CN105742713B - All-solid-state polymer lithium battery - Google Patents
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Abstract
The invention discloses an all-solid-state polymer lithium battery, which comprises a negative plate, a positive plate and an all-solid-state polymer electrolyte membrane arranged between the negative plate and the positive plate, wherein the negative plate takes a lithium alloy formed by lithium and one or more of K, Ru, Cs, Fr, Mg, Ca, Sr and Ba as a negative electrode material, the mass content ratio of lithium metal in the lithium alloy is 70-99.9%, and the sum of the mass content ratios of other metals is 0.1-30%. Compared with the prior art, the lithium alloy cathode material used in the invention has good compatibility and interface stability with the all-solid-state polymer electrolyte, so that the cycle performance of the all-solid-state polymer lithium battery manufactured by using the lithium alloy cathode material is remarkably improved compared with the existing all-solid-state polymer lithium battery.
Description
Technical Field
The invention belongs to the field of all-solid-state polymer lithium batteries, and particularly relates to an all-solid-state polymer lithium battery with a long cycle life.
Background
Currently, the negative active material of a lithium ion battery is mainly graphite, but the graphite has a limited specific mass capacity and a very small space for increasing the specific volume capacity, and further increase of the weight energy density and the volume energy density of the lithium battery is severely limited. With the development of consumer electronics and electric vehicle technologies, it has become an urgent task to develop a battery system having a higher energy density.
Lithium metal has high mass (3860Ah/KG) and volume (2050Ah/L) energy density, and can be used as a negative electrode material of a lithium battery, for example, the lithium metal is used as a negative electrode, an organic system and an aqueous system double-electrolyte system are used as electrolytes, and an assembled novel battery system has extremely high energy density. However, this new battery system requires the use of a highly ion conductive separator to separate the organic and aqueous dual electrolyte systems, and is complicated and costly to manufacture, which is not suitable for large scale applications. In addition, since the battery system contains the high-chemical-activity lithium metal negative electrode and the aqueous electrolyte, a violent chemical reaction is easily generated due to structural damage of the battery, and the battery system has great potential hazards.
In order to solve the safety risk caused by using the lithium metal cathode, one idea is to use a nonflammable all-solid electrolyte instead of a liquid electrolyte. For example, it has been proposed to use polyethylene oxide or silicone based polymers as solid electrolytes for lithium batteries, and due to the high thermal stability (above 300 ℃) of these polymer electrolytes, the assembled batteries still have very good safety performance even when lithium metal is used as the negative electrode material. However, such batteries suffer from relatively severe capacity fade during cycling due to side reactions at the lithium metal negative electrode interface with the all-solid-state polymer electrolyte. Although researchers have attempted to improve the cycle performance of lithium metal batteries by plating a buffer layer on the surface of lithium metal by physical or chemical deposition, such methods are complicated and costly to operate, and are not suitable for mass production and large-scale application of lithium metal cathodes. On the other hand, the method of plating on the surface of lithium metal can greatly increase the internal resistance of the battery, so that the capacity and rate performance of the battery are seriously affected.
In view of the above, there is a need to provide a solution to the above-mentioned problems, so as to effectively improve the cycle life of all-solid polymer lithium battery.
Disclosure of Invention
The invention aims to: an all-solid-state polymer lithium battery is provided, which has good cycle performance, and the improvement of the cycle performance does not affect other performances of the battery.
In order to achieve the above object, the present invention provides an all-solid polymer lithium battery, which includes a negative electrode plate, a positive electrode plate, and an all-solid polymer electrolyte membrane spaced between the negative electrode plate and the positive electrode plate, wherein the negative electrode plate uses a lithium alloy formed by lithium and one or more of K, Ru, Cs, Fr, Mg, Ca, Sr, Ba as a negative electrode material, the mass content ratio of lithium metal in the lithium alloy is 70% to 99.9%, and the sum of the mass content ratios of other metals is 0.1% to 30%.
As an improvement of the all-solid-state polymer lithium battery, the mass content ratio of lithium metal in the lithium alloy is preferably 90-99%, and the sum of the mass content ratios of other metals is 1-10%.
The lithium content ratio in the alloy is limited by the invention because: too low a lithium content may lower the energy density of the negative electrode, and too high a lithium content may lower the interfacial stability with the all-solid polymer electrolyte membrane.
As an improvement of the all-solid-state polymer lithium battery of the present invention, the lithium alloy is preferably a Li-Cs alloy.
As an improvement of the all-solid-state polymer lithium battery of the present invention, the all-solid-state polymer lithium battery uses a metal sheet made of the lithium alloy as a negative electrode sheet, and the lithium alloy is used as both a negative electrode active material and a current collector.
As an improvement of the all-solid-state polymer lithium battery, the all-solid-state polymer electrolyte membrane comprises a polymer with the capability of conducting lithium ions and a lithium salt; the polymer includes, but is not limited to, polyether polymers (such as PEO, PPO, etc.), polyamine polymers (such as polyethylene diamine, etc.), and polythioether polymers (such as ethylene glycol thiol, etc.); lithium salts include, but are not limited to, LiPF6、LiAsF6、LiBF4、LiCl、LiAlCl4、LiSbF6、LiSCN、LiCF3SO3、LiCF3CO2、LiTFSI、LiN(C4F9SO2)2、Li2B12F12、LiBOB。
As an improvement of the all-solid-state polymer lithium battery, the positive plate comprises a positive current collector and a positive material layer coated on the positive current collector.
As an improvement of the all-solid-state polymer lithium battery of the present invention, the positive electrode current collector is selected from the group consisting of stainless steel, nickel, copper, titanium, carbon, conductive resin, and a copper sheet or a stainless steel sheet coated with nickel or titanium.
As an improvement of the all-solid-state polymer lithium battery of the present invention, the positive electrode material layer includes a positive electrode active material, a conductive material, and an all-solid-state polymer electrolyte; wherein, the components of the all-solid polymer electrolyte and the all-solid polymer electrolyte membrane are the same; the positive active material is selected from lithium-containing metal oxides including, but not limited to, layered lithium metal oxides (e.g., lithium cobaltate LCO, lithium nickel cobalt manganese NMC, etc.), lithium-free metal oxides (e.g., V)2O5、MnO2Etc.), spinel-structured lithium metal oxides (e.g., lithium manganate LiMn)2O4Etc.), lithium metal phosphates (e.g., lithium iron phosphate LFP, etc.), lithium metal fluorinated sulfates (e.g., fluorinated cobalt lithium sulfate LiCoFSO)4Etc.), lithium metal vanadates (e.g., nickel lithium vanadate, LiNiVO)4Etc.); the conductive material includes, but is not limited to, graphite (e.g., natural graphite, artificial graphite, etc.), acetylene black (e.g., ketjen black, etc.), conductive fibers (e.g., carbon fibers, metal fibers, etc.), metal powders (e.g., copper powders and nickel powders), organic conductive polymers (e.g., polyphenylene derivatives, etc.).
Compared with the prior art, the all-solid-state polymer lithium battery uses the lithium alloy containing other alkali metals or alkaline earth metal elements as the cathode material, can improve the interface stability between the all-solid-state polymer electrolyte and the cathode and reduce the generation of side reactions on the basis of ensuring the high energy density of the lithium metal battery, thereby prolonging the cycle life of the all-solid-state polymer lithium metal battery, and has high practical value and good application prospect in the fields of electric vehicles, energy storage power stations and the like.
Detailed Description
In order to make the objects, technical solutions and technical effects of the present invention more clear, the present invention is further described in detail below with reference to examples. It should be understood that the embodiments described in this specification are only for the purpose of explaining the present invention and are not intended to limit the present invention.
Example 1
Preparing a positive plate:
dissolving polyethylene oxide (PEO) and a lithium salt (LiTFSI) in NMP, adding lithium iron phosphate (LFP) serving as a positive electrode active material and acetylene black serving as a conductive agent, and thoroughly mixing to prepare a slurry, wherein the amount of PEO is 20 parts by weight per 100 parts by weight of LFP, the amount of LiTFSI is 10 parts by weight per 100 parts by weight of LFP, and the amount of acetylene black is 8 parts by weight per 100 parts by weight of LFP; the slurry was applied to both sides of a copper foil 12 μm thick, air-dried at 85 ℃ for 20 hours, and rolled up to prepare a positive electrode sheet.
Preparation of all-solid polymer electrolyte membrane:
polyethylene oxide PEO and lithium salt LiTFSI were mixed at a ratio of 2: 1 in acetonitrile, the electrolyte slurry was applied to a polytetrafluoroethylene membrane, dried at 70 ℃ for 5 hours, and then rolled up.
Preparing an all-solid-state polymer lithium battery:
and compounding the positive plate, the electrolyte membrane with the torn polytetrafluoroethylene membrane and the lithium cesium alloy negative plate together by using the prepared pole plate as a positive electrode and the lithium cesium alloy plate with the Cs content of 3% as a negative electrode, and rolling to obtain the all-solid-state polymer lithium metal battery A.
Example 2
Battery B was prepared as in example 1, except that the negative electrode material used was a lithium cesium alloy sheet having a Cs content of 8%.
Example 3
Battery C was prepared as in example 1, except that the negative electrode material used was a lithium cesium alloy sheet having a Cs content of 15%.
Example 4
Battery D was prepared as in example 1, except that the negative electrode material used was a lithium cesium alloy sheet having a Cs content of 30%.
Example 5
Battery E was prepared as in example 1, except that the negative electrode material used was a lithium cesium alloy sheet having a Cs content of 1%.
Example 6
Battery F was prepared as in example 1, except that the negative electrode material used was a lithium cesium alloy sheet having a Cs content of 0.1%.
Example 7
Battery G was prepared as in example 1, except that the negative electrode material used was a lithium strontium alloy sheet having a Sr content of 3%.
Example 8
A battery H was prepared as in example 1, except that the negative electrode material used was a lithium barium alloy sheet having a Ba content of 3%.
Example 9
Battery I was prepared as in example 1, except that the negative electrode material used was a lithium calcium alloy sheet having a Ca content of 3%.
Example 10
Preparing a positive plate:
dissolving polyethylene diamine and lithium salt LiFSI in NMP, adding V used as positive active material2O5And acetylene black as a conductive agent, and sufficiently mixing to prepare a slurry, wherein the amount of the polyethylene diamine is per 100 parts by weight of V2O5Is 20 parts by weight, the amount of LiFSI being per 100 parts by weight of V2O5Is 10 parts by weight, the amount of acetylene black is per 100 parts by weight of V2O58 parts by weight; the slurry was applied to both sides of a copper foil 12 μm thick, air-dried at 85 ℃ for 20 hours, and rolled up to prepare a positive electrode sheet.
Preparation of all-solid polymer electrolyte membrane:
mixing polyethylene diamine and lithium salt LiFSI in a ratio of 2: 1 in acetonitrile, the electrolyte slurry was applied to a polytetrafluoroethylene membrane, dried at 70 ℃ for 5 hours, and then rolled up.
Preparing an all-solid-state polymer lithium battery:
and compounding the positive plate, the electrolyte membrane with the torn polytetrafluoroethylene membrane and the lithium magnesium alloy negative plate together by using the prepared pole plate as a positive electrode and the lithium magnesium alloy plate with the Mg content of 1% as a negative electrode, and rolling to obtain the all-solid-state polymer lithium metal battery J.
Example 11
Preparing a positive plate:
dissolving polypropylene oxide (PPO) and lithium salt LiBOB in NMP, adding Lithium Cobaltate (LCO) used as a positive electrode active material and acetylene black used as a conductive agent, and fully mixing to prepare slurry, wherein the amount of the PPO is 20 parts by weight per 100 parts by weight of the LCO, the amount of the LiBOB is 15 parts by weight per 100 parts by weight of the LCO, and the amount of the acetylene black is 8 parts by weight per 100 parts by weight of the LCO; the slurry was applied to both sides of a copper foil 12 μm thick, air-dried at 85 ℃ for 20 hours, and rolled up to prepare a positive electrode sheet.
Preparation of all-solid polymer electrolyte membrane:
propylene oxide PPO and lithium salt LiBOB in a ratio of 3: 2 in acetonitrile, the electrolyte slurry was applied to a polytetrafluoroethylene membrane, dried at 70 ℃ for 5 hours, and then rolled up.
Preparing an all-solid-state polymer lithium battery:
and compounding the positive plate, the electrolyte membrane with the torn polytetrafluoroethylene membrane and the lithium potassium alloy negative plate together by using the prepared pole plate as a positive electrode and the lithium potassium alloy plate with the potassium content of 2% as a negative electrode, and rolling to obtain the all-solid-state polymer lithium metal battery K.
Example 12
Preparing a positive plate:
mixing polyethylene glycol thiol and lithium salt LiN (C)4F9SO2)2Dissolving in NMP, adding a lithium nickel manganese oxide ternary material NMC as a positive electrode active material and acetylene black as a conductive agent, and thoroughly mixing to prepare a slurry in which the amount of polyethylene glycol thiol is 25 parts by weight per 100 parts by weight of NMC, and LiN (C)4F9SO2)2The amount of (A) is 25 parts by weight per 100 parts by weight NMC and the amount of acetylene black is 8 parts by weight per 100 parts by weight LCO; the slurry was applied to both sides of a copper foil 12 μm thick, air-dried at 85 ℃ for 20 hours, and rolled up to prepare a positive electrode sheet.
Preparation of all-solid polymer electrolyte membrane:
mixing polyethylene glycol thiol and lithium salt LiN (C)4F9SO2)2Mixing the raw materials in a ratio of 1: 1 in acetonitrile, the electrolyte slurry was applied to a polytetrafluoroethylene membrane, dried at 70 ℃ for 5 hours, and then rolled up.
Preparing an all-solid-state polymer lithium battery:
and compounding the positive plate, the electrolyte membrane with the torn polytetrafluoroethylene membrane and the lithium strontium cesium alloy negative plate together by using the prepared pole plate as a positive electrode and the lithium strontium cesium alloy plate with the Sr content of 5% and the Cs content of 5% as a negative electrode, and rolling to obtain the all-solid-state polymer lithium metal battery L.
Comparative example 1
Battery M was prepared as in example 1, except that the negative electrode material used was a pure lithium sheet.
Comparative example 2
Battery N was prepared as in example 10, except that the negative electrode material used was a pure lithium sheet.
Comparative example 3
Battery O was prepared as in example 11, except that the negative electrode material used was a pure lithium sheet.
Comparative example 4
Battery P was prepared as in example 12, except that the negative electrode material used was a pure lithium sheet.
And (3) performance testing:
the 16 groups of lithium ion batteries were tested using the following procedure: 4 batteries in each group are charged to 4.3V at a constant current of 0.1C at 70 ℃, are subjected to constant voltage to charge cut-off voltage, are subjected to static standing for half an hour, are subjected to discharge at a constant current of 0.1C to discharge cut-off voltage, and are subjected to static standing for half an hour, and the procedure is circulated for 500 times; wherein the charge-discharge cut-off voltage of the batteries A-F and J is 2.5-3.75V, the charge-discharge cut-off voltage of the batteries G and K is 2.0-4.2V, the charge-discharge cut-off voltage of the batteries H and L is 3.0-4.3V, and the charge-discharge cut-off voltage of the batteries I and M is 3.0-4.4V; EIS test is carried out on the batteries before and after circulation at 70 ℃ under 5mv voltage and within the frequency range of 0.03Hz-500KHz, and the interface resistance is obtained by analysis.
Taking 4 batteries of each group of the 16 batteries, charging to 4.3V at a constant current of 0.1C at 70 ℃, keeping constant voltage to a charge cut-off voltage, standing for half an hour, then discharging to a discharge cut-off voltage at a constant current of 0.1C to obtain a discharge capacity C1 of 0.1C, standing for half an hour, charging to 4.3V at a constant current of 0.1C, keeping constant voltage to a charge cut-off voltage, standing for half an hour, then discharging to a discharge cut-off voltage at a constant current of 2C to obtain a discharge capacity C2 of 2C.
After the cycle test, the capacity retention rate of each group of batteries was calculated, wherein the capacity retention rate at the N-th week was the discharge capacity at the N-th week/100% of the discharge capacity at the first week, the increase rate of the interface resistance was 100% of the interface resistance (the interface resistance of the battery after 500 weeks-the interface resistance of the fresh battery)/100% of the interface resistance of the fresh battery, and the retention rate of the large-rate discharge capacity was 100% of C2/C1. The results of the calculations are shown in Table 1.
TABLE 1 Capacity Retention ratio of each battery pack after 500 cycles
As can be seen from table 1, compared to the battery M-P made of ordinary lithium metal as the negative electrode material, the lithium alloy negative electrode material containing other alkali metals or alkaline earth metals of the present invention can significantly improve the interface stability of the all-solid-state polymer lithium battery, and especially, the battery a-F made of Li-Cs alloy has no significant change in the interface resistance after 500 battery cycles, which may be related to the stability of the structure of the Li-Cs alloy itself and the good compatibility of the metal lithium deposited on the surface during the battery charging process.
In addition, the capacity retention rate of the batteries A-L made of the lithium alloy negative electrode material is remarkably improved after 500-week circulation compared with the batteries M-P made of common metal lithium. The lithium alloy material can greatly optimize the cycle performance of the all-solid-state polymer lithium battery by improving the interface between the negative electrode and the electrolyte; and the retention rate of the large-rate (2C) discharge capacity is equivalent to that of batteries M-P made of common metal lithium, which shows that the lithium alloy material can greatly optimize the cycle performance of the all-solid-state polymer lithium battery without influencing the rate performance of the batteries by improving the interface of a negative electrode and an electrolyte.
Appropriate changes and modifications to the embodiments described above will become apparent to those skilled in the art from the disclosure and teachings of the foregoing description. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some modifications and variations of the present invention should fall within the scope of the claims of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (5)
1. An all-solid-state polymer lithium battery comprises a negative plate, a positive plate and an all-solid-state polymer electrolyte membrane arranged between the negative plate and the positive plate, and is characterized in that:
the negative plate is made of Li-Cs alloy which is used as a negative active material and a current collector at the same time; the mass content proportion of lithium metal in the Li-Cs alloy is 70-99.9%, and the mass content proportion of Cs metal is 0.1-30%;
the positive plate comprises a positive current collector and a positive material layer coated on the positive current collector, wherein the positive material layer comprises a positive active substance, a conductive material and an all-solid-state polymer electrolyte; wherein, the all-solid polymer electrolyte has the same components as the all-solid polymer electrolyte membrane, and the positive active material is a metal oxide containing lithium; the conductive material comprises one or more of graphite, acetylene black, conductive fibers, metal powder and organic conductive polymers;
the increase rate of the interface resistance of the all-solid-state polymer lithium battery after 500 cycles is less than 5%.
2. The all-solid-state polymer lithium battery according to claim 1, wherein: the mass content proportion of lithium metal in the Li-Cs alloy is 90-99%, and the mass content proportion of Cs metal is 1-10%.
3. The all-solid-state polymer lithium battery according to claim 1, wherein: the all-solid-state polymer electrolyte membrane comprises a polymer with the lithium ion conducting capacity and a lithium salt; wherein the polymer is selected from polyether polymer, polyamine polymer, and polythioether polymerOne or more of the substances; the lithium salt is selected from LiPF6、LiAsF6、LiBF4、LiCl、LiAlCl4、LiSbF6、LiSCN、LiCF3SO3、LiCF3CO2、LiTFSI、LiN(C4F9SO2)2、Li2B12F12And one or more of LiBOB.
4. The all-solid-state polymer lithium battery according to claim 1, wherein: the positive current collector is selected from stainless steel, nickel, copper, titanium, carbon, conductive resin and a copper sheet or a stainless steel sheet coated with nickel or titanium.
5. The all-solid-state polymer lithium battery according to claim 1, wherein: the positive active material comprises lithium cobaltate LCO, lithium nickel cobalt manganese oxide NMC and V2O5、MnO2Lithium manganate LiMn2O4Lithium iron phosphate LFP, lithium cobalt fluoride sulfate LiCoFSO4Lithium nickel vanadate LiNiVO4One or more of them.
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| FR3134243A1 (en) * | 2022-04-01 | 2023-10-06 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | SPECIFIC LITHIUM-BASED NEGATIVE ELECTRODE AND LITHIUM ELECTROCHEMICAL GENERATOR COMPRISING SUCH A NEGATIVE ELECTRODE |
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| Publication number | Publication date |
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| CN105742713A (en) | 2016-07-06 |
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