CN114784361A - All-solid-state lithium battery with excellent rate performance and preparation method thereof - Google Patents
All-solid-state lithium battery with excellent rate performance and preparation method thereof Download PDFInfo
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 39
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000003792 electrolyte Substances 0.000 claims abstract description 65
- 239000002002 slurry Substances 0.000 claims abstract description 28
- 239000012528 membrane Substances 0.000 claims abstract description 22
- 238000000576 coating method Methods 0.000 claims abstract description 13
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000004806 packaging method and process Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 239000002033 PVDF binder Substances 0.000 claims description 8
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 8
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 claims description 6
- 229910003002 lithium salt Inorganic materials 0.000 claims description 6
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical group [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 159000000002 lithium salts Chemical class 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 229910052493 LiFePO4 Inorganic materials 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 2
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims description 2
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 claims description 2
- 239000007784 solid electrolyte Substances 0.000 abstract description 12
- 230000008595 infiltration Effects 0.000 abstract description 3
- 238000001764 infiltration Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 22
- 238000012360 testing method Methods 0.000 description 10
- 210000002966 serum Anatomy 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 230000001351 cycling effect Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000013543 active substance Substances 0.000 description 2
- 229910003480 inorganic solid Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 208000033978 Device electrical impedance issue Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000003115 supporting electrolyte Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- 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
- H01M10/052—Li-accumulators
-
- 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
- H01M10/058—Construction or manufacture
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- Manufacturing & Machinery (AREA)
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- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Secondary Cells (AREA)
Abstract
The invention discloses an all-solid-state lithium battery with excellent rate performance and a preparation method thereof, wherein the battery structure refers to a battery structure integrating a positive electrode layer and an electrolyte membrane with a gradient structure, the preparation method comprises the steps of treating a positive electrode and an electrolyte interface in a coating mode, directly coating electrolyte slurry CPE-1 on the positive electrode layer, drying, completely curing, directly coating electrolyte slurry CPE-2 on a cured CPE-1 membrane, drying, completely curing to obtain the electrolyte membrane integrating the positive electrode and the electrolyte with the gradient structure, slicing, and finally packaging the electrolyte membrane and a negative electrode in a battery case to obtain the all-solid-state lithium battery. The method provided by the invention ensures the infiltration and adhesion of the solid electrolyte to the positive electrode layer, effectively reduces the interface impedance, and the prepared electrolyte membrane with the gradient structure has enough mechanical strength, thereby improving the high-rate charge-discharge performance and the cycle stability of the battery.
Description
Technical Field
The invention belongs to the technical field of solid electrolytes of lithium ion batteries, and particularly relates to an all-solid-state lithium battery with excellent rate capability and a preparation method thereof.
Background
All solid-state lithium metal batteries (ASSLBs) hold great promise for meeting future demands for high safety and high energy density for energy storage. The electrolyte of the solid lithium battery is solid, plays a role in isolating positive and negative electrodes and conducting ions, and plays a role as a diaphragm and an electrolyte of liquid Lithium Ion Batteries (LIBs), so that the ASSLBs is simpler than the LIBs in structure. However, the solid electrolyte of ASSLBs has problems of low ionic conductivity, poor contact with electrode interface, etc., as compared with LIBs, which hinders its practical application.
Conventional solid electrolyte materials are largely classified into solid polymer materials, inorganic solid electrolytes, and composite solid electrolytes. The solid polymer electrolyte material has low ion conductivity (particularly under room temperature condition) and low ion migration number; the inorganic solid electrolyte material has large interface resistance, is easy to be brittle, has large processing difficulty, high cost and the like; the composite electrolyte system and the addition of inorganic materials increase the ionic conductivity and the lithium ion transference number t of the electrolyteLi+And the mechanical strength and the voltage stability window of the electrolyte can be improved, and the flexibility and the processability of the composite electrolyte are not influenced. However, since the assembly process of the parts of the conventional solid-state battery is layer-by-layer stacking, such solid-solid rigid contact is achieved as compared with the liquid electrolyteThe contact property and the wettability between the positive electrode layer and the solid electrolyte layer are extremely poor, and extra interface impedance is caused, so that the rate performance of the prepared all-solid-state lithium battery is greatly reduced. Therefore, in order to prepare an all-solid-state lithium battery with excellent rate capability, designing and developing a battery internal structure with good electrolyte wettability to the positive electrode layer is one of the hot spots of all-solid-state lithium battery research.
Disclosure of Invention
In order to solve the technical problems, the invention provides an all-solid-state lithium battery with excellent rate performance and a preparation method thereof, the method ensures the infiltration and adhesion of solid electrolyte to a positive electrode layer, effectively reduces the interface impedance, and the prepared electrolyte membrane with a gradient structure has enough mechanical strength, thereby improving the high-rate charge-discharge performance and the cycling stability of the battery; the prepared electrolyte membrane with the gradient structure supported by the anode ensures the infiltration and the adhesion of a solid electrolyte to the anode layer, effectively reduces the interface impedance, and has enough mechanical strength, so that the all-solid-state lithium battery with excellent rate capability is prepared;
in order to achieve the technical purpose, the invention is realized by the following technical scheme: a preparation method of an all-solid-state lithium battery with excellent rate performance comprises the following steps:
s1: coating the electrolyte slurry CPE-1 which is uniformly stirred on the positive electrode layer, drying, and waiting for the CPE-1 layer to be completely dried; coating the uniformly stirred electrolyte slurry CPE-2 on a dry CPE-1 layer, drying, and waiting for the CPE-2 layer to be completely dried to obtain a gradient structure electrolyte membrane supported by the anode;
s2: slicing the gradient structure electrolyte membrane supported by the anode, and finally packaging the electrolyte membrane and the cathode in a battery case together to obtain the all-solid-state lithium battery with high rate performance;
preferably, the positive electrode layer in S1 is self-made LiFePO4A positive electrode layer; the negative electrode described in S2 was a commercially available lithium plate;
preferably, the height of the scraper coated with the electrolyte slurry CPE-1 in the S1 is adjusted to be 150-200 μm, and the height of the scraper coated with the electrolyte slurry CPE-2 is adjusted to be 300-400 μm;
preferably, the method for uniformly stirring in the S1 is to stir for 4 to 6 hours at the constant temperature of 50 to 70 ℃ and the stirring speed of 50 to 200 r/min;
preferably, the electrolyte slurries CPE-1 and CPE-2 in S1 comprise PEO, PVDF and Al2O3Lithium salt and organic solvent, wherein the lithium salt is LiTFSI and LiClO4、Li2CO3Wherein the organic solvent is one of DMF or NMP;
preferably, the electrolyte pastes CPE-1 and CPE-2 in S1 comprise powder in a certain ratio (10:5:2: 3): PEO, PVDF, Al2O3And a lithium salt;
preferably, in the electrolyte slurry CPE-1 in S1, the ratio of powder: DMF-1: 15, in the electrolyte slurry CPE-2, powder: DMF-1: 10;
preferably, the drying treatment in the step S1 is to heat the mixture for 12 hours at a constant temperature of 60 ℃ in the atmospheric environment, then transfer the mixture to a vacuum drying oven, adjust the vacuum degree to be-0.07 MPa, and heat the mixture for 12 hours at a constant temperature of 45 ℃.
The invention has the beneficial effects that:
1) according to the invention, the wettability of the electrolyte slurry CPE-1 to deep pores of the anode layer can be increased by a direct coating mode, after drying treatment, the electrolyte slurry CPE-2 can wet pores of the dried CPE-1 layer electrolyte by a direct coating mode, and after drying treatment, an integrally structured anode supported gradient structure electrolyte membrane is formed, so that a certain stabilizing effect is exerted on the structure of the electrolyte;
2) the structure of the invention can prepare the all-solid-state lithium battery with excellent rate performance.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a graph comparing the rate performance of batteries;
FIG. 3 is a graph of a long cycle of a battery;
fig. 4 is an EIS curve before and after a long cycle of the battery.
Detailed Description
In order to clearly and completely describe the technical scheme and the effects of the invention, detailed description is given through embodiments;
example 1
A preparation method of an all-solid-state lithium battery with excellent rate performance comprises the following steps:
s1: weighing PEO, PVDF and Al according to the proportion (10:5:2:3)2O3And LiTFSI in a serum bottle, adding a certain amount of DMF according to the proportion (powder: DMF 1: 15);
s2: placing the serum bottle filled with the mixture in S1 on a magnetic stirrer, and stirring for 6h under the conditions of constant temperature of 60 ℃ and stirring speed of 200r/min to obtain uniform electrolyte slurry CPE-1;
s3: adjusting the height of a scraper to be 200 mu m, and coating the electrolyte slurry CPE-1 described in S2 on the positive electrode layer by using the scraper; heating at constant temperature of 60 ℃ for 12h in atmospheric environment, transferring to a vacuum drying oven, adjusting the vacuum degree to-0.07 MPa, and heating at constant temperature of 45 ℃ for 12h to obtain a dry positive electrode supported CPE-1 layer;
s4: weighing PEO, PVDF and Al according to the proportion (10:5:2:3)2O3And LiTFSI in a serum bottle, adding a certain amount of DMF according to the proportion (powder: DMF 1: 10);
s5: placing the serum bottle filled with the mixture in S4 on a magnetic stirrer, and stirring for 12h under the conditions of constant temperature of 60 ℃ and stirring speed of 100r/min to obtain uniform electrolyte slurry CPE-2;
s6: coating the electrolyte slurry CPE-2 of S5 on the dried cathode-supported CPE-1 layer of S3 using a doctor blade with a doctor blade height of 400 μm; heating at constant temperature of 60 ℃ for 12h in atmospheric environment, transferring to a vacuum drying oven, adjusting the vacuum degree to-0.07 MPa, and heating at constant temperature of 45 ℃ for 12h to obtain a dry anode-supported gradient structure electrolyte membrane;
s7: and (4) slicing the electrolyte membrane with the gradient structure supported by the anode in the S6, and finally packaging the sliced electrolyte membrane and the lithium metal cathode in a battery case together to obtain the all-solid-state lithium battery with high rate performance.
Comparative example 1
Comparative example 1 is a comparative example to example 1, the main differences with respect to example 1 being: the doctor blade height of S3 was adjusted to 400 μm, and it was not necessary to prepare the electrolyte slurry CPE-2.
The preparation method of the all-solid-state lithium battery of the comparative example includes the steps of:
s1: weighing PEO, PVDF and Al according to the proportion (10:5:2:3)2O3And LiTFSI in a serum bottle, adding a certain amount of DMF according to the proportion (powder: DMF ═ 1: 15);
s2: placing the serum bottle filled with the mixture in the S1 on a magnetic stirrer, and stirring for 6 hours under the conditions of constant temperature of 60 ℃ and stirring speed of 200r/min to obtain uniform electrolyte slurry CPE-1;
s3: adjusting the height of a scraper to 400 μm, and coating the electrolyte slurry CPE-1 described in S2 on the positive electrode layer by using the scraper; heating at constant temperature of 60 ℃ for 12h in atmospheric environment, transferring to a vacuum drying oven, adjusting the vacuum degree to-0.07 MPa, and heating at constant temperature of 45 ℃ for 12h to obtain a dry positive electrode supported CPE-1 layer;
s4: and (4) slicing the CPE-1 layer supported by the anode in the S3, and finally packaging the sliced CPE-1 layer and the lithium metal cathode in a battery case to obtain the all-solid-state lithium battery.
Comparative example 2
Comparative example 2 is a comparative example to example 1, the main differences with respect to example 1 being: no coating process is used. The preparation method of the all-solid-state lithium battery of the comparative example includes the steps of:
s1: weighing PEO, PVDF and Al according to the proportion (10:5:2:3)2O3And LiTFSI in a serum bottle, adding a certain amount of DMF according to the proportion (powder: DMF 1: 10);
s2: placing the serum bottle filled with the mixture in S1 on a magnetic stirrer, and stirring for 12h under the conditions of constant temperature of 60 ℃ and stirring speed of 100r/min to obtain uniform electrolyte slurry CPE-2;
s3: pouring the electrolyte slurry CPE-2 in the S2 into a culture dish, heating for 12h at the constant temperature of 60 ℃ in the atmospheric environment, then transferring into a vacuum drying oven, adjusting the vacuum degree to be-0.07 MPa, and heating for 12h at the constant temperature of 45 ℃ to obtain a dry CPE-2 layer;
s4: slicing the CPE-2 layer described in S3, and finally mixing with LiFePO4And packaging the positive electrode and the lithium metal negative electrode in a battery case together to obtain the all-solid-state lithium battery.
Performance test
1. Rate capability test
The all-solid-state lithium batteries prepared in the example 1, the comparative example 1 and the comparative example 2 are respectively subjected to different multiplying power charge and discharge performance tests, the cut-off voltage is set to be 2.8-3.8V, the current density is set to be 0.5-6C, and the test temperature is 60 ℃.
As can be seen from fig. 2, the initial discharge capacities of the battery of example 1 at the current densities of 0.5C, 3C and 6C are 163, 140 and 115mAh/g, respectively, the initial discharge capacities of the battery of comparative example 1 at the current densities of 0.5C, 3C and 6C are 159, 130 and 100mAh/g, respectively, and the initial discharge capacities of the battery of comparative example 2 at the current densities of 0.5C, 3C and 6C are 118, 102 and 10mAh/g, respectively, which indicates that, compared to the conventional structure in which the positive electrode and the electrolyte layer are independent, the positive electrode supporting electrolyte of the structure in which the positive electrode and the electrolyte are integrated has a significant promoting effect of increasing the charge/discharge specific capacity of the all-solid-state battery. The electrolyte slurry is directly coated on the positive electrode layer, so that the wettability of the solid electrolyte membrane to the positive electrode layer is improved, the interface contact between the solid electrolyte membrane and the positive electrode active substance is increased, the utilization rate of the active substance in the positive electrode layer is improved, more lithium ions can be provided to participate in electrochemical reaction, and the all-solid-state lithium metal battery prepared by the electrolyte membrane with the structure has more excellent rate capability; compared with the comparative example 1 and the comparative example 1, the wettability of the electrolyte to the positive electrode layer is basically consistent, but the advantages of the battery of the example 1 are more and more obvious along with the increase of the current density, and the fact that the gradient structure electrolyte membrane supported by the positive electrode can achieve higher charging and discharging capacities of the battery at a high rate is shown.
2. Long cycle stability test
The all-solid-state lithium batteries prepared in example 1, comparative example 1 and comparative example 2 were subjected to a long-cycle charge-discharge test, with a cut-off voltage of 2.8 to 3.8V, a current density of 5C or 5.25C, and a test temperature of 60 ℃.
As can be seen from FIG. 3, the specific discharge capacity of the first ring of the battery in comparative example 2 is 120mAh/g, and after 300 cycles of charge and discharge, the capacity retention rate is 25%; the discharge specific capacity of the first circle of the battery of the comparative example 1 is 100mAh/g, and after 300 cycles of charge and discharge, the capacity retention rate is 87%; the battery of example 1 had a high capacity retention of 99% after 350 cycles (initial 121mAh/g, 120mAh/g after 200 cycles, 120mAh/g after 350 cycles, 5.34C), and the test results showed that: the all-solid-state lithium metal battery with the gradient-structure electrolyte membrane supported by the anode has good high-rate cycle performance and high-rate cycle stability at 60 ℃.
3. EIS testing of full cells
EIS tests were performed on the cells of example 1, comparative example 1 and comparative example 2 before and after the long-period cycle test, and the frequency range of the tests was 0.01Hz to 1 MHz.
As can be seen from fig. 4, the impedance of the battery of example 1 before and after long-period high-rate cycling is about 44 Ω and 29 Ω, respectively, and after long-period cycling, the impedance of the battery of example 1 is rather reduced, and the impedance change is 15 Ω; the impedance of the cell of comparative example 1 before and after the long-period high-rate cycle was about 125 Ω and 175 Ω, respectively, and the impedance increased by 50 Ω. The impedance of the battery of comparative example 2 varied greatly, increasing by about 235 Ω. The above-mentioned impedance test results also explain the capacity size and capacity fading of all-solid-state batteries of three structures in the long-period charge-discharge cycle curve, and the extremely low interfacial impedance and the improvement in the wettability of the electrolyte to the electrode during the cycle, which are also the reasons why the gradient-structure battery exhibits good capacity retention (60 ℃, 5.34C, about 100%).
Claims (8)
1. A preparation method of an all-solid-state lithium battery with excellent rate performance is characterized by comprising the following steps:
s1: coating the electrolyte slurry CPE-1 which is uniformly stirred on the positive electrode layer, drying the electrolyte slurry and waiting for the CPE-1 layer to be completely dried; coating the uniformly stirred electrolyte slurry CPE-2 on a dry CPE-1 layer, drying, and waiting for the CPE-2 layer to be completely dried to obtain a gradient structure electrolyte membrane supported by the anode;
s2: and slicing the electrolyte membrane with the gradient structure supported by the anode, and finally packaging the sliced electrolyte membrane and the cathode together in a battery shell to obtain the all-solid-state lithium battery with high rate capability.
2. The method for preparing an all-solid-state lithium battery with excellent rate capability according to claim 1, wherein the positive electrode layer in S1 is made of self-made LiFePO4A positive electrode layer; the negative electrode described in S2 was a commercially available lithium plate.
3. The method for preparing an all-solid-state lithium battery with excellent rate capability according to claim 1, wherein the blade height of the coated electrolyte paste CPE-1 in S1 is adjusted to be 150-200 μm, and the blade height of the coated electrolyte paste CPE-2 is adjusted to be 300-400 μm.
4. The method for preparing the all-solid-state lithium battery with excellent rate performance according to claim 1, wherein the stirring in the step S1 is performed under the conditions of constant temperature of 50-70 ℃ and stirring speed of 50-200r/min for 4-6 h.
5. The method for preparing all-solid-state lithium battery with excellent rate capability according to claim 1, wherein electrolyte slurries CPE-1 and CPE-2 in S1 comprise PEO, PVDF and Al2O3Lithium salt and organic solvent, wherein the lithium salt is LiTFSI and LiClO4、Li2CO3Wherein the organic solvent is one of DMF or NMP.
6. The method for preparing the all-solid-state lithium battery with excellent rate performance according to claim 1, wherein the electrolyte slurries CPE-1 and CPE-2 in S1 comprise a certain ratio (10:5:2:3) of powder: PEO, PVDF, Al2O3And a lithium salt.
7. The method for preparing the all-solid-state lithium battery with excellent rate capability according to claim 1, wherein in the electrolyte slurry CPE-1 in S1, the ratio of powder: DMF 1:15, and in the electrolyte slurry CPE-2, powder: DMF-1: 10.
8. The method for preparing an all-solid-state lithium battery with excellent rate capability according to claim 1, wherein the drying process in S1 comprises the steps of heating at a constant temperature of 60 ℃ for 12 hours in an atmospheric environment, transferring to a vacuum drying oven, adjusting the vacuum degree to-0.07 MPa, and heating at a constant temperature of 45 ℃ for 12 hours.
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