CN106816597B - A kind of preparation method of lithium position magnalium codope collaboration nitrogen sulfur doping coated modified carbon barium titanate lithium titanate cathode material - Google Patents
A kind of preparation method of lithium position magnalium codope collaboration nitrogen sulfur doping coated modified carbon barium titanate lithium titanate cathode material Download PDFInfo
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- 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
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Abstract
The present invention relates to a kind of lithium position magnalium codopes to cooperate with nitrogen sulfur doping coated modified carbon barium titanate lithium titanate cathode material, characterized by the following steps: take barium nitrate, lithium nitrate, magnesium acetate, aluminum acetate, nano-titanium dioxide, acetylene black in ball milling mixing, then resulting powder is sintered in Muffle furnace, the first constant temperature progress pre-burning in 4 hours at 650 DEG C is to decompose salt, then it is sintered 14 hours at 980 DEG C again, naturally cooling to room temperature can be obtained lithium position magnalium codope metatitanic acid barium-lithium.Next; resulting lithium position magnalium codope metatitanic acid barium-lithium is put into porcelain boat to be placed in tube-type atmosphere furnace; then another porcelain boat for holding cystine is also placed in tube-type atmosphere furnace; it is placed in the upstream end of air-flow; it uses argon gas as protection gas, is handled 2 hours at 680 DEG C, after naturally cooling to room temperature; it takes out product and pulverizes, products therefrom is lithium position magnalium codope collaboration nitrogen sulfur doping coated modified carbon barium titanate lithium titanate cathode material.
Description
Technical field
The present invention relates to a kind of barium titanate lithium titanate cathode materials of lithium ion battery, are co-doped with more particularly, to a kind of lithium position magnalium
The preparation method of miscellaneous collaboration nitrogen sulfur doping coated modified carbon barium titanate lithium titanate cathode material.
Background technique
China puts into effect new-energy automobile support policy in succession in recent years, and it is especially electronic to new-energy automobile to embody country
The attention of development of automobile.However, what China's major part electric car was equipped with is all lead-acid battery, this kind of battery specific energy is low, the longevity
It orders short, often just needs to scrap update using battery after 1 year, and the heavy metals such as lead, cadmium contained in battery and sulfuric acid pair
Environment has serious harm, and the recovery technology difficulty of this kind of battery is big, and current recovery operation stays cool.Cause
This, needs Development of Novel power battery.
Among all kinds of chemomotive force power supplys, dynamic lithium battery is because it is with high operating potential, high-energy-density and circulation longevity
It orders the advantages that long and is considered as the new energy storage device for most having development potentiality, gradually substitute lead-acid battery conduct at present
The power source of electric car.Although comparative maturity will be very for power battery for the protection circuit of lithium ion battery
Positive to guarantee safety, the selection of negative electrode material is very crucial.The negative electrode material of commercial li-ion battery is mostly carbon material at present, and
The intercalation potential of carbon material is close to lithium metal, and when the battery is overcharged, lithium metal may generate dendrite on Carbon anode surface, thus
Piercing through diaphragm leads to battery short circuit.Metatitanic acid based material intercalation potential with higher it is possible to prevente effectively from lithium metal precipitation,
And there is certain oxygen absorption function at high temperature, thus there are apparent security features, it is considered to be instead of graphite as lithium
The ideal chose of ion battery cathode material.Wherein Li4Ti5O12It is the titanium system negative electrode material of successful commercialization, it is maximum excellent
Volume is unchanged during point is removal lithium embedded, and good cycle is not easy to form Li dendrite in charge and discharge process, safety
It is high.But relatively low lithium ion diffusion rate, low electric conductivity and theoretical capacity all constrains Li4Ti5O12It is more extensive
Application；In addition, relatively high voltage platform (1.55 V), hence it is evident that reduce Li4Ti5O12Full battery electricity as cathode
Pressure, thereby reduces the energy density of battery.Therefore, it is born it is necessary to develop the lower novel titanate of reliable potential plateau
Pole material.
BaLi2Ti6O14It is a kind of novel titanate negative electrode material, its average embedding de- lithium current potential with 1.2V, this makes
Handy BaLi2Ti6O14Full battery as cathode has higher operating voltage, energy density and power density.?
BaLi2Ti6O14Crystal structure in, [TiO6] octahedron passes through total side and vertex forms basic [Ti altogether6O14]n -4nThree dimensional network
Network skeleton, [LiO4] tetrahedron and [BaO11] polyhedron is in this [TiO6] octahedra [Ti constituted6O14]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 vacancy 8f, these different vacancy provide a large amount of space for the storage of lithium ion, so that these compounds are made
There is biggish potential using value for lithium storage materials.In addition, with [LiO4] tetrahedron adjacent tetrahedral vacancy and octahedron
Vacancy is connected by coplanar, and the void geometry being mutually communicated in these tunnels provides expansion for the quick insertion abjection of lithium ion
Dissipate channel.It follows that BaLi2Ti6O14It is highly suitable as lithium ion battery electrode material, however merely
BaLi2Ti6O14Have the shortcomings that electronics and ionic conductivity are low, therefore there is an urgent need to adopt an effective measure to be modified it,
To promote its chemical property.
Existing BaLi2Ti6O14The method of modifying of negative electrode material mainly carries out metal ion mixing, including Ag to barium position+、
Pb2+、Al3+、La3+Plasma, while surface silver cladding has also been attempted, however, single modified measures all fail effectively to obtain
High performance metatitanic acid barium-lithium, so that it is negative to obtain a kind of high power extended-life lithium ion battery for being able to satisfy current social demand
Pole material.
Summary of the invention
Lithium position magnalium codope collaboration nitrogen sulfur doping carbon packet is prepared technical problem to be solved by the invention is to provide a kind of
The method of modified barium carbonate lithium titanate cathode material is covered, the synthetic method is by first constructing a kind of granular lithium position magnalium codope titanium
Then sour barium-lithium negative electrode material carries out nitrogen sulfur doping carbon coating, to obtain a kind of stable structure, fine and close titanium system cathode material
Material, the particle of obtained barium titanate lithium titanate cathode material is uniform, particle diameter distribution is uniform, electronics and ionic conductivity are high, to have
Effect improves the chemical property of barium titanate lithium titanate cathode material.
The technical scheme of the invention to solve the technical problem is: a kind of lithium ion battery is co-doped with lithium position magnalium
The preparation method of miscellaneous collaboration nitrogen sulfur doping coated modified carbon barium titanate lithium titanate cathode material, comprising the following steps: firstly, taking 0.1 to rub
That barium nitrate, 0.2 molar nitric acid lithium, 0.005-0.02 mole of acetic acid magnesium, 0.01 molar acetate aluminium, 0.6 mole of nanometer titanium dioxide
Titanium (6 nm), 0.1 mol. Acetylene it is black 500 revs/min lower ball milling mixing 19 hours, after being placed in the drying of 100 DEG C of baking ovens, 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
The progress pre-burning in 4 hours of lower constant temperature was then warming up to 980 DEG C with 5 hours again to decompose salt, and holding 14 is small at such a temperature
When, naturally cooling to room temperature can be obtained lithium position magnalium codope metatitanic acid barium-lithium.Next, by resulting lithium position magnalium codope
Metatitanic acid barium-lithium is put into porcelain boat and is placed in tube-type atmosphere furnace, another porcelain boat for holding cystine is then also placed in tubular type atmosphere
Furnace is placed in the upstream end of air-flow, uses argon gas as protection gas, with 5 hours from room temperature to 680 DEG C, and at such a temperature
Heat preservation 2 hours after naturally cooling to room temperature, takes out product and pulverizes, and products therefrom is the collaboration of lithium position magnalium codope
Nitrogen sulfur doping coated modified carbon barium titanate lithium titanate cathode material.
Compared with the prior art, the advantages of the present invention are as follows: (1) particle of the barium titanate lithium titanate cathode material of this method preparation
Uniform particle diameter, stable structure, densification.Wherein the addition of nanometer acetylene black can make the homogenization of barium titanate lithium particle, lithium position
Magnalium codope can significantly promote the ionic conductivity in metatitanic acid barium-lithium structure, and nitrogen sulfur doping carbon coating can obviously change
The electronic conductivity of kind metatitanic acid barium-lithium, so that barium titanate lithium titanate cathode material has superior chemical property.(2) simultaneously,
This method carries out nitrogen sulfur doping carbon coating using the technology of cystine transpiration, and the technological operation is easy, resulting carbon-coating Bao Erjun
One, in the case where not reducing barium titanate lithium titanate cathode material reversible capacity, it can significantly improve its high rate performance, be able to satisfy height
The needs of power, extended-life lithium ion battery practical application.
Detailed description of the invention
Fig. 1 is that gained lithium position magnalium codope cooperates with nitrogen sulfur doping coated modified carbon metatitanic acid barium-lithium negative in the embodiment of the present invention
The scanning electron microscope (SEM) photograph of pole material.
Specific embodiment
The present invention will be described in further detail below with reference to the embodiments of the drawings.
Embodiment 1: take 0.1 molar nitric acid barium, 0.2 molar nitric acid lithium, 0.005 mole of acetic acid magnesium, 0.01 molar acetate aluminium,
0.6 mole of nano-titanium dioxide (6 nm), 0.1 mol. Acetylene it is black 500 revs/min lower ball milling mixing 19 hours, be placed in 100 DEG C
It is finely ground in the agate mortar after baking oven drying, then powder is sintered in Muffle furnace, first with 2 hours from room temperature
To 650 DEG C, and at such a temperature, constant temperature progress pre-burning in 4 hours is to decompose salt, then again with being warming up within 5 hours 980 DEG C, and
It is kept for 14 hours at this temperature, naturally cooling to room temperature can be obtained lithium position magnalium codope metatitanic acid barium-lithium.Next, by gained
Lithium position magnalium codope metatitanic acid barium-lithium be put into porcelain boat and be placed in tube-type atmosphere furnace, then will hold another porcelain of cystine
Boat is also placed in tube-type atmosphere furnace, is placed in the upstream end of air-flow, uses argon gas as protection gas, with 5 hours from room temperature to 680
DEG C, and 2 hours are kept the temperature at such a temperature, after naturally cooling to room temperature, takes out product and pulverize, products therefrom is lithium position
Magnalium codope cooperates with nitrogen sulfur doping coated modified carbon barium titanate lithium titanate cathode material.Using resulting product as Electrode, gold
Belong to lithium piece to be used as to electrode, fastening lithium ionic cell is assembled into the glove box full of argon gas, with the multiplying power of 0.1C in 0.5-
Charge and discharge cycles are carried out in 3.0V potential region, can obtain discharge capacity for the first time is 187mAh/g, charging capacity 163mAh/g,
Reversible capacity after recycling 100 weeks is 155mAh/g；Charge and discharge cycles are carried out in 0.5-3.0V potential region with the multiplying power of 5C,
It is 161mAh/g, charging capacity 152mAh/g that discharge capacity for the first time, which can be obtained, and reversible capacity of the circulation after 100 weeks is
142mAh/g, it is shown that excellent chemical property.
Embodiment 2: take 0.1 molar nitric acid barium, 0.2 molar nitric acid lithium, 0.02 mole of acetic acid magnesium, 0.01 molar acetate aluminium,
0.6 mole of nano-titanium dioxide (6 nm), 0.1 mol. Acetylene it is black 500 revs/min lower ball milling mixing 19 hours, be placed in 100 DEG C
It is finely ground in the agate mortar after baking oven drying, then powder is sintered in Muffle furnace, first with 2 hours from room temperature
To 650 DEG C, and at such a temperature, constant temperature progress pre-burning in 4 hours is to decompose salt, then again with being warming up within 5 hours 980 DEG C, and
It is kept for 14 hours at this temperature, naturally cooling to room temperature can be obtained lithium position magnalium codope metatitanic acid barium-lithium.Next, by gained
Lithium position magnalium codope metatitanic acid barium-lithium be put into porcelain boat and be placed in tube-type atmosphere furnace, then will hold another porcelain of cystine
Boat is also placed in tube-type atmosphere furnace, is placed in the upstream end of air-flow, uses argon gas as protection gas, with 5 hours from room temperature to 680
DEG C, and 2 hours are kept the temperature at such a temperature, after naturally cooling to room temperature, takes out product and pulverize, products therefrom is lithium position
Magnalium codope cooperates with nitrogen sulfur doping coated modified carbon barium titanate lithium titanate cathode material.Using resulting product as Electrode, gold
Belong to lithium piece to be used as to electrode, fastening lithium ionic cell is assembled into the glove box full of argon gas, with the multiplying power of 0.1C in 0.5-
Charge and discharge cycles are carried out in 3.0V potential region, can obtain discharge capacity for the first time is 199mAh/g, charging capacity 176mAh/g,
Reversible capacity after recycling 100 weeks is 169mAh/g；Charge and discharge cycles are carried out in 0.5-3.0V potential region with the multiplying power of 5C,
It is 171mAh/g, charging capacity 162mAh/g that discharge capacity for the first time, which can be obtained, and reversible capacity of the circulation after 100 weeks is
155mAh/g, it is shown that excellent chemical property.
Embodiment 3: take 0.1 molar nitric acid barium, 0.2 molar nitric acid lithium, 0.01 mole of acetic acid magnesium, 0.01 molar acetate aluminium,
0.6 mole of nano-titanium dioxide (6 nm), 0.1 mol. Acetylene it is black 500 revs/min lower ball milling mixing 19 hours, be placed in 100 DEG C
It is finely ground in the agate mortar after baking oven drying, then powder is sintered in Muffle furnace, first with 2 hours from room temperature
To 650 DEG C, and at such a temperature, constant temperature progress pre-burning in 4 hours is to decompose salt, then again with being warming up within 5 hours 980 DEG C, and
It is kept for 14 hours at this temperature, naturally cooling to room temperature can be obtained lithium position magnalium codope metatitanic acid barium-lithium.Next, by gained
Lithium position magnalium codope metatitanic acid barium-lithium be put into porcelain boat and be placed in tube-type atmosphere furnace, then will hold another porcelain of cystine
Boat is also placed in tube-type atmosphere furnace, is placed in the upstream end of air-flow, uses argon gas as protection gas, with 5 hours from room temperature to 680
DEG C, and 2 hours are kept the temperature at such a temperature, after naturally cooling to room temperature, takes out product and pulverize, products therefrom is lithium position
Magnalium codope cooperates with nitrogen sulfur doping coated modified carbon barium titanate lithium titanate cathode material.Using resulting product as Electrode, gold
Belong to lithium piece to be used as to electrode, fastening lithium ionic cell is assembled into the glove box full of argon gas, with the multiplying power of 0.1C in 0.5-
Charge and discharge cycles are carried out in 3.0V potential region, can obtain discharge capacity for the first time is 182mAh/g, charging capacity 160mAh/g,
Reversible capacity after recycling 100 weeks is 154mAh/g；Charge and discharge cycles are carried out in 0.5-3.0V potential region with the multiplying power of 5C,
It is 168mAh/g, charging capacity 159mAh/g that discharge capacity for the first time, which can be obtained, and reversible capacity of the circulation after 100 weeks is
158mAh/g, it is shown that excellent chemical property.
Claims (1)
1. a kind of preparation method of lithium position magnalium codope collaboration nitrogen sulfur doping coated modified carbon barium titanate lithium titanate cathode material, special
Sign be the following steps are included: firstly, take 0.1 molar nitric acid barium, 0.2 molar nitric acid lithium, 0.005-0.02 mole of acetic acid magnesium,
0.01 molar acetate aluminium, 0.6 mole of nano-titanium dioxide, 0.1 mol. Acetylene it is black 500 revs/min lower ball milling mixing 19 hours,
It is finely ground in the agate mortar after being placed in the drying of 100 DEG C of baking ovens, then powder is sintered in Muffle furnace, first with 2 hours from
To 650 DEG C, and at such a temperature, constant temperature progress pre-burning in 4 hours was then warming up to 5 hours room temperature again with decomposing salt
980 DEG C, and kept for 14 hours at such a temperature, naturally cooling to room temperature can be obtained lithium position magnalium codope metatitanic acid barium-lithium；It connects
Get off, resulting lithium position magnalium codope metatitanic acid barium-lithium is put into porcelain boat and is placed in tube-type atmosphere furnace, Guang ammonia then will be held
Acid another porcelain boat be also placed in tube-type atmosphere furnace, be placed in the upstream end of air-flow, use argon gas as protect gas, with 5 hours from
Room temperature keeps the temperature 2 hours to 680 DEG C, and at such a temperature, after naturally cooling to room temperature, takes out product and pulverizes, institute
Obtaining product is lithium position magnalium codope collaboration nitrogen sulfur doping coated modified carbon barium titanate lithium titanate cathode material.
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| 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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| 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 |
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| 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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