Classifications

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  • C01G45/1221—Manganates or manganites with trivalent manganese, tetravalent manganese or mixtures thereof
  • C01G45/1228—Manganates or manganites with trivalent manganese, tetravalent manganese or mixtures thereof of the type (MnO2)-, e.g. LiMnO2 or Li(MxMn1-x)O2
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  • H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
  • H01M10/0562—Solid materials
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  • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
  • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
  • H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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  • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
  • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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  • H01M4/06—Electrodes for primary cells
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  • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
  • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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  • H01M4/36—Selection of substances as active materials, active masses, active liquids
  • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
  • H01M4/381—Alkaline or alkaline earth metals elements
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  • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
  • H01M4/381—Alkaline or alkaline earth metals elements
  • H01M4/382—Lithium
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  • H01M4/36—Selection of substances as active materials, active masses, active liquids
  • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
  • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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  • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
  • H01M4/621—Binders
  • H01M4/622—Binders being polymers
  • H01M4/623—Binders being polymers fluorinated polymers
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  • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
  • H01M4/624—Electric conductive fillers
  • H01M4/625—Carbon or graphite
• • C—CHEMISTRY; METALLURGY
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  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2002/00—Crystal-structural characteristics
  • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
  • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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  • H01M2004/027—Negative electrodes
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  • H01M2004/028—Positive electrodes
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  • H01M2300/00—Electrolytes
  • H01M2300/0017—Non-aqueous electrolytes
  • H01M2300/0065—Solid electrolytes
  • H01M2300/0068—Solid electrolytes inorganic
  • H01M2300/0071—Oxides
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  • H01M2300/0082—Organic polymers
• • 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
  • Y02E60/10—Energy storage using batteries

Definitions

• ELECTRODE MATERIALS COMPRISING SODIUM, LITHIUM, MANGANESE AND FE-DOPED TUNNEL-TYPE METAL OXIDE, ELECTRODES COMPRISING THEM AND THEIR USE IN ELECTROCHEMISTRY
• the present application generally relates to the field of electrochemically active materials and their uses in electrochemical applications. More particularly, the present application relates to electrode materials comprising an oxide of sodium, magnesium and at least one tunnel type metal partially substituted with lithium as electrochemically active material, the electrodes comprising them, their methods of manufacturing and their use in electrochemical cells.
• the weighted average price of cobalt could limit future applications of BLIs and so-called all-solid-state batteries.
• Positive electrode materials containing reduced amounts of cobalt and cobalt-free positive electrode materials therefore attract much attention, especially in large-scale and high energy density energy storage systems.
• lithium iron phosphate (LiFePCO 4 or LFP) has attracted great interest due to the cost-effectiveness of its materials.
• the energy density of LFP batteries has not improved enough to meet the demands of the electric vehicle market.
• new electrode materials which exclude one or more of the disadvantages of conventional commercial positive electrode materials.
• M is chosen from manganese (Mn), titanium (Ti), vanadium (V), nickel (Ni), cobalt (Co), chromium (Cr), molybdenum (Mo), zirconium (Zr), ruthenium (Ru), other similar metals and a combination of two or more of these.
• M is titanium (Ti).
• a is a number such that 0.01 ⁇ a ⁇ 0.22, or 0.02 ⁇ a ⁇ 0.22, or 0.03 ⁇ a ⁇ 0.22, or 0.04 ⁇ a ⁇ 0.22, or 0.05 ⁇ a ⁇ 0.22, or 0.06 ⁇ a ⁇ 0.22, or 0.07 ⁇ a ⁇ 0.22, or 0.08
• a is a number such that 0.08 ⁇ a ⁇ 0.21.
• b is a number such that 0.19 ⁇ b ⁇ 0.40, or 0.20 ⁇ b ⁇ 0.40, or 0.20 ⁇ b
• b is a number such that 0.20 ⁇ b ⁇ 0.38.
• c is a number such that 0.05 ⁇ c ⁇ 0.40, or 0.10 ⁇ c ⁇ 0.40, or 0.15 ⁇ c
• c is a number such that 0.30 ⁇ c ⁇ 0.40.
• d is a number such that 0.44 ⁇ d ⁇ 1, or 0.44 ⁇ d ⁇ 0.95, or 0.44 ⁇ d ⁇ 0.90, or 0.44 ⁇ d ⁇ 0, 85, or 0.44 ⁇ d ⁇ 0.80, or 0.44 ⁇ d ⁇ 0.75, or 0.44 ⁇ d ⁇ 0.70, or 0.44 ⁇ d ⁇ 0.65, or 0.44 ⁇ d ⁇ 0.60, or 0.44 ⁇ d ⁇ 0.55.
• d is a number such that 0.44 ⁇ d ⁇ 0.55.
• the oxide of sodium, manganese and at least one metal tunnel type element doped with iron and substituted with lithium is chosen from the group consisting of Na 0 , 10 Li o, 33 Fe o, 34 Mn o,44 Ti o,22 0 2 , Na 0.08 Li 0.38 Fe 0.30 Mn 0.55 Ti 0.15 O 2 , Na 0.20 Li 0.24 Fe 0.34 Mn 0.55 Ti 0.11 O 2 , Na 0.21 Li 0.20 Fe 0.40 Mn 0.50 Ti 0.10 0 2 , Na 0.10 Li 0.40 Fe 0.08 Mn 0, 81 Ti0.nO 2 and Na 0.10 Li 0.40 Fe0.11Mn 0.78 Ti 0.11 0 2 .
• the present technology relates to an electrode material comprising the electrochemically active material as defined herein.
• said electrode material further comprises an electronic conductive material.
• the electronic conductor material is chosen from the group consisting of carbon black, acetylene black, graphite, graphene, carbon fibers, carbon nanofibers, carbon nanotubes and a combination of at least two of these.
• the electronic conductor material comprises carbon black.
• carbon black is Super P TM carbon or Ketjen TM carbon.
• the electronic conductor material comprises carbon fibers.
• carbon fibers are gas-formed carbon fibers (VGCFs).
• said electrode material further comprises a binder.
• the binder is chosen from the group consisting of a polymer binder of the polyether type, a fluoropolymer and a water-soluble binder.
• the binder is a fluoropolymer.
• the fluoropolymer is polyvinylidene fluoride (PVDF).
• said electrode material further comprises an additive.
• the additive is chosen from the group consisting of ionic conductors, inorganic particles, glass particles, ceramic particles, salts, and other similar additives.
• the present technology relates to an electrode comprising the electrode material as defined herein on a current collector.
• the electrode is a positive electrode.
• the present technology relates to an electrochemical cell comprising a negative electrode, a positive electrode and an electrolyte, in which the positive electrode is as defined here.
• the negative electrode comprises an alkali metal, an alloy comprising an alkali metal or a prelithiated electrochemically active material.
• the negative electrode comprises metallic lithium or an alloy comprising metallic lithium.
• the negative electrode comprises metallic lithium.
• the electrolyte is a glass or ceramic electrolyte.
• the electrolyte is a liquid electrolyte comprising a salt in a solvent.
• the electrolyte is a gel electrolyte comprising a salt in a solvent and optionally a solvating polymer.
• the electrolyte is a solid polymer electrolyte comprising a salt in a solvating polymer.
• the salt is a lithium salt.
• the lithium salt is chosen from the group consisting of lithium hexafluorophosphate (LiPFe), lithium bis(trifluoromethanesulfonyl)imide (LiTFSI), lithium bis(fluorosulfonyl)imide (LiFSI), 2- lithium trifluoromethyl-4,5-dicyanoimidazolate (LiTDI), lithium 4,5-dicyano-1,2,3-triazolate (LiDCTA), lithium bis(pentafluoroethylsulfonyl)imide (LiBETI), lithium tetrafluoroborate ( LiBF 4 ), lithium bis(oxalato) borate (LiBOB), lithium nitrate (UNO3), lithium chloride (LiCI), lithium bromide (LiBr), lithium fluoride (LiF), perchlorate lithium (LiCIO 4 ), lithium hexafluoroarsenate (LiPFe),
• the present technology relates to a battery comprising at least one electrochemical cell as defined here.
• said battery is chosen from the group consisting of a lithium battery, a lithium-ion battery, a sodium battery, a sodium-ion battery, a potassium battery , a potassium-ion battery, a magnesium battery and a magnesium-ion battery.
• said battery is a lithium battery or a lithium-ion battery.
• Figure 1 is an X-ray diffraction pattern for a tunnel-type sodium, lithium and manganese oxide powder of formula Na 0.08 Li 0.36 Mn0 2 , as described in Example 1 ( d).
• Figure 2 is an X-ray diffraction pattern for a tunnel-type sodium lithium iron manganese titanium oxide powder of formula
• Figure 3 is an X-ray diffraction pattern for a tunnel-type sodium lithium iron manganese titanium oxide powder of formula
• Figure 4 is an X-ray diffraction pattern for a tunnel-type sodium, lithium, iron, manganese, and titanium oxide powder of formula
• Figure 5 is an X-ray diffraction pattern for a tunnel-type sodium lithium iron manganese titanium oxide powder of formula
• Figure 6 presents charge and discharge profiles obtained for Cell 1 and recorded in (1) at a cycling speed of 0.1 C between 2.0 V and 4.8 V vs Li + /Li, and in (2) between 2.0 V and 4.6 V vs Li + /Li, as described in Example 2(b). The results are presented for the second cycle of discharge and charge.
• Figure 7 shows a charge and discharge profile obtained for Cell 2 and recorded at a cycling rate of 0.1 C between 2.0 V and 4.6 V vs Li + /Li, as described in Example 2(b). The results are presented for the second cycle of discharge and charge.
• Figure 8 shows a charge and discharge profile obtained for Cell 3 and recorded at a cycling rate of 0.1 C between 2.0 V and 4.6 V vs Li + /Li, as described in Example 2(b). The results are presented for the second cycle of discharge and charge.
• Figure 9 shows charge and discharge profiles obtained for Cell 4 and recorded at a cycling rate of 0.1 C between 2.0 V and 4.8 V vs Li + /Li, as described in Example 2(b). Results are shown for the second (1) and fifth (2) charge and discharge cycles.
• Figure 10 shows charge and discharge profiles obtained for Cell 5 and recorded at a cycling rate of 0.1 C between 2.5 V and 4.8 V vs Li + /Li, as described in Example 2(b). The results are presented for the second charge and discharge cycle.
• Figure 11 shows in (a) charge and discharge profiles recorded at a cycling rate of 0.1 C between 2.0 V and 4.8 V vs Li7Li; and in (b) a graph representing the capacity as a function of the number of cycles obtained for Cell 6, as described in Example 2(b).
• Figure 12 shows in (a) charge and discharge profiles recorded at a cycling speed of 0.1 C between 2.0 V and 4.8 V vs Li7Li; and in (b) a graph representing the capacity as a function of the number of cycles obtained for Cell 7, as described in Example 2(b).
• the present technology generally relates to electrochemically active materials, their manufacturing processes and their use in electrochemical cells. More particularly, the present technology relates to an electrochemically active material comprising an oxide of sodium, manganese and at least one tunnel-type metallic element doped with iron and substituted with lithium.
• the metallic element of sodium oxide, manganese and at least one tunnel type metallic element doped with iron and substituted with lithium may be a transition metal, a post-transition metal, a metalloid, an alkali metal other than lithium or sodium, an alkaline earth metal, or a combination thereof, when compatible.
• the metal may be a transition metal or a post-transition metal chosen from the group consisting of manganese (Mn), titanium (Ti), vanadium (V), nickel (Ni), cobalt ( Co), chromium (Cr), molybdenum (Mo), zirconium (Zr), tin (Sn), ruthenium (Ru) and other similar metallic elements, or a combination thereof here, when compatible.
• the metallic element (M) is a transition metal chosen from the group consisting of manganese (Mn), titanium (Ti), vanadium (V), nickel (Ni), cobalt (Co) , chromium (Cr), molybdenum (Mo), zirconium (Zr), ruthenium (Ru) and other similar transition metals, or a combination thereof, when compatible.
• the metallic element is titanium (Ti).
• a is a number such that 0.01 ⁇ a ⁇ 0.22, or 0.02 ⁇ a ⁇ 0.22, or 0.03 ⁇ a ⁇ 0.22, or 0.04 ⁇ a ⁇ 0 .22, or 0.05 ⁇ a ⁇ 0.22, or 0.06 ⁇ a ⁇ 0.22, or 0.07 ⁇ a ⁇ 0.22, or 0.08
• a is a number such that 0.08 ⁇ a ⁇ 0.21.
• b is a number such that a + b is 0.38 ⁇ a + b ⁇ 0.61, or 0.38 ⁇ a + b
• b is a number such that a + b is 0.40 ⁇ a + b ⁇ 0.47.
• b can be a number such as 0.19 ⁇ b ⁇ 0.40, or 0.20 ⁇ b ⁇ 0.40, or 0.20 ⁇ b ⁇ 0.39, or 0.20 ⁇ b ⁇ 0 .38.
• b is a number such that 0.20 ⁇ b ⁇ 0.38.
• c is a number such as 0.05 ⁇ c ⁇ 0.40, or 0.10 ⁇ c ⁇ 0.40, or 0.15 ⁇ c ⁇ 0.40, or 0.20 ⁇ c ⁇ 0 .40, or 0.25 ⁇ c ⁇ 0.40, or 0.30 ⁇ c ⁇ 0.40. According to some examples of interest, c is a number such that 0.30 ⁇ c ⁇ 0.40.
• d is a number such that 0.44 ⁇ d ⁇ 1, or 0.44 ⁇ d ⁇ 0.95, or 0.44 ⁇ d ⁇ 0.90, or 0.44 ⁇ d ⁇ 0.85 , or 0.44 ⁇ d ⁇ 0.80, or 0.44 ⁇ d ⁇ 0.75, or 0.44 ⁇ d ⁇ 0.70, or 0.44 ⁇ d
• d is a number such that 0.44 ⁇ d ⁇ 0.55.
• Non-limiting examples of oxides of sodium, manganese and at least one metal tunnel element doped with iron and substituted with lithium include
• the electrochemically active material may further include at least one doping element which may be included in smaller quantities, for example, to modulate or optimize its electrochemical properties.
• the electrochemically active material can be doped by the partial substitution of the metallic element by at least one other element.
• the electrochemically active material can be lightly doped with at least one doping element chosen from a transition metal (for example, iron (Fe), cobalt (Co), nickel (Ni), manganese (Mn) , titanium (Ti), chromium (Cr), copper (Cu), vanadium (V), zinc (Zn), and/or yttrium (Y)) a post-transition metal (e.g. , Al), an alkaline earth metal (for example, Mg) and/or a metalloid (for example, Sb).
• a transition metal for example, iron (Fe), cobalt (Co), nickel (Ni), manganese (Mn) , titanium (Ti), chromium (Cr), copper (Cu), vanadium (V), zinc (Zn), and/or yttrium (Y)
• a post-transition metal e.g. , Al
• an alkaline earth metal for example, Mg
• a metalloid for example, Sb
• the electrochemically active material may be in the form of particles (e.g., microparticles or nanoparticles) which may be freshly formed and may further include a coating material.
• the coating material may be an electronically conductive material, for example, a carbon coating.
• partial substitution of sodium ions with lithium ions can significantly improve the electrochemical performance of an electrochemical cell comprising the present electrochemically active material.
• the partial substitution of sodium ions by lithium ions in sodium oxide, manganese and at least one metal tunnel type element doped with iron and substituted with lithium can substantially improve the electrochemical properties of the material electrochemically active.
• the partial substitution of sodium ions by lithium ions can stabilize the structure of the electrochemically active material based on sodium oxide, manganese and at least one iron-doped tunnel-type metallic element. and, therefore, substantially improve its electrochemical performance.
• the electrochemical properties of the electrochemically active material can be modulated by varying the degree of lithium substitution.
• the doping of sodium oxide, manganese oxide and at least one metallic tunnel type element substituted with lithium with iron ions can also substantially improve the electrochemical properties of the electrochemically active material.
• partial substitution of manganese with iron ions can significantly increase the average operating voltage of the electrochemically active material.
• the electrochemical properties of the electrochemically active material can be modulated by varying the degree of iron substitution.
• the cationic doping of sodium oxide, manganese and at least one metal element of the tunnel type doped with iron and substituted with lithium by a transition metal or a post-transition metal such as those described above can also substantially improve the electrochemical properties of the electrochemically active material.
• partial substitution of manganese by titanium can substantially improve the electrochemical properties of the electrochemically active material.
• the electrochemical properties of the electrochemically active material can be modulated by varying the composition of said transition metal or said posttransition metal in sodium, manganese oxide and at least one iron-doped tunnel-type metal element. and substituted with lithium.
• the present technology also relates to a process for manufacturing the electrochemically active material as defined here, the process including the following steps:
• a is a number such that 0.38 ⁇ a ⁇ 0.62
• c is a number such that 0 ⁇ c ⁇ 0.40
• the metallic element (M) is a transition metal chosen from the group consisting of manganese (Mn), titanium (Ti), vanadium (V), nickel (Ni), cobalt (Co) , chromium (Cr), molybdenum (Mo), zirconium (Zr), ruthenium (Ru) and other similar transition metals, or a combination thereof, when compatible.
• the metallic element is titanium (Ti).
• a is a number such that 0.38 ⁇ a ⁇ 0.62, or 0.38 ⁇ a ⁇ 0.60, or 0.38 ⁇ a ⁇ 0.58, or 0.38 ⁇ a ⁇ 0 .56, or 0.38 ⁇ a ⁇ 0.54, or 0.38 ⁇ a ⁇ 0.52, or 0.38 ⁇ a ⁇ 0.50, or 0.38 ⁇ a ⁇ 0.48, or 0, 38 ⁇ a ⁇ 0.46, or 0.40 ⁇ a ⁇ 0.46, or 0.41 ⁇ a ⁇ 0.46.
• a is a number such that 0.41 ⁇ a ⁇ 0.46.
• Non-limiting examples of iron-doped oxides of sodium, manganese and at least one metal tunnel element include Nao,44Feo,34Mno,44Tio,2202, Na 0.43 Fe 0.34 Mn 0.44 Ti 0, 22 O 2 , Na 0.44 Fe 0.30 Mn 0.55 Ti0.1502, Nao,46Feo.3oMno,55Tio.i502,
• the oxide of sodium, manganese and at least one tunnel-type metal element doped with iron can be prepared by a solid-state synthesis technique or by a synthesis technique in a liquid medium.
• the synthesis technique in a liquid medium can be a sol-gel process.
• the oxide of sodium, manganese and at least one iron-doped metal tunnel element can be prepared via a solid-state synthesis process.
• the solid-state synthesis process may involve mixing and grinding appropriate precursors (metal oxides or metal carbonates) in selected quantities to obtain an oxide of sodium, manganese and at least one element.
• metal tunnel type doped with iron having a desired stoichiometry can be carried out sequentially, simultaneously or partially overlapping in time. According to certain examples, the mixing and grinding steps are carried out simultaneously. All compatible mixing and grinding methods are possible.
• solid precursors can be mixed and ground manually or by any compatible mechanical method, such as mechanical grinding.
• the solid-state synthesis process may also involve heating the mixed and ground precursors to obtain the desired iron-doped tunnel element of sodium, manganese, and at least one metallic element.
• the heating step can be carried out at a temperature and for a duration sufficient to obtain the powder of sodium oxide, manganese and at least one tunnel-type metallic element doped with iron.
• the heating step may be carried out, for example, in an oven at a temperature between about 800°C and about 1000°C, limits inclusive.
• the heating step can be carried out, for example, for a period ranging from approximately 3 hours to approximately 24 hours, upper and lower limits included.
• the heating step can be carried out under any suitable conditions in order to obtain the desired powder of sodium oxide, manganese and at least one metal tunnel type element doped with iron.
• the heating step can be carried out under an atmosphere of air or oxygen, but any other compatible atmosphere is considered.
• the oxide of sodium, manganese and at least one tunnel-type metal element doped with iron can be prepared via a chemical synthesis process in a liquid medium, such as a sol-gel process.
• the sol-gel process can be carried out in an aqueous medium using inorganic salt precursors and a chelating agent.
• the inorganic salt precursors may be metal carbonate, acetate, oxalate or alkoxide precursors and the chelating agent may be an organic acid such as citric acid.
• the sol-gel process may consist of dissolving an appropriate quantity of inorganic salt precursors in water and in a (Na + Mn): chelating agent with a molar ratio of approximately 10.
• the step of dissolution can be carried out with stirring.
• the solution thus obtained can then be heated with stirring to a temperature and for a duration sufficient to form the sol-gel precursors.
• the solution can then be heated to a temperature of approximately 80°C until the sol-gel precursors are formed.
• the sol-gel precursors thus obtained can then be calcined at a temperature and for a time sufficient to decompose the organic and inorganic contents.
• the sol-gel precursors can then be calcined in an oven at a temperature of around 400°C for around 6 hours.
• the powders thus obtained can then be crushed and calcined at a sufficient temperature and for a sufficient time to obtain the desired powder of sodium oxide, manganese and at least one tunnel-type metal element doped with iron.
• the calcination step can be carried out in an oven at a temperature of around 900°C for around 9 hours.
• the calcination step can be carried out under any suitable conditions in order to obtain the desired powder of sodium oxide, manganese and at least one tunnel-type metal element doped with iron.
• the calcination step can be carried out under an atmosphere of air or oxygen, but any other compatible atmosphere is considered.
• partial substitution of sodium ions with lithium ions can be accomplished via a one- or two-step ion exchange process.
• the ion exchange reaction can be carried out by mixing the powder of sodium oxide, manganese and at least one iron-doped tunnel-type metal element prepared in step (i) with an excess amount a lithium salt or a lithium salt composition.
• the composition of lithium salt may be a mixture of lithium nitrate (UNO3) and lithium chloride (LiCI) or lithium hydroxide (LiOH), for example in a UNO3: LiCI or LiOH molar ratio of approximately 2:1.
• the powder prepared in step (i) may be mixed with up to a 20-fold molar excess of a lithium salt or lithium salt composition.
• the mixture can then be heated to a temperature and for a time sufficient to obtain the electrochemically active material, namely an oxide of sodium, manganese and at least one tunnel-type metallic element doped with iron and substituted with iron. lithium having a desired stoichiometry.
• the mixture may be heated to a temperature between about 240°C and about 400°C, either once for about 4 hours to about 15 hours, or twice for about 2 hours to about 10 hours.
• the present technology also relates to electrode materials comprising the electrochemically active material as defined herein or an electrochemically active material prepared by the method as defined herein.
• the electrode material as defined here may also include an electronic conductive material.
• electronic conductive materials include a carbon source such as carbon black (e.g., Ketjen TM carbon and Super P TM carbon), acetylene black (e.g., Shawinigan carbon and black Denka TM ), graphite, graphene, carbon fibers (e.g., gas-formed carbon fibers (VGCFs)), carbon nanofibers, carbon nanotubes (CNTs), and a combination of at least two of these.
• the electronic conductive material is chosen from Ketjen MC carbon, Super P MC carbon, VGCFs and a combination of at least two of these.
• the electronic conductor material is a mixture of VGCFs and carbon black.
• the electrode material as defined here may also include a binder.
• the binder can be chosen for its compatibility with the different elements of an electrochemical cell. Any known compatible binder is considered.
• the binder may be a polymer binder of the polyether type, a fluoropolymer or a water-soluble binder.
• the binder is a fluoropolymer such as polyvinylidene fluoride (PVDF) and polytetrafluoroethylene (PTFE).
• the binder is a water-soluble binder such as styrene-butadiene rubber (SBR), acrylonitrile-butadiene rubber (NBR), hydrogenated NBR (HNBR), epichlorohydrin rubber (CHR) or acrylate rubber (ACM), optionally comprising a thickening agent such as carboxymethylcellulose (CMC) or an acidic polymer such as poly(acrylic acid) (PAA), poly(methyl methacrylate) (PMMA) or a combination thereof.
• the binder is a polymer binder of the optionally crosslinked polyether type.
• the polyether type polymer binder is linear, branched and/or branched and is based on poly(ethylene oxide) (POE), poly(propylene oxide) (POP) or on a combination of the two ( or as an EO/POP copolymer), and optionally includes crosslinkable units.
• the binder is polyvinylidene fluoride (PVDF).
• the electrode material as defined here may also optionally include at least one additional additive such as ionic conductors, inorganic particles, glass or ceramic particles, nanoceramics (for example, aluminum oxide (AI2O3), titanium dioxide (TiO2), silicon dioxide (SiO2) and other similar compounds), salts (for example, lithium salts) and other similar additives.
• the additional additive may be an ionic conductor chosen from the group consisting of NASICON, LISICON, thio-LiSICON, garnets, sulfides, sulfur halides, phosphates, thio-phosphates, in crystalline form and/or amorphous, and a combination of at least two of these.
• the present technology relates to an electrode comprising the electrode material as defined herein on a current collector (for example, aluminum or copper foil).
• the electrode may also be a self-supporting electrode.
• the electrode is a positive electrode.
• the present technology relates to an electrochemical cell comprising a negative electrode, a positive electrode and an electrolyte, in which the positive electrode is as defined here.
• the negative electrode includes an electrochemically active material chosen from all known compatible electrochemically active materials.
• the electrochemically active material of the negative electrode can be chosen for its electrochemical compatibility with the different elements of the electrochemical cell as defined here.
• Non-limiting examples of electrochemically active negative electrode materials include alkali metals, alkali metal alloys, and prelithiated electrochemically active materials.
• the material electrochemically active of the negative electrode may be a metallic lithium film or an alloy including metallic lithium.
• the electrolyte can be chosen for its compatibility with the different elements of the electrochemical cell. Any type of compatible electrolyte is considered.
• the electrolyte may be a liquid electrolyte comprising a salt in a solvent.
• the electrolyte may also be a gel electrolyte comprising a salt in a solvent and optionally a solvating polymer.
• the electrolyte may also be a solid polymer electrolyte comprising a salt in a solvating polymer.
• the electrolyte may also be a glass or ceramic electrolyte.
• the salt if present in the electrolyte, may be an ionic salt, such as a lithium salt.
• lithium salts include lithium hexafluorophosphate (LiPFe), lithium bis(trifluoromethanesulfonyl)imide (LiTFSI), lithium bis(fluorosulfonyl)imide (LiFSI), 2-trifluoromethyl-4,5 lithium -dicyano-imidazolate (LiTDI), lithium 4,5-dicyano-1,2,3- triazolate (LiDCTA), lithium bis (pentafluoroethylsulfonyl) imide (LiBETI), lithium tetrafluoroborate (UBF4), lithium bis(oxalato)borate (LiBOB), lithium nitrate (UNO3), lithium chloride (LiCI), lithium bromide (LiBr), lithium fluoride (LiF), lithium perchlorate (UCIO4 ), lithium
• the solvent if present in the electrolyte, is preferably a non-aqueous solvent.
• non-aqueous solvents include cyclic carbonates such as ethylene carbonate (EC), propylene carbonate (PC), butylene carbonate (BC), and vitelene carbonate (VC); acyclic carbonates such as dimethyl carbonate (DMC), diethyl carbonate (DEC), methyl ethyl carbonate (EMC) and dipropyl carbonate (DPC); lactones such as y-butyrolactone (y-BL) and y-valerolactone (y-VL); acyclic ethers such as 1,2-dimethoxyethane (DME), 1,2-diethoxyethane (DEE), ethoxy methoxy ethane (EME), trimethoxymethane, tetraethylene glycol dimethyl ether or tetraglyme (TEGDME) and ethylmonoglyme; cyclic carbonates such as
• the non-aqueous solvent is a mixture of at least two carbonates, for example, a mixture of ethylene carbonate and methyl ethyl carbonate (EC/EMC).
• the electrolyte is a liquid electrolyte and comprises LiPFe in an EC/EMC mixture ([3:7] by volume) with 5% fluoroethylene carbonate (FEC).
• the electrolyte is a liquid electrolyte
• the electrode material comprises an electrochemically active material as defined herein or an electrochemically active material prepared by the process as defined herein, PVDF as a binder and an electronic conductive material chosen from the group consisting of Ketjen MC carbon, Super P MC carbon and VGCFs.
• the electrolyte is a gel electrolyte or a gel polymer electrolyte.
• the gel polymer electrolyte may comprise, for example, a polymer precursor, a salt (for example, a salt as defined above), a solvent (for example, a solvent as defined above) and a polymerization initiator and /or crosslinking, if necessary.
• examples of gel electrolytes include, without limitation, gel electrolytes such as those described in PCT patent applications published under numbers W02009/111860 (Zaghib et al.) and W02004/068610 (Zaghib et al.).
• a liquid electrolyte or a gel electrolyte as defined above can also impregnate a separator.
• separators include, but are not limited to, separators, such as Whatman TM type GF glass fiber filters.
• the electrolyte is a solid polymer electrolyte including a salt in a solvent polymer.
• the solid polymer electrolyte can be chosen from all known solid polymer electrolytes and can be chosen for its compatibility with the various elements of the electrochemical cell.
• the solid polymer electrolyte is chosen for its compatibility with lithium.
• Solid polymer electrolytes may generally include one or more solid polar polymer(s), optionally crosslinked, and a salt (for example, a salt as defined above).
• Polyether type polymers can be used, such as those based on PEO, but several other compatible polymers are also known for the preparation of solid polymer electrolytes and are also considered.
• the polymer can be crosslinked. Examples of such polymers include branched polymers, for example, star polymers or comb polymers such as those described in U.S. Patent Number 7,897,674 B2 (Zaghib et al.) (IIS'674).
• the solid polymer electrolyte may include a block copolymer composed of at least one lithium ion solvation segment and optionally at least one crosslinkable segment.
• the lithium ion solvation segment is chosen from homo- or copolymers having repeating units of Formula I:
• R is chosen from a hydrogen atom, and a Ci-C alkyl group or -(CH2-OR a R b );
• R a is (CH 2 -CH 2 -O) y ;
• R b is chosen from a hydrogen atom and a Ci-C alkyl group; x is an integer chosen from the range 10 to 200,000; and y is an integer chosen from the range 0 to 10.
• the crosslinkable segment may be a polymer segment comprising at least one functional group crosslinkable in a multidimensional manner by irradiation or heat treatment.
• the electrolyte is a solid polymer electrolyte including LiPF 6 and a solvating polymer based on POE.
• the electrolyte is a solid polymer electrolyte as defined above and the electrode material comprises an electrochemically active material as defined here or an electrochemically active material prepared by the process as defined here and a conductive material electronic chosen from the group consisting of Ketjen MC carbon, Super P MC carbon and VGCFs.
• the electrode material may, for example, include from about 80 wt% to about 90 wt% of the electrochemically active material, from about 1 wt% to about 5% by weight of the electronic conductive material and from about 5% by weight to about 19% by weight of the solid polymer electrolyte.
• the electrolyte is a glass or ceramic electrolyte.
• the glass or ceramic electrolyte may include an ion-conductive crystalline ceramic, an ion-conductive amorphous ceramic, an ion-conductive amorphous glass, or an ion-conductive glass ceramic.
• Non-limiting examples of glass or ceramic electrolytes include site-deficient perovskite type electrolytes, garnet type electrolytes, NASICON type glass ceramic electrolytes, LISICON type electrolytes, lithium-stabilized sodium ion (Na + ) conductive aluminum oxides (AI2O3), and other similar glass or ceramic electrolytes.
• the electrolyte may also optionally include at least one additional additive, such as ionic conductive materials, inorganic particles, glass or ceramic particles, for example, nanoceramics (for example, carbon dioxide). aluminum (AI2O3), titanium dioxide (TiCh), silicon dioxide (SiCh) and other similar compounds), and other additives of the same type.
• the additional additive can be chosen from NASICON, LISICON, thio-LISICON, garnets, sulphides, sulfur halides, phosphates, thio-phosphates, in crystalline and/or amorphous form, and their combinations.
• the additional additive may be substantially dispersed in the electrolyte.
• the additional additive may also be in a separate layer.
• the present technology also relates to a battery comprising at least one electrochemical cell as defined here.
• the battery may be a lithium battery or a lithium-ion battery, a sodium battery or a sodium-ion battery, a magnesium battery or a magnesium-ion battery, or a potassium battery or a potassium-ion battery. ion.
• the battery is a lithium battery or a lithium-ion battery.
• the battery is a sodium battery or a sodium-ion battery.
• Example 1 Synthesis of electrochemically active materials a) Solid-state synthesis of sodium oxides, manganese oxides and at least one tunnel-type metallic element doped with iron
• the respective precursors, sodium carbonate (Na 2 CO 3 ), manganese (III) oxide (Mn 2 O 3 ), iron (III) oxide (Fe 2 O 3 ), and titanium dioxide ( TiO 2 ) were weighed in order to obtain the desired stoichiometries.
• the samples were prepared by grinding and mixing the precursor powders. The ground and mixed precursor powders were then put into an oven and heated to a temperature between about 700°C and about 1000°C under an atmosphere of air or oxygen for 2 to 24 hours b) Chemical synthesis in liquid medium of sodium oxides, manganese oxides and at least one tunnel-type metallic element doped with iron
• Sol-gel powders are synthesized using citric acid (C 6 H 8 O 7 ) as a chelating agent.
• sol-gel precursors were then calcined in an oven at a temperature of approximately 400 °C for approximately 6 hours to decompose the organic and inorganic contents (including anionic salts and CeHsO?).
• the powders thus obtained were ground in a mortar and calcined in an oven at a temperature of approximately 900 °C for approximately 9 hours under an atmosphere of air or oxygen in order to obtain the Nao sol-gel powders.
• UNO3 lithium nitrate eutectic lithium salt composition
• LiCI lithium chloride
• LiOH lithium hydroxide
• an oxide of sodium, lithium, manganese and at least one tunnel-type metallic element of formula Nao.osLio.seMnCh was also prepared for comparison purposes.
• This material was obtained by the ion exchange reaction of the present example using an oxide tunnel type sodium and manganese of formula Nao44Mn02 as described in the PCT patent application published under number WO2021/195778 (Wang et al.).
• XRD X-ray diffraction
• the atomic and molecular structure of the electrochemically active materials was studied by X-ray diffraction carried out on the powders of sodium, lithium, manganese oxides and at least one tunnel-type metallic element doped with iron, as prepared in Example 1 (c).
• Figures 1 to 5 show the X-ray diffraction patterns respectively for the powders of Nao,osLio,36Mn02, Nao,ioLio,33Feo,34Mno,44Tio,2202, Nao.osLio.ssFeo.soMno.ssTio sC ⁇ , Nao, 2oLio,24Feo,34Mno,5sTio,n02 and Nao,2iLio,2oFeo,4oMno,soTio,io02 tunnel type.
• Example 2 Electrochemical properties a) Configurations of electrochemical cells
• Example 1 (c) The electrochemical properties of the electrochemically active materials prepared in Example 1 (c) were studied. All cells were assembled in 2032 type coin cell battery packages with components shown in Table 1 and negative electrodes comprising metallic lithium film on aluminum current collectors. All cells were assembled with Whatman TM GF glass fiber filter paper separators impregnated with a 1 M solution of LiPFe in a non-aqueous EC/EMC solvent mixture ([3:7] by volume) and 5% FEC as liquid electrolyte.
• the electronic conductor material was a mixture of Ketjen MC carbon and Super P MC carbon ([1:1] by weight).
• This example illustrates the electrochemical behavior of electrochemical cells as described in Example 2(a).
• Figure 6 shows the charge and discharge profiles for two comparative cells (Cell 1). Charging and discharging were carried out in (1) at a cycling rate of 0.1 C between approximately 2.0 V and approximately 4.8 V vs Li + /Li, and in (2) between approximately 2.0 V and approximately 4.6 V vs Li + /Li. Charging and discharging were carried out at a temperature of approximately 25°C. Results are presented for a second discharge and charge cycle.
• Figure 7 shows a second charge and discharge profile for Cell 2. Charge and discharge were performed at a cycling rate of 0.1 C between approximately 2.0 V and approximately 4.8 V vs Li + /Li. Charging and discharging were carried out at a temperature of approximately 25°C.
• Figure 8 shows a charge and discharge profile for Cell 3. Charge and discharge were performed at a cycling rate of 0.1 C between approximately 2.0 V and approximately 4.8 V vs Li + / Li. Charging and discharging were carried out at a temperature of approximately 25°C. Results are presented for a second charge and discharge cycle.
• Figure 9 shows the charging and discharging profiles for Cell 4. Charging and discharging were performed at a cycling rate of 0.1 C between approximately 2.0 V and approximately 4.8
• V vs. Li + /Li. Charging and discharging were carried out at a temperature of approximately 25°C. Results are shown for a second (1) and fifth (2) charge and discharge cycle.
• Figure 10 shows a charge and discharge profile for Cell 5. Charge and discharge were performed at a cycling rate of 0.1 C between approximately 2.0 V and approximately 4.8
• V vs. Li + /Li. Charging and discharging were carried out at a temperature of approximately 25°C. Results are presented for a second charge and discharge cycle.
• Figure 11(a) shows charging and discharging profiles for Cell 6. Charging and discharging were performed at a cycling rate of 0.1 C between approximately 2.0 V and approximately 4.8 V vs. Li + /Li. Charging and discharging were carried out at a temperature of approximately 25°C.
• Figure 11(b) is a graph representing the capacity versus the number of cycles obtained for Cell 6.
• Figure 12(a) shows charging and discharging profiles for Cell 7. Charging and discharging were performed at a cycling rate of 0.1 C between approximately 2.0 V and approximately 4.8
• FIG. 12(b) is a graph representing the capacity versus the number of cycles obtained for Cell 7.
• Table 2 shows that the electrochemical properties of the electrochemically active material can be substantially improved by the partial substitution of sodium ions by lithium ions and/or by the partial substitution of manganese ions by titanium ions.

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