CN104868118A - Preparation method of sodium ion battery anode FePO4/Graphene composite - Google Patents

Preparation method of sodium ion battery anode FePO4/Graphene composite Download PDF

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Publication number
CN104868118A
CN104868118A CN201510160213.5A CN201510160213A CN104868118A CN 104868118 A CN104868118 A CN 104868118A CN 201510160213 A CN201510160213 A CN 201510160213A CN 104868118 A CN104868118 A CN 104868118A
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China
Prior art keywords
graphene
ion battery
fepo4
fepo
graphene composite
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CN201510160213.5A
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Chinese (zh)
Inventor
张俊喜
刘瑶
周义荣
戴念维
徐硕炯
范金辰
任平
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Shanghai University of Electric Power
University of Shanghai for Science and Technology
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Shanghai University of Electric Power
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Publication of CN104868118A publication Critical patent/CN104868118A/en
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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
    • 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
    • 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
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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
    • 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 relates to a preparation method of a sodium ion battery anode FePO4/Graphene composite. The FePO4/Graphene composite is synthesized once by a microemulsion method. FePO4 nano spherical particles are uniformly loaded on the two sides of graphene in a single layer by a non-covalent bond. Serving as a sodium ion battery anode material, the composite is unique and similar to a sandwich structure, and an electron conduction rate is greatly increased due to existence of the graphene. In addition, an FePO4 nano structure increases the surface area of an electrode material, and increases reversible extraction and insertion rates of Na<+> ions. Serving as the sodium ion battery anode material, the FePO4/Graphene composite represents an excellent electrochemical property. The microemulsion synthesis method adopted by the preparation method is simple in synthesis technology and simple in reaction condition, greatly shortens the synthesis time, and is suitable for large-scale industrialization.

Description

A kind of sodium-ion battery positive pole FePO 4/ Graphene composite material and preparation method thereof
Technical field
The present invention relates to a kind of sodium-ion battery material, particularly a kind of sodium-ion battery positive pole FePO 4/ Graphene composite material and preparation method thereof.
Background technology
In recent years, because environmental problem is day by day serious, energy crisis, the exploitation of new forms of energy and energy storage technology develop into the mankind jointly faced by problem.Lithium ion battery, because of the performance of its excellence, has been widely used in portable digital product.Future, lithium ion battery because of the long life, advantages such as high-energy-density and be subject to the attention of energy storage field worker.But lithium ion battery applications is also faced with some challenges in energy storage field.Secondly first, on the earth, lithium source reserves are limited, and the price of lithium metal can rise gradually along with lithium ion battery large-scale application, develop desirable electrode material and improve its performance further and seem particularly important.
Be in the sodium of same main group with lithium, have similar chemical property to lithium.Sodium-ion battery and lithium ion battery have similar principle, and importantly sodium reserves are on earth far above lithium.After the technical bottleneck breakthrough of sodium-ion battery, more wide application prospect must be shown.At present, many research work about sodium ion positive electrode are reported, in succession as Na xcoO 2, Na 0.44mnO 2, Na 0.6mnO 2, NaCrO 2, Na xvO 2, Na 3v 2(PO 4) 3, Na 3v 2(PO 4) 2f 3, Na 3v 2o 2(PO 4) 2f, Na 2fePO 4f, NaFeF 3deng, but the performance of these positive electrodes still can not meet the requirement of the industrial applications of sodium-ion battery.Developing desirable electrode material is the industrialized key of sodium-ion battery.
Iron-based positive electrode NaFePO 4as sodium-ion battery positive material, existing relevant report.In charge and discharge process, the reversible deintercalation of Na+, that in fact corresponding is NaFePO 4with FePO 4two-phase transforms mutually.In theory, FePO 4also can as sodium-ion battery positive material.FePO 4as electrode material, there is many advantages.First, iron trivalent iron compound is enriched as raw material sources, and cost is low, easily obtains; Secondly, FePO 4chemical synthesis process simple, environmental friendliness and do not need inert gas shielding; Finally, FePO 4there is the theoretical specific capacity up to 178 mAh/g.But, FePO 4and LiFePO 4the same, the shortcoming such as also there is electron conduction difference and ionic diffusion coefficient is low, researcher has used a lot of method to improve FePO 4the electron conduction of material and ionic diffusion coefficient, such as nanometer, load MCNT, metal cation doping etc.But acquired effect is also unsatisfactory.
Within 2004, from graphite, successfully isolating Graphene (Graphene) first from Univ Manchester UK physicist An Deliehaimu (Andre Geim) and Constantine Nuo Woxiaoluofu (Konstantin Novoselov) and confirming that it can since individualism.Because of electron conduction and the two-dimensional structure of its excellence, be widely used in improving electrode material chemical property.But, at present all the concentrating on the Graphene of active material load after finishing of most report.Generally of this sort Measures compare is complicated, and modified graphene conductive performance can obviously decline.How to pass through a kind of simple synthetic method, by the load of nanometer Fe PO4 particle in-situ on Graphene, the FePO4/Graphene composite material synthesizing excellent performance is problem to be solved by this invention.
Summary of the invention
The performance that the present invention be directed to present positive electrode still can not meet the problem of the requirement on industrial application of sodium-ion battery, proposes a kind of sodium-ion battery positive pole FePO 4/ Graphene composite material and preparation method thereof, by the method for microemulsion, one-step synthesis FePO 4/ Graphene composite material.FePO 4nanometer spherical particle by the load of non-covalent strong uniform individual layer on graphite two sides.As sodium-ion battery positive material, because the similar sandwich structure that its uniqueness is, the existence of Graphene substantially increases electrical conductivity speed.In addition, FePO 4nanostructure also increases electrode material surface and amasss, and improves Na +ion reversible deintercalation speed.FePO 4/ Graphene composite material shows excellent chemical property as sodium-ion battery positive material.
Technical scheme of the present invention is: a kind of sodium-ion battery positive pole FePO 4/ Graphene composite material preparation side, specifically comprises the steps:
1) by Triton X-100, n-butanol, cyclohexane by volume 3:1:5 configure two parts of microemulsion systems, be labeled as A and B respectively;
2) configuration standard concentration is the Fe (NO of 0.1mol/l 3) 39H 2o and NH 4h 2pO 4;
3) in A, 100mg Graphene is added, ultrasonic disperse 30min, then respectively to the Fe (NO adding 50ml, 0.1mol/l in A and B 3) 39H 2o and NH 4h 2pO 4;
4) with after magnetic stirring apparatus stirs, A and B is transferred in reactor, add ammoniacal liquor and liquid pH value is adjusted to 2.6, maintain 45 DEG C, 450r/min reacts 3h, ageing 3h, by the mixed liquor centrifugation obtained, centrifugal product acetone/ethanol by volume 1/1 solution be made into cleans three times;
5) the centrifugal product obtained dry 12h in 120 DEG C, then under nitrogen atmosphere, 460 DEG C of heat treatment 3h, obtain sodium-ion battery positive material FePO 4/ Graphene composite material.
Beneficial effect of the present invention is: sodium-ion battery positive pole FePO of the present invention 4/ Graphene composite material and preparation method thereof, is mainly applied to the synthetic method of microemulsion in the preparation of electrode material and goes.From report before different with load electrode active material on modified Graphene, this preparation method can combination directly by non-covalent bond in reaction system, and make the surface of the direct load Graphene of active material, synthesis technique is simple.In addition, prepare the synthetic method of the microemulsion that active material adopts unlike, the present invention with the hydrothermal synthesis method that someone reports before, because reaction condition is simple, greatly shortens the time required for synthesis, be applicable to extensive industrialization.The most important thing is the FePO be synthesized 4/ Graphene composite material, as sodium-ion battery positive material, shows excellent chemical property.
Accompanying drawing explanation
Fig. 1 is the SEM figure of Graphene;
Fig. 2 is FePO of the present invention 4the SEM figure of/Graphene composite material;
Fig. 3 is FePO of the present invention 4the Raman spectrogram of/Graphene and Graphene;
Fig. 4 is FePO of the present invention 4/ Graphene and FePO 4as the specific discharge capacity figure under 0.1C of sodium-ion battery positive material;
Fig. 5 is FePO under different multiplying condition of the present invention 4/ Graphene and FePO 4specific discharge capacity figure.
Embodiment
Sodium-ion battery positive material FePO 4the preparation method of/Graphene composite material:
(1) by hummers method synthesizing graphite alkene.Using flaky graphite as raw material.Take 0.5g crystalline flake graphite, 0.2g sodium nitrate, the 20ml concentrated sulfuric acid, mixes in ice-water bath.Add 6g potassium permanganate slowly again.Maintain the temperature at about 0 DEG C, stir 10mins.Then rapid temperature increases causes 35 DEG C of reaction 1h, adds 60ML deionized water.Then be warmed up to 95 DEG C add 80ml deionized water continue reaction.Then the hydrogen peroxide 8ML of volume fraction 30% is added.After reaction 1h, solution is in golden yellow.Add a certain amount of hydrazine hydrate as reducing agent, react one hour.Then high speed centrifugation, washing, until pH > 6, obtains redox graphene aqueous solution.Then 60 DEG C of oven dry.This is existing graphene preparation method, as shown in Figure 1 the SEM figure of Graphene.
(2) 3:1:5(Triton X-100 by volume: n-butanol: cyclohexane) configure two parts of microemulsion systems, be labeled as A and B respectively.Configuration standard concentration is the Fe (NO of 0.1mol/l 3) 39H 2o and NH 4h 2pO 4.100mg Graphene is added, ultrasonic disperse 30min, then respectively to the Fe (NO adding 50m, l0.1mol/l in A and B in A 3) 39H 2o and NH 4h 2pO 4.Power blender stirs.Again A and B is transferred in reactor, add ammoniacal liquor and liquid pH value is adjusted to 2.6, maintain 45 DEG C, 450r/min reacts 3h.Ageing 3h, the solution centrifugal obtained is separated, and the desired product acetone/ethanol obtained by volume 1/1 solution be made into cleans three times.Again the centrifugal product obtained dry 12h in 120 DEG C, then exist, under blanket of nitrogen, 460 DEG C of heat treatment 3h.A kind of sodium-ion battery positive material FePO 4/ Graphene composite material just obtains.FePO of the present invention as shown in Figure 2 4the SEM figure of/Graphene composite material.
At preparation FePO 4in/Graphene composite material.Because " Water-In-Oil " system of this uniqueness of microemulsion, is conducive to making Graphene well disperse.The ferric nitrate added and Graphene are dispersed in microemulsion system, then add NH 4h 2pO 4after, on the surface of Graphene, ferric phosphate can original position nucleating growth.Thisly make FePO by non-covalent bond 4the evengranular load of nanometer spherical, on Graphene surface, defines FePO 4/ Graphene composite material.Fig. 3 is FePO of the present invention 4the Raman spectrogram of/Graphene and Graphene, as can be seen from the figure, FePO 4/ Graphene composite material and Graphene are at 1353.1cm -1with 1590.5 cm -1demonstrate obvious absworption peak, this correspondence be Graphene D band and G be with, result shows that the synthetic method that the present invention uses can ensure that Graphene structure in course of reaction can not change.
Electrode preparation and test: the material of synthesis and conductive agent (graphite (upper marine products, AR): carbon black (upper marine products, AR)=4:6) in mass ratio for 62:30 is mixed to join in ball grinder, planetary ball mill is dry grinded two hours, then use alcohol as dispersant wet-milling two hours, the active material obtained is dry in thermostatic drying chamber.Take 15mg active material and PTFE(Japan produces, LITHIUM BATTERY) (mass ratio 92:8) be mixed into slurries, and be coated in and be welded with on 2016 type button cell anode covers of stainless (steel) wire.Compacting is placed in vacuum drying chamber, dries 12h under 100 ° of C conditions.
Then Ar is being filled 2in glove box, be negative pole with metal Na (upper marine products, CP) sheet, electrolyte is the NaClO of 1mol/L 4(upper marine products, AR) (being dissolved in the EC(Tianjin product that volume ratio is 1:1, AR) upper marine products of/DMC(, AR) in), be barrier film with glass felt fiber (Fujian dragon's fountain produces, LITHIUM BATTERY), be assembled into 2016 type button cells.Carry out constant current charge-discharge test with Land battery test system (China, Wuhan), probe temperature controls at constant temperature 25 ° of C, and test voltage is between 1.5V ~ 4.2V.Under 0.1C condition, circulate 70 times, still can keep 151.5mAh/g specific discharge capacity.Under 1C condition, FePO 4/ Graphene composite material still can keep 105.3mAh/g.FePO as shown in Figure 4 4/ Graphene and FePO 4as the specific discharge capacity figure under 0.1C of sodium-ion battery positive material, FePO under different multiplying condition as shown in Figure 5 again 4/ Graphene and FePO 4specific discharge capacity figure, result shows, by microemulsion method synthesis FePO4/Graphene positive electrode, shows excellent cycle performance, volumetric properties and high rate performance.

Claims (1)

1. a sodium-ion battery positive pole FePO 4/ Graphene composite material preparation side, is characterized in that, specifically comprise the steps:
1) by Triton X-100, n-butanol, cyclohexane by volume 3:1:5 configure two parts of microemulsion systems, be labeled as A and B respectively;
2) configuration standard concentration is the Fe (NO of 0.1mol/l 3) 39H 2the NH of O and 0.1mol/l 4h 2pO 4;
3) in A, 100mg Graphene is added, ultrasonic disperse 30min, then respectively to the Fe (NO adding 50ml, 0.1mol/l in A and B 3) 39H 2o and NH 4h 2pO 4;
4) after stirring on magnetic stirring apparatus, A and B is transferred in reactor, add ammoniacal liquor and liquid pH value is adjusted to 2.6, maintain 45 ° of C, 450r/min reacts 3h, ageing 3h, the solution centrifugal obtained is separated, and centrifugal product acetone/ethanol by volume 1/1 solution be made into cleans three times;
5) the centrifugal product obtained dry 12h in 120 DEG C, then under nitrogen atmosphere, 460 DEG C of heat treatment 3h, obtain sodium-ion battery positive material FePO 4/ Graphene composite material.
CN201510160213.5A 2015-04-07 2015-04-07 Preparation method of sodium ion battery anode FePO4/Graphene composite Pending CN104868118A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105514431A (en) * 2016-01-07 2016-04-20 山东省科学院能源研究所 Spherical graphene/FePO4 composite and preparing method thereof
CN105938904A (en) * 2016-05-31 2016-09-14 中南大学 Composite positive electrode material for sodium-ion battery and preparation method of composite positive electrode material
CN106099104A (en) * 2016-08-26 2016-11-09 常开军 A kind of for secondary cell manufacture without lithium anode material and manufacture method thereof
CN108878822A (en) * 2018-06-22 2018-11-23 宜春学院 Coat the preparation method of nano ferric phosphate composite material
CN109336227A (en) * 2018-09-03 2019-02-15 同济大学 Unformed phosphoric acid iron electrode material of graphene coated and preparation method thereof
CN114335693A (en) * 2021-12-28 2022-04-12 盐城工学院 High-safety iron-based phosphate sodium ion full cell and preparation method thereof

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105514431A (en) * 2016-01-07 2016-04-20 山东省科学院能源研究所 Spherical graphene/FePO4 composite and preparing method thereof
CN105514431B (en) * 2016-01-07 2018-06-22 山东省科学院能源研究所 A kind of spherical graphite alkene/FePO4Composite material and preparation method thereof
CN105938904A (en) * 2016-05-31 2016-09-14 中南大学 Composite positive electrode material for sodium-ion battery and preparation method of composite positive electrode material
CN105938904B (en) * 2016-05-31 2018-09-18 中南大学 A kind of sodium-ion battery composite positive pole and preparation method thereof
CN106099104A (en) * 2016-08-26 2016-11-09 常开军 A kind of for secondary cell manufacture without lithium anode material and manufacture method thereof
CN106099104B (en) * 2016-08-26 2019-07-26 常开军 It is a kind of for secondary cell manufacture without lithium anode material and its manufacturing method
CN108878822A (en) * 2018-06-22 2018-11-23 宜春学院 Coat the preparation method of nano ferric phosphate composite material
CN108878822B (en) * 2018-06-22 2021-04-09 宜春学院 Preparation method of coated nano iron phosphate composite material
CN109336227A (en) * 2018-09-03 2019-02-15 同济大学 Unformed phosphoric acid iron electrode material of graphene coated and preparation method thereof
CN114335693A (en) * 2021-12-28 2022-04-12 盐城工学院 High-safety iron-based phosphate sodium ion full cell and preparation method thereof
CN114335693B (en) * 2021-12-28 2023-09-12 盐城工学院 High-safety iron-based phosphate sodium ion full battery and preparation method thereof

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Application publication date: 20150826