Patent application title: Containers made of coated ceramic matrix composites
Patent Information
- Application Number
- JP2024537968
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2021-12-23
- Filing Date
- 2022-12-23
- Publication Date
- 2025-12-02
AI Technical Summary
The existing containers used for producing lithium-containing oxide powders, such as LiFePO4, LiMn2O4, or lithium-nickel-cobalt-manganese oxides, face significant degradation during the demanding synthesis processes, leading to a short service life and limited number of cycles.
A container made of ceramic matrix composite (CMC) with an internal wall coated by at least 80% with a crystalline oxide or its precursor, comprising elements Li and Al, enhances the durability and resistance to degradation.
The CMC container exhibits reduced deterioration and extended service life, allowing for a higher number of cycles in producing metal oxide powders, particularly those containing lithium.
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Abstract
Description
[Technical field]
[0001] The present invention relates to a container made of ceramic matrix composite, i.e. CMC, the surface of the inner wall of which is at least partially, preferably more than 80%, covered by a coating comprising at least one layer containing a crystalline oxide comprising at least the elements Li and Al, the invention also relates to the use of said container for the production of lithium-containing oxide powders, in particular oxides of metals or oxides of several lithiated transition metals. [Background technology]
[0002] The need for lithium-ion batteries is constantly increasing. Most of them include a part, typically the cathode, made of an oxide containing lithium, in particular an oxide of a metal or of several lithiated transition metals, in particular LiFePO4 (or LPF), LiMn2O4 (or LMO), or Lithium-Nickel-Cobalt-Manganese (or Li-NMC) oxide.
[0003] The cathode is typically made by forming a powder of the above-mentioned oxide of the metal or of one or more of the lithiated transition metals.
[0004] Among the conventional methods for producing said powders are the production of a mixture of oxides and / or a mixture of various oxide precursors, followed by a heat treatment that makes it possible to carry out a solid-phase synthesis of the oxide of the metal or of several lithiated transition metals. During said heat treatment, the mixture is placed in a container, generally called a sagger. The conditions for synthesizing said powders and said mixtures, in particular the lithium-containing elements, are particularly demanding for the container. Summary of the Invention [Problem to be solved by the invention]
[0005] There is a need to extend the useful life of such containers.
[0006] One object of the present invention is to at least partially meet this need. [Means for solving the problem]
[0007] According to the invention, this object is achieved by a vessel made of a ceramic matrix composite, i.e. CMC, the surface of the internal wall of said vessel is at least partially, preferably more than 80%, and more preferably over the entirety of said internal wall, covered by a coating comprising at least one layer comprising a crystalline oxide comprising at least the elements Li and Al, or a precursor of said crystalline oxide.
[0008] The inventors have discovered that the container according to the present invention undergoes relatively little degradation during use, which allows for a relatively long service life, and in particular a relatively large number of cycles, for producing metal oxide powders or oxide powders of multiple lithiated transition metals.
[0009] According to preferred but non-limiting embodiments of the present invention, which may be combined with one another where appropriate, are the following: - said crystalline oxide also contains the element Si; - The above crystalline oxides are LiAlO2, LiAlSi2O6, Li3AlSiO5, LiAlSi4O 10 , LiAlSiO4, and mixtures thereof; in particular LiAlSi2O6, Li3AlSiO5, LiAlSi4O 10 , LiAlSiO4, and mixtures thereof; - the ceramic fibers of the ceramic matrix composite are optionally assembled in the form of single bundles and / or assembled bundles and are selected from fibers containing more than 95% by weight, preferably consisting essentially of, oxides, carbides, nitrides, carbon, and mixtures thereof; the ceramic fibers of the ceramic matrix composite are optionally aggregated in the form of single bundles and / or aggregated bundles and are selected from the following fibers: - Those having a chemical analysis that contains more than 95% by mass of oxides, preferably consisting essentially of oxides, and in terms of percentage of total oxides, SiO2 > 70% by mass. - Those having a chemical analysis that contains more than 95% by mass of oxides, preferably consisting essentially of oxides, and in terms of percentage of total oxides, 45% < SiO2 < 80% by mass, and an amount of iron oxide in the form of Fe2O3 such that 1% < Fe2O3 < 20% by mass, and 5% < Al2O3 < 25%. - Those having a chemical analysis that contains more than 95% by mass of oxides, preferably consisting essentially of oxides, and in terms of percentage of total oxides, Al2O3 > 65% by mass. - Those containing more than 95% by mass of silicon carbide, preferably consisting essentially of silicon carbide. - Those containing more than 95% by mass of carbon, preferably consisting essentially of carbon. - And mixtures thereof; - The ceramic fibers of the ceramic matrix composite are optionally assembled in the form of a single bundle and / or an assembled bundle, and are fibers composed of more than 95% by mass of alumina, fibers composed of more than 95% by mass of silica, fibers composed of more than 95% by mass of mullite, fibers composed of more than 95% by mass of mullite and cordierite, fibers composed of more than 90% by mass of basalt, fibers composed of more than 95% by mass of glass, fibers composed of more than 95% by mass of silicon carbide, fibers composed of more than 95% by mass of carbon, and are selected from mixtures thereof; - The matrix of the ceramic matrix composite is selected from matrices containing more than 95% by mass of oxides, carbides, nitrides, sialons, and mixtures thereof, particularly matrices consisting essentially of oxides, carbides, nitrides, sialons, and mixtures thereof; - The matrix of the ceramic matrix composite is selected from the following matrices: - Those having a chemical analysis that contains more than 95% by mass of oxides, and in terms of percentage of total oxides, SiO2 + Al2O3 + ZrO2 + HfO2 + MgO > 70% by mass. - Those having a chemical analysis that contains more than 95% by mass of oxides and, in percentage with respect to all oxides, SiO2 + Al2O3 > 70% by mass; - Those having a chemical analysis that contains more than 95% by mass of oxides and, in percentage with respect to all oxides, Al2O3 + ZrO2 + HfO2 > 70% by mass; - Those having a chemical analysis that contains more than 95% by mass of oxides and, in percentage with respect to all oxides, SiO2 + Al2O3 + MgO > 70% by mass; - Those containing more than 90% by mass of SiC + Si3N4 + SiAlON; - The coating contains at least one layer that contains a crystalline oxide containing at least the elements Li, Al, and Si; - The coating consists of one or more crystalline oxides containing at least the elements Li and Al, more than 15% by mass; - The coating contains a precursor of at least one crystalline oxide containing at least the elements Li and Al, and is preferably selected from lithiated byalite, Li4SiO4, and mixtures thereof; - The coating has the following chemical composition in percentage with respect to all oxides: - SiO2 + Al2O3 + Li2O > 50% by mass, and, - Li2O: more than 0.5% by mass and less than 30% by mass, and / or, - Al2O3: more than 2% by mass and less than 80% by mass, and / or, - SiO2: more than 5% by mass, or 10% < SiO2 < 80% by mass; - The coating consists of more than 90% by mass of oxides; - The coating has a thickness greater than 50 μm and / or less than 2000 μm; - More than 99% of the surface of the inner wall is covered by the above coating; - The container has a bottom and at least one side surface.
[0010] The invention also relates to the use of the above-mentioned vessel for the production of lithium-containing oxide powders, in particular oxides of a metal or oxides of multiple lithiated transition metals.
[0011] definition
[0012] - "Ceramic Matrix Composite" or "CMC" is conventionally understood to mean an article composed of ceramic fibers firmly bound together by a ceramic matrix. "Ceramic" is understood to mean an article that is neither metallic nor organic. In the context of the present invention, oxide glasses and materials that contain or consist of carbon are considered as ceramic articles. - "coating" is understood to mean one or more layers of one or more materials of a different nature from the CMC substrate, at least one of said layers, in particular a layer comprising a crystalline oxide comprising at least the elements Li and Al, may be the result of a reaction of the CMC substrate, in particular after an elevated temperature, and of a deposition on the surface of said CMC. - "precursor" of a crystalline oxide is understood to mean one or more materials which, after heat treatment, preferably in air at temperatures above 400°C, in particular during the first use of the container according to the invention, will lead to said crystalline oxide, optionally in combination with one or more elements of the CMC. - "Fiber" means a filament having a length greater than five times its equivalent diameter. - The "equivalent diameter" of a fiber is the diameter of a disk of the same surface as its cross section at half its length. - "single bundle" means a collection of fibres containing, in cross section, at least 10 fibres, preferably less than 500,000 fibres, and having a length greater than 5 times its diameter. - An "aggregated bundle" is a collection of bundles. "Sialon", SiAlON, is a compound of oxynitrides of at least the elements Si, Al and N, in particular a compound conforming to one of the following formulae: -Si x Aly O u N v Here: - x is greater than or equal to 0, greater than 0.05, greater than 0.1, or greater than 0.2, and less than or equal to 1, less than or equal to 0.8, or less than or equal to 0.4, - y is greater than or equal to 0, or greater than 0.1, greater than 0.3, or greater than 0.5, and less than or equal to 1, - u is greater than 0, greater than 0.1, or greater than 0.2, and less than or equal to 1, or less than or equal to 0.7, - v is greater than 0, greater than 0.1, greater than 0.2, or greater than 0.5, or greater than 0.7, and less than or equal to 1, - x + y > 0, x, y, u, and v are stoichiometric exponents, normalized with respect to the highest one, which is made equal to 1; - Me x Si 12-(m+n) Al (m+n) O n N 16-n Here, 0 ≤ x ≤ 2, Me is a cation selected from lanthanides, Fe, Y, Ca, Li cations, and mixtures thereof, 0 ≤ m ≤ 12, 0 ≤ n ≤ 12, and 0 < n + m ≤ 12, and is generally referred to as "α'-SiAlON" or "SiAlON-α'". - For clarity, simple oxide chemical formulas are used to specify the content levels of these oxides in the composition. For example, "SiO2" or "Al2O3" indicates the content of these simple oxides in the selected composition, while "silica" and "alumina" are used to indicate the actual presence of the phases of these oxides consisting of SiO2 and Al2O3, respectively. - Unless otherwise specified, all oxide contents are mass percentages based on the oxide. The mass content rate of the oxide of a metal element relates to the total content of this element expressed in the most stable oxide form according to industry convention. - HfO2 is not chemically separable from ZrO2. However, according to the present invention, HfO2 is not added intentionally. HfO2 therefore refers only to the inevitable impurity of hafnium oxide, which is always naturally present in the zirconia source in a mass content generally less than 5%, generally less than 2%. For clarity, the total content of zirconium oxide and the total content of traces of hafnium oxide may be interchangeably written as "ZrO2" or "ZrO2+HfO2". - The sum of the oxide contents does not imply the presence of all these oxides. - "Comprising" is to be interpreted in an open-ended manner, in that other elements than those indicated may be present. [Brief description of the drawings]
[0013] [Figure 1] FIG. 1 is an image obtained by observing the thickness of the cut-out coated tile of Example 3 under an optical microscope before carrying out the deterioration resistance test. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0014] CMCs are traditionally articles in which ceramic fibers are tightly bound together by a ceramic matrix.
[0015] Preferably, the ceramic fibers, optionally assembled in the form of single bundles and / or assembled bundles, are selected from fibers comprising 95% by weight or more, preferably more than 97% by weight, preferably more than 98% by weight, preferably more than 99% by weight, preferably more than 99.5% by weight of oxides, carbides, nitrides, carbon, and mixtures thereof.
[0016] Preferably, the ceramic fibers, optionally assembled in the form of single bundles and / or assembled bundles, are selected from the following fibers: - Containing more than 95% by mass, preferably more than 97% by mass, preferably more than 98% by mass, preferably more than 99% by mass, preferably more than 99.5% by mass of oxides, and having a chemical analysis such that, in percentage by total oxides, SiO2 > 70% by mass, preferably SiO2 > 80% by mass, preferably SiO2 > 90% by mass, or even SiO2 > 99% by mass, - Containing more than 95% by mass, preferably more than 97% by mass, preferably more than 98% by mass, preferably more than 99% by mass, preferably more than 99.5% by mass of oxides, and having a chemical analysis such that, in percentage by total oxides, SiO2 > 45% by mass, preferably SiO2 > 50% by mass, SiO2 < 80% by mass, and an amount of iron oxide in the form of Fe2O3 such that 1% by mass < Fe2O3 < 20% by mass, and 5% by mass < Al2O3 < 25% by mass, - Containing more than 95% by mass, preferably more than 97% by mass, preferably more than 98% by mass, preferably more than 99% by mass, preferably more than 99.5% by mass of oxides, and having a chemical analysis such that, in percentage by total oxides, Al2O3 > 65% by mass, preferably Al2O3 > 70% by mass, or even Al2O3 > 80% by mass, or even Al2O3 > 90% by mass, or even Al2O3 > 95% by mass, - Containing more than 95% by mass, preferably more than 97% by mass, preferably more than 98% by mass, preferably more than 99% by mass, preferably more than 99.5% by mass of silicon carbide, - Containing more than 95% by mass, preferably more than 97% by mass, preferably more than 98% by mass, preferably more than 99% by mass, preferably more than 99.5% by mass of carbon, - And mixtures thereof.
[0017] In one embodiment, the ceramic fibers, optionally assembled in the form of single bundles and / or assembled bundles, are selected from: fibers composed of more than 95%, preferably more than 98%, preferably more than 99%, preferably substantially 100% by weight of alumina; fibers composed of more than 95%, preferably more than 98%, preferably more than 99%, preferably substantially 100% by weight of silica, preferably composed of more than 95%, preferably more than 98%, preferably more than 99%, preferably substantially 100% by weight of amorphous silica; fibers composed of more than 95%, preferably more than 98%, preferably more than 99%, preferably substantially 100% by weight of mullite; Preferably, fibers comprised of more than 99% by weight, preferably substantially 100% by weight, of mullite and corundum; fibers comprised of more than 90% by weight, preferably more than 95% by weight, preferably more than 98% by weight, preferably more than 99% by weight, preferably substantially 100% by weight, of basalt; fibers comprised of more than 95% by weight, preferably more than 98% by weight, preferably more than 99% by weight, preferably substantially 100% by weight, of glass, preferably washed; fibers comprised of more than 95% by weight, preferably more than 98% by weight, preferably more than 99% by weight, preferably substantially 100% by weight, of silicon carbide; fibers comprised of more than 95% by weight, preferably more than 98% by weight, preferably more than 99% by weight, preferably substantially 100% by weight, of carbon, and mixtures thereof.
[0018] Preferably, the CMC matrix is selected from matrices comprising more than 95% by weight, preferably more than 97% by weight, preferably more than 98% by weight, preferably more than 99% by weight, preferably more than 99.5% by weight of oxides, carbides, nitrides, sialons, and mixtures thereof.
[0019] Preferably, the CMC matrix is selected from the following matrices: - comprising more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99%, preferably more than 99.5% by weight of oxides and having a chemical analysis such that, expressed as percentages relative to the total oxides, SiO2+Al2O3+ZrO2+HfO2+MgO>70% by weight, preferably SiO2+Al2O3+ZrO2+HfO2+MgO>80% by weight, preferably SiO2+Al2O3+ZrO2+HfO2+MgO>90% by weight, preferably SiO2+Al2O3+ZrO2+HfO2+MgO>95% by weight, preferably SiO2+Al2O3+ZrO2+HfO2+MgO>98% by weight or even SiO2+Al2O3+ZrO2+HfO2+MgO>99% by weight, - comprising more than 95% by weight, preferably more than 97% by weight, preferably more than 98% by weight, preferably more than 99% by weight, preferably more than 99.5% by weight of oxides and having a chemical analysis such that, expressed as percentages relative to the total oxides, SiO2+Al2O3>70% by weight, preferably SiO2+Al2O3>80% by weight, preferably SiO2+Al2O3>90% by weight, preferably SiO2+Al2O3>95% by weight, preferably SiO2+Al2O3>98% by weight, or even SiO2+Al2O3>99% by weight, - comprising more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99%, preferably more than 99.5% by weight of oxides and having a chemical analysis such that, expressed as percentages relative to the total oxides, Al2O3+ZrO2+HfO2>70% by weight, preferably Al2O3+ZrO2+HfO2>80% by weight, preferably Al2O3+ZrO2+HfO2>90% by weight, preferably Al2O3+ZrO2+HfO2>95% by weight, preferably Al2O3+ZrO2+HfO2>98% by weight or even Al2O3+ZrO2+HfO2>99% by weight, - comprising more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99%, preferably more than 99.5% by weight of oxides and having a chemical analysis such that, expressed as percentages relative to the total oxides, SiO2+Al2O3+MgO>70% by weight, preferably SiO2+Al2O3+MgO>80% by weight, preferably SiO2+Al2O3+MgO>90% by weight, preferably SiO2+Al2O3+MgO>95% by weight, preferably SiO2+Al2O3+MgO>98% by weight or even SiO2+Al2O3+MgO>99% by weight; - containing more than 90%, preferably more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99% by weight of SiC+Si3N4+SiAlON. In one embodiment, in particular when the matrix contains more than 50%, preferably more than 60%, preferably more than 70%, preferably more than 80% by weight of SiC, the complement to SiC+Si3N4+SiAlON in said matrix comprises metallic silicon, preferably said complement consists of more than 70%, preferably more than 80%, preferably more than 90% by weight of metallic silicon.
[0020] In one embodiment, the CMC is such that the fibers of said CMC, optionally assembled in the form of single and / or assembled bundles, comprise more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99%, preferably more than 99.5% by weight of oxides, and have a chemical analysis such that, as a percentage of the total oxides, SiO2>70%, preferably SiO2>80%, preferably SiO2>90% or even SiO2>99% by weight, and the matrix of said CMC is selected from the following matrices: - comprising more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99%, preferably more than 99.5% by weight of oxides and having a chemical analysis such that, expressed as percentages relative to the total oxides, SiO2+Al2O3+ZrO2+HfO2+MgO>70% by weight, preferably SiO2+Al2O3+ZrO2+HfO2+MgO>80% by weight, preferably SiO2+Al2O3+ZrO2+HfO2+MgO>90% by weight, preferably SiO2+Al2O3+ZrO2+HfO2+MgO>95% by weight, preferably SiO2+Al2O3+ZrO2+HfO2+MgO>98% by weight or even SiO2+Al2O3+ZrO2+HfO2+MgO>99% by weight, - comprising more than 95% by weight, preferably more than 97% by weight, preferably more than 98% by weight, preferably more than 99% by weight, preferably more than 99.5% by weight of oxides and having a chemical analysis such that, expressed as percentages relative to the total oxides, SiO2+Al2O3>70% by weight, preferably SiO2+Al2O3>80% by weight, preferably SiO2+Al2O3>90% by weight, preferably SiO2+Al2O3>95% by weight, preferably SiO2+Al2O3>98% by weight, or even SiO2+Al2O3>99% by weight, - comprising more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99%, preferably more than 99.5% by weight of oxides and having a chemical analysis such that, expressed as percentages relative to the total oxides, Al2O3+ZrO2+HfO2>70% by weight, preferably Al2O3+ZrO2+HfO2>80% by weight, preferably Al2O3+ZrO2+HfO2>90% by weight, preferably Al2O3+ZrO2+HfO2>95% by weight, preferably Al2O3+ZrO2+HfO2>98% by weight or even Al2O3+ZrO2+HfO2>99% by weight, - Those having a chemical analysis that contains more than 95% by mass, preferably more than 97% by mass, preferably more than 98% by mass, preferably more than 99% by mass, preferably more than 99.5% by mass of oxides, and in percentage of total oxides, SiO2 + Al2O3 + MgO > 70% by mass, preferably SiO2 + Al2O3 + MgO > 80% by mass, preferably SiO2 + Al2O3 + MgO > 90% by mass, preferably SiO2 + Al2O3 + MgO > 95% by mass, preferably SiO2 + Al2O3 + MgO > 98% by mass, or even more preferably SiO2 + Al2O3 + MgO > 99% by mass.
[0021] In one embodiment, the CMC is optionally assembled in the form of a single bundle and / or an assembled bundle, and the fibers of the CMC contain more than 95% by mass, preferably more than 97% by mass, preferably more than 98% by mass, preferably more than 99% by mass, preferably more than 99.5% by mass of oxides, and in percentage of total oxides, SiO2 > 45% by mass, preferably SiO2 > 50% by mass, and SiO2 < 80% by mass, and an amount of iron oxide in the form of Fe2O3 such that 1% by mass < Fe2O3 < 20% by mass, and 5% by mass < Al2O3 < 25% by mass, and the matrix of the CMC is selected from the following matrices: - Those having a chemical analysis that contains more than 95% by mass, preferably more than 97% by mass, preferably more than 98% by mass, preferably more than 99% by mass, preferably more than 99.5% by mass of oxides, and in percentage of total oxides, SiO2 + Al2O3 + ZrO2 + HfO2 + MgO > 70% by mass, preferably SiO2 + Al2O3 + ZrO2 + HfO2 + MgO > 80% by mass, preferably SiO2 + Al2O3 + ZrO2 + HfO2 + MgO > 90% by mass, preferably SiO2 + Al2O3 + ZrO2 + HfO2 + MgO > 95% by mass, preferably SiO2 + Al2O3 + ZrO2 + HfO2 + MgO > 98% by mass, or even more preferably SiO2 + Al2O3 + ZrO2 + HfO2 + MgO > 99% by mass. - comprising more than 95% by weight, preferably more than 97% by weight, preferably more than 98% by weight, preferably more than 99% by weight, preferably more than 99.5% by weight of oxides and having a chemical analysis such that, expressed as percentages relative to the total oxides, SiO2+Al2O3>70% by weight, preferably SiO2+Al2O3>80% by weight, preferably SiO2+Al2O3>90% by weight, preferably SiO2+Al2O3>95% by weight, preferably SiO2+Al2O3>98% by weight, or even SiO2+Al2O3>99% by weight, - comprising more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99%, preferably more than 99.5% by weight of oxides and having a chemical analysis such that, expressed as percentages relative to the total oxides, Al2O3+ZrO2+HfO2>70% by weight, preferably Al2O3+ZrO2+HfO2>80% by weight, preferably Al2O3+ZrO2+HfO2>90% by weight, preferably Al2O3+ZrO2+HfO2>95% by weight, preferably Al2O3+ZrO2+HfO2>98% by weight or even Al2O3+ZrO2+HfO2>99% by weight, - comprising more than 95% by weight, preferably more than 97% by weight, preferably more than 98% by weight, preferably more than 99% by weight, preferably more than 99.5% by weight of oxides and having a chemical analysis such that, expressed as percentages relative to the total oxides, SiO2+Al2O3+MgO>70% by weight, preferably SiO2+Al2O3+MgO>80% by weight, preferably SiO2+Al2O3+MgO>90% by weight, preferably SiO2+Al2O3+MgO>95% by weight, preferably SiO2+Al2O3+MgO>98% by weight, or even SiO2+Al2O3+MgO>99% by weight.
[0022] In one embodiment, the CMC is such that the fibres of said CMC, optionally assembled in the form of single and / or assembled bundles, comprise more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99%, preferably more than 99.5% by weight of oxides, with a chemical analysis such that, as a percentage of the total oxides, Al2O3>65%, preferably Al2O3>70%, or even Al2O3>80%, or even Al2O3>90%, or even Al2O3>95% by weight, and the matrix of said CMC is selected from the following matrices: - comprising more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99%, preferably more than 99.5% by weight of oxides and having a chemical analysis such that, expressed as percentages relative to the total oxides, SiO2+Al2O3+ZrO2+HfO2+MgO>70% by weight, preferably SiO2+Al2O3+ZrO2+HfO2+MgO>80% by weight, preferably SiO2+Al2O3+ZrO2+HfO2+MgO>90% by weight, preferably SiO2+Al2O3+ZrO2+HfO2+MgO>95% by weight, preferably SiO2+Al2O3+ZrO2+HfO2+MgO>98% by weight or even SiO2+Al2O3+ZrO2+HfO2+MgO>99% by weight, - comprising more than 95% by weight, preferably more than 97% by weight, preferably more than 98% by weight, preferably more than 99% by weight, preferably more than 99.5% by weight of oxides and having a chemical analysis such that, expressed as percentages relative to the total oxides, SiO2+Al2O3>70% by weight, preferably SiO2+Al2O3>80% by weight, preferably SiO2+Al2O3>90% by weight, preferably SiO2+Al2O3>95% by weight, preferably SiO2+Al2O3>98% by weight, or even SiO2+Al2O3>99% by weight, - comprising more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99%, preferably more than 99.5% by weight of oxides and having a chemical analysis such that, expressed as percentages relative to the total oxides, Al2O3+ZrO2+HfO2>70% by weight, preferably Al2O3+ZrO2+HfO2>80% by weight, preferably Al2O3+ZrO2+HfO2>90% by weight, preferably Al2O3+ZrO2+HfO2>95% by weight, preferably Al2O3+ZrO2+HfO2>98% by weight or even Al2O3+ZrO2+HfO2>99% by weight, - comprising more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99%, preferably more than 99.5% by weight of oxides and having a chemical analysis such that, expressed as percentages relative to the total oxides, SiO2+Al2O3+MgO>70% by weight, preferably SiO2+Al2O3+MgO>80% by weight, preferably SiO2+Al2O3+MgO>90% by weight, preferably SiO2+Al2O3+MgO>95% by weight, preferably SiO2+Al2O3+MgO>98% by weight or even SiO2+Al2O3+MgO>99% by weight; - those containing more than 85%, preferably more than 90%, preferably more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99% by weight of SiC+Si3N4+SiAlON. In one embodiment, in particular when the matrix contains more than 50%, preferably more than 60%, preferably more than 70%, preferably more than 80% by weight of SiC, the complement to SiC+Si3N4+SiAlON comprises metallic silicon, preferably said complement consists of more than 70%, preferably more than 80%, preferably more than 90% by weight of metallic silicon.
[0023] In one embodiment, the CMC is such that the fibers of said CMC, optionally assembled in the form of single and / or assembled bundles, comprise more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99%, preferably more than 99.5% by weight of silicon carbide and the matrix of said CMC is selected from matrices comprising more than 90%, preferably more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99% by weight of SiC+Si3N4+SiAlON. In one embodiment, especially when the matrix comprises more than 50%, preferably more than 60%, preferably more than 70%, preferably more than 80% by weight of SiC, the complement to SiC+Si3N4+SiAlON in said matrix comprises metallic silicon, preferably said complement consists of more than 70%, preferably more than 80%, preferably more than 90% by weight of metallic silicon.
[0024] In one embodiment, the CMC is such that the fibers of said CMC, optionally assembled in the form of single and / or assembled bundles, comprise more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99%, preferably more than 99.5% by weight of carbon and the matrix of said CMC is selected from matrices comprising more than 90%, preferably more than 95%, preferably more than 97%, preferably more than 98%, preferably more than 99% by weight of SiC+Si3N4+SiAlON. In one embodiment, especially when the matrix comprises more than 50%, preferably more than 60%, preferably more than 70%, preferably more than 80% by weight of SiC, the complement to SiC+Si3N4+SiAlON in said matrix comprises metallic silicon, preferably said complement consists of more than 70%, preferably more than 80%, preferably more than 90% by weight of metallic silicon.
[0025] In one embodiment, the CMC is such that the fibers of said CMC, optionally assembled in the form of single and / or assembled bundles, comprise more than 95% by weight, preferably more than 97% by weight, preferably more than 98% by weight, preferably more than 99% by weight, preferably more than 99.5% by weight of oxides, with a chemical analysis such that, as a percentage by weight of all oxides, SiO2>70%, preferably SiO2>80%, preferably SiO2>90% or even SiO2>99%, and the matrix of said CMC is selected from matrices comprising more than 90% by weight, preferably more than 95% by weight, preferably more than 97% by weight, preferably more than 98% by weight, preferably more than 99% by weight of SiC+Si3N4+SiAlON. In one embodiment, in particular when the matrix comprises more than 50% by weight, preferably more than 60% by weight, preferably more than 70% by weight, preferably more than 80% by weight of SiC, the complement to SiC+Si3N4+SiAlON in said matrix comprises metallic silicon, preferably said complement consists of more than 70% by weight, preferably more than 80% by weight, preferably more than 90% by weight of metallic silicon.
[0026] Preferably, regardless of the above-mentioned embodiment, the CMC has one or more of the following optional features: - the CMC is sintered. In one embodiment, the sintering may be performed upon first use (in other words, in situ); - the CMC has a porosity, measured by immersion according to the buoyancy principle, of more than 15%, preferably more than 20%, preferably more than 25%, preferably more than 30% and preferably less than 45%, preferably less than 40%; - the CMC comprises more than 30% by volume, preferably more than 40% by volume, preferably more than 50% by volume, preferably more than 60% by volume and / or less than 70% by volume of fibers, optionally assembled in the form of single threads and / or assembled threads; - the fibres are grouped in the form of bundles, which typically contain hundreds to thousands of fibres; - the fibres, preferably the bundles, have a length of more than 50 mm, or even more than 100 mm; In a preferred embodiment, the fibres, preferably bundles, are arranged in the form of a (non-woven) web, a knit (single mesh or reinforced with unidirectional fibres and / or bundles), a braided (with weft and warp bundles) structure or in the form of an object in which the fibres and / or bundles are laminated to one another (filament winding or ESF ("engineered speciality fabric")).
[0027] All manufacturing methods that make it possible to obtain CMC may be implemented.
[0028] The manufacturing method may in particular comprise the following steps: - impregnating, after drying and / or sintering, a set of fabrics or webs, preferably a bundle of fabrics or webs, with a slip capable of forming a matrix; laminating said fabrics and / or webs, said lamination being capable of being carried out by means of a press or under vacuum.
[0029] The fabrics or layers may be stacked so that the different fabric or layer bundles all face substantially in the same direction, or in different directions, for example at 45°, depending on the particular mechanical properties desired.
[0030] coating
[0031] The coating comprises at least one layer comprising a crystalline oxide containing at least the elements Li and Al, said oxide optionally containing preferentially Si.
[0032] Preferably, the crystalline oxide has a melting temperature higher than the maximum temperature reached during the production of lithiated powders, in particular during the production of lithiated transition metal oxide powders.
[0033] Preferably, said crystalline oxide is selected from LiAlO2, LiAlSi2O6, Li3AlSiO5, LiAlSi4O10, LiAlSiO4, and mixtures thereof, preferably from LiAlO2, Li3AlSiO5, LiAlSi2O6, and mixtures thereof. More preferably, said crystalline oxide is selected from Li3AlSiO5, LiAlSi2O6, and mixtures thereof.
[0034] The inventors have demonstrated that the desired degradation resistance can be obtained when small amounts of said crystalline oxides are present in the coating, particularly in the range of 15% to 25% by weight, and especially when using Al-free precursors of said crystalline oxides (in which case Al comes from CMC).
[0035] Preferably, the coating comprises at least two layers, at least one of said layers comprising a crystalline oxide comprising at least the elements Li and Al, such as a layer comprising Li4SiO4, preferably consisting essentially of Li4SiO4, and a layer comprising a crystalline oxide comprising at least the elements Li, Si and Al, preferably comprising the crystallized compound Li3AlSiO5.
[0036] For example, the layer comprising a compound containing at least the elements Li, Si, and Al (preferably the crystallized compound Li3AlSiO5) is located between the layer comprising a crystalline oxide containing at least the elements Li and Al (preferably a layer of Li4SiO4) and the CMC.
[0037] According to one embodiment, the coating consists of one or more crystalline oxides comprising more than 15% by weight, preferably more than 20% by weight, preferably more than 25% by weight of at least the elements Li and Al, and optionally Si.
[0038] According to one embodiment, the coating is composed of more than 30% by weight, preferably more than 40% by weight, more preferably more than 50% by weight, preferably more than 60% by weight, more preferably more than 70% by weight, preferably more than 80% by weight, more preferably more than 90% by weight, preferably more than 95% by weight, or even more preferably more than 98% by weight of one or more crystalline oxides comprising at least the elements Li and Al, and optionally Si. More preferably, the coating consists essentially of one or more crystalline oxides comprising at least the elements Li and Al, and optionally Si.
[0039] In one embodiment, the coating contains a precursor of at least one crystalline oxide comprising at least the elements Li and Al, and optionally Si, in which the at least one crystalline oxide comprising at least the elements Li and Al, and optionally Si, will be subsequently formed, such as upon first use, by increasing the temperature.
[0040] In one embodiment, at least a portion of the Al and / or at least a portion of the Si of the crystalline oxide, which comprises at least the elements Li and Al, and optionally Si, is derived from the CMC, in particular by reacting with Li by increasing the temperature, e.g., during initial use.
[0041] Preferably, the coating has the following chemical composition, expressed as a percentage of the total oxides: LiO: more than 0.5% by weight, preferably more than 1% by weight, preferably more than 2% by weight, preferably more than 3% by weight, and preferably less than 30% by weight, preferably less than 25% by weight, and / or Al2O3: more than 2% by weight, preferably more than 4% by weight, preferably more than 6% by weight, preferably more than 8% by weight, preferably more than 10% by weight, preferably more than 12% by weight and preferably less than 80% by weight, and / or SiO2: less than 5% by weight in one embodiment. In one embodiment, more than 10% by weight, preferably more than 15% by weight, preferably more than 20% by weight, preferably more than 25% by weight, preferably more than 30% by weight, and preferably less than 80% by weight, preferably less than 75% by weight, preferably less than 70% by weight; SiO2+Al2O3+Li2O is more than 50% by weight, preferably more than 60% by weight, preferably more than 70% by weight, or more than 80% by weight, or more than 90% by weight.
[0042] Preferably, the coating consists of more than 90% by weight of the oxide, preferably more than 95% by weight, preferably more than 98% by weight, preferably more than 99% by weight, preferably more than 99.5% by weight. Preferably, the coating consists essentially of the oxide.
[0043] The thickness of said coating is preferably more than 50 μm, preferably more than 100 μm (microns), preferably more than 200 μm, preferably more than 300 μm, or even more than 400 μm, or even more than 500 μm, or even more than 600 μm, and / or preferably less than 2000 μm, preferably less than 1500 μm, preferably less than 1000 μm, preferably less than 800 μm.
[0044] Preferably, the coated inner wall surface comprises the bottom of the container and the portion of the side surface in contact with said bottom, in other words the coating extends over the lower portion of the side surface of the container, the container being considered to be in its working position, said portion being in contact with powder during use of said container.
[0045] Preferably, more than 85%, preferably more than 90%, preferably more than 95%, preferably more than 96%, preferably more than 98%, preferably more than 99% of the surface of the interior wall of the container is covered (coated) with said coating. Preferably, the coating extends over substantially the entire surface of the interior wall of the container.
[0046] Preferably, at least a portion, preferably the entire surface, of the bottom outer wall of the container is covered with a coating.
[0047] In one embodiment, greater than 90%, preferably greater than 95%, more preferably greater than 99% of the total surface area of the container wall is covered with the coating.
[0048] Preferably, the coating is subjected to a heat treatment prior to its use, the maximum temperature reached during said heat treatment being preferably above 900° C., preferably above 950° C., and below the decomposition temperature of the CMC.
[0049] In the case of a CMC comprising fibers having a chemical analysis such that SiO2 > 80 wt. %, optionally assembled in the form of bundles, the maximum temperature reached during said heat treatment is preferably below 1000°C.
[0050] In the case of a CMC comprising fibres having a chemical analysis such that Al2O3>65% by weight, optionally assembled in the form of bundles, or a CMC comprising fibres comprising more than 95% by weight of silicon carbide, optionally assembled in the form of bundles, the maximum temperature reached during said heat treatment is preferably below 1300°C.
[0051] Preferably, the hold time at said maximum temperature is more than 5 hours, preferably more than 8 hours, and less than 20 hours, preferably less than 15 hours.
[0052] Carrying out a heat treatment advantageously makes it possible to improve considerably the adhesion of the coating.
[0053] Said heat treatment may also make it possible to obtain at least one crystalline oxide comprising at least the elements Li and Al present in the coating, in particular from precursors of said oxides and / or when at least part of the Al originates from the CMC.
[0054] The coating may be applied to at least a part of the surface of the inner wall of the container according to any technique known to the person skilled in the art, in particular by application with a brush, by spraying, in particular wet spraying, by vacuum impregnation.
[0055] In one variation, a precursor of the oxide is applied to at least a portion of the surface of the container wall and then converted to the oxide, for example using a heat treatment.
[0056] Preferably, the precursor of said oxide is selected from: - lithiated bayerite, - Li4SiO4, where Al in this case comes from the CMC (a crystalline oxide containing at least the elements Li and Al, and which may be Li3AlSiO5); - and mixtures thereof.
[0057] container
[0058] The container can have any shape.
[0059] The perimeter of the container according to the invention may be chosen from a polygon, in particular a rectangle and a square, a circle or an oval.
[0060] Preferably, the container according to the invention has a bottom and at least one side, the bottom and at least one side preferably having an average thickness of less than 20 mm, more preferably less than 15 mm, or even preferably less than 10 mm, and / or preferably more than 2 mm, preferably more than 4 mm, more preferably more than 5 mm.
[0061] In one embodiment, the bottom of the container has a thickness greater than the thickness of its sides, preferably more than 10% greater, more preferably more than 20%, more preferably more than 30% greater.
[0062] In one embodiment, the bottom and sides of the container have a difference in thickness of less than 10%, preferably less than 5%. Preferably, in said embodiment, the bottom of the container has substantially the same thickness as its sides.
[0063] In one embodiment, the wall thickness is not constant. Preferably, the thickness of the side is greater than the thickness at the surface of the container bottom. Preferably, the portion of the side in contact with the container bottom has a thickness that is greater than 10% of the thickness of the portion of the side located opposite the container bottom.
[0064] In one embodiment, the container according to the invention has a length, i.e. a length less than 500 mm, preferably less than 400 mm, or / and preferably more than 100 mm, preferably more than 200 mm, and a width, i.e. a width in the smallest dimension measured perpendicular to the length, less than 500 mm, preferably less than 400 mm, or / and preferably more than 100 mm, preferably more than 200 mm.
[0065] In one embodiment, the container may be partitioned into at least two parts, said at least two parts being separated by a space allowing the circulation of gas during the heat treatment aimed at synthesizing a powder comprising lithium oxide, in particular an oxide of a metal or oxides of several lithiated transition metals.
[0066] In one embodiment, the angle between the bottom surface of the container and said at least one side surface is equal to 90°. In one embodiment, said angle is greater than 90° and less than 100°.
[0067] In one embodiment the container according to the invention has a diameter less than 500 mm, preferably less than 400 mm, and / or preferably more than 100 mm, preferably more than 200 mm.
[0068] Preferably, the container according to the invention has a volume of more than 0.1 litre, preferably more than 1 litre, preferably more than 2 litres, preferably more than 3 litres and / or preferably less than 25 litres, preferably less than 20 litres, preferably less than 15 litres.
[0069] In one embodiment, the CMC bottom and sides of the container according to the invention form a monolithic assembly, in other words said bottom and sides are integral and the connection between the bottom and the sides preferably has a radius of more than 5 mm, preferably more than 10 mm, preferably more than 20 mm.
[0070] In one embodiment, the container is an assembly of different parts made of CMC, for example plates made of CMC, and the connections between said different parts can be made in particular by mortise and tenon joints, and / or bracket assemblies, and / or nesting assemblies (in particular using notches or grooves), and / or metal or ceramic pins, and / or metal or ceramic screws, and / or metal or ceramic rivets, and / or metal or ceramic keys. EXAMPLES
[0071] The following non-limiting examples are given for the purpose of illustrating the present invention.
[0072] The resistance to degradation during synthesis of the metal oxide powder or the oxide powder of multiple lithiated transition metals is evaluated by the following method: 2 g of lithium hydroxide are placed in the center of the surface of each tile, with or without coating depending on the example. The assembly is then placed in an electric furnace and subjected to the following heat treatment in air: - Heat up to 900℃, - 900℃ for 10 hours, - Allow to cool to ambient temperature.
[0073] For each example, before the deterioration resistance test, the coated or uncoated tile according to the example is cut to obtain the end face of the central zone of the tile, and the end face is coated with resin and mirror-polished.The polished end face is then observed using an optical microscope before the deterioration resistance test, thereby measuring the average thickness E0 of the tile in the example, the average thickness E0 being the arithmetic mean of the thicknesses measured over five different observation zones.
[0074] For each example, after the deterioration resistance test, the coated or uncoated tiles according to the example are cut to obtain the end faces of the central zone of the tiles, which are coated with resin and mirror-polished.The polished end faces are then observed using an optical microscope, thereby measuring the average thickness E1 of the example tiles, which corresponds to the thickness of the unmodified material by visual observation, and the average thickness E1 is the arithmetic mean of the thicknesses measured over five different observation zones.
[0075] The degradation resistance of the example is defined by E0-E1, where the smaller the difference E0-E1, the higher the degradation resistance.
[0076] An example manufacturing protocol is described below:
[0077] (a) Tile used in Comparative Example 1 outside the present invention
[0078] The tiles used in Comparative Example 1 outside the invention are plates of Alundum® AH199 sold by Saint-Gobain Performance Ceramics and Refractories, with the following dimensions: 50x50x11 mm. 3 .
[0079] (b) Tiles used in Comparative Example 2 outside the present invention and Example 3 according to the present invention
[0080] The tiles used in the above examples are HT-C Type SM sintered CMC tiles sold by Inovaceram, with dimensions of 50x50x4.5mm. 3 It is.
[0081] (c) Suspensions for obtaining the coatings on the coated tiles of Comparative Example 1 and Example 3
[0082] Lithium hydroxide is introduced into the water at a concentration of 0.3 mol / L and the mass is kept under stirring until the lithium hydroxide has dissolved. Ludox AS40 colloidal silica, sold by Sigma Aldrich, is then added under stirring so that the molar ratio of lithium hydroxide to SiO2 is 4.
[0083] The pH is then adjusted to 8.5 with citric acid. Stirring is maintained for 10 minutes after the introduction of the citric acid. The suspension obtained is then placed in a drying oven at 65° C. for 18 hours.
[0084] (d) Producing a coating on the surface of the tile being coated.
[0085] Coatings are obtained on Alundum® AH199 tiles and on sintered CMC tiles using the following method.
[0086] To carry out comparative example 1, the suspension obtained at the end of paragraph (c) is applied by means of a brush to the tile described in paragraph (a).
[0087] To carry out Example 3, the suspension obtained in paragraph (c) is applied by means of a brush to one of the tiles described in paragraph (b).
[0088] Then, after drying at 60° C. for 12 hours, the dried coated tiles are subjected to the following heat treatment HT in an electric furnace: - Heat from 20°C to 900°C at a rate of 10°C / min. - 900℃ for 10 hours, - Allow to cool naturally to room temperature.
[0089] Attached Figure 1 shows an image obtained when observing under an optical microscope the thickness of a cut-out of a coated tile of Example 3, before carrying out the ageing resistance test. Two layers present on the surface of the CMC tile (1) can be distinguished: a layer of Li4SiO4 (2) and a layer containing the crystallized compound Li3AlSiO5 (3).
[0090] The tiles thus obtained are then subjected to the deterioration resistance test described above.
[0091] Table 1 below summarizes the results of the degradation resistance tests, with examples representative of containers used for the synthesis of metal oxide powders or multiple lithiated transition metal oxide powders.
[0092] [Table 1]
[0093] The presence of the crystalline oxide Li3AlSiO5 in the coating of Example 3 is demonstrated by X-ray diffraction carried out on the polished surface of the end face of this example before the degradation resistance test.
[0094] After the heat treatment HT, comparative example 1 outside the invention has a scaly coating that does not adhere to the Alundum® AH199 support plate, and therefore it was not possible to carry out a resistance test to degradation.
[0095] In contrast, Example 3 according to the present invention has a homogeneous coating without cracks on the surface. Comparison of Comparative Example 1 outside the present invention with Example 3 according to the present invention shows the necessity of CMC as a support material for the coating.
[0096] A comparison between Comparative Example 2 outside the invention and Example 3 according to the invention shows that the resistance to degradation of Example 3 is equal to 1 mm, which is much smaller than that of Comparative Example 2, which is equal to 4.5 mm.
[0097] The above examples show the advantages of the present invention and in particular of the particular choice of combination of a ceramic matrix composite with a coating thereof comprising a crystalline oxide containing at least the elements Li and Al or a precursor of said crystalline oxide.
[0098] A lower resistance to degradation was also measured when a suspension of lithiated bayerite was alternatively used to produce a coating on the CMC tile surface.
[0099] These results demonstrate the effectiveness of the container according to the present invention.
[0100] Of course, the present invention is not limited to the described embodiments, which are provided purely for illustrative purposes.
[0101] In particular, articles according to the present invention are not limited to any particular shape or size.
Claims
1. A container made of a ceramic matrix composite, wherein the surface of the interior wall of the container is at least partially, preferably 80% or more, covered with a coating having at least one layer containing a crystalline oxide or a precursor of said crystalline oxide, comprising at least the elements Li and Al.
2. The container of claim 1 , wherein the crystalline oxide further comprises elemental Si.
3. The crystalline oxide is LiAlO 2 , LiAlSi 2 O 6 , Li 3 AlSiO 5 , LiAlSi 4 O 10 , LiAlSiO 4 3. The container according to claim 1, wherein the polyisocyanate is selected from the group consisting of , , , and mixtures thereof.
4. 3. The container of claim 1 or 2, wherein the ceramic fibers of the ceramic matrix composite are optionally aggregated in the form of single bundles and / or aggregated bundles and are selected from fibers comprising greater than 95% by weight of oxides, carbides, nitrides, carbon, and mixtures thereof.
5. The ceramic fibers of the ceramic matrix composite are optionally collected in the form of single bundles and / or collected bundles, and include the following fibers: - containing more than 95% by weight of oxides, the percentage of which, relative to the total oxides, is SiO 2 Fibers having a chemical analysis that is >70% by weight, or - containing more than 95% by weight of oxides, with the percentage of all oxides being 45% by weight < SiO 2 <80% by weight of Fe 2 O 3 and 1 mass % or less of Fe is expressed in the form of 2 O 3 Iron oxide in an amount of <20% by weight and <5% by weight of Al 2 O 3 < 25% by mass of fibers, or - containing more than 95% by weight of oxides, the percentage of which, relative to the total oxides, is Al 2 O 3 Fibers having a chemical analysis of >65% by weight, or - Fibres containing more than 95% by weight of silicon carbide, or - fibres containing more than 95% by mass of carbon, - and mixtures thereof, The container of claim 4, wherein the container is selected from the group consisting of:
6. 6. The container of claim 5, wherein the ceramic fibers of the ceramic matrix composite are optionally assembled in the form of single bundles and / or assembled bundles and are selected from fibers composed of greater than 95% by weight alumina, fibers composed of greater than 95% by weight silica, fibers composed of greater than 95% by weight mullite, fibers composed of greater than 95% by weight mullite and corundum, fibers composed of greater than 90% by weight basalt, fibers composed of greater than 95% by weight glass, fibers composed of greater than 95% by weight silicon carbide, fibers composed of greater than 95% by weight carbon, and mixtures thereof.
7. 3. The container of claim 1 or 2, wherein the matrix of the ceramic matrix composite is selected from matrices comprising more than 95% by weight of oxides, carbides, nitrides, sialons, and mixtures thereof.
8. The matrix of the ceramic matrix composite is a matrix of: - containing more than 95% by weight of oxides, the percentage of which, relative to the total oxides, is SiO 2 +Al 2 O 3 + ZrO 2 +HfO 2 + a matrix having a chemical analysis in which MgO > 70% by weight, or - containing more than 95% by weight of oxides, the percentage of which, relative to the total oxides, is SiO 2 +Al 2 O 3 a matrix having a chemical analysis of greater than >70% by weight; or - containing more than 95% by weight of oxides, the percentage of which, relative to the total oxides, is Al 2 O 3 + ZrO 2 +HfO 2 a matrix having a chemical analysis of >70% by weight; or - containing more than 95% by weight of oxides, the percentage of which, relative to the total oxides, is SiO 2 +Al 2 O 3 + a matrix having a chemical analysis in which MgO>70% by weight, or - more than 90% by weight of SiC+Si 3 N 4 + a matrix comprising SiAlON, The container of claim 7, wherein the container is selected from the group consisting of:
9. The container of claim 1 or 2, wherein the coating is: - comprises at least one layer comprising a crystalline oxide containing at least the elements Li, Al and Si; and / or - consisting of one or more crystalline oxides containing more than 15% by weight of at least the elements Li and Al; and / or - containing a precursor of at least one crystalline oxide containing at least the elements Li and Al, and / or - the following chemical composition, expressed as a percentage of the total oxides: SiO 2 +Al 2 O 3 +Li 2 O>50% by mass, and Li 2 O: more than 0.5% by mass and less than 30% by mass, and / or Al 2 O 3 : More than 2% by mass and less than 80% by mass, and / or SiO 2 : Less than 5% by mass or 10% by mass or more of SiO 2 <80% by mass, and / or - consists of more than 90% by weight of oxides, and / or - have a thickness greater than 50 μm and / or less than 2000 μm, container.
10. The precursor of a crystalline oxide containing at least the elements Li and Al is: - lithiated bayerite, - Li 4 SiO 4 , - and mixtures thereof, The container of claim 9, wherein the container is selected from the group consisting of:
11. 3. The container of claim 1 or 2, wherein greater than 99% of the surface of the interior wall is covered by the coating.
12. 3. The container of claim 1 or 2, having a bottom and at least one side.
13. 3. Use of a container according to claim 1 or 2 for the production of lithium-containing oxide powders, in particular metal oxides or oxides of several lithiated transition metals.