CN109244379A - A kind of LiFePO4The preparation method of ultrathin nanometer piece@graphene aerogel positive electrode - Google Patents

A kind of LiFePO4The preparation method of ultrathin nanometer piece@graphene aerogel positive electrode Download PDF

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CN109244379A
CN109244379A CN201710855921.XA CN201710855921A CN109244379A CN 109244379 A CN109244379 A CN 109244379A CN 201710855921 A CN201710855921 A CN 201710855921A CN 109244379 A CN109244379 A CN 109244379A
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graphene
preparation
lifepo
graphene aerogel
sodium alginate
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CN109244379B (en
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杨东江
王兵
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

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Abstract

The invention discloses a kind of LiFePO4The preparation method of ultrathin nanometer piece@graphene aerogel anode material for lithium-ion batteries, this method are the hydrosol and Fe after mixing sodium alginate with graphene3+, PO4 3‑, Li+Ion exchange is carried out, obtains Li-Fe-P sodium alginate graphene hydrogel, then be freeze-dried to obtain Li-Fe-P alginic acid/graphene aerogel, LiFePO is made after high-temperature roasting under tube furnace nitrogen4Ultrathin nanometer piece@graphene aerogel.Seaweed sodium used in the preparation method is biological material, is environmentally protective new material, and preparation method is simple, gained LiFePO4Ultrathin nanometer piece@graphene aerogel specific capacity with higher, cyclical stability and high rate performance due to its ultra-thin [010] is to lithium diffusion admittance and special three-dimensional porous conductive network.It is widely used in electronic product, the fields such as electric bicycle and electric car.

Description

A kind of LiFePO4The preparation method of ultrathin nanometer piece@graphene aerogel positive electrode
Technical field
The invention belongs to field of lithium ion battery material, and in particular to a kind of LiFePO of ion-exchange preparation4It is ultra-thin The preparation method of nanometer sheet@graphene aerogel positive electrode.
Background technique
The LiFePO of olivine-type4Anode material for lithium-ion batteries, it is highly-safe due to high with reversible capacity, to ring The advantages that border is pollution-free, it is considered to be the ideal chose of anode material for lithium-ion batteries.Traditional LiFePO4The conjunction of positive electrode It include coprecipitation, high temperature solid-state method at method, carbothermic method, hydro-thermal and solvent-thermal method etc..However, these methods obtain Chunk products often make the one-dimensional diffusion admittance of lithium ion elongated, the efficient abundant diffusion of lithium ion is hindered, so as to cause again Rate performance is bad, and duct is undeveloped, and the specific surface area of material is small, thus, it the disadvantages of specific capacity is lower, restricts LiFePO4Extensive use in Large Electric equipment.
In view of it is above the problems such as, the present invention using sodium alginate/graphene be carbon source, first sodium alginate be using from The raw material extracted in natural seaweed, secondly the carboxyl in alginate fibre and hydroxyl can form stable Egg tray structure with iron ion Chelate, the two embody good binding ability, while the carboxyl in alginate fibre can adsorb Li using electrostatic interaction+, This can assemble through inhibition lithium iron phosphate particles in high-temperature process, to obtain ultra-thin LiFePO4Nanometer sheet, this can be big It is big to shorten Li+[010] to lithium diffusion admittance, while the three-dimensional multistage cellular structure of graphene aerogel provides not only and more has The electrode and electrolyte liquor contact area of effect, and effectively increase LiFePO4Conductivity, to effectively improve LiFePO4It is ultra-thin to receive The specific capacity and high rate performance of rice piece@graphene aerogel.Secondly three-dimensional multistage cellular structure can be buffered since lithium ion is anti- The pressure for causing material lattice volume change to generate generated when multiple deintercalation, while the network structure of three-dimensional grapheme is as ultra-thin LiFePO4The distribution skeleton of nanometer sheet is conducive to the stable circulation for improving material this greatly enhances integrally-built stability Property.Therefore, LiFePO4Ultrathin nanometer piece@graphene aerogel positive electrode will be a feasible raising LiFePO4Positive material Expect 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 LiFePO4Specific capacity existing for positive electrode is relatively It is low, the disadvantages of high rate performance is poor, and stability is poor, seek the height ratio capacity for preparing a kind of green, high power is forthright and high stable The LiFePO of property4Positive electrode.
Lithium ion battery LiFePO proposed by the present invention4The preparation side of ultrathin nanometer piece@graphene aerogel positive electrode Method, comprising the following steps:
1. configuration quality concentration, which is dissolved in water for sodium alginate, obtains the hydrosol, and a certain amount of graphene is added, sea is obtained Mosanom/graphene the hydrosol.
2. ferric nitrate, the phosphoric acid of a certain concentration ratio are added in the sodium alginate that step 1 is handled well/graphene hydrosol Ammonium dihydrogen and lithium nitrate mixed solution are sufficiently mixed, so that ion occurs for sodium alginate and iron ion, phosphate anion, lithium ion Exchange.Obtain sodium alginate/graphene hydrogel that load only has iron ion, phosphate anion, lithium ion.
3. (- 70 DEG C) freezing 12h, subsequent taking-up are immediately placed in freezing and do in ultra low temperature freezer by the hydrogel of step 2 Dry 48h, obtains Li-Fe-P alginic acid/graphene aerogel in dry machine.
4. the aeroge of step 3 is led to Ar/H in tube furnace2Mixed gas, 700 DEG C of calcining 8h, obtains LiFePO4It is ultra-thin Nanometer sheet@graphene aerogel positive electrode.
The concentration of the sodium alginate hydrosol described in step 1 is 1wt%-2wt%, and graphene additional amount is sodium alginate 2%-10%.
The concentration of ferric nitrate, ammonium dihydrogen phosphate described in step 2 and lithium nitrate mixed solution is 0.1mol/L-0.4mol/L, Ratio is 1: 1: 1.
Cryogenic temperature described in step 3 is -60 DEG C -80 DEG C, cooling time 10-24h, drying time 48h-36h.
Calcination temperature described in step 4 is 650 DEG C -850 DEG C, carbonization time 6-12h, and heating rate is 1-5 DEG C/min.
It compared with prior art, is mainly alginic acid the beneficial effects of the invention are as follows the raw material for using a present invention to use Sodium, sodium alginate are extracted from seaweed, from a wealth of sources, environment-friendly and green, highly-safe.The LiFePO being prepared4 Ultrathin nanometer piece@graphene aerogel is due to its ultra-thin [010] is to lithium diffusion admittance and special three-dimensional porous conductive network Specific capacity with higher, cyclical stability and high rate performance, due to commercially using LiFePO4。
Detailed description of the invention
Fig. 1 LiFePO4The electron microscopic picture of ultrathin nanometer piece@graphene aerogel.
Fig. 2 LiFePO4The TEM picture of ultrathin nanometer piece@graphene aerogel.
Fig. 3 LiFePO4The AFM picture of ultrathin nanometer piece@graphene aerogel.
Fig. 4 LiFePO4The rate discharge characteristic of ultrathin nanometer piece@graphene aerogel.
Fig. 5 LiFePO4The cyclical stability of ultrathin nanometer piece graphene aerogel.
Embodiment
One: 0.404g sodium alginate of embodiment is dissolved in 40g secondary deionized water solution, is stirred 6-8 hours, is mixed The sodium alginate hydrosol of uniform 1wt%, is denoted as solution 1.
0.008g graphene is mixed into the sodium alginate hydrosol of above-mentioned preparation, stirs 6-8 hours, obtains sodium alginate stone The hydrosol of black alkene is denoted as solution 2.
Configuration concentration is ferric nitrate, ammonium dihydrogen phosphate and the lithium nitrate mixed solution of 0.1mol/L, is denoted as solution 3.
Solution 2 is poured into the syringe of 10ml, is instilled in solution 3 by syringe, Li-Fe-P alginic acid graphite is formed Alkene hydrogel after the completion of instillation, stands 2-3 hours.
Hydrogel obtained above is separated, and is cleaned 3 times with secondary deionized water.
The Li-Fe-P alginic acid graphene hydrogel obtained after cleaning is put into ultra low temperature freezer (- 70 DEG C) freezings 12h then takes out and is immediately placed in freeze drier dry 48h, obtains Li-Fe-P alginic acid/graphene aerogel.
Li-Fe-P- alginic acid/graphene aerogel is put into tube furnace and is calcined, Ar/H is led to2Mixed gas, 700 DEG C are forged 8h is burnt, LiFePO is obtained4Ultrathin nanometer piece@graphene aerogel positive electrode.
By above-mentioned obtained LiFePO4Ultrathin nanometer piece graphene aerogel positive electrode utilizes blue electrical measurement test system Carry out electro-chemical test.
Embodiment 2
0.404g sodium alginate is dissolved in 40g secondary deionized water solution, is stirred 6-8 hours, is obtained uniformly mixed The sodium alginate hydrosol of 1wt%, is denoted as solution 1.
0.040g ink alkene is mixed into the sodium alginate soln of above-mentioned preparation, stirs 6-8 hours, obtains sodium alginate graphite The mixing hydrosol of alkene, is denoted as solution 2.
Configuration concentration is ferric nitrate, ammonium dihydrogen phosphate and the lithium nitrate mixed solution of 0.4mol/L, is denoted as solution 3.
Solution 2 is poured into the syringe of 10ml, is instilled in solution 3 by syringe, Li-Fe-P alginic acid graphite is formed Alkene hydrogel after the completion of instillation, stands 2-3 hours.
Hydrogel obtained above is separated, and is cleaned 3 times with secondary deionized water.
The Li-Fe-P alginic acid graphene hydrogel obtained after cleaning is put into ultra low temperature freezer (- 60 DEG C) freezings 12h then takes out and is immediately placed in freeze drier dry 48h, obtains Li-Fe-P- alginic acid/graphene aerogel.
Li-Fe-P- alginic acid/graphene aerogel is put into tube furnace and is calcined, Ar/H is led to2Mixed gas, 800 DEG C are forged 6h is burnt, LiFePO is obtained4Ultrathin nanometer piece@graphene aerogel positive electrode.
By above-mentioned obtained LiFePO4Ultrathin nanometer piece graphene aerogel positive electrode utilizes blue electrical measurement test system Carry out electro-chemical test.

Claims (7)

1. a kind of LiFePO4The preparation method of ultrathin nanometer piece@graphene aerogel positive electrode, it is characterised in that: use environmental protection Biomass new material sodium alginate and graphene be raw material, pass through ion exchange, freeze-drying and high-temperature heat treatment system Standby LiFePO4The method of ultrathin nanometer piece@graphene aerogel positive electrode.
2. LiFePO according to claim 14The preparation method of ultrathin nanometer piece@graphene aerogel positive electrode, it is special Sign is: realizing iron ion, phosphate anion and lithium ion and sodium alginate/graphene aerogel knot by ion exchange It closes, and then obtains LiFePO4Ultrathin nanometer piece@graphene aerogel positive electrode.
3. LiFePO according to claim 24The preparation method of ultrathin nanometer piece@graphene aerogel positive electrode, it is special Sign is: it is first that sodium alginate is soluble in water, the sodium alginate hydrosol is obtained, a certain amount of graphene is added afterwards, mixing is equal After even, it is added in iron ion/phosphate anion/lithium ion mixed salt solution that concentration is 0.025mol/L-0.1mol/L In, obtained Fe-P-Li alginic acid/graphene hydrogel.By obtained Fe-Li-P- sodium alginate/graphene hydrogel super (- 70 DEG C) freezing 12h in low temperature refrigerator, then taking-up, which is immediately placed in freeze drier, is freeze-dried 48h, obtains Fe-Li-P- Sodium alginate/graphene aerogel, in Ar/H2700 DEG C of calcining 8h in atmosphere, heating rate are 2 DEG C/min, obtain LiFePO4It is super Thin nanometer sheet@graphene aerogel positive electrode.
4. preparation method according to claim 3, it is characterised in that: the concentration of the sodium alginate hydrosol is 1wt%-2wt%, Graphene additional amount is the 2%-10% of sodium alginate.
5. preparation method according to claim 3, it is characterised in that: iron ion/phosphate anion/lithium ion salt mixing is molten Liquid is ferric nitrate, ammonium dihydrogen phosphate, lithium nitrate.Concentration is 0.1mol/L-0.4mol/L.
6. preparation method according to claim 3, it is characterised in that: cryogenic temperature is -60 DEG C -80 DEG C, cooling time 10- For 24 hours, drying time 48h-36h.
7. preparation method according to claim 3, it is characterised in that: calcination temperature is 650 DEG C -850 DEG C, carbonization time 6- 12h, heating rate are 1-5 DEG C/min.
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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
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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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
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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