Surface-activated solid electrolyte particles

WO2026180476A1PCT designated stage Publication Date: 2026-09-03SCHOTT AG
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Application Number
PCT/EP2026/055047
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2025-02-28
Filing Date
2026-02-25
Publication Date
2026-09-03

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Abstract

The present disclosure relates to a powder whose particles have a core made of an ion-conducting material and a carbon-containing surface layer. The disclosure also relates to a method for producing the powder and to a hybrid electrolyte comprising the powder. The disclosure also relates to the use of the hybrid electrolyte, in particular in a separator, an anode, a cathode, a battery and / or a rechargeable battery.
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Description

[0001] February 25, 2026

[0002] 1

[0003] Surface-activated solid electrolyte particles

[0004] The present disclosure relates to powders whose particles have a core made of an ion-conducting material and a carbon-containing surface layer. The disclosure also relates to a process for producing the powder and to a hybrid electrolyte comprising the powder. The disclosure also relates to the use of the hybrid electrolyte, in particular in a separator, an anode, a cathode, a battery, and / or an accumulator.

[0005] The subject of the disclosure is the provision of solid electrolyte particles whose surface is specially activated or functionalized / modified during comminution by means of a wet milling process, so that there is a high chemical compatibility with the polymer electrolyte component with which the corresponding solid electrolyte particles are processed together to form a hybrid electrolyte, and that as a result there is a high potential for low contact resistances to form between the polymeric and (glass-)ceramic component of the resulting hybrid electrolyte.

[0006] Furthermore, the hybrid electrolyte itself is the subject of the disclosure, as well as solid-state battery cells for whose components corresponding hybrid electrolytes are used in their manufacture.

[0007] Furthermore, the wet milling process is the subject of the invention, which leads to an advantageous activation or modification of the comminuted solid electrolyte particles in such a way that there is a high chemical compatibility with the polymer electrolyte component with which the corresponding solid electrolyte particles are processed together to form a hybrid electrolyte, and that as a result there is a high potential for low contact resistances to form between the polymeric and (glass-)ceramic components of the resulting hybrid electrolyte.

[0008] Technical background

[0009] Hybrid electrolytes, in the form of a combination of a polymer electrolyte and (glass-)ceramic solid electrolyte particles, represent an attractive option among solid electrolytes because they combine the advantages of the individual components. With regard to the polymer electrolytes, these advantages include, above all, ease of processing in industrial processes, while with regard to the (glass-)ceramic solid electrolytes, they offer significantly higher ionic conductivity and considerably better mechanical stability at elevated operating temperatures compared to polymer electrolytes. 25.02.2026

[0010] 2

[0011] Hybrid electrolytes, which serve as the basis for the membrane to separate the electrodes in a solid-state battery cell, are ideally designed to be as thin as possible, especially with thicknesses of less than 20 pm, since they themselves have no storage function and therefore do not actively contribute to the storage density of the cell.

[0012] Accordingly, the (glass-)ceramic solid electrolyte particles integrated into the hybrid electrolytes should have diameters in the lower single-digit pm range, or better yet in the sub-pm to nanometer range.

[0013] Solid electrolyte particles of this size can, in principle, be produced using bottom-up or top-down processes, with the latter generally being preferred due to production scalability and manufacturing costs. Within such a process chain, intermediate bulk materials are generated as semi-finished products. In a final comminution step (milling), these semi-finished products are ground into the final solid electrolyte powder, which is then combined with the polymer electrolyte to form the actual hybrid electrolyte. Depending on the desired particle size, the milling can be carried out using either dry or wet methods.

[0014] A particular challenge in ensuring good performance of hybrid electrolytes is the fact that the contact resistance between the polymeric and (glass-)ceramic solid electrolyte components must be sufficiently low so that ion conduction occurs not only through the polymer electrolyte matrix, but also through the (glass-)ceramic solid electrolyte particles.

[0015] Accordingly, it is advantageous if the surface of the (glass-)ceramic solid electrolyte particles is activated in a suitable manner.

[0016] The literature describes how activation of (glass) ceramic particles can be achieved particularly when grinding is carried out using wet methods. For this purpose, water or organic solvents can be used as the grinding medium. Alcohols, for example, are frequently used as grinding media. These do not lead to activation or modification of the particle surfaces as described in this disclosure. Rather, the activation described in the literature can be advantageous for the grinding process itself: Compared to dry grinding methods, the grinding progress can be faster and more extensive, meaning that smaller particle sizes can be achieved using wet methods. Furthermore, significantly narrower particle size distributions are generally obtained in this way.

[0017] The prior art also describes how surface activation can be achieved by 25.02.2026

[0018] 3

[0019] The presence of particles during a wet milling process can favorably influence the processability of corresponding powders in subsequent process steps such as flotation.

[0020] However, in the prior art, a relatively high interfacial resistance results when appropriately manufactured particles are used as a (glass-)ceramic solid electrolyte component in hybrid electrolytes for solid-state batteries. This is because the chemical character of prior art powders is not explicitly adapted to that of the polymer component of the subsequent hybrid electrolyte, and there is insufficient chemical compatibility between the two phases or at their interface. This increases the activation energy for charge transfer across the interface, thus kinetically hindering charge transport, which ultimately results in increased interfacial resistance.

[0021] Task and solution

[0022] Against this background, one of the tasks of the present disclosure is to overcome the disadvantages of the prior art.

[0023] The purpose of the disclosure is in particular the activation of (glass-)ceramic ion-conducting particles in such a way that in a hybrid electrolyte, in which the (glass-)ceramic ion-conducting particles are incorporated as a dispersed phase into an ion-conducting polymer electrolyte matrix functioning as a continuous phase, there is an improved chemical compatibility of the surfaces of the (glass-)ceramic solid electrolyte particles with the polymer electrolyte matrix.

[0024] In this way, the prerequisite should be created that the contact resistance between the (glass-)ceramic and polymeric solid electrolyte phase can be reduced to such an extent that the ion conduction takes place not only through the polymer electrolyte matrix, but also through the (glass-)ceramic solid electrolyte particles, and accordingly the ion conductivity of the hybrid electrolyte is not reduced compared to that of the pure polymer electrolyte.

[0025] The problem can be solved in particular by activating the surfaces of the (glass-)ceramic solid electrolyte particles by grinding the (glass-)ceramic solid electrolyte particles using a wet process in a liquid medium whose chemical character is very close to that of the polymer electrolyte matrix or which exhibits a high tendency to react with the polymer matrix. 25.02.2026

[0026] 4

[0027] Activation of the surfaces of the (glass-)ceramic solid electrolyte particles means that, after milling (even after a subsequent washing step with a suitable solvent), at least one monolayer of the milling medium molecules remains on the particle surface. Alternatively, after processing the powder, a layer consisting of several monolayers of molecules from the milling medium remains on the particle surface, forming a corresponding shell composed of the organic material.

[0028] Ideally, during grinding, the molecules of the grinding medium bind chemically to the particle surface, that is, through the formation of a covalent bond during a reaction (for example, esterification or anhydride formation). At a minimum, however, the binding occurs via a physical pathway, that is, through the formation of electrostatic, polar, or at least strong van der Waals interactions between certain chemical groups present in the molecules of the grinding medium and chemical groups located on the surface of the (glass-)ceramic solid electrolyte particles that are particularly suitable for such an interaction.

[0029] The binding of the grinding medium molecules leads to a change in the chemical composition of the surface of the (glass-)ceramic solid electrolyte particles. This change, in the sense of activation, is particularly advantageous in cases where the newly created chemical character of the solid electrolyte particle surface is either (1) chemically similar to the polymer component of the hybrid electrolyte into which the activated solid electrolyte particles are subsequently incorporated, or (2) is a potential starting point for a chemical reaction with functional groups present in the polymer component. The reactivity varies in each individual case and must be specifically evaluated by a person skilled in the art.In both cases, good bonding of the solid electrolyte particles to the polymer electrolyte component can be expected, which consequently creates the prerequisite for a significant reduction in contact resistance compared to solid electrolyte particles whose surface was not activated.

[0030] The chemical similarity between activated solid electrolyte particles, i.e., the molecules of the grinding medium bound to the particle surface and the polymer component of the subsequent hybrid electrolyte, can be defined or (quantitatively) characterized in three ways:

[0031] 1. The monomer units of the molecules from the milling medium and the polymer component are identical or differ in the presence or absence of a CH or CH2 unit within the polymer backbone and / or a CH, CH2 or CHs unit in 25.02.2026

[0032] 5

[0033] the polymer side chains (if they exist).

[0034] 2. The distance R a The Hansen solubility parameter of surface-activated solid electrolyte particles and grinding medium is significantly reduced compared to that of non-activated solid electrolyte particles, i.e., reduced to at least 95%, preferably to at least 90%. The quotient of the distance R ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a 2. The Hansen solubility parameter of particles from the ion-conducting material that do not have the carbon-containing surface layer, relative to those of the grinding medium, is therefore at most 0.95 (= 95%).

[0035] 3. The sedimentation rate of the activated solid electrolyte particles in polymer-analogous solvents, particularly in the milling medium, is reduced by at least 10% compared to that of non-activated solid electrolyte particles. Polymer-analogous solvents are defined as short-chain solvents whose backbone consists of one or more monomer units that are identical to, or differ from, the monomer unit of the backbone of the polymer component of the hybrid electrolyte to be formulated later by the presence or absence of a CH or CH2 unit. Furthermore, the end and side groups of the molecules of the polymer-analogous solvent may each contain one more or fewer CH, CH2, or CHs group.

[0036] The problems are solved by the subject matter of the patent claims.

[0037] Summary of Revelation

[0038] In a first aspect, the disclosure relates to a powder, in particular a powder according to the third, fourth and / or fifth aspect, the particles of which have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material and wherein the silicon content of the surface layer is at most 5.0 pmol / m² 2 The silicon content of the surface layer can be derived, for example, from the chemically determined Si content of the powder and / or from the results of a BET measurement of the specific surface area.

[0039] In a second aspect, the disclosure relates to a process for producing a powder, in particular a powder according to the first, third, fourth and / or fifth aspect, comprising the following step: 25.02.2026

[0040] 6

[0041] • Grinding of an ion-conducting material in a liquid grinding medium, wherein the grinding medium is a first organic solvent.

[0042] In a third aspect, the disclosure relates to a powder produced or producible according to the process of the second aspect, in particular a powder according to the first, fourth and / or fifth aspect, wherein the quotient of the distance R ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a 2. The Hansen solubility parameter of particles from the ion-conducting material that do not have the carbon-containing surface layer is at most 0.95 relative to that of the grinding medium.

[0043] In a fourth aspect, the disclosure relates to a powder produced or producible according to the process of the second aspect, in particular a powder according to the first, third and / or fifth aspect, wherein the quotient of the sedimentation rate of the powder particles normalized to the particle size and the sedimentation rate of particles from the ion-conducting material that do not have the carbon-containing surface layer in the liquid milling medium is at most 0.90.

[0044] In a fifth aspect, the disclosure relates to a powder produced or producible according to the process of the second aspect, in particular a powder according to the first, third and / or fourth aspect, wherein the relative energy difference (RED) between the powder particles and the grinding medium is defined as the quotient of the distance R aiThe Hansen solubility parameter of the powder particles to that of the grinding medium and the radius Ro of the Hansen sphere spanned by the powder particles is at most 1.00.

[0045] In a sixth aspect, the disclosure relates to a hybrid electrolyte comprising at least one polymer electrolyte and the powder according to the first, third, fourth and / or fifth aspect.

[0046] In a seventh aspect, the disclosure relates to the use of the hybrid electrolyte of the sixth aspect in a separator, an anode, a cathode, a battery and / or a rechargeable battery.

[0047] Detailed description of the revelation

[0048] powder

[0049] The present disclosure relates in particular to a powder whose particles have a core made of an ion-conducting material and a carbon-containing surface layer, wherein 25.02.2026

[0050] 7

[0051] the surface layer is covalently bonded to the ion-conducting material and the silicon content of the surface layer is at most 5.0 pmol / m 2 The powder can be produced or producible, in particular, according to the process described in the second aspect. In some embodiments, the quotient of the distance R is ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a2. The Hansen solubility parameters of particles from the ion-conducting material that do not have the carbon-containing surface layer, relative to those of the grinding medium, are at most 0.95. In some embodiments, the quotient of the sedimentation velocity of the powder particles, normalized to particle size, and the sedimentation velocity of particles from the ion-conducting material that do not have the carbon-containing surface layer, normalized to particle size, in the liquid grinding medium is at most 0.90. In some embodiments, the relative energy difference (RED) between the powder particles and the grinding medium, defined as the quotient of the distance R, is at most 0.90. ai The Hansen solubility parameter of the powder particles to that of the grinding medium and the radius Ro of the Hansen sphere spanned by the powder particles is at most 1.00.

[0052] The calculation of the weight ratio between the core and the surface layer is explained using the following example: If a milling of LATP (density: 2.9 g / cm³) 3 ) in dipropylene glycol monomethyl ether (DPM; molecular formula: C7H16O3; molar mass: 148.2 g / mol, density: 0.95 g / cm³ 3If a particle size distribution (DPM) is carried out to a target fineness of d50 = 1.1 pm (corresponding to a specific surface area of ​​approximately 3 m² / g) and a carbon content of 0.7% (C atomic mass = 12 g / mol) is detected in the final powder, then 100 g of powder contains 0.7 g of carbon on the particle surface, which corresponds to 0.7 g : 12 g / mol = 0.0583 mol of carbon. Since one DPM molecule contains 7 carbon atoms, there are 0.0583 mol : 7 = 0.0083 mol of DPM on the particle surface, i.e., 0.0083 mol x 148.2 g / mol = 1.235 g of DPM. 100 g of powder therefore consist of 1.235 g of DPM surface layer and 98.765 g of LATP core particles (since 100 g - 1.235 g = 98.765 g). In some embodiments, the particle size (particle size) is specified as a d50 value in a range of 0.01 to 10 pm, for example from 0.02 pm to 5.0 pm, from 0.05 pm to 3.0 pm, or from 0.10 pm to 1.5 pm.In some embodiments, the particle size, when specified as a d50 value, is at least 0.05 pm, for example at least 0.1 pm, at least 0.2 pm, or at least 0.5 pm. In some embodiments, the particle size, when specified as a d50 value, is at most 10 pm, for example at most 5.0 pm, at most 3.0 pm, or at most 1.5 pm.

[0053] The maximum particle size is limited for some applications, for example, when the particles are to be integrated into very thin membrane components. Furthermore, the specific surface area decreases inversely with increasing size. (25.02.2026)

[0054] 8

[0055] Particle diameters decrease, so very large particle sizes are not advantageous. The d50 value, as used in this invention, indicates that 50 wt.% of the particles have a diameter less than or equal to the specified value. According to the invention, particle size refers to the diameter of the particles. Particle sizes are measured, in particular, using the method of static light scattering, for example, on a particle size analyzer from CILAS, type 1064, or from 3P Instruments, type BetterSizer S3. The measurement is carried out, in particular, in water (refractive index: 1.33) as the medium and evaluated according to the Fraunhofer method. Evaluation according to the Mie method (in particular refractive index: Re = 2.12, Im = 0.1) is also possible. Preferably, the particle sizes are determined according to ISO 13320:2009-12-01.

[0056] The powder is in particular an ion-conducting powder, for example an alkali ion-conducting powder, for example a lithium ion conductor or a sodium ion conductor.

[0057] surface layer

[0058] The surface layer is covalently bonded to the ion-conducting material. This can be demonstrated by the fact that the surface layer remains on the particle surface even after washing. This can be shown, for example, using temperature-fractionated carbon phase analysis based on the TOC (total organic carbon content), which still remains on the particles after washing. The washing process is carried out as follows:

[0059] The particles in the milled slurry are sedimented by centrifugation. The liquid supernatant is then decanted, and a suitable washing solvent is added to the moist sediment remaining in the centrifuge beaker. The mixture is then slurried. Centrifugation is repeated, and the washing process is repeated twice more in the same manner. Finally, the wet sediment is reabsorbed into the solvent, and the solvent is distilled off the slurry using a rotary evaporator. The solvent is preferably an organic solvent, such as acetonitrile. However, water can also be used as a solvent.

[0060] The advantage of the covalent bond is its stability, which makes it possible to reduce the interfacial resistance between the (glass) ceramic and polymer solid electrolyte phases and thus effectively facilitate the charge transfer through the interface.

[0061] The silicon content of the surface layer is at most 5.0 pmol / m². 2 , for example, a maximum of 2.0 pmol / m³ 2 , at most 1.0 pmol / m 2 , at most 0.5 pmol / m 2 , at most 0.2 pmol / m 2 or 25.02.2026

[0062] 9

[0063] at most 0.1 pmol / m 2 Preferably, no silicon is introduced into the system at all – or at least the silicon content of the surface layer should be below the detection limit. The low or non-existent silicon content is ensured by the polymer-analogous and silicon-free solvent in which milling takes place according to the invention.

[0064] Does a powder have a specific surface area O [in m²]? 2 / g], the silicon content of the surface layer can be calculated in relation to the total mass of the particles by expressing the silicon content in "pmol / m³". 2 “with specific surface area O (in m²) 2 / g) multiplied. This results in proportions in the unit "pmol / g". Multiplying this value in turn by the molar mass of silicon (28.09 g / mol) yields the silicon content of the surface layer relative to the total mass of the particles in ppm on a weight basis (m / m).

[0065] For a powder with a specific surface area of, for example, 3 m² 2 / g and a silicon content of the surface layer of, for example, 5 pmol / m 2 , the silicon content of the surface layer, relative to the total mass of the particles, is 5 pmol / m 2 x 3 m 2 / g = 15 pmol / g or 5 pmol / m 2 x 3 m 2 / gx 28.09 g / mol » 420 ppm (m / m).

[0066] In some embodiments, the silicon content of the surface layer, based on the total mass of the particles, is at most 15 pmol / g, for example at most 10 pmol / g, at most 5.0 pmol / g, at most 2.0 pmol / g, at most 1.0 pmol / g, at most 0.5 pmol / g or at most 0.2 pmol / g.

[0067] In some embodiments, the silicon content of the surface layer is at most 500 ppm on a weight basis (m / m) relative to the total mass of the particles, for example at most 200 ppm, at most 100 ppm, at most 50 ppm, at most 20 ppm, at most 10 ppm or at most 5 ppm.

[0068] In some embodiments, the specific surface area of ​​the particles ranges from 0.1 to 300 m². 2 / g. Preferably, the specific surface area of ​​the particles is in the range of 0.1 to 50 m². 2 / g for example 0.2 to 15 m 2 / g, 0.2 to 10 m 2 / g, 0.5 to 7.5 m 2 / g or 1.0 to 5.0 m 2 / g. In some embodiments, the specific surface area of ​​the particles is at least 0.1 m². 2 / g, for example at least 0.2 m 2 / g, at least 0.5 m 2 / g or at least 1.0 m 2 / g. In some embodiments, the specific surface area of ​​the particles is at most 15 m². 2 / g, for example, a maximum of 10 m 2 / g, maximum 7.5 m 2 / g or at most 5.0 m 2 / G.

[0069] In some embodiments, the powder has a total organic carbon content (TOC) of at least 0.1 wt.%, 25.02.2026

[0070] 10

[0071] For example, at least 0.2 wt.%, at least 0.5 wt.%, or at least 1.0 wt.%. The TOC content is preferably determined by temperature-fractionated carbon phase analysis according to DIN 19539:2016-12. In some embodiments, the TOC content is in the range of 0.1 wt.% to 15 wt.%, for example, from 0.2 wt.% to 10 wt.%, from 0.5 wt.% to 7.5 wt.%, or from 1.0 wt.% to 5.0 wt.%. In some embodiments, the TOC content is at most 15 wt.%, for example, at most 10 wt.%, at most 7.5 wt.%, or at most 5.0 wt.%.

[0072] An advantage of the coating described in this disclosure is that, unlike coatings based on silanization, it can be multilayered without losing the desired coating properties. Silanization requires careful attention to depositing only a single monolayer. This is because an additional layer would have reversed orientations, with the polar head groups facing outwards. This is undesirable, as the purpose of silanization is to improve the chemical compatibility of the particles with the polymer electrolyte matrix surrounding them in the final hybrid electrolyte. The coating described in this disclosure does not have this disadvantage. Even in a multilayered structure, the desired properties are retained because there is no possibility of forming additional spheres in which silicon atoms might again be facing outwards.The more layers the coating has, the higher the TOC content of the powder. According to a preferred embodiment, particles with a double-layered coating can be provided.

[0073] In some embodiments, the carbon-containing surface layer comprises at least one polymer. The monomer units from the polymer backbone may, in particular, comprise glycol units, for example, ethylene glycol units or propylene glycol units.

[0074] In some embodiments, the carbon-containing surface layer comprises at least one oligomer.

[0075] ion-conducting material

[0076] In some embodiments, the ion-conducting material is a glassy material, a glass-ceramic material, or a ceramic material. In some embodiments, the ion-conducting material is a glass-ceramic material. In some embodiments, the ion-conducting material is a ceramic material.

[0077] In some embodiments, the ion-conducting material is an alkali-ion-conducting material, for example, lithium-ion conductors or sodium-ion conductors. According to a 25.02.2026

[0078] 11

[0079] In this embodiment, the conductivity is at least 10' 6 S / cm. Particularly good results were achieved with embodiments in which the conductivity was at least 10⁻⁵. 5 S / cm, at least 10 -4 S / cm, at least 10 -3 S / cm or at least 10 -2The values ​​are S / cm. These values ​​refer to the total conductivity, which results from the superposition of the conductivity of the grain core, which forms during the sintering process, on the one hand, and the conductivity at the grain boundaries on the other. The conductivity at the grain boundaries is typically about an order of magnitude lower than the conductivity of the corresponding grains.

[0080] The synthesis of these materials can be carried out via various methods, in particular using a solid-state reaction from a mixture of oxides, carbonates or hydroxides, via a sol-gel synthesis based on the hydrolysis and condensation of nitrates and alkoxides, with spray pyrolysis or from the gas phase or from plasma (sputtering process or CVD) or via a melting process as glass or glass-ceramic with subsequent grinding.

[0081] Lithium-ion conductors can be, in particular, oxide materials such as lithium lanthanum zirconate (LLZO), materials with a LiSICon structure such as Li2+2xZni- x GeO4 or NaSICon structures such as lithium aluminum titanium phosphate (LATP) or lithium aluminum germanium phosphate (LAGP), as well as materials with a perovskite structure, e.g., lithium lanthanum titanate, can be used. The use of hydrides such as lithium boron hydride or halide-containing compounds is also possible. As a further alternative, sulfide-based ionic conductors such as lithium phosphorus sulfide (LiPS) can be employed.

[0082] When using non-oxide materials, the chemical stability towards oxygen and / or even small amounts of H2O is often low, so that the carbon-containing surface layer according to the invention can also act as a protective layer.

[0083] In some embodiments, the ion-conducting powder comprises a material with a garnet structure, which is described by the molecular formula Li7-3x+y-zAl x My ll M3-y lll M2-z lv M z v Oi2±ö is described, where M" is one or more divalent cations, M IH one or more trivalent cations, M IV one or more tetravalent cations and M v comprises one or more five-valent cations and where x+z > 0, y < 1 and θ < 0.5.

[0084] The lithium-ion conductive material with garnet structure can, for example, comprise the following components in the specified proportions (in wt.%):

[0085] Li2O 10 - 15 %

[0086] La2O345 - 60% 25.02.2026

[0087] ZrO217 - 35%

[0088] HfO20 - 5%

[0089] SiO20 - 2%

[0090] Ta20s 0 - 15 %

[0091] Nb2O50 - 15%

[0092] AI2O3+Ga2O3 0 - 6 %

[0093] MO 0 - 10 % (MO: alkaline earth oxides and / or ZnO)

[0094] RE2O30 - 15% (RE2O30: Rare Earth Oxide)

[0095] In some embodiments, the ion-conducting powder comprises a material with a NaSICon structure, which is given by the molecular formula Li(i+ x -y) M x lll My v M 2.x -y lv (PO4)3 is described, where M IH one or more trivalent cations, M IV one or more tetravalent cations and M v comprises one or more five-valent cations and where x and y are in the range from 0 to 1, (1 + x - y) > 1.

[0096] The lithium-ion conductive material with NaSICon structure can, for example, comprise the following components in the specified proportions (in wt.%):

[0097] Li2O 2 - 12%

[0098] AI2O3>0 - 20 %

[0099] TiO2+ZrO2+GeO20 - 38%, preferably GeO2<10%

[0100] SiO20 - 15%

[0101] B2O30 - 15%

[0102] Nb2O5+Ta2O50 - 20%

[0103] P2O530 - 60%

[0104] Materials with a NaSICon structure, such as sodium zircon phosphate (NaI), are particularly suitable as sodium ion conductors. +x Zr2Si x P3- x Oi2, 0 < x < 3), sodium β-aluminate or materials with Krista II structures of the form Na x My IH (Si, M IV ) Z (P, M v ) v O( X+ 3 y +4z+5v) / 2 contains, where M HI one or more trivalent cations, M IV one or more tetravalent cations and M v comprises one or more pentavalent cations. M IH In a preferred embodiment, it contains rare earth ions.

[0105] Advantageous materials are those containing crystals with the structure Nas+q(R)(M)40i2±ö, so-called N5 materials. R stands for divalent, trivalent, tetravalent, or pentavalent ions, M stands for Si and optionally P and / or B. q denotes the sodium excess compared to the stoichiometric composition, and preferably q>0.

[0106] The composition of sodium ion conductors with NaSICon structure can be, for example, the 25.02.2026

[0107] 13

[0108] The following components, in the specified proportions (in wt.%), include: Na2O 15 - 35%

[0109] AI2O30 - 10%

[0110] B2O3 0 - 10 %

[0111] P2O5 10 - 30 %

[0112] SiO220 - 35%

[0113] MO 0 - 10 % (MO: alkaline earth oxides and / or ZnO)

[0114] The composition of sodium ion conductors with rare earth ions can, for example, include the following components in the specified proportions (in wt.%): Na2O 20 - 45%

[0115] AI2O3 0 - 10 %

[0116] B2O3 0 - 10 %

[0117] P2O5 0 - 15 %

[0118] SiO225 - 60%

[0119] RE2O3 0 - 30 %

[0120] TiO2+ZrO2+HfO20 - 20%

[0121] In analogy to the lithium-ion conductors described above, non-oxide materials, such as halides or sulfides, can also be used as sodium-ion conductors.

[0122] Surface properties

[0123] By functionalizing the ion-conducting material with the carbon-containing coating, the powder particles acquire advantageous surface properties. In particular, high chemical compatibility with the polymer electrolyte component is achieved, with which the corresponding solid electrolyte particles are processed to form a hybrid electrolyte. This, in turn, results in low contact resistances between the polymeric and (glass-)ceramic components of the resulting hybrid electrolyte.

[0124] A suitable measure for the compatibility of two substances arises from considerations of solubility. In general, solubility parameters are based on intermolecular interactions and serve to predict the compatibility of two substances. If these interactions are similar, the substances are compatible and intersoluble. This follows the intuitive principle "like dissolves like" and can also be applied to the dispersibility of particles (or pigments, especially in the paint industry) in solvents.

[0125] Hansen's solubility parameters are based on the work of Hildebrand, who developed them on February 25, 2026.

[0126] 14

[0127] Originally developed for mixtures of different organic solvents based on thermodynamic considerations, it described the solubility of a component using the enthalpy of vaporization A. vapW and scaled these to the molar volume V m He defined this quotient as the so-called cohesive energy density c:

[0128]

[0129] This value essentially indicates how much energy is required to overcome intermolecular interactions so that the molecules transition into the gas phase, and can thus be understood as the bond strength between the individual molecules. This also directly explains why two liquids with similar cohesive energy densities mix well: A defined amount of energy must be supplied when a molecule transitions into the gas phase. From a thermodynamic perspective, this energy must be compensated for by the energy released when the liquids mix. The square root of the cohesive energy density is then called the Hildebrand parameter (HP) and has the unit [5] = (J m -3 ) 1 / 2 = (MPa) 1 / 2 .

[0130] One disadvantage of the HP, however, is that the nature of the interactions, for example polar or dispersive, is not precisely defined. For this reason, Hansen divided the HP 8 into three components, resulting in the so-called Hansen solubility parameters (HSP):

[0131]

[0132] These describe dispersed interactions due to atomic London dispersion forces (5 D ), polar interactions between permanent dipoles (8 P ) at the molecular level and the hydrogen bonding contribution 8 H , which is based on the proton donor (8 HDon = acid) and -acceptor- interaction (8 HAcc = Base) according to the Bronsted concept.

[0133] The division into individual components is based on experimental data, the categorization of molecules into functional groups, and correlation equations relating to physical properties such as the refractive index or dipole moment of liquids. In recent years, the empirical data have been validated by thermodynamic statistical calculations.

[0134] The definition of the three parameters results in a three-dimensional space, the so-called Hansen space, in which each substance is defined by its Hansen solubility parameter (HSP). 25.02.2026

[0135] 15

[0136] possesses a specific coordinate.

[0137] The Hansen solubility parameters are determined using an analytical centrifuge, specifically the LUMiSizer from LUM. The procedure used is described in detail in: Sebastian Süß, Titus Sobisch, Wolfgang Peukert, Dietmar Lerche, Doris Segets: “Determination of Hansen parameters for particles: A standardized routine based on analytical centrifugation”, Advanced Powder Technology 29 (2018) 1550-1561. Deviations from the literature are as follows:

[0138] • The first deviation from the literature is that the threshold value of the integral transmission, at which the "ts (norm)" is determined, is lower than described in the literature. This is not a problem, as there is only one criterion: the threshold value must intersect all extinction curves. The lower the value, the more finely differences in the descending integral extinction curves can be resolved. Particularly in the lower region of the curves, where int. Ext. ~ 0, the fine particles are taken into account and the agglomerates are weighted less.

[0139] • Another deviation lies in the choice of the threshold value (SW) for considering the RST (norm). This is typically set to 0.5 (>0.5 good, <0.5 bad), but here it is set to 0.6. Increasing the SW allows the radius to be optimized. Ideally, this excludes dispersing media at the threshold of the sphere near Ra. The center of the sphere may therefore shift slightly.

[0140] A solubility parameter that can be particularly advantageously influenced by coating the ion-conducting particles is εp. This parameter is generally relatively high for uncoated particles and can be significantly reduced by coating, approaching the low values ​​of typical polymer electrolyte components. In some embodiments, the powder particles of the present disclosure exhibit a Hansen solubility parameter εp in a range of 1.0 to 12.5, for example, from 2.0 to 11.5, from 3.5 to 10.0, from 5.0 to 8.5, or from 6.0 to 7.5. In some embodiments, εp is... P at least 1.0, for example at least 2.0, at least 3.5, at least 5.0 or at least 6.0. In some embodiments, the value is ö P at most 12.5, for example at most 11.5, at most 10.0, at most 8.5, or at most 7.5.

[0141] compatibility

[0142] Figure 1 schematically shows the three-dimensional Hansen space with corresponding Hansen solubility parameters for two substances. Additionally, their distance R is shown. a February 25, 2026

[0143] 16

[0144] drawn, which can be calculated using the following relationship:

[0145]

[0146] The smaller the distance R a The more similar and compatible the two substances are, the greater the prefactor 4 of the dispersed fraction is supported by numerous experimental data and is based on the distinction between atomic (o D ) and molecular (8 P and ö H ) due to interactions.

[0147] Based on this, the HSPs of unknown substances can also be determined by mixing them with organic solvents of known HSP and then classifying them in the Hansen space according to their compatibility. Originally, this was only performed for solutions of two liquids, but the concept can also be applied to dispersions and thus to the compatibility between the particle surface and the solvent. For this purpose, the sedimentation behavior of the particles in different solvents is usually used as an evaluation criterion for a stable (compatible) or unstable (incompatible) dispersion.

[0148] To compare the surface properties of the coated particles of the disclosure with the surface properties of uncoated reference particles, reference particles are produced that do not have the carbon-containing surface layer of the disclosure. These reference particles, lacking the carbon-containing surface layer, are obtained via a dry milling process. The surface of the reference particles is thus characterized by the ion-conducting material itself. Therefore, the surface properties of the ion-conducting material can be compared with those of the surface layer. For this purpose, the coated particles of the disclosure and the uncoated reference particles have the same particle size for determining the respective surface properties, for example, a particle size of 2 pm when specified as a d50 value.

[0149] Sedimentation is a characteristic particle property and results from the approach of force equilibrium consisting of friction, weight, and buoyancy forces:

[0150] Friction, Weight, Buoyancy

[0151] For spherical bodies, the sedimentation velocity v is thus a function of the acceleration, expressed as multiples of the acceleration due to gravity g and the particle size r. The density difference between the continuous (solvent) and dispersed phases (particles) is also a factor. 25.02.2026

[0152] 17

[0153] Ap and the viscosity p of the solvent are included in the calculation (Stokes equation):

[0154]

[0155] It should be noted that this is based on the assumption of ideally spherical particles and is only valid for laminar flows.

[0156] For the particle sizes described in this disclosure, the settling velocity is influenced by intermolecular interactions between the continuous phase and the particle surface. If these interactions are compatible and form stable dispersions, low sedimentation velocities result, and vice versa. This allows for classification as compatible or incompatible solvents. If the high-level potential (HSP) of the solvents is known, the HSP of the particles can also be determined, and a statement can be made about their surface properties. These properties are defined as the center of a sphere in the Hansen space, which represents the boundary between compatible and incompatible solvents.

[0157] In this context, the term "low sedimentation rates" means that the measured values ​​closely approximate the ideal of the Stokes equation. If the chemical compatibility of the particle surface chemistry with that of the surrounding continuous phase is impaired, the particles tend to form agglomerates to a certain extent due to increased interparticle interaction. These agglomerates are naturally larger than the primary particles present in a good dispersion and therefore sediment more quickly.

[0158] The sedimentation rate and Hansen solubility parameters of coated and uncoated particles are determined using an analytical centrifuge, specifically the LUMiSizer from LUM. The procedure used is described in detail in: Sebastian Süß, Titus Sobisch, Wolfgang Peukert, Dietmar Lerche, Doris Segets: “Determination of Hansen parameters for particles: A standardized routine based on analytical centrifugation”, Advanced Powder Technology 29 (2018) 1550-1561. The cited reference pertains to the determination of the Hansen solubility parameters (HSP), for which normalization of the sedimentation rates is not necessary, as differences between powders are only evaluated once the HSP determination is complete.

[0159] When comparing two powders from different milling processes, "a normalization of the sedimentation rate" or conversely "a normalization of the 25.02.2026

[0160] 18

[0161] The "sedimentation time" requires that the particle sizes are ideally identical or at least differ only slightly. Otherwise, the difference in sedimentation behavior measured in these powders is caused by both the degree of chemical compatibility to be determined and the differences in the size of the primary particles. In the worst case, both effects overlap to such an extent that it is no longer possible to clearly infer the chemical compatibility of the particle surface with the surrounding continuous phase.

[0162] Minor differences in particle size can also be taken into account when comparing two powders by not directly comparing the sedimentation rates, but by calculating the quotient (v / (d50)) based on the Stokes equation. A 2) is used as a key parameter. The d50 value is determined from the measurement of the size distribution of the primary particles. Practical experience has shown that the v / d50 ratio is also very useful.

[0163] In some embodiments, the quotient of the sedimentation velocity of the powder particles normalized to the particle size and the sedimentation velocity of particles from the ion-conducting material that do not have the carbon-containing surface layer in the liquid grinding medium is at most 0.90, for example at most 0.75, at most 0.60, at most 0.50, or at most 0.45. In some embodiments, the quotient of the sedimentation velocity of the powder particles normalized to the particle size and the sedimentation velocity of particles from the ion-conducting material that do not have the carbon-containing surface layer in the liquid grinding medium lies in a range of 0.01 to 0.90, for example from 0.02 to 0.75, from 0.05 to 0.60, from 0.10 to 0.50, or from 0.15 to 0.45.In some embodiments, the quotient of the sedimentation velocity of the powder particles normalized to the particle size and the sedimentation velocity of particles from the ion-conducting material that do not have the carbon-containing surface layer in the liquid grinding medium is at least 0.01, for example at least 0.02, at least 0.05, at least 0.10, or at least 0.15.

[0164] In some embodiments, the quotient of the distance R is ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a 2. The Hansen solubility parameter of particles from the ion-conducting material that do not have the carbon-containing surface layer is at most 0.95 relative to that of the grinding medium, for example, at most 0.90 or at most 0.85. In some embodiments, the 25.02.2026

[0165] 19

[0166] Quotient of the distance R ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a 2. The Hansen solubility parameter of particles from the ion-conducting material, which do not have the carbon-containing surface layer, to that of the grinding medium is in a range of 0.50 to 0.95, for example from 0.65 to 0.90 or from 0.75 to 0.85. In some embodiments, the quotient of the distance R is ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a2 The Hansen solubility parameter of particles from the ion-conducting material that do not have the carbon-containing surface layer is at least 0.50 relative to that of the grinding medium, for example at least 0.65 or at least 0.75.

[0167] In some embodiments, the quotient is the absolute value of the difference of the ö P-Values ​​of the powder particles and the grinding medium and the amount of the difference of the ö P -Values ​​of particles from the ion-conducting material, which do not have the carbon-containing surface layer, and the grinding medium in a range of 0.05 to 0.75, for example from 0.10 to 0.50, from 0.15 to 0.35, or from 0.20 to 0.27. In some embodiments, the quotient of the magnitude of the difference of the ö P -Values ​​of the powder particles and the grinding medium and the amount of the difference of the ö P - Values ​​of particles from the ion-conducting material that do not have the carbon-containing surface layer and the grinding medium at least 0.05, for example at least 0.10, at least 0.15, or at least 0.20. In some embodiments, the quotient of the magnitude of the difference is P -Values ​​of the powder particles and the grinding medium and the amount of the difference of the ö P- Values ​​of particles from the ion-conducting material that do not have the carbon-containing surface layer and the grinding medium not more than 0.75, for example not more than 0.50, not more than 0.35, or not more than 0.27.

[0168] The relative energy difference (RED) is defined as the quotient of the distance R a the HSP of the powder particles to those of a solvent and the radius Ro of the Hansen sphere spanned by the powder particles,

[0169] RED = R a / R0

[0170] and serves as a quick indicator of compatibility. A RED value of ≤ 1 indicates very good compatibility. However, if the RED value is close to 1, the particles and surrounding matrix are only conditionally compatible. A RED value of ≤ 1 indicates no compatibility between the particles and the solvent. Ro is determined using the HSPiP software. The cited reference uses the same method. Ro represents the maximum Ra value, which is the outermost "good" solvent from the center. 25.02.2026

[0171] 20

[0172] In some embodiments, the relative energy difference RED between the powder particles and the grinding medium is defined as the quotient of the distance R. aiThe Hansen solubility parameter of the powder particles to that of the grinding medium and the radius Ro of the Hansen sphere spanned by the powder particles is at most 1.00, for example at most 0.75, at most 0.50, or at most 0.25. In some embodiments, the relative energy difference RED between the powder particles and the grinding medium is defined as the quotient of the distance R ai the Hansen solubility parameter of the powder particles to that of the grinding medium and the radius R o the Hansen sphere spanned by the powder particles in a range of 0.01 to 1.00, for example from 0.02 to 0.75, from 0.05 to 0.50, or from 0.10 to 0.25. In some embodiments, the relative energy difference RED between the powder particles and the grinding medium is defined as the quotient of the distance R aiThe Hansen solubility parameter of the powder particles to that of the grinding medium and the radius Ro of the Hansen sphere spanned by the powder particles must be at least 0.01, for example at least 0.02, at least 0.05, or at least 0.10.

[0173] Production

[0174] In one aspect, the disclosure relates to a process for producing a powder, in particular a powder according to the first, third, fourth and / or fifth aspect, comprising the following step:

[0175] • Grinding of an ion-conducting material in a liquid grinding medium, wherein the grinding medium is a first organic solvent.

[0176] In some embodiments, a dispersion of particles of the ion-conducting material and the grinding medium is produced before grinding. This can be done, for example, using a dissolver. Such a dispersion can also be referred to as a grinding slurry.

[0177] Before milling, the particles of the ion-conducting material have a particle size d50 in the range of >5 pm to 100 pm, for example, from 10 to 85 pm, from 15 to 75 pm, or from 25 to 65 pm. In some embodiments, the particle size d50 is greater than 5 pm, for example, at least 10 pm, at least 15 pm, or at least 25 pm. In some embodiments, the particle size d50 is at most 100 pm, for example, at most 85 pm, at most 75 pm, or at most 65 pm.

[0178] In some embodiments, the weight ratio of the grinding medium to the ion-conducting material is in a range of 1.0 to 10, for example from 1.1 to 8.0, from 1.3 to 6.0, 25.02.2026

[0179] 21

[0180] from 1.5 to 5.0, or from 1.7 to 4.5. In some embodiments, the weight ratio of the grinding medium to the ion-conducting material is at least 1.0, for example at least 1.1, at least 1.3, at least 1.5, or at least 1.7. In some embodiments, the weight ratio of the grinding medium to the ion-conducting material is at most 10, for example at most 8.0, at most 6.0, at most 5.0, or at most 4.5.

[0181] Grinding can be carried out, in particular, using grinding balls. These grinding balls can, for example, be made of ZrO2.

[0182] In some embodiments, grinding takes place in a grinding chamber containing the grinding balls (grinding media) and the grinding slurry. The grinding slurry, in turn, contains the particles to be ground and the grinding medium, or consists of the particles to be ground and the grinding medium. In some embodiments, the grinding slurry is pumped through the grinding chamber in a closed loop, intermittently, and in a pendulum motion. In some embodiments, grinding takes place in a stirred ball mill, for example, in a Netzsch Zeta-type stirred ball mill.

[0183] Although the agitator also requires space to set the grinding balls in motion, it has no significant impact on the filling volume of the grinding chamber compared to the grinding balls and the grinding slurry. The volume of the grinding chamber is therefore essentially filled by the grinding balls and the grinding slurry. The sum of the filling volume of the grinding balls and the filling volume of the grinding slurry can, for example, be at least 95 vol% of the volume of the grinding chamber, and in particular at least 98 vol%, at least 99 vol%, at least 99.9 vol%, or substantially 100 vol%.

[0184] In some embodiments, the grinding balls fill 60 to 95 vol% of the grinding chamber, for example, 70 to 90 vol% or 75 to 85 vol%. In some embodiments, the grinding balls fill at least 60 vol% of the grinding chamber, for example, at least 70 vol% or at least 75 vol%. In some embodiments, the grinding balls fill at most 95 vol% of the grinding chamber, for example, at most 90 vol% or at most 85 vol%.

[0185] In some embodiments, the grinding slurry fills 5 to 40 vol% of the grinding chamber, for example, 10 to 30 vol% or 15 to 25 vol%. In some embodiments, the grinding slurry fills at least 5 vol% of the grinding chamber, for example, at least 10 vol% or at least 15 vol%. In some embodiments, the grinding slurry fills at most 40 vol% of the grinding chamber, for example, at most 30 vol% or at most 25 vol%. 25.02.2026

[0186] 22

[0187] In some embodiments, the ratio of the volume fractions of grinding balls and grinding slurry in the grinding chamber is in the range of 1.2 to 20, for example, 1.5 to 15, 2.0 to 10, 2.5 to 7.5, or 3.0 to 5.0. In some embodiments, the ratio of the volume fractions of grinding balls and grinding slurry in the grinding chamber is at least 1.2, for example, at least 1.5, at least 2.0, at least 2.5, or at least 3.0. In some embodiments, the ratio of the volume fractions of grinding balls and grinding slurry in the grinding chamber is at most 20, for example, at most 15, at most 10, at most 7.5, or at most 5.0. Such ratios are particularly advantageous for grinding performance and product quality.

[0188] In some embodiments, the grinding balls have a diameter in the range of 0.1 to 5.0 mm, for example, 0.2 to 2.5 mm, 0.3 to 1.5 mm, 0.4 to 1.0 mm, or 0.5 to 0.8 mm. In some embodiments, the grinding balls have a diameter of at least 0.1 mm, for example, at least 0.2 mm, at least 0.3 mm, at least 0.4 mm, or at least 0.5 mm. In some embodiments, the grinding balls have a diameter of at most 5.0 mm, for example, at most 2.5 mm, at most 1.5 mm, at most 1.0 mm, or at most 0.8 mm.

[0189] In some embodiments, grinding takes place with an agitator speed in the range of 1 to 15 m / s, for example, from 2 to 10 m / s or from 3 to 10 m / s. In some embodiments, grinding takes place with an agitator speed of at least 1 m / s, for example, at least 2 m / s or at least 3 m / s. In some embodiments, grinding takes place with an agitator speed of at most 15 m / s, for example, at most 12 m / s or at most 10 m / s. The agitator speed is the speed of the agitator at its outer circumference.

[0190] The grinding progress can be described in particular by the change in surface area per unit of time within a grinding chamber volume unit:

[0191] VMahlung — AA grinding material / (At X Viviahlraum)

[0192] The specific surface area O of the ground material is, by definition:

[0193]

[0194] The following relationship for the grinding progress is derived accordingly:

[0195] VMahlung — (mGrind X AOGrind) / (At X VGrinding Room)02 / 25 / 2026

[0196] 23

[0197] It can accordingly be described as the change over time of the specific surface area multiplied by the mass of the material being ground per unit volume of the grinding chamber.

[0198] Unabridged unit: [v Ma hiun g ] = (kg xm 2 ) / (gxhx L)

[0199] In the case of an ideally spherical particle with diameter d, the specific surface area is:

[0200] 0| <ugel — A| <ugel / mKugel — A| <ugel / (p X V|<ugel)

[0201] = (7T d 2 ) / [px (K d 3 / 6)] =

[0202] = 6 / (pxd)

[0203] This means that specific surface area and particle diameter are inversely proportional to each other. Accordingly, the dso value of the size distribution of a particle collective is inversely proportional to its specific surface area, i.e., the following holds true:

[0204] OMahlgut ~ 1 / dso

[0205] Thus, the grinding progress can be formulated as follows:

[0206] V grinding ~~ [mgrind XA(1 / dso)] / (At X V grinding room)

[0207] The grinding progress can alternatively be described as the change over time of the material mass-weighted, reciprocal d50 value per unit of grinding chamber volume.

[0208] Unabbreviated unit: [VMahiung] = kg / (pm x h x L)

[0209] This parameter is independent of density and therefore particularly well suited for evaluating the grindability of different materials or process parameters.

[0210] In some embodiments, the change over time of the specific surface area multiplied by the mass of the material being ground within a grinding chamber volume unit is in a range of 0.002 to 25 (kg x m²). 2 ) / (g x h x L), for example from 0.005 to 20 (kg x m³) 2 ) / (g x h x L), from 0.008 to 18 (kg x m³) 2 ) / (g x h x L). In some embodiments, the change over time of the specific surface area multiplied by the mass of the material being ground within a unit volume of the grinding chamber is at least 0.002 (kg x m³). 2 ) / (gxhx L), for example at least

[0211] 0.005 (kg xm 2 ) / (g x h x L) or at least 0.008 (kg x m 2 ) / (gxhx L). In some embodiments, the change in specific surface area over time multiplied by the 25.02.2026

[0212] 24

[0213] Maximum mass of material ground per unit of grinding chamber volume: 25 kg x m³ 2) / (g x h x L), for example, at most 20 (kg x m³) 2 ) / (g x h x L) or at most 18 (kg x m 2 ) / (gxhx L).

[0214] In some embodiments, the time-dependent change of the material mass-weighted, reciprocal dso value of the particle size distribution per unit grinding chamber volume ranges from 0.0015 to 18 kg / (pm xh x L), for example, from 0.004 to 15 kg / (pm xh x L) or from 0.006 to 12 kg / (pm xh x L). In some embodiments, the time-dependent change of the material mass-weighted, reciprocal d5o value of the particle size distribution per unit grinding chamber volume is at least 0.0015 kg / (pm xh x L), for example, at least

[0215] 0.004 kg / (pm xh x L) or at least 0.006 kg / (pm xh x L). In some embodiments, the time-dependent change of the material mass-weighted, reciprocal d50 value of the particle size distribution per unit of grinding chamber volume is at most 18 kg / (pm xh x L), for example at most 15 kg / (pm xh x L) or at most 12 kg / (pm xh x L).

[0216] In some embodiments, the grinding medium is an ether, in particular a glycol monomethyl ether, for example dipropylene glycol monomethyl ether, triethylene glycol monomethyl ether or ethylene glycol monomethyl ether.

[0217] In some embodiments, the process after milling comprises one or more washing steps, for example two, three, four, or five washing steps. In some embodiments, the powder is washed with a second organic solvent, for example with a dipolar aprotic solvent, in particular with acetonitrile.

[0218] In some embodiments, the process additionally includes the step of drying the ground and optionally washed powder, particularly as a final process step.

[0219] Hybrid electrolyte

[0220] The disclosure also relates to a hybrid electrolyte comprising at least one polymer electrolyte and the powder according to the first, third, fourth and / or fifth aspect.

[0221] In some embodiments, the relative energy difference between the powder particles and a polymer-analogous solvent is defined as the quotient of the distance R. a 3. The Hansen solubility parameters of the powder particles relative to those of the polymer-analogous solvent and the radius R o the Hansen sphere spanned by the powder particles at most 1.00, for example at most 0.75, at most 0.50, or at most 0.25. 25.02.2026

[0222] 25

[0223] Polymer-analogous solvents are short-chain solvents whose backbone consists of one or more monomer units that are identical to, or differ from, the monomer unit of the polymer electrolyte backbone by the presence or absence of a CH or CH2 unit, wherein the end and side groups of the polymer-analogous solvent each contain at most one more or fewer CH, CH2, or CHs group compared to the end and side groups of the polymer electrolyte. "Short-chain" solvents are those polymer-analogous solvents whose backbone has at most 10 monomer units, in particular at most 8 or at most 7 monomer units.If the number of monomer units is too high, the substances become solid or waxy, or at least exhibit a comparatively high viscosity, which is disadvantageous for the use of the corresponding solvent as a medium for grinding, since in particular the shock loads necessary for the comminution process are unnecessarily dampened and the grinding progress is thus hindered.

[0224] In some embodiments, the relative energy difference between the powder particles and a polymer-analogous solvent is defined as the quotient of the distance R. a3. The Hansen solubility parameters of the powder particles relative to those of the polymer-analogous solvent and the radius Ro of the Hansen sphere spanned by the powder particles in a range of 0.01 to 1.00, for example, from 0.01 to 0.75, from 0.01 to 0.50, from 0.01 to 0.25, from 0.02 to 1.00, from 0.02 to 0.75, from 0.02 to 0.50, from 0.02 to 0.25, from 0.05 to 1.00, from 0.05 to 0.75, from 0.05 to 0.50, from 0.05 to 0.25, from 0.10 to 1.00, from 0.10 to 0.75, from 0.10 to 0.50, or from 0.10 to 0.25. In some embodiments, the relative energy difference between the powder particles and a polymer-analogous solvent is defined as the quotient of the distance R. a 3. The Hansen solubility parameters of the powder particles relative to those of the polymer-analogous solvent and the radius Ro of the Hansen sphere spanned by the powder particles must be at least 0.01, for example at least 0.02, at least 0.05, or at least 0.10.

[0225] use

[0226] The disclosure also relates to the use of the powder and / or the hybrid electrolyte of the disclosure in a separator, an anode, a cathode, a battery and / or a rechargeable battery. The disclosure also relates to a separator, an anode, a cathode, a battery and / or a rechargeable battery containing the powder and / or the hybrid electrolyte of the disclosure.

[0227] Exemplary forms of implementation

[0228] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer. 25.02.2026

[0229] 26

[0230] exhibiting, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the silicon content of the surface layer is at most 5.0 pmol / m 2 the powder has a total organic carbon content of at least 0.1 wt.%.

[0231] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the silicon content of the surface layer is at most 5.0 pmol / m² 2 is and where the particle size, when specified as a d50 value, is in a range of 0.05 to 10 pm.

[0232] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the silicon content of the surface layer is at most 5.0 pmol / m² 2is and wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP).

[0233] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the silicon content of the surface layer is at most 5.0 pmol / m² 2 wherein the powder has a total organic carbon content of at least 0.1 wt% and wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP).

[0234] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the silicon content of the surface layer is at most 5.0 pmol / m² 2 wherein the powder has a total organic carbon content of at least 0.1 wt% and wherein the particle size, when expressed as a d50 value, is in the range of 0.05 to 10 pm.

[0235] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the silicon content of the surface layer is at most 5.0 pmol / m² 2is, where the particle size, when specified as a d50 value, is in a range of 0.05 to 10 pm and where the 25.02.2026

[0236] 27

[0237] The ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP).

[0238] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the silicon content of the surface layer is at most 5.0 pmol / m² 2 wherein the powder has a total organic carbon content of at least 0.1 wt%, wherein the particle size, when expressed as a d50 value, is in the range of 0.05 to 10 pm, and wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP).

[0239] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the powder has a total organic carbon content (TOC) of at least 0.1 wt.%.

[0240] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material and wherein the powder has a total organic carbon content of at least 0.1 wt.%.

[0241] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the silicon content of the surface layer is at most 5.0 pmol / m². 2 the powder has a total organic carbon content of at least 0.1 wt.%.

[0242] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the particle size, when specified as a d50 value, is in a range of 0.05 to 10 pm.

[0243] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material. 25.02.2026

[0244] 28

[0245] and where the particle size, when specified as a d50 value, lies in a range of 0.05 to 10 pm.

[0246] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the silicon content of the surface layer is at most 5.0 pmol / m². 2 is and where the particle size, when specified as a d50 value, is in a range of 0.05 to 10 pm.

[0247] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP).

[0248] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material and wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP).

[0249] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the silicon content of the surface layer is at most 5.0 pmol / m². 2 is and wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP).

[0250] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the powder has a total organic carbon content of at least 0.1 wt.% and wherein the particle size, when expressed as a d50 value, is in a range of 0.05 to 10 pm.

[0251] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the powder has a total organic carbon content of at least 0.1 wt.% and wherein the particle size, expressed as a d50 value, is in the range of 0.05 to 10 pm. 25.02.2026

[0252] 29

[0253] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the silicon content of the surface layer is at most 5.0 pmol / m². 2wherein the powder has a total organic carbon content of at least 0.1 wt.% and wherein the particle size, when expressed as a d50 value, is in the range of 0.05 to 10 pm.

[0254] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the particle size, when specified as a d50 value, is in a range of 0.05 to 10 pm and wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP).

[0255] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the particle size, when specified as a d50 value, is in a range of 0.05 to 10 pm, and wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP).

[0256] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the silicon content of the surface layer is at most 5.0 pmol / m². 2is, wherein the particle size, when specified as a d50 value, is in a range of 0.05 to 10 pm and wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP).

[0257] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP) and wherein the powder has a total organic carbon content of at least 0.1 wt.%.

[0258] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the ion-conducting material is lithium lanthanum zirconium oxide (LLZO) and / or 25.02.2026

[0259] 30

[0260] comprising lithium aluminum titanium phosphate (LATP) and wherein the powder has a total organic carbon content of at least 0.1 wt.%.

[0261] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the silicon content of the surface layer is at most 5.0 pmol / m². 2wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP) and wherein the powder has a total organic carbon content of at least 0.1 wt.%.

[0262] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the powder has a total organic carbon content of at least 0.1 wt.%, wherein the particle size, when expressed as a d50 value, is in the range of 0.05 to 10 pm, and wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP).

[0263] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the powder has a total organic carbon content of at least 0.1 wt.%, wherein the particle size, when expressed as a d50 value, is in the range of 0.05 to 10 pm, and wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP).

[0264] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the silicon content of the surface layer is at most 5.0 pmol / m². 2wherein the powder has a total organic carbon content of at least 0.1 wt%, wherein the particle size, when expressed as a d50 value, is in the range of 0.05 to 10 pm, and wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP).

[0265] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the powder is produced or producible in a process comprising the step of grinding the ion-conducting material in a liquid grinding medium, wherein the grinding medium is a first organic solvent, and wherein 25.02.2026

[0266] 31

[0267] • the quotient of the distance R ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a2. The Hansen solubility parameter of particles from the ion-conducting material that do not have the carbon-containing surface layer is at most 0.95 relative to that of the grinding medium.

[0268] • the quotient of the sedimentation velocity of the powder particles normalized to particle size and the sedimentation velocity of particles from the ion-conducting material that do not have the carbon-containing surface layer, normalized to particle size, in the liquid milling medium is at most 0.90, and / or

[0269] • the relative energy difference RED between the powder particles and the grinding medium is defined as the quotient of the distance R ai The Hansen solubility parameter of the powder particles to that of the grinding medium and the radius Ro of the Hansen sphere spanned by the powder particles is at most 1.00.

[0270] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the silicon content of the surface layer is at most 5.0 pmol / m² 2 is, wherein the powder is produced or producible by a process comprising the step of grinding the ion-conducting material in a liquid grinding medium, wherein the grinding medium is a first organic solvent, and wherein

[0271] • the quotient of the distance R ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a2 The Hansen solubility parameter of particles from the ion-conducting material that do not have the carbon-containing surface layer is at most 0.95 relative to that of the grinding medium.

[0272] • the quotient of the sedimentation velocity of the powder particles normalized to particle size and the sedimentation velocity of particles from the ion-conducting material that do not have the carbon-containing surface layer, normalized to particle size, in the liquid milling medium is at most 0.90, and / or 25.02.2026

[0273] 32

[0274] • the relative energy difference RED between the powder particles and the grinding medium is defined as the quotient of the distance R ai The Hansen solubility parameter of the powder particles to that of the grinding medium and the radius Ro of the Hansen sphere spanned by the powder particles is at most 1.00.

[0275] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the silicon content of the surface layer is at most 5.0 pmol / m². 2 is, wherein the powder is produced or producible by a process comprising the step of grinding the ion-conducting material in a liquid grinding medium, wherein the grinding medium is a first organic solvent, and wherein

[0276] • the quotient of the distance R ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a 2. The Hansen solubility parameter of particles from the ion-conducting material that do not have the carbon-containing surface layer is at most 0.95 relative to that of the grinding medium.

[0277] • the quotient of the sedimentation velocity of the powder particles normalized to particle size and the sedimentation velocity of particles from the ion-conducting material that do not have the carbon-containing surface layer, normalized to particle size, in the liquid milling medium is at most 0.90, and / or

[0278] • the relative energy difference RED between the powder particles and the grinding medium is defined as the quotient of the distance R ai the Hansen solubility parameter of the powder particles to that of the grinding medium and the radius R o the Hansen sphere spanned by the powder particles is at most 1.00.

[0279] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the powder is produced or producible in a process comprising the step of grinding the ion-conducting material in a liquid grinding medium, wherein the grinding medium is a first organic solvent, and wherein

[0280] the quotient of the distance R ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a 2 of the Hansen-25.02.2026

[0281] 33

[0282] The solubility parameter of particles from the ion-conducting material that do not have the carbon-containing surface layer is at most 0.95 relative to that of the grinding medium.

[0283] • the quotient of the sedimentation velocity of the powder particles normalized to particle size and the sedimentation velocity of particles from the ion-conducting material that do not have the carbon-containing surface layer, normalized to particle size, in the liquid milling medium is at most 0.90, and / or

[0284] • the relative energy difference RED between the powder particles and the grinding medium is defined as the quotient of the distance R ai The Hansen solubility parameter of the powder particles to that of the grinding medium and the radius Ro of the Hansen sphere spanned by the powder particles is at most 1.00.

[0285] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the silicon content of the surface layer is at most 5.0 pmol / m² 2 wherein the powder has a total organic carbon content of at least 0.1 wt%, wherein the powder is produced or producible by a process comprising the step of grinding the ion-conducting material in a liquid grinding medium, wherein the grinding medium is a first organic solvent, and wherein

[0286] • the quotient of the distance R ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a2The Hansen solubility parameter of particles from the ion-conducting material that do not have the carbon-containing surface layer is at most 0.95 relative to that of the grinding medium.

[0287] • the quotient of the sedimentation velocity of the powder particles normalized to particle size and the sedimentation velocity of particles from the ion-conducting material that do not have the carbon-containing surface layer, normalized to particle size, in the liquid milling medium is at most 0.90, and / or

[0288] The relative energy difference (RED) between the powder particles and the grinding medium is defined as the quotient of the distance (25.02.2026).

[0289] 34

[0290] Rai, the Hansen solubility parameter of the powder particles to that of the grinding medium, and the radius Ro of the Hansen sphere spanned by the powder particles, is at most 1.00.

[0291] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the silicon content of the surface layer is at most 5.0 pmol / m² 2 is, wherein the particle size, when specified as a d50 value, is in the range of 0.05 to 10 pm, wherein the powder is produced or producible by a process comprising the step of grinding the ion-conducting material in a liquid grinding medium, wherein the grinding medium is a first organic solvent, and wherein

[0292] • the quotient of the distance R ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a2. The Hansen solubility parameter of particles from the ion-conducting material that do not have the carbon-containing surface layer is at most 0.95 relative to that of the grinding medium.

[0293] • the quotient of the sedimentation velocity of the powder particles normalized to particle size and the sedimentation velocity of particles from the ion-conducting material that do not have the carbon-containing surface layer, normalized to particle size, in the liquid milling medium is at most 0.90, and / or

[0294] • the relative energy difference RED between the powder particles and the grinding medium is defined as the quotient of the distance R ai the Hansen solubility parameter of the powder particles to that of the grinding medium and the radius R o the Hansen sphere spanned by the powder particles is at most 1.00.

[0295] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the silicon content of the surface layer is at most 5.0 pmol / m² 2 is, wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP), wherein the powder is produced or producible by a process comprising the step of grinding the ion-conducting material in a liquid grinding medium, wherein the grinding medium is a first organic solvent, and wherein 25.02.2026

[0296] 35

[0297] • the quotient of the distance R ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a2. The Hansen solubility parameter of particles from the ion-conducting material that do not have the carbon-containing surface layer is at most 0.95 relative to that of the grinding medium.

[0298] • the quotient of the sedimentation velocity of the powder particles normalized to particle size and the sedimentation velocity of particles from the ion-conducting material that do not have the carbon-containing surface layer, normalized to particle size, in the liquid milling medium is at most 0.90, and / or

[0299] • the relative energy difference RED between the powder particles and the grinding medium is defined as the quotient of the distance R ai The Hansen solubility parameter of the powder particles to that of the grinding medium and the radius Ro of the Hansen sphere spanned by the powder particles is at most 1.00.

[0300] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the silicon content of the surface layer is at most 5.0 pmol / m² 2 wherein the powder has a total organic carbon content of at least 0.1 wt%, wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP), wherein the powder is produced or producible by a process comprising the step of grinding the ion-conducting material in a liquid grinding medium, wherein the grinding medium is a first organic solvent, and wherein

[0301] • the quotient of the distance R ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance Ra 2. The Hansen solubility parameter of particles from the ion-conducting material that do not have the carbon-containing surface layer is at most 0.95 relative to that of the grinding medium.

[0302] • the quotient of the sedimentation velocity of the powder particles normalized to particle size and the sedimentation velocity of particles from the ion-conducting material that do not have the carbon-containing surface layer, normalized to particle size, in the liquid milling medium is at most 0.90, and / or 25.02.2026

[0303] 36

[0304] • the relative energy difference RED between the powder particles and the grinding medium is defined as the quotient of the distance R ai The Hansen solubility parameter of the powder particles to that of the grinding medium and the radius Ro of the Hansen sphere spanned by the powder particles is at most 1.00.

[0305] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the silicon content of the surface layer is at most 5.0 pmol / m² 2 wherein the powder has a total organic carbon content of at least 0.1 wt%, wherein the particle size, expressed as a d50 value, is in the range of 0.05 to 10 pm, wherein the powder is produced or producible by a process comprising the step of grinding the ion-conducting material in a liquid grinding medium, wherein the grinding medium is a first organic solvent, and wherein

[0306] • the quotient of the distance R ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a2. The Hansen solubility parameter of particles from the ion-conducting material that do not have the carbon-containing surface layer is at most 0.95 relative to that of the grinding medium.

[0307] • the quotient of the sedimentation velocity of the powder particles normalized to particle size and the sedimentation velocity of particles from the ion-conducting material that do not have the carbon-containing surface layer, normalized to particle size, in the liquid milling medium is at most 0.90, and / or

[0308] • the relative energy difference RED between the powder particles and the grinding medium is defined as the quotient of the distance R ai The Hansen solubility parameter of the powder particles to that of the grinding medium and the radius Ro of the Hansen sphere spanned by the powder particles is at most 1.00.

[0309] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the silicon content of the surface layer is at most 5.0 pmol / m² 2 is, where the particle size, when specified as a d50 value, is in a range of 0.05 to 10 pm, where the ion-conducting material is lithium lanthanum zirconium oxide (LLZO) and / or 25.02.2026

[0310] 37

[0311] comprising lithium aluminum titanium phosphate (LATP), wherein the powder is produced or producible by a process comprising the step of grinding the ion-conducting material in a liquid grinding medium, wherein the grinding medium is a first organic solvent, and wherein

[0312] • the quotient of the distance R aithe Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a 2. The Hansen solubility parameter of particles from the ion-conducting material that do not have the carbon-containing surface layer is at most 0.95 relative to that of the grinding medium.

[0313] • the quotient of the sedimentation velocity of the powder particles normalized to particle size and the sedimentation velocity of particles from the ion-conducting material that do not have the carbon-containing surface layer, normalized to particle size, in the liquid milling medium is at most 0.90, and / or

[0314] • the relative energy difference RED between the powder particles and the grinding medium is defined as the quotient of the distance R aiThe Hansen solubility parameter of the powder particles to that of the grinding medium and the radius Ro of the Hansen sphere spanned by the powder particles is at most 1.00.

[0315] In some embodiments, the present disclosure relates to a powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material, wherein the silicon content of the surface layer is at most 5.0 pmol / m² 2wherein the powder has a total organic carbon content of at least 0.1 wt%, wherein the particle size, expressed as a d50 value, is in the range of 0.05 to 10 pm, wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP), wherein the powder is produced or producible by a process comprising the step of milling the ion-conducting material in a liquid milling medium, wherein the milling medium is a first organic solvent, and wherein

[0316] • the quotient of the distance R ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a 2. The Hansen solubility parameter of particles from the ion-conducting material that do not have the carbon-containing surface layer is at most 0.95 relative to that of the grinding medium, 25.02.2026

[0317] 38

[0318] • the quotient of the sedimentation velocity of the powder particles normalized to particle size and the sedimentation velocity of particles from the ion-conducting material that do not have the carbon-containing surface layer, normalized to particle size, in the liquid milling medium is at most 0.90, and / or

[0319] • the relative energy difference RED between the powder particles and the grinding medium is defined as the quotient of the distance R ai the Hansen solubility parameter of the powder particles to that of the grinding medium and the radius R o the Hansen sphere spanned by the powder particles is at most 1.00.

[0320]

[0321] Figure 1 is a schematic representation of Hansen space with the three coordinates resulting from the contributions of the Hansen solubility parameters (HSP). The HSPs of two substances and their separation Ra are shown as examples.

[0322] Figure 2 shows the results of a temperature-fractionated carbon phase analysis. The x-axis represents the temperature in °C and the y-axis represents the carbon fraction in an arbitrary unit (au).

[0323] Detailed

[0324]

[0325] Figure 1 is a schematic representation of Hansen space with the three coordinates resulting from the contributions of the Hansen solubility parameters (HSP). The HSP of two substances and their separation R are shown as examples. a drawn in. The distance R a is calculated according to:

[0326]

[0327] The smaller the distance R a The more similar and compatible the two substances are, the greater the prefactor 4 of the dispersed fraction is supported by numerous experimental data and is based on the distinction between atomic (o D) and molecular (8 P and ö H ) due to interactions.

[0328] Figure 2 shows the results of a temperature-fractionated carbon phase analysis. The x-axis represents the temperature in °C and the y-axis the carbon fraction in arbitrary units (au). A pronounced signal can be observed for the activated LATP particles ("functionalized") in the temperature range between 200 and 400 °C. (25.02.2026)

[0329] 39

[0330] The signal is detected, which leaches out at temperatures up to 600 °C and originates predominantly from organic carbon. In the case of non-activated LATP particles ("non-functionalized"), the signal does not appear in the measurement; that is, the particles do not carry any organic residues on their surface. Figure 2 also names the different carbon phases. TOO stands for "total organic carbon content," EC for "elemental carbon content," and TIC for "total inorganic carbon content."

[0331]

[0332] 1. Production and characterization of particle surface-activated lithium aluminum titanium phosphate powder

[0333] Powder production:

[0334] 110 g of coarsely pre-ground and sieved lithium aluminum titanium phosphate powder with a particle size <63 pm were dispersed in 200 g of dipropylene glycol monomethyl ether (DPM) using a dissolver, with as little agglomerate as possible.

[0335] The particles will later be incorporated into a hybrid electrolyte whose polymer electrolyte component is based on a polyethylene oxide derivative. Accordingly, the relevant monomer units of the polymer differ.

[0336]

[0337] Ethylene glycol units) and milling medium propylene glycol units) in the presence and absence of a CH2 group within the polymer backbone.

[0338] Subsequently, 1470 g of ZrO₂ grinding balls with a diameter of 0.8 mm were added to the suspension, placed in a ZrO₂ grinding chamber suitable for use on a Netzsch P075 attritor, inserted into the attritor, and ground for 3 hours using a stirring shaft with 3 eccentric discs, all components of which (eccentric discs, bushings, and cap) were made of ZrO₂ ceramic. The stirring shaft rotational speed was 1500 rpm. At the end of the grinding process, 50% of the particles in the grinding slurry had a diameter of less than 1.1 pm, 90% had a diameter of less than 2.0 pm, and 99% had a diameter of less than 2.9 pm.

[0339] Particle sizes were measured using static light scattering on a BetterSizer S3 particle size analyzer from 3P Instruments. The measurement was performed in water (refractive index: 1.33) and evaluated using the Mie method (refractive index: Re = 2.12, Im = 0.1). 25.02.2026

[0340] 40

[0341] For the purpose of powder drying, the particles in the milling slurry were sedimented by centrifugation. The liquid supernatant was then decanted, acetonitrile was added to the moist sediment remaining in the centrifuge beaker, and the mixture was slurried. Centrifugation was then repeated, and the washing process was repeated twice more in the same manner. Finally, the wet sediment was again rehydrated in acetonitrile, and the solvent was distilled off the slurry using a rotary evaporator.

[0342] Powder characterization:

[0343] To demonstrate successful activation, the activated LATP particles were subjected to temperature-fractionated carbon phase analysis, and the measurement results were compared with those obtained from non-activated LATP particles. As shown in Figure 2, a pronounced signal can be detected in the former case in the temperature range between 200 and 400 °C, which fades up to a temperature of 600 °C and originates predominantly from organic carbon. In the case of the non-activated LATP particles, the signal does not appear in the measurement; that is, the particles do not carry any organic residues on their surface.

[0344] 2. Production and characterization of particle surface-activated lithium lanthanum zirconium oxide powder

[0345] Powder production:

[0346] 0.6 kg of coarsely pre-ground and sieved lithium lanthanum zirconium oxide powder with a particle size <63 pm was dispersed in 2.4 kg of triethylene glycol monomethyl ether using a dissolver, with as little agglomerate as possible.

[0347] The particles are later to be incorporated into a hybrid electrolyte whose polymer electrolyte component is based on a polyethylene oxide derivative. Accordingly, the relevant monomer units of polymer that repeat within the polymer backbone are...

[0348]

[0349] Ethylene glycol units) and grinding medium

[0350]

[0351] Ethylene glycol units) identical.

[0352] The suspension was then milled for 3 hours using 1.6 kg of ZrC>2 grinding balls with a diameter of 0.8 mm on a Netzsch Lab-Star stirred ball mill. A grinding chamber with a volume of 0.62 L and a suitable pin agitator were used for the milling process. The agitator was operated at a speed of 2100 rpm.

[0353] At the end of the grinding process, 50% of the particles present in the grinding slurry exhibited a 25.02.2026

[0354] 41

[0355] The particle sizes measured were less than 1.0 pm in diameter, 90% less than 2.2 pm in diameter, and 99% less than 3.4 pm in diameter. Particle sizes were measured using static light scattering on a 3P Instruments BetterSizer S3 particle size analyzer. The measurement was performed in water (refractive index 1.33) and evaluated using the Mie method (refractive index Re = 2.12, Im = 0.1).

[0356] For the purpose of powder drying, the particles in the milling slurry were sedimented by centrifugation. The liquid supernatant was then decanted, acetonitrile was added to the moist sediment remaining in the centrifuge beaker, and the mixture was slurried. Centrifugation was then repeated, and the washing process was repeated twice more in the same manner. Finally, the wet sediment was again rehydrated in acetonitrile, and the solvent was distilled off the slurry using a rotary evaporator.

[0357] Powder characterization:

[0358] To demonstrate successful activation, the Hansen parameters of activated and non-activated LLZO particles were determined using a LUM LUMiSizer analytical centrifuge. The procedure used is described in detail in: Sebastian Süß, Titus Sobisch, Wolfgang Peukert, Dietmar Lerche, Doris Segets: “Determination of Hansen parameters for particles: A standardized routine based on analytical centrifugation”, Advanced Powder Technology 29 (2018) 1550-1561. Deviations from the literature were as follows:

[0359] • The first deviation from the literature was that the threshold for integral transmission, at which the determination of the “ts (norm)” takes place, is lower than described in the literature. The literature describes a threshold (= IE threshold) of 0.2, while the evaluation according to this disclosure is carried out at a threshold of 0.1.

[0360] • Another deviation lay in the choice of the threshold value (SW) for considering the RST (norm). This is typically set to 0.5 (>0.5 good, <0.5 bad), but here it was set to 0.6.

[0361] In the present example, the Hansen solubility parameters of the non-activated LLZO particles were dD = 17.2, dP = 12.9, dH = 11.4, and those of the functionalized LLZO particles were dD = 15.6, dP = 6.4, dH = 15.5. The milling medium used had the following values: dD = 16.3, dP = 7.1, dH = 10.8 (taken from the HSPiP database). Thus, the distance of the HSP25.02.2026

[0362] 42

[0363] The relative particle size of the non-activated LLZO material to the grinding medium is Ra = 6.10, while for the activated LLZO it is only Ra = 4.95, meaning it is reduced to 81% compared to the non-activated material. The difference becomes even clearer when considering the differences in the dP value: Between the non-activated LLZO particles and the grinding medium, this value is A(dP) = 5.3, while in the case of the activated particles it is reduced to an absolute value of only A(dP) = 1.2, i.e., a relative reduction of 23%.

[0364] 3. Production and characterization of particle surface-activated lithium lanthanum zirconium oxide powder

[0365] Powder production:

[0366] 110 g of coarsely pre-ground and sieved lithium lanthanum zirconium oxide powder with a particle size <63 pm were dispersed in 200 g of ethylene glycol monomethyl ether using a dissolver to minimize agglomeration.

[0367] The particles are to be incorporated later into a hybrid electrolyte whose polymer electrolyte component is based on a polyethylene oxide derivative. Accordingly, the relevant monomer units repeating within the polymer backbone are derived from the polymer backbone (ethylene glycol units) and the milling medium.

[0368]

[0369] Ethylene glycol unit) identical.

[0370] Subsequently, 1470 g of ZrC>2 grinding balls with a diameter of 0.5 mm were added to the suspension, placed in a grinding chamber made of ZrC>2 suitable for use on a Netzsch P075 attritor, inserted into the attritor, and ground for 45 minutes using a stirring shaft with three eccentric discs, all components of which (eccentric discs, bushings, and cap) are made of ZrO2 ceramic. The stirring shaft rotated at 1500 rpm. At the end of the grinding process, 50% of the particles in the grinding slurry had a diameter of less than 0.6 pm, 90% had a diameter of less than 1.8 pm, and 99% had a diameter of less than 3.5 pm.

[0371] The particle sizes were measured using the static light scattering method on a CILAS type 1064 particle size analyzer. The measurement was performed in water as the medium and evaluated according to the Fraunhofer method.

[0372] For the purpose of powder drying, in a first variant the solvent was distilled off the grinding slurry using a rotary evaporator. In a second variant, the particles in the grinding slurry were sedimented by centrifugation, and the liquid supernatant was then decanted to the moist sediment remaining in the centrifuge beaker. Acetonitrile 25.02.2026

[0373] 43

[0374] The mixture was added and slurried. It was then centrifuged again and the washing process repeated twice more. After the final slurry formation, the acetonitrile was distilled off from the washing solution using a rotary evaporator.

[0375] Powder characterization:

[0376] To demonstrate successful functionalization, the particle size-normalized sedimentation rate of the LLZO component in ethylenediglycol dimethyl ether (EGDME) was determined using a LUM LUMiSizer analytical centrifuge. EGDME is chemically very similar to polyethylene oxide, as the relevant monomer units are derived from the polymer backbone.

[0377]

[0378] Ethylene glycol units) and solvent (ethylene glycol unit) are identical. Accordingly, EGDME can be considered a solvent analogous to PEO and thus a good liquid substitute for PEO. In contrast to non-activated LLZO particles originating from a dry milling process, the sedimentation rate of the LLZO particles activated in the milling process described above was reduced to 45% for the variant in which the solvent is distilled directly from the milling slurry, and to 15% when the particles were washed again with acetonitrile before final drying.

Claims

February 25, 2026 44 1. Powder whose particles have a core of an ion-conducting material and a carbon-containing surface layer, wherein the surface layer is covalently bonded to the ion-conducting material and wherein the silicon content of the surface layer is at most 5.0 pmol / m 2 amounts.

2. Powder according to claim 1, wherein the powder has a total organic carbon content (TOC) of at least 0.1 wt.%.

3. Powder according to at least one of the preceding claims, wherein the particle size, when specified as a d50 value, is in a range of 0.05 to 10 pm.

4. Powder according to at least one of the preceding claims, wherein the ion-conducting material comprises lithium lanthanum zirconium oxide (LLZO) and / or lithium aluminum titanium phosphate (LATP).

5. A method for producing a powder, in particular a powder according to one of the preceding claims, comprising the following step: • Grinding of an ion-conducting material in a liquid grinding medium, wherein the grinding medium is a first organic solvent.

6. Method according to claim 5, wherein the grinding medium is an ether, in particular a glycol monomethyl ether, for example dipropylene glycol monomethyl ether, triethylene glycol monomethyl ether or ethylene glycol monomethyl ether.

7. Method according to at least one of claims 5 and 6, wherein the method after grinding comprises one or more washing steps.

8. The method of claim 7, wherein the powder is washed with a second organic solvent, for example with a dipolar aprotic solvent, in particular with acetonitrile.

9. A method according to at least one of claims 5 to 8, wherein the method additionally comprises the step of drying the ground and optionally washed powder, in particular as a final process step. 25.02.2026 45 10. Powder, manufactured or manufactureable according to the method of at least one of claims 5 to 9, in particular powder according to at least one of claims 1 to 4, wherein the quotient of the distance R ai the Hansen solubility parameter of the powder particles to those of the grinding medium and the distance R a 2. The Hansen solubility parameter of particles from the ion-conducting material that do not have the carbon-containing surface layer is at most 0.95 relative to that of the grinding medium.

11. Powder, produced or producible according to the method of at least one of claims 5 to 9, in particular powder according to at least one of claims 1 to 4 and 10, wherein the quotient of the sedimentation velocity of the powder particles normalized to the particle size and the sedimentation velocity normalized to the particle size of particles from the ion-conducting material that do not have the carbon-containing surface layer in the liquid grinding medium is at most 0.

90.

12. Powder, produced or producible according to the process of at least one of claims 5 to 9, in particular powder according to at least one of claims 1 to 4, 10 and 11, wherein the relative energy difference (RED) between the powder particles and the grinding medium is defined as the quotient of the distance R aiThe Hansen solubility parameter of the powder particles to that of the grinding medium and the radius Ro of the Hansen sphere spanned by the powder particles is at most 1.

00.

13. Hybrid electrolyte comprising at least one polymer electrolyte and the powder according to at least one of claims 1 to 4 and 10 to 12.

14. Hybrid electrolyte according to claim 13, wherein the relative energy difference between the powder particles and a polymer-analogous solvent is defined as the quotient of the distance R a3 the Hansen solubility parameter of the powder particles to those of the polymer-analogous solvent and the radius R othe Hansen sphere spanned by the powder particles is at most 1.00, wherein polymer-analogous solvents are short-chain solvents whose backbone is composed of one or more monomer units that are identical to the monomer unit of the backbone of the polymer electrolyte or differ from it by the presence or absence of a CH or CH2 unit, wherein the end and side groups of the polymer-analogous solvent each bear at most one more or less CH, CH2, or CH3 group compared to the end and side groups of the polymer electrolyte. 25.02.2026 46 Use of the hybrid electrolyte according to at least one of claims 13 and 14 in a separator, an anode, a cathode, a battery and / or an accumulator.