CN1817800A - Synthesis of series nanometer lithium and manganese oxide for lithium ion battery - Google Patents

Synthesis of series nanometer lithium and manganese oxide for lithium ion battery Download PDF

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CN1817800A
CN1817800A CNA200610038148XA CN200610038148A CN1817800A CN 1817800 A CN1817800 A CN 1817800A CN A200610038148X A CNA200610038148X A CN A200610038148XA CN 200610038148 A CN200610038148 A CN 200610038148A CN 1817800 A CN1817800 A CN 1817800A
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lithium
manganese oxide
oxide
distilled water
thermal reaction
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CN100371256C (en
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张卫新
杨则恒
王强
刘怡
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Hefei University of Technology
Hefei Polytechnic University
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    • 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

Synthesis of series nanometer lithium manganese oxide for lithium ion battery is carried out by taking mangano-manganic oxide or basic manganese oxide as precursor, hydrothermal reacting with excessive lithium hydrate in water or alcohol solution of autoclave, inserting lithium ion into lattice of manganese oxide, separating, washing and drying to obtain final product. It is simple and safe, has lower energy consumption, uniform granularity, better electrical performance and no environmental pollution.

Description

A kind of synthetic method of series nanometer lithium and manganese oxide for lithium ion battery
One, technical field
The present invention relates to a kind of preparation method of chemical power source positive electrode material, particularly a kind of preparation method of anode material for lithium-ion batteries exactly is a kind of synthetic method of series nanometer lithium and manganese oxide for lithium ion battery.
Two, background technology
Along with the fast development of electronic industry, require power supply to develop along the direction of miniaturization, high-energy-density and high power density.From nineteen ninety Japan Sony work out lithium ion battery for the first time since, this novel store battery has satisfied this requirement to a large extent.Lithium ion battery has been widely used among the electrical equipment of miniaturizations such as mobile phone, notebook computer now, and uses also first meeting achievement in electriclocomotive.
At present, the positive electrode material of lithium ion battery mainly is LiCoO 2(cobalt acid lithium), but because LiCoO 2Cost an arm and a leg, pollute greatly, the researchist is seeking hardy can substitute LiCoO 2Positive electrode material.Specific storage is big because lithium manganese oxide has, low price and the little advantage of pollution, people is looked it do the most attractive a kind of positive electrode material.Now, the method for preparing lithium manganese oxide mainly is solid reaction process, sol-gel method, coprecipitation method.Yet, these methods need powder to calcine under comparatively high temps inevitably, resulting solid product shows great ununiformity on structure, composition and size-grade distribution, and the whether even chemical property that influences electrode materials to a large extent of these factors.
The lithium manganese oxide of nanostructure has unique microtexture, has superior embedding lithium characteristic when making it as electrode, concrete shows: the insert depth of lithium ion is little, process short, has than bigger serface, helps bigger electric current it is discharged and recharged; And it has bigger embedding lithium locus, helps increasing the capacity of its embedding lithium.
U.S.'s " inorganic chemistry communication " (Inorganic Chemistry Communications) is (2004 recently, the 7th volume, the 308-310 page or leaf) reported potassium permanganate and hexadecyl trimethyl ammonium bromide (CTAB) mixing, be prepared into purple gel, be prepared into intermediate product through processes such as ageings, relief itself and lithium hydroxide solution adopt hydrothermal method to synthesize the lithium manganese oxide of spinel structure under 70 ℃-190 ℃ condition.But the intermediate steps of this method is various, and is difficult to extend to the serial lithium manganese oxide of preparation.
Three, summary of the invention
The present invention aims to provide lithium manganese oxide that a kind of new hydrothermal synthesis method prepares nanoscale to solve the even particle size distribution problem, provides a kind of chemical property good positive level material for lithium ion battery simultaneously.
So-called serial lithium manganese oxide is meant that chemical formula is LiMnO 2, LiMn 2O 4And Li 2MnO 3Three kinds of lithium manganese compounds.
The synthetic method of series lithium manganese oxide is with trimanganese tetroxide (Mn 3O 4) or alkali formula manganese oxide (γ-MnOOH) in autoclave, carry out hydro-thermal reaction for precursor in water or in the aqueous ethanolic solution (calling ethanolic soln in the following text) with excessive lithium hydroxide (LiOH), among the lattice that makes lithium ion embedding Mn oxide under certain temperature, the pressure, reaction finishes after separation, washing and drying obtain serial lithium manganese oxide.
Precursor Mn 3O 4And γ-MnOOH is all with potassium permanganate (KMnO 4) be raw material, in Different concentrations of alcohol solution, in autoclave pressure, carry out hydro-thermal reaction and through separate, the dry and nano level precursor that obtains.
Preparation Mn 3O 4The time dehydrated alcohol volume parts 〉=70%, 100～200 ℃ of temperature of reaction, pressure 1.0～2.0MPa, 12～24 hours time, Mn 3O 4Particle diameter 30～100nm.
The volume parts of dehydrated alcohol is 0.5～10% during preparation γ-MnOOH, when the preparation nano wire, and 90～99 ℃ of temperature of reaction, pressure 0.1～1.0MPa, 12～18 hours time, γ-MnOOH nanowire diameter 10～50nm; When the preparation nanometer rod, 100～120 ℃ of temperature of reaction, pressure 0.1～1.0MPa, 15～24 hours time, γ-MnOOH nanometer rod diameter 30～150nm.
Comprise hydro-thermal reaction and separation, washing and the drying of precursor with precursor synthesizing series lithium manganese oxide with excessive LiOH.
Synthetic LiMnO 2The time, nano level γ-MnOOH and excessive LiOH carry out hydro-thermal reaction in ethanolic soln, 120～170 ℃ of temperature, pressure 0.5～1.5MPa, 5～7 days time, the volume ratio of dehydrated alcohol and distilled water is: 1: 1.5～4, and the amount of distilled water makes the concentration of LiOH be not less than 4mol/L.When γ-MnOOH is nano bar-shape, LiMnO 2Also be nano bar-shape, diameter 150～250nm; When γ-MnOOH is the nanometer wire, LiMnO 2Nanoparticle in the form of sheets, diameter 10～50nm.
Synthetic LiMn 2O 4The time, nanometer Mn 3O 4In distilled water, carry out hydro-thermal reaction with excessive LiOH, 150～180 ℃ of temperature, pressure 1.2～1.6MPa, 5～7 days time, the amount of distilled water makes the concentration of LiOH be not less than 4mol/L.LiMn 2O 4Be nanoparticle, median size 20～100nm.
Synthetic Li 2MnO 3The time, can use nanometer γ-MnOOH or Mn 3O 4Respectively with excessive LiOH in distilled water in Potassium Persulphate (K 2S 2O 8) carry out hydro-thermal reaction under the existence condition, the temperature of control, pressure and time are identical, are respectively 120～170 ℃, 0.25～1.0MPa, 2～7 days.γ-MnOOH or Mn 3O 4With K 2S 2O 8Mol ratio be: 1: 20～30, the amount of distilled water makes the concentration of LiOH be not less than 4mol/L.When using Mn 3O 4The time, Li 2MnO 3Be nanoparticle, median size 30～100nm.When using γ-MnOOH, Li 2MnO 3Or being nano bar-shape or flake nano particle, mean diameter is respectively 150～250nm, 20～100nm.Li 2MnO 3Nanometer rod length is 1～10 μ m.
The synthetic method of serial nano lithium manganese oxide provided by the invention is simple, red-tape operati is convenient, and next step just can synthesize the LiMnO of nanoscale at the reaction conditions of gentleness 2, LiMn 2O 4And Li 2MnO 3, use the precursor of different-shape can prepare the oxide compound of the same race of different-shape, there is not follow-up high-temperature calcination process, compared with prior art, energy consumption is low, safety, environmental protection.Granularity Distribution is even, and electric property is good.
With LiMn 2O 4Nanoparticle and acetylene black, polyvinylidene difluoride (PVDF) (PVDF) evenly are coated on the aluminium foil with 88: 8: 4 (mass ratio) thorough mixing of proportioning furnishing pasty state, make positive plate after oven dry, the compacting.With the metal lithium sheet is negative plate, and Cellgard2002 type polypropylene screen is made barrier film, 1mol/L LiPF 6Solution (NSC 11801+methylcarbonate (volume ratio=1: 1)) is electrolytic solution, is assembled into Experimental cell in the argon gas glove box.Under 25 ℃, respectively this electrode is carried out the constant current charge-discharge experiment then.
Show by the constant current charge-discharge experimental result: made electrode materials LiMn 2O 4The initial charge capacity is 160mAhg -1, loading capacity is 146mAhg first -1
Four, description of drawings
Fig. 1 is LiMnO 2XRD figure:
Fig. 2 is for being that precursor prepares LiMnO with γ-MnOOH nanometer rod 2The TEM figure of nanometer rod:
Fig. 3 is for being that precursor prepares LiMnO with γ-MnOOH nano wire 2The TEM figure of nanoparticle:
Fig. 4 is LiMn 2O 4XRD figure:
Fig. 5 is with Mn 3O 4Nanoparticle is that precursor prepares LiMn 2O 4The TEM figure of nanoparticle:
Fig. 6 is Li 2MnO 3XRD figure:
Fig. 7 is for being that precursor prepares Li with γ-MnOOH nanometer rod 2MnO 3The TEM figure of nanometer rod:
Fig. 8 is for being that precursor prepares Li with γ-MnOOH nano wire 2MnO 3The TEM figure of nanoparticle:
Fig. 9 is with Mn 3O 4Nanoparticle is that precursor prepares Li 2MnO 3The TEM figure of nanoparticle:
Figure 10 is the XRD figure of γ-MnOOH:
Figure 11 is the TEM figure of γ-MnOOH nano wire:
Five, embodiment
Embodiment 1:LiMnO 2The preparation of nanometer rod or nanoparticle
With 0.100g γ-MnOOH nanometer rod (or nano wire), 5.035g LiOHH 2O, 10ml distilled water and 20ml dehydrated alcohol be reaction 5 days under 120 ℃, the condition of 1.0-1.5Mpa in the 50ml reactor.After reaction finishes, take out product, with the distilled water rinsing repeatedly to the pH value of upper strata clear liquid near 7.The black precipitate that obtains in vacuum drying oven with 60 ℃ of oven dry.The outward appearance of product is the powder of black.
The XRD figure of product (Fig. 1) analytical results shows that product is the LiMnO of rhombic system 2Powder.The pattern that the TEM figure result of product shows product is divided into two kinds because of the pattern difference of precursor.Precursor is γ-MnOOH nanometer rod, and obtaining product is nanometer rod (Fig. 2), and between 150nm-250nm, length is between 1～5 μ m greatly for diameter.Precursor is γ-MnOOH nano wire, and then product is flake nano particle (Fig. 3), and diameter is approximately 10～50nm.
Embodiment 2:LiMn 20 4The preparation of nanoparticle
With 0.4g Mn 3O 4Nanoparticle, 33.568g LiOHH 2O, 200ml distilled water mix in the magnetic agitation reactor, under the condition of 160～170 ℃ of temperature, pressure 1.3～1.5MPa, react 7 days with the stirring velocity of 150～250r/min.After reaction finishes, take out product, with the distilled water wash sample repeatedly to upper strata clear liquid pH value near 7, the black precipitate that obtains is dried under 60 ℃ condition.The outward appearance of product is the powder of black.
Through XRD (Fig. 4) analysis revealed: product is the LiMn of isometric system 2O 4Powder.TEM photo (Fig. 5) shows: the pattern of product is a nanoparticle, and its diameter is approximately 20nm-100nm.
Embodiment 3:Li 2MnO 3The preparation of nanometer rod or nanoparticle
With 0.100g precursor γ-MnOOH nanometer rod (or nano wire) or 0.1gMn 3O 4Nanoparticle respectively with 6.758gK 2S 2O 8, 5.035g LiOHH 2Put into the 50ml reactor after O and 30ml distilled water mix under 150 ℃, the condition of 0.25-1.0MPa, reacted 2 days.After reaction finishes, take out product, with the distilled water wash sample repeatedly to the pH value of upper strata clear liquid near 7, the black precipitate that obtains is dried under 60 ℃ condition.The outward appearance of product is the powder of black.
Through XRD (Fig. 6) analysis revealed: product is monoclinic Li 2MnO 3Powder.The pattern of TEM photo demonstration product is divided into two kinds because of the pattern difference of precursor.If precursor is γ-MnOOH nanometer rod, product is nanometer rod (Fig. 7), and between 150nm-250nm, length is between 1～10 μ m greatly for its diameter.If precursor is γ-MnOOH nano wire, then product is flake nano particle (Fig. 8), and diameter is approximately between the 20nm-100nm.If precursor is Mn 3O 4Nanoparticle, then product is flake nano particle (Fig. 9), diameter is approximately between the 30nm-100nm.
Embodiment 4: the preparation of γ-MnOOH nano wire
With 4g KMnO 4Put into the mixing solutions that contains 4ml dehydrated alcohol and 400ml distilled water, under 95 ℃-99 ℃, the condition of 0.1-0.5MPa, reaction 18h.After reaction finishes, take out product, with the distilled water wash sample repeatedly, the brown that obtains is deposited in the vacuum drying oven with 60 ℃ of oven dry.The outward appearance of product is the powder of brown.Through XRD (Figure 10) analysis revealed: product is monoclinic γ-MnOOH powder.TEM photo (Figure 11) shows that the pattern of product is a nano wire, and diameter is greatly between 15-20nm.
Embodiment 5: the preparation of γ-MnOOH nanometer rod
After 4g potassium permanganate, 400mL distilled water, 4mL dehydrated alcohol mixed, reaction was 24 hours under 150 ℃, 0.5-1.0Mpa.Then take out product, use distilled water wash 3-5 time earlier, use absolute ethanol washing again 1 time.70 ℃ of following vacuum-dryings 4 hours, promptly obtain pale brown toner end.
Through X-ray powder diffraction (XRD) and transmission electron microscope (TEM) analysis revealed products therefrom is monoclinic γ-MnOOH nanometer rod, and diameter is between 30-150nm, and length is at several microns to tens microns.
Embodiment 6:Mn 3O 4The preparation of nanoparticle
After 4g potassium permanganate, 20mL distilled water, 400mL dehydrated alcohol mixed, reaction was 24 hours under 150 ℃, 1.0-2.0Mpa.Then take out product, use distilled water wash 3-5 time earlier, use absolute ethanol washing again 1 time.70 ℃ of following vacuum-dryings 4 hours, promptly obtain khaki Mn 3O 4Nanoparticle.
Through X-ray powder diffraction (XRD) and transmission electron microscope (TEM) analysis revealed products therefrom is the Mn of tetragonal system 3O 4, size of particles is more even, and median size is about 20～100nm.

Claims (4)

1, a kind of lithium manganese oxide LiMnO 2Synthetic method, comprise hydro-thermal reaction and separation, washing and drying, it is characterized in that: described hydro-thermal reaction is that nanometer alkali formula manganese oxide and excessive hydrogen Lithium Oxide 98min react in ethanolic soln, 120～170 ℃ of temperature of reaction, pressure 0.5～1.5MPa, 5～7 days time, the volume ratio of distilled water and dehydrated alcohol is 1: 1.5～4, and the amount of distilled water makes the concentration of lithium hydroxide be not less than 4mol/L.
2, a kind of lithium manganese composite oxide LiMn 2O 4Synthetic method, comprise hydro-thermal reaction and separation, washing and drying, it is characterized in that: described hydro-thermal reaction is that nano manganic manganous oxide and excessive hydrogen Lithium Oxide 98min react in distilled water, 150～180 ℃ of temperature of reaction, pressure 1.2～1.6MPa, 5～7 days time, the amount of distilled water makes the concentration of lithium hydroxide be not less than 4mol/L.
3, a kind of lithium manganese oxide Li 2MnO 3Synthetic method, comprise hydro-thermal reaction and separation, washing and drying, it is characterized in that: described hydro-thermal reaction is that nanometer alkali formula manganese oxide or nano manganic manganous oxide react under the Potassium Persulphate existence condition in distilled water with the excessive hydrogen Lithium Oxide 98min respectively, 120～170 ℃ of temperature of reaction, pressure 0.25～1.0MPa, 2～7 days time, the mol ratio of alkali formula manganese oxide or trimanganese tetroxide and Potassium Persulphate is 1: 20～30, and the amount of distilled water makes the concentration of lithium hydroxide be not less than 4mol/L.
4, by the preparation method of a kind of alkali formula manganese oxide nano wire in claim 1 and the 3 described nanometer alkali formula manganese oxide, the hydro-thermal reaction and separation and the drying that comprise potassium permanganate, it is characterized in that: potassium permanganate reacted 12～18 hours under 90～99 ℃ of temperature, pressure 0.1～1.0MPa condition in ethanolic soln, and the volume parts of dehydrated alcohol is 0.5～10%.
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TWI489683B (en) * 2010-03-31 2015-06-21 Namics Corp Lithium ion secondary battery
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CN102800855A (en) * 2012-08-15 2012-11-28 北京师范大学 Preparation method of lithium ion battery positive electrode material layered LiMnO2
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US11522182B2 (en) 2017-09-26 2022-12-06 Lg Energy Solution, Ltd. Method for producing lithium manganese oxide-based cathode active material
EP3666733A4 (en) * 2017-09-26 2020-12-02 LG Chem, Ltd. Method for producing lithium manganese oxide-based positive electrode active material
CN109616632A (en) * 2018-11-29 2019-04-12 深圳清华大学研究院 Manganese based solid solution material and preparation method thereof, positive electrode and battery
CN110767898A (en) * 2019-09-30 2020-02-07 合肥国轩高科动力能源有限公司 Manganese-based nanowire bundle and preparation method and application thereof
CN110767898B (en) * 2019-09-30 2022-06-07 合肥国轩高科动力能源有限公司 Manganese-based nanowire bundle and preparation method and application thereof
CN112919546B (en) * 2019-12-06 2022-03-18 南京理工大学 Positive electrode material of monoclinic/tetragonal spinel heterostructure and preparation method thereof
CN112919546A (en) * 2019-12-06 2021-06-08 南京理工大学 Positive electrode material of monoclinic/tetragonal spinel heterostructure and preparation method thereof
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