CN105609721A - Preparation method for three-dimensional carbon net coated lithium manganese borate composite positive electrode material - Google Patents
Preparation method for three-dimensional carbon net coated lithium manganese borate composite positive electrode material 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
A preparation method for a three-dimensional carbon net coated lithium manganese borate composite positive electrode material is disclosed. The preparation method comprises the following steps of (1) dissolving a lithium source, a manganese source, a boron source and critic acid into deionized water at a molar ratio of lithium to manganese to boron to critic acid of 1:1:1:1-5, and controlling the concentration of metal manganese ions to be 0.01-0.15mol/L; (2) putting to water bath at a temperature of 60-100 DEG C and stirring for 4-12h, and uniformly mixing to form sol; (3) drying the sol to be gel-shaped to obtain a lithium manganese borate precursor; and (4) sintering the lithium manganese borate precursor under protective atmosphere at a temperature of 500-800 DEG C for 8-22h, and then performing furnace cooling to room temperature to obtain the three-dimensional carbon net coated lithium manganese borate composite positive electrode material. The obtained three-dimensional carbon net coated lithium manganese borate composite positive electrode material is high in specific discharge capacity, excellent in rate capability, good in charge-discharge characteristics, and long in service life; and in addition, the preparation method is simple in process, and low in required reaction temperature.
Description
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries, be specifically related to a kind of method that uses sol-gel technique to prepare the coated manganese borate lithium composite positive pole of three-dimensional carbon net.
Background technology
The survival and development of the energy and human society are closely related, and sustainable development is the whole mankind's common aspiration and the objective of the struggle. Fossil energy very soon can be exhausted, and this is everybody common recognition. Green secondary cell is a kind of high effect cleaning new energy devices can be recycled, and is a kind of important technological approaches of comprehensively alleviating the energy, resources and environment problem. And the feature such as lithium ion battery has that energy density is high, security performance good, pollution-free, memory-less effect, low price has become one of " green secondary power supply " of having at present good development prospect. The plurality of advantages of lithium ion battery becomes and solves energy crisis, alleviates strong " the green secondary power supply " for candidate of environmental pollution.
Borate family positive electrode LiMnBO3There is the structural advantage as anode material for lithium-ion batteries, its two kinds of crystal structure forms, monoclinic system and hexagonal crystal system have three-dimensional frame structure, and this structure has more stability than the material of two-dimentional frame structure and can be Li+Embedding/deintercalation broader diffusion admittance is provided. Meanwhile, due to borate (BO3)3-There is less molal weight (M=58.8g/mol), therefore, LiMnBO3There is higher theoretical specific capacity (～220mAh/g). But, comprise LiMnBO3Reversible deintercalation ability at interior borate family electrode material to lithium, initial discharge capacity and reversible specific capacity are all lower. At present, the method for preparing manganese borate lithium is mostly solid phase method, has primary particle large, reunite serious, and the shortcoming that specific capacity is lower. Therefore, need that one can be prepared granule, structure is special badly, and the good LiMnBO of high rate capability3Novel method.
The disclosed lithium ion battery LiMnBO of CN103943857A3/ KB composite positive pole, the specific discharge capacity under C/40, C/20, C/10, C/5 multiplying power is only 127mAh/g, 114mAh/g, 112mAh/g, 98mAh/g, far below theoretical capacity.
CN104821390A discloses a kind of preparation of anode material for lithium-ion batteries manganese borate lithium/Graphene. Its preparation adopts spray drying process, and sample purity is low, and degree of crystallinity is not high, and under high magnification, decay is serious.
CN104064773A discloses the preparation method of the coated manganese borate lithium anode material of a kind of lithium ion battery carbon, and its technical scheme is at 700～850 DEG C of calcining 12～24h, but specific discharge capacity is only 83.0mAh/g under 0.1C current density.
CN105047873A discloses the preparation method of the coated manganese borate lithium composite positive pole of a kind of carbon in lithium ion battery, and its technical scheme is the manganese borate lithium that goes out the hexagonal structure of pure phase at 800～850 DEG C of sintering, and sintering temperature is too high, consumes energy higher.
CN102403505B discloses a kind of preparation method of lithium ion battery cathode material in-situ carbon coated lithium manganese borate composite material, adopt solid phase method, but primary particle is more than 500nm～2 μ m, reunites serious.
CN103833044A discloses a kind of preparation method of anode material for lithium-ion batteries manganese borate lithium, is to adopt freeze drying-solid-phase sintering preparation method, but its complicated operation, resulting materials is not carbon clad structure, can not embody good high rate performance.
Said method carrys out composite electrode material with solid phase method, and its shortcoming exists primary particle large exactly, reunites serious, and carbon is coated inhomogeneous defect, easily causes air poisoning effect.
Summary of the invention
Technical problem to be solved by this invention is, overcomes the above-mentioned defect that prior art exists, and provides a kind of products obtained therefrom purity high, and specific discharge capacity is high, high rate performance excellence, the preparation method of the coated manganese borate lithium composite positive pole of three-dimensional carbon net simple to operate.
The technical solution adopted for the present invention to solve the technical problems is as follows: the preparation method of the coated manganese borate lithium composite positive pole of a kind of three-dimensional carbon net, comprises the following steps:
(1) ratio that is 1:1:1:1～5 by lithium source, manganese source, boron source and citric acid according to the mol ratio of elemental lithium, manganese element, boron element and citric acid is dissolved in deionized water, and the concentration of controlling manganese metal ion is 0.01～0.15mol/L;
(2) step (1) gained solution is placed in to 60～100 DEG C of stirred in water bath 4～12h, mixes formation colloidal sol;
(3) step (2) gained colloidal sol is dried as gel, obtains manganese borate lithium presoma;
(4) by step (3) gained manganese borate lithium presoma in protective atmosphere, at 500～800 DEG C, sintering 8～22h, cools to room temperature with the furnace, obtains the coated manganese borate lithium composite positive pole of three-dimensional carbon net.
Further, in step (1), the concentration of controlling manganese metal ion is 0.05～0.10mol/L. Lithium, manganese, boron element ratio are according to the stoichiometric proportion of reaction, select citric acid to use as complexing agent and carbon source, because such as oxalic acid and all more difficult formation colloidal sol of glucose, if and the too low meeting of consumption is unfavorable for the formation of carbon net clad structure and the generation of collosol and gel, do not have the effect that increases electric conductivity yet, if the too high carbon content that can cause again of consumption is too high, specific discharge capacity reduces. The object of controlling the concentration of manganese metal ion is, if the too low meeting of the concentration of manganese metal ion causes output too low, if too high meeting causes the generation of impurity.
Further, in step (2), the temperature of described water-bath is 70～90 DEG C, and the time of stirring is 5～10h. If the temperature of water-bath is too low or the too high formation that is all unfavorable for colloidal sol, the described water-bath time is in actual experiment, to be easy to the time that colloidal sol forms most, if overlong time can directly form precipitation on the contrary.
Further, in step (3), described dry temperature is 80～120 DEG C, and the dry time is 2～6h. Described baking temperature is too low can increase drying time, and too high meeting increases manganese borate lithium granular precursor.
Further, in step (4), the temperature of described sintering is 650～750 DEG C, and the time of sintering is 10～20h. Described sintering temperature and time draw after thermogravimetric analysis and experimental exploring, if the manganese borate lithium of the too low hexagonal structure that can not form pure phase of sintering temperature will cause nucleus increase sharply if sintering temperature is too high, properties of product reduce.
Further, in step (4), described protective atmosphere is argon gas, nitrogen, hydrogen, carbon monoxide or hydrogen/argon-mixed; The volumetric concentration of described hydrogen/argon-mixed middle hydrogen is 4～8%. Be to uprise with the valence state that stops manganese by appropriate increase hydrogen reduction atmosphere with hydrogen/argon-mixed as protective atmosphere, but the too high meeting of density of hydrogen cause dangerous. The high-purity gas of preferred purity >=99.99% of described protective atmosphere.
Further, in step (1), described lithium source is one or more in lithium carbonate, lithium nitrate, lithium fluoride, lithium oxalate, lithium dihydrogen phosphate, lithium hydroxide, lithium acetate or lithium chloride etc.
Further, in step (1), described manganese source is one or more in four hydration manganese acetates, Manganous sulfate monohydrate or two oxalic acid hydrate manganese etc.
Further, in step (1), described boron source is one or more in boric acid, ammonium borate or diboron trioxide etc.
Manganese borate lithium anode material prepared by the inventive method, its microstructure is that manganese borate lithium is covered by three-dimensional carbon web frame equably; Chemistry homogeneity is good, and chemical reaction more easily carries out compared with solid reaction, has the tiny and highly purified advantage of particle; The coated structure of three-dimensional carbon net can further prevent that wherein manganese borate lithium particle is grown up; and can increase lithium ion transmittability and improve electric conductivity; the simultaneously protection of carbon net can reduce the haptoreaction of active material and air, moisture etc.; thereby effectively reduce its surface poisoning effect, improve multiplying power, the cycle performance of material.
The coated manganese borate lithium composite positive pole of the inventive method gained three-dimensional carbon net is under 1.0～4.8V voltage, 0.1C first discharge specific capacity can reach 184.3mAh/g, 0.5C first discharge specific capacity can reach 136.1mAh/g, 1C first discharge specific capacity can reach 118mAh/g, the obvious lifting of high rate performance, illustrated that its electrical conductivity is improved greatly, after 1C circulation 20 times, still kept 101.5mAh/g, the polarization of excellent cycle performance testimonial material greatly reduces. Visible, the coated manganese borate lithium composite positive pole of the inventive method gained three-dimensional carbon net has excellent chemical property, has represented good charge-discharge characteristic and cycle life, has effectively solved the poor shortcoming of circulation, high rate performance of material.
The raw materials used wide material sources of the inventive method, technological process is simple, reacts temperature required low.
Brief description of the drawings
Fig. 1 is the XRD figure of the coated manganese borate lithium composite positive pole of the embodiment of the present invention 1 gained three-dimensional carbon net;
Fig. 2 is the TEM figure of the coated manganese borate lithium composite positive pole of the embodiment of the present invention 1 gained three-dimensional carbon net;
Fig. 3 is the Raman spectrogram of the coated manganese borate lithium composite positive pole of the embodiment of the present invention 1 gained three-dimensional carbon net;
Fig. 4 is the battery of assembling of the manganese borate lithium composite positive pole coated with the embodiment of the present invention 1 gained three-dimensional carbon net curve of charge and discharge first under 0.1C, 0.5C and 1C multiplying power.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the invention will be further described.
The high-purity hydrogen that the embodiment of the present invention is used and purity >=99.99% of high-purity argon gas; The chemical reagent using, if no special instructions, all obtains by conventional commercial sources.
Embodiment 1
(1) take lithium nitrate 0.005mol, four hydration manganese acetate 0.005mol, boric acid 0.005mol, citric acid 0.005mol, is dissolved in the deionized water of 100mL;
(2) step (1) gained solution is placed in to 80 DEG C of stirred in water bath 6h, mixes formation colloidal sol;
(3) step (2) gained colloidal sol is placed in to baking oven, at 120 DEG C, dry 2h is gel, obtains manganese borate lithium presoma;
(4) step (3) gained manganese borate lithium presoma is placed in to pipe type sintering furnace, in High Purity Hydrogen/argon-mixed atmosphere (hydrogen volume concentration is 5%), at 750 DEG C, sintering 10h, naturally cools to room temperature with stove, obtains the coated manganese borate lithium composite positive pole of three-dimensional carbon net.
The assembling of battery: take the prepared LiMnBO of 0.32g the present embodiment3Positive electrode, add 0.04g acetylene black as conductive agent and 0.04g Kynoar (PVDF) as binding agent, after fully grinding, add 2mLN-methyl pyrrolidone (NMP) as solvent, disperse to mix, size mixing to after evenly, on the thick aluminium foil of 16 μ m, slurry is made into positive plate, in the glove box that is full of argon gas taking metal lithium sheet as negative pole, taking Celgard2300 as barrier film, 1mol/LLiPF6/ EC:DMC:EMC(volume ratio 1:1:1) be electrolyte, be assembled into the button cell of CR2025. Battery is surveyed in 1.0～4.8V voltage range to its charge/discharge capacity and high rate performance, wherein the first discharge specific capacity under 0.1C, 0.5C, 1C multiplying power is followed successively by 184.3mAh/g, 136.1mAh/g, 118mAh/g(is as shown in Figure 4), after 1C circulation 20 times, still keep the specific discharge capacity of 101.5mAh/g.
As seen from Figure 1, the XRD diffraction maximum of the coated manganese borate lithium composite positive pole of gained three-dimensional carbon net is consistent with hexagonal structure manganese borate lithium standard card, without other dephasigns, illustrates that purity is higher, and wherein, carbon is amorphous form, so carbon-free peak occurs herein.
As seen from Figure 2, the coated manganese borate lithium composite positive pole of gained three-dimensional carbon net is three-dimensional carbon net clad structure, and wherein, ellipticity particle is manganese borate lithium, and what around light and shade was staggered is carbon net.
As seen from Figure 3, the coated manganese borate lithium composite positive pole of gained three-dimensional carbon net is positioned at 1352cm-1And 1593cm-1Corresponding disordered carbon and the in order vibration peak of carbon respectively, proved that the tridimensional network that Fig. 2 China and foreign countries bread covers is carbon.
Embodiment 2
(1) take lithium acetate 0.01mol, Manganous sulfate monohydrate 0.01mol, diboron trioxide 0.005mol, citric acid 0.05mol, is dissolved in the deionized water of 100mL;
(2) step (1) gained solution is placed in to 90 DEG C of stirred in water bath 5h, mixes formation colloidal sol;
(3) step (2) gained colloidal sol is placed in to air dry oven, at 110 DEG C, dry 4h is gel, obtains manganese borate lithium presoma;
(4) step (3) gained manganese borate lithium presoma is placed in to pipe type sintering furnace, in high-purity argon gas atmosphere, at 700 DEG C, sintering 15h, naturally cools to room temperature with stove, obtains the coated manganese borate lithium composite positive pole of three-dimensional carbon net.
The assembling of battery: take the prepared LiMnBO of 0.32g the present embodiment3Positive electrode, add 0.04g acetylene black as conductive agent and 0.04g Kynoar (PVDF) as binding agent, after fully grinding, add 2mLN-methyl pyrrolidone (NMP) as solvent, disperse to mix, size mixing to after evenly, on the thick aluminium foil of 16 μ m, slurry is made into positive plate, in the glove box that is full of argon gas taking metal lithium sheet as negative pole, taking Celgard2300 as barrier film, 1mol/LLiPF6/ EC:DMC:EMC(volume ratio 1:1:1) be electrolyte, be assembled into the button cell of CR2025. Battery is surveyed in 1.0～4.8V voltage range to its charge/discharge capacity and high rate performance, wherein the first discharge specific capacity under 0.1C, 0.5C, 1C multiplying power is followed successively by 178.2mAh/g, 126.5mAh/g, 102.7mAh/g, still keeps the specific discharge capacity of 86.3mAh/g after 1C circulation 20 times.
Embodiment 3
(1) take lithium dihydrogen phosphate 0.008mol, two oxalic acid hydrate manganese 0.008mol, boric acid 0.008mol, citric acid 0.024mol, is dissolved in the deionized water of 100mL;
(2) step (1) gained solution is placed in to 70 DEG C of stirred in water bath 10h, mixes formation colloidal sol;
(3) step (2) gained colloidal sol is placed in to baking oven, at 80 DEG C, dry 6h is gel, obtains manganese borate lithium presoma;
(4) step (3) gained manganese borate lithium presoma is placed in to pipe type sintering furnace, in high-purity argon gas atmosphere, at 800 DEG C, sintering 8h, naturally cools to room temperature with stove, obtains the coated manganese borate lithium composite positive pole of three-dimensional carbon net.
The assembling of battery: take the prepared LiMnBO of 0.32g the present embodiment3Positive electrode, add 0.04g acetylene black as conductive agent and 0.04g Kynoar (PVDF) as binding agent, after fully grinding, add 2mLN-methyl pyrrolidone (NMP) as solvent, disperse to mix, size mixing to after evenly, on the thick aluminium foil of 16 μ m, slurry is made into positive plate, in the glove box that is full of argon gas taking metal lithium sheet as negative pole, taking Celgard2300 as barrier film, 1mol/LLiPF6/ EC:DMC:EMC(volume ratio 1:1:1) be electrolyte, be assembled into the button cell of CR2025. Battery is surveyed in 1.0～4.8V voltage range to its charge/discharge capacity and high rate performance, wherein the first discharge specific capacity under 0.1C, 0.5C, 1C multiplying power is followed successively by 167.4mAh/g, 126.1mAh/g, 98.3mAh/g, still keeps the specific discharge capacity of 85.2mAh/g after 1C circulation 20 times.
Claims (9)
1. a preparation method for the coated manganese borate lithium composite positive pole of three-dimensional carbon net, is characterized in that, comprises the following steps:
(1) ratio that is 1:1:1:1～5 by lithium source, manganese source, boron source and citric acid according to the mol ratio of elemental lithium, manganese element, boron element and citric acid is dissolved in deionized water, and the concentration of controlling manganese metal ion is 0.01～0.15mol/L;
(2) step (1) gained solution is placed in to 60～100 DEG C of stirred in water bath 4～12h, mixes formation colloidal sol;
(3) step (2) gained colloidal sol is dried as gel, obtains manganese borate lithium presoma;
(4) by step (3) gained manganese borate lithium presoma in protective atmosphere, at 500～800 DEG C, sintering 8～22h, cools to room temperature with the furnace, obtains the coated manganese borate lithium composite positive pole of three-dimensional carbon net.
2. the preparation method of the coated manganese borate lithium composite positive pole of three-dimensional carbon net according to claim 1, is characterized in that: in step (1), the concentration of controlling manganese metal ion is 0.05～0.10mol/L.
3. according to the preparation method of the coated manganese borate lithium composite positive pole of three-dimensional carbon net described in claim 1 or 2, it is characterized in that: in step (2), the temperature of described water-bath is 70～90 DEG C, and the time of stirring is 5～10h.
4. according to the preparation method of the coated manganese borate lithium composite positive pole of the described three-dimensional carbon net of one of claim 1～3, it is characterized in that: in step (3), described dry temperature is 80～120 DEG C, and the dry time is 2～6h.
5. according to the preparation method of the coated manganese borate lithium composite positive pole of the described three-dimensional carbon net of one of claim 1～4, it is characterized in that: in step (4), the temperature of described sintering is 650～750 DEG C, and the time of sintering is 10～20h.
6. according to the preparation method of the coated manganese borate lithium composite positive pole of the described three-dimensional carbon net of one of claim 1～5, it is characterized in that: in step (4), described protective atmosphere is argon gas, nitrogen, hydrogen, carbon monoxide or hydrogen/argon-mixed; The volumetric concentration of described hydrogen/argon-mixed middle hydrogen is 4～8%.
7. according to the preparation method of the coated manganese borate lithium composite positive pole of the described three-dimensional carbon net of one of claim 1～6, it is characterized in that: in step (1), described lithium source is one or more in lithium carbonate, lithium nitrate, lithium fluoride, lithium oxalate, lithium dihydrogen phosphate, lithium hydroxide, lithium acetate or lithium chloride.
8. according to the preparation method of the coated manganese borate lithium composite positive pole of the described three-dimensional carbon net of one of claim 1～7, it is characterized in that: in step (1), described manganese source is one or more in four hydration manganese acetates, Manganous sulfate monohydrate or two oxalic acid hydrate manganese.
9. according to the preparation method of the coated manganese borate lithium composite positive pole of the described three-dimensional carbon net of one of claim 1～8, it is characterized in that: in step (1), described boron source is one or more in boric acid, ammonium borate or diboron trioxide.
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| CN113809319A (en) * | 2021-08-03 | 2021-12-17 | 广东邦普循环科技有限公司 | High-performance lithium nickel cobalt manganese oxide positive electrode material for power battery and preparation method of high-performance lithium nickel cobalt manganese oxide positive electrode material |
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