CN105428612A - Nano MoO2-MoSe2@SFC lithium ion battery negative electrode material and preparation method therefor - Google Patents
Nano MoO2-MoSe2@SFC lithium ion battery negative electrode material and preparation method therefor Download PDFInfo
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- CN105428612A CN105428612A CN201510749686.9A CN201510749686A CN105428612A CN 105428612 A CN105428612 A CN 105428612A CN 201510749686 A CN201510749686 A CN 201510749686A CN 105428612 A CN105428612 A CN 105428612A
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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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- H01M4/362—Composites
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- 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
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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
- H01M4/581—Chalcogenides or intercalation compounds thereof
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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
- H01M4/58—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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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a nano MoO2-MoSe2@SFC lithium ion battery negative electrode material and a preparation method therefor. A nano MoO2-MoSe2@SFC composite material takes sisal fiber carbon (SFC) with a hierarchical pore-shaped structure as a substrate material, and MoO2 and MoSe2 are uniformly dispersed in the surface and pores of the SFC. Ammonium molybdate tetrahydrate, ammonium molybdate dehydrate or molybdenum dioxide is taken as a molybdenum source; selenium dioxide, sodium selenite or selenium powder is taken as a selenium source; carbonized, ball-milled and sieved SFC is taken as a substrate material; hydrazine hydrate and polyethylene glycol 400 are used as a reductant and a dispersant respectively; a hydrothermal reaction is performed by utilizing a high-pressure reaction kettle; and dispersoid materials with different particle sizes can be obtained by changing different reaction conditions. The obtained nano MoO2-MoSe2@SFC composite powder is relatively high in reversible capacity, relatively stable in cyclic performance and relatively high in charging/discharging rate performance when being used as the lithium ion battery negative electrode material, so that the nano MoO2-MoSe2@SFC composite powder has relatively good application prospects.
Description
Technical field
The invention belongs to new material and electrochemical field, be specifically related to a kind of can the preparation method of charging-discharging lithium ion battery negative material.
Background technology
At present, under the pressure of the pressure of environment, energy storage device lithium ion battery captures consumption market just gradually, and constantly expand its application, except some intelligence and portable electric appts, the application of some main equipments such as electric motor car, electric automobile is also brought into schedule, meanwhile, higher requirement be it is also proposed to the storage lithium performance of lithium ion battery.Negative material is as the important part of lithium ion battery, and researcher is more prone to the exploration to carbon based negative electrodes material.Part researcher is for the consideration to environment and natural advantageous physical chemical property thereof, to the important component part obtained from plant waste, as rice husk, cherry stone, dento liva, mangrove, velveteen, peanut shell, human hair, it is processed, and it is studied as lithium ion battery negative material.
Guangxi special product sisal fiber has the features such as abundance easily obtains, natural porous profit activates, green energy resource cost is low, stable chemical performance, can make the raw material of lithium ion battery negative material.But in actual applications, still there is the demand for development that coulombic efficiency is first low, reversible capacity cannot meet the epoch in sisal fiber charcoal.Modification is carried out to it and is considered to a kind of feasible approach.The molybdenum dioxide of molybdenum dioxide, particularly nano-scale, a kind of as transition metal oxide, there is low resistivity, higher electro-chemical activity and higher stability, be considered to a kind of promising lithium ion battery negative material.For selenizing molybdenum, current research concentrates on the selenizing molybdenum of synthesis two-dimensional layer mostly, and the selenizing molybdenum about three-dimensional structure but rarely has report.
The present invention utilizes two-phase molybdenum based compound and sisal fiber charcoal to carry out compound, utilize the physicochemical properties of decentralized photo uniqueness on the one hand, on the other hand utilize the loose structure of matrix to make up defect problem that decentralized photo is used alone as lithium ion battery negative material, in the hope of reaching good effect.
Summary of the invention
The object of this invention is to provide a kind of reversible capacity, charge-discharge magnification better performances, the good MoO of cyclical stability
2-MoSe
2sFC lithium ion battery negative material and preparation method.
The nanometer MoO that the present invention obtains
2-MoSe
2the feature of SFC lithium ion battery negative material on composition, structure and pattern is: described nanometer MoO
2-MoSe
2sFC lithium ion battery negative material comprises MoO
2, MoSe
2with sisal fiber charcoal.Described MoO
2(hexagonal crystal system, JCPDS, 77-1715) and MoSe
2(monoclinic system, JCPDS, 32-0671) is at nanometer MoO
2-MoSe
2in two kinds of forms in SFC lithium ion battery negative material, be respectively particle diameter and be about the nutty structure of 10nm and particle diameter is about 15nm, reaches the vermicular texture of about 150nm, and in the surface being evenly dispersed in the sisal fiber charcoal with multi-stage porous gap structure and hole.
Nanometer MoO
2-MoSe
2preparation method's step of SFC lithium ion battery negative material is as follows:
(1) acquisition of sisal fiber charcoal: pretreated sisal fiber is carried out carbonizing at tube-type atmosphere furnace, ball milling, to sieve, carbonization temperature 600-1000 DEG C, temperature retention time is 0.5-2 hour, heating rate is 1-10 DEG C/min, the 400r/min of ball milling speed, Ball-milling Time is 6-12 hour, and sieving is 200 mesh sieves.
(2) solution is configured: join in 70mL deionized water by the molybdenum source of 0.39-1.56g and 0.035-0.14g selenium source, during colourless transparent solution to be formed, add the sisal fiber charcoal of 0.5-0.64g step (1) gained, after stirring 15-20 minutes, add the pure PEG400 of analysis of 0.5-1mL, continue to stir 15-20 minute, add the hydrazine hydrate that 2-10mL mass percent concentration is 80%, continued stirring overnight, this suspension is designated as A suspension.
(3) hydro-thermal reaction: A suspension is transferred in stainless steel cauldron at 120-180 DEG C of reaction 12-48 hour, suction filtration separation is carried out after reaction terminates, and rinse with deionized water and absolute ethyl alcohol, be placed on 60 DEG C of dry 12-24 hour in vacuum drying chamber, after obtain precursor product B.
(4) heat treatment: by precursor product B at N
2in tube furnace, first rise to 200 DEG C with 1-3 DEG C/min heating rate in protection atmosphere, insulation 0.5-1 hour, after be warming up to 800 DEG C with 5-10 DEG C/min, insulation 0.5-1 hour, be cooled to room temperature with stove after heating schedule stops and take out, obtain nanometer MoO
2-MoSe
2sFC lithium ion battery negative material powder.
(5) pole piece is made: the ratio being 8:1:1 or 90:2:8 in mass ratio by the negative electrode material powder of step (4) gained and acetylene black and Kynoar (PVDF) mixes, adding rank is analytically pure solvent N-methyl pyrilidone (NMP), stir to pasty state, uniform application is on the Copper Foil of 5-20 μm at thickness, prior to drying under 40-60 DEG C of condition, vacuumize 12 hours under 100-120 DEG C of condition again, punching becomes diameter to be the circular pole piece of 16mm.
(6) battery assembling: with lithium sheet to electrode, the circular pole piece that step (5) obtains is work electrode, microporous polypropylene membrane is barrier film, as electrolyte, (in electrolyte, LiPF6 is solute to LiPF6/EC (ethylene carbonate)+DMC (the dimethyl carbonate)+DEC (diethyl carbonate) of 1mol/L, the volume ratio of solvent EC+DMC+DEC is 1:1:1), be full of high-purity argon gas glove box in be assembled into CR2025 type button simulated battery, and to seal.
(7) test: battery step (6) assembled is placed after 12-24 hour and carried out electro-chemical test.The loop test of experiment lithium ion battery at room temperature cell tester (BTS-10mA, Shenzhen many Science and Technology Ltd.s of new Weir) completes, and voltage range is 0.01-3.0V.
Described molybdenum source is the one in Ammonium Molybdate Tetrahydrate, two Ammonium paramolybdate tetrahydrates and molybdenum dioxide.
Described selenium source is the one in selenium dioxide, sodium selenite and selenium powder.
The lithium ion battery negative material that the present invention obtains has excellent electrochemical properties, show: when current density is 50mA/g, first discharge specific capacity is the highest 724mAh/g, initial charge specific capacity can reach 445mAh/g, coulombic efficiency is up to 61% first, after 30 circulations, specific discharge capacity reaches as high as 494mAh/g.Exceed 305mA/g compared with single sisal fiber charcoal specific capacity, illustrate that two-phase molybdenum based compound and sisal fiber charcoal carry out compound, improve the specific capacity of composite material.When current density is 500mA/g, after 30 circulations, specific discharge capacity is the highest is still 340mAh/g.Describe its good cyclical stability and high rate performance.
Accompanying drawing explanation
Fig. 1 is MoO prepared by the embodiment of the present invention
2-MoSe
2the XRD figure of SFC lithium ion battery negative material.
Fig. 2 is nanometer MoO prepared by the embodiment of the present invention
2-MoSe
2the cycle performance curve chart that SFC compound and single SFC record under current density is the condition of 50mA/g respectively as lithium ion battery negative material.
Fig. 3 is nanometer MoO prepared by the embodiment of the present invention
2-MoSe
2the cycle performance curve chart that SFC compound and single SFC record under current density is the condition of 500mA/g respectively as lithium ion battery negative material.
Embodiment
embodiment:
(1) acquisition of sisal fiber charcoal: pretreated sisal fiber carried out in tube-type atmosphere furnace charing ball milling, sieve, heating rate is 3 DEG C/min, carbonization temperature 900 DEG C, temperature retention time is 0.5 hour, ball milling speed is 400r/min, Ball-milling Time is 12 hours, and crossing mesh size is 0.074mm(200 mesh sieve).
(2) solution is configured: join in 70mL deionized water by the Ammonium Molybdate Tetrahydrate of 1.56g and 0.14g selenium dioxide (selenium: molybdenum=1:1), during colourless transparent solution to be formed, add the sisal fiber charcoal that 0.64g step (1) obtains, stir after 20 minutes, add the pure PEG400 of analysis of 1mL, continue stirring 20 minutes, add the hydrazine hydrate that 5mL mass percent concentration is 80%, continued stirring overnight.This suspension is designated as A suspension.
(3) hydro-thermal reaction: A suspension being transferred to inner bag volume is in the stainless steel cauldron of 100mL, react 24 hours at 160 DEG C, suction filtration separation is carried out after reaction terminates, and rinse with deionized water and absolute ethyl alcohol, to be placed in vacuum drying chamber 60 DEG C of dryings 12 hours, to obtain precursor product B.
(4) heat treatment: by precursor product B at N
2in tube furnace, first rise to 200 DEG C with 3 DEG C/min heating rate under protection atmosphere, be incubated 0.5 hour, after be warming up to 800 DEG C with 5 DEG C/min, be incubated 0.5 hour, is cooled to room temperature taking-up with stove after heating schedule termination, obtains nanometer MoO
2-MoSe
2sFC lithium ion battery negative material powder.
(5) pole piece is made: the ratio being 8:1:1 in mass ratio by the negative electrode material powder of preparation in step (4) and acetylene black and Kynoar (PVDF) mixes, adding rank is analytically pure solvent N-methyl pyrilidone (NMP), stir to pasty state, uniform application is on the Copper Foil of 10 μm at thickness, prior to drying under 60 DEG C of conditions, vacuumize 12 hours under 110 DEG C of conditions again, punching becomes diameter to be the circular pole piece of 16mm.
(6) battery assembling: with lithium sheet to electrode, the circular pole piece that step (5) obtains is work electrode, microporous polypropylene membrane is barrier film, as electrolyte, (in electrolyte, LiPF6 is solute to LiPF6/EC (ethylene carbonate)+DMC (the dimethyl carbonate)+DEC (diethyl carbonate) of 1mol/L, the volume ratio of solvent EC+DMC+DEC is 1:1:1), be full of high-purity argon gas glove box in be assembled into CR2025 type button simulated battery, and to seal.
(7) test: after the battery that step (6) assembles is placed 12 hours, carry out electro-chemical test.The loop test of experiment lithium ion battery at room temperature cell tester (BTS-10mA, Shenzhen many Science and Technology Ltd.s of new Weir) completes, and voltage range is 0.01-3.0V.
Test result shows: when current density is 50mA/g, first discharge specific capacity is 724mAh/g, and initial charge specific capacity is 445mAh/g, and coulombic efficiency reaches 61% first, and after 30 circulations, specific discharge capacity can reach 494mAh/g.Specific capacity compared with single sisal fiber charcoal exceeds 305mAh/g, after illustrating that two-phase molybdenum based compound and sisal fiber charcoal carry out compound, improves the specific capacity of sisal fiber charcoal.When current density is 500mA/g, after 30 circulations, specific discharge capacity still keeps 340mAh/g, describes composite material and has good cyclical stability and high rate performance.
Claims (1)
1. a MoO
2-MoSe
2the preparation method of SFC lithium ion battery negative material, is characterized in that concrete steps are:
(1) pretreated sisal fiber is carried out carbonizing at tube-type atmosphere furnace, ball milling, to sieve, carbonization temperature 600-1000 DEG C, temperature retention time is 0.5-2 hour, heating rate is 1-10 DEG C/min, the 400r/min of ball milling speed, Ball-milling Time is 6-12 hour, and sieving is 200 mesh sieves, obtains sisal fiber charcoal;
(2) the molybdenum source of 0.39-1.56g and 0.035-0.14g selenium source are joined in 70mL deionized water, during colourless transparent solution to be formed, add the sisal fiber charcoal of 0.5-0.64g step (1) gained, after stirring 15-20 minutes, add the pure PEG400 of analysis of 0.5-1mL, continue to stir 15-20 minute, add the hydrazine hydrate that 2-10mL mass percent concentration is 80%, continued stirring overnight, this suspension is designated as A suspension;
(3) A suspension is transferred in stainless steel cauldron at 120-180 DEG C of reaction 12-48 hour, suction filtration separation is carried out after reaction terminates, and rinse with deionized water and absolute ethyl alcohol, be placed on 60 DEG C of dry 12-24 hour in vacuum drying chamber, after obtain precursor product B;
(4) by precursor product B at N
2in tube furnace, first rise to 200 DEG C with 1-3 DEG C/min heating rate in protection atmosphere, insulation 0.5-1 hour, after be warming up to 800 DEG C with 5-10 DEG C/min, insulation 0.5-1 hour, be cooled to room temperature with stove after heating schedule stops and take out, obtain nanometer MoO
2-MoSe
2sFC lithium ion battery negative material powder;
Described molybdenum source is the one in Ammonium Molybdate Tetrahydrate, two Ammonium paramolybdate tetrahydrates and molybdenum dioxide;
Described selenium source is the one in selenium dioxide, sodium selenite and selenium powder.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106450314A (en) * | 2016-11-19 | 2017-02-22 | 桂林理工大学 | Spring-shaped SFC (sisal fiber carbon) 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 |
| CN109830657A (en) * | 2019-01-14 | 2019-05-31 | 陕西科技大学 | A kind of MoS2/MoO2The preparation method of/three-dimensional carbon lithium ion battery negative material |
| 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 |
| CN111785928A (en) * | 2019-04-04 | 2020-10-16 | 中南大学 | Solid electrolyte interface material, negative electrode precursor material and negative electrode of lithium metal battery, and preparation and application thereof |
| CN114291797A (en) * | 2021-12-31 | 2022-04-08 | 杭州电子科技大学 | Ultrathin three-dimensional MoSe2Nanosphere and preparation and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106450314A (en) * | 2016-11-19 | 2017-02-22 | 桂林理工大学 | Spring-shaped SFC (sisal fiber carbon) and preparation method thereof |
| 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 |
| CN109830657A (en) * | 2019-01-14 | 2019-05-31 | 陕西科技大学 | A kind of MoS2/MoO2The preparation method of/three-dimensional carbon lithium ion battery negative material |
| CN111785928A (en) * | 2019-04-04 | 2020-10-16 | 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 |
| CN114291797A (en) * | 2021-12-31 | 2022-04-08 | 杭州电子科技大学 | Ultrathin three-dimensional MoSe2Nanosphere and preparation and application 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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