Patents by Inventor Ilias Belharouak

Ilias Belharouak has filed for patents to protect the following inventions. This listing includes patent applications that are pending as well as patents that have already been granted by the United States Patent and Trademark Office (USPTO).

  • Patent number: 12187610
    Abstract: A positive electrode for a sodium ion battery is provided. The positive electrode includes a sodium metal vanadium fluorophosphate having a formula according to Formula I: Na3V2-xMxOy(PO4)2F3-y??I; wherein 0<x?1, 0?y?1, and M is one or more additional metals.
    Type: Grant
    Filed: June 15, 2021
    Date of Patent: January 7, 2025
    Assignee: UT-BATTELLE, LLC
    Inventors: Ilias Belharouak, Ruhul Amin, Rachid Essehli
  • Publication number: 20250002371
    Abstract: A method of forming a cathode material precursor is provided. The method is an ethanol-assisted, hydrothermal synthesis and includes dissolving a nickel nitrate hydrate in ethanol to obtain a first mixture. The first mixture is then heated at a first temperature for a first period of time. Subsequently, the first mixture is cooled, filtered, washed, and dried to obtain a nickel hydroxide hydrate precipitate that is the cathode material precursor. In the method, the first mixture is free of ammonia. The cathode material precursor obtained may be ?-3Ni(OH)2·2H2O. A method of forming a cobalt-free, nickel-rich cathode material from the cathode material precursor is also provided. The resulting cathode material may be LiNi0.9Mn0.05Al0.05 O2 (NMA9055).
    Type: Application
    Filed: June 27, 2024
    Publication date: January 2, 2025
    Inventors: Ilias Belharouak, Marm B. Dixit, Rachid Essehli, Nitin Muralidharan
  • Publication number: 20240396110
    Abstract: A method for recycling lithium-ion battery materials is provided. The method includes the step of isolating and recovering a composite electrode. The composite electrode includes an electrode material adhered to a current collector. The composite electrode is combined with a dual function solution comprising an organic acid compound and polyol to form a leaching mixture. The electrode material is leached and separated from the current collector and binder/carbon black film to give a metal ion containing leachate, a free current collector and free binder/carbon black. The metal ion containing leachate, the free current collector, and the binder/carbon black are recovered from the leaching mixture. Upon heating the metal leachate, the dual function solution works as precipitation agent and gives a coprecipitated cathode precursor and a metal ion leachate. The coprecipitated cathode precursor may be used for cathode resynthesis.
    Type: Application
    Filed: May 24, 2024
    Publication date: November 28, 2024
    Inventors: Ilias Belharouak, Lu Yu, Yaocai Bai, Rachid Essehli
  • Publication number: 20240339630
    Abstract: A method of making an anti-perovskite solid electrolyte is provided. The method includes: providing an anti-perovskite material that is in the form of a powder; heating a die to a temperature between approximately 200 and 400° C.; loading the anti-perovskite powder into the heated die; compressing the anti-perovskite powder in the heated die; and allowing the heated die to cool to ambient temperature under pressure by maintaining the compression until the die has cooled to ambient temperature. The compression may be performed uniaxially and at a pressure in a range of 1 to 500 MPa. The anti-perovskite may undergo phase transformation, densification, and grain growth during compression at the elevated temperature. An anti-perovskite solid electrolyte formed by the method, and an anti-perovskite solid-state battery including the solid electrolyte are also provided.
    Type: Application
    Filed: April 5, 2024
    Publication date: October 10, 2024
    Inventors: Marm Dixit, Ruhul Amin, Rachid Essehli, Ilias Belharouak, Mahalingam Balasubramanian, Nitin Muralidharan
  • Patent number: 12068472
    Abstract: A method for the regeneration of cathode material from spent lithium-ion batteries is provided. The method includes dissolving a lithium precursor in a polyhydric alcohol to form a solution. Degraded cathode material containing lithium metal oxides are dispersed into the solution under mechanical stirring, forming a mixture. The mixture is heat treated within a reactor vessel or microwave oven. During this heat treatment, lithium is intercalated into the degraded cathode material. The relithiated electrode material is collected by filtration, washing with solvents, and drying. The relithiated electrode material is then ground with a lithium precursor and thermally treated at a relatively low temperature for a predetermined time period to obtain regenerated cathode material.
    Type: Grant
    Filed: June 30, 2021
    Date of Patent: August 20, 2024
    Assignee: UT-BATTELLE, LLC
    Inventors: Ilias Belharouak, Yaocai Bai, Rachid Essehli, Jianlin Li
  • Patent number: 12027664
    Abstract: A super ion conductor composition is disclosed. The super ion conductor composition has the general formula: A1+xMx/2Zr2?x/2(PO4)3, where each A is independently Na or Li, M is Mn or Mg, and subscript x is from 0.5 to 3. A solid electrolyte comprising the super ion conductor composition, and a method of preparing the solid electrolyte, are also disclosed. The method comprises combining a zirconium compound, a manganese or magnesium compound, a sodium compound, and a phosphate compound to give a mixture; and calcining the mixture to give the super ion conductor composition, thereby preparing the solid electrolyte. Functional materials and devices comprising the super ion conductor composition are also disclosed, including a catholyte composition, an ion conducting solid electrolyte membrane, as well as all-solid-state batteries.
    Type: Grant
    Filed: May 20, 2021
    Date of Patent: July 2, 2024
    Assignee: UT-BATTELLE, LLC
    Inventors: Ruhul Amin, Rachid Essehli, Ilias Belharouak
  • Patent number: 11996557
    Abstract: A method for relithiating cathode material from spent lithium-based batteries, the method comprising: (i) mixing delithiated cathode material and a lithium salt with an ionic liquid in which the lithium salt is at least partially soluble to form an initial mixture; (ii) heating the initial mixture to a temperature of 100° C. to 300° C. to result in relithiation of the delithiated cathode material; and (iii) separating the ionic liquid from the relithiated cathode material; wherein, in embodiments, the cathode material is a lithium metal oxide, wherein the metal is selected from the group consisting of Ni, Co, Fe, Mn, Al, Zr, Ti, Nb, and combinations thereof, or wherein the cathode material has the formula LiNixMnyCozO2, wherein x>0, y>0, z>0, and x+y+z=1; wherein, in some embodiments, the ionic liquid has a nitrogen-containing cationic portion, such as an imidazolium ionic liquid.
    Type: Grant
    Filed: May 4, 2022
    Date of Patent: May 28, 2024
    Assignee: UT-Battelle, LLC
    Inventors: Huimin Luo, Sheng Dai, Tao Wang, Ilias Belharouak, Jianlin Li, Yaocai Bai
  • Patent number: 11916206
    Abstract: A method of recycling lithium-ion batteries is disclosed. The method includes isolating a composite electrode that comprises an electrode material adhered to a current collector with a polyvinylidene difluoride (PVDF) binder from a spent lithium-ion battery. The method also includes contacting the composite electrode in a polyol fluid capable of releasing the PVDF binder from the current collector without substantially altering either component. The composite electrode may be a cathode or an anode. The method also includes rapidly delaminating the electrode material from the current collector to give a free electrode material and a free current collector, and recovering each of the free electrode material and the free current collector from the mixture. The free electrode material may be reused to prepare another composite electrode, as well as a lithium-ion battery comprising the same, which are also disclosed.
    Type: Grant
    Filed: February 16, 2021
    Date of Patent: February 27, 2024
    Assignee: UT-BATTELLE, LLC
    Inventors: Ilias Belharouak, Yaocai Bai, Jianlin Li, Rachid Essehli
  • Publication number: 20230361266
    Abstract: A method of improving interfacial contact at an electrode-to-solid-electrolyte interface in a solid-state battery cell is provided. The method includes providing a solid-state battery cell including a solid-state electrolyte and electrodes defining an anode and a cathode. Each of the anode and cathode are adjacent to the solid-state electrolyte at an interface. The method further includes electrochemically increasing interfacial contact between at least one of the electrodes and the solid-state electrolyte by applying a voltage pulse to the cell at a high current density for a short duration, wherein electrode material diffuses into pores formed in the solid electrolyte interface, thereby healing the pores and eliminating an interfacial space charge effect.
    Type: Application
    Filed: May 2, 2023
    Publication date: November 9, 2023
    Inventors: Anand Vasudevbhai Parejiya, Ruhul Amin, Marm Dixit, Rachid Essehli, Ilias Belharouak
  • Patent number: 11721850
    Abstract: An improved method of recycling lithium-ion battery anode scraps is provided. The method involves isolating an anode scrap including a graphite anode film adhered to a current collector foil with a polyvinylidene fluoride binder. The anode scrap is combined with deionized water to form a first mixture. The graphite anode film is delaminated from the current collector foil to form a second mixture comprising a free collector foil and a free graphite anode film. The free graphite anode film is filtered and dried from the second mixture to recover the free graphite anode film. The free graphite anode film is combined with a solvent comprising N-methyl-2-pyrrolidone (NMP) to form an anode formation slurry. The slurry is coated onto a copper current collector to produce a new anode.
    Type: Grant
    Filed: July 28, 2021
    Date of Patent: August 8, 2023
    Assignee: UT-BATTELLE, LLC
    Inventors: Yaocai Bai, Ilias Belharouak, Rachid Essehli
  • Patent number: 11664542
    Abstract: A method for recycling lithium-ion battery materials is provided. The method includes isolating a composite electrode comprising an electrode material adhered to a current collector with a polyvinylidene difluoride (PVDF) binder. The composite electrode is combined with triethyl phosphate (TEP) as a solvent to form a mixture. The electrode material is delaminated from the current collector in the mixture to give a free electrode material and a free current collector. Each of the free electrode material and the free current collector is recovered from the mixture. The free electrode material may be reused to prepare another composite electrode, as well as a lithium-ion battery comprising the same, which are also disclosed.
    Type: Grant
    Filed: December 15, 2021
    Date of Patent: May 30, 2023
    Assignee: UT-BATTELLE, LLC
    Inventors: Ilias Belharouak, Yaocai Bai, Rachid Essehli
  • Publication number: 20230108561
    Abstract: A method of reviving a lithium-ion battery cell in which dendrites are formed providing a lithium-ion battery cell including a lithium-metal-containing electrolyte and one of a graphite or a lithium-metal-containing anode. Lithium dendrites are formed at an anode/electrolyte interface in the cell and extend into the electrolyte of the cell. The method further includes electrochemically healing the battery cell by actively applying a plurality of continuous low current density galvanostatic charge-discharge cycles to the battery cell. Lithium metal is thusly oxidized from tips of the dendrites thereby causing dissolution of the dendrites.
    Type: Application
    Filed: September 28, 2022
    Publication date: April 6, 2023
    Inventors: Ruhul Amin, Ilias Belharouak, Anand Vasudevbhai Parejiya
  • Publication number: 20230033430
    Abstract: An improved method of recycling lithium-ion battery anode scraps is provided. The method involves isolating an anode scrap including a graphite anode film adhered to a current collector foil with a polyvinylidene fluoride binder. The anode scrap is combined with deionized water to form a first mixture. The graphite anode film is delaminated from the current collector foil to form a second mixture comprising a free collector foil and a free graphite anode film. The free graphite anode film is filtered and dried from the second mixture to recover the free graphite anode film. The free graphite anode film is combined with a solvent comprising N-methyl-2-pyrrolidone (NMP) to form an anode formation slurry. The slurry is coated onto a copper current collector to produce a new anode.
    Type: Application
    Filed: July 28, 2021
    Publication date: February 2, 2023
    Inventors: Yaocai Bai, Ilias Belharouak, Rachid Essehli
  • Publication number: 20220376240
    Abstract: A method for relithiating cathode material from spent lithium-based batteries, the method comprising: (i) mixing delithiated cathode material and a lithium salt with an ionic liquid in which the lithium salt is at least partially soluble to form an initial mixture; (ii) heating the initial mixture to a temperature of 100° C. to 300° C. to result in relithiation of the delithiated cathode material; and (iii) separating the ionic liquid from the relithiated cathode material; wherein, in embodiments, the cathode material is a lithium metal oxide, wherein the metal is selected from the group consisting of Ni, Co, Fe, Mn, Al, Zr, Ti, Nb, and combinations thereof, or wherein the cathode material has the formula LiNixMnyCozO2, wherein x>0, y>0, z>0, and x+y+z=1; wherein, in some embodiments, the ionic liquid has a nitrogen-containing cationic portion, such as an imidazolium ionic liquid.
    Type: Application
    Filed: May 4, 2022
    Publication date: November 24, 2022
    Inventors: Huimin Luo, Sheng Dai, Tao Wang, Ilias Belharouak, Jianlin Li, Yaocai Bai
  • Patent number: 11508962
    Abstract: A cathode active material precursor for a lithium metal oxide is provided. The cathode active material precursor comprises a metal-containing oxyhydroxide. The metal-containing oxyhydroxide comprises nickel and an additional metal. At least 50 mol. % of the nickel of the metal-containing oxyhydroxide has an oxidation state of +3. A method of forming a cathode active material precursor is also provided. The method comprises combining a nickel-containing compound, an additional metal-containing compound, an oxidizing agent, and a solvent to form a solution. The method further comprises exposing the solution to heat at a temperature of from about 30° C. to about 90° C. to form a precipitate comprising the metal-containing oxyhydroxide.
    Type: Grant
    Filed: February 4, 2020
    Date of Patent: November 22, 2022
    Assignee: UT-BATTELLE, LLC
    Inventors: Ilias Belharouak, Nitin Muralidharan
  • Publication number: 20220344737
    Abstract: A method of recycling lithium-ion battery materials is provided. The method includes isolating a composite electrode that includes an electrode material adhered to a current collector. The composite electrode is combined with an aqueous buffer solution to form a mixture. The electrode material is delaminated from the current collector in the mixture to give a free electrode material and a free current collector. Each of the free electrode material and the free current collector is recovered from the mixture. Combining the composite electrode with the aqueous buffer solution occurs before delaminating the electrode material from the current collector. The step of delaminating optionally may include adding a surfactant to the mixture.
    Type: Application
    Filed: March 29, 2022
    Publication date: October 27, 2022
    Inventors: Ilias Belharouak, Yaocai Bai
  • Publication number: 20220328800
    Abstract: A method for the regeneration of cathode material from spent lithium-ion batteries is provided. The method includes dissolving a lithium precursor in a polyhydric alcohol to form a solution. Degraded cathode material containing lithium metal oxides are dispersed into the solution under mechanical stirring, forming a mixture. The mixture is heat treated within a reactor vessel or microwave oven. During this heat treatment, lithium is intercalated into the degraded cathode material. The relithiated electrode material is collected by filtration, washing with solvents, and drying. The relithiated electrode material is then ground with a lithium precursor and thermally treated at a relatively low temperature for a predetermined time period to obtain regenerated cathode material.
    Type: Application
    Filed: June 30, 2021
    Publication date: October 13, 2022
    Inventors: Ilias Belharouak, Yaocai Bai, Rachid Essehli, Jianlin Li
  • Patent number: 11394020
    Abstract: A cathode for a lithium battery includes LiNi0.5-x/2Mn0.5-x/2MxO2 where M is at least one selected from the group consisting of Mo, Ti, Cr, Zr and V, and x is between 0.005-0.02. The LiNi0.5-x/2Mn0.5-x/2MxO2 can be coated with Mn2P2O7. The Mn2P2O7 can be 1-3 wt. %, based on the total weight of the LiNi0.5-x/2Mn0.5-x/2MxO2 and Mn2P2O7. A cathode composition, a lithium battery, and a method of making a lithium battery are also disclosed.
    Type: Grant
    Filed: June 21, 2019
    Date of Patent: July 19, 2022
    Assignee: UT-BATTELLE, LLC
    Inventors: Jagjit Nanda, Ilias Belharouak, Ethan C. Self, Devendrasinh Udaisinh Darbar
  • Publication number: 20220200074
    Abstract: A method for recycling lithium-ion battery materials is provided. The method includes isolating a composite electrode comprising an electrode material adhered to a current collector with a polyvinylidene difluoride (PVDF) binder. The composite electrode is combined with triethyl phosphate (TEP) as a solvent to form a mixture. The electrode material is delaminated from the current collector in the mixture to give a free electrode material and a free current collector. Each of the free electrode material and the free current collector is recovered from the mixture. The free electrode material may be reused to prepare another composite electrode, as well as a lithium-ion battery comprising the same, which are also disclosed.
    Type: Application
    Filed: December 15, 2021
    Publication date: June 23, 2022
    Inventors: Ilias Belharouak, Yaocai Bai, Rachid Essehli
  • Publication number: 20220200073
    Abstract: A method for recycling lithium-ion battery materials is provided. The method includes isolating a composite electrode that includes an electrode material adhered to a current collector. The isolated composite electrode is combined with a citrate-based solvent to form a mixture. The electrode material is delaminated from the current collector in the mixture to give a free electrode material and a free current collector. Each of the free electrode material and the free current collector is recovered from the mixture. The free electrode material may be reused to prepare another composite electrode, as well as a lithium-ion battery comprising the same, which are also disclosed.
    Type: Application
    Filed: December 15, 2021
    Publication date: June 23, 2022
    Inventors: Ilias Belharouak, Yaocai Bai, Rachid Essehli