CN105609753B - The preparation method of one-dimensional multi-layer porous fibrous anode material for lithium-ion batteries - Google Patents
The preparation method of one-dimensional multi-layer porous fibrous anode material for lithium-ion batteries Download PDFInfo
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- CN105609753B CN105609753B CN201510943863.7A CN201510943863A CN105609753B CN 105609753 B CN105609753 B CN 105609753B CN 201510943863 A CN201510943863 A CN 201510943863A CN 105609753 B CN105609753 B CN 105609753B
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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 kind of one-dimensional multi-layer porous threadiness Li (Ni0.333Co0.333Mn0.333)O2The preparation method of ternary cathode material of lithium ion battery, this method is by the calcium alginate fibre and metallic divalent nickel ion of wet process spinning, cobalt ions, manganese ion carries out ion exchange, alginic acid fibre after exchange is immersed in lithium carbonate/dehydrated alcohol suspension, drying is taken out afterwards, then is made after tube furnace high-temperature oxydation.Alginate fibre used in the preparation method is biological material, is environmentally protective new fiber materials, and preparation method is simple, gained multi-layer fiber shape Li (Ni0.333Co0.333Mn0.333)O2Tertiary cathode material specific capacity with higher, cyclical stability and high rate performance due to its special one-dimensional multilayer porous structure, particularly.It is widely used in electronic product, the fields such as electric bicycle and electric car.
Description
Technical field
The invention belongs to field of lithium ion battery material, and in particular to a kind of multi-layer fiber shape lithium of ion-exchange preparation
Ion battery Li (Ni0.333Co0.333Mn0.333)O2The preparation method of tertiary cathode material.
Background technique
Ternary layered Li (Ni0.333Co0.333Mn0.333)O2Anode material for lithium-ion batteries, due to reversible capacity
Height, it is highly-safe, the advantages that no pollution to the environment, it is considered to be the ideal chose of anode material for lithium-ion batteries.Traditional Li
(Ni0.333Co0.333Mn0.333)O2The synthetic method of tertiary cathode material includes coprecipitation, high temperature solid-state method, sol-gal process
Deng.However, often duct is undeveloped for the obtained chunk products of these methods, the specific surface area of material is small, to hinder lithium ion
Efficient abundant diffusion, specific capacity lower the disadvantages of bad so as to cause high rate performance restrict answering extensively for ternary material
With.
In view of it is above the problems such as, the present invention is template using alginate fibre, and alginate fibre is using from natural sea first
The alginic acid extracted in algae is raw material, a kind of high-performance fiber of green as made from wet spinning, secondly in alginate fibre
Carboxyl and hydroxyl can be with bivalent metal ion (Ni2+, Co2+, Mn2+) stable Egg tray structure chelate is formed, the two embodies
Good binding ability, while carboxyl in alginate fibre can adsorb Li using electrostatic interaction+, the fiber after high-temperature process
The carbon of skeleton, nitrogen, hydrogen can thermally decompose, and metal is constantly enriched with to form one-dimensional multi-layer porous fibrous tertiary cathode material, should
The one-dimentional structure of material provides not only more effective electrode and electrolyte liquor contact area, and provides more for the transmission of lithium ion
Short path, to effectively improve the forthright again of ternary material.Secondly, multilayered structure provides the logical of more lithium ion transports
Road and short transmission path help to improve the specific capacity of material and forthright again.The porous structure on fibre wall can buffer simultaneously
Due to lithium ion repeatedly deintercalation when generate cause material lattice volume change generate pressure, be conducive to improve material circulation
Stability.Therefore, one-dimensional multi-layer fiber shape Li (Ni0.333Co0.333Mn0.333)O2Tertiary cathode material will be one and feasible mention
High tertiary cathode material specific capacity, again forthright and cyclical stability method.
Summary of the invention
It is an object of the invention to overcome existing lithium ion battery Li (Ni0.333Co0.333Mn0.333)O2Tertiary cathode material
The disadvantages of existing specific capacity is relatively low, and high rate performance is poor, and stability is poor seeks the Fabrication of High Specific Capacitance for preparing a kind of green
Amount, the forthright lithium ion Li (Ni with high stability of high power0.333Co0.333Mn0.333)O2Tertiary cathode pole material.
The one-dimensional multi-layer porous threadiness Li (Ni of lithium ion battery proposed by the present invention0.333Co0.333Mn0.333)O2Ternary is just
The preparation method of pole material, comprising the following steps:
1. a certain amount of calcium alginate fibre and the sonicated carry out ion exchange of a certain concentration hydrochloric acid, seaweed is fallen in exchange
Calcium ion in sour calcium fiber.
2. nickel acetate, cobalt acetate and manganese acetate that the alginic acid fibre that step 1 is handled well is added to a certain concentration ratio
It is sufficiently mixed in mixed solution, so that ion exchange occurs for fiber and nickel ion, cobalt ions, manganese ion.
3. the fiber that step 2 is obtained is added in certain density lithium carbonate/(water+ethyl alcohol) suspension and is sufficiently mixed,
Finally obtain the Precursors of Fibers that load only has lithium ion, nickel cobalt manganese ion.
4. the Precursors of Fibers of step 3 is aoxidized in tube furnace high temperature.
5. the product of step 5 is sufficiently dry, obtain one-dimensional multi-layer porous fibrous tertiary cathode material.
The calcium alginate fibre is wet spinning.
Described is sufficiently mixed ultrasonic disperse, ultrasonic power 30W, jitter time 30min.
Concentration of hydrochloric acid described in step 1 is 0.5mol/L-3mol/L.
The concentration of nickel cobalt manganese mixed solution described in step 2 is 0.025mol/L-0.1mol/L, ratio 1: 1: 1.
The concentration of lithium carbonate suspension described in step 3 is 0.05-0.2mol/L, and the ratio of water and ethyl alcohol is 1: 2.
Oxidizing temperature described in step 4 is 850-950 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows use a kind of environmentally protective alginate fibre as template,
Accelerate lithium ion and electronics in one-dimensional channel using the one-dimensional multi-layer porous fibrous tertiary cathode material obtained after high-temperature oxydation
Transfer, multilayer porous structure, particularly is conducive to the diffusion and transmission of lithium ion and electronics, so that the charge/discharge capacity of ternary material is improved,
Improvement is forthright again, and the secondary particle of constituent material can buffer the cell volume generated in charge and discharge process due to lithium ion deintercalation
Variation, makes material have extraordinary cyclical stability.
Detailed description of the invention
The one-dimensional multi-layer porous threadiness Li (Ni of Fig. 10.333Co0.333Mn0.333)O2The electron microscopic picture of electrode material
The one-dimensional multi-layer porous threadiness Li (Ni of Fig. 20.333Co0.333Mn0.333)O2The cycle performance curve of electrode material
The one-dimensional multi-layer porous threadiness Li (Ni of Fig. 30.333Co0.333Mn0.333)O2The rate discharge characteristic of electrode material
The one-dimensional multi-layer porous threadiness Li (Ni of Fig. 40.333Co0.333Mn0.333)O2The first charge-discharge curve of electrode material
Embodiment
Embodiment one: weighing 2g calcium alginate fibre, primary with deionized water soaking and washing, the calcium alginate that will be cleaned
It is to be ultrasonically treated 40 minutes, ultrasound in the hydrochloric acid solution of 1mol/L that fiber, which is immersed in the concentration that 200mL deionized water is configured to,
It filters, then is dipped into hydrochloric acid after the completion, in triplicate.Alginic acid fibre is then added to 200mL deionized water to be configured to
Concentration be the nickel acetate of 0.1mol/L, cobalt acetate, in manganese acetate mixed solution, impregnate 30 minutes.Obtained fiber is existed
30min is impregnated in the lithium carbonate of 0.1mol/L/(water+ethyl alcohol) aaerosol solution, is dried in vacuum drying oven later.By fiber in pipe
Be warming up to 850 DEG C in formula furnace, heating rate is 2 DEG C/min, aoxidize 8h in air, after be cooled to room temperature, it is more to obtain one-dimensional multilayer
Hole threadiness tertiary cathode material.
Embodiment two: weighing 2g calcium alginate fibre, primary with deionized water soaking and washing, the calcium alginate that will be cleaned
It is to be ultrasonically treated 40 minutes, ultrasound in the hydrochloric acid solution of 1mol/L that fiber, which is immersed in the concentration that 200mL deionized water is configured to,
It filters, then is dipped into hydrochloric acid after the completion, in triplicate.Alginic acid fibre is then added to 200mL deionized water to be configured to
Concentration be the nickel acetate of 0.1mol/L, cobalt acetate, in manganese acetate mixed solution, impregnate 30 minutes.Obtained fiber is existed
30min is impregnated in the lithium carbonate of 0.1mol/L/(water+ethyl alcohol) aaerosol solution, is dried in vacuum drying oven later.By fiber in pipe
Be warming up to 900 DEG C in formula furnace, heating rate is 2 DEG C/min, aoxidize 8h in air, after be cooled to room temperature, it is more to obtain one-dimensional multilayer
Hole threadiness tertiary cathode material.
Embodiment three: weighing 2g calcium alginate fibre, primary with deionized water soaking and washing, the calcium alginate that will be cleaned
It is to be ultrasonically treated 40 minutes, ultrasound in the hydrochloric acid solution of 1mol/L that fiber, which is immersed in the concentration that 200mL deionized water is configured to,
It filters, then is dipped into hydrochloric acid after the completion, in triplicate.Alginic acid fibre is then added to 200mL deionized water to be configured to
Concentration be the nickel acetate of 0.025mol/L, cobalt acetate, in manganese acetate mixed solution, impregnate 30 minutes.Obtained fiber is existed
30min is impregnated in the lithium carbonate of 0.05mol/L/(water+ethyl alcohol) aaerosol solution, is dried in vacuum drying oven later.Fiber is existed
Be warming up to 950 DEG C in tube furnace, heating rate is 2 DEG C/min, aoxidize 8h in air, after be cooled to room temperature, obtain one-dimensional multilayer
Porous fibrous tertiary cathode material.
Example IV: weighing 2g calcium alginate fibre, primary with deionized water soaking and washing, the calcium alginate that will be cleaned
It is to be ultrasonically treated 40 minutes, ultrasound in the hydrochloric acid solution of 1mol/L that fiber, which is immersed in the concentration that 200mL deionized water is configured to,
It filters, then is dipped into hydrochloric acid after the completion, in triplicate.Alginic acid fibre is then added to 200mL deionized water to be configured to
Concentration be the nickel acetate of 0.025mol/L, cobalt acetate, in manganese acetate mixed solution, impregnate 30 minutes.Obtained fiber is existed
30min is impregnated in the lithium carbonate of 0.2mol/L/(water+ethyl alcohol) aaerosol solution, is dried in vacuum drying oven later.By fiber in pipe
Be warming up to 900 DEG C in formula furnace, heating rate is 2 DEG C/min, aoxidize 8h in air, after be cooled to room temperature, it is more to obtain one-dimensional multilayer
Hole threadiness tertiary cathode material.
Claims (6)
1. one-dimensional multi-layer porous threadiness Li (Ni0.333Co0.333Mn0.333)O2The preparation method of tertiary cathode material, feature exist
In: it uses the biomass new material alginic acid fibre of environmental protection as template, bivalent metal ion Ni is realized by ion exchange2+,
Co2+, Mn2+In conjunction with alginate fibre, obtained alginic acid nickel cobalt manganese fiber, after by dry above-mentioned fiber impregnation lithium salts/
In (water+ethyl alcohol) solution, the Precursors of Fibers that load only has lithium ion, nickel cobalt manganese ion is obtained, using high-temperature oxydation, in turn
Obtain one-dimensional multi-layer porous threadiness Li (Ni0.333Co0.333Mn0.333)O2Tertiary cathode material.
2. preparation method according to claim 1, it is characterised in that: calcium alginate fibre is immersed in 0.5mol/L- first
In the hydrochloric acid solution of 3mol/L, the calcium ion in calcium alginate fibre is fallen in exchange, is then by alginic acid fibre addition concentration
In the nickel cobalt manganese mixed salt solution of 0.025mol/L-0.1mol/L, after by dry above-mentioned fiber impregnation in 0.025mol/L-
The lithium salts of 0.1mol/L/(water+ethyl alcohol) solution 30min, dries in vacuum drying oven later, then rises fiber in tube furnace
For temperature to 900 DEG C, heating rate is 2 DEG C/min, aoxidizes 8h in air, after be cooled to room temperature, obtain one-dimensional multi-layer porous threadiness
Tertiary cathode material.
3. preparation method according to claim 2, it is characterised in that: hydrochloric acid solution can be replaced with nitric acid solution, sulfuric acid solution,
Concentration is 0.5mol/L-3mol/L.
4. preparation method according to claim 2, it is characterised in that: nickel cobalt manganese salt be nickel acetate, cobalt acetate, manganese acetate and
Nickel nitrate, cobalt nitrate and manganese nitrate, concentration 0.025mol/L-0.1mol/L.
5. preparation method according to claim 2, it is characterised in that: lithium salts is lithium carbonate, lithium nitrate, lithium acetate.
6. preparation method according to claim 2, it is characterised in that: oxidizing temperature is 850 DEG C -950 DEG C, carbonization time 6-
12h, heating rate are 1-5 DEG C/min.
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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 |
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| 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 |
| GB201803983D0 (en) | 2017-09-13 | 2018-04-25 | Unifrax I Llc | Materials |
| CN109244379B (en) * | 2017-09-14 | 2021-06-22 | 太原理工大学 | LiFePO4Preparation method of ultrathin nanosheet @ graphene aerogel positive electrode material |
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| 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 |
| CN108963218B (en) * | 2018-07-09 | 2021-01-26 | 王丹亮 | Preparation method and application of low-cobalt high-nickel ternary lithium |
| 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 |
| CN112713261B (en) * | 2019-10-24 | 2023-04-07 | 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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| CN103000879A (en) * | 2012-12-19 | 2013-03-27 | 南开大学 | Preparation method of spinel type lithium-nickel-manganese oxide with one-dimensional porous structure |
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Address after: 266071 Shandong city of Qingdao province Ningxia City Road No. 308 Patentee after: QINGDAO University Address before: 266071 Ningxia Road, Shandong, China, No. 308, No. Patentee before: QINGDAO University |