CN103928672B - A kind of positive electrode active material for lithium ion battery and preparation method thereof - Google Patents
A kind of positive electrode active material for lithium ion battery and preparation method thereof Download PDFInfo
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
- H01M4/1315—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx containing halogen atoms, e.g. LiCoOxFy
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- 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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The present invention provides a kind of positive electrode active material for lithium ion battery and preparation method thereof, and this positive active material is the Li of Fluorin doped2MnO3, its composition formula is: Li2MnO3-xFx(0.03≤x≤0.12).Preparation method is simple, and by the battery made by the present invention, when electric current density is 5mA/g, first discharge specific capacity reaches 172.4～209.1mAh/g, is maintained at 112.7～139.9mAh/g after 20 circulations, and conservation rate is 58.6～66.9%.
Description
Technical field
The invention belongs to cell manufacturing techniques field, be specifically related to a kind of positive electrode active material for lithium ion battery and preparation method thereof.
Background technology
Exhaustion day by day along with Fossil fuel, and the fast development of portable electric appts and electric vehicle, the research of the new forms of energy such as power-supply battery has become the focus of global concern, wherein lithium ion battery because its voltage height, specific energy height, discharge and recharge time length, memory-less effect, environmental pollution are little, quick charge, the excellent specific property such as have extended cycle life be widely used.Lithium ion battery structure mainly includes pole piece and nonaqueous electrolytic solution, described pole piece and nonaqueous electrolytic solution are sealed in battery container, described pole piece includes positive pole, negative pole and the barrier film between positive pole and negative pole, described positive pole includes collector body and load positive electrode on the current collector, and positive electrode includes positive active material and binding agent.
Anode material for lithium-ion batteries, as the important component part of lithium ion battery, is all the study hotspot of domestic and international scientist all the time.In recent years, along with the continuous extension of development in science and technology and lithium ion battery applications field, the energy density of anode material for lithium-ion batteries is had higher requirement by people, and therefore high theoretical capacity positive active material causes the extensive concern of researcher.At present commercialization or study more positive active material and include LiCoO2、LiNiO2、LiMn2O4And LiFePO4Deng, but by materials theory capacity limit, it is difficult to meet the social development demand to lithium ion battery with high energy density.
Li2MnO3Sill is the active substance of lithium ion battery anode that a class is novel, owing to the advantages such as its theoretical capacity is high, with low cost, environmentally friendly become the focus that positive electrode is paid close attention to.It is generally acknowledged pure Li2MnO3Electro-chemical activity is poor, and specific discharge capacity is very low.At present, mainly through forming Li2MnO3-LiMO2(M=Ni, Co, Mn etc.) solid solution improves its performance, shows high specific discharge capacity.But raw material Co, Ni etc. that this kind of material adopts are costly, synthesis temperature is high, and material stability in cyclic process is good not.
Summary of the invention
The technical problem to be solved is for above shortcomings in prior art, it is provided that a kind of positive electrode active material for lithium ion battery and preparation method thereof, and cost of material is low, and technique is simple, and synthesis temperature is low, the Li of prepared Fluorin doped2MnO3Stable in properties, improves anode material for lithium-ion batteries Li2MnO3Chemical property, corresponding lithium ion battery specific capacity is big, good cycle.
Solve the technology of the present invention problem and be employed technical scheme comprise that the Li that this positive electrode active material for lithium ion battery is Fluorin doped2MnO3, its composition formula is: Li2MnO3-xFx(0.03≤x≤0.12)。
The preparation method that the present invention also provides for above-mentioned positive electrode active material for lithium ion battery, it is characterised in that comprise the following steps:
(1) lithium salts is weighed, manganese salt and lithium fluoride (0.03≤x≤0.12), it is dissolved in deionized water and is configured to saline solution, described lithium salts is in lithium, manganese salt is in manganese, lithium salts, the mol ratio of manganese salt and lithium fluoride is 2-x:1:x, in saline solution, manganese element molar concentration is 2～5mol/L, the aqueous citric acid solution that concentration is 3～6mol/L is added aforementioned salt solution is formed mixed solution, citric acid is 0.5～1.5:1 with the mol ratio of metal cation in saline solution, mixed solution pH value is regulated to 7～9 subsequently with ammonia, again mixed solution is stirred 6～8 hours at 60～80 DEG C, make solution that sufficient complexation to occur, form colloidal sol, obtain liquid precursor；
(2) at 130～150 DEG C, 8～12h is heated at 60～80 DEG C after step (1) gained liquid precursor being heated 16～24 hours, it is thus achieved that solid precursor；
(3) grind after step (2) gained solid precursor being calcined 3～7 minutes at 450～500 DEG C, obtain Powdered presoma, again the pre-burning at 300～350 DEG C of Powdered presoma was heated to 600～700 DEG C with the programming rate of 2-4 DEG C/min after 1～2 hour, and it is incubated 9～15h, obtain the Li of Fluorin doped after furnace cooling2MnO3, namely obtain positive electrode active material for lithium ion battery.
The present invention program adopts the F ion part that bond energy is bigger to replace O ion, makes cathode material structure more stable, and improves the chemical property of material.The method is by preparing liquid precursor by lithium salts, manganese salt, lithium fluoride and citric acid and deionized water Homogeneous phase mixing, and the solid precursor that liquid precursor heated and stirred is obtained after drying carries out pre-burning and calcination processing obtains end product.
By such scheme, step (1) described lithium salts includes any one in lithium nitrate, lithium carbonate, lithium acetate；Described manganese salt includes any one in manganese nitrate, manganese carbonate, manganese acetate.
Present invention additionally comprises and state, according to above-mentioned, the lithium ion battery positive pole that positive electrode active material for lithium ion battery prepared by method prepares, and use the lithium ion battery of this positive pole.
The invention has the beneficial effects as follows: use simple and easy method to prepare positive electrode active material for lithium ion battery, improve Li2MnO3Chemical property.In the specific capacity improving lithium ion battery and cycle performance, there is marked improvement, by the battery made by the present invention, when electric current density is 5mA/g, first discharge specific capacity reaches 172.4～209.1mAh/g, being maintained at 112.7～139.9mAh/g after 20 circulations, conservation rate is that 58.6～66.9%(adopts unadulterated Li2MnO3Battery first discharge specific capacity be 154.2mAh/g；Being maintained at 77.8mAh/g after circulating 20 times, capability retention is 50.4%).
Accompanying drawing explanation
Fig. 1 is the Li prepared by comparative example 1 of the present invention2MnO3XRD figure spectrum；
Fig. 2 is the Li of the Fluorin doped prepared by the embodiment of the present invention one2MnO3Discharge capacity figure first under 5mA/g electric current density；
Fig. 3 is the Li of the Fluorin doped prepared by the embodiment of the present invention one2MnO3Cycle performance figure under 5mA/g electric current density.
Detailed description of the invention
For making those skilled in the art be more fully understood that technical scheme, below in conjunction with accompanying drawing, the present invention is described in further detail.
The embodiment of the present invention provides a kind of positive electrode active material for lithium ion battery with good chemical property.
Comparative example 1
Weigh 5.5160gLiNO3、7.1576gMn(NO3)2It is dissolved in 10ml deionized water and forms saline solution, by 12.6718g citric acid with adding formation mixed solution in aforementioned salt solution after 10ml deionized water dissolving, mixed solution pH to 8 is adjusted with ammonia, subsequently mixed solution is placed on continuously stirred 8 hours of constant temperature 60 DEG C on magnetic force heating stirrer, obtains liquid precursor.Liquid precursor is placed in drying baker and dry at 150 DEG C after dry 16 hours within 12 hours, obtains solid precursor in 80 DEG C, it is ground into powder presoma after being placed in Muffle furnace by solid precursor at 500 DEG C calcining 3 minutes, is heated to 600 DEG C with the programming rate of 2 DEG C/min after Powdered presoma be incubated one hour at 300 DEG C and is incubated 12h and obtains Li2MnO3。
The XRD figure spectrum of this comparative example gained solid product is as it is shown in figure 1, its main diffraction peak and Li2MnO3Standard diagram (01-084-1634) coincide.
Adopt positive active material Li prepared by this comparative example2MnO3Mix by the mass ratio of 80:12:8 with conductive agent acetylene black and bonding agent polyvinylidene fluoride (PVDF1300), be dissolved in (Li in solvent N-methyl pyrilidone (NMP)2MnO3-xFxIt is 1:3 with NMP mass ratio), stir into pasted positive coating, be coated uniformly on the stainless steel substrate of diameter 14.8mm.Being placed in vacuum drying oven by the positive plate coated, at 80 DEG C, namely vacuum drying can be used for the assembling of battery after 12 hours.
Anhydrous, the anaerobic that carry out lithium ion battery in the MBRAUN glove box of full high-purity argon gas assemble (wherein the content of moisture is less than 1ppm, and the content of oxygen is less than 1ppm).Assembling sequence is followed successively by negative electrode casing, currect collecting net, metal lithium sheet negative pole, barrier film, electrolyte (EC:DMC=1:2), Li from top to bottom2MnO3-xFxPositive plate, currect collecting net, anode cover, finally with MSK-110 battery sealing machine encapsulation battery.Electro-chemical test is carried out after the CR2025 type button room temperature battery standing 24h being assembled into.Adopt LandCT2001A battery test system, characterize the specific discharge capacity of battery, cyclical stability (voltage 2.0-4.8V).
Test result shows, under the electric current density of 5mA/g, and Li2MnO3First discharge specific capacity be 154.2mAh/g, after circulating 20 times, capacity is 77.8mAh/g, and the conservation rate of capacity is 50.4%.
Embodiment one
Weigh 2.9113gLi2CO3、7.1576gMn(NO3)2And 0.0314gLiF is dissolved in 10ml deionization and forms saline solution, add after 12.6718g citric acid is dissolved with 10ml deionization in aforementioned salt solution and form mixed solution, mixed solution pH to 8 is adjusted with ammonia, subsequently mixed solution is placed on continuously stirred 8 hours of constant temperature 60 DEG C on magnetic force heating stirrer, obtains liquid precursor.Liquid precursor is placed in drying baker and dry at 150 DEG C after dry 16 hours within 12 hours, obtains solid precursor in 80 DEG C, it is ground into powder presoma after being placed in Muffle furnace by solid precursor at 500 DEG C calcining 3 minutes, is heated to 600 DEG C with the heating rate of 2 DEG C/min after be incubated one hour at 300 DEG C by Powdered presoma and is incubated 12h and obtains the Li of Fluorin doped2MnO3(Li2MnO2.97F0.03).
Adopt the method identical with comparative example 1 to prepare CR2025 type button room temperature battery, its capacity, high rate performance, cyclical stability are tested (voltage 2.0-4.8V).Test result shows, under the electric current density of 5mA/g, and Li2MnO2.97F0.03Discharge capacity first be 209.1mAh/g, after circulating 20 times, capacity is 139.8mAh/g, and the conservation rate of capacity is 66.9%.The specific capacity circulation figure of its first discharge specific capacity and 20 times is as shown in Fig. 2, Fig. 3.
Embodiment two
Weigh 5.3505gLiNO3、4.5980gMnCO3And 0.0629gLiF is dissolved in 8ml deionized water and forms saline solution, by 25.3435g citric acid with adding formation mixed solution in aforementioned salt solution after 30ml deionized water dissolving, mixed solution pH to 7 is adjusted with ammonia, subsequently mixed solution is placed on continuously stirred 6 hours of constant temperature 80 DEG C on magnetic force heating stirrer, obtains liquid precursor.Liquid precursor is placed in drying baker and dry at 130 DEG C after dry 24 hours within 8 hours, obtains solid precursor in 80 DEG C, it is ground into powder presoma after being placed in Muffle furnace by solid precursor at 500 DEG C calcining 5 minutes, is heated to 700 DEG C with the heating rate of 4 DEG C/min after be incubated one hour at 300 DEG C by Powdered presoma and is incubated 9h and obtains the Li of Fluorin doped2MnO3(Li2MnO2.94F0.06).
Adopt the method identical with comparative example 1 to prepare CR2025 type button room temperature battery, its capacity, high rate performance, cyclical stability are tested (voltage 2.0-4.8V).Test result shows, under the electric current density of 5mA/g, and Li2MnO2.94F0.06Discharge capacity first be 196.3mAh/g, after circulating 20 times, capacity is 115mAh/g, and the conservation rate of capacity is 58.6%.
Embodiment three
Weigh 5.2778gLiNO3、6.9211gMn(CH3COO)2And 0.0943gLiF is dissolved in 20ml deionized water and forms saline solution, by 38.0153g citric acid with adding formation mixed solution in aforementioned salt solution after 30ml deionized water dissolving, mixed solution pH to 9 is adjusted with ammonia, subsequently mixed solution is placed on continuously stirred 6 hours of constant temperature 80 DEG C on magnetic force heating stirrer, obtains liquid precursor.Liquid precursor is placed in drying baker and dry at 150 DEG C after dry 16 hours within 8 hours, obtains solid precursor in 80 DEG C, it is ground into powder presoma after being placed in Muffle furnace by solid precursor at 450 DEG C calcining 7 minutes, is heated to 600 DEG C with the heating rate of 3 DEG C/min after be incubated 2 hours at 300 DEG C by Powdered presoma and is incubated 15h and obtains the Li of Fluorin doped2MnO3(Li2MnO2.91F0.09).
Adopt the method identical with comparative example 1 to prepare CR2025 type button room temperature battery, its capacity, high rate performance, cyclical stability are tested (voltage 2.0-4.8V).Test result shows, under the electric current density of 5mA/g, and Li2MnO2.91F0.09Discharge capacity first be 188.4mAh/g, after circulating 20 times, capacity is 116.4mAh/g, and the conservation rate of capacity is 61.8%.
Embodiment four
Weigh 4.9621gCH3COOLi、7.1576gMn(NO3)2And 0.1258gLiF is dissolved in 10ml deionized water and forms saline solution, by 12.6718g citric acid with adding formation mixed solution in aforementioned salt solution after 20ml deionized water dissolving, mixed solution pH to 8 is adjusted with ammonia, subsequently mixed solution is placed on continuously stirred 6 hours of constant temperature 80 DEG C on magnetic force heating stirrer, obtains liquid precursor.Liquid precursor is placed in drying baker and dry at 130 DEG C after dry 24 hours within 12 hours, obtains solid precursor in 60 DEG C, it is ground into powder presoma after being placed in Muffle furnace by solid precursor at 500 DEG C calcining 7 minutes, is heated to 700 DEG C with the heating rate of 2 DEG C/min after be incubated one hour at 350 DEG C by Powdered presoma and is incubated 9h and obtains the Li of Fluorin doped2MnO3(Li2MnO2.88F0.12).
Adopt the method identical with comparative example 1 to prepare CR2025 type button room temperature battery, its capacity, high rate performance, cyclical stability are tested (voltage 2.0-4.8V).Test result shows, under the electric current density of 5mA/g, and Li2MnO2.88F0.12Discharge capacity first be 172.4mAh/g, after circulating 20 times, capacity is 112.7mAh/g, and the conservation rate of capacity is 65.4%.
By the above detailed description to the embodiment of the present invention, it will be appreciated that the invention solves conventional Li2MnO3Material electricity rate is led low, and electro-chemical activity is poor, the problem that cycle performance and discharge capacity are all relatively low, and the cost of material of employing is low, and synthesis temperature is low, prepared Fluorin doped Li2MnO3Electro-chemical activity is excellent, and under the electric current density of 5mA/g, first discharge specific capacity, at 172.4～209.1mAh/g, is maintained at 112.7～139.9mAh/g after 20 circulations, and conservation rate is 58.6～66.9%.
It is understood that the principle that is intended to be merely illustrative of the present of embodiment of above and the illustrative embodiments that adopts, but the invention is not limited in this.For those skilled in the art, without departing from the spirit and substance in the present invention, it is possible to make various modification and improvement, these modification and improvement are also considered as protection scope of the present invention.
Claims (3)
1. a preparation method for positive electrode active material for lithium ion battery, described positive active material is the Li of Fluorin doped2MnO3, its composition formula is: Li2MnO3-xFx, wherein 0.03≤x≤0.12, it is characterised in that comprise the following steps:
(1) lithium salts is weighed, manganese salt and lithium fluoride, it is dissolved in deionized water and is configured to saline solution, described lithium salts is in lithium, manganese salt is in manganese, lithium salts, the mol ratio of manganese salt and lithium fluoride is 2-x:1:x, in saline solution, manganese element molar concentration is 2～5mol/L, the aqueous citric acid solution that concentration is 3～6mol/L is added aforementioned salt solution is formed mixed solution, citric acid is 0.5～1.5:1 with the mol ratio of metal cation in saline solution, mixed solution pH value is regulated to 7～9 subsequently with ammonia, again mixed solution is stirred 6～8 hours at 60～80 DEG C, make solution that sufficient complexation to occur, form colloidal sol, obtain liquid precursor；
(2) at 130～150 DEG C, 8～12h is heated at 60～80 DEG C after step (1) gained liquid precursor being heated 16～24 hours, it is thus achieved that solid precursor；
(3) grind after step (2) gained solid precursor being calcined 3～7 minutes at 450～500 DEG C, obtain Powdered presoma, again the pre-burning at 300～350 DEG C of Powdered presoma was heated to 600～700 DEG C with the programming rate of 2-4 DEG C/min after 1～2 hour, and it is incubated 9～15h, obtain the Li of Fluorin doped after furnace cooling2MnO3, namely obtain positive electrode active material for lithium ion battery；
Step (1) described lithium salts includes any one in lithium nitrate, lithium carbonate, lithium acetate；Described manganese salt includes any one in manganese nitrate, manganese carbonate, manganese acetate.
2. a lithium ion battery positive pole, it is characterised in that include positive electrode active material for lithium ion battery prepared by method according to claim 1.
3. a lithium ion battery, it is characterised in that use lithium ion battery positive pole according to claim 2.
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| JP6872705B2 (en) | 2015-07-23 | 2021-05-19 | パナソニックＩｐマネジメント株式会社 | Positive electrode active material and battery |
| CN107408688A (en) | 2015-09-16 | 2017-11-28 | 松下知识产权经营株式会社 | Positive active material and battery |
| WO2017047019A1 (en) | 2015-09-16 | 2017-03-23 | パナソニックＩｐマネジメント株式会社 | Battery |
| WO2017047021A1 (en) * | 2015-09-16 | 2017-03-23 | パナソニックＩｐマネジメント株式会社 | Positive electrode active material and battery |
| CN107431203B (en) | 2015-09-16 | 2021-08-20 | 松下知识产权经营株式会社 | Positive electrode active material and battery |
| JP6861403B2 (en) | 2015-09-16 | 2021-04-21 | パナソニックＩｐマネジメント株式会社 | battery |
| CN107431242B (en) | 2015-09-16 | 2021-03-23 | 松下知识产权经营株式会社 | Battery with a battery cell |
| WO2017047018A1 (en) * | 2015-09-16 | 2017-03-23 | パナソニックＩｐマネジメント株式会社 | Battery |
| JP6861402B2 (en) | 2015-09-16 | 2021-04-21 | パナソニックＩｐマネジメント株式会社 | battery |
| JP6952251B2 (en) | 2016-11-15 | 2021-10-20 | パナソニックＩｐマネジメント株式会社 | Positive electrode active material for batteries and batteries |
| JP6979586B2 (en) | 2016-11-15 | 2021-12-15 | パナソニックＩｐマネジメント株式会社 | Positive electrode active material for batteries and batteries using positive electrode active materials for batteries |
| DE102016223246A1 (en) * | 2016-11-24 | 2018-05-24 | Robert Bosch Gmbh | Active material for a positive electrode of a battery cell, positive electrode and battery cell |
| JP6964246B2 (en) | 2016-12-02 | 2021-11-10 | パナソニックＩｐマネジメント株式会社 | Positive electrode active material and battery using positive electrode active material |
| JP6952247B2 (en) | 2017-01-19 | 2021-10-20 | パナソニックＩｐマネジメント株式会社 | Positive electrode active material and battery |
| JP7065341B2 (en) | 2017-01-19 | 2022-05-12 | パナソニックＩｐマネジメント株式会社 | Positive electrode active material and battery |
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| CN102790209A (en) * | 2011-05-19 | 2012-11-21 | 中国科学院宁波材料技术与工程研究所 | Positive pole material of lithium ion battery and preparation method thereof |
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| Title |
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| "New investigation of fluorine-substituted spinel LiMn2O4−xFx by using sol–gel process";J.T.Son等;《Journal of Power Sources》;20050801;第147卷(第1-2期);第220～226页 * |
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