CN105609753A - Preparation method for one-dimensional multi-layer porous fibrous positive electrode material of lithium ion battery - Google Patents
Preparation method for one-dimensional multi-layer porous fibrous positive electrode material of lithium ion battery Download PDFInfo
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- CN105609753A CN105609753A CN201510943863.7A CN201510943863A CN105609753A CN 105609753 A CN105609753 A CN 105609753A CN 201510943863 A CN201510943863 A CN 201510943863A CN 105609753 A CN105609753 A CN 105609753A
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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
- 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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- 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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a preparation method for a one-dimensional multi-layer porous fibrous Li(Ni<0.333>Co<0.333>Mn<0.333>)O2 ternary positive electrode material of a lithium ion battery. The method comprises the following steps of carrying out ion exchange between calcium alginate fiber spun by a wet method and metal bivalent nickel ions, cobalt ions and manganese ions; immersing the exchanged calcium alginate fiber in a lithium carbonate/absolute ethanol suspension liquid; taking out and drying the calcium alginate fiber; and carrying out high-temperature oxidation on the calcium alginate fiber with a tubular furnace. According to the preparation method, alginate fiber is taken as a biomass material and is a green and environment-friendly fiber new material; moreover, the preparation method is simple, and the obtained multi-layer fibrous Li(Ni<0.333>Co<0.333>Mn<0.333>)O2 ternary positive electrode material has relatively high specific capacity, cycle stability and rate performance due to the special one-dimensional multi-layer porous structure and is widely applied to the fields of electronic products, an electric bicycle, an electromobile and the like.
Description
Technical field
The invention belongs to lithium ion battery material field, be specifically related to multi-layer fiber shape lithium prepared by a kind of ion-exchange fromSub-battery Li (Ni0.333Co0.333Mn0.333)O2The preparation method of tertiary cathode material.
Background technology
Ternary layered Li (Ni0.333Co0.333Mn0.333)O2Anode material for lithium-ion batteries, high owing to thering is reversible capacity,Safe, the advantages such as environmentally safe, are considered to the ideal chose of anode material for lithium-ion batteries. TraditionalLi(Ni0.333Co0.333Mn0.333)O2The synthetic method of tertiary cathode material comprises coprecipitation, high temperature solid-state method, sol-gal processDeng. But the chunk products that these methods obtain often duct is undeveloped, the specific area of material is little, thereby hinders lithium ionEfficient fully diffusion, thereby cause high rate performance bad, the shortcoming such as specific capacity is lower, is restricting the extensive use of ternary material.
Consider with first-class problem, the present invention utilizes alginate fibre for masterplate, and first alginate fibre is to utilize from natural seaweedThe alginic acid of middle extraction is raw material, the high-performance fiber of a kind of green making by wet spinning, the secondly carboxylic in alginate fibreBase and hydroxyl can with bivalent metal ion (Ni2+，Co2+，Mn2+) forming stable Egg tray structure chelate, the two has embodiedWell binding ability, the carboxyl in alginate fibre can utilize electrostatic interaction absorption Li simultaneously+, fiber bone after high-temperature processThe carbon of frame, nitrogen, hydrogen meeting thermal decomposition, thus the continuous enrichment of metal forms the multi-layer porous fibrous tertiary cathode material of one dimension, this materialThe one-dimentional structure of material not only provides more effective electrode and electrolyte liquor contact area, and provides shorter for the transmission of lithium ionPath, thus the doubly forthright of ternary material effectively improved. Secondly, sandwich construction provide more lithium ion transmission passage andShort transmission path, contributes to improve the specific capacity of material and doubly forthright. Loose structure on fibre wall can cushion due to lithium simultaneouslyThe pressure that what ion produced when deintercalation repeatedly cause material lattice Volume Changes to produce, is conducive to improve the cyclical stability of material.Therefore, one dimension multi-layer fiber shape Li (Ni0.333Co0.333Mn0.333)O2Tertiary cathode material will be a feasible raising tertiary cathodeMaterial specific capacity, the method for forthright and cyclical stability doubly.
Summary of the invention
The object of the invention is to overcome existing lithium ion battery Li (Ni0.333Co0.333Mn0.333)O2Tertiary cathode material existsSpecific capacity relatively low, the shortcoming such as high rate performance is poor, less stable, seeks to prepare a kind of height ratio capacity of green,Lithium ion Li (the Ni of the forthright and high stability of high power0.333Co0.333Mn0.333)O2Tertiary cathode utmost point material.
The multi-layer porous fibrous Li (Ni of lithium ion battery one dimension that the present invention proposes0.333Co0.333Mn0.333)O2Tertiary cathode materialThe preparation method of material, comprises the following steps:
1. a certain amount of calcium alginate fibre and finite concentration hydrochloric acid carry out ion-exchange through ultrasonic processing, and exchange is fallen in calcium alginate fibreCalcium ion.
2. nickel acetate, cobalt acetate and manganese acetate that the alginic acid fibre of step 1 being handled well joins finite concentration ratio mixIn solution, fully mix, make fiber and nickel ion, cobalt ions, manganese ion generation ion-exchange.
3. fiber step 2 being obtained joins in certain density lithium carbonate/(water+ethanol) suspension and fully mixes,Obtain eventually load and only have the Precursors of Fibers of lithium ion, nickel cobalt and manganese.
4. by the Precursors of Fibers of step 3 high-temperature oxydation in tube furnace.
The product of step 5 is fully dry 5., obtain the multi-layer porous fibrous tertiary cathode material of one dimension.
Described calcium alginate fibre is wet spinning system.
The described ultrasonic dispersion of abundant mixing, ultrasonic power is 30W, jitter time is 30min.
Described in step 1, concentration of hydrochloric acid is 0.5mol/L-3mol/L.
Described in step 2, the concentration of nickel cobalt manganese mixed solution is 0.025mol/L-0.1mol/L, and ratio is 1: 1: 1.
Described in step 3, the concentration of lithium carbonate suspension is 0.05-0.2mol/L, and the ratio of water and ethanol is 1: 2.
Described in step 4, oxidizing temperature is 850-950 DEG C.
Compared with prior art, the invention has the beneficial effects as follows and use a kind of alginate fibre of environmental protection as masterplate, profitWith one dimension passage quickening lithium ion and the electronics transfer of the multi-layer porous fibrous tertiary cathode material of one dimension obtaining after high-temperature oxydation,Multilayer porous structure, particularly is conducive to diffusion and the transmission of lithium ion and electronics, thereby improves the charge/discharge capacity of ternary material, improves doublyForthright, the secondary particle of constituent material can cushion the lattice Volume Changes producing due to lithium ion deintercalation in charge and discharge process, makesMaterial has possessed extraordinary cyclical stability.
Brief description of the drawings
The multi-layer porous fibrous Li (Ni of Fig. 1 one dimension0.333Co0.333Mn0.333)O2The Electronic Speculum picture of electrode material
The multi-layer porous fibrous Li (Ni of Fig. 2 one dimension0.333Co0.333Mn0.333)O2The cycle performance curve of electrode material
The multi-layer porous fibrous Li (Ni of Fig. 3 one dimension0.333Co0.333Mn0.333)O2The multiplying power discharging characteristic of electrode material
The multi-layer porous fibrous Li (Ni of Fig. 4 one dimension0.333Co0.333Mn0.333)O2The first charge-discharge curve of electrode material
Embodiment
Embodiment mono-: take 2g calcium alginate fibre, use deionized water soaking and washing once, by the calcium alginate cleaningFiber is immersed in the hydrochloric acid solution that concentration that 200mL deionized water is configured to is 1mol/L, ultrasonic processing 40 minutes,Filtration after ultrasonic completing, then be dipped in hydrochloric acid, in triplicate. Subsequently alginic acid fibre is joined to 200mL deionized waterThe concentration being configured to is in the nickel acetate, cobalt acetate, manganese acetate mixed solution of 0.1mol/L, floods 30 minutes. By what obtainFiber floods 30min in lithium carbonate/(water+ethanol) aaerosol solution of 0.1mol/L, dries afterwards in vacuum drying oven. By fibreDimension is warmed up to 850 DEG C in tube furnace, and heating rate is 2 DEG C/min, is oxidized 8h in air, and rear cool to room temperature, obtainsThe multi-layer porous fibrous tertiary cathode material of one dimension.
Embodiment bis-: take 2g calcium alginate fibre, use deionized water soaking and washing once, the calcium alginate fibre cleaning is soakedIn the hydrochloric acid solution that the concentration that bubble is configured in 200mL deionized water is 1mol/L, ultrasonic processing 40 minutes, ultrasonic completeAfter becoming, filter, then be dipped in hydrochloric acid, in triplicate. Subsequently alginic acid fibre being joined to 200mL deionized water is configured toThe concentration nickel acetate that is 0.1mol/L, cobalt acetate, manganese acetate mixed solution in, flood 30 minutes. The fiber obtaining is existedIn lithium carbonate/(water+ethanol) aaerosol solution of 0.1mol/L, flood 30min, in vacuum drying oven, dry afterwards. Fiber is managedIn formula stove, be warmed up to 900 DEG C, heating rate is 2 DEG C/min, is oxidized 8h in air, and rear cool to room temperature, obtains one dimension manyLayer porous fibre shape tertiary cathode material.
Embodiment tri-: take 2g calcium alginate fibre, use deionized water soaking and washing once, the calcium alginate fibre cleaning is soakedIn the hydrochloric acid solution that the concentration that bubble is configured in 200mL deionized water is 1mol/L, ultrasonic processing 40 minutes, ultrasonic completeAfter becoming, filter, then be dipped in hydrochloric acid, in triplicate. Subsequently alginic acid fibre being joined to 200mL deionized water is configured toThe concentration nickel acetate that is 0.025mol/L, cobalt acetate, manganese acetate mixed solution in, flood 30 minutes. By the fiber obtainingIn lithium carbonate/(water+ethanol) aaerosol solution of 0.05mol/L, flood 30min, in vacuum drying oven, dry afterwards. Fiber is existedIn tube furnace, be warmed up to 950 DEG C, heating rate is 2 DEG C/min, is oxidized 8h in air, and rear cool to room temperature, obtains one dimensionMulti-layer porous fibrous tertiary cathode material.
Embodiment tetra-: take 2g calcium alginate fibre, use deionized water soaking and washing once, the calcium alginate fibre cleaning is soakedIn the hydrochloric acid solution that the concentration that bubble is configured in 200mL deionized water is 1mol/L, ultrasonic processing 40 minutes, ultrasonic completeAfter becoming, filter, then be dipped in hydrochloric acid, in triplicate. Subsequently alginic acid fibre being joined to 200mL deionized water is configured toThe concentration nickel acetate that is 0.025mol/L, cobalt acetate, manganese acetate mixed solution in, flood 30 minutes. By the fiber obtainingIn lithium carbonate/(water+ethanol) aaerosol solution of 0.2mol/L, flood 30min, in vacuum drying oven, dry afterwards. Fiber is existedIn tube furnace, be warmed up to 900 DEG C, heating rate is 2 DEG C/min, is oxidized 8h in air, and rear cool to room temperature, obtains one dimensionMulti-layer porous fibrous tertiary cathode material.
Claims (7)
1. the multi-layer porous fibrous Li (Ni of one dimension0.333Co0.333Mn0.333)O2The preparation method of tertiary cathode material, is characterized in that:Use the living beings new material alginic acid fibre of environmental protection as template, prepare one dimension by ion exchange and high-temperature heat treatment manyLayer porous fibre shape Li (Ni0.333Co0.333Mn0.333)O2Tertiary cathode material.
2. the multi-layer porous fibrous Li (Ni of one dimension according to claim 10.333Co0.333Mn0.333)O2The system of tertiary cathode materialPreparation Method, is characterized in that: realize bivalent metal ion and lithium ion is combined with alginate fibre by ion-exchange, and then obtainOne dimension fibre shape Li (Ni0.333Co0.333Mn0.333)O2Tertiary cathode material.
3. multi-layer fiber shape Li (Ni according to claim 20.333Co0.333Mn0.333)O2The preparation method of tertiary cathode material,It is characterized in that: first calcium alginate fibre is immersed in the hydrochloric acid solution of 0.5mol/L-3mol/L, calcium alginate is fallen in exchangeCalcium ion in fiber, subsequently alginic acid fibre being added to concentration is nickel/cobalt/manganese mixed salt solution of 0.025mol/L-0.1mol/LIn, the alginic acid nickel/cobalt/manganese fiber obtaining, by dry above-mentioned fiber impregnation the lithium salts of 0.025mol/L-0.1mol/L/(water+Ethanol) solution 30min, in vacuum drying oven, dry afterwards, then fiber is warmed up in tube furnace to 900 DEG C, speed heats upRate is 2 DEG C/min, is oxidized 8h in air, and rear cool to room temperature obtains the multi-layer porous fibrous tertiary cathode material of one dimension.
4. preparation method according to claim 3, is characterized in that: hydrochloric acid solution can use salpeter solution, sulfuric acid solution to replace,Concentration is 0.5mol/L-3mol/L.
5. preparation method according to claim 3, is characterized in that: nickel/cobalt/manganese salt is nickel acetate, cobalt acetate, manganese acetate and nitreAcid nickel, cobalt nitrate and manganese nitrate, concentration is 0.025mol/L-0.1mol/L.
6. preparation method according to claim 3, is characterized in that: lithium salts is lithium carbonate, lithium nitrate, lithium acetate.
7. preparation method according to claim 3, is characterized in that: oxidizing temperature is 850 DEG C-950 DEG C, and carbonization time is 6-12h, heating rate is 1-5 DEG C/min.
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Cited By (10)
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| CN106207114A (en) * | 2016-07-19 | 2016-12-07 | 青岛富强新材料科技有限公司 | A kind of preparation method of low ferrum lithium porous LiFePO4 positive electrode |
| CN106814111A (en) * | 2017-02-13 | 2017-06-09 | 山东旭晟东阳新材料科技有限公司 | A kind of hollow porous SnO2Micro-pipe gas sensor and preparation method thereof |
| CN107579258A (en) * | 2017-08-02 | 2018-01-12 | 中北大学 | One-dimensional multilayer takes off the air electrode of zinc-air cell method for preparing catalyst of lithium defect |
| CN107715883A (en) * | 2017-10-26 | 2018-02-23 | 青岛大学 | A kind of Ni3The preparation method of FeN@graphenes/marine alga aeroge elctro-catalyst |
| CN108365189A (en) * | 2018-01-10 | 2018-08-03 | 青岛大学 | A kind of preparation method of metal sulfide@carbon fibre composite anode material of lithium-ion batteries |
| CN108950736A (en) * | 2018-08-22 | 2018-12-07 | 贵州森环活性炭有限公司 | Nanoporous carbon fiber and preparation method thereof |
| CN108963218A (en) * | 2018-07-09 | 2018-12-07 | 王丹亮 | A kind of preparation method and application of the nickelic ternary lithium of low cobalt |
| CN109244379A (en) * | 2017-09-14 | 2019-01-18 | 太原理工大学 | A kind of LiFePO4The preparation method of ultrathin nanometer piece@graphene aerogel positive electrode |
| CN111315686A (en) * | 2017-09-13 | 2020-06-19 | 尤尼弗瑞克斯 I 有限责任公司 | Silicon-based anode material for lithium ion battery |
| CN112713261A (en) * | 2019-10-24 | 2021-04-27 | 中国石油化工股份有限公司 | Preparation method of ternary cathode material and lithium ion battery containing ternary cathode material |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106207114A (en) * | 2016-07-19 | 2016-12-07 | 青岛富强新材料科技有限公司 | A kind of preparation method of low ferrum lithium porous LiFePO4 positive electrode |
| CN106814111A (en) * | 2017-02-13 | 2017-06-09 | 山东旭晟东阳新材料科技有限公司 | A kind of hollow porous SnO2Micro-pipe gas sensor and preparation method thereof |
| CN107579258A (en) * | 2017-08-02 | 2018-01-12 | 中北大学 | One-dimensional multilayer takes off the air electrode of zinc-air cell method for preparing catalyst of lithium defect |
| CN111315686A (en) * | 2017-09-13 | 2020-06-19 | 尤尼弗瑞克斯 I 有限责任公司 | Silicon-based anode material for lithium ion battery |
| US11652201B2 (en) | 2017-09-13 | 2023-05-16 | Unifrax I Llc | Silicon-based anode material for lithium ion battery |
| CN109244379A (en) * | 2017-09-14 | 2019-01-18 | 太原理工大学 | A kind of LiFePO4The preparation method of ultrathin nanometer piece@graphene aerogel positive electrode |
| CN109244379B (en) * | 2017-09-14 | 2021-06-22 | 太原理工大学 | LiFePO4Preparation method of ultrathin nanosheet @ graphene aerogel positive electrode material |
| CN107715883A (en) * | 2017-10-26 | 2018-02-23 | 青岛大学 | A kind of Ni3The preparation method of FeN@graphenes/marine alga aeroge elctro-catalyst |
| CN108365189A (en) * | 2018-01-10 | 2018-08-03 | 青岛大学 | A kind of preparation method of metal sulfide@carbon fibre composite anode material of lithium-ion batteries |
| CN108963218A (en) * | 2018-07-09 | 2018-12-07 | 王丹亮 | A kind of preparation method and application of the nickelic ternary lithium of low cobalt |
| CN108950736A (en) * | 2018-08-22 | 2018-12-07 | 贵州森环活性炭有限公司 | Nanoporous carbon fiber and preparation method thereof |
| CN112713261A (en) * | 2019-10-24 | 2021-04-27 | 中国石油化工股份有限公司 | Preparation method of ternary cathode material and lithium ion battery containing ternary cathode material |
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