CN105428612B - A kind of nanometer MoO2‑MoSe2@SFC lithium ion battery negative materials and preparation method thereof - Google Patents
A kind of nanometer MoO2‑MoSe2@SFC lithium ion battery negative materials and preparation method thereof Download PDFInfo
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- CN105428612B CN105428612B CN201510749686.9A CN201510749686A CN105428612B CN 105428612 B CN105428612 B CN 105428612B CN 201510749686 A CN201510749686 A CN 201510749686A CN 105428612 B CN105428612 B CN 105428612B
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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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- H01M4/36—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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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Abstract
The invention discloses a kind of nanometer MoO2‑MoSe2@SFC lithium ion battery negative materials and preparation method thereof.Nanometer MoO2‑MoSe2@SFC composites are used as matrix material, MoO using the sisal fiber charcoal (SFC) with multistage cavernous structure2And MoSe2It is dispersed in its surface and hole.Using Ammonium Molybdate Tetrahydrate, two Ammonium paramolybdate tetrahydrates or molybdenum dioxide as molybdenum source, using selenium dioxide, sodium selenite or selenium powder as selenium source, matrix material is used as using the sisal fiber charcoal after charing, ball milling, sieving, reducing agent and dispersant are done with hydrazine hydrate and polyethylene glycol 400 respectively simultaneously, hydro-thermal reaction is carried out using autoclave, the different dispersion material of particle diameter can be obtained by changing different reaction conditions.The nanometer MoO that the present invention obtains2‑MoSe2The compound powders of@SFC reversible capacity when as lithium ion battery negative material is higher, cycle performance is relatively stable, charge-discharge magnification better performances, has preferable application prospect.
Description
Technical field
The invention belongs to new material and electrochemical field, and in particular to it is a kind of can charging-discharging lithium ion battery negative material
Preparation method.
Background technology
At present, under the pressure of the pressure of environment, energy storage device lithium ion battery just gradually captures consumption market, and constantly expands it
Application field, in addition to some intelligence and portable electric appts, the application to some large scale equipments such as electric car, electric automobiles
Also bring into schedule, at the same time, the storage lithium performance to lithium ion battery it is also proposed higher requirement.Negative material as lithium from
The important part of sub- battery, researcher are more likely to the exploration to carbon based negative electrodes material.Part researcher is for ring
Border and its consideration of natural advantageous physical chemical property, to the important component obtained from plant waste, such as rice husk, cherry
Core, dento liva, mangrove, velveteen, peanut shell, human hair, are handled it, and are used as negative electrode of lithium ion battery to it
Material is studied.
There is Guangxi special product sisal fiber abundance easily to obtain, natural porous profit activates, green energy resource cost is low, chemical
The features such as stable performance, the raw material of lithium ion battery negative material can be made.But in actual applications, sisal fiber charcoal is still
In the presence of the demand for development that coulombic efficiency first is low, reversible capacity can not meet the epoch.It is considered as one that processing is modified to it
The feasible approach of kind.The molybdenum dioxide of molybdenum dioxide, particularly nano-scale, it is a kind of as transition metal oxide, have low
Resistivity, higher electro-chemical activity and higher stability, it is considered to be a kind of promising negative electrode of lithium ion battery
Material.For selenizing molybdenum, current research has focused largely on the selenizing molybdenum of synthesis two-dimensional layer, the selenium on three-dimensional structure
Change molybdenum to be but rarely reported.
The present invention is compound using two-phase molybdenum base compound and the progress of sisal fiber charcoal, on the one hand utilizes the unique thing of dispersed phase
Physicochemical property, on the other hand make up dispersed phase using the loose structure of matrix and be used alone as lacking for lithium ion battery negative material
The problem of falling into, in the hope of good effect can be reached.
The content of the invention
It is an object of the invention to provide a kind of reversible capacity, charge-discharge magnification better performances, cyclical stability are preferable
MoO2-MoSe2@SFC lithium ion battery negative materials and preparation method.
The nanometer MoO that the present invention obtains2-MoSe2@SFC lithium ion battery negative materials are on composition, structure and pattern
Feature is：The nanometer MoO2-MoSe2@SFC lithium ion battery negative materials include MoO2、MoSe2With sisal fiber charcoal.Institute
State MoO2（Hexagonal crystal system, JCPDS, 77-1715）And MoSe2（Monoclinic system, JCPDS, 32-0671）In nanometer MoO2-
MoSe2It is in the nutty structure and particle diameter of two kinds of forms, respectively particle diameter about 10nm in@SFC lithium ion battery negative materials
About 15nm, the vermicular texture up to 150nm or so, and it is evenly dispersed in the sisal fiber charcoal with multistage pore structure
In surface and hole.
Nanometer MoO2-MoSe2The preparation method step of@SFC lithium ion battery negative materials is as follows：
（1）The acquisition of sisal fiber charcoal：Pretreated sisal fiber is carbonized in tube-type atmosphere furnace, ball milling,
Sieving, 600-1000 DEG C of carbonization temperature, soaking time is 0.5-2 hours, and heating rate is 1-10 DEG C/min, ball milling speed
400r/min, Ball-milling Time are 6-12 hours, are sieved as 200 mesh sieves.
（2）Configure solution：0.39-1.56g molybdenum source and 0.035-0.14g selenium sources are added to 70mL deionized waters
In, during colourless transparent solution to be formed, add 0.5-0.64g steps（1）The sisal fiber charcoal of gained, when stirring 15-20 minutes
Between after, add the 0.5-1mL pure polyethylene glycol 400 of analysis, continue to stir 15-20 minutes, add 2-10mL mass percents
Concentration is 80% hydrazine hydrate, and continued stirring overnight, this suspension is designated as A suspension.
（3）Hydro-thermal reaction：A suspension is transferred in stainless steel cauldron and reacts 12-48 hours at 120-180 DEG C, instead
Suction filtration separation is carried out after should terminating, and is rinsed with deionized water and absolute ethyl alcohol, after be placed in vacuum drying chamber 60 DEG C it is dry
Dry 12-24 hours, after obtain precursor product B.
（4）Heat treatment：By precursor product B in N2First with 1-3 DEG C/min heating rates in tube furnace in protection atmosphere
Rise to 200 DEG C, be incubated 0.5-1 hours, after with 5-10 DEG C/min be warming up to 800 DEG C, be incubated 0.5-1 hours, heating schedule terminates
Room temperature is cooled to stove to take out, obtain a nanometer MoO afterwards2-MoSe2@SFC lithium ion battery negative material powders.
（5）Make pole piece：By step（4）The negative electrode material powder of gained and acetylene black and Kynoar（PVDF）By matter
Amount is than being 8:1:1 or 90:2:8 ratio mixing, addition rank is analytically pure solvent N-methyl pyrilidone（NMP）, stir
Mix uniformly to pasty state, be uniformly applied on the copper foil that thickness is 5-20 μm, prior to 40-60 DEG C under the conditions of dry, then at 100-
It is dried in vacuo 12 hours under the conditions of 120 DEG C, circular pole piece of the punching into a diameter of 16mm.
（6）Battery assembles：With lithium piece to electrode, step（5）Obtained circular pole piece is working electrode, microporous polypropylene membrane
For barrier film, 1mol/L LiPF6/EC (ethylene carbonate)+DMC (dimethyl carbonate)+DEC (carbonic acid diethyls
Ester) it is used as electrolyte（LiPF6 is solute in electrolyte, and solvent EC+DMC+DEC volume ratio is 1:1:1）, full of high-purity
CR2025 type button simulated batteries are assembled into the glove box of argon gas, and are sealed.
（7）Test：By step（6）The battery assembled carries out electro-chemical test after placing 12-24 hours.Test lithium from
The loop test of sub- battery is cell tester at room temperature（BTS-10mA, Shenzhen more Science and Technology Ltd.s of new Weir）Upper completion
, voltage range is 0.01-3.0 V.
The molybdenum source is one kind in Ammonium Molybdate Tetrahydrate, two Ammonium paramolybdate tetrahydrates and molybdenum dioxide.
The selenium source is one kind in selenium dioxide, sodium selenite and selenium powder.
The lithium ion battery negative material that the present invention obtains has excellent electrochemical properties, shows：In current density
In the case of 50mA/g, first discharge specific capacity is the mAh/g of highest 724, and initial charge specific capacity can reach 445
MAh/g, first coulombic efficiency be up to 61%, by 30 circulation after, specific discharge capacity reaches as high as 494mAh/g.Compared with
Single sisal fiber charcoal specific capacity is higher by 305mA/g, and it is compound to illustrate that two-phase molybdenum base compound is carried out with sisal fiber charcoal, improves
The specific capacity of composite.Current density be 500 mA/g in the case of, by 30 circulation after specific discharge capacity highest still
For 340 mAh/g.Illustrate its preferable cyclical stability and high rate performance.
Brief description of the drawings
Fig. 1 is MoO prepared by the embodiment of the present invention2-MoSe2The XRD of@SFC lithium ion battery negative materials.
Fig. 2 is nanometer MoO prepared by the embodiment of the present invention2-MoSe2@SFC compounds and single SFC respectively as lithium from
The cycle performance curve map that sub- cell negative electrode material measures under conditions of current density is 50mA/g.
Fig. 3 is nanometer MoO prepared by the embodiment of the present invention2-MoSe2@SFC compounds and single SFC are respectively as lithium ion
The cycle performance curve map that cell negative electrode material measures under conditions of current density is 500mA/g.
Embodiment
Embodiment：
（1）The acquisition of sisal fiber charcoal：Pretreated sisal fiber in tube-type atmosphere furnace carbonize and ball milling,
Sieving, heating rate are 3 DEG C/min, and 900 DEG C of carbonization temperature, soaking time is 0.5 hour, ball milling speed 400r/min, ball
Consume time as 12 hours, it is 0.074mm to cross mesh size（200 mesh sieves）.
（2）Configure solution：By 1.56g Ammonium Molybdate Tetrahydrate and 0.14g selenium dioxide (selenium：Molybdenum=1:1) it is added to
In 70mL deionized waters, during colourless transparent solution to be formed, 0.64g steps are added（1）Resulting sisal fiber charcoal, stirring
After 20 minutes, the 1mL pure polyethylene glycol 400 of analysis is added, continues stirring 20 minutes, adding 5mL mass percent concentrations is
80% hydrazine hydrate, continued stirring overnight.This suspension is designated as A suspension.
（3）Hydro-thermal reaction：A suspension is transferred in the stainless steel cauldron that inner bag volume is 100mL, at 160 DEG C
Reaction 24 hours, reaction carry out suction filtration separation after terminating, and are rinsed with deionized water and absolute ethyl alcohol, after be placed in vacuum and do
60 DEG C of dryings 12 hours, obtain precursor product B in dry case.
（4）Heat treatment：By precursor product B in N2First with 3 DEG C/min heating rate liters in tube furnace under protection atmosphere
To 200 DEG C, be incubated 0.5 hour, after with 5 DEG C/min be warming up to 800 DEG C, be incubated 0.5 hour, heating schedule terminate after with stove
Room temperature taking-up is cooled to, obtains a nanometer MoO2-MoSe2@SFC lithium ion battery negative material powders.
（5）Make pole piece：By step（4）The negative electrode material powder of middle preparation and acetylene black and Kynoar（PVDF）Press
Mass ratio is 8:1:1 ratio mixing, addition rank is analytically pure solvent N-methyl pyrilidone（NMP）, it is evenly stirred until
Pasty state, being uniformly applied to thickness is on 10 μm of copper foil, prior to 60 DEG C under the conditions of dry, vacuum is done under the conditions of 110 DEG C
Dry 12 hours, circular pole piece of the punching into a diameter of 16mm.
（6）Battery assembles：With lithium piece to electrode, step（5）Obtained circular pole piece is working electrode, microporous polypropylene membrane
For barrier film, 1mol/L LiPF6/EC (ethylene carbonate)+DMC (dimethyl carbonate)+DEC (carbonic acid diethyls
Ester) it is used as electrolyte（LiPF6 is solute in electrolyte, and solvent EC+DMC+DEC volume ratio is 1:1:1）, full of high-purity
CR2025 type button simulated batteries are assembled into the glove box of argon gas, and are sealed.
（7）Test：By step（6）The battery assembled carries out electro-chemical test after placing 12 hours.Test lithium ion
The loop test of battery is cell tester at room temperature（BTS-10mA, Shenzhen more Science and Technology Ltd.s of new Weir）Upper completion
, voltage range is 0.01-3.0 V.
Test result is shown：In the case where current density is 50mA/g, first discharge specific capacity is 724 mAh/g, first
Secondary charge specific capacity is 445 mAh/g, and coulombic efficiency reaches 61% first, and after 30 circulations, specific discharge capacity is reachable
494mAh/g.Specific capacity compared with single sisal fiber charcoal is higher by 305mAh/g, illustrates two-phase molybdenum base compound and sisal fiber
After charcoal progress is compound, the specific capacity of sisal fiber charcoal is improved.In the case where current density is 500 mA/g, followed by 30
Specific discharge capacity still keeps 340 mAh/g after ring, illustrates that composite has preferable cyclical stability and high rate performance.
Claims (1)
- A kind of 1. MoO2-MoSe2The preparation method of@SFC lithium ion battery negative materials, it is characterised in that concretely comprise the following steps：（1）Pretreated sisal fiber is carbonized in tube-type atmosphere furnace, ball milling, sieving, carbonization temperature 600-1000 DEG C, soaking time is 0.5-2 hours, and heating rate is 1-10 DEG C/min, the 400r/min of ball milling speed, Ball-milling Time 6-12 Hour, sieve as 200 mesh sieves, obtain sisal fiber charcoal；（2）0.39-1.56g molybdenum source and 0.035-0.14g selenium sources are added in 70mL deionized waters, it is to be formed colourless During bright solution, 0.5-0.64g steps are added（1）The sisal fiber charcoal of gained, after stirring 15-20 minutes, add 0.5- The 1mL pure polyethylene glycol 400 of analysis, continue to stir 15-20 minutes, add the hydration that 2-10mL mass percent concentrations are 80% Hydrazine, continued stirring overnight, gained suspension are designated as A suspension；（3）A suspension is transferred in stainless steel cauldron and reacted 12-48 hours at 120-180 DEG C, reaction is taken out after terminating Filter separation, and is rinsed with deionized water and absolute ethyl alcohol, after be placed in 60 DEG C of dry 12-24 hours in vacuum drying chamber, after Obtain precursor product B；（4）By precursor product B in N2200 DEG C first are risen to 1-3 DEG C/min heating rates in tube furnace in protection atmosphere, is protected Warm 0.5-1 hours, after with 5-10 DEG C/min be warming up to 800 DEG C, be incubated 0.5-1 hours, heating schedule cools down after terminating with stove Taken out to room temperature, obtain a nanometer MoO2-MoSe2@SFC lithium ion battery negative material powders；The molybdenum source is one kind in Ammonium Molybdate Tetrahydrate, two Ammonium paramolybdate tetrahydrates and molybdenum dioxide；The selenium source is one kind in selenium dioxide, sodium selenite and selenium powder.
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| CN106450314B (en) * | 2016-11-19 | 2018-12-21 | 桂林理工大学 | One kind " spring like " sisal fiber charcoal and preparation method thereof |
| CN109192939A (en) * | 2018-08-06 | 2019-01-11 | 桂林理工大学 | Flower-shaped molybdenum disulfide coats the preparation and its application of spherical sisal carbon electrode material |
| CN109830657B (en) * | 2019-01-14 | 2020-11-03 | 陕西科技大学 | MoS2/MoO2Preparation method of three-dimensional carbon lithium ion battery cathode material |
| CN111785928B (en) * | 2019-04-04 | 2021-11-16 | 中南大学 | Solid electrolyte interface material, negative electrode precursor material and negative electrode of lithium metal battery, and preparation and application thereof |
| CN111193015A (en) * | 2020-01-09 | 2020-05-22 | 桂林理工大学 | MoSe2-MoO2Preparation method of @ sisal fiber activated carbon lithium ion battery negative electrode material |
| CN114291797B (en) * | 2021-12-31 | 2023-05-26 | 杭州电子科技大学 | Ultrathin three-dimensional MoSe 2 Nanosphere and preparation and application thereof |
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| CN102580673B (en) * | 2012-02-18 | 2013-07-24 | 桂林理工大学 | Method for hydrothermally activating sisal hemp based carbon fibers |
| CN104078656B (en) * | 2014-07-09 | 2016-04-06 | 桂林理工大学 | The preparation method of nano ferriferrous oxide/sisal carbon lithium ion battery negative material |
| CN104157857A (en) * | 2014-08-04 | 2014-11-19 | 桂林理工大学 | Preparation method for nano-Fe2O3/SFC lithium ion battery composite anode material |
| CN104852016B (en) * | 2015-05-17 | 2017-05-31 | 桂林理工大学 | A kind of submicron order copper sulfide/sisal fiber charcoal lithium ion battery negative material and preparation method thereof |
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Application publication date: 20160323 Assignee: Guangxi aid Energy Technology Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2022450000464 Denomination of invention: A nano MoO2- MoSe2@ SFC lithium ion battery cathode material and its preparation method Granted publication date: 20171212 License type: Common License Record date: 20221228 |
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Application publication date: 20160323 Assignee: GUANGXI YANGSHENG NEW ENERGY CO.,LTD. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2022450000636 Denomination of invention: A nano MoO2- MoSe2@ SFC lithium ion battery cathode material and its preparation method Granted publication date: 20171212 License type: Common License Record date: 20221230 |
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