CN110980784A - β' -Al2O3Method for preparing solid electrolyte powder - Google Patents

β' -Al2O3Method for preparing solid electrolyte powder Download PDF

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CN110980784A
CN110980784A CN201911015259.2A CN201911015259A CN110980784A CN 110980784 A CN110980784 A CN 110980784A CN 201911015259 A CN201911015259 A CN 201911015259A CN 110980784 A CN110980784 A CN 110980784A
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solid electrolyte
materials
mixer
preparation
electrolyte powder
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郭文飞
陈忠伟
毛治宇
张洪涛
石再军
张国肖
郭宽红
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Zhejiang Anli Energy Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
    • C01F7/306—Thermal decomposition of hydrated chlorides, e.g. of aluminium trichloride hexahydrate
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
    • H01M10/0562—Solid materials
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
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  • Organic Chemistry (AREA)
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  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Conductive Materials (AREA)

Abstract

The invention relates to β' -Al2O3The preparation method of the solid electrolyte powder is characterized by comprising the following steps of (1) Li solution preparation, (2) dry powder mixing, (3) granulation, (4) sieving, (5) calcination, and β' -Al prepared by the method2O3β' -Al for preparing high-crystallinity and high-stability powder2O3The ceramic isolating membrane has the advantages of high density, high conductivity, high strength, low porosity and the like, and can be used for batch production.

Description

β' -Al2O3Method for preparing solid electrolyte powder
Technical Field
The invention relates to the field of sodium salt batteries, in particular to a solid electrolyte for a sodium salt battery.
Background
Since the 21 st century, the energy problem becomes the focus of worldwide attention, and wind energy and solar energy are clean energy, and are rapidly attracting attention of people due to no pollution, large application scenes and wide development prospects. However, both wind energy and solar energy have the characteristics of intermittency and distribution, and cannot stably and continuously supplement electric power. There is therefore a need for an energy storage battery for power storage.
As a novel energy storage battery, the sodium-nickel battery and the sodium-sulfur battery become research hotspots due to the advantages of high specific energy, strong environmental adaptability, large discharge power, no self-discharge, low cost, no pollution and the like, and are the first choice of the distributed energy storage battery2O3The preparation and quality of the alloy put severe requirements β' -Al2O3Is a complex sodium-aluminum composite oxide with a non-stoichiometric equation of Na2O·5.33Al2O3Its other isomer β -Al2O3Empirical formula of Na2O·11Al2O3The difference is that β' -Al2O3Has a theoretical conductivity of β -Al2O3A number 10 times that of Na but in Na2O-Al2O3β -Al is often simultaneously present in the system2O3And β' -Al2O3Two crystal phases, and β' -Al is prepared in the high-temperature synthesis process of powder2O3β -Al is contained in the powder2O3Concomitant, high purity β' -Al is thus produced in a stable manner2O3The phase powder becomes the key for preparing sodium salt battery material, and β' -Al is synthesized conventionally2O3The main method is to mix high-purity α -Al2O3、Na2CO3And a small amount of stabilizer such as MgO, etc., and sintering at a high temperature of 1580 deg.C or above, which is obtained by using high-purity α -Al2O3β -Al with higher cost and low conductivity due to raw materials2O3In recent decades, β' -Al was prepared by new chemical methods such as sol-gel method, alkoxide hydrolysis method, solvent combustion method, coprecipitation method, etc2O3The related reports of (A) and (B),the synthesis methods have the advantages of high purity of synthesis materials, uniform distribution, low sintering temperature and the like, but the synthesis processes are complex, the requirements on equipment and operation are high, batch production cannot be carried out, the significance on industrial application is not great, and compared with the traditional solid phase method, the industrial mass production is difficult.
However, the traditional calcining method has various problems in material selection, synthesis process and the like, and the β' -Al prepared by the traditional calcining method2O3Containing other hetero-phases, e.g. β -Al2O3、 Na2O·11Al2O3And sodium aluminate, etc., the β' -Al containing impurity phase2O3The prepared ceramic isolation membrane has low density, high porosity, low conductivity, low strength and unstable performance, and cannot be used for preparing sodium salt battery isolation membrane products with higher performance requirements, the traditional calcining method has a small synthesis temperature window, under-burnt powder and over-burnt powder are easy to appear, the under-burnt powder contains a large amount of sodium aluminate, the obtained product has low density and low strength when the post-ceramic sintering is carried out, and the over-burnt powder is in a metastable state of β' -Al due to overhigh synthesis temperature2O3Phase inversion occurs to form a large amount of β -Al2O3This transformation is irreversible and the resulting ceramic separator has low electrical conductivity during the subsequent ceramic sintering.
Disclosure of Invention
In order to solve the technical problem, the invention provides β' -Al2O3The preparation method of the solid electrolyte powder comprises the following steps: (1) preparing a Li solution: weighing lithium salt, weighing deionized water, adding the deionized water into a liquid preparation tank, adding the lithium salt after the deionized water is added, and stirring until the solution is clear; (2) mixing dry powder: weighing an aluminum source, and adding the aluminum source into a mixer; weighing a sodium source, adding the sodium source into a mixer, starting the mixer to mix materials, and stopping dry powder mixing after agglomeration does not exist and the materials are uniformly mixed; (3) and (3) granulation: spraying the lithium salt solution into a mixer, starting the mixer for granulation, stopping granulation when the granularity reaches the required granules, pouring out the granulated materials, and ageing until the temperature is reduced to room temperature; (4) sieving: screening the granulated particles to obtain qualified materials; (5) calcining: loading the qualified materials into a saggerAnd placing the mixture into a kiln for calcination after the mixture is covered and sealed, and preserving the heat for a certain time to cool after the calcination temperature is reached.
Further, the step 1 includes a step of testing whether the conductivity of the Li solution meets the requirement.
Further, in the step 4, the oversize material of the fine screen mesh below the coarse screen mesh is taken as the qualified material through coarse screening and fine screening.
Further, the lithium salt is one of lithium hydroxide, lithium hydroxide monohydrate, lithium acetate and lithium acetate dihydrate, and the preparation concentration of the lithium solution is 1-20 wt%.
Further, the aluminum source is one of boehmite, pseudoboehmite, calcined pseudoboehmite, and calcined boehmite.
Further, the sodium source is one of sodium carbonate, sodium acetate and sodium hydroxide.
Furthermore, the proportion ratio of the aluminum source, the sodium source and the lithium salt solution is required to be 100:10: 10-100: 30: 40.
Further, in the step 5, the calcining temperature is 1150-1350 ℃, and the calcining heat preservation time is 0.25-2 hours.
Further, in the step 5, the calcined β' -Al2O3In the range of the ratio of each component in the composition, Li20.5 to 4 weight percent of O and Na2The content of O is 8 to 13 weight percent, and Al is2O3The content is 75 wt% -95 wt%.
β' -Al prepared by the invention2O3β' -Al for preparing high-crystallinity and high-stability powder2O3The ceramic isolating membrane has the advantages of high density, high conductivity, high strength, low porosity and the like, and can be used for batch production.
Detailed Description
The specific operation process of the invention is as follows: preparing a Li solution according to a mass ratio of (1): weighing 2-4 parts of lithium salt and 20-40 parts of deionized water; adding deionized water into a liquid preparation tank, adding lithium salt after the deionized water is added, and stirring until the solution is clear; the conductivity was measured after the solution was clarifiedIf the requirement is met, lithium salt can be one of lithium hydroxide, lithium hydroxide monohydrate, lithium acetate and lithium acetate dihydrate, the preparation concentration of a lithium solution is 1-20 wt%, 2, a dry powder mixing step of weighing 100 parts of an aluminum source and adding the weighed aluminum source into a mixer, weighing 12-25 parts of a sodium source and adding the weighed sodium source into the mixer, starting the mixer to mix materials for 10-20 min, sampling and observing that no agglomeration exists and the materials are uniformly mixed, stopping the dry powder mixing step, wherein the ratio of the aluminum source, the sodium source and the lithium salt solution is 100:10: 10-100: 30:40, the aluminum source can be one of boehmite, pseudo-boehmite, calcined pseudo-boehmite and calcined boehmite, and the sodium source can be one of sodium carbonate, sodium acetate and sodium hydroxide, (3) a granulation step of spraying 20-40 parts of the lithium salt solution into the mixer, starting the mixer to granulate, wherein the granulation step is carried out once fixed, observation is carried out, granulation is stopped when the granularity reaches the requirement, the materials are poured out, screened until the temperature reaches 4 ″, and put into a coarse screen, and put into a screen for a time of 355-25 h, and a screen mesh screen for a qualified calcining time after calcining time, the calcining time is set for a calcining time, the calcining time2O3In the range of the ratio of each component in the composition, Li20.5 to 4 weight percent of O and Na2The content of O is 8 to 13 weight percent, and Al is2O3The content is 75 wt% -95 wt%.
The invention is based on the principle of controlling the incoming materials, avoids the lattice synthesis defect caused by α aluminum oxide adopted by the traditional calcining method by selecting the aluminum source with a certain crystalline phase, can ensure the uniformity of the raw materials during mixing by adopting the lithium solution as the granulating agent, produces uniform spheres and simultaneously controls the temperature of β' -Al2O3Introduction of Li2The O stabilizer stabilizes the crystal phase and suppresses β -Al2O3、Na2O·11Al2O3And sodium aluminate formation, ensuring β' -Al2O3The purity of the phases is such that,
the invention is further described with reference to specific examples.
Example 1:
(1) weighing 38g of deionized water, adding the deionized water into a solution tank, starting stirring, weighing 1.47g of lithium hydroxide, slowly adding the lithium hydroxide into a stirring tank, and stirring for dissolving;
(2) after stirring for 20min, taking out the lithium hydroxide solution for conductivity test to obtain the conductivity of 253 ms/cm;
(3) weighing 100g of calcined pseudo-boehmite and 19.4g of sodium carbonate, adding the calcined pseudo-boehmite and the sodium carbonate into a mixer, starting the mixer, mixing at a medium speed for 20 min;
(4) slowly adding a lithium hydroxide solution into a mixer, starting high-speed mixing at the same time, finishing adding the lithium hydroxide solution for 5min, continuously mixing for 10min, observing particle generation, growing up particles after 14min, and stopping the mixer to stop granulation;
(5) after the mixer is shut down for 20min, the temperature of the materials measured by a handheld thermometer is reduced to room temperature, the materials are taken out, 136g of materials are sieved by a 1mm coarse sieve, 134g of materials are sieved by a 0.2mm fine sieve, and the materials are taken as qualified aggregate;
(6) loading the qualified granulated material into a sagger for calcination, wherein the calcination temperature is 1200 ℃, the calcination heat preservation time is 1h, and the furnace cooling is carried out after the calcination is finished;
(7) XRD testing of the calcined material gave β' -Al2O3The phase content was 91.4%.
Example 2:
(1) weighing 30g of deionized water, adding the deionized water into a solution tank, starting stirring, weighing 2.58g of lithium hydroxide monohydrate, slowly adding the lithium hydroxide monohydrate into a stirring tank, and stirring for dissolving;
(2) after stirring for 20min, taking out the lithium hydroxide solution for conductivity test to obtain the conductivity of 281 ms/cm;
(3) weighing 100g of calcined boehmite and 19.4g of sodium carbonate, adding into a mixer, starting the mixer, mixing at a medium speed for 20 min;
(4) slowly adding a lithium hydroxide solution into a mixer, starting high-speed mixing, finishing adding the lithium hydroxide solution after 5min, continuously mixing for 4min, observing particle generation, growing up particles after 7min, and stopping the mixer to stop granulation;
(5) after the mixer is shut down for 20min, the temperature of the materials measured by a handheld thermometer is reduced to room temperature, the materials are taken out, the materials are sieved by a 1mm coarse sieve to obtain 131g of sieved materials, the 131g of sieved materials are sieved by a 0.2mm fine sieve to obtain 130g of sieved materials, and the materials are taken as qualified granulated materials;
(6) loading the qualified granulated material into a sagger for calcination, wherein the calcination temperature is 1290 ℃, the calcination heat preservation time is 1h, and the furnace cooling is carried out after the calcination is finished;
(7) XRD testing of the calcined material gave β' -Al2O3The phase content was 94.7%.
Example 3:
(1) weighing 17g of deionized water, adding the deionized water into a solution tank, starting stirring, weighing 2.58g of lithium hydroxide monohydrate, slowly adding the lithium hydroxide monohydrate into a stirring tank, and stirring for dissolving;
(2) after stirring for 20min, taking out the lithium hydroxide solution for conductivity test to obtain the conductivity of 317 ms/cm;
(3) weighing 129g of pseudo-boehmite and 19.4g of sodium carbonate, adding the weighed pseudo-boehmite and the sodium carbonate into a mixer, starting the mixer, mixing at a medium speed for 20 min;
(4) slowly adding a lithium hydroxide solution into a mixer, starting high-speed mixing at the same time, finishing adding the lithium hydroxide solution for 5min, continuously mixing for 12min, observing particle generation, growing up particles after 15min, and stopping the mixer to stop granulation;
(5) after the mixer is shut down for 20min, the temperature of the materials measured by a handheld thermometer is reduced to room temperature, the materials are taken out, 126g of sieved materials are obtained by sieving the materials through a 1mm coarse sieve, 119g of sieved materials are obtained by sieving the 126g of materials through a 0.2mm fine sieve, and the sieved materials are taken as qualified granulated materials;
(6) loading the qualified granulated material into a sagger for calcination, wherein the calcination temperature is 1200 ℃, the calcination heat preservation time is 1h, and the furnace cooling is carried out after the calcination is finished;
(7) XRD testing of the calcined material gave β' -Al2O3The phase content was 96.6%.
Example 4:
(1) weighing 16g of deionized water, adding the deionized water into a solution tank, starting stirring, weighing 2.58g of lithium hydroxide monohydrate, slowly adding the lithium hydroxide monohydrate into a stirring tank, and stirring for dissolving;
(2) stirring for 20min, taking out the lithium hydroxide solution, and carrying out conductivity test to obtain the conductivity of 491 ms/cm;
(3) weighing 118g of calcined pseudo-boehmite and 19.4g of sodium carbonate, adding into a mixer, starting the mixer, mixing at a medium speed for 20 min;
(4) slowly adding a lithium hydroxide solution into a mixer, starting high-speed mixing at the same time, finishing adding the lithium hydroxide solution for 5min, continuously mixing for 17min, observing generation of particles, growing up the particles after 20min, and stopping the mixer to stop granulation;
(5) after the mixer is shut down for 20min, the temperature of the materials measured by a handheld thermometer is reduced to room temperature, the materials are taken out, 113g of sieved materials are obtained by sieving the materials through a 1mm coarse sieve, 104g of sieved materials are obtained by sieving 113g of the materials through a 0.2mm fine sieve, and the materials are taken as qualified granulated materials;
(6) loading the qualified granulated material into a sagger for calcination, wherein the calcination temperature is 1290 ℃, the calcination heat preservation time is 1h, and the furnace cooling is carried out after the calcination is finished;
(7) XRD testing of the calcined material gave β' -Al2O3The phase content was 91.9%.
Example 5:
(1) weighing 34g of deionized water, adding the deionized water into a solution tank, starting stirring, weighing 6.26g of lithium acetate dihydrate, slowly adding the lithium acetate dihydrate into a stirring tank, and stirring for dissolving;
(2) after stirring for 20min, taking out the lithium hydroxide solution for conductivity test to obtain the conductivity of 257 ms/cm;
(3) weighing 100g of calcined pseudo-boehmite and 19.4g of sodium carbonate, adding the calcined pseudo-boehmite and the sodium carbonate into a mixer, starting the mixer, mixing at a medium speed for 20 min;
(4) slowly adding a lithium hydroxide solution into a mixer, starting high-speed mixing at the same time, finishing adding the lithium hydroxide solution for 5min, continuously mixing for 11min, observing particle generation, growing up particles after 13min, and stopping the mixer to stop granulation;
(5) after the mixer is shut down for 20min, the temperature of the materials measured by a handheld thermometer is reduced to room temperature, the materials are taken out, the materials are sieved by a 1mm coarse sieve to obtain 131g of sieved materials, the 131g of sieved materials are sieved by a 0.2mm fine sieve to obtain 124g of sieved materials, and the sieved materials are taken as qualified granulation materials;
(6) loading the qualified granulated material into a sagger for calcination, wherein the calcination temperature is 1200 ℃, the calcination heat preservation time is 1h, and the furnace cooling is carried out after the calcination is finished;
(7) XRD testing of the calcined material gave β' -Al2O3The phase content was 90.4%.
Example 6:
(1) weighing 12g of deionized water, adding the deionized water into a solution tank, starting stirring, weighing 4.05g of lithium acetate, slowly adding the lithium acetate into a stirring tank, and stirring for dissolving;
(2) after stirring for 20min, taking out the lithium hydroxide solution for conductivity test to obtain the conductivity of 751 ms/cm;
(3) weighing 100g of calcined pseudo-boehmite and 14.6g of sodium hydroxide, adding into a mixer, starting the mixer, mixing at a medium speed for 20 min;
(4) slowly adding a lithium hydroxide solution into a mixer, starting high-speed mixing at the same time, finishing adding the lithium hydroxide solution for 5min, continuously mixing for 2min, observing generation of particles, growing up the particles after 5min, and stopping the mixer to stop granulation;
(5) after the mixer is shut down for 20min, the temperature of the materials measured by a handheld thermometer is reduced to room temperature, the materials are taken out, 123g of materials are sieved out through a 1mm coarse sieve, 114g of materials on the sieve are sieved out through a 0.2mm fine sieve, and the materials are taken as qualified aggregate;
(6) loading the qualified granulated material into a sagger for calcination, wherein the calcination temperature is 1200 ℃, the calcination heat preservation time is 1h, and the furnace cooling is carried out after the calcination is finished;
(7) XRD testing of the calcined material gave β' -Al2O3The phase content was 93.4%.
The invention provides β' -Al with stable Li2O3The invention is characterized in that Li raw material is adopted as a crystal stabilizer in the formula, and β' -Al is stabilized by introducing Li ions2O3Crystalline phase, suppression of β' -Al during calcination synthesis2O3To othersPhase β' -Al2O3、 Na2O·11Al2O3In addition, boehmite, pseudo-boehmite, calcined boehmite and calcined pseudo-boehmite are used as raw materials in selection of an aluminum source, so that β' -Al is effectively improved2O3Phase conversion of (2), the resulting product β' -Al2O3Rate of phase inversion>90 percent in the preparation process, the invention adopts a mixing-granulating-calcining process, firstly, an aluminum source and a sodium source are dry-mixed according to a certain proportion to be fully and uniformly mixed, then a lithium salt solution is added for granulation, a certain particle sphere is obtained after homogenization and mixing so as to ensure the mixing uniformity of all the raw materials in the batching process, after the mixing is finished, the particles are screened, and a granulated material in a certain particle range is selected for calcination so as to ensure that the material in the calcination process is uniformly filled into a sagger, thereby obtaining β' -Al with stable crystalline phase2O3The phenomenon of under burning and over burning caused by uneven filling is avoided, and the stability and consistency of the product are ensured.

Claims (9)

1.β' -Al2O3The preparation method of the solid electrolyte powder is characterized by comprising the following steps: (1) preparing a Li solution: weighing lithium salt, weighing deionized water, adding the deionized water into a liquid preparation tank, adding the lithium salt after the deionized water is added, and stirring until the solution is clear; (2) mixing dry powder: weighing an aluminum source, and adding the aluminum source into a mixer; weighing a sodium source, adding the sodium source into a mixer, starting the mixer to mix materials, and stopping dry powder mixing after agglomeration does not exist and the materials are uniformly mixed; (3) and (3) granulation: spraying the lithium salt solution into a mixer, starting the mixer for granulation, stopping granulation when the granularity reaches the required granules, pouring out the granulated materials, and ageing until the temperature is reduced to room temperature; (4) sieving: screening the granulated particles to obtain qualified materials; (5) and (3) calcining: and (3) putting the qualified materials into a sagger, covering and sealing the sagger, putting the sagger into a kiln for calcination, and preserving the heat for a certain time until the temperature reaches the calcination temperature.
2.β "-Al as claimed in claim 12O3A method for preparing the solid electrolyte powder, characterized in thatIn the step 1, a step of testing whether the conductivity of the Li solution meets a requirement is further included.
3.β "-Al as claimed in claim 22O3The preparation method of the solid electrolyte powder is characterized in that in the step 4, the oversize material of the fine screen mesh below the coarse screen mesh is taken as the qualified material through the coarse screen mesh and the fine screen mesh.
4.β "-Al as claimed in any one of claims 1-42O3The preparation method of the solid electrolyte powder is characterized in that the lithium salt is one of lithium hydroxide, lithium hydroxide monohydrate, lithium acetate and lithium acetate dihydrate, and the preparation concentration of the lithium solution is 1-20 wt%.
5.β "-Al as claimed in any one of claims 1-42O3A method for producing a solid electrolyte powder, characterized in that the aluminum source is one of boehmite, pseudoboehmite, calcined pseudoboehmite, and calcined boehmite.
6.β "-Al as claimed in any one of claims 1-42O3The preparation method of the solid electrolyte powder is characterized in that the sodium source is one of sodium carbonate, sodium acetate and sodium hydroxide.
7.β "-Al as claimed in any one of claims 1-42O3The preparation method of the solid electrolyte powder is characterized in that the proportion of the aluminum source, the sodium source and the lithium salt solution is 100:10: 10-100: 30: 40.
8.β "-Al as claimed in any one of claims 1-42O3The preparation method of the solid electrolyte powder is characterized in that in the step 5, the calcination temperature is 1150-1350 ℃, and the calcination heat preservation time is 0.25-2 hours.
9.β "-Al as claimed in any one of claims 1-42O3The preparation method of the solid electrolyte powder is characterized in that in the step 5, β' -Al after calcination2O3In the range of the ratio of each component in the composition, Li20.5 to 4 weight percent of O and Na2The content of O is 8 to 13 weight percent, and Al is2O3The content is 75 wt% -95 wt%.
CN201911015259.2A 2019-10-24 2019-10-24 β' -Al2O3Method for preparing solid electrolyte powder Pending CN110980784A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86104187A (en) * 1985-05-24 1987-04-29 利利怀特公司 β " the preparation method of aluminum oxide

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86104187A (en) * 1985-05-24 1987-04-29 利利怀特公司 β " the preparation method of aluminum oxide

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Application publication date: 20200410