CN117229057A - Simple and convenient LaGaO preparation 3 Method for preparing electrolyte sheet - Google Patents
Simple and convenient LaGaO preparation 3 Method for preparing electrolyte sheet Download PDFInfo
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- CN117229057A CN117229057A CN202311186926.XA CN202311186926A CN117229057A CN 117229057 A CN117229057 A CN 117229057A CN 202311186926 A CN202311186926 A CN 202311186926A CN 117229057 A CN117229057 A CN 117229057A
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 22
- 238000005266 casting Methods 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000000498 ball milling Methods 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 14
- 239000002002 slurry Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000006259 organic additive Substances 0.000 claims abstract description 6
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 12
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 claims description 12
- 239000003292 glue Substances 0.000 claims description 10
- 238000005520 cutting process Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical group OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 6
- 230000001070 adhesive effect Effects 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 239000004014 plasticizer Substances 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 2
- 238000011161 development Methods 0.000 abstract description 2
- 239000011777 magnesium Substances 0.000 description 27
- 239000012071 phase Substances 0.000 description 8
- 238000003746 solid phase reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000446 fuel Substances 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- -1 oxygen ions Chemical class 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 238000009849 vacuum degassing Methods 0.000 description 3
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 3
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001453 impedance spectrum Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910002215 La0.9Sr0.1Ga0.8Mg0.2O3 Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910002076 stabilized zirconia Inorganic materials 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Classifications
-
- 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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- Conductive Materials (AREA)
- Fuel Cell (AREA)
Abstract
The invention discloses a method for simply and conveniently preparing LaGaO 3 A method for preparing a base electrolyte sheet comprises the steps of mixing raw material powder and an organic additive, ball-milling to prepare slurry, casting and forming to obtain a green body, and sintering to obtain compact La with a pure phase structure 1‑x Sr x Ga 1‑y Mg y O 3 An electrolyte sheet. Compared with the prior La preparation 1‑ x Sr x Ga 1‑y Mg y O 3 Compared with the process of electrolyte sheet, the invention does not need to use pure La 1‑x Sr x Ga 1‑y Mg y O 3 The powder is taken as a raw material, and the raw material powder is directly prepared into La with pure phase in one step 1‑x Sr x Ga 1‑ y Mg y O 3 Thin electrolyteTablets, which shorten La 1‑x Sr x Ga 1‑y Mg y O 3 The preparation flow of the electrolyte sheet is La with low cost and high performance 1‑ x Sr x Ga 1‑y Mg y O 3 The development of the electrolyte sheet provides a new thought and has good industrialization prospect.
Description
Technical Field
The invention relates to the field of fuel cells, in particular to a method for simply and conveniently preparing LaGaO 3 A method of preparing a sheet of electrolyte.
Background
Solid Oxide Fuel Cells (SOFC) are clean and efficient energy conversion devices, have the advantages of wide fuel application range, low cost, easy modular design, wide application field, all-solid-state devices and the like, and have become a focus of social attention. The electrolyte is one of the key materials of the SOFC, and functions to conduct oxygen ions between the cathode and anode and separate the fuel from the oxidant. The electrolyte material commonly used at present is Yttria Stabilized Zirconia (YSZ), but the oxygen ion conductivity is relatively low and needs to be operated at a higher temperature. In order to reduce the operating temperature of the battery, it is common to thin the electrolyte thickness or to use materials of high conductivity.
Strontium and magnesium doped LaGaO 3 Base electrolyte La 1-x Sr x Ga 1-y Mg y O 3 Has excellent oxygen ion conductivity, which is higher than YSZ, and is close to scandia-stabilized zirconia, and is therefore commonly used in some medium temperature SOFCs. At present, la is prepared 1- x Sr x Ga 1-y Mg y O 3 The powder is usually prepared by solid phase reaction, which comprises pre-sintering at 1000-1200deg.C, ball milling, calcining at high temperature, and calcining at high temperature to obtain La 1-x Sr x Ga 1-y Mg y O 3 Electrolyte powder is used as a molding raw material to prepare an electrolyte sheet, and it can be seen that the existing solid phase reaction method is used for preparing La 1-x Sr x Ga 1-y Mg y O 3 Multiple heat treatments are required during the electrolyte process to avoid the generation of impurity phases.
The casting method is a method capable of efficiently and mass-producing a thin electrolyte having a certain shape, size and properties (density, strength, microstructure, etc.), in La 1-x Sr x Ga 1-y Mg y O 3 The electrolyte is widely applied in the preparation of the electrolyte, which is mainly La in phase 1-x Sr x Ga 1-y Mg y O 3 The powder is used as a raw material to realize the formation of the electrolyte.
Disclosure of Invention
The invention aims to provide a method for simply preparing LaGaO 3 A method for preparing a pure phase La from a raw material powder directly by one-step method by combining a solid phase reaction with casting 1-x Sr x Ga 1-y Mg y O 3 The electrolyte sheet can effectively reduce the preparation flow and cost of the electrolyte.
In order to achieve the above purpose, the invention adopts the following technical scheme:
simple and convenient LaGaO preparation 3 A method of forming a base electrolyte sheet comprising the steps of:
(1) According to La 1-x Sr x Ga 1-y Mg y O 3 Stoichiometric ratio of (x=0-0.3, y=0-0.3) preparing La 2 O 3 、SrCO 3 、Ga 2 O 3 MgO raw material powder;
(2) Ball-milling and uniformly mixing the prepared raw material powder and an organic additive to obtain slurry;
(3) The obtained slurry is prepared into La by a casting method 1-x Sr x Ga 1-y Mg y O 3 Drying the green body at room temperature and cutting the green body into required sizes;
(4) Removing the glue from the cut green body, and sintering at high temperature to obtain compact La with pure phase structure 1-x Sr x Ga 1- y Mg y O 3 An electrolyte sheet.
Further, the organic additive in the step (2) comprises 40-60% of solvent, 1-3% of dispersing agent, 4-8% of plasticizer and 3-10% of adhesive by weight.
Further, the solvent is formed by mixing absolute ethyl alcohol and butanone according to a mass ratio of 3:2.
Still further, the dispersant is triethanolamine.
Further, the plasticizer is formed by mixing polyethylene glycol and diethyl phthalate according to a mass ratio of 1:1.
Still further, the binder is polyvinyl butyral.
Further, the ball milling time in the step (2) is 4-20 h, and the rotating speed is 100-400 r.min -1 。
Further, the casting speed in the step (3) is 20 to 50 mm s -1 The height of the scraper is 100-2000 μm.
Further, the room temperature drying time in the step (3) is 4-30 h.
Further, the temperature of the adhesive discharging in the step (4) is 400-600 ℃ and the time is 1-5 h.
Further, the high-temperature sintering temperature in the step (4) is 1400-1550 ℃ and the time is 3-20 h.
The invention has the beneficial effects that:
the invention obtains slurry by directly mixing and ball milling raw material powder and organic additive, obtains green compact by tape casting and drying, and finally obtains compact La by glue discharging and one-step high-temperature sintering 1-x Sr x Ga 1-y Mg y O 3 (x=0-0.3, y=0-0.3) electrolyte sheet. Compared with the prior art, the invention does not need to use pure La 1-x Sr x Ga 1-y Mg y O 3 The powder is used as raw material, avoids the complex operation of two-step sintering in the traditional solid phase reaction, shortens La 1-x Sr x Ga 1-y Mg y O 3 The preparation flow of the electrolyte sheet is La with low cost and high performance 1-x Sr x Ga 1-y Mg y O 3 The development of the electrolyte sheet provides a new idea and has good industrialization prospect.
Drawings
FIG. 1 shows the preparation of La according to the present invention 1-x Sr x Ga 1-y Mg y O 3 Schematic flow diagram of electrolyte sheet;
FIG. 2 shows La prepared in example 1 0.9 Sr 0.1 Ga 0.8 Mg 0.2 O 3 XRD pattern of the electrolyte sheet;
FIG. 3 shows La prepared in example 1 0.9 Sr 0.1 Ga 0.8 Mg 0.2 O 3 Bending strength test curve of electrolyte sheet;
FIG. 4 shows La prepared in example 1 0.9 Sr 0.1 Ga 0.8 Mg 0.2 O 3 Topography of the surface (a) and cross section (b) of the electrolyte sheet.
FIG. 5 shows La prepared in example 1 0.9 Sr 0.1 Ga 0.8 Mg 0.2 O 3 Element distribution map of electrolyte sheet;
FIG. 6 shows La prepared in example 1 0.9 Sr 0.1 Ga 0.8 Mg 0.2 O 3 Electrolyte sheet and La prepared in comparative example 0.9 Sr 0.1 Ga 0.8 Mg 0.2 O 3 Ac impedance spectrum of the electrolyte sheet at 800 ℃.
Detailed Description
Simple and convenient LaGaO preparation 3 A method of forming a base electrolyte sheet, as in fig. 1, comprising the steps of:
(1) According to La 1-x Sr x Ga 1-y Mg y O 3 Stoichiometric ratio of (x=0-0.3, y=0-0.3) preparing La 2 O 3 、SrCO 3 、Ga 2 O 3 MgO raw material powder;
(2) Mixing the prepared raw material powder with a solvent (mixing absolute ethanol and butanone according to a mass ratio of 3:2), a dispersant triethanolamine and a plasticizer(mixing polyethylene glycol and diethyl phthalate according to the mass ratio of 1:1), mixing adhesive polyvinyl butyral, and performing 100-400 r min -1 Ball milling for 4-20 and h to mix evenly to obtain slurry;
(3) Setting the casting speed to be 20-50 mm s -1 The doctor blade height is 100-2000 μm, and La is prepared from the obtained slurry by casting method 1-x Sr x Ga 1-y Mg y O 3 Drying the green body at room temperature for 4-30 and h, and cutting the green body into required sizes;
(4) Discharging glue from the cut green body at 400-600deg.C for 1-5 h, and sintering at 1400-1550 deg.C for 3-20 h to obtain compact La with pure phase structure 1-x Sr x Ga 1-y Mg y O 3 An electrolyte sheet.
Wherein, the components in the step (2) account for 40 to 60 percent of the total mass of the materials, 1 to 3 percent of dispersing agent, 4 to 8 percent of plasticizer, 3 to 10 percent of adhesive and the balance of raw material powder.
In order to make the contents of the present invention more easily understood, the technical scheme of the present invention will be further described with reference to the specific embodiments, but the present invention is not limited thereto.
Example 1:
(1) 25.58 g La was weighed out 2 O 3 、2.58 g SrCO 3 、13.08 g Ga 2 O 3 1.41 g MgO, 1 g triethanolamine, 2.5g polyethylene glycol, 2.5g diethyl phthalate, 8 g polyvinyl butyral, 30 g absolute ethanol, 20 g butanone, at 300r min -1 Ball milling 8 h to obtain electrolyte slurry;
(2) Placing the electrolyte slurry in a vacuum deaeration machine, and performing vacuum deaeration for 35 min under the condition of 0.9 MPa; after the vacuum degassing was completed, the doctor blade height was set to 1200. Mu.m, and the casting speed was set to 35 mm. Mu.s -1 Carrying out casting operation; drying 24 h at room temperature after casting is finished to obtain a casting green body;
(3) Cutting the obtained green body, and sampling by using a circular cutting die with phi of 20; then placing the sample in a sintering furnace, and discharging glue 5 h at 500 ℃; then the sample after glue discharge is sintered at 1450 ℃ in solid phase 15 h,la can be obtained 0.9 Sr 0.1 Ga 0.8 Mg 0.2 O 3 (LSGM) electrolyte sheet.
Example 2:
(1) 22.74 g La is weighed 2 O 3 、5.15 g SrCO 3 、13.08 g Ga 2 O 3 1.41 g MgO, 1 g triethanolamine, 2.1 g polyethylene glycol, 2.1 g diethyl phthalate, 9 g polyvinyl butyral, 40 g absolute ethanol, 26 g butanone, at 300r min -1 Ball milling 8 h to obtain electrolyte slurry;
(2) Placing the electrolyte slurry in a vacuum deaeration machine, and performing vacuum deaeration for 35 min under the condition of 0.9 MPa; after the vacuum degassing was completed, the doctor blade height was set to 1200. Mu.m, and the casting speed was set to 35 mm. Mu.s -1 Carrying out casting operation; drying 24 h at room temperature after casting is finished to obtain a casting green body;
(3) Cutting the obtained green body, and sampling by using a circular cutting die with phi of 20; then placing the sample in a sintering furnace, and discharging glue 5 h at 500 ℃; then the sample after glue removal is subjected to high temperature solid phase sintering at 1450 ℃ for 15 h, and La can be obtained 0.8 Sr 0.2 Ga 0.8 Mg 0.2 O 3 (LSGM) electrolyte sheet.
Comparative example:
(1) 22.74 g La is weighed 2 O 3 、5.15 g SrCO 3 、13.08 g Ga 2 O 3 1.41 g MgO, absolute ethyl alcohol as solvent, 300r min -1 Ball milling 10 h, and drying 10 h at 80 ℃ to obtain initial powder. The initial powder is pressed and molded by a mold, presintered for 10 h at 1200 ℃, and then the presintered sample is crushed and then subjected to 300 r.min -1 Ball milling 10 h to obtain presintered powder. The presintered powder was press-molded using a mold and sintered at 1450℃for 10 h, and then the sintered sample was pulverized for 300 r. Min -1 Ball milling 10 h to obtain La 0.9 Sr 0.1 Ga 0.8 Mg 0.2 O 3 (LSGM) powder.
(2) 41.4 g LSGM powder, 1 g triethanolamine, 2.5g polyethylene glycol, 2.5g diethyl phthalate, 8 g polyvinyl alcohol are weighedButyral, 30 g absolute ethyl alcohol, 20 g butanone, 300r min -1 Ball milling 8 h to obtain electrolyte slurry;
(3) Placing the electrolyte slurry in a vacuum deaeration machine, and performing vacuum deaeration for 35 min under the condition of 0.9 MPa; after the vacuum degassing was completed, the doctor blade height was set to 1200. Mu.m, and the casting speed was set to 35 mm. Mu.s -1 Carrying out casting operation; drying 24 h at room temperature after casting is finished to obtain a casting green body;
(4) Cutting the obtained green body, and sampling by using a circular cutting die with phi of 20; then placing the sample in a sintering furnace, and discharging glue 5 h at 500 ℃; and then, carrying out solid-phase sintering on the sample subjected to glue removal at a high temperature of 1450 ℃ for 15 h to obtain the LSGM electrolyte sheet.
Characterization of the properties:
fig. 2 is an XRD pattern of LSGM electrolyte sheet prepared in example 1. The figure shows that the crystal structure of LSGM is cubic perovskite phase, basically no impurity phase is generated, and the LSGM electrolyte with pure phase can be obtained by the method.
Fig. 3 is a bending strength test curve of the LSGM electrolyte prepared in example 1. The bending strength of the LSGM electrolyte is 132 MPa through fitting calculation.
Fig. 4 is a surface (a) and cross-section (b) profile of LSGM electrolyte prepared in example 1. As can be seen, the resulting electrolyte thickness was about 140 μm, the electrolyte surface and cross section were dense, and substantially free of voids, indicating that the present invention is capable of producing fully dense electrolyte sheets.
Fig. 5 is an elemental distribution diagram of the LSGM electrolyte prepared in example 1. As can be seen from the figure, the constituent elements of LSGM electrolyte are uniformly distributed, indicating that the solid phase reaction proceeds very thoroughly.
Fig. 6 is an ac impedance spectrum at 800 c of the electrolyte sheet prepared in example 1 and comparative example. As can be seen from the figures, the electrolyte sheets prepared in example 1 and comparative example have ohmic resistances of 0.18Ω·cm, respectively, at 800 ℃ 2 And 0.19 Ω·cm 2 The ion conductivities obtained by calculation were 0.105 S.cm respectively ‒1 And 0.103S cm ‒1 The conductivity of the LSGM electrolyte sheet prepared by the invention is compared with that of the LSGM electrolyte sheet prepared by the prior artThe electrolyte sheet performance is not quite different, which illustrates the feasibility of the invention.
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (7)
1. Simple and convenient LaGaO preparation 3 A method of forming a base electrolyte sheet comprising the steps of:
(1) According to La 1-x Sr x Ga 1-y Mg y O 3 Is prepared for La by stoichiometric ratio 2 O 3 、SrCO 3 、Ga 2 O 3 MgO raw material powder, wherein x=0 to 0.3 and y=0 to 0.3;
(2) Ball-milling and uniformly mixing the prepared raw material powder and an organic additive to obtain slurry;
(3) The obtained slurry is prepared into La by a casting method 1-x Sr x Ga 1-y Mg y O 3 Drying the green body at room temperature and cutting the green body into required sizes;
(4) Removing the glue from the cut green body, and sintering at high temperature to obtain compact La with pure phase structure 1-x Sr x Ga 1-y Mg y O 3 An electrolyte sheet.
2. The simple preparation of LaGaO according to claim 1 3 A method of forming a base electrolyte sheet, characterized by: the organic additive in the step (2) comprises 40-60% of solvent, 1-3% of dispersing agent, 4-8% of plasticizer and 3-10% of adhesive by weight.
3. The simple preparation of LaGaO according to claim 2 3 A method of forming a base electrolyte sheet, characterized by: the solvent is formed by mixing absolute ethyl alcohol and butanone according to a mass ratio of 3:2;
the dispersing agent is triethanolamine;
the plasticizer is formed by mixing polyethylene glycol and diethyl phthalate according to a mass ratio of 1:1;
the binder is polyvinyl butyral.
4. The simple preparation of LaGaO according to claim 1 3 A method of forming a base electrolyte sheet, characterized by: the rotational speed of the ball milling in the step (2) is 100-400 r min -1 The time is 4-20 h.
5. The simple preparation of LaGaO according to claim 1 3 A method of forming a base electrolyte sheet, characterized by: the casting speed in the step (3) is 20-50 mm s -1 The height of the scraper is 100-2000 μm.
6. The simple preparation of LaGaO according to claim 1 3 A method of forming a base electrolyte sheet, characterized by: the temperature of the adhesive discharging in the step (4) is 400-600 ℃ and the time is 1-5 h.
7. The simple preparation of LaGaO according to claim 1 3 A method of forming a base electrolyte sheet, characterized by: the high-temperature sintering temperature in the step (4) is 1400-1550 ℃ and the time is 3-20 h.
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| CN202311186926.XA CN117229057A (en) | 2023-09-14 | 2023-09-14 | Simple and convenient LaGaO preparation 3 Method for preparing electrolyte sheet |
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| CN202311186926.XA CN117229057A (en) | 2023-09-14 | 2023-09-14 | Simple and convenient LaGaO preparation 3 Method for preparing electrolyte sheet |
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