CN116216747A - Preparation method of sulfate inverse perovskite, product and application thereof - Google Patents
Preparation method of sulfate inverse perovskite, product and application thereof Download PDFInfo
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- CN116216747A CN116216747A CN202310040686.6A CN202310040686A CN116216747A CN 116216747 A CN116216747 A CN 116216747A CN 202310040686 A CN202310040686 A CN 202310040686A CN 116216747 A CN116216747 A CN 116216747A
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- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 36
- 239000007784 solid electrolyte Substances 0.000 claims abstract description 24
- 238000000137 annealing Methods 0.000 claims abstract description 21
- 238000000227 grinding Methods 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 238000005303 weighing Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000011734 sodium Substances 0.000 description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- 239000004570 mortar (masonry) Substances 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 238000001354 calcination Methods 0.000 description 8
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- -1 hydride anions Chemical class 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
-
- 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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- 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
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
- C01P2006/40—Electric properties
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Conductive Materials (AREA)
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Abstract
The invention discloses a preparation method of sulfate inverse perovskite, a product and application thereof, and belongs to the technical field of solid electrolyte materials. The preparation method of the sulfate inverse perovskite comprises the following steps: 1) Weighing NaF and Na according to the stoichiometric ratio 2 SO 4 Mixing and grinding to obtain a mixture; 2) Continuously performing mechanical ball milling on the mixture, tabletting and vacuum sealing; 3) And (3) carrying out high-temperature annealing treatment on the sealed sample, and cooling to obtain the sulfate anti-perovskite. The sulfate inverse perovskite prepared by the invention is used as a solid electrolyte, and the ionic conductivity at room temperature reaches: 8.43×10 ‑8 Scm ‑1 The preparation method combining mechanical ball milling and annealing is adopted, the raw materials are easy to obtain, the operation is simple, the preparation process is safe and efficient, and the stable sulfate inverse perovskite at room temperature can be obtainedThe solid electrolyte has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of solid electrolyte materials, and particularly relates to a preparation method of sulfate inverse perovskite, a product and application thereof.
Background
In electric vehicles, airplanes and next generation portable electronic products, safety is energy storage on a large scaleCritical requirements. Compared with the currently available liquid electrolyte batteries, all-solid-state batteries are considered to be the most advantageous electrochemical energy storage devices of the next generation due to the advantages of high safety, high energy density, simple packaging, wide operating temperature range and the like. Compared with the solid-state lithium ion battery, the solid-state sodium ion battery has the additional advantages of rich resources and low cost. Is of the formula Li 3 Inspired by the lithium-rich anti-perovskite of OX (X being a halogen or a mixture of halogens), researchers have also found some structurally similar sodium-rich anti-perovskites, such as Na 3 OBr、Na 3 OBH 4 Has high ion conductivity. However, chemical instability or strong hygroscopicity of halogen or hydride anions can increase the likelihood of undesirable structural decomposition or hydration during operation.
Disclosure of Invention
In view of the above, the invention provides a preparation method of sulfate inverse perovskite, a product and application thereof.
A method for preparing sulfate inverse perovskite, comprising the following steps:
1) Weighing NaF and Na according to the stoichiometric ratio 2 SO 4 Mixing, and fully grinding with an agate mortar to obtain a mixture;
2) Adding the mixture into a ball milling tank for mechanical ball milling, continuously grinding the obtained sample, tabletting and vacuum sealing;
3) And (3) carrying out high-temperature annealing treatment on the sealed sample, and cooling to obtain the sulfate anti-perovskite.
Further, in step 1), the NaF and Na 2 SO 4 The stoichiometric ratio of (2) is 1: (1-2.5).
Further, in step 2), the parameters of the mechanical ball milling are as follows: ball milling rotation speed is 600rpm, ball milling time is 10-25h, ball material ratio is (30-45): 1, the ball milling body is zirconia balls.
Further, in the step 2), the mass of the sample after tabletting is 100-300mg, and the specification of the grinding tool is phi 5 mm-phi 10mm.
Further, in step 3), the high temperature annealing treatment specifically means: raising the temperature to 400-500 ℃ at a heating rate of 5 ℃/min, and annealing for 24-72h.
Further, the processes of the step 1) and the step 2) are all operated under the protection of argon atmosphere.
The invention also provides sulfate inverse perovskite (kogarkoite, the chemical formula is Na) prepared by the preparation method 3 SO 4 F)。
The invention also provides application of the sulfate inverse perovskite as a solid electrolyte.
The key component of an all-solid battery is a solid electrolyte. Although Na is 3 SO 4 F has a sodium ion conductivity of 10 at room temperature -8 But based on the flexible structure of the anti-perovskite phase, the ion conductivity is greatly improved after simple heterovalent doping modification. In addition, the natural mineral is low in cost and chemical stability, and is a potential sodium ion solid electrolyte.
Compared with the prior art, the invention has the beneficial effects that:
the sulfate inverse perovskite prepared by the invention is used as a solid electrolyte, and the ionic conductivity at room temperature reaches: 8.43×10 - 8 S cm -1 The preparation method combining mechanical ball milling and annealing can effectively eliminate grain boundary resistance, has the advantages of easily available raw materials, simple operation, safe and efficient preparation process, can obtain stable sulfate inverse perovskite type solid electrolyte at room temperature, and has wide application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a Na prepared before annealing of example 1 3 SO 4 XRD pattern of solid electrolyte powder;
FIG. 2 is a Na produced after annealing of example 1 3 SO 4 F solid electrolyte powderIs a XRD pattern of (C).
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
A method for preparing sulfate inverse perovskite, comprising the following steps:
1)weighing NaF and Na according to the stoichiometric ratio 2 SO 4 Mixing well, and fully grinding for 15min by an agate mortar to obtain a mixture;
2) Adding the mixture into a ball milling tank, putting the ball milling tank into a high-energy ball mill for mechanical ball milling, continuously grinding the obtained sample in an agate mortar, tabletting and vacuum sealing;
3) And (3) placing the sealed sample into a muffle furnace for high-temperature annealing treatment, and cooling to obtain the sulfate anti-perovskite.
In some preferred embodiments, in step 1), the NaF and Na 2 SO 4 The stoichiometric ratio of (2) is 1: (1-2.5).
In some preferred embodiments, in step 2), the parameters of the mechanical ball milling are: the ball milling speed is 600rpm, and the ball milling time is 10-25h, more preferably 10h, 15h, 20h and 25h, and still more preferably 25h; the ball-to-material ratio is (30-45): 1, preferably 30:1, 32:1, 34:1, 35:1, 36:1, 40:1, 45:1; the ball mill body is zirconia balls.
In some preferred embodiments, in step 2), the mass of the sample after tabletting is 100-300mg, the specification of the grinding tool is phi 5 mm-phi 10mm, preferably phi 8mm (i.e. the diameter is 8 mm).
In some preferred embodiments, in step 3), the high temperature annealing treatment specifically refers to: raising the temperature to 400-500 ℃, preferably 400 ℃ and 500 ℃ at a heating rate of 5 ℃/min; the annealing time is 24-72h. Preferably 24h, 36h, 48h, 72h. More preferably 72h.
In some preferred embodiments, the processes of step 1) and step 2) are all operated under an argon atmosphere.
The invention also provides sulfate inverse perovskite (kogarkoite, the chemical formula is Na) prepared by the preparation method 3 SO 4 F)。
The invention also provides application of the sulfate inverse perovskite as a solid electrolyte.
The raw material information used in the invention is Na 2 SO 4 (Mackin,99％)，NaF(Alfa,metal basis,99.99％)。
The "room temperature" in the examples of the present invention refers to 25℃unless otherwise specified.
Example 1
A preparation method of sulfate inverse perovskite comprises the following steps:
1) Weighing NaF and Na according to the molar ratio (namely stoichiometric ratio) of 1:1 2 SO 4 Mixing well, and fully grinding for 15min by an agate mortar to obtain a mixture;
2) Weighing and adding a sample weight ratio of 1:30 (namely the sample weight to zirconia ball milling beads weight ratio is 1:30, denoted by a) into a ball milling tank, putting the ball milling tank into a high-energy ball mill, ball milling for 10 hours at a rotating speed of 600rpm, putting the ball milled sample into an agate mortar, grinding for 15 minutes, pressing into a sheet with the mass of 8mm (1 g), and vacuum sealing the pressed sample;
3) Placing the vacuum sealed sample into a muffle furnace for high-temperature annealing treatment, heating to 500 ℃ at a heating rate of 5 ℃/min, calcining for 24 hours, and cooling to obtain sulfate anti-perovskite, namely Na 3 SO 4 F solid electrolyte. The whole process is carried out under the protection atmosphere of argon except for calcination.
The ionic conductivity of the solid electrolyte at room temperature was: 5.00×10 -8 S cm -1 。
Example 2
A preparation method of sulfate inverse perovskite comprises the following steps:
1) Weighing NaF and Na according to the mol ratio of 1:1.5 2 SO 4 Mixing well, and fully grinding for 15min by an agate mortar to obtain a mixture;
2) Weighing zirconia balls with the mass ratio of 1:35 (namely, the mass of the sample and the mass of zirconia ball-milling balls are 1:35), adding the zirconia balls into a ball-milling tank, putting the ball-milling tank into a high-energy ball mill, ball-milling for 15 hours at the rotating speed of 600rpm, putting the ball-milled sample into an agate mortar, grinding for 15 minutes, pressing the sample into a sheet with the mass of 8mm (1 g), and vacuum sealing the pressed sample;
3) Placing the vacuum sealed sample into a muffle furnace for high-temperature annealing treatment, heating to 450 ℃ at a heating rate of 5 ℃/min, calcining for 36h, and cooling to obtain sulfate counterPerovskite, i.e. Na 3 SO 4 F solid electrolyte. The whole process is carried out under the protection atmosphere of argon except for calcination.
The ionic conductivity of the solid electrolyte at room temperature was: 5.50×10 -8 S cm -1 。
Example 3
A preparation method of sulfate inverse perovskite comprises the following steps:
1) Weighing NaF and Na according to the mol ratio of 1:2 2 SO 4 Mixing, and grinding with agate mortar (grinding to particle size below 1 mm) to obtain mixture;
2) Weighing zirconia balls with the mass ratio of 1:40 (namely, the mass of the sample and the mass of zirconia ball-milling balls are 1:40), adding the zirconia balls into a ball-milling tank, putting the ball-milling tank into a high-energy ball mill, ball-milling for 20 hours at the rotating speed of 600rpm, putting the ball-milled sample into an agate mortar, grinding for 15 minutes, pressing the sample into a sheet with the mass of 8mm (1 g), and vacuum sealing the pressed sample;
3) Placing the sealed sample into a muffle furnace for high-temperature annealing treatment, heating to 500 ℃ at a heating rate of 5 ℃/min, calcining for 48 hours, and cooling to obtain sulfate anti-perovskite, namely Na 3 SO 4 F solid electrolyte. The whole process is carried out under the protection atmosphere of argon except for calcination.
The ionic conductivity of the solid electrolyte at room temperature was: 4.60×10 -8 S cm -1 。
Example 4
A preparation method of sulfate inverse perovskite comprises the following steps:
1) Weighing NaF and Na according to the mol ratio of 1:2.5 2 SO 4 Mixing, and grinding with agate mortar (grinding to particle size below 1 mm) to obtain mixture;
2) Weighing zirconia balls with the mass ratio of 1:45 (namely, the mass of the sample and the mass of zirconia ball-milling balls are 1:45), adding the zirconia balls into a ball-milling tank, putting the ball-milling tank into a high-energy ball mill, ball-milling for 25 hours at the rotating speed of 600rpm, putting the ball-milled sample into an agate mortar, grinding for 15 minutes, pressing the sample into a sheet with the mass of 8mm (1 g), and vacuum sealing the pressed sample;
3) Placing the sealed sample into a muffle furnace for high-temperature annealing treatment, heating to 450 ℃ at a heating rate of 5 ℃/min, calcining for 72 hours, and cooling to obtain sulfate anti-perovskite (Na) 3 SO 4 F solid electrolyte. The whole process is carried out under the protection atmosphere of argon except for calcination.
The ionic conductivity of the solid electrolyte at room temperature was: 6.0X10 -8 S cm -1 。
FIG. 1 is a Na prepared before annealing of example 1 3 SO 4 XRD pattern of solid electrolyte powder.
FIG. 2 is a Na produced after annealing of example 1 3 SO 4 As can be seen by comparing XRD patterns of the F solid electrolyte powder with those of FIG. 1, na after annealing treatment 3 SO 4 The peak of F is more obvious and the crystallinity is higher.
Comparative example 1
The difference from example 1 is that step 3) is not performed.
The ionic conductivity of the solid electrolyte at room temperature was: 3X 10 -9 S cm -1 。
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the particular embodiments disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (8)
1. A method for preparing sulfate inverse perovskite, which is characterized by comprising the following steps:
1) Weighing NaF and Na according to the stoichiometric ratio 2 SO 4 Mixing and grinding to obtain a mixture;
2) Carrying out mechanical ball milling on the mixture, continuously grinding the obtained sample, tabletting and vacuum sealing;
3) And (3) carrying out high-temperature annealing treatment on the sealed sample, and cooling to obtain the sulfate anti-perovskite.
2. A sulfate inverse perovskite according to claim 1Characterized in that in step 1), the NaF and Na are 2 SO 4 The stoichiometric ratio of (2) is 1: (1-2.5).
3. The method for preparing sulfate inverse perovskite according to claim 1, wherein in the step 2), the parameters of the mechanical ball milling are: ball milling rotation speed is 600rpm, ball milling time is 10-25h, ball material ratio is (30-45): 1, the ball milling body is zirconia balls.
4. The method for preparing sulfate inverse perovskite according to claim 1, wherein in the step 2), the mass of the sample after tabletting is 100-300mg, and the specification of the grinding tool is phi 5 mm-phi 10mm.
5. The method for preparing sulfate inverse perovskite according to claim 1, wherein in the step 3), the high-temperature annealing treatment specifically means: and (3) heating to 400-500 ℃ at a heating rate of 5 ℃/min for annealing for 24-72h.
6. The method for preparing sulfate inverse perovskite according to claim 1, wherein the processes of step 1) and step 2) are all operated under the protection of argon atmosphere.
7. A sulfate inverse perovskite prepared by the method for preparing a sulfate inverse perovskite according to any one of claims 1 to 6.
8. Use of the sulfate inverse perovskite according to claim 7 as a solid electrolyte.
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| CN114551986A (en) * | 2021-08-16 | 2022-05-27 | 万向一二三股份公司 | High-conductivity composite solid electrolyte and preparation method thereof |
| CN115084639A (en) * | 2022-06-10 | 2022-09-20 | 南方科技大学 | Anti-perovskite solid electrolyte with low electronic conductivity and preparation method thereof |
| US20220333028A1 (en) * | 2011-09-01 | 2022-10-20 | Akbev Group, Llc | High Protein Organic Materials as Fuel and Processes for Making the Same |
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| US20220333028A1 (en) * | 2011-09-01 | 2022-10-20 | Akbev Group, Llc | High Protein Organic Materials as Fuel and Processes for Making the Same |
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| CN114551986A (en) * | 2021-08-16 | 2022-05-27 | 万向一二三股份公司 | High-conductivity composite solid electrolyte and preparation method thereof |
| CN115084639A (en) * | 2022-06-10 | 2022-09-20 | 南方科技大学 | Anti-perovskite solid electrolyte with low electronic conductivity and preparation method thereof |
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