CN106848266A - A kind of preparation method of lithium position sodium-doped collaboration nitrogen-doped carbon coating modification barium titanate lithium titanate cathode material - Google Patents

A kind of preparation method of lithium position sodium-doped collaboration nitrogen-doped carbon coating modification barium titanate lithium titanate cathode material Download PDF

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CN106848266A
CN106848266A CN201710223534.4A CN201710223534A CN106848266A CN 106848266 A CN106848266 A CN 106848266A CN 201710223534 A CN201710223534 A CN 201710223534A CN 106848266 A CN106848266 A CN 106848266A
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lithium
doped
hours
barium
sodium
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CN106848266B (en
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罗明贺
舒杰
吴瑶瑶
杨科
张延玉
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Ningbo 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
    • 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
    • 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
    • H01M4/485—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
    • H01M4/58—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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
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Abstract

A kind of lithium position sodium-doped collaboration nitrogen-doped carbon coating modification barium titanate lithium titanate cathode material, comprises the following steps：Take barium nitrate, lithium nitrate, sodium acetate, titanium dioxide, carbon black ball milling mixing, then the powder of gained is sintered in Muffle furnace, first constant temperature carries out pre-burning to decompose salt for 5 hours at 650 DEG C, then sintered 10 hours at 950 DEG C again, naturally cool to room temperature and can obtain lithium position sodium-doped metatitanic acid barium-lithium.Next; the lithium position sodium-doped metatitanic acid barium-lithium of gained is put into porcelain boat to be placed in tube-type atmosphere furnace; then another porcelain boat that melamine will be held is also placed in tube-type atmosphere furnace; it is placed in the upstream end of air-flow; with argon gas as protection gas, processed 2 hours at 650 DEG C, after naturally cooling to room temperature; take out product and pulverize, products therefrom is lithium position sodium-doped collaboration nitrogen-doped carbon coating modification barium titanate lithium titanate cathode material.

Description

A kind of lithium position sodium-doped collaboration nitrogen-doped carbon coating modification barium titanate lithium titanate cathode material Preparation method
Technical field
The present invention relates to a kind of barium titanate lithium titanate cathode material of lithium ion battery, more particularly, to a kind of lithium position sodium-doped association With the preparation method of nitrogen-doped carbon coating modification barium titanate lithium titanate cathode material.
Background technology
China puts into effect new-energy automobile support policy in succession in recent years, embodies country particularly electronic to new-energy automobile The attention of development of automobile.However, China's major part electric automobile outfit is all lead-acid battery, this kind of battery specific energy is low, the longevity Life is short, often using 1 year afterwards battery be accomplished by scrapping renewal, and heavy metal and the sulfuric acid pair such as lead, cadmium contained in battery Environment has serious harm, and the recovery technology difficulty of this kind of battery is big, and current recovery operation stays cool.Cause This is, it is necessary to Development of Novel electrokinetic cell.
Among all kinds of chemomotive force power supplys, dynamic lithium battery has high workload current potential, high-energy-density and circulation longevity because of it The advantages of ordering long and be considered as the novel energy storage device for most having development potentiality, at present progressively substitute lead-acid battery conduct The power source of electric automobile.It is true for electrokinetic cell although the protection circuit of lithium ion battery comparative maturity Positive to ensure safety, the selection of negative material is very crucial.The negative material of current commercial li-ion battery is mostly carbon material, and Close to lithium metal, when the battery is overcharged, lithium metal may produce dendrite to the intercalation potential of carbon material on Carbon anode surface, so that Piercing through barrier film causes battery short circuit.Metatitanic acid based material has intercalation potential higher it is possible to prevente effectively from the precipitation of lithium metal, And there is certain oxygen uptake function at high temperature, thus with obvious security features, it is considered to be instead of graphite as lithium The ideal chose of ion battery cathode material.Wherein Li4Ti5O12The titanium system negative material of successful commercialization, its maximum it is excellent Point is that volume is unchanged during removal lithium embedded, and good cycle is difficult to form Li dendrite in charge and discharge process, security It is high.But, relatively low lithium ion diffusion rate, low electric conductivity and theoretical capacity all constrain Li4Ti5O12It is more extensive Application；In addition, of a relatively high voltage platform (1.55 V), hence it is evident that reduce Li4Ti5O12As the full battery electricity of negative pole Pressure, and then reduce the energy density of battery.Therefore, the relatively low new titanate of the necessary reliable potential plateau of exploitation is born Pole material.
BaLi2Ti6O14It is a kind of new titanate negative material, it has the average embedding de- lithium current potential of 1.2V, and this makes Handy BaLi2Ti6O14Full battery as negative pole has operating voltage higher, energy density and power density. BaLi2Ti6O14Crystal structure in, [TiO6] octahedra [Ti basic with summit composition altogether by common side6O14]n -4nThree dimensional network Network skeleton, [LiO4] tetrahedron and [BaO11] polyhedron is in this [TiO6] octahedra [Ti for constituting6O14]n -4nIn tunnel structure It is staggered.Meanwhile, [Ti6O14]n -4nThere is tetrahedral vacancy 4a, tetrahedral vacancy 4b, octahedral voids 8c in tunnel structure And polyhedron room 8f, these different rooms provide substantial amounts of space for the storage of lithium ion so that these compounds are made For lithium storage materials have larger potential using value.In addition, with [LiO4] tetrahedron adjacent tetrahedral vacancy and octahedron Room is connected by coplanar, and the void geometry being mutually communicated in these tunnels provides expansion for the quick embedded abjection of lithium ion Dissipate passage.It follows that BaLi2Ti6O14Lithium ion battery electrode material is highly suitable as, however it is simple BaLi2Ti6O14Have the shortcomings that electronics and ionic conductivity are low, therefore it is modified in the urgent need to adopting an effective measure, To lift its chemical property.
Existing BaLi2Ti6O14The method of modifying of negative material, mainly carries out metal ion mixing, including Ag to barium position+、 Pb2+、Al3+、La3+Plasma, while surface silver cladding is have also been attempted, however, single modified measures all fail effective acquisition High performance metatitanic acid barium-lithium, so as to a kind of high power extended-life lithium ion battery that can meet current social demand can not be obtained bear Pole material.
The content of the invention
The technical problems to be solved by the invention are to provide one kind and prepare lithium position sodium-doped collaboration nitrogen-doped carbon coating modification The method of barium titanate lithium titanate cathode material, the synthetic method is by first building a kind of granular lithium position sodium-doped barium titanate cathode of lithium Material, then carries out nitrogen-doped carbon cladding, so as to obtain a kind of Stability Analysis of Structures, fine and close titanium system negative material, resulting titanium The particle of sour barium-lithium negative material is homogeneous, particle diameter distribution is uniform, electronics and ionic conductivity are high, so as to effectively improve barium titanate The chemical property of lithium titanate cathode material.
The present invention solve the technical scheme that is used of above-mentioned technical problem for：A kind of lithium position sodium-doped association of lithium ion battery With the preparation method of nitrogen-doped carbon coating modification barium titanate lithium titanate cathode material, comprise the following steps：First, 0.1 molar nitric acid is taken Barium, 0.2 molar nitric acid lithium, 0.01-0.05 mole of acetic acid sodium, 0.6 mole of nano titanium oxide（6 nm）, 0.1 mole of carbon black exist 400 revs/min of lower ball milling mixings 19 hours, it is finely ground in agate mortar after being placed in 150 DEG C of oven for drying, then powder is existed Be sintered in Muffle furnace, first with 2 hours from room temperature to 650 DEG C, and at such a temperature constant temperature carry out within 5 hours pre-burning with point Solution salt, was then warmed up to 950 DEG C with 2 hours again, and was kept for 10 hours at such a temperature, naturally cools to room temperature and can obtain Lithium position sodium-doped metatitanic acid barium-lithium.Next, the lithium position sodium-doped metatitanic acid barium-lithium of gained is put into porcelain boat is placed in tube-type atmosphere furnace In, another porcelain boat that then will hold melamine is also placed in tube-type atmosphere furnace, is placed in the upstream end of air-flow, is made with argon gas Be protection gas, with 2 hours from room temperature to 650 DEG C, and at such a temperature be incubated 2 hours, after naturally cooling to room temperature, take out Product is simultaneously pulverized, and products therefrom is lithium position sodium-doped collaboration nitrogen-doped carbon coating modification barium titanate lithium titanate cathode material.
Compared with prior art, the advantage of the invention is that：（1）The particle of barium titanate lithium titanate cathode material prepared by the method Uniform particle diameter, Stability Analysis of Structures, densification.The addition of wherein nano grade carbon black can cause the homogenization of metatitanic acid barium-lithium particle, lithium position Natrium doping can significantly lift the ionic conductivity in metatitanic acid barium-lithium structure, and nitrogen-doped carbon cladding can be obviously improved metatitanic acid The electronic conductivity of barium-lithium, and then cause that barium titanate lithium titanate cathode material has superior chemical property.（2）Meanwhile, the method Nitrogen-doped carbon cladding is carried out using the rising technology of melamine, the technological operation is easy, the carbon-coating of gained is thin and homogeneous, not In the case of reducing barium titanate lithium titanate cathode material reversible capacity, can significantly improve its high rate performance, high power, length can be met The need for life-span lithium ion battery practical application.
Brief description of the drawings
Fig. 1 is the lithium position sodium-doped collaboration nitrogen-doped carbon coating modification barium titanate lithium titanate cathode material of gained in the embodiment of the present invention Scanning electron microscope (SEM) photograph.
Specific embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
Embodiment 1：Take 0.1 molar nitric acid barium, 0.2 molar nitric acid lithium, 0.01 mole of acetic acid sodium, 0.6 mole of nano-silica Change titanium（6 nm）, 0.1 mole of carbon black in 400 revs/min of lower ball milling mixings 19 hours, after being placed in 150 DEG C of oven for drying, in agate It is finely ground in mortar, then powder is sintered in Muffle furnace, first with 2 hours from room temperature to 650 DEG C, and in the temperature Lower constant temperature carries out pre-burning for 5 hours to decompose salt, is then warmed up to 950 DEG C with 2 hours again, and holding 10 is small at such a temperature When, naturally cool to room temperature and can obtain lithium position sodium-doped metatitanic acid barium-lithium.Next, by the lithium position sodium-doped metatitanic acid barium-lithium of gained It is put into porcelain boat to be placed in tube-type atmosphere furnace, another porcelain boat that then will hold melamine is also placed in tube-type atmosphere furnace, and Be placed in the upstream end of air-flow, with argon gas as protection gas, with 2 hours from room temperature to 650 DEG C, and be incubated 2 at such a temperature Hour, after naturally cooling to room temperature, taking out product and pulverize, products therefrom is lithium position sodium-doped collaboration nitrogen-doped carbon bag Cover modified barium carbonate lithium titanate cathode material.Using the product of gained as Electrode, metal lithium sheet as to electrode, full of argon gas Glove box in be assembled into fastening lithium ionic cell, carrying out discharge and recharge in 0.5-3.0V potential regions with the multiplying power of 0.1C follows Ring, it is 192mAh/g that can obtain discharge capacity first, and charging capacity is 174mAh/g, and the reversible capacity after it is circulated 100 weeks is 168mAh/g；Charge and discharge cycles are carried out in 0.5-3.0V potential regions with the multiplying power of 5C, can obtain discharge capacity first is 168mAh/g, charging capacity is 160mAh/g, and its reversible capacity after circulating 100 weeks is 155mAh/g, it is shown that excellent electricity Chemical property.
Embodiment 2：Take 0.1 molar nitric acid barium, 0.2 molar nitric acid lithium, 0.03 mole of acetic acid sodium, 0.6 mole of nano-silica Change titanium（6 nm）, 0.1 mole of carbon black in 400 revs/min of lower ball milling mixings 19 hours, after being placed in 150 DEG C of oven for drying, in agate It is finely ground in mortar, then powder is sintered in Muffle furnace, first with 2 hours from room temperature to 650 DEG C, and in the temperature Lower constant temperature carries out pre-burning for 5 hours to decompose salt, is then warmed up to 950 DEG C with 2 hours again, and holding 10 is small at such a temperature When, naturally cool to room temperature and can obtain lithium position sodium-doped metatitanic acid barium-lithium.Next, by the lithium position sodium-doped metatitanic acid barium-lithium of gained It is put into porcelain boat to be placed in tube-type atmosphere furnace, another porcelain boat that then will hold melamine is also placed in tube-type atmosphere furnace, and Be placed in the upstream end of air-flow, with argon gas as protection gas, with 2 hours from room temperature to 650 DEG C, and be incubated 2 at such a temperature Hour, after naturally cooling to room temperature, taking out product and pulverize, products therefrom is lithium position sodium-doped collaboration nitrogen-doped carbon bag Cover modified barium carbonate lithium titanate cathode material.Using the product of gained as Electrode, metal lithium sheet as to electrode, full of argon gas Glove box in be assembled into fastening lithium ionic cell, carrying out discharge and recharge in 0.5-3.0V potential regions with the multiplying power of 0.1C follows Ring, it is 195mAh/g that can obtain discharge capacity first, and charging capacity is 177mAh/g, and the reversible capacity after it is circulated 100 weeks is 171mAh/g；Charge and discharge cycles are carried out in 0.5-3.0V potential regions with the multiplying power of 5C, can obtain discharge capacity first is 162mAh/g, charging capacity is 151mAh/g, and its reversible capacity after circulating 100 weeks is 144mAh/g, it is shown that excellent electricity Chemical property.
Embodiment 3：Take 0.1 molar nitric acid barium, 0.2 molar nitric acid lithium, 0.05 mole of acetic acid sodium, 0.6 mole of nano-silica Change titanium（6 nm）, 0.1 mole of carbon black in 400 revs/min of lower ball milling mixings 19 hours, after being placed in 150 DEG C of oven for drying, in agate It is finely ground in mortar, then powder is sintered in Muffle furnace, first with 2 hours from room temperature to 650 DEG C, and in the temperature Lower constant temperature carries out pre-burning for 5 hours to decompose salt, is then warmed up to 950 DEG C with 2 hours again, and holding 10 is small at such a temperature When, naturally cool to room temperature and can obtain lithium position sodium-doped metatitanic acid barium-lithium.Next, by the lithium position sodium-doped metatitanic acid barium-lithium of gained It is put into porcelain boat to be placed in tube-type atmosphere furnace, another porcelain boat that then will hold melamine is also placed in tube-type atmosphere furnace, and Be placed in the upstream end of air-flow, with argon gas as protection gas, with 2 hours from room temperature to 650 DEG C, and be incubated 2 at such a temperature Hour, after naturally cooling to room temperature, taking out product and pulverize, products therefrom is lithium position sodium-doped collaboration nitrogen-doped carbon bag Cover modified barium carbonate lithium titanate cathode material.Using the product of gained as Electrode, metal lithium sheet as to electrode, full of argon gas Glove box in be assembled into fastening lithium ionic cell, carrying out discharge and recharge in 0.5-3.0V potential regions with the multiplying power of 0.1C follows Ring, it is 187mAh/g that can obtain discharge capacity first, and charging capacity is 166mAh/g, and the reversible capacity after it is circulated 100 weeks is 160mAh/g；Charge and discharge cycles are carried out in 0.5-3.0V potential regions with the multiplying power of 5C, can obtain discharge capacity first is 163mAh/g, charging capacity is 159mAh/g, and its reversible capacity after circulating 100 weeks is 155mAh/g, it is shown that excellent electricity Chemical property.

Claims (1)

1. it is a kind of it is lithium position sodium-doped collaboration nitrogen-doped carbon coating modification barium titanate lithium titanate cathode material preparation method, it is characterised in that Comprise the following steps：First, take 0.1 molar nitric acid barium, 0.2 molar nitric acid lithium, 0.01-0.05 mole of acetic acid sodium, 0.6 mole receive Rice titanium dioxide（6 nm）, 0.1 mole of carbon black in 400 revs/min of lower ball milling mixings 19 hours, after being placed in 150 DEG C of oven for drying, It is finely ground in agate mortar, then powder is sintered in Muffle furnace, first with 2 hours from room temperature to 650 DEG C, and Constant temperature carries out pre-burning for 5 hours to decompose salt at this temperature, is then warmed up to 950 DEG C with 2 hours again, and keep at such a temperature 10 hours, naturally cool to room temperature and can obtain lithium position sodium-doped metatitanic acid barium-lithium；Next, by the lithium position sodium-doped metatitanic acid of gained Barium-lithium is put into porcelain boat and is placed in tube-type atmosphere furnace, and another porcelain boat that then will hold melamine is also placed in tubular type atmosphere Stove, is placed in the upstream end of air-flow, with argon gas as protection gas, with 2 hours from room temperature to 650 DEG C, and at such a temperature Insulation 2 hours, after naturally cooling to room temperature, takes out product and pulverizes, and products therefrom is lithium position sodium-doped collaboration nitrogen and mixes Miscellaneous coated modified carbon barium titanate lithium titanate cathode material.
CN201710223534.4A 2017-04-07 2017-04-07 A kind of preparation method of lithium position sodium-doped collaboration nitrogen-doped carbon coating modification barium titanate lithium titanate cathode material Active CN106848266B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113066971A (en) * 2021-03-30 2021-07-02 宁波容百新能源科技股份有限公司 Gas phase coating method of lithium-rich manganese-based positive electrode material

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US20090208847A1 (en) * 2008-02-15 2009-08-20 Samsung Sdi Co., Ltd. Anode active material, method of preparing the same, and anode and lithium battery containing the anode active material
CN101924201A (en) * 2010-07-26 2010-12-22 郑州大学 Method for preparing lithium ion battery negative material carbon-coated and metal-doped lithium titanate
CN104409712A (en) * 2014-09-19 2015-03-11 四川省有色冶金研究院有限公司 Preparation method of carbon and nitrogen coated lithium titanate material

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Publication number Priority date Publication date Assignee Title
US20090208847A1 (en) * 2008-02-15 2009-08-20 Samsung Sdi Co., Ltd. Anode active material, method of preparing the same, and anode and lithium battery containing the anode active material
CN101924201A (en) * 2010-07-26 2010-12-22 郑州大学 Method for preparing lithium ion battery negative material carbon-coated and metal-doped lithium titanate
CN104409712A (en) * 2014-09-19 2015-03-11 四川省有色冶金研究院有限公司 Preparation method of carbon and nitrogen coated lithium titanate material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113066971A (en) * 2021-03-30 2021-07-02 宁波容百新能源科技股份有限公司 Gas phase coating method of lithium-rich manganese-based positive electrode material

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