CN109244379B - LiFePO4Preparation method of ultrathin nanosheet @ graphene aerogel positive electrode material - Google Patents

LiFePO4Preparation method of ultrathin nanosheet @ graphene aerogel positive electrode material Download PDF

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CN109244379B
CN109244379B CN201710855921.XA CN201710855921A CN109244379B CN 109244379 B CN109244379 B CN 109244379B CN 201710855921 A CN201710855921 A CN 201710855921A CN 109244379 B CN109244379 B CN 109244379B
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graphene
sodium alginate
graphene aerogel
lifepo
ultrathin nanosheet
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CN109244379A (en
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王兵
杨东江
胡江亮
王建成
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Taiyuan University of Technology
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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
    • H01M4/364—Composites as mixtures
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • 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
    • 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
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • 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

The invention discloses LiFePO4The preparation method of the ultrathin nanosheet @ graphene aerogel lithium ion battery cathode material comprises the step of mixing sodium alginate and graphene to obtain hydrosol and Fe3+，PO4 3‑，Li+Performing ion exchange to obtain Li-Fe-P sodium alginate graphene hydrogel, freeze-drying to obtain Li-Fe-P alginic acid/graphene aerogel, and roasting at high temperature in a tube furnace under nitrogen to obtain LiFePO4Ultrathin nanosheet @ graphene aerogel. The sodium alginate used in the preparation method is a biomass material, is a green and environment-friendly new material, and the preparation method is simple, so that the obtained LiFePO is4Ultrathin nanosheet @ graphene aerogel [010 ] due to ultrathin nanosheet @ graphene aerogel]The lithium ion battery has high specific capacity, cycling stability and rate capability towards a lithium diffusion channel and a special three-dimensional porous conductive network. The method is widely applied to the fields of electronic products, electric bicycles, electric automobiles and the like.

Description

LiFePO4Preparation method of ultrathin nanosheet @ graphene aerogel positive electrode material
Technical Field
The invention belongs to the field of lithium ion battery materials, and particularly relates to LiFePO prepared by an ion exchange method4A preparation method of an ultrathin nanosheet @ graphene aerogel positive electrode material is provided.
Background
Olivine-type LiFePO4The positive electrode material of the lithium ion battery is safe due to high reversible capacityHigh performance, no environmental pollution and the like, and is considered as an ideal choice for the anode material of the lithium ion battery. Conventional LiFePO4The synthesis method of the anode material comprises a coprecipitation method, a high-temperature solid phase method, a carbothermic method, a hydrothermal method, a solvothermal method and the like. However, the bulk products obtained by these methods often lengthen the one-dimensional diffusion channel of lithium ions, and hinder efficient and sufficient diffusion of lithium ions, thereby resulting in poor rate capability, undeveloped pore channels, small specific surface area of the material, and thus low specific capacity, and the like, and restrict LiFePO4The method is widely applied to large-scale electric equipment.
In view of the problems, the invention utilizes sodium alginate/graphene as a carbon source, firstly sodium alginate is a raw material extracted from natural seaweed, secondly carboxyl and hydroxyl in seaweed fiber can form stable egg box structure chelate with iron ions, the two reflect good binding capacity, and simultaneously carboxyl in seaweed fiber can adsorb Li by utilizing electrostatic action+This inhibits aggregation of lithium iron phosphate particles during high temperature processing, thereby obtaining ultra-thin LiFePO4Nanosheets, which can greatly shorten Li+[010 ] of]To lithium diffusion passageway, the three-dimensional multistage pore structure of graphite alkene aerogel not only provides more effective electrode electrolyte area of contact simultaneously, has effectively improved LiFePO moreover4Thereby effectively improving the LiFePO4The specific capacity and the rate capability of the ultrathin nanosheet @ graphene aerogel. Secondly, the three-dimensional multilevel pore channel structure can buffer the pressure generated by the change of the material lattice volume caused by the repeated deintercalation of lithium ions, and meanwhile, the network structure of the three-dimensional graphene is used as ultrathin LiFePO4The distribution framework of the nano-sheets greatly enhances the stability of the whole structure and is beneficial to improving the cycling stability of the material. Thus, LiFePO4The ultrathin nanosheet @ graphene aerogel cathode material is a feasible LiFePO4The specific capacity, the multiplying power and the cycling stability of the anode material.
Disclosure of Invention
The invention aims to overcome the defect of LiFePO of the existing lithium ion battery4Specific volume of positive electrode materialThe preparation method has the defects of relatively low capacity, poor rate capability, poor stability and the like, and seeks to prepare green LiFePO with high specific capacity, high rate capability and high stability4And (3) a positive electrode material.
The invention provides LiFePO of a lithium ion battery4The preparation method of the ultrathin nanosheet @ graphene aerogel cathode material comprises the following steps:
1. and preparing the sodium alginate/graphene hydrosol by dissolving sodium alginate in water to obtain the hydrosol and adding a certain amount of graphene.
2. And (3) adding a mixed solution of ferric nitrate, ammonium dihydrogen phosphate and lithium nitrate with a certain concentration ratio into the sodium alginate/graphene hydrosol treated in the step (1) and fully mixing to enable the sodium alginate to perform ion exchange with iron ions, phosphate ions and lithium ions. And obtaining the sodium alginate/graphene hydrogel loaded with only iron ions, phosphate ions and lithium ions.
3. And (3) freezing the hydrogel obtained in the step (2) in an ultralow temperature refrigerator (-70 ℃) for 12h, taking out the hydrogel, immediately putting the hydrogel into a freeze dryer, and drying the hydrogel for 48h to obtain the Li-Fe-P alginic acid/graphene aerogel.
4. Introducing Ar/H to the aerogel obtained in the step 3 in a tube furnace2Calcining the mixed gas for 8 hours at 700 ℃ to obtain LiFePO4Ultrathin nanosheet @ graphene aerogel positive electrode material.
The concentration of the sodium alginate hydrosol in the step 1 is 1-2 wt%, and the addition amount of the graphene is 2-10% of the sodium alginate.
And 2, the concentration of the mixed solution of the ferric nitrate, the ammonium dihydrogen phosphate and the lithium nitrate is 0.1-0.4 mol/L, and the ratio is 1: 1.
The freezing temperature in the step 3 is-60-80 ℃, the freezing time is 10-24h, and the drying time is 48-36 h.
In the step 4, the calcining temperature is 650-850 ℃, the carbonization time is 6-12h, and the heating rate is 1-5 ℃/min.
Compared with the prior art, the invention has the beneficial effects that the raw material used in the invention is mainly sodium alginate, the sodium alginate is extracted from seaweed, the source is wide, the environment is protected, and the invention is greenAnd the safety is high. Prepared LiFePO4Ultrathin nanosheet @ graphene aerogel [010 ] due to ultrathin nanosheet @ graphene aerogel]Has higher specific capacity, cycling stability and rate capability to lithium diffusion channels and special three-dimensional porous conductive networks due to commercial LiFePO4。
Drawings
FIG. 1 LiFePO4An electron microscope picture of the ultrathin nanosheet @ graphene aerogel.
FIG. 2 LiFePO4TEM picture of ultra-thin nanometer piece @ graphene aerogel.
FIG. 3 LiFePO4AFM pictures of ultrathin nanosheet @ graphene aerogel.
FIG. 4 LiFePO4The rate discharge characteristic of the ultrathin nanosheet @ graphene aerogel is disclosed.
FIG. 5 LiFePO4The cycling stability of the ultrathin nanosheet @ graphene aerogel is improved.
Examples
The first embodiment is as follows: 0.404g of sodium alginate is dissolved in 40g of the secondary deionized water solution, and the mixture is stirred for 6 to 8 hours to obtain 1wt% of uniformly mixed sodium alginate hydrosol which is marked as solution 1.
And (3) mixing 0.008g of graphene into the sodium alginate hydrosol prepared above, and stirring for 6-8 hours to obtain the sodium alginate graphene hydrosol, which is marked as solution 2.
A mixed solution of 0.1mol/L ferric nitrate, ammonium dihydrogen phosphate and lithium nitrate was prepared and recorded as solution 3.
And pouring the solution 2 into a 10ml syringe, dripping the solution into the solution 3 through the syringe to form the Li-Fe-P alginic acid graphene hydrogel, and standing for 2-3 hours after dripping is finished.
The hydrogel obtained above was separated and washed 3 times with secondary deionized water.
And (3) putting the cleaned Li-Fe-P alginic acid graphene hydrogel into an ultralow temperature refrigerator (70 ℃ below zero) for freezing for 12h, taking out the hydrogel, immediately putting the hydrogel into a freeze dryer for drying for 48h, and obtaining the Li-Fe-P alginic acid/graphene aerogel.
Putting Li-Fe-P-alginic acid/graphene aerogel into a tubular furnace for calcination, and introducing Ar/H2Calcining the mixed gas for 8 hours at 700 ℃ to obtain LiFePO4Ultrathin nanosheet @ graphene aerogel positive electrode material.
The LiFePO obtained above is subjected to4The ultrathin nanosheet @ graphene aerogel positive electrode material is subjected to electrochemical testing by using a blue testing system.
Example 2
0.404g of sodium alginate is dissolved in 40g of the secondary deionized water solution, and the mixture is stirred for 6 to 8 hours to obtain 1wt% of uniformly mixed sodium alginate hydrosol which is marked as solution 1.
0.040g of graphene is mixed into the sodium alginate solution prepared above, and stirring is carried out for 6-8 hours, so as to obtain the mixed hydrosol of the sodium alginate graphene, which is marked as solution 2.
A mixed solution of 0.4mol/L ferric nitrate, ammonium dihydrogen phosphate and lithium nitrate was prepared and recorded as solution 3.
And pouring the solution 2 into a 10ml syringe, dripping the solution into the solution 3 through the syringe to form the Li-Fe-P alginic acid graphene hydrogel, and standing for 2-3 hours after dripping is finished.
The hydrogel obtained above was separated and washed 3 times with secondary deionized water.
And (3) putting the cleaned Li-Fe-P alginic acid graphene hydrogel into an ultralow temperature refrigerator (minus 60 ℃) for freezing for 12h, taking out the frozen Li-Fe-P alginic acid graphene hydrogel, immediately putting the frozen Li-Fe-P alginic acid graphene hydrogel into a freeze dryer for drying for 48h, and obtaining the Li-Fe-P-alginic acid/graphene aerogel.
Putting Li-Fe-P-alginic acid/graphene aerogel into a tubular furnace for calcination, introducing Ar/H2Calcining the mixed gas for 6 hours at 800 ℃ to obtain LiFePO4Ultrathin nanosheet @ graphene aerogel positive electrode material.
The LiFePO obtained above is subjected to4The ultrathin nanosheet @ graphene aerogel positive electrode material is subjected to electrochemical testing by using a blue testing system.

Claims (5)

1. LiFePO4The preparation method of the ultrathin nanosheet @ graphene aerogel cathode material is characterized by comprising the following steps of: using sodium alginate and graphene as raw materials, firstly dissolving the sodium alginate in water to obtain seaweedAdding a certain amount of graphene into sodium hydrosol, uniformly mixing, adding a salt mixed solution of iron ions/phosphate ions/lithium ions with the concentration of 0.025mol/L-0.1mol/L into the sodium hydrosol to obtain Fe-P-Li sodium alginate/graphene hydrogel, freezing the obtained Fe-Li-P sodium alginate/graphene/hydrogel in an ultra-low temperature refrigerator, immediately putting the frozen hydrogel into a freeze dryer for freeze drying to obtain Fe-Li-P sodium alginate/graphene aerogel, and performing freeze drying on the Fe-Li-P sodium alginate/graphene aerogel in Ar/H2Calcining in atmosphere to obtain LiFePO4Ultrathin nanosheet @ graphene aerogel positive electrode material.
2. The LiFePO according to claim 14The preparation method of the ultrathin nanosheet @ graphene aerogel cathode material is characterized by comprising the following steps of: the concentration of the sodium alginate hydrosol is 1-2 wt%, and the addition amount of the graphene is 2-10 wt% of the sodium alginate.
3. The LiFePO according to claim 14The preparation method of the ultrathin nanosheet @ graphene aerogel cathode material is characterized by comprising the following steps of: the iron ion/phosphate ion/lithium ion salt mixed solution is a mixed salt solution of ferric nitrate, ammonium dihydrogen phosphate and lithium nitrate, and the concentration of the mixed salt solution is 0.1-0.4 mol/L.
4. The LiFePO according to claim 14The preparation method of the ultrathin nanosheet @ graphene aerogel cathode material is characterized by comprising the following steps of: the freezing temperature is-60-80 ℃, the freezing time is 10-24h, and the drying time is 48-36 h.
5. The LiFePO according to claim 14The preparation method of the ultrathin nanosheet @ graphene aerogel cathode material is characterized by comprising the following steps of: the calcining temperature is 650-850 ℃, the carbonization time is 6-12h, and the heating rate is 1-5 ℃/min.
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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
CN112151800A (en) * 2020-09-18 2020-12-29 成都新柯力化工科技有限公司 High-tap-density honeycomb lithium battery positive electrode material and preparation method thereof

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