CN114349507A - Method for improving sintering relative density of lithium lanthanum zirconium oxygen ceramic wafer - Google Patents
Method for improving sintering relative density of lithium lanthanum zirconium oxygen ceramic wafer Download PDFInfo
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- CN114349507A CN114349507A CN202111659651.8A CN202111659651A CN114349507A CN 114349507 A CN114349507 A CN 114349507A CN 202111659651 A CN202111659651 A CN 202111659651A CN 114349507 A CN114349507 A CN 114349507A
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- lanthanum zirconium
- zirconium oxygen
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- XRNHBMJMFUBOID-UHFFFAOYSA-N [O].[Zr].[La].[Li] Chemical compound [O].[Zr].[La].[Li] XRNHBMJMFUBOID-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000000919 ceramic Substances 0.000 title claims abstract description 32
- 238000005245 sintering Methods 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 32
- 239000007789 gas Substances 0.000 claims abstract description 12
- NRJJZXGPUXHHTC-UHFFFAOYSA-N [Li+].[O--].[O--].[O--].[O--].[Zr+4].[La+3] Chemical compound [Li+].[O--].[O--].[O--].[O--].[Zr+4].[La+3] NRJJZXGPUXHHTC-UHFFFAOYSA-N 0.000 claims description 24
- 238000003825 pressing Methods 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000011224 oxide ceramic Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052754 neon Inorganic materials 0.000 claims description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims 1
- 239000012535 impurity Substances 0.000 claims 1
- 229910052744 lithium Inorganic materials 0.000 description 12
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 11
- 239000007784 solid electrolyte Substances 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 229910003480 inorganic solid Inorganic materials 0.000 description 3
- 239000005486 organic electrolyte Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000004880 explosion Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention provides a method for improving the relative sintering density of a Lithium Lanthanum Zirconium Oxygen (LLZO) ceramic wafer, which is characterized in that powder with the same components is added on the upper side and the lower side of the Lithium Lanthanum Zirconium Oxygen (LLZO) ceramic wafer during sintering, and gas is introduced to improve the relative density of the sintered Lithium Lanthanum Zirconium Oxygen (LLZO) ceramic wafer.
Description
Technical Field
The invention relates to a method for improving the sintering relative density of a lithium lanthanum zirconium oxygen ceramic wafer, which is applied to the field of manufacturing of all-solid-state lithium ion batteries.
Background
The lithium ion battery has the advantages of high energy density, wide working temperature range, environmental friendliness, large output power, low self-discharge and the like, and is widely applied to the fields of electric automobiles, energy storage equipment, electronic equipment and the like. However, the traditional lithium ion battery contains organic electrolyte which has the characteristics of flammability and easy explosion. If the organic electrolyte leaks under the action of external force, faults such as short circuit and the like are easily caused, and accidents such as combustion, explosion and the like of the battery can be caused in serious cases.
The solid electrolyte is used as a substitute for organic electrolyte, and has the advantages of good chemical stability, long cycle life, high energy density, good mechanical property, stability for lithium metal cathode, simple preparation and assembly and the like. The solid electrolyte comprises an inorganic solid electrolyte, an organic solid electrolyte and a composite electrolyte. Wherein the inorganic solid electrolyte effects the transfer of charge primarily through the movement of lithium ions.
The cubic-phase lithium lanthanum zirconium oxide is a material which is researched more in inorganic solid electrolyte and has the advantages of high lithium ion conductivity, good chemical stability, wide electrochemical window and the like. However, the solid-phase sintering method for preparing the lithium lanthanum zirconium oxide ceramic wafer needs to be sintered in an environment with the temperature of more than 1000 ℃. At high temperature, lithium in lithium lanthanum zirconium oxide is easily converted into lithium vapor, and the lithium vapor is easily volatilized or reacts with oxygen in air, so that pores appear in the material and lithium loss is caused. In the invention, powder with the same components is added on the upper side and the lower side of the lithium lanthanum zirconium oxide ceramic plate in the sintering process, and gas which does not react with lithium is introduced, thereby supplementing the lithium lost by volatilization, reducing the lithium consumed by side reaction and improving the relative density of the sintered lithium lanthanum zirconium oxide ceramic plate.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a method for improving the sintering relative density of a lithium lanthanum zirconium oxygen ceramic wafer.
The purpose of the invention is realized by the following scheme: the method for improving the relative density of the sintered lithium lanthanum zirconium oxide ceramic wafer comprises the following steps of adding powder with the same components to the upper side and the lower side of the lithium lanthanum zirconium oxide ceramic wafer during sintering, and introducing gas to improve the relative density of the sintered lithium lanthanum zirconium oxide ceramic wafer:
(1) taking a proper amount of lithium lanthanum zirconium oxygen powder, and prepressing for 3-10min under the pressure of 30-45MPa to form a wafer to obtain a lithium lanthanum zirconium oxygen prepressurizing sheet;
(2) taking a proper amount of lithium lanthanum zirconium oxygen powder, placing the lithium lanthanum zirconium oxygen pre-pressing sheet in a crucible, and adding the lithium lanthanum zirconium oxygen powder again to cover the pre-pressing sheet;
(3) placing the crucible in the step (2) in a tubular furnace and introducing gas;
(4) adjusting the temperature of the tube furnace, sintering at 1100-1250 ℃ for 2-8 hours, and cooling along with the furnace to obtain the lithium lanthanum zirconium oxygen ceramic wafer.
On the basis of the scheme, in the step (2), the crucible used can be one of an alumina crucible and a platinum crucible.
On the basis of the scheme, in the step (3), the introduced gas can be one or a mixture of helium, neon and argon.
The invention finds a method for improving the sintering relative density of a lithium lanthanum zirconium oxygen ceramic wafer, which supplements lithium lost due to high-temperature gasification in the sintering process by adding lithium lanthanum zirconium oxygen powder with the same components at the lower two sides of a lithium lanthanum zirconium oxygen pre-pressing wafer and introducing gas which does not react with lithium in the sintering process, and simultaneously eliminates the influence of oxygen in air and prevents a second phase formed by insufficient lithium in a product due to the reaction of the lithium and the oxygen. The lithium lanthanum zirconium oxygen ceramic wafer prepared by the method has higher relative density, less defects such as air holes, microcracks and the like in the material, and the material phase is a pure cubic phase and has better ion conductivity.
The invention has the advantages that: a new method for sintering the LLZO ceramic chip is found, so that the relative density of the sintered LLZO ceramic chip is greatly improved, the relative density of the sintered and molded LLZO ceramic chip is more than 95%, the defects of air holes, microcracks and the like in the finished LLZO ceramic chip are fewer, the grain size is uniform and tightly combined, and the LLZO ceramic chip has excellent ionic conductivity and better mechanical properties.
Drawings
FIG. 1 is a Nyquist plot of the completed LLZO ceramic wafer prepared in example 1;
FIG. 2 is a schematic representation of the relative densities of the completed LLZOs prepared in examples 1 to 3.
Detailed Description
The present invention is described in detail by the following specific examples, but the scope of the present invention is not limited to these examples.
Example 1
The utility model provides a lithium lanthanum zirconium oxygen ceramic plate LLZO, improves the relative density of lithium lanthanum zirconium oxygen ceramic plate after the sintering through add the same composition powder and let in corresponding gas in lithium lanthanum zirconium oxygen ceramic plate upper and lower both sides during sintering, according to following step:
(1) pre-pressing lithium lanthanum zirconium oxide powder for 3-10min under the pressure of 30-45MPa to form a wafer to obtain a lithium lanthanum zirconium oxide pre-pressed sheet;
(2) placing the lithium lanthanum zirconium oxygen powder in a crucible, then placing a lithium lanthanum zirconium oxygen pre-pressing sheet on the crucible, and adding the lithium lanthanum zirconium oxygen powder again to cover the pre-pressing sheet;
(3) placing the crucible in the step (2) in a tubular furnace and introducing argon;
(4) and adjusting the temperature of the tube furnace, sintering for 6 hours at 1200 ℃, and cooling along with the furnace to obtain the lithium lanthanum zirconium oxygen ceramic wafer.
The Nyquist plot for the LLZO ceramic sheet is shown in fig. 1. The room-temperature ionic conductivity (S/cm) is 1.39X 10 as shown in Table 1-4The relative density was 95.8%, as shown in FIG. 2.
Example 2
Compared with the example 1, the lithium lanthanum zirconium oxygen ceramic plate LLZO adopts gallium-doped lithium lanthanum zirconium oxygen powder in the step (1), and comprises the following steps:
(1) taking a proper amount of gallium-doped lithium lanthanum zirconium oxide powder, and prepressing for 3-10min under the pressure of 30-45MPa to form a wafer to obtain a lithium lanthanum zirconium oxide prepressing piece;
(2) taking a proper amount of lithium lanthanum zirconium oxygen powder, placing the lithium lanthanum zirconium oxygen pre-pressing sheet in a crucible, and adding the lithium lanthanum zirconium oxygen powder again to cover the pre-pressing sheet;
(3) placing the crucible obtained in the step (2) in a tubular furnace and introducing argon;
(4) and adjusting the temperature of the tube furnace, sintering for 6 hours at 1200 ℃, and cooling along with the furnace to obtain the gallium-doped lithium lanthanum zirconium oxygen ceramic wafer.
The room temperature ionic conductivity (S/cm) of the obtained gallium-doped lithium lanthanum zirconium oxide ceramic sheet is 7.94 multiplied by 10 as shown in Table 1-4. The relative density was 97.3%, as shown in FIG. 2.
Example 3
Compared with the example 1, the lithium lanthanum zirconium oxygen ceramic plate LLZO changes the gas introduced in the step (3) into helium gas, and comprises the following steps:
(1) taking a proper amount of lithium lanthanum zirconium oxygen powder, and prepressing for 3-10min under the pressure of 30-45MPa to form a wafer to obtain a lithium lanthanum zirconium oxygen prepressurizing sheet;
(2) taking a proper amount of lithium lanthanum zirconium oxygen powder, placing the lithium lanthanum zirconium oxygen pre-pressing sheet in a crucible, and adding the lithium lanthanum zirconium oxygen powder again to cover the pre-pressing sheet;
(3) placing the crucible obtained in the step (2) in a tubular furnace and introducing helium;
(4) and adjusting the temperature of the tube furnace, sintering for 6 hours at 1200 ℃, and cooling along with the furnace to obtain the lithium lanthanum zirconium oxygen ceramic wafer.
The room-temperature ionic conductivity (S/cm) of the obtained lithium lanthanum zirconium oxygen ceramic wafer is 2.95 multiplied by 10-4. The relative density was 96.2%, as shown in FIG. 2.
Table 1 shows the ion conductivity at room temperature of LLZO prepared in three examples
Claims (7)
1. The method for improving the sintering relative density of the lithium lanthanum zirconium oxide ceramic wafer is characterized in that the relative density of the sintered lithium lanthanum zirconium oxide ceramic wafer is improved by adding powder with the same components on the upper side and the lower side of the lithium lanthanum zirconium oxide ceramic wafer during sintering and introducing gas, and the method comprises the following steps:
(1) pre-pressing lithium lanthanum zirconium oxide powder for 3-10min under the pressure of 30-45MPa to form a wafer to obtain a lithium lanthanum zirconium oxide pre-pressed sheet;
(2) placing the lithium lanthanum zirconium oxygen powder in a crucible, then placing a lithium lanthanum zirconium oxygen pre-pressing sheet on the crucible, and adding the lithium lanthanum zirconium oxygen powder again to cover the pre-pressing sheet;
(3) placing the crucible in the step (2) in a tubular furnace and introducing gas;
(4) adjusting the temperature of the tube furnace, sintering at 1100-1250 ℃ for 2-8 hours, and cooling along with the furnace to obtain the lithium lanthanum zirconium oxygen ceramic wafer.
2. The method as claimed in claim 1, wherein the lithium lanthanum zirconium oxygen ceramic sheet has a cubic phase of lithium lanthanum zirconium oxygen powder phase and does not contain tetragonal phase of lithium lanthanum zirconium oxygen or other impurities.
3. The method as claimed in claim 1, wherein the crucible used in step (2) is one of an alumina crucible and a platinum crucible.
4. The method as claimed in claim 1, wherein in step (3), the introduced gas may be one or more of helium, neon and argon.
5. The method for preparing a lithium lanthanum zirconium oxygen ceramic wafer according to claim 1, which comprises the following steps:
(1) pre-pressing lithium lanthanum zirconium oxide powder for 3-10min under the pressure of 30-45MPa to form a wafer to obtain a lithium lanthanum zirconium oxide pre-pressed sheet;
(2) placing the lithium lanthanum zirconium oxygen powder in a crucible, then placing a lithium lanthanum zirconium oxygen pre-pressing sheet on the crucible, and adding the lithium lanthanum zirconium oxygen powder again to cover the pre-pressing sheet;
(3) placing the crucible in the step (2) in a tubular furnace and introducing argon;
(4) and adjusting the temperature of the tube furnace, sintering for 6 hours at 1200 ℃, and cooling along with the furnace to obtain the lithium lanthanum zirconium oxygen ceramic wafer.
6. The method for preparing a lithium lanthanum zirconium oxide ceramic wafer according to any one of claims 1 to 4, wherein the method comprises the following steps:
(1) taking a proper amount of gallium-doped lithium lanthanum zirconium oxide powder, and prepressing for 3-10min under the pressure of 30-45MPa to form a wafer to obtain a lithium lanthanum zirconium oxide prepressing piece;
(2) taking a proper amount of lithium lanthanum zirconium oxygen powder, placing the lithium lanthanum zirconium oxygen pre-pressing sheet in a crucible, and adding the lithium lanthanum zirconium oxygen powder again to cover the pre-pressing sheet;
(3) placing the crucible obtained in the step (2) in a tubular furnace and introducing argon;
(4) and adjusting the temperature of the tube furnace, sintering for 6 hours at 1200 ℃, and cooling along with the furnace to obtain the gallium-doped lithium lanthanum zirconium oxygen ceramic wafer.
7. The method for preparing a lithium lanthanum zirconium oxide ceramic wafer according to any one of claims 1 to 4, wherein the method comprises the following steps: (1) taking a proper amount of lithium lanthanum zirconium oxygen powder, and prepressing for 3-10min under the pressure of 30-45MPa to form a wafer to obtain a lithium lanthanum zirconium oxygen prepressurizing sheet;
(2) taking a proper amount of lithium lanthanum zirconium oxygen powder, placing the lithium lanthanum zirconium oxygen pre-pressing sheet in a crucible, and adding the lithium lanthanum zirconium oxygen powder again to cover the pre-pressing sheet;
(3) placing the crucible obtained in the step (2) in a tubular furnace and introducing helium;
(4) and adjusting the temperature of the tube furnace, sintering for 6 hours at 1200 ℃, and cooling along with the furnace to obtain the lithium lanthanum zirconium oxygen ceramic wafer.
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