CN104993101B - Orthosilicate nanofiber anode active material of lithium ion battery and preparation method thereof - Google Patents

Orthosilicate nanofiber anode active material of lithium ion battery and preparation method thereof Download PDF

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CN104993101B
CN104993101B CN201510255755.0A CN201510255755A CN104993101B CN 104993101 B CN104993101 B CN 104993101B CN 201510255755 A CN201510255755 A CN 201510255755A CN 104993101 B CN104993101 B CN 104993101B
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orthosilicate
lithium ion
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anode active
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李东林
雍红团华
樊小勇
苟蕾
张巍
谢荣
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Changan University
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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
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    • H01M4/02—Electrodes composed of, or comprising, active material
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    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • H01M10/052—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
    • H01M4/48—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
    • 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
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    • 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
    • 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
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    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract

The present invention relates to lithium ion battery preparation field, a kind of orthosilicate nanofiber anode active material of lithium ion battery and preparation method thereof is disclosed.The positive electrode active materials are orthosilicate Li2MSiO4The orthosilicate carbon Li of nanocrystal and amorphous carbon composition2MSiO4/ C composite nano fiber anode active material of lithium ion battery, wherein M Fe, Mn, Co or Ni；Preparation method are as follows: weigh carbon raw material first and be dissolved in liquid solvent, form the first solution；Silicon raw material, lithium salts and M salt are successively weighed again to be separately dissolved in the liquid solvent, form the second solution；Then, the first solution is added in the second solution, constant temperature stirs evenly, form third solution, then by third solution evaporation at constant temperature at gel, finally to gel be heat-treated to get.

Description

Orthosilicate nanofiber anode active material of lithium ion battery and preparation method thereof
Technical field
The present invention relates to lithium ion battery preparation field, in particular to a kind of orthosilicate nanofiber lithium ion battery is just Pole active material and preparation method thereof, the positive electrode active materials are used to prepare lithium ion cell positive.
Background technique
Lithium ion battery is widely used in various portable due to the advantages that its voltage is high, capacity is high and has extended cycle life In formula electronic product, and it is expected to the main power source as electric car, is the secondary electricity for generally believing most development potentiality Pond.Positive electrode had not only been used as electrode material to participate in electrochemical reaction, but also was lithium ion source, decide the work electricity of lithium ion battery The performances such as pressure, working time and stability.Therefore, the key that obtain high performance lithium ion secondary battery be obtain it is high performance Positive electrode.
Silicon (Si) one of highest element of content on earth, and it is all harmless to environment and the mankind, thus in many poly- yin Silicate has special researching value in ionic material.In silicate systems, all oxonium ions all with Si4+It constitutes and stablizes Covalent type (Si04)4-Polyanion group, therefore the oxygen in lattice is not easy to lose, this makes the material have safety well Property, it is expected to become cheap anode material for lithium-ion batteries.
Summary of the invention
Aiming at the problems existing in the prior art, the object of the present invention is to provide a kind of simple Li2MSiO4(M=Fe, Mn, Co, Ni) and the compound orthosilicate nanofiber anode active material of lithium ion battery and preparation method thereof of amorphous carbon.
In order to achieve the above object, the technical proposal of the invention is realized in this way.
(1) a kind of orthosilicate nanofiber anode active material of lithium ion battery, which is characterized in that its silicic acid that is positive Salt Li2MSiO4The orthosilicate carbon Li of nanocrystal and amorphous carbon composition2MSiO4/ C composite nano fiber lithium ion cell positive Active material, wherein M Fe, Mn, Co or Ni.
(2) above-mentioned orthosilicate nanofiber anode active material of lithium ion battery, which is characterized in that including following original Expect component: carbon raw material, silicon raw material, lithium salts and M salt, M Fe, Mn, Co or Ni.
The carbon raw material is polyethylene oxide-polypropylene oxide-polyethylene oxide block copolymer, and silicon raw material is positive silicic acid Ethyl ester, methyl orthosilicate or sodium metasilicate；Lithium salts is lithium nitrate, lithium carbonate or lithium acetate；M salt is nitrate, carbonate or acetic acid Salt, M Fe, Mn, Co or Ni.
Wherein, carbon raw material is both the carbon raw material of nanofiber pattern forming agent and the composite material.
(3) preparation method of above-mentioned orthosilicate nanofiber anode active material of lithium ion battery, which is characterized in that Include the following steps
Step 1 weighs carbon raw material (or nanofiber forming agent) and is dissolved in liquid solvent, forms the first solution；Again according to Secondary silicon raw material, lithium salts and the M salt of weighing separately is dissolved in the liquid solvent, forms the second solution；Then, the second solution is added the One solution, constant temperature stir evenly, and form third solution, then by third solution evaporation at constant temperature at gel；
Step 2 is heat-treated gel, obtains orthosilicate nanofiber anode active material of lithium ion battery.
Preferably, the carbon raw material is polyethylene oxide-polypropylene oxide-polyethylene oxide block copolymer；Further Preferably, the carbon raw material is Pluronic P123(EO20PO70EO20) or F127(EO106PO70EO106))。
Preferably, the silicon raw material is ethyl orthosilicate, methyl orthosilicate or sodium metasilicate.Silicon raw material can also be organic with other Silicon and inorganic silicon, and go synthesis to obtain the intermediate of silicon source class by other methods.
Preferably, the lithium salts is lithium nitrate, lithium carbonate or lithium acetate.Lithium salts be also possible to other inorganic salts, organic salt, The inorganic lithium salt that metal alkoxide and other methods synthesize.
Preferably, the M salt is nitrate, carbonate or acetate, M Fe, Mn, Co or Ni.M salt may be to include The salt containing M element that inorganic salts, organic salt, metal alkoxide, organic compound and the other methods of M element obtain.
Preferably, the liquid solvent is water, ethyl alcohol, ethylene glycol or ethylene glycol ethyl ether.Liquid solvent may be solvable Solve other organic solvents or inorganic solvent of M salt.
Preferably, the evaporation at constant temperature temperature is from room temperature within the scope of 80 DEG C；It is further preferred that the constant temperature stirring Temperature is from room temperature within the scope of 60 DEG C.
The preferably described heat treatment is heat-treated 6-20 hours for 600-800 DEG C of nitrogen atmosphere stove calcining.Inorganic raw material transformation For Li2MSiO4Nanoparticle is changed into amorphous carbon after organic polymer carbonization, Li is collectively formed2MSiO4/ C composite Nano is fine Dimension.
Orthosilicate nanofiber anode active material of lithium ion battery of the invention has formula Li2MSiO4Nanocrystal With the Li of amorphous carbon composition2MSiO4/ C nano fibrous composite is of virtually one-dimensional nano structure, " Nanowire therein Dimension " refers to the one-dimensional nano structure of various Chineses, such as " nanofiber ", " nanobelt ", " nano wire " and " nanometer rods " All kinds of Chineses of equal one-dimensional nano structures.
The orthosilicate nanofiber anode active material of lithium ion battery prepared using the present invention, by itself and conductive agent It is mixed with binder according to conventional ratio, and appropriate Conventional solvents is added, be coated on aluminium foil after mixing evenly, can be used as lithium The electrode film of ion battery uses.
Compared with prior art, the present invention has the following advantages that and beneficial technical effect: (1) preparation method of the invention Middle raw material forms the uniformity of molecular level, the phase interaction in sol-gel process, between reactant easily in liquid solvent With the mixing for more easily reacing molecular level.In the evaporation whipping process of liquid solvent, can farthest carry out each ion it Between uniform mixing, easily form desired collosol substance.(2) when using block polymer surfactant P123For Nanowire When tieing up forming agent formation nanofibrous structures, simple process is easily operated, and synthesis temperature is low；Moreover, surfactant P123It can make Li is coated for carbon source2MSiO4Nano crystal material, P123Amorphous carbon is formed after heating carbonization, improves electric conductivity, Neng Gouhe At the orthosilicate nanofiber anode active material of lithium ion battery with good circulation performance.(3) it is prepared by the present invention just Silicate nano-fiber anode active material of lithium ion battery is received, and nanowire structure can be effectively improved the conduction speed of lithium ion Rate shortens the transmission range of lithium ion, and the permeability of electrolyte is improved by building nanofibrous structures.
Detailed description of the invention
The present invention is described in further details in the following with reference to the drawings and specific embodiments.
Fig. 1 is the x-ray diffraction pattern of orthosilicate nanofiber anode active material of lithium ion battery of the invention；
Fig. 2 is sweeping for the x-ray diffraction pattern of orthosilicate nanofiber anode active material of lithium ion battery of the invention Retouch Electronic Speculum (SEM) figure；
Fig. 3 is times of the x-ray diffraction pattern of orthosilicate nanofiber anode active material of lithium ion battery of the invention Rate cyclic curve figure.
Specific embodiment
The present invention is described in further details combined with specific embodiments below, but the present invention is not limited to these Examples.
Embodiment 1: preparation Li2FeSiO4The orthosilicate nanofiber lithium ion cell positive activity compound with amorphous carbon Material, specific steps:
Step 1 weighs 0.5g surfactant P123(EO20PO70EO20), it is dissolved in 15mL ethyl alcohol, forms the first solution； 2.088g ethyl orthosilicate, 0.02moL lithium nitrate and 0.01moL ferric nitrate are successively weighed again to be dissolved in 10mL ethyl alcohol, form the Two solution；The first solution is added in second solution, 40 DEG C of constant temperature water baths stir evenly, and form third solution, then by third solution 10mL gel is flashed in 40 DEG C of constant temperature water baths；
10mL colloidal sol is placed in 650 DEG C of calcining 7h of argon gas atmosphere stove, obtains Li by step 22FeSiO4It is compound with amorphous carbon Orthosilicate nanofiber anode active material of lithium ion battery.
Embodiment 2: preparation Li2CoSiO4The orthosilicate nanofiber lithium ion cell positive activity compound with amorphous carbon Material, specific steps:
Step 1 weighs 0.7 surfactant P123, it is dissolved in 15mL ethylene glycol, forms the first solution；It successively weighs again 2.088g methyl orthosilicate, 0.02moL lithium acetate and 0.01moL cobalt acetate are dissolved in 3mL ethylene glycol, form the second solution；By The first solution is added in two solution, and 50 DEG C of constant temperature water baths stir evenly, and forms third solution, then by third solution in 50 DEG C of water-bath perseverances Temperature flashes to 10mL gel；
10mL colloidal sol is placed in 800 DEG C of calcining 6h of nitrogen atmosphere stove, it is compound with amorphous carbon to obtain Li2CoSiO4 by step 2 Orthosilicate nanofiber anode active material of lithium ion battery.
Embodiment 3: preparation Li2MnSiO4The orthosilicate nanofiber lithium ion cell positive activity compound with amorphous carbon Material, specific steps:
Step 1 weighs 0.5 surfactant P123, it is dissolved in 15mL ethylene glycol ethyl ether, forms the first solution；Again successively It weighs 2.088g sodium metasilicate, 0.02moL lithium carbonate and 0.01moL manganese carbonate and is dissolved in 3mL ethylene glycol ethyl ether, form the second solution； The first solution is added in second solution, 45 DEG C of constant temperature water baths stir evenly, and form third solution, then by third solution in 45 DEG C of water Evaporation at constant temperature is bathed into 10mL gel；
10mL colloidal sol is placed in 650 DEG C of calcining 7h of argon gas atmosphere stove by step 2, obtains preparation Li2MnSiO44With amorphous carbon Compound orthosilicate nanofiber anode active material of lithium ion battery.
Embodiment 4: preparation Li2NiSiO4The orthosilicate nanofiber lithium ion cell positive activity compound with amorphous carbon Material, specific steps:
Step 1 weighs 0.5 surfactant P123, it is dissolved in 15mL water, forms the first solution；It successively weighs again 2.088g sodium metasilicate, 0.02moL lithium nitrate and 0.01moL nickel nitrate are dissolved in 3mL water, form the second solution；By the second solution The first solution is added, 45 DEG C of constant temperature water baths stir evenly, and form third solution, then third solution is evaporated in 45 DEG C of constant temperature water baths At 10mL gel；
10mL colloidal sol is placed in 650 DEG C of calcining 7h of nitrogen atmosphere stove, obtains Li by step 22NiSiO4It is compound with amorphous carbon Orthosilicate nanofiber anode active material of lithium ion battery.
To the Li of all embodiments2MSiO4The orthosilicate nanofiber lithium ion cell positive activity compound with amorphous carbon The electrochemistry of material can be carried out detection.By taking embodiment 1 as an example, in conjunction with Fig. 1, Fig. 2 and Fig. 3, illustrate Li2FeSiO4With amorphous carbon The structure and chemical property of compound orthosilicate nanofiber anode active material of lithium ion battery, characterization result is such as Under:
It referring to Fig.1, is Li2FeSiO4The orthosilicate nanofiber anode material for lithium-ion batteries compound with amorphous carbon X-ray diffraction (XRD) map；Its abscissa is 2 θ of measurement angle of X-ray diffraction, and unit is ° (degree), and ordinate is material Diffraction the sealing strength intensity, unit a.u. in this angle of diffraction.It is analyzed by profiling results it is found that synthesizing just Silicate nano-fiber anode active material of lithium ion battery is pure phase Li2FeSiO4, and it is miscellaneous without other, purity is higher.
It is Li referring to Fig. 22FeSiO4The orthosilicate nanofiber lithium ion cell positive activity material compound with amorphous carbon Scanning electron microscope (SEM) map of material.It can be seen from the figure that diameter, which is 20-30 nanometers, is about 200-300 nanometers Li2FeSi04/ C composite nano fiber good dispersion, nanofiber yield are very high.
It is Li referring to Fig. 32FeSiO4The orthosilicate nanofiber lithium ion cell positive activity material compound with amorphous carbon The circulation curve graph of material.Its abscissa is cycle-index cycle number, and ordinate is the specific capacity of material Specific capacity, unit mAh/g；Closed square indicates that the data of charging charge, empty circles indicate electric discharge The data of discharge.As seen from the figure, in 0.1C multiplying power, the orthosilicate nanofiber lithium ion cell positive activity material The specific capacity of material maintains 190mAh/g or so, and in repeatedly circulation 10C high magnification, specific capacity remains to maintain 110mAh/g Left and right, shows good high rate performance.
Obviously, according to Li prepared by the present invention2FeSiO4Orthosilicate (M=Fe, Mn, Co, Ni) compound with amorphous carbon is received Rice fiber anode active material of lithium ion battery, can effectively improve electrolyte in Li2FeSiO4Infiltration during material circulation Thoroughly, while P123The stable circulation performance of material can be effectively improved by introducing amorphous carbon material.
(M=Mn, Co, the Ni) and the compound orthosilicate nanofiber lithium ion battery of amorphous carbon of other embodiments preparation Quite, same purity is high, good dispersion also show good, stable circulation for positive electrode active materials, performance and embodiment 1 Performance.
The above is only preferable case of the invention, does not make any restrictions to the present invention, all for the present invention Any simple modification, alteration or imitation that technology contents do the above case study on implementation belongs to the protection of technical solution of the present invention Range.

Claims (5)

1. a kind of preparation method of orthosilicate nanofiber anode active material of lithium ion battery, the orthosilicate Nanowire Dimension anode active material of lithium ion battery is orthosilicate Li2MSiO4The orthosilicate of nanocrystal and amorphous carbon composition Li2MSiO4/ C composite nano fiber anode active material of lithium ion battery, including following material component: carbon raw material, silicon raw material, lithium Salt and M salt, M Fe, Mn, Co or Ni；Characterized by comprising the following steps:
Step 1 weighs carbon raw material and is dissolved in liquid solvent, forms the first solution；Silicon raw material, lithium salts and M salt are successively weighed again It is separately dissolved in the liquid solvent, forms the second solution；Then, the first solution is added in the second solution, constant temperature stirs evenly, shape At third solution, then by third solution evaporation at constant temperature at gel；Wherein, the carbon raw material is polyethylene oxide-polypropylene oxide- Polyethylene oxide block copolymer surfactant；The silicon raw material is ethyl orthosilicate, methyl orthosilicate or sodium metasilicate；It is described Lithium salts is lithium nitrate, lithium carbonate or lithium acetate；The M salt is nitrate, carbonate or acetate, M Fe, Mn, Co or Ni；
Step 2 is heat-treated gel, obtains orthosilicate nanofiber anode active material of lithium ion battery.
2. the preparation method of orthosilicate nanofiber anode active material of lithium ion battery according to claim 1, It is characterized in that, the liquid solvent is methanol, ethyl alcohol, ethylene glycol or ethylene glycol ethyl ether.
3. the preparation method of orthosilicate nanofiber anode active material of lithium ion battery according to claim 1, It is characterized in that, the evaporation at constant temperature temperature is from room temperature within the scope of 80 DEG C.
4. the preparation method of orthosilicate nanofiber anode active material of lithium ion battery according to claim 1, It is characterized in that, the heat treatment is heat-treated 6-20 hours for 600-800 DEG C of inert atmosphere furnace calcining.
5. the preparation method of orthosilicate nanofiber anode active material of lithium ion battery according to claim 4, It is characterized in that, the atmosphere in the inert gas atmosphere furnace is nitrogen, argon gas, carbon dioxide.
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CN103078120A (en) * 2013-01-22 2013-05-01 武汉理工大学 Ferrous silicate lithium ion battery cathode material with hierarchical structure and preparation method
CN104183827A (en) * 2014-08-21 2014-12-03 浙江大学 Lithium iron phosphate nanorods and preparation method thereof

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CN103078120A (en) * 2013-01-22 2013-05-01 武汉理工大学 Ferrous silicate lithium ion battery cathode material with hierarchical structure and preparation method
CN104183827A (en) * 2014-08-21 2014-12-03 浙江大学 Lithium iron phosphate nanorods and preparation method thereof

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