading chamber 20 is the point of entry where the solid material is initially introduced into the gas-loading and packaging system 10 .
- the sample loading chamber 20 includes a door 34 through which a solid material is placed inside the sample loading chamber 20 . When closed, the door 34 forms a seal that is capable of holding pressure or vacuum inside the sample loading chamber 20 .
- a pressure gauge 28 measures the gas pressure inside the sample loading chamber 20 .
- a linear transfer apparatus 36 is disposed inside the sample loading chamber 20 for transferring the solid material from the sample loading chamber 20 to the process chamber 40 as hereinafter described in greater detail.
- the sample loading chamber 20 is connected to the process chamber 40 by a sealed passageway 30 including a gate valve 32 for isolating the sample loading chamber from the process chamber 40 , and vice versa.
- the passageway 30 and gate valve 32 are sized to allow the transfer of the solid material from the sample loading chamber 20 to the process chamber 40 while maintaining the gas atmosphere and high gas pressure.
- the process chamber 40 is where the solid material is exposed to and loaded with hydrogen gas.
- a pressure gauge 48 measures the gas pressure inside the process chamber 40 .
- a scale 54 inside the process chamber 40 continuously measures the mass of the solid material while the solid material is in the process of being loaded with hydrogen gas. As described in more detail below, the measurements of the mass of the solid material are used to determine when the solid material is loaded with a desired amount of hydrogen gas. Measurements of the mass of the solid material may be made when the solid material is initially placed in the process chamber 40 to determine the starting mass of the solid material and at predetermined or periodic time intervals during the loading of gas into the solid material to determine the change in mass of the solid material. The measurements may continue until the predetermined amount of gas is loaded into the solid material.
- the process chamber 40 is connected to the packaging chamber 60 by a sealed passageway 50 including a gate valve 52 for isolating the process chamber 40 from the packaging chamber 60 , and vice versa.
- the passageway 50 and gate valve 52 are sized to allow the transfer of the solid material from the process chamber 40 to the packaging chamber 60 while maintaining the gas atmosphere and high gas pressure.
- the packaging chamber 60 is where the solid material loaded with hydrogen gas is packaged in a sealed container.
- a pressure gauge 68 measures the gas pressure inside the packaging chamber 60 .
- the packaging chamber 60 includes a door 72 through which the sealed container containing the solid material is removed from the gas loading and packaging system 10 . When closed, the door 34 forms a seal that is capable of holding pressure or vacuum inside the packaging chamber 60 .
- a linear transfer apparatus 70 is disposed inside the packaging chamber 60 . The linear transfer apparatus is used to transfer the solid material after it is loaded with hydrogen gas from the process chamber 40 to the packaging chamber 60 .
- the operation of the gas loading and packaging system 10 can be broken down into five processes: an intake process, a first transfer process, a gas loading process, a second transfer process, and a packaging process.
- a sample of solid material e.g. palladium
- the sample loading chamber 20 is evacuated to remove contaminants. Once the contaminants are removed, the sample loading chamber 20 is pressurized to about 760 Torr, which is one atmosphere.
- the intake process ends and the first transfer process begins, during which the solid material is transferred from the sample loading chamber 20 to the process chamber 40 .
- the pressure in the process chamber is raised to about 10 Torr to 50 Torr above the sample loading chamber pressure.
- the higher pressure in the process chamber 40 relative to the sample loading chamber 20 serves to minimize the flow of any contaminants from the sample loading chamber 20 to the process chamber 40 during the transfer of the solid material.
- the gate valve 32 isolating the sample loading chamber 20 is then opened and the linear transfer apparatus 36 transfers the sample of solid material into the process chamber 40 and places the sample on the scale 54 .
- the linear transfer apparatus 36 may comprise a retractable arm that picks up the solid material, extends into the process chamber 40 and deposits the solid material on the scale 54 , and then retracts back into the sample loading chamber 20 .
- the gate valve 32 is closed. At this point, the first transfer process ends and the gas loading process begins, during which the solid material is loaded with hydrogen gas.
- both gate valves 32 and 52 are closed to isolate the process chamber 40 .
- the process chamber pressure is increased to a pressure in the range of about 3800 Torr to about 7600 Torr.
- hydrogen gas is absorbed into and adsorbed onto the solid material.
- the amount of hydrogen gas loaded onto the solid material, by absorption and/or adsorption, is determined by the change of mass of the solid material.
- the change of mass of the solid material is related to the amount of hydrogen by:
- L is the loading ratio of atoms of hydrogen to atoms of palladium
- ⁇ m is the change in mass of the palladium sample in grams
- P is the mass of the palladium sample in grams.
- the mass of the solid material is continuously or periodically checked during the gas loading process to determine when the solid material is loaded with a desired amount of hydrogen gas.
- the change of mass is calculated and compared to a pre-computed mass change threshold to determine when the solid material is loaded with a desired amount of hydrogen gas.
- the amount of hydrogen gas loaded onto the solid material is computed according to Equation 1. The gas loading process ends when the change of mass reaches the threshold, or when the calculated amount of hydrogen gas loaded onto the solid material equals the desired amount.
- the second transfer process begins.
- the pressure inside the packaging chamber is raised to about 10 Torr to about 50 Torr below the process chamber pressure and the gate valve 52 is opened.
- the lower pressurization of the packaging chamber 60 relative to the process chamber 40 serves to minimize the flow of any contaminants from the packaging chamber 60 to the process chamber 40 since the packaging chamber 60 is opened to the atmosphere to remove the sample.
- the linear transfer apparatus 70 in the packaging chamber 60 transfers the solid material loaded with hydrogen gas from the process chamber 40 into the packaging 60 .
- the linear transfer apparatus 70 may comprise a retractable arm that extends into the process chamber 40 , picks up the solid material, and then retracts back into the packaging chamber 60 .
- the gate valve 52 is closed to isolate the packaging chamber 60 . At this point the second transfer process ends and the packaging process begins.
- a sealed container is placed inside the packaging chamber 60 prior to the start of the packaging process.
- the sealed container may be introduced into the packaging chamber 60 anytime before the start of the second transfer process.
- the packaging chamber 60 Prior to the start of the packaging process, the packaging chamber 60 may be evacuated to remove contaminants.
- the packaging chamber 60 is outfitted with vacuum/high pressure mechanical arms or other accessories as needed to transfer the solid material sample into a container that is capable of maintaining the process gas at the process pressure.
- the packaging chamber 60 may comprise a glove box that enables a human user to handle and package the solid material.
- the packaging chamber 60 may be evacuated to atmospheric pressure, nominally 760 Torr (101 kPa).
- the door 72 to the packaging chamber 60 is then opened and the packaged solid material sample is removed.
- the packaging enables the solid material sample to maintain the incorporated gas, maximizing its usefulness in application and longevity.
- FIGS. 2A-2J illustrate some of these steps.
- FIG. 3 illustrates an exemplary control circuit 100 for controlling the operation of the gas loading and packaging system 10 .
- the control circuit 100 comprises a processing circuit 102 that implements the main control functions of the gas loading and packaging system 10 .
- the processing circuit 102 may comprise one or more processors, hardware circuits, firmware, of a combination thereof.
- the processing circuit 102 receives inputs from the pressure gauges 28 , 48 , and 68 , and the scale 54 and outputs control signals to various solenoids and switches that control the valves as hereinabove described.
- Solenoids or switches S 22 , S 24 , S 26 , S 42 , S 44 , S 46 , S 62 ,S 64 , and S 66 control valves 22 , 24 , 26 , 42 , 44 , 46 , 62 , 64 , and 66 respectively.
- Solenoids or switches S 32 and S 52 control gate valves 32 and 52 respectively.
- Solenoids or switches S 12 , S 15 and S 17 control the gas source 12 , rough/backing pump 15 , and turbo-molecular pump 17 respectively.
- the processing circuit 102 may also send control signals to the linear transfer apparatus 36 and 70 .
- FIGS. 4A and 4B illustrate an exemplary method 150 of gas loading and packaging a solid material.
- the solid material is transferred to a process chamber 40 (block 155 ).
- the process chamber 40 is pressurized with hydrogen gas until the process chamber pressure reaches a first pressure level (block 160 ).
- the process chamber pressure is maintained above the first pressure level to load the solid material with hydrogen gas.
- the mass of the solid material is measured and the measurements are used to determine when the solid material is loaded with a predetermined amount of hydrogen gas based (blocks 165 and 170 ).
- the packaging chamber 60 When the desired amount of hydrogen gas is loaded into the solid material, pressurize the packaging chamber 60 with hydrogen gas until the packaging chamber pressure reaches a second pressure level lower than the first predetermined pressure level and transfer the solid material from the process chamber to the packaging chamber (blocks 175 and 180 ) The solid material is then packaged in a sealed container while maintaining the packaging chamber pressure at or above second pressure level, after which the sample chamber is opened and the sealed container is removed from the packaging chamber 60 (blocks 190 and 195 ).
- the packaging chamber pressure may be raised to a third pressure level higher than the first pressure level while the solid material is packaged (block 185 ).
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Abstract
Description
- This application is a divisional application of U.S. Utility patent application Ser. No. 15/615,137, titled “Gas-Loading and Packaging Method and Apparatus,” filed on Jun. 6, 2017, which claims the benefit of priority of U.S. Provisional Patent Application No. 62/346,238, titled “GAS-LOADING AND PACKAGING METHOD AND APPARATUS” filed on Jun. 6, 2016 which are incorporated herein in its entirety by this reference.
- The present disclosure relates generally to alternative energy technologies and, more particularly, to methods and apparatus for gas-loading and packaging solid materials for use in hydrogen fuel cells and low-energy nuclear reactions (LENRs).
- The loading of hydrogen (or its isotopes) into a solid material is an important technology for hydrogen fuel cells and low energy nuclear reactors. A hydrogen loading ratio in palladium above 0.8 is widely believed to be a necessary condition to produce a LENR. High loading of hydrogen into a fuel cell compatible material increases the life of the fuel cell. The loading of methane into metal-organic frameworks is an important, emerging technology to increase the storage capacity of this fuel source. In each of these scenarios, the loading process must be controllable, quantifiable and sustainable to be repeatable and production-worthy.
- Several techniques are known for measuring the amount of hydrogen that is loaded into a solid material. The amount of hydrogen loaded into a solid material can be quantified by measuring an increase in a sample's mass or a decrease in pressure of a fixed quantity of gas in the presence of the material.
- Measuring the pressure decrease in a fixed quantity of gas suffers from one major source of error. The gas may adsorb on all surfaces present in addition to the material of interest. Also, the existing technologies do not allow for the hydrogen load to be sustained after quantification. For high purity, homogeneous materials this does not necessarily present a problem because sample of the same material may be used in other processes. In the case of multi-component materials such as layered thin films, nano-particles, or temperature sensitive alloys, sample-to-sample variability can be considerable creating a need to characterize materials for fuel cell or LENR use.
- The present disclosure describes a method and apparatus for loading a solid material with a gas and packaging the solid material in a sealed container. The solid material is placed in a chamber with a controlled environment. The environment may be a vacuum, hydrogen or one of its isotopes, or any other gas of interest. The loading of a gas into or onto a solid material is quantified by measuring the solid material's increase in mass. The loaded material is transferred to a second chamber where it is packaged while maintaining the loading gas atmosphere and pressure.
-
FIG. 1 is a schematic diagram illustrating a system for gas-loading and packaging a solid material. -
FIGS. 2A-2C illustrate an intake process during which the sample loading chamber of the gas-loading and packaging system is evacuated and then pressurized. -
FIGS. 2D and 2E illustrate a first transfer process during which the solid material is transferred from the sample loading chamber to a process chamber of the gas-loading and packaging system. -
FIG. 2F illustrates a gas-loading process during which the solid material is loaded with hydrogen gas in the process chamber. -
FIGS. 2G and 2H illustrate a second transfer process during which the solid material is transferred from the process chamber to a packaging chamber gas-loading and packaging system. -
FIGS. 2I and 2J illustrate the packaging process during which the solid material is packaged into a sealed container. -
FIG. 3 illustrates an exemplary controller for controlling the gas loading and packaging system -
FIGS. 4A and 4B illustrate an exemplary method for gas-loading and packaging a solid material. - Referring now to the drawings,
FIG. 1 illustrates an exemplary gas-loading andpackaging system 10 according to one exemplary embodiment. The main function of the gas-loading andpackaging system 10 is to load a solid material used in a hydrogen fuel cell or LENR with gas and package the solid material. The gas may comprise a hydrogen gas or other gas. As used herein, the term hydrogen gas includes all gaseous isotopes of hydrogen including deuterium and tritium. The solid material may, for example, comprise palladium, a nickel alloy, platinum, or other metal. The solid material is loaded with gas by exposing the solid material to the gas under high pressure. When the solid material is exposed to gas under pressure, the gas absorbs into or adsorbs onto the solid material. After the solid material is loaded with gas, the gas atmosphere and high pressure are maintained while the solid material is packaged in a sealed container that is capable of retaining the high pressure gas. - In the following description, an exemplary embodiment is described for loading a solid material such as palladium with hydrogen gas. Those skilled in the art will appreciate that similar procedures may be used for loading the solid material with other gases.
- The main functional components of the gas-loading and
packaging system 10 comprise agas source 12, rough/backing pump 15, turbo-molecular pump 17,sample loading chamber 20,process chamber 40, andpackaging chamber 60. Thegas source 12 connects viagas supply line 14 to thesample loading chamber 20,process chamber 40, andpackaging chamber 60.Control valves gas source 12 into thesample loading chamber 20,process chamber 40, andpackaging chamber 60 respectively. The rough/backing pump 15 connects viavacuum line 16 to thesample loading chamber 20,process chamber 40, andpackaging chamber 60.Control valves sample loading chamber 20,process chamber 40, andpackaging chamber 60 respectively from the rough/backing pump 15. The turbo-molecular pump 17 connects viavacuum line 18 to thesample loading chamber 20,process chamber 40, andpackaging chamber 60.Control valves sample loading chamber 20,process chamber 40, andpackaging chamber 60 respectively from the turbo-molecular pump 17. - The
sample loading chamber 20 is the point of entry where the solid material is initially introduced into the gas-loading andpackaging system 10. Thesample loading chamber 20 includes adoor 34 through which a solid material is placed inside thesample loading chamber 20. When closed, thedoor 34 forms a seal that is capable of holding pressure or vacuum inside thesample loading chamber 20. Apressure gauge 28 measures the gas pressure inside thesample loading chamber 20. Alinear transfer apparatus 36 is disposed inside thesample loading chamber 20 for transferring the solid material from thesample loading chamber 20 to theprocess chamber 40 as hereinafter described in greater detail. - The
sample loading chamber 20 is connected to theprocess chamber 40 by a sealedpassageway 30 including agate valve 32 for isolating the sample loading chamber from theprocess chamber 40, and vice versa. Thepassageway 30 andgate valve 32 are sized to allow the transfer of the solid material from thesample loading chamber 20 to theprocess chamber 40 while maintaining the gas atmosphere and high gas pressure. - The
process chamber 40 is where the solid material is exposed to and loaded with hydrogen gas. Apressure gauge 48 measures the gas pressure inside theprocess chamber 40. Ascale 54 inside theprocess chamber 40 continuously measures the mass of the solid material while the solid material is in the process of being loaded with hydrogen gas. As described in more detail below, the measurements of the mass of the solid material are used to determine when the solid material is loaded with a desired amount of hydrogen gas. Measurements of the mass of the solid material may be made when the solid material is initially placed in theprocess chamber 40 to determine the starting mass of the solid material and at predetermined or periodic time intervals during the loading of gas into the solid material to determine the change in mass of the solid material. The measurements may continue until the predetermined amount of gas is loaded into the solid material. - The
process chamber 40 is connected to thepackaging chamber 60 by a sealedpassageway 50 including agate valve 52 for isolating theprocess chamber 40 from thepackaging chamber 60, and vice versa. Thepassageway 50 andgate valve 52 are sized to allow the transfer of the solid material from theprocess chamber 40 to thepackaging chamber 60 while maintaining the gas atmosphere and high gas pressure. - The
packaging chamber 60 is where the solid material loaded with hydrogen gas is packaged in a sealed container. Apressure gauge 68 measures the gas pressure inside thepackaging chamber 60. Thepackaging chamber 60 includes adoor 72 through which the sealed container containing the solid material is removed from the gas loading andpackaging system 10. When closed, thedoor 34 forms a seal that is capable of holding pressure or vacuum inside thepackaging chamber 60. Alinear transfer apparatus 70 is disposed inside thepackaging chamber 60. The linear transfer apparatus is used to transfer the solid material after it is loaded with hydrogen gas from theprocess chamber 40 to thepackaging chamber 60. - The operation of the gas loading and
packaging system 10 can be broken down into five processes: an intake process, a first transfer process, a gas loading process, a second transfer process, and a packaging process. During the intake process, a sample of solid material, e.g. palladium, is placed inside thesample loading chamber 20. Thesample loading chamber 20 is evacuated to remove contaminants. Once the contaminants are removed, thesample loading chamber 20 is pressurized to about 760 Torr, which is one atmosphere. At this point, the intake process ends and the first transfer process begins, during which the solid material is transferred from thesample loading chamber 20 to theprocess chamber 40. - During the first transfer process, the pressure in the process chamber is raised to about 10 Torr to 50 Torr above the sample loading chamber pressure. The higher pressure in the
process chamber 40 relative to thesample loading chamber 20 serves to minimize the flow of any contaminants from thesample loading chamber 20 to theprocess chamber 40 during the transfer of the solid material. Thegate valve 32 isolating thesample loading chamber 20 is then opened and thelinear transfer apparatus 36 transfers the sample of solid material into theprocess chamber 40 and places the sample on thescale 54. Thelinear transfer apparatus 36 may comprise a retractable arm that picks up the solid material, extends into theprocess chamber 40 and deposits the solid material on thescale 54, and then retracts back into thesample loading chamber 20. When the transfer of the solid material is complete, thegate valve 32 is closed. At this point, the first transfer process ends and the gas loading process begins, during which the solid material is loaded with hydrogen gas. - At the start of the hydrogen loading process, both
gate valves process chamber 40. The process chamber pressure is increased to a pressure in the range of about 3800 Torr to about 7600 Torr. When the solid material is exposed to hydrogen gas under high pressure, hydrogen gas is absorbed into and adsorbed onto the solid material. The amount of hydrogen gas loaded onto the solid material, by absorption and/or adsorption, is determined by the change of mass of the solid material. The change of mass of the solid material is related to the amount of hydrogen by: -
- where L is the loading ratio of atoms of hydrogen to atoms of palladium, Δm is the change in mass of the palladium sample in grams, and P is the mass of the palladium sample in grams.
- The mass of the solid material is continuously or periodically checked during the gas loading process to determine when the solid material is loaded with a desired amount of hydrogen gas. In one embodiment, the change of mass is calculated and compared to a pre-computed mass change threshold to determine when the solid material is loaded with a desired amount of hydrogen gas. In other embodiments, the amount of hydrogen gas loaded onto the solid material is computed according to Equation 1. The gas loading process ends when the change of mass reaches the threshold, or when the calculated amount of hydrogen gas loaded onto the solid material equals the desired amount.
- Once the solid material is loaded with a desired amount of hydrogen gas, the second transfer process begins. During the second transfer process, the pressure inside the packaging chamber is raised to about 10 Torr to about 50 Torr below the process chamber pressure and the
gate valve 52 is opened. The lower pressurization of thepackaging chamber 60 relative to theprocess chamber 40 serves to minimize the flow of any contaminants from thepackaging chamber 60 to theprocess chamber 40 since thepackaging chamber 60 is opened to the atmosphere to remove the sample. Thelinear transfer apparatus 70 in thepackaging chamber 60 transfers the solid material loaded with hydrogen gas from theprocess chamber 40 into thepackaging 60. Thelinear transfer apparatus 70 may comprise a retractable arm that extends into theprocess chamber 40, picks up the solid material, and then retracts back into thepackaging chamber 60. After the solid material is transferred into thepackaging chamber 60, thegate valve 52 is closed to isolate thepackaging chamber 60. At this point the second transfer process ends and the packaging process begins. - It is assumed that a sealed container is placed inside the
packaging chamber 60 prior to the start of the packaging process. The sealed container may be introduced into thepackaging chamber 60 anytime before the start of the second transfer process. Prior to the start of the packaging process, thepackaging chamber 60 may be evacuated to remove contaminants. In one embodiment, thepackaging chamber 60 is outfitted with vacuum/high pressure mechanical arms or other accessories as needed to transfer the solid material sample into a container that is capable of maintaining the process gas at the process pressure. In another embodiment, thepackaging chamber 60 may comprise a glove box that enables a human user to handle and package the solid material. After sealing the container, thepackaging chamber 60 may be evacuated to atmospheric pressure, nominally 760 Torr (101 kPa). Thedoor 72 to thepackaging chamber 60 is then opened and the packaged solid material sample is removed. The packaging enables the solid material sample to maintain the incorporated gas, maximizing its usefulness in application and longevity. - The following is a more detailed, step-by-step description of the gas loading and packaging process.
FIGS. 2A-2J illustrate some of these steps. -
- 1. Load a solid material sample into the sample loading chamber and seal the
sample loading chamber 20. - 2.
Open valve 24 to connect thesample loading chamber 20 to rough/backing pump 15 and begin evacuation of thesample loading chamber 20 as shown inFIG. 2A . - 3. When the pressure level in
sample loading chamber 20 reaches approximately 0.1 Torr (13 Pa),close valve 24 andopen valve 26 to connect thesample loading chamber 20 to turbo-molecular pump 17 and continue evacuation of thesample loading chamber 20 as shown inFIG. 2B . - 4. When the pressure level in
sample loading chamber 20 reaches approximately 1×10−6 Torr (1×10−4 Pa),close valve 26. - 5.
Open valve 22 to connect thesample loading chamber 20 togas source 12 and fill thesample loading chamber 20 with the hydrogen gas as shown inFIG. 2C . The pressure inside thesample loading chamber 20 is measured by thepressure gauge 28. - 6. Continue adding gas until the pressure in the
sample loading chamber 20 reaches nominally 760 Torr (101 kPa), which is the working pressure of thesample loading chamber 20 reached. Shut offvalve 22 when the pressure reaches the working pressure. This step ends the intake process. - 7. Begin the first transfer process by opening
valve 42 to add process gas to theprocess chamber 40 as shown inFIG. 2D . Continue adding hydrogen gas until the pressure inside theprocess chamber 40 reaches between 10 and 50 Torr (1.3 and 6.7 kPa) greater than the sample loading chamber pressure. - 8.
Close valve 42 andopen gate valve 32 connecting thesample loading chamber 20 to theprocess chamber 40. The higher pressure level of theprocess chamber 40 relative to thesample loading chamber 20 serves to minimize the flow of any contaminants from thesample loading chamber 20 to theprocess chamber 40. - 9. Transfer the solid material sample from the
sample loading chamber 20 to theprocess chamber 40 and place the solid material sample on thescale 54 as shown inFIG. 2E . - 10.
Close gate valve 32 when the transfer of the solid material sample to theprocess chamber 40 is completed. - 11. If it is desirable or required to increase the process gas pressure for adsorption on and absorption into the solid material sample,
open valve 42 to increase the process gas pressure up to nominally 3800 Torr (507 kPa) to about 7600 Torr (1014 kPa) as shown inFIG. 2F . The sample will be loaded with hydrogen gas by absorption and adsorption. The amount of gas adsorbed and absorbed is calculated from the mass change measured by the scale after correcting for a change in chamber pressure. - 12. During the gas-loading process, periodically measure the mass of the solid material sample and calculate the mass change of the solid material sample. Continue gas-loading until a desired amount of gas is added to the solid material sample. When the mass change and/or the solid material sample is loaded with a desired amount of gas, start the second transfer process to transfer the solid material sample to the
packaging chamber 60. - 13. To start the second transfer process,
open valve 62 to supply gas to theprocess packaging chamber 60 as shown inFIG. 2G . Continue supplying gas to thepackaging chamber 60 until the gas pressure in thepackaging chamber 60, indicated bypressure gauge 68, is between 10 and 50 Torr (1.3 and 6.7 kPa) lower than theprocess chamber 40 pressure indicated bypressure gauge 48, at whichtime valve 62 is closed. The lower pressurization of thepackaging chamber 60 relative to theprocess chamber 40 serves to minimize the flow of any contaminants from thepackaging chamber 60 to theprocess chamber 40 since thepackaging chamber 60 is opened to atmosphere to remove the sample. - 14.
Open gate valve 52 and transfer the solid material sample from theprocess chamber 40 to thepackaging chamber 60 using the secondlinear transfer apparatus 70 as shown inFIG. 2H . When the transfer of the metal sample to thepackaging chamber 60 is complete,close gate valve 52 to isolate thepackaging chamber 60. This step ends the second transfer process. - 15. In some cases, it may be desirable to increase the pressure in the
packaging chamber 60 at the start of the packaging process. In this case,open valve 62 as shown inFIG. 2I to pressurize thepackaging chamber 60 to a desired pressure level above the processing pressure to maintain the loading of the solid material sample. - 16. Package solid material sample into a pressure sealed container. The
packaging chamber 60 may be outfitted with vacuum/high pressure mechanical arms or other accessories as needed to transfer the solid material sample into a container that is capable of maintaining the process gas at the process pressure. - 17. After sealing the container,
open valve 66 to evacuate thepackaging chamber 60 to atmospheric pressure, nominally 760 Torr (101 kPa) a shown inFIG. 2J . - 18. Open the
packaging chamber 60 and remove the packaged solid material sample. The packaging enables the solid material sample to maintain the incorporated gas—maximizing its usefulness in application and longevity.
- 1. Load a solid material sample into the sample loading chamber and seal the
-
FIG. 3 illustrates anexemplary control circuit 100 for controlling the operation of the gas loading andpackaging system 10. Thecontrol circuit 100 comprises aprocessing circuit 102 that implements the main control functions of the gas loading andpackaging system 10. Theprocessing circuit 102 may comprise one or more processors, hardware circuits, firmware, of a combination thereof. Theprocessing circuit 102 receives inputs from the pressure gauges 28, 48, and 68, and thescale 54 and outputs control signals to various solenoids and switches that control the valves as hereinabove described. Solenoids or switches S22, S24, S26, S42, S44, S46, S62,S64, andS66 control valves control gate valves gas source 12, rough/backing pump 15, and turbo-molecular pump 17 respectively. Theprocessing circuit 102 may also send control signals to thelinear transfer apparatus -
FIGS. 4A and 4B illustrate an exemplary method 150 of gas loading and packaging a solid material. The solid material is transferred to a process chamber 40 (block 155). Once the solid material is loaded in to theprocess chamber 40, theprocess chamber 40 is pressurized with hydrogen gas until the process chamber pressure reaches a first pressure level (block 160). The process chamber pressure is maintained above the first pressure level to load the solid material with hydrogen gas. While the solid material is being loaded with hydrogen gas, the mass of the solid material is measured and the measurements are used to determine when the solid material is loaded with a predetermined amount of hydrogen gas based (blocks 165 and 170). When the desired amount of hydrogen gas is loaded into the solid material, pressurize thepackaging chamber 60 with hydrogen gas until the packaging chamber pressure reaches a second pressure level lower than the first predetermined pressure level and transfer the solid material from the process chamber to the packaging chamber (blocks 175 and 180) The solid material is then packaged in a sealed container while maintaining the packaging chamber pressure at or above second pressure level, after which the sample chamber is opened and the sealed container is removed from the packaging chamber 60 (blocks 190 and 195). In some embodiments, the packaging chamber pressure may be raised to a third pressure level higher than the first pressure level while the solid material is packaged (block 185).
Claims (17)
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US15/891,416 US20180194625A1 (en) | 2016-06-06 | 2018-02-08 | Gas-Loading and Packaging Method and Apparatus |
US16/178,649 US20190077657A1 (en) | 2016-06-06 | 2018-11-02 | Gas-Loading and Packaging Method and Apparatus |
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US201662346238P | 2016-06-06 | 2016-06-06 | |
US15/615,137 US10053362B2 (en) | 2016-06-06 | 2017-06-06 | Gas-loading and packaging method and apparatus |
US15/891,416 US20180194625A1 (en) | 2016-06-06 | 2018-02-08 | Gas-Loading and Packaging Method and Apparatus |
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US5384147A (en) * | 1991-08-16 | 1995-01-24 | Int Equipment Sales, Inc. | Method of processing avocado pulp |
US20090090022A1 (en) * | 2007-10-09 | 2009-04-09 | Hememics Biotechnologies, Inc. | Desiccation Chamber and Methods for Drying Biological Materials |
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US5384147A (en) * | 1991-08-16 | 1995-01-24 | Int Equipment Sales, Inc. | Method of processing avocado pulp |
US20090090022A1 (en) * | 2007-10-09 | 2009-04-09 | Hememics Biotechnologies, Inc. | Desiccation Chamber and Methods for Drying Biological Materials |
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