EP3802460A1 - Céramiques, leurs procédés de préparation et leurs utilisations - Google Patents
Céramiques, leurs procédés de préparation et leurs utilisationsInfo
- Publication number
- EP3802460A1 EP3802460A1 EP19811540.4A EP19811540A EP3802460A1 EP 3802460 A1 EP3802460 A1 EP 3802460A1 EP 19811540 A EP19811540 A EP 19811540A EP 3802460 A1 EP3802460 A1 EP 3802460A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- metal oxide
- ceramic
- oxide
- temperature
- carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
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- C01G25/00—Compounds of zirconium
- C01G25/006—Compounds containing, besides zirconium, two or more other elements, with the exception of oxygen or hydrogen
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- C04B35/2616—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing lithium
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Definitions
- the technical field generally relates to ceramics and their use in solid electrolytes, their methods of preparation and the electrochemical cells comprising them.
- Kim et al. have reported a carbothermal decomposition of U2CO3 and Na2CO3 using carbon (Kim, J. & Lee, H., Metall, Mater Trans, B, 2001, 32, 17-24).
- the use of carbon during the synthesis of lithitum titanate (LUTi50i2, also called LTO) and ceramics (such as LTO combined with Y2O3 and ZrO2) has also been presented by Zaghib et al. in the US patent application published under number US2010 / 0173160.
- Cubic phase LLZO is generally prepared in the presence of dopants such as aluminum (Hubaud, AA et al., J. Mater Chemsitry A 1, 8813-8818 (2013)) or gallium (Li, C. “Gallium Substitution in Zirconate-Based Fast Ionia Conducting Ceramics. "(2016) Ail Theses, Clemson University, 2457).
- dopants such as aluminum (Hubaud, AA et al., J. Mater Chemsitry A 1, 8813-8818 (2013)) or gallium (Li, C. “Gallium Substitution in Zirconate-Based Fast Ionia Conducting Ceramics. "(2016) Ail Theses, Clemson University, 2457).
- One aspect of the present technology relates to a process for preparing a lithium-based ceramic.
- the method comprises at least the steps of:
- step (b) heating the powder mixture obtained in step (a) at a treatment temperature
- step (a) wherein the lithium ion source of step (a) has a melting point lower than the treatment temperature of step (b).
- step (b) is carried out under an inert atmosphere and the method further comprises a step (c) of heating the product of step (b) in the presence of oxygen (for example in the air).
- step (b) is performed in the presence of oxygen (for example, in the presence of air).
- the heating step in the presence of air is performed for a period of time sufficient for the removal of the carbon material.
- the method further comprises a step (b) (i) of mixing the product obtained in step (b) with a metal oxide or phosphate and a carbon material; and (b) (ii) heating the mixture obtained in (b) (i) to a second process temperature to obtain a second product, wherein the product of step (b) has a melting point above above the treatment temperature of step b (ii).
- the at least one metal oxide or phosphate is an oxide or phosphate of a metal selected from zirconium, titanium, germanium, gallium, tantalum, iron and niobium.
- the at least one oxide or metal phosphate comprises at least two oxides or phosphates of metals chosen from lanthanum, aluminum, zirconium, titanium, germanium, gallium, tantalum, iron and niobium. provided that at least one metal is lanthanum or aluminum.
- the at least one metal oxide or phosphate comprises at least three oxides or phosphates of metals.
- the at least one oxide or phosphate is a lanthanum or aluminum oxide.
- the at least one oxide or phosphate is a lanthanum oxide and the process further comprises a second metal oxide selected from zirconium oxide and titanium oxide.
- the method may also include a third oxide of an element selected from aluminum, germanium, gallium, tantalum, niobium, iron, barium, boron, and silicon.
- the molar ratio "carbon lithiur ion" is in the range of 0.50 to 2.4, the lithium ion from the ion source lithium.
- a second aspect of the present technology relates to a method of preparing a ceramic, the method comprising the steps of: a) mixing lithium carbonate, a first metal oxide, and a carbon material to obtain a first powder mixture;
- step (b) heating the first powder mixture of step (a) to a temperature of at least 800 ° C;
- step (b) mixing the product of step (b) with a second metal oxide and optionally a third metal oxide, to obtain a second mixture of powders;
- step (c) heating the second powder mixture obtained in step (c) to a temperature of at least 800 ° C;
- the first metal oxide comprises at least one metal oxide selected from zirconium oxides, titanium oxides, germanium oxides, gallium oxides, tantalum oxides, iron oxides, and niobium oxides.
- the second and third metal oxides comprise at least one metal oxide selected from lanthanum oxides, zirconium oxides, and aluminum oxides.
- the product of step (b) comprises a lithiated metal oxide of Formula LisM v 04 or LisIVTOs, wherein M v is Ga, Al or Fe, and M w is Ta or Nb.
- the mixing step (c) comprises the third metal oxide.
- the mixing step may also further comprise a phosphate salt.
- the molar ratio "L COsicarbone” is in the range of 0.25 to
- the carbon material is selected from carbon black (such as acetylene black, Ketjen black MC , etc.), graphene, graphite, carbon nanotubes, carbon fibers or nanofibers, and combinations thereof.
- the heating step of the methods described above may be carried out at a temperature in the range of 800 ° C to 1400 ° C, for example, for a period of time in the range of 30 minutes to 3 hours or from 45 minutes to 1.5 hours, preferably for a period of about 1 hour.
- a third aspect of the present technology relates to a method of preparing a ceramic, the method comprising the steps of:
- step (b) heating the mixture of powders obtained in step (a) under an inert gas flow rate up to a first temperature below the decomposition temperature of the
- step (b) stopping the inert gas flow of step (b) and heat treating at a second temperature above the first temperature;
- the first metal oxide has the formula M z 2q 3, where M z is a metal of oxidation state III (such as La, Al, Ga, etc.), preferably M z is the lanthanum.
- the second metal oxide is a metal dioxide of an oxidation state metal IV (such as Zr, Ti, Ge, etc.), preferably the second metal oxide is carbon dioxide. zirconium.
- the ceramic comprises a compound of cubic crystalline structure.
- the first temperature is equal to or below 800 ° C, or equal to or below 750 ° C, or equal to or below 700 ° C.
- the second temperature is in the range of 800 to 1400 ° C, or in the range of 800 to 1200 ° C, or in the range of 850 to 1100 ° C, or included in the range of 900 to 1000 ° C.
- the heating of step (b) is carried out for a period of time in the range of 30 minutes to 3 hours, or the interval of 1 hour to 3 hours, or a period of about 2 hours .
- step (a) further comprises a carbon material, for example, selected from carbon black (such as acetylene black, Ketjen black MC , etc.), graphene, graphite, carbon nanotubes, carbon fibers or nanofibers, and combinations thereof.
- step (a) is free of added carbon material.
- the mixing step of one or the other of the above processes is carried out by ball milling or in a planetary mixer.
- the mixture is made by ball milling, for example, in a zirconium dioxide vessel, using zirconium dioxide beads.
- a fourth aspect relates to a ceramic obtained or obtainable by a process as defined herein.
- the ceramic comprises a compound chosen from the compounds of Formulas (I) to (IV):
- M is selected from Al, Ga, Ta, Fe, and Nb;
- M x is selected from Ti and Ge
- M y is selected from Ba, B, Al, Si and Ta;
- x is in the range of 0 to 1;
- y is greater than 0 and smaller than or equal to 0.67;
- the compound comprises ionic vacancies. According to another embodiment, the compound does not comprise ionic vacancies.
- the compound is of Formula (I), for example, having a tetragonal or cubic crystalline structure.
- the Compound is of Formula (II), for example, having a tetragonal or cubic crystalline structure.
- the compound is of Formula (I) or (II) and of cubic crystalline structure.
- the compound is an undoped compound of Formula (I) and has a cubic crystal structure.
- the compound is of Formula (III), for example, having a perovskite-like crystalline structure.
- the compound is of Formula (IV), for example, having a crystalline structure of NASICON type.
- the ceramic has a residual carbon content below 10% by weight, or a residual carbon content below 5% by weight, or even below 2% by weight, or below 1% by weight. According to another embodiment, the ceramic is free of residual carbon.
- a fifth aspect relates to an electrolyte comprising a ceramic as defined herein.
- the electrolyte is a solid electrolyte.
- the electrolyte further comprises a polymer, a solvent (such as an aprotic polar solvent) or a combination of both.
- the electrolyte has an ionic conductivity in the range of 10 5 to 10 3 S / cm.
- a sixth aspect relates to an electrode material comprising a ceramic as defined herein, for example, the material further comprising an electrochemically active material and optionally a binder and / or an electronically conductive material.
- the present document relates to an electrochemical cell comprising a negative electrode, a positive electrode and an electrolyte, wherein at least one of these three elements comprises the present ceramic.
- the electrolyte is as defined herein.
- the positive or negative electrode comprises an electrode material as defined herein.
- the positive or negative electrode comprises an electrode material as defined herein and the electrolyte is as defined herein.
- Other aspects relate to a battery comprising at least one cell electrochemical as defined here, for example, the battery being a lithium or lithium-ion battery.
- Figure 1 shows the results of the X-ray diffraction analysis of LLZO prepared in Example 1 against a standard of reference.
- Figure 2 shows the results of the X-ray diffraction analysis of LLZO prepared in Example 2 against reference standards.
- Figure 3 shows the results of the X-ray diffraction analysis of LATP prepared in Example 3 against reference standards.
- Figure 4 shows the results of the X-ray diffraction analysis of LLZO prepared in Example 4 against reference standards.
- Figure 5 shows the results of the X-ray diffraction analysis of a mixture of Li5Ga04 with La2O3 and ZrO2 prepared as an intermediate in Example 5 with respect to the reference standards.
- Figure 6 shows the results of X-ray diffraction analysis of LLZO with LiGaO2 prepared in Example 5 against reference standards.
- Figure 7 shows the results of X-ray diffraction analysis of (a) cubic LLZO (heating without gas flow), and (b) LLZO tetragonal (heating with gas flow), compared to the reference standard, both LLZO being undoped and prepared according to the procedure of Example 6.
- Figure 8 shows the results of the X-ray diffraction analysis of the undoped cubic LLZO (annealing without gas flow in the presence of carbon), prepared in Example 7, in comparison with a reference standard.
- This document presents a new process for the preparation of lithium-based ceramics for use in electrochemical applications, in electrolyte compositions as well as in cathode and anode materials.
- This method uses a sacrificial carbon additive which is then removed during heat treatment.
- the carbon additive may serve as a dispersant or surfactant when a source of lithium ions having a melting point below the heat treatment temperature is used, such as lithium carbonate.
- this dispersion may facilitate obtaining a uniform particle distribution and a smaller ceramic particle size, i.e., a smaller particle size than that of their commercial equivalents.
- the process is also simple and economical and / or requires shorter reaction times.
- the present process for preparing a lithium-based ceramic comprises at least one step of mixing a lithium ion source, at least one metal oxide or phosphate and a carbon material to obtain a powder mixture. and heating the powder mixture to a given processing temperature.
- the lithium ion source is a lithium salt having a melting point below the processing temperature.
- lithium salt has a lower melting point at 800 ° C, such as lithium carbonate.
- the lithium carbonate may be used in a molar ratio L COsicarbone between 0.25 and 1, 2, or between 0.5 and 1.1.
- the molar ratio Li: carbon is between 0.50 and 2.4, or between 1 and 2.2.
- the process may comprise a sequence of mixing / heating steps, or comprise two or more mixing / heating sequences.
- the first sequence of mixing / heating steps comprises mixing the lithium ion source and at least one metal oxide or phosphate and the carbon material and heating the mixture to obtain a first compound lithiated metal oxide.
- This compound is then mixed, in a second mixing step, with at least one additional metal oxide or phosphate and a carbon material, and the resulting mixture is heated to a second treatment temperature.
- the carbon may be from the first mixing / heating sequence if the first heating has been carried out under conditions which have not led to its removal (for example, heating under an inert atmosphere, at a temperature and / or for a period insufficient for burn the carbon material completely or in part).
- the carbon material may also be a second carbon material, which may be added in the second mixing step. In this case, the second carbon material may be of the same nature as the first carbon material or different.
- the carbon material may be carbon in any known, commercially available reference form, such as carbon black (e.g., acetylene black, Ketjenblack TM , etc.), graphene, graphite, carbon nanotubes, carbon nanowires, carbon fibers or nanofibers, or one of their combinations.
- carbon black e.g., acetylene black, Ketjenblack TM , etc.
- graphene graphite
- carbon nanotubes carbon nanowires
- carbon fibers or nanofibers or one of their combinations.
- the product of the first sequence preferably has a melting temperature higher than the processing temperature of the first heating step.
- the one or more heating steps are performed in the presence of oxygen and the carbon material is burned off.
- the Heating steps are performed under an inert atmosphere (eg under argon) and the method includes an additional heating step in the presence of oxygen to remove the carbon source by combustion.
- the term "remove” may include complete removal as well as partial or substantial removal, for example, a residual carbon content of less than 10% by weight, or less than 5% by weight, or less than 2% by weight or even less than 1% by weight.
- the metal oxide or phosphate is an oxide or a phosphate of a metal selected from lanthanum, aluminum, zirconium, titanium, germanium, gallium, tantalum, iron and niobium .
- the method comprises reacting at least two metal oxides or phosphates, together with the lithium ion source, in a single sequence of mixing / heating steps or each in a separate mixing / heating sequence.
- first metal oxides or phosphates include the oxides or phosphates of a metal which may be selected from zirconium, titanium, germanium, gallium, tantalum, iron and niobium.
- a second metal oxide include lanthanum oxide and aluminum oxide.
- the process comprises oxides or phosphates of at least two metals selected from lanthanum, aluminum, zirconium, titanium, germanium, gallium, tantalum, iron and niobium, provided that at least one metal is lanthanum or aluminum.
- An example also includes three oxides or phosphates of metals.
- the present process may comprise the following nonlimiting examples of combinations of metal oxides (in addition to materials based on lithium ion and possibly carbon):
- Another example of the present process comprises the following steps: a) mixing U2CO3, a first metal oxide, and a carbon material to obtain a first powder mixture; b) heating the first mixture obtained in step (a) to a temperature of at least 800 ° C; c) mixing the product of step (b) with a second metal oxide and optionally a third metal oxide, to obtain a second mixture; d) heating the second mixture obtained in step (c) to a temperature of at least 800 ° C; wherein the first metal oxide is different from the second metal oxide.
- phosphate ions preferably ammonium phosphate, for example [NH4KH2PO4]
- the first metal oxide include at least one metal oxide selected from oxides of zirconium, titanium, germanium, gallium, tantalum, iron and niobium.
- the second oxide may comprise at least one metal oxide selected from lanthanum, zirconium and aluminum oxides.
- the product of step (b) comprises a lithiated metal oxide of Formula U5MO4 or LisIVTOs, where M v is Ga, Al or Fe, and M w is Ta or Nb.
- the mixing step (s) in the present process can be carried out by any known method of the field such as ball milling, planetary mixer, etc.
- the mixing step (s) are carried out by ball milling, for example, in a zirconium dioxide jar with zirconium dioxide beads.
- the heating steps can be carried out in the presence of oxygen (with removal of carbon) or in an inert atmosphere, provided that a final heating step is performed in the presence of oxygen for the carbon reaction. and its elimination.
- step (b) is carried out under an inert atmosphere
- step (d) is carried out in the presence of oxygen.
- steps (b) and (d) are carried out under an inert atmosphere and the process comprises a step additional heating (e) in the presence of oxygen at a temperature of at least 800 ° C.
- the heating steps of the present process are carried out in a crucible resistant to temperatures of at least 800 ° C, for example in a graphite or alumina crucible.
- the present process comprises the steps of:
- step (b) heating the powder mixture obtained in step (a) under gas flow (for example an inert gas such as argon or nitrogen) to a first temperature below the decomposition temperature of L12CO3;
- gas flow for example an inert gas such as argon or nitrogen
- step (b) stopping the gas flow of step (b) and heat treatment at a second temperature above the first temperature
- the first metal oxide has the formula M z 2q 3, where M z is a metal of oxidation state III, such as La, Al, Ga, etc.
- the first oxide is lanthanum oxide.
- the second metal oxide may be any metal oxide, for example, selected from oxidation state (IV) metal dioxides.
- the second oxide include oxides of zirconium, titanium, germanium, etc.
- the second oxide is a zirconium oxide.
- the use of this method can provide a compound having a cubic crystal structure while avoiding the use of a doping element. Therefore, the resulting ceramic may comprise a compound having a cubic crystal structure.
- the first temperature is generally less than or equal to 800 ° C or less than or equal to 750 ° C, or even lower than or equal to 700 ° C and the second temperature is between 800 and 1400 ° C, or between 800 and 1200 ° C, or between 850 and 1100 ° C, or between 900 and 1000 ° C.
- the heat treatment of step (b) can be carried out for a period of between 30 minutes and 3 hours, or between 1 hour and 3 hours, or about 2 hours.
- the mixing step of the process may be carried out by ball milling or in a planetary mixer, for example, by ball milling in a zirconium dioxide vessel, using zirconium dioxide beads.
- the mixing step (a) can be carried out with or without the addition of a carbonaceous material.
- the carbonaceous material may be chosen from carbon black (for example acetylene black, Ketjenblack TM , etc.), graphene, graphite, carbon nanotubes, fibers or nanofibres. of carbon, and their combinations.
- the mixing step (a) of this process excludes the addition of a carbon material.
- the ceramics obtainable by the present process are also contemplated.
- the ceramics produced by the present process may have a uniform particle distribution and a smaller ceramic particle size, for example, a particle size smaller than commercially available equivalents.
- the ceramics comprise a compound of at least one of the following formulas (I) to (IV):
- M is selected from Al, Ga, Ta, Fe, and Nb;
- M x is selected from Ti and Ge
- M y is selected from Ba, B, Al, Si and Ta;
- x is in the range of 0 to 1;
- y is greater than 0 and less than 0.67
- y ' is greater than 0 and less than 1; and z is in the range of 0 to 1.
- the ceramic may also comprise a mixture of oxides and / or phosphates.
- the ceramic is a mixture of a compound of one of the above formulas and at least one other metal oxide.
- the ceramic may also comprise a compound of one of the above formulas and further include a doping material, for example, an additional metal oxide.
- the ceramic comprises at least 50% by weight of a compound of one of Formulas I to IV, or at least 60% by weight, or at least 70% by weight, or at least 80% by weight, or at least 90% by weight, or even at least 90% by weight.
- the ceramic may comprise a compound of Formula (I) or (II), for example, having a tetragonal or cubic crystalline structure, or a mixture thereof.
- the compound may be an undoped compound of Formula (I) and have a cubic crystal structure.
- the ceramic may comprise a compound of Formula (III), for example, having a perovskite crystal structure.
- the ceramic comprises a compound of Formula (IV), for example, having a crystalline structure of NASICON type.
- the ceramic may be free or substantially carbon free or may comprise a residual carbon content of less than 10% by weight, or less than 5% by weight, or less than 2% by weight, or even less than 1% by weight.
- the above ceramics are intended to be used, for example, in electrochemistry or wherever lithium ion exchange is required.
- the present disclosure also contemplates electrolytes comprising one of the present ceramics, alone or in combination with other electrolytic elements such as other inorganic particles, lithium salts, separators, solvents and solvating polymers.
- the electrolyte is a solid electrolyte or gel, preferably a solid electrolyte.
- the electrolyte preferably has an ionic conductivity in the range of 10 5 to 10 3 S / cm.
- the solvent is a non-aqueous polar aprotic solvent.
- non-aqueous solvents examples include cyclic carbonates such as ethylene carbonate (EC), propylene carbonate (PC), butylene carbonate (BC), and vinylene carbonate (VC); acyclic carbonates such as dimethyl carbonate (DMC), diethyl carbonate (DEC), ethyl and methyl carbonate (EMC), and dipropyl carbonate (DPC); lactones such as g-butyrolactone (g-BL) and ⁇ -valerolactone (g-VL); acyclic ethers such as 1,2-dimethoxyethane (DME), 1,2-diethoxyethane (DEE), ethoxymethoxyethane (EME), and trimethoxymethane; cyclic ethers such as tetrahydrofuran, 2-methyltetrahydrofuran, 1,3-dioxolane, and derivatives thereof; and other solvents such as dimethylsulfoxide, formamide, acetamide, dimethyl
- Non-limiting examples of solvating polymers useful in electrolytes include polyethylene oxide and copolymers comprising ethylene oxide units, poly (propylene oxide) and copolymers comprising propylene oxide units, polyethylene oxide, and polyethylene oxide units. and copolymers comprising dimethylsiloxane units, polyalkylene carbonate and copolymers comprising alkylene carbonate units, polyalkylene sulfone and copolymers comprising copolymers comprising alkylene sulfide units, polyurethanes and copolymers comprising urethane units, polyvinyl alcohol and copolymers comprising vinyl alcohol units, and combinations thereof.
- the solvating polymers may be linear, but also branched or crosslinked.
- Electrode materials comprising one of the present ceramics, for example in combination with other electrode material components such as an electrochemically active material, a conductive material, inorganic particles, salts and the like. of lithium and binders.
- electrochemically active materials include, but are not limited to, lithium titanates and titanates (such as PO2, L TiOs, LUTi50i2, FteTisOn, H2TUO9, or a combination thereof), lithiated metal phosphates (such as LiM a PO4 where M a is Fe, Ni, Mn, Co, or a combination thereof), lithiated or non-lithiated vanadium oxides (such as UV3O8, V2O5, UV2O5, etc.), and other lithiated metal oxides such as that LiMn 2 O 4, LiM b 02 (M b being Mn, Co, Ni, or a combination thereof), Li (NiM c ) O 2 (M c being Mn, Co, Al, Fe, Cr,
- the active material is selected from lithium iron phosphate (LFP), lithium manganese iron phosphate (LMFP), lithium titanate (LTO), nickel cobalt oxide and lithium aluminum (NCA), lithiated cobalt oxide (LCO), and nickel manganese oxide and lithiated cobalt (NMC).
- LFP lithium iron phosphate
- LMFP lithium manganese iron phosphate
- LTO lithium titanate
- NCA nickel cobalt oxide and lithium aluminum
- NMC nickel cobalt oxide
- LCO nickel manganese oxide and lithiated cobalt
- NMC nickel manganese oxide and lithiated cobalt
- the particles may be freshly formed or commercially available, in the form of microparticles or nanoparticles, and may further include a carbon coating.
- Examples of conductive materials include carbon black, Ketjen TM black, acetylene black, graphite, graphene, carbon fibers (or nanofibres) (eg, VGCF), carbon nanotubes, or combination of these.
- Examples of binders include one of the above solvating polymers, as well as water-soluble binders such as SBR (styrene-butadiene rubber), NBR (butadiene-acrylonitrile rubber), HNBR (hydrogenated NBR) , CHR (epichlorohydrin rubber), ACM (alkyl acrylate rubber), and other similar binders, and cellulose-based binders (such as carboxyalkylcellulose and hydroxyalkylcellulose), or a combination of two or more of the foregoing binders.
- SBR styrene-butadiene rubber
- NBR butadiene-acrylonitrile rubber
- HNBR hydrogenated NBR
- CHR epichlorohydrin
- the carboxyalkylcellulose may be carboxymethylcellulose (CMC) or carboxyethylcellulose. Hydroxypropylcellulose is an example of hydroxyalkylcellulose.
- Other examples of binders include fluorinated polymeric binders such as PVDF and PTFE.
- the present disclosure also relates to an electrochemical cell comprising at least one of the present ceramics in at least one of its components, ie in a positive or negative electrode material or in the electrolyte.
- the electrochemical cell comprises an electrolyte as defined herein, comprising the present ceramic, a negative electrode and a positive electrode.
- the electrochemical cell may also comprise an electrolyte as herein defined comprising the present ceramic, a negative electrode and a positive electrode where the negative electrode is as defined above and comprises at least one of the present ceramics.
- the electrochemical cell may also comprise an electrolyte as herein defined comprising the present ceramic, a negative electrode and a positive electrode where the positive electrode is as defined above and comprises at least one of the present ceramics.
- An electrode material used in the present electrochemical cells can be prepared without adding the ceramic of the present invention, for example from an electrochemically active material as defined above, as well as any additional components, such as a conductive material, inorganic particles, salts or binders.
- An electrode material may also comprise a metal lithium film or an alloy thereof, such as an extruded lithium film, or be made of a material such as graphite.
- the battery is a lithium or lithium-ion battery.
- the battery is a lithium or lithium-ion battery.
- Other uses of the present ceramics may also include electrochromic devices (ECDs) as well as optoelectronic devices.
- Example 1 Li7La3Zr20i2 (LL2O)
- L12CO3 (3.38g), La2O3 (5.82g), ZrO2 (2.93g), and acetylene black (0.500g) were milled together in a zirconium oxide jar with zirconium oxide beads for 10 minutes.
- the resulting powder was then placed in an alumina crucible and heated in a stagnant air oven at 900 ° C for 1 hour. After cooling to room temperature, the final powder was analyzed by X-ray diffraction and Li7La3Zr20i2 (LLZO) of tetragonal phase was observed (see Figure 1).
- L12CO3 (2.99g), Al2O3 (0.150g), La203 (5.76g), ZrO2 (2.90g), and acetylene black (0.500g) were milled together in a zirconium oxide jar with zirconium oxide beads for 10 minutes.
- the resulting powder was then placed in an alumina crucible and heated in a stagnant air oven at 900 ° C for 1 hour. After cooling to room temperature, the final powder was analyzed by X-ray diffraction.
- Figure 2 shows that Li7La3Zr20i2 (LLZO) of cubic structure was mainly observed as well as AI2O3. A minor phase of LLZO with a tetragonal structure was also observed.
- Li 2 CO 3 (0.79 g), Al 2 O 3 (0.22 g), T 2 O 2 (2.03 g), NH 4 H 2 R0 4 (5.17 g) and acetylene black (0 12 g) were ground together in a zirconium oxide jar with zirconium oxide beads for 10 minutes.
- the resulting powder was then placed in an alumina crucible and heated in a stagnant air oven at 1000 ° C for 1 hour. After cooling to room temperature, the final powder was analyzed by X-ray diffraction. LiI.3AlO.3Tii.7 (P04) 3 (LATP) having a NASICON type structure was observed as well as a minor phase of PO2 (see FIG. 3).
- Example 4 Li7La3Zr2O2 Powder of U2CO3 (3.38g), La2O3 (5.82g), ZrO2 (2.93g), and acetylene black (0.750g) were milled together in an oxide jar. of zirconium with zirconium oxide beads for 10 minutes. The resulting powder was then placed in an alumina crucible and heated in a stagnant air oven at 900 ° C for 1 hour. After cooling to room temperature, the final powder was analyzed by X-ray diffraction. La2Zr2O7 (LZO) and L7La3Zr20i2 (LLZO) having a tetragonal structure were observed (see Figure 4).
- Example 5 Li7La3Zr2O2 with LiGaO2
- L12CO3 (3.83 g), Ga2O3 (1.94 g) and acetylene black (1.24 g) were ground together in a zirconium oxide jar with zirconium oxide beads for 10 minutes. minutes.
- the resulting powder was heated in a carbon crucible under an argon atmosphere.
- the black powder (1.29 g) was then mixed with La 2 O 3 (0.53 g) and ZrO 2 (0.26 g) and ground together in a zirconium oxide jar with silica gel beads. zirconium for 10 minutes.
- the resulting intermediate powder was analyzed by X-ray diffraction, demonstrating the presence of LisGaC, La2O3 and ZrO2 (see Figure 5).
- L12CO3 (6.77 g), La2O3 (11.94 g), and ZrO2 (5.87 g) were mixed with zirconium oxide beads under an air atmosphere for 10 minutes.
- the powder obtained was heated in a tubular oven on a graphite boat.
- the nitrogen flow rate in the oven was maintained at 2 L / min from room temperature up to 700 ° C.
- the nitrogen flow was then stopped and the temperature was raised until it reached 950 ° C.
- the powder was then annealed at this temperature (950 ° C) for 2 hours under static conditions without nitrogen flow, and then cooled.
- the resulting powder had a cubic structure as indicated in the X-ray diffraction pattern of Figure 7 (a).
- L12CO3 (6.77 g), La2O3 (11.94 g), ZrO2 (5.87 g), and graphite (1 g) were mixed with zirconium oxide beads under an air atmosphere. for 10 minutes.
- the resulting powder was heated in a tubular furnace on a graphite boat.
- the nitrogen flow rate in the oven was maintained at 2 L / min from room temperature up to 700 ° C.
- the nitrogen flow was then stopped and the temperature was raised until it reached 950 ° C.
- the powder was annealed at this temperature (950 ° C) for 2 hours under static conditions without nitrogen flow and then cooled.
- the resulting powder had a cubic structure as indicated in the X-ray diffraction pattern of Figure 8.
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