CN103531776A - High-safety ultralong-life lithium ion battery, and positive pole material and formation method thereof - Google Patents
High-safety ultralong-life lithium ion battery, and positive pole material and formation method thereof Download PDFInfo
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- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
The invention relates to a main active material used as a lithium ion battery positive pole and a battery formation method. The main active material in the positive pole comprises spinel structure lithium manganate LiMn2O4, main additive nickel-containing lithium transition metal oxide, and subadditive alkaline metal or non-metal oxide. The high-safety ultralong-life lithium ion battery is prepared from the positive pole, a negative pole and a diaphragm by a lamination or coiling technique, wherein the active material of the negative pole is lithium titanate, and the battery is prepared by a specific formation method. The invention is characterized in that after the main additive nickel-containing lithium transition metal oxide and subadditive alkaline metal or non-metal oxide are added into the lithium manganate and subjected to specific formation, the aerogenesis phenomenon of the battery can be effectively inhibited in the use process, and the problem of inflation of the battery is solved, thereby maximally displaying the advantages of high safety and ultralong life of the material.
Description
Technical field
The present invention relates to the chemical synthesizing method of positive pole, the battery that comprises described positive pole and described battery that a kind of anode material for lithium-ion batteries, described material make, relate in particular to a kind of Design and manufacture field of the lithium rechargeable battery for power and stored energy application.
Background technology
Lithium ion battery is the new generation of green high-energy rechargeable battery after Ni-MH battery developing rapidly in early 1990s.It has that monomer voltage is high, energy density is large, self-discharge rate is low, efficiency for charge-discharge is high, have extended cycle life, memory-less effect and advantages of environment protection, become the leading supporting power supply of the portable type electronic products such as mobile phone, digital camera, notebook computer, and started to show up prominently in electric bicycle, electric car power supply.In recent years, along with day by day improving and the continuous decline of production cost of performance of lithium ion battery, its application and the market share are still in continuous expansion.
Lithium ion battery positive and negative electrode material all adopts the lithium ion with stratiform or tunnel structure that lithium ion can freely embed and deviate to embed compound.During charging, lithium ion is deviate from from positive pole, embeds negative pole; During electric discharge, lithium ion is deviate from from negative pole, embeds anodal.In charge and discharge process, lithium ion embeds and deviates from reciprocating motion between both positive and negative polarity, just as rocking chair or the reciprocating shuttlecock swinging back and forth, be therefore called visually " rocking chair (rocking chair) " or " shuttlecock (shuttlecock) " battery.
At present, the lithium titanate (Li of spinel structure
4ti
5o
12) as lithium ion battery negative material of new generation, be more and more subject to people's attention.Lithium titanate has the not available advantage of conventional carbon material.First, lithium titanate belongs to zero strain material, and in charge and discharge process, its skeleton remains unchanged; Secondly, high (the 1.5V vs Li/Li of its charge and discharge platform
+), can not there is the deposition of lithium metal; Again, it has lithium ion three-dimensional diffusion passage, and lithium ion diffusion coefficient is than high 1 order of magnitude of carbon negative pole material.The lithium titanate of usining replaces material with carbon element as the negative pole of lithium ion battery, can improve cycle life, fail safe and the power-performance of battery, and in recent years, its Novel anode material as power and energy-storage battery is more and more paid close attention to.In addition, compare the LiMn2O4 (LiMn of spinel structure with traditional lithium ion cell anode material lithium cobaltate
2o
4) have that abundant raw material, price are low, non-environmental-pollution, easily reclaim, the advantage such as current potential is high and fail safe is good.Therefore, adopt the lithium ion battery that LiMn2O4 is negative pole for anodal, lithium titanate can take into account the many advantages such as safety, long-life and low cost, be considered to the battery system that power and energy storage field have prospect.
Yet, it is found that under study for action, traditional lithium titanate/lithium manganate battery easily produces gas in cyclic process, thereby cause battery impedance to increase, performance decays fast, even when inner pressure of battery acquires a certain degree, cause battery container to break, security incident occurs.The shortcoming that this is fatal, has coverd with to the development prospect of lithium titanate/LiMn2O4 system lithium ion battery light to be difficult to together the shade dispersing.Flatulence problem becomes this system lithium ion battery bottleneck problem urgently to be resolved hurrily.
Summary of the invention
In order to solve above-mentioned practical problem, the invention provides a kind of Design and manufacture method of improved lithium titanate/LiMn2O4 system lithium ion battery, the method can solve the flatulence problem of this system battery effectively, and the battery producing by the method can give full play of high security that this material system has and the feature of extra long life.
First aspect of the present invention provides a kind of anode material for lithium-ion batteries, and described positive electrode comprises main active material, and described main active material comprises spinel structure LiMn2O4 LiMn
2o
4, main additive and subadditive.
Described main additive refers to nickeliferous lithium transition-metal oxide; Described subadditive refers to the metal or the nonmetal oxide that are alkaline.
In first aspect of the present invention, in described main active material, described spinel structure LiMn2O4, main additive and subadditive quality percentage composition are preferably (60%-95%): (35%-5%): (5%-0%).
In first aspect of the present invention, described main additive is selected from one or more combination of lithium nickelate, lithium nickel cobalt dioxide, nickel LiMn2O4 and nickle cobalt lithium manganate.
In first aspect of the present invention, described subadditive is selected from one or more combination of aluminium oxide, calcium oxide, zirconia, zinc oxide, silica.
In first aspect of the present invention, described positive electrode also comprises conductive agent and binding agent.
Wherein, main active material, conductive agent and binding agent quality percentage composition are preferably (60%-99%): (30%-0%): (10%-1%).
Wherein, described conductive agent is selected from one or more the combination in acetylene black, furnace black, VGCF, carbon nano-tube.
Wherein, described binding agent is selected from one or more the combination in SBR, PVDF.
Second aspect of the present invention provides a kind of lithium ion cell positive, and described anode comprises the positive electrode described in first aspect of the present invention.
Lithium ion cell positive described in aspect second of the present invention, is coated on substrate and is prepared by described positive electrode; Wherein said substrate can be any electric conducting material, as Cu, Al, Ag or electrical conductivity alloy, and is preferably Al.
Third aspect of the present invention provides a kind of lithium ion battery of high security extra long life, comprises the anode described in second aspect of the present invention, also comprises negative pole and diaphragm.
Described negative pole also comprises lithium titanate, conductive agent and binding agent.
Lithium titanate wherein, conductive agent and binding agent quality percentage composition are preferably (60%～99%): (30%～0%): (10%～1%).
Wherein, described conductive agent is selected from one or more the combination in acetylene black, furnace black, VGCF, carbon nano-tube.
Wherein, described binding agent is selected from one or more the combination in SBR, PVDF.
At the lithium ion battery negative described in third aspect of the present invention, by described negative material, be coated on substrate and prepare; Wherein said substrate can be any electric conducting material, as Cu, Al, Ag or electrical conductivity alloy, and is preferably Al.
The 4th aspect of the present invention provides a kind of lithium ion battery production method of high security extra long life, and battery is made by lamination or winding process by the anode described in second aspect of the present invention and negative pole and barrier film.
In the 4th aspect of the present invention, the chemical synthesizing method of the lithium ion battery of described high security extra long life comprises: shelve, be no less than charging process or the charge and discharge cycles process of one early stage, and the later stage is shelved three phases.
Wherein, shelve early stage and refer to, before charge and discharge cycles, battery be opened a way and shelved 12-48 hour at 45 ℃-80 ℃.
Wherein, in one or more steps of charge or discharge process, electric current is not less than 0.5C(C for the nominal capacity of this battery), better scheme is: one or above constant current-constant voltage charge/constant-current discharge cyclic process, consist of, the electric current in constant current charge/constant-current discharge stage is 1-5C.
Wherein, the later stage shelves and refers to, after charge and discharge cycles, battery be opened a way and shelved 12-48 hour at 45 ℃-80 ℃.
The above-mentioned various aspects of the present invention and various preferred embodiment thereof, in the situation that being not particularly limited, can combine by those skilled in the art are unrestricted.
The reason that the present invention can solve the flatulence phenomenon that traditional lithium titanate/lithium manganate battery produces in cyclic process effectively shows as: using nickeliferous lithium transition-metal oxide be alkaline metal or nonmetal oxide and add in LiMn2O4 as major and minor additive, additive material can consume the sour corrosion materials such as moisture in electrolyte, free acid, protection battery main material, thus aerogenesis in battery process recycling reduced; Simultaneously, battery is through specifically changing into after system, and the unstable material that participates in battery producing gas in battery fully decomposes, thereby reduces its adverse effect to battery in battery normal circulation is used, thereby suppress in use aerogenesis of battery, solved the inflatable problem of battery.Lithium titanate/LiMn2O4 system lithium ion battery that employing a process for preparing, can fully eliminate the adverse effect of inflatable to battery, thereby the advantage of having given play to greatest extent the peculiar high security of its material and extra long life, fully meets the instructions for use in power and stored energy application field.In addition, the method is simple to operate, and successful can be used existing lithium ion battery production equipment to produce completely, does not increase any production cost and technology difficulty, is highly suitable for large-scale production.
Accompanying drawing explanation
Fig. 1 is the cycle performance curve comparison figure of comparative example and embodiment lithium ion battery.
Fig. 2 is comparative example and the outward appearance comparison diagram of embodiment lithium ion battery after long-term circulation.
Embodiment
In order to fully demonstrate implementation result of the present invention, the pure LiMn2O4 of first usining is prepared conventional 11198148 type aluminum plastic film packing rectangular lithium ion batteries as the main active material of positive pole.Concrete steps are as follows.
Comparative example
After LiMn2O4 and Supper P, Kynoar are mixed according to the part by weight of 92: 4: 4, be dissolved in 1-METHYLPYRROLIDONE, uniform stirring is made anode sizing agent, then according to conventional lithium ion battery manufacture process, is coated with, dries, rolls, cuts and make positive plate; After lithium titanate and Supper P, Kynoar are mixed according to the part by weight of 92: 4: 4, be dissolved in 1-METHYLPYRROLIDONE, uniform stirring is made cathode size, then according to conventional lithium ion battery manufacture process, is coated with, dries, rolls, cuts and make negative plate; Positive and negative plate is separated with barrier film, adopt zigzag lamination, make battery core, through operations such as welding, encapsulation, baking, fluid injections, make battery.Battery changes into through conventional method, with 0.1C charging 1 time.Finally, battery is carried out to vacuum exhaust sealing, make final products.
Adopt method provided by the invention to prepare the concrete steps of lithium ion battery as follows.
Adopt nickle cobalt lithium manganate LiNi
1/3co
1/3mn
1/3o
2and aluminium oxide Al
2o
3respectively as major and minor additive, the ratio that LiMn2O4 is 90%, 9%, 1% with major and minor additive according to quality percentage composition is mixed the main active material of formation, after main active material and Supper P, Kynoar are mixed according to the part by weight of 92: 4: 4, be dissolved in 1-METHYLPYRROLIDONE, uniform stirring is made anode sizing agent, then according to conventional lithium ion battery manufacture process, is coated with, dries, rolls, cuts and make positive plate; After lithium titanate and Supper P, Kynoar are mixed according to the part by weight of 92: 4: 4, be dissolved in 1-METHYLPYRROLIDONE, uniform stirring is made cathode size, then according to conventional lithium ion battery manufacture process, is coated with, dries, rolls, cuts and make negative plate; Positive and negative plate is separated with barrier film, adopt zigzag lamination, make battery core, through operations such as welding, encapsulation, baking, fluid injections, make battery.The chemical synthesizing method of battery is: battery is opened a way and shelved 24 hours at 60 ℃; With 1C charge and discharge cycles 5 times; Then battery is full of to electricity with 1C, at 70 ℃, opens a way and shelve 24 hours.Finally, battery is carried out to vacuum exhaust sealing, make final products.
Embodiment 2
Adopt nickle cobalt lithium manganate LiNi
1/3co
1/3mn
1/3o
2with calcium oxide CaO respectively as major and minor additive, the ratio that LiMn2O4 is 90%, 8%, 2% with major and minor additive according to quality percentage composition is mixed the main active material of formation, after main active material and Supper P, Kynoar are mixed according to the part by weight of 92: 4: 4, be dissolved in 1-METHYLPYRROLIDONE, uniform stirring is made anode sizing agent, then according to conventional lithium ion battery manufacture process, is coated with, dries, rolls, cuts and make positive plate; After lithium titanate and Supper P, Kynoar are mixed according to the part by weight of 92: 4: 4, be dissolved in 1-METHYLPYRROLIDONE, uniform stirring is made cathode size, then according to conventional lithium ion battery manufacture process, is coated with, dries, rolls, cuts and make negative plate; Positive and negative plate is separated with barrier film, adopt zigzag lamination, make battery core, through operations such as welding, encapsulation, baking, fluid injections, make battery.The chemical synthesizing method of battery is: battery is opened a way and shelved 36 hours at 60 ℃; With 2C charge and discharge cycles 5 times; Then battery is full of to electricity with 1C, at 70 ℃, opens a way and shelve 24 hours.Finally, battery is carried out to vacuum exhaust sealing, make final products.
According to the requirement of GB GB/T18287-2000, comparative example and embodiment lithium ion battery are carried out to fail safe and charge-discharge performance test, test result is as shown in table 1, Fig. 1 and Fig. 2.As can be seen from Table 1, comparative example and embodiment battery all can be tested by security performance, and embodiment battery in short circuit and in overcharging test process temperature obviously lower, this has embodied the advantage of lithium titanate/LiMn2O4 system lithium ion battery aspect fail safe; As can be seen from Figure 1, when having circulated after 800 times, the capacity of embodiment battery is still in 20000mAh left and right, and comparative example battery capacity has dropped to 16000mAh left and right by 20000mAh left and right, and this explanation embodiment battery has excellent cycle performance; As shown in Figure 2, in long-term charge and discharge cycles process, circulating after 800 times, comparative example cell thickness increasing degree is larger, from 11mm, be increased to 21mm, show that more serious flatulence has occurred for it, and embodiment cell thickness remain within the scope of 11-12mm always, do not find significant change, show that embodiment battery flatulence phenomenon is obviously suppressed.
The safety test result of table 1 comparative example and embodiment battery
From above-described embodiment, can find out, provided by the present invention by spinel structure LiMn2O4 LiMn
2o
4, the nickeliferous lithium transition-metal oxide of main additive and subadditive be main active material and the battery formation method thereof that alkaline metal or nonmetal oxide form by a certain percentage and can effectively suppress the flatulence phenomenon that traditional lithium titanate/lithium manganate battery produces in cyclic process, thereby the advantage of having given play to greatest extent the peculiar high security of its material and extra long life, fully meets the instructions for use in power and stored energy application field.
Above specific embodiments of the invention be have been described in detail, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and alternative also all among category of the present invention.Therefore, equalization conversion and the modification done without departing from the spirit and scope of the invention, all should contain within the scope of the invention.
Claims (10)
1. an anode material for lithium-ion batteries, is characterized in that, described positive electrode comprises main active material, and described main active material comprises spinel structure LiMn2O4 LiMn
2o
4, main additive and subadditive;
Described main additive refers to nickeliferous lithium transition-metal oxide; Described subadditive refers to the metal or the nonmetal oxide that are alkaline.
2. main active material according to claim 1, is characterized in that, described spinel structure LiMn2O4, main additive and subadditive quality percentage composition are (60%-95%): (35%-5%): (5%-0%).
3. main active material according to claim 1, is characterized in that, described main additive is selected from one or more of lithium nickelate, lithium nickel cobalt dioxide, nickel LiMn2O4 and nickle cobalt lithium manganate; Described subadditive is selected from one or more of aluminium oxide, calcium oxide, zirconia, zinc oxide, silica.
4. positive electrode according to claim 1, is characterized in that, described positive electrode also comprises conductive agent and binding agent.
5. positive electrode according to claim 4, is characterized in that, the quality percentage composition of described main active material, conductive agent and binding agent is (60%-99%): (30%-0%): (10%-1%);
Described conductive agent is selected from one or more in acetylene black, furnace black, VGCF, carbon nano-tube; Described binding agent is selected from a kind of in SBR, PVDF.
6. a lithium ion cell positive, is characterized in that, described anode comprises positive electrode claimed in claim 1.
7. a lithium ion battery for high security extra long life, is characterized in that: comprise anode claimed in claim 6, also comprise negative pole and diaphragm;
Described negative pole also comprises lithium titanate, conductive agent and binding agent; Lithium titanate wherein, conductive agent and binding agent quality percentage composition are (60%-99%): (30%-0%): (10%-1%).
8. a lithium ion battery production method for high security extra long life, is characterized in that, battery is made by lamination or winding process by positive pole claimed in claim 6 and negative pole and barrier film.
9. a chemical synthesizing method for the lithium ion battery of high security extra long life claimed in claim 7, it is characterized in that comprising: shelve, be no less than charging process or the charge and discharge cycles process of one early stage, and the later stage is shelved three phases.
10. the chemical synthesizing method of the lithium ion battery of high security extra long life according to claim 9, is characterized in that: shelve early stage and refer to, before charge and discharge cycles, battery be opened a way and shelved 12-48 hour at 45 ℃-80 ℃; In one or more steps of charge or discharge process, electric current is not less than 0.5C; Later stage shelves and refers to, after charge and discharge cycles, battery be opened a way and shelved 12-48 hour at 45 ℃-80 ℃;
The better scheme of described charging process or charge and discharge cycles process is to consist of one or above constant current-constant voltage charge/constant-current discharge cyclic process, and the electric current in constant current charge/constant-current discharge stage is 1-5C.
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| CN107403908A (en) * | 2017-07-05 | 2017-11-28 | 天津普兰能源科技有限公司 | A kind of method for suppressing lithium titanate battery flatulence |
| CN109378520A (en) * | 2018-11-13 | 2019-02-22 | 上海电气国轩新能源科技有限公司 | A kind of nickle cobalt lithium manganate and lithium titanate system battery and preparation method thereof |
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