CN110165165A - Rich lithium NiTi molybdenum oxide positive electrode, anode pole piece and preparation method thereof and lithium battery - Google Patents

Rich lithium NiTi molybdenum oxide positive electrode, anode pole piece and preparation method thereof and lithium battery Download PDF

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CN110165165A
CN110165165A CN201910393354.XA CN201910393354A CN110165165A CN 110165165 A CN110165165 A CN 110165165A CN 201910393354 A CN201910393354 A CN 201910393354A CN 110165165 A CN110165165 A CN 110165165A
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positive electrode
niti
lithium
molybdenum oxide
preparation
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杨志远
王聪
张天赐
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Hubei Lithium Nuo Amperex Technology Ltd
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Hubei Lithium Nuo Amperex Technology Ltd
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    • H01—ELECTRIC ELEMENTS
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    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • H01M4/366—Composites as layered products
    • H—ELECTRICITY
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    • 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
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • H01M4/52—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
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract

The invention discloses rich lithium NiTi molybdenum oxide positive electrode, anode pole piece and preparation method thereof and lithium batteries, belong to technical field of lithium batteries.Wherein, which includes metal oxide LixNiyTizMowO2Be coated on metal oxide LixNiyTizMowO2The sull on surface, sull with a thickness of 5~10nm, and x, y, z and w meet following relationship: the invention also discloses the preparation methods of positive electrode by x+y+z+w=2, specifically take metal oxide LixNiyTizMowO2It is combined with polyvinylpyrrolidone induction, and esters of silicon acis forms silica membrane under polyvinylpyrrolidone wet process auxiliary, then SiO is made through calcination processing2Coat LixNiyTizMowO2Positive electrode.The lithium battery that the present invention designs, due to SiO in positive electrode2Film can effectively prevent the side reaction between metal oxide and electrolyte, be conducive to the service life cycle for improving entire battery.

Description

Rich lithium NiTi molybdenum oxide positive electrode, anode pole piece and preparation method thereof and lithium Battery
Technical field
The present invention relates to cell positive materials, belong to technical field of lithium batteries, more particularly to a kind of rich lithium NiTi molybdenum oxygen Compound positive electrode, anode pole piece and preparation method thereof and lithium battery.
Background technique
With being continuously increased to high performance lithium ion battery demand, the positive electrode of high-energy density is from various chemistry Seek to be prepared in space.Common richness lithium rock salt transition metal oxide, such as Li1.3Mn0.4Nb0.3O2、 Li1.2Mn0.4Ti0.4O2、Li9/7Nb2/7Mo3/7O2And Li1.2Ni1/3Ti1/3Mo2/15O2, as a kind of novel high-capacity anode material Material is just by increasingly extensive concern, this is because the battery prepared by such material, capacity are up to 300mAh/g, however, by The presence of minor amount of water in battery is easier to react generation hydrofluoric acid with electrolyte, and then corrode positive electrode surface to cause This kind of richness lithium material is faced with the problem that battery capacity decaying is very fast and cycle performance is poor.
In order to solve the above technical problems, being usually chosen in rich lithium material surface coats one layer of protective oxide film, by this Protective layer plays the role of physical protection barrier, electronic conduction medium, ion conducting medium or HF scavenger.However single oxygen There is the disadvantages of having a single function, clad is coarse in compound clad.And most of oxides have low lithium diffusivity and increased Interface resistance, this limits to a certain extent through oxide cladding layers the further expansion application for improving battery performance.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of rich lithium NiTi molybdenum oxide positive electrode and its preparation sides Method and lithium battery.The sull on the positive electrode surface can prevent to react between interior metal oxide and electrolyte Probability, to improve the service life cycle and stability of entire lithium battery.
To achieve the above object, the invention discloses a kind of rich lithium NiTi molybdenum oxide positive electrode, it includes metal oxygen Compound LixNiyTizMowO2Be coated on the metal oxide LixNiyTizMowO2The sull on surface, the oxidation Object film with a thickness of 5~10nm, and x, y, z and w meet following relationship: x+y+z+w=2.
Further, discharge capacity is 200~230mAh/g to the positive electrode for the first time.
Preferably, discharge capacity is 208.4mAh/g to the positive electrode for the first time.
Further, the sull includes SiO2Film.
Further, the molecular formula of x=1.15, y=0.375, z=0.375, w=0.1, i.e., the described metal oxide is Li1.15Ni0.375Ti0.375Mo0.1O2, which has higher capacity.
In order to preferably realize technical purpose of the invention, the invention also discloses above-mentioned rich lithium NiTi molybdenum oxide anodes The preparation method of material, it includes taking metal oxide LixNiyTizMowO2It is combined with polyvinylpyrrolidone induction, and silicic acid Ester forms silica membrane under polyvinylpyrrolidone wet process auxiliary, then SiO is made through calcination processing2Cladding LixNiyTizMowO2Positive electrode.
Specifically, the preparation process of rich lithium NiTi molybdenum oxide positive electrode is as follows:
Take metal oxide LixNiyTizMowO2It is dispersed in n-methyl-2-pyrrolidone, adds polyvinylpyrrolidine Ketone stirs evenly, and continues that silicic acid ester solution is added dropwise, after reacting a period of time, washed, filtering and vacuum drying, most afterwards through calcining Processing.
Further, detailed process is as follows for the calcination processing:
4~8h is calcined at 500~600 DEG C of temperature of control.It is preferred that direct calcination processing in air.
Further, the esters of silicon acis includes at least one of methyl orthosilicate, ethyl orthosilicate or positive silicic acid propyl ester.
Further, the metal oxide LixNiyTizMowO2Preparation process it is as follows:
Take Li2CO3、NiO、TiO2And MoO2It mixes and ground mixture of powders, adds Li2CO3, 550~650 8~12h is calcined at DEG C, is continuously heating to 800~950 DEG C of 4~6h of calcining.
Preferably, pass through control molar ratio Ni:Ti:Mo=0.375:0.375:0.1 and excess Li is added2CO3, preparation Li1.15Ni0.375Ti0.375Mo0.1O2。
Preferably, mixture of powders is obtained by ball milling.
At the same time, the invention also discloses a kind of rich lithium NiTi molybdenum oxide anode pole piece, it includes plus plate current-collecting body And above-mentioned rich lithium NiTi molybdenum oxide positive electrode, the richness lithium NiTi molybdenum oxide positive electrode are coated on the anode collection Body surface face.
In addition, the invention also discloses a kind of lithium battery, it include above-mentioned rich lithium NiTi molybdenum oxide positive electrode or on State rich lithium NiTi molybdenum oxide anode pole piece.
Preferably, the discharge capacity for the first time of the lithium battery is 208.9~209.6mAh/g.
Optimal, the discharge capacity for the first time of the lithium battery is 209.6mAh/g.
Preferably, the capacity retention ratio of the lithium battery is 88.1~88.7%.
Optimal, the capacity retention ratio of the lithium battery is 88.7%.
Preferably, the coulombic efficiency for the first time of the lithium battery is 98.3~98.8.
Optimal, the coulombic efficiency for the first time of the lithium battery is 98.8%.
Preferably, the recovery rate of the lithium battery is 96.9~97.8%.
Optimal, the lithium battery reverts to 97.8%.
The beneficial effects are mainly reflected as follows following aspects:
1, the SiO that the present invention designs2Coat Li1.15Ni0.375Ti0.375Mo0.1O2Positive electrode, since sull can The probability to react between interior metal oxide and electrolyte is prevented, so that discharge capacity is the lithium battery of preparation for the first time 208.9~209.6mAh/g；Capacity retention ratio is 88.1~88.7%；Coulombic efficiency is 98.3~98.8 for the first time；Lithium battery Recovery rate is 96.9~97.8%.
2, the cycle performance of present invention design lithium battery is higher than the uncoated positive electrode in surface, and also higher than surface coats it The positive electrode of its sull.
Detailed description of the invention
Fig. 1 is the lithium battery performance comparison figure of preparation of the embodiment of the present invention；
Fig. 2 is the lithium battery performance comparison figure of preparation of the embodiment of the present invention.
Specific embodiment
In order to better explain the present invention, below in conjunction with the specific embodiment main contents that the present invention is furture elucidated, but The contents of the present invention are not limited solely to following embodiment.
Embodiment 1
Li1.15Ni0.375Ti0.375Mo0.1O2The preparation of material: by Li2CO3、NiO、TiO2And MoO2Mixing in acetone, Excessive 10% Li is added in ball milling 10h under 300rpm revolving speed2CO3, molar ratio Ni:Ti:Mo=0.375:0.375:0.1.Mixing Powder 600 DEG C of calcining 10h in air, then proceed to 850 DEG C of calcining 6h in air and obtain Li1.15Ni0.375Ti0.375Mo0.1O2Material.
SiO2Coat Li1.15Ni0.375Ti0.375Mo0.1O2The preparation of positive electrode: by 3g Li1.15Ni0.375Ti0.375Mo0.1O2Powder, which is distributed in 100mL n-methyl-2-pyrrolidone (NMP), stirs 30min.Then plus Enter 0.5g PVP K-30 to continue to stir 30min.The 20mL ethyl alcohol mixing containing 7.6mL tetraethyl orthosilicate (TEOS) is added dropwise again Liquid, stirs 6h, and washing, filtering calcine 500 DEG C of holding 8h in air, obtain SiO in 120 DEG C of vacuum drying 12h2Cladding Li1.15Ni0.375Ti0.375Mo0.1O2Material.
Embodiment 2
Li1.15Ni0.375Ti0.375Mo0.1O2The preparation of material: by Li2CO3、NiO、TiO2And MoO2Mixing in acetone, Excessive 10% Li is added in ball milling 10h under 300rpm revolving speed2CO3, molar ratio Ni:Ti:Mo=0.375:0.375:0.1.Mixing Powder 600 DEG C of calcining 10h in air, then proceed to 900 DEG C of calcining 5h in air and obtain Li1.15Ni0.375Ti0.375Mo0.1O2Material.
SiO2Coat Li1.15Ni0.375Ti0.375Mo0.1O2The preparation of positive electrode: by 3g Li1.15Ni0.375Ti0.375Mo0.1O2Powder, which is distributed in 100mL n-methyl-2-pyrrolidone (NMP), stirs 30min.Then plus Enter 0.3g PVP K-30 to continue to stir 30min.The 20mL alcohol mixeding liquid containing 2.5mL TEOS, positive silicic acid tetrem are added dropwise again The molar ratio of ester and rich lithium material is 1:3, stirs 5h, and washing, filtering in 120 DEG C of vacuum drying 12h, calcine 550 in air DEG C keep 6h, obtain SiO2Coat Li1.15Ni0.375Ti0.375Mo0.1O2Material.
Embodiment 3
Li1.15Ni0.375Ti0.375Mo0.1O2The preparation of material: by Li2CO3、NiO、TiO2And MoO2Mixing in acetone, Excessive 10% Li is added in ball milling 10h under 300rpm revolving speed2CO3, molar ratio Ni:Ti:Mo=0.375:0.375:0.1.Mixing Powder 600 DEG C of calcining 10h in air, then proceed to 950 DEG C of calcining 4h in air and obtain Li1.15Ni0.375Ti0.375Mo0.1O2Material.
SiO2Coat Li1.15Ni0.375Ti0.375Mo0.1O2The preparation of positive electrode: by 3g Li1.15Ni0.375Ti0.375Mo0.1O2Powder, which is distributed in 100mL n-methyl-2-pyrrolidone (NMP), stirs 30min.Then plus Enter 0.1g PVP K-30 to continue to stir 30min.The 20mL alcohol mixeding liquid containing 1.5mL TEOS, positive silicic acid tetrem are added dropwise again The molar ratio of ester and rich lithium material is 1:5, stirs 4h, and washing, filtering in 120 DEG C of vacuum drying 12h, calcine 600 in air DEG C keep 4h, obtain SiO2Coat Li1.15Ni0.375Ti0.375Mo0.1O2Material.
Embodiment 4
SiO2Coat lithium-rich manganese-based Li1.18Ni0.15Co0.15Mn0.52O2The preparation of positive electrode: by 3g Li1.18Ni0.15Co0.15Mn0.52O2Powder, which is distributed in 100mL n-methyl-2-pyrrolidone (NMP), stirs 30min.Then plus Enter 0.1g PVP K-30 to continue to stir 30min.The 20mL alcohol mixeding liquid containing 1.5mL TEOS, positive silicic acid tetrem are added dropwise again The molar ratio of ester and rich lithium material is 1:5, stirs 4h, and washing, filtering in 120 DEG C of vacuum drying 12h, calcine 600 in air DEG C keep 4h obtain SiO2Coat Li1.18Ni0.15Co0.15Mn0.52O2Material.
Embodiment 5
Al2O3Coat Li1.15Ni0.375Ti0.375Mo0.1O2The preparation of material: Al (NO3)3With Li1.15Ni0.375Ti0.375Mo0.1O2It is dispersed in 50mL ethyl alcohol, 300rpm revolving speed ball milling 10min, 100 DEG C of dry 2h, in air In 300 DEG C of calcining 5h, obtain Al2O3Coat Li1.15Ni0.375Ti0.375Mo0.1O2Material.
Embodiment 6
Li of the surface without any cladding1.15Ni0.375Ti0.375Mo0.1O2The preparation of material: by Li2CO3、NiO、TiO2With MoO2In acetone, excessive 10% Li is added in the ball milling 10h under 300rpm revolving speed for mixing2CO3, molar ratio Ni:Ti:Mo= 0.375:0.375:0.1.Mixed powder 600 DEG C of calcining 10h in air, then proceed to 1000 DEG C of calcining 6h in air and obtain To Li1.15Ni0.375Ti0.375Mo0.1O2Material.
The positive electrode material of above-described embodiment 1~6 prepares the performance test of battery: where controls other variables；
The capabilities list of each battery of table 1
Electro-chemical test in research is completed by CR-2032 button half-cell.Table 1 is Examples 1 to 6 preparation Battery recycled under the conditions of 1C and 1.5~4.6V 50 circle discharge capacities for the first time, respectively 209.6mAh/g, 208.9mAh/g, 209.3mAh/g, 201.7mAh/g, 208.8mAh/g and 208.4mAh/g, capacity retention ratio is respectively as follows: 88.1%, 88.7%, 88.5%, 80.8%, 84.9% and 75.2%.By above-mentioned table 1, and Fig. 1 and Fig. 2 is combined it is found that using SiO of the present invention2Cladding Li1.15Ni0.375Ti0.375Mo0.1O2The lithium battery of positive electrode preparation, discharge capacity and capacity retention ratio effect are best for the first time, this It may be that uniform SiO is synthesized using PVP Aided Wet because of what the present invention designed2Clad, one side PVP and metal ion In conjunction with another aspect SiO2Help that electrolyte is protected to reduce a possibility that side reaction occurs, to improve Li1.15Ni0.375Ti0.375Mo0.1O2The cycle performance of positive electrode.
At the same time, using Al2O3Coat Li1.15Ni0.375Ti0.375Mo0.1O2The performance phase of lithium battery is made in positive electrode Than the application SiO2Coat Li1.15Ni0.375Ti0.375Mo0.1O2Positive electrode be made lithium battery performance it is slightly worse, this may be because For Al2O3Clad is uneven in forming process, and influences its chemical property.And in example 4, SiO2Coat rich lithium Manganese base Li1.18Ni0.15Co0.15Mn0.52O2It is poor compared with the chemical property in other embodiments, the lithium-rich manganese-based of preparation may be attributed to Stratiform Li1.18Ni0.15Co0.15Mn0.52O2Than rock salt phase Li1.15Ni0.375Ti0.375Mo0.1O2Performance is poor.
And Li of the surface without any cladding1.15Ni0.375Ti0.375Mo0.1O2The capacity retention ratio of lithium battery is made in positive electrode Lower than SiO2Conservation rate after cladding, because with electrolyte side reaction may occur for rich lithium material, capacity attenuation is very fast, cycle performance It is poor；And side reaction is inhibited to carry out raising cycle performance after coating.
Above embodiments are only best citing, rather than a limitation of the embodiments of the present invention.Except above-described embodiment Outside, there are also other embodiments by the present invention.All technical solutions formed using equivalent substitution or equivalent transformation, all fall within the present invention It is required that protection scope.

Claims (10)

1. a kind of richness lithium NiTi molybdenum oxide positive electrode, it includes metal oxide LixNiyTizMowO2Be coated on the gold Belong to oxide LixNiyTizMowO2The sull on surface, the sull with a thickness of 5~10nm, and x, y, z and w Meet following relationship: x+y+z+w=2.
2. rich lithium NiTi molybdenum oxide positive electrode according to claim 1, it is characterised in that: the positive electrode is put for the first time Capacitance is 200~230mAh/g.
3. richness lithium NiTi molybdenum oxide positive electrode according to claim 1 or claim 2, it is characterised in that: the sull Including SiO2Film.
4. richness lithium NiTi molybdenum oxide positive electrode according to claim 1 or claim 2, it is characterised in that: x=1.15, y= 0.375, z=0.375, w=0.1.
5. the preparation method of richness lithium NiTi molybdenum oxide positive electrode described in a kind of claim 1, it includes taking metal oxide LixNiyTizMowO2It is combined with polyvinylpyrrolidone induction, and esters of silicon acis forms two under polyvinylpyrrolidone wet process auxiliary Silicon oxide film, then SiO is made through calcination processing2Coat LixNiyTizMowO2Positive electrode.
6. the preparation method of rich lithium NiTi molybdenum oxide positive electrode according to claim 5, it is characterised in that: the calcining Detailed process is as follows for processing:
4~8h is calcined at 500~600 DEG C of temperature of control.
7. according to the preparation method of the rich lithium NiTi molybdenum oxide positive electrode of claim 5 or 6, it is characterised in that: described Esters of silicon acis includes at least one of methyl orthosilicate, ethyl orthosilicate or positive silicic acid propyl ester.
8. according to the preparation method of the rich lithium NiTi molybdenum oxide positive electrode of claim 5 or 6, it is characterised in that: described Metal oxide LixNiyTizMowO2Preparation process it is as follows:
Take Li2CO3、NiO、TiO2And MoO2It mixes and ground mixture of powders, adds Li2CO3, at 550~650 DEG C 8~12h is calcined, 800~950 DEG C of 4~6h of calcining are continuously heating to.
9. a kind of richness lithium NiTi molybdenum oxide anode pole piece, it is characterised in that: it includes plus plate current-collecting body and Claims 1 to 4 Any one of described in richness lithium NiTi molybdenum oxide positive electrode, the richness lithium NiTi molybdenum oxide positive electrode is coated on described Plus plate current-collecting body surface.
10. a kind of lithium battery, it is characterised in that: it includes richness lithium NiTi molybdenum oxide described in any one of Claims 1 to 4 Richness lithium NiTi molybdenum oxide anode pole piece described in positive electrode or claim 9.
CN201910393354.XA 2019-05-13 2019-05-13 Rich lithium NiTi molybdenum oxide positive electrode, anode pole piece and preparation method thereof and lithium battery Pending CN110165165A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114678510A (en) * 2022-04-18 2022-06-28 合肥工业大学 Selenium-coated disordered lithium-rich material and preparation method thereof

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Application publication date: 20190823