CN110407251A - A kind of V3S4The preparation method and application of material - Google Patents
A kind of V3S4The preparation method and application of material Download PDFInfo
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Abstract
The invention discloses a kind of V3S4The preparation method and application of material, preparation method are to first pass through solvent heat one-step synthesis method V3S4Presoma, the high-temperature heat treatment after freeze-drying or vacuum drying obtain flower-shaped or granular V3S4.Wherein, flower-shaped V3S4It is to be formed by nano flake self assembly, the size of flower is about 1-2 μm；The V of fine granularity3S4Size in 100 ~ 200 nm；The V of large grained3S4Size at 1 μm or so.The V of this method preparation3S4Material can be used in lithium ion battery.The present invention has the advantages that the method that (1) provides through the invention, prepares the V of morphology controllable for the first time3S4Material；(2) V that the present invention prepares3S4As negative electrode of lithium ion battery electrode material charging and discharging capacity with higher, good high rate performance；(3) preparation method provided by the present invention is simple for process, mild condition, can be used for being mass produced.
Description
Technical field
The present invention relates to ion battery cathode material technical fields, and in particular to a kind of lithium ion battery negative material V3S4
Preparation method and applications.
Background technique
Transient metal sulfide (such as Sb2S3, MoS2, Co9S8Deng) due to its unique physics, chemistry, optics and magnetic property
Etc. properties, be widely studied in recent years and be applied to the multiple fields such as energy storage, photoelectrocatalysis and sensing.
As vanadium is typically represented in transition metal family, sulfide includes VS2、VS4、V3S4Deng mainly as electricity
Pole material is applied in lithium/sodium-ion battery.Compared with its oxide, the sulfide of vanadium theoretical specific capacity with higher；It leads
Electrically opposite enhancing；And the bond strength ratio V-O's of V-S is weak, this advantageously reduces electrode polarization, improves energy efficiency, reduces
Fuel factor, therefore it is now subjected to very big concern.However, the sulfide of vanadium is faced in charge and discharge process in battery system
Volume expansion, it is unstable the problems such as.In order to improve its performance in the battery, (such as sheet, flower of a variety of nanostructures
Shape etc.) vanadic sulfide and its composite material (such as VS2/rGO、VS4/ CNT etc.) it is researched and developed in succession, especially VS2, preparation process and
Using comparative maturity.
However to V3S4Correlative study and report and few, prepared V at present3S4It requires first to synthesize barium oxide,
Again with H2S gas or sulphur source high-temperature process obtain, and yield is also to need to be further increased.Qixing Liu et al. people is 2017
October in year has delivered V3S4 nanoparticles anchored on three-dimensional porous graphene
Gel for superior lithium storage, preparation method are first hydrothermal synthesis VOx- rGO three dimensional gel, then
By high temperature in H2Three-dimensional porous V is obtained in S/Ar mixed gas3S4/ rGO composite material, as negative electrode of lithium ion battery material
Material, in 0.2C, specific discharge capacity is 873 mAh/g, and in 10C, specific discharge capacity is 338.7 mAh/g, and the gas under high temperature
Atmosphere is H2S/Ar, than relatively hazardous.Patent No. 201610285884.9 reports a kind of " nano bar-shape V3S4Preparation method and
Using ".Preparation method is equally first hydrothermal synthesis VO2, then with the sulphur source of certain mass acquisition is calcined in high temperature process furnances
The V of nano bar-shape3S4.This method process is more complex, and the sulphur steam that sulphur source generates at high temperature easily blocks pipeline opening, forms peace
Full hidden danger.Therefore, a kind of V is studied3S4The preparation method that controllability is strong, purity is high, performance are good, easy to operate, safe be very
Significant.
Summary of the invention
It is an object of the invention in view of the above-mentioned problems, proposing a kind of by a step solvent structure V3S4Presoma,
High-temperature heat treatment obtains V under an inert gas later3S4The preparation method of material, and be applied in lithium ion battery.
Realizing the specific technical solution of the object of the invention is:
A kind of V3S4The preparation method of material, this method comprising the following specific steps
A) 1-Methyl-2-Pyrrolidone solution is poured into three neck round bottom flask；
B) vanadyl acetylacetonate and L-cysteine is added, wherein vanadyl acetylacetonate: the molar ratio of L-cysteine is 1: 5-
6, concentration of the L-cysteine in 1-Methyl-2-Pyrrolidone solution is 0.417-0.5 mol/L；
C) it places in oil bath pan, flow back and heats 100-120 DEG C, stirring 2-3 h obtains bottle-green clear mixed solution；
D) mixed solution is placed in reaction kettle and carries out solvent thermal reaction；
E) the product deionized water and dehydrated alcohol after reacting are collected with 4000-8000 r/min eccentric cleaning；
F) product vacuum of collection is freeze-dried 6-48 h, temperature is-18-- 80 DEG C；
G) product after drying is placed in tube furnace, is heat-treated under an inert atmosphere to get the V of morphology controllable is arrived3S4
Material.
The inert atmosphere is nitrogen；The heat treatment is: with the heating of 5-10 DEG C/min rate, holding temperature 400-900
DEG C, soaking time is 2 h.
V made from a kind of above method3S4Application of the material as negative electrode of lithium ion battery electrode material.
The application specifically includes: by V3S4Material is 6: 2: 2 points according to mass ratio with Super P and carboxymethyl cellulose
Dissipate and slurry is made in deionized water is coated on Cu foil, be subsequently placed at baking oven under vacuum conditions 80 ~ 110 DEG C of drying 10 ~
12h to get arrive battery cathode electrode material.
It will obtain battery cathode electrode material and be cut into the circular electrode that diameter is 14 mm, using lithium metal as reference electrode
With to electrode, use Whatman GF/D as diaphragm, be assembled into CR2032 in the glove box that water, oxygen content are respectively less than 0.5ppm
Button cell, and tested by indigo plant electricity cell tester CT2001A.
The present invention is using solvent heat and is heat-treated V of the two-step method synthesis with excellent electrochemical performance3S4Material；The present invention
Method morphology controllable, it is easy to operate, be V3S4Preparation provide a kind of new approach.
The present invention has the advantages that
(1) a step solvent structure V is utilized3S4Presoma, method is simple, is easy manipulation；
(2) method provided through the invention, the V of preparation3S4The morphology controllable of material, purity is high；
(3) method provided through the invention, the V of preparation3S4There is excellent electrochemistry as lithium ion battery negative material
Performance；
(4) preparation method provided by the present invention is simple for process, mild condition, can be used for being mass produced.
Detailed description of the invention
Fig. 1 is flower-shaped V in the embodiment of the present invention 13S4XRD spectrum；
Fig. 2 is 2 small particles shape V of the embodiment of the present invention3S4XRD spectrum；
Fig. 3 is large grained V in the embodiment of the present invention 33S4XRD spectrum；
Fig. 4 is flower-shaped V in the embodiment of the present invention 13S4Stereoscan photograph；
Fig. 5 is 2 small particles shape V of the embodiment of the present invention3S4Stereoscan photograph；
Fig. 6 is large grained V in the embodiment of the present invention 33S4Stereoscan photograph；
Fig. 7 is V in 1-3 of the embodiment of the present invention3S4As cycle performance figure of the cathode in lithium ion battery；
Fig. 8 is V in 1-3 of the embodiment of the present invention3S4As high rate performance figure of the cathode in lithium ion battery.
Specific embodiment
With reference to the accompanying drawing and specific embodiment, the present invention will be further elaborated.It should be understood that these embodiments are only
For illustrating rather than for limiting the scope of the invention.In addition, after reading the contents of the present invention, this field
Technical staff can make various changes or modifications the present invention, and such equivalent forms equally fall within the attached claim of the application institute
The range that book limits.
Embodiment 1
1.V3S4The preparation of persursor material
A) the 1-Methyl-2-Pyrrolidone solution of 120 mL is measured into three neck round bottom flask；
B) vanadyl acetylacetonate/L-cysteine that molar ratio is 1:5 is added (L-cysteine is 6.0575 g)；
C) it places in oil bath pan, flows back and heat 100 DEG C of 3 h of stirring, obtain bottle-green clear mixed solution；
D) solution is fallen and is placed in baking oven in reaction kettle, 180 DEG C of reaction temperature, reaction time 12h；
E) product deionized water and dehydrated alcohol centrifugation (8000 r/min) after reacting are collected；
F) product after centrifugation is freezed in -18 DEG C and is placed in freeze drier within 48 hours drying 24 hours under vacuum condition,
Obtain V3S4Presoma；
2. flower-shaped V3S4The preparation of material
By V made from step 13S4Presoma is placed in tube furnace, and in a nitrogen atmosphere, heating rate is that 5 DEG C/min is warming up to
2 h are kept the temperature at 400 DEG C to be heat-treated to get flower-shaped V is arrived3S4Material；
3. flower-shaped V3S4Preparation as lithium ion battery electrode material
By V made from step 23S4Material, Super P and carboxymethyl cellulose are that 6:2:2 is scattered in deionization according to mass ratio
Slurry is made in water to be coated on Cu foil, be subsequently placed at baking oven under vacuum conditions 80 DEG C of drying 12h to get to battery electrode material
Material.
4.V3S4Test as lithium ion battery electrode material
Flower-shaped V prepared by step 33S4Electrode material is cut into the circular electrode that diameter is 14mm, electric using lithium metal as reference
Pole and to electrode, use Whatman GF/D as diaphragm, be assembled into the glove box that water, oxygen content are respectively less than 0.5ppm
CR2032 button cell.Lithium-ion electrolyte, ingredient are 1 M LiPF6It is dissolved in ethylene carbonate, diethyl carbonate and carbonic acid first
Mixing (mass ratio 1: 1: 1) solvent of ethyl ester.CR2032 button cell carries out constant current by indigo plant electricity cell tester CT2001A and fills
It discharges (0.001-3.0V), current density is 0.1 A/g, tests its cycle performance such as Fig. 7 embodiment 1, high rate performance such as Fig. 8
Embodiment 1.
With flower-shaped V prepared by the present embodiment 13S4Material, structure is from the XRD of Fig. 1 as can be seen that crystallinity is opposite
It is poor；It can be observed how it is to be self-assembled into three-dimensional flower-shaped structure by nano flake from the scanning electron microscope (SEM) photograph of Fig. 4, colored size
About at 1-2 μm；When as lithium ion battery anode active material, coulombic efficiency is 78.7% for the first time, is 0.1 in current density
A/g, after 50 circles, specific discharge capacity is 935 mAh/g；When current density is respectively 0.1,0.2,0.5,1,2,5 A/g,
Specific discharge capacity works as current density and returns to small electricity respectively up to 1396.5,997,887.5,779.2,704.8,641.4 mAh/g
Current density (0.1A/g), specific discharge capacity still keep capacity in 808.6 mAh/g, it can be seen that its preferable electrochemistry
Energy.
Embodiment 2
1.V3S4The preparation of persursor material
A) the 1-Methyl-2-Pyrrolidone solution of 125mL is measured into three neck round bottom flask；
B) vanadyl acetylacetonate/L-cysteine that molar ratio is about 1:5.5 is added (L-cysteine is 6.66325 g)；
C) it places in oil bath pan, flows back and heat 110 DEG C of 2.5 h of stirring, obtain bottle-green clear mixed solution；
D) solution is fallen and is placed in baking oven in reaction kettle, 180 DEG C of reaction temperature, reaction time 12h；
E) product deionized water and dehydrated alcohol centrifugation (6000 r/min) after reacting are collected；
F) product after centrifugation is placed in -60 DEG C of freezings to be placed in freeze drier within 24 hours under vacuum condition dry 24 small
When, i.e. acquisition V3S4Presoma.
2. fine granularity V3S4The preparation of material
By V made from step 13S4Presoma is placed in tube furnace, and in a nitrogen atmosphere, heating rate is that 5 DEG C/min is warming up to
2 h are kept the temperature at 600 DEG C to be heat-treated to get fine granularity V is arrived3S4Material.
3. fine granularity V3S4Preparation as lithium ion battery electrode material
By V made from step 23S4Material, Super P and carboxymethyl cellulose are that 6:2:2 is scattered in deionization according to mass ratio
Slurry is made in water to be coated on Cu foil, be subsequently placed at baking oven under vacuum conditions 100 DEG C of 10 h of drying to get to battery electrode
Material.
4.V3S4Test as lithium ion battery electrode material
Fine granularity V prepared by step 33S4Electrode material is cut into the circular electrode that diameter is 14mm, using lithium metal as ginseng
It than electrode and to electrode, uses Whatman GF/D as diaphragm, is assembled into the glove box that water, oxygen content are respectively less than 0.5ppm
CR2032 button cell.Lithium-ion electrolyte, ingredient are 1 M LiPF6It is dissolved in ethylene carbonate, diethyl carbonate and carbonic acid first
Mixing (mass ratio 1: 1: 1) solvent of ethyl ester.CR2032 button cell carries out constant current by indigo plant electricity cell tester CT2001A and fills
It discharges (0.001-3.0V), current density is 0.1 A/g, tests its cycle performance such as Fig. 7 embodiment 2, high rate performance such as Fig. 8
Embodiment 2.
With fine granularity V prepared by the present embodiment 23S4Material, structure is from the XRD of Fig. 2 as can be seen that its crystallization
Property enhancing；It can be that little particle by size in 100 ~ 200 nm is accumulated with it from Fig. 5；When it is negative as lithium ion battery
When the active material of pole, coulombic efficiency is 72.3% for the first time；It is 0.1 A/g in current density, after 50 circles, specific discharge capacity
For 1095.4 mAh/g；Specific discharge capacity under the different current densities of 0.1,0.2,0.5,1,2,5 A/g reaches respectively
1327.7,840.2,767.3,716.6,690.8,600 mAh/g, and work as current density and return to low current density (0.1A/g),
Its specific discharge capacity still keeps the specific discharge capacity of 824 mAh/g, it can be seen that its chemical property increases.
Embodiment 3
1.V3S4The preparation of persursor material
A) the 1-Methyl-2-Pyrrolidone solution of 130mL is measured into three neck round bottom flask；
B) vanadyl acetylacetonate/L-cysteine that molar ratio is about 1:6 is added (L-cysteine is 0.7269 g)；
C) it places in oil bath pan, flows back and heat 120 DEG C of 2 h of stirring, obtain bottle-green clear mixed solution；
D) solution is fallen and is placed in baking oven in reaction kettle, 180 DEG C of reaction temperature, 12 h of reaction time；
E) product deionized water and dehydrated alcohol after reacting repeatedly are centrifuged after (4000 r/min) is cleaned and collect；
F) product of collection is placed in -80 DEG C of freezings and is placed in freeze drier within 12 hours drying 24 hours under vacuum condition,
Obtain V3S4Presoma.
2. large grained V3S4The preparation of material
By V made from step 13S4Presoma is placed in tube furnace, and in a nitrogen atmosphere, heating rate is that 10 DEG C/min is warming up to
2 h are kept the temperature at 900 DEG C to be heat-treated to get large grained V is arrived3S4；
3. large grained V3S4Preparation as lithium ion battery electrode material
By V made from step 23S4Material, Super P and carboxymethyl cellulose are that 6:2:2 is scattered in deionization according to mass ratio
Slurry is made in water to be coated on Cu foil, be subsequently placed at baking oven under vacuum conditions 110 DEG C of drying 8h to get to battery electrode material
Material.
4.V3S4Test as lithium ion battery electrode material
Large grained V prepared by step 33S4Electrode material is cut into the circular electrode that diameter is 14mm, using lithium metal as ginseng
It than electrode and to electrode, uses Whatman GF/D as diaphragm, is assembled into the glove box that water, oxygen content are respectively less than 0.5ppm
CR2032 button cell.Lithium-ion electrolyte, ingredient are 1 M LiPF6It is dissolved in ethylene carbonate, diethyl carbonate and carbonic acid first
Mixing (mass ratio 1: 1: 1) solvent of ethyl ester.CR2032 button cell carries out constant current by indigo plant electricity cell tester CT2001A and fills
It discharges (0.001-3.0V), current density is 0.1 A/g, tests its cycle performance such as Fig. 7 embodiment 3, high rate performance such as Fig. 8
Embodiment 3.
With large grained V prepared by the present embodiment 33S4Material, structure is from the XRD of Fig. 3 as can be seen that its crystallization
Degree is very high, but partial impurities peak occurs, corresponds to V2O3；As can be seen from Figure 6 its particle significantly increases, and size is uneven
One, about 1 μm；When its as lithium ion battery negative material its current density be 0.1A/g when, coulombic efficiency is for the first time
78.33%, after 50 circles, specific discharge capacity is 636.5 mAh/g；It is close in the different electric currents of 0.1,0.2,0.5,1,2,5 A/g
Specific discharge capacity under degree works as current density respectively up to 776.4,620.2,580.3,544.2,507.9,484.6 mAh/g
Low current density (0.1A/g) is returned to, specific discharge capacity still keeps the 86.7% of initial capacity, shows preferable cyclicity
It can be with excellent high rate performance.
Claims (4)
1. a kind of V3S4The preparation method of material, which is characterized in that this method comprising the following specific steps
A) 1-Methyl-2-Pyrrolidone solution is poured into three neck round bottom flask；
B) vanadyl acetylacetonate and L-cysteine is added, wherein vanadyl acetylacetonate: the molar ratio of L-cysteine is 1: 5-
6, concentration of the L-cysteine in 1-Methyl-2-Pyrrolidone solution is 0.417-0.5 mol/L；
C) it places in oil bath pan, flow back and heats 100-120 DEG C, stirring 2-3 h obtains bottle-green clear mixed solution；
D) mixed solution is placed in reaction kettle and carries out solvent thermal reaction；
E) the product deionized water and dehydrated alcohol after reacting are collected with 4000-8000 r/min eccentric cleaning；
F) product vacuum of collection is freeze-dried 6-48 h, temperature is-18-- 80 DEG C；
G) product after drying is placed in tube furnace, is heat-treated under an inert atmosphere to get the V of morphology controllable is arrived3S4Material
Material.
2. V as described in claim 13S4The preparation method of material, which is characterized in that the inert atmosphere is nitrogen；At the heat
Reason is: with the heating of 5-10 DEG C/min rate, 400-900 DEG C of holding temperature, soaking time is 2 h.
3. V made from a kind of claim 1 the method3S4Application of the material as negative electrode of lithium ion battery electrode material.
4. application according to claim 3, which is characterized in that the application specifically includes: by V3S4Material and Super P and
Carboxymethyl cellulose is to be scattered in deionized water be made slurry be coated on Cu foil at 6: 2: 2 according to mass ratio, is subsequently placed at baking
Case under vacuum conditions 80 ~ 110 DEG C of 10 ~ 12h of drying to get arrive battery cathode electrode material.
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| CN113921817A (en) * | 2021-08-23 | 2022-01-11 | 济南大学 | V-shaped groove3S4@V2C composite material and preparation method and application thereof |
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| CN110407251B (en) | 2021-10-15 |
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