CN110282660A - A kind of four vanadic sulfide powder of nano bar-shape and its preparation method and application - Google Patents
A kind of four vanadic sulfide powder of nano bar-shape and its preparation method and application Download PDFInfo
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- CN110282660A CN110282660A CN201910595665.4A CN201910595665A CN110282660A CN 110282660 A CN110282660 A CN 110282660A CN 201910595665 A CN201910595665 A CN 201910595665A CN 110282660 A CN110282660 A CN 110282660A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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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
- 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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- 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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- 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
Abstract
The invention discloses a kind of four vanadic sulfide raw powder's production technologies of nano bar-shape, comprising the following steps: (1) takes thioacetamide to dissolve in dehydrated alcohol, stir to whole dissolutions, obtain mixture A；(2) ammonium metavanadate is added in mixture A, stirs to whole dissolutions, obtains mixture B；(3) dilute hydrochloric acid is instilled in mixture B under agitation, forms clear solution, obtains mixture C；(4) mixture C is gone in hydrothermal reaction kettle, 24~25h of hydro-thermal reaction；(5) natural cooling after reaction, centrifuge washing for several times after, be dried in vacuo to get four vanadic sulfide powder of nano bar-shape.Four vanadic sulfide of nano bar-shape specific capacity with higher that the present invention prepares, excellent cyclical stability, length service life and higher electric conductivity.
Description
Technical field
The present invention relates to battery material field, more particularly to a kind of four vanadic sulfide powder of nano bar-shape and its system
Preparation Method and application.
Background technique
Currently, the main bugbear that ion battery is faced is still probing into and designing for high-performance negative electrode material.
Graphite is widely applied in ion battery as negative electrode material, but graphite cathode material actual specific capacity is relatively
It is low, it is difficult to meet the growing energy storage demand of people.
In order to find suitable ion battery cathode material, correlative study person's extension a collection of compound is explored.At this
In a little negative electrode materials, researchers generally believe that the metal sulfide with high theoretical capacity is that one kind has promising time very much
The person of choosing, and carrying out regulation to their nanostructure is a kind of very important plan for being further improved its chemical property
Slightly.
Four vanadic sulfides have attracted the concern of many researchers due to its similar unique two-dimensional layered structure.It is this kind of that there is standard
The sulfide of two-dimensional layer structure is typical sandwich structure, i.e., clips transition metal layer V between two S layers.In crystalline substance
In body structure, it is covalent bond between V-S atom that in S-V-S layers, each V atom, which is hexa-coordinate in octahedron, between layers with
Van der Waals force is connected.This structure makes internal key effect in compound middle layer strong, and the interaction force of interlayer is relatively weak, interlayer
Gap can allow the entrance of foreign substance.This kind of stratiform transient metal sulfide is maximum as lithium/sodium ion negative electrode material
The advantages of be that good lithium/sodium ion diffusion admittance can be provided, the volume occurred during buffer cycles when de-/embedding lithium/sodium is swollen
It is swollen, it is to have much one of lithium/anode material of lithium-ion battery of development prospect.
Although based on above-mentioned special physical characteristic, four vanadic sulfides theoretical capacity with higher, excellent charge and discharge times
Rate performance and cycle performance, however, there is also some disadvantages, four vanadic sulfides and other transient metal sulfides one for four vanadic sulfides
Sample, in lithium ion insertion/extraction process, it may appear that conductivity is low, the big feature of volume change, hinders VS4As high-performance electric
Pole material, Three-dimensional VS4/graphene hierarchical architecture as high-
Capacity anode for lithium-ion batteries, Lithium reaction mechanism and high
rate capability ofVS4–graphene nanocomposite as an anode material
There is related report in the documents such as forlithiumbatteries.
Therefore, it is high how to provide a kind of conductivity, the small VS of volume change4Electrode material is that those skilled in the art need
The technical issues of solution.
Summary of the invention
In view of this, the present invention provides a kind of preparation method of four vanadic sulfide of nano bar-shape, the nano bar-shape prepared
Four vanadic sulfides specific capacity with higher, excellent cyclical stability, length service life and higher electric conductivity.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of four vanadic sulfide raw powder's production technology of nano bar-shape, comprising the following steps:
(1) it takes thioacetamide to dissolve in dehydrated alcohol, stirs to whole dissolutions, obtain mixture A；
(2) ammonium metavanadate is added in mixture A, stirs to whole dissolutions, obtains mixture B；
(3) dilute hydrochloric acid is instilled in mixture B under agitation, forms clear solution, obtains mixture C；
(4) mixture C is gone in hydrothermal reaction kettle, 24~25h of hydro-thermal reaction；
(5) natural cooling after reaction, centrifuge washing for several times after, vacuum drying vulcanizes vanadium powder to get nano bar-shape four
Body.
Preferably, the thioacetamide: ammonium metavanadate: dehydrated alcohol: dilute hydrochloric acid=(4~5) mmol:(0.5-1)
mmol:(60-70)mL:1mL。
Preferably, the thioacetamide: ammonium metavanadate: dehydrated alcohol: dilute hydrochloric acid=5mmol:1mmol:70mL:1mL.
Preferably, the dilute hydrochloric acid concentration is 20wt%.
Preferably, the temperature of the hydro-thermal reaction is controlled at 180~190 DEG C.
Preferably, the step (1), step (2), the middle stirring of step (3) are magnetic agitation, and stirring rate is
300r/min~400r/min, step (1) mixing time is 1~2h, step (2) mixing time is 1~2h, step (3) stirring
Time is 0.5~1h.
Preferably, the step (5) specifically: natural cooling after reaction, with anhydrous dehydrated alcohol centrifuge washing four
It is secondary, deionized water centrifuge washing four times, it is dried in vacuo 12-13h.
A kind of four vanadic sulfide powder of nano bar-shape, the four vanadic sulfide powder of nano bar-shape are that diameter is 20~60nm, length
For the nano bar-shape structure of 1~2um.
A kind of application of the four vanadic sulfide powder of nano bar-shape prepared by the above method, the four vanadic sulfides nano-powder are answered
For in sodium/lithium/Magnesium ion battery or photocatalysis field.
Compared with prior art, the invention has the benefit that
1, the high sulfur content of four vanadic sulfides makes it show apparent Li-S characteristic, thus VS in lithium-ion energy storage4Table
Reveal higher specific capacity；The preparation method effectively inhibits receiving of occurring in crystallization process by the way that certain dilute hydrochloric acid is added
The rodlike four vanadic sulfides agglomeration traits of rice.By adjusting the usage amount of dilute hydrochloric acid, a certain amount of H is obtained+To control VS4Growth,
Dilute hydrochloric acid dosage is more, and agglomeration is fewer, and when reaching 1mL dilute hydrochloric acid, agglomeration disappears substantially.
2, the change of solvent will affect the shape of material, such as sea urchin sample VS4, octopus sample VS4, sea grass shape VS4, flower-shaped VS4Shape
Shape difference is exactly caused by solvent is different, and the present invention is prepared for rodlike VS as solvent using dehydrated alcohol for the first time4, dehydrated alcohol
As reaction dissolvent primarily to inhibiting the hydrolysis rate of vanadate, the speed of growth can be effectively controlled in this way.
3, four vanadic sulfide of nano bar-shape shows to have excellent cyclical stability by electrochemical property test and longer makes
Use the service life；Lesser internal driving also indicates that four vanadic sulfide negative electrode material electric conductivity with higher of nano bar-shape, promotes its excellent
Chemical property more.
4, the configuration of the entire solution of the present invention is carried out under continuously stirring.It is produced by the present invention
VS4With biggish specific surface area, reunion and the dusting certainly of four vanadic sulfide nanometer rods can be alleviated well, can effectively be promoted
VS4Chemical property.Meanwhile this method is easy to operate, can be obtained by a step hydro-thermal, and reaction temperature is low, reaction week
Phase is short, VS obtained4Chemical constituent is uniform, purity is high.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 attached drawing is the SEM figure of four vanadic sulfide of nano bar-shape prepared by the embodiment of the present invention 1；
Fig. 2 attached drawing is the electrochemical impedance spectrogram of four vanadic sulfide of nano bar-shape prepared by the embodiment of the present invention 1；
Fig. 3 attached drawing is that four vanadic sulfide of nano bar-shape prepared by the embodiment of the present invention 1 is used as lithium ion battery negative material
Chemical property figure；
Fig. 4 attached drawing is the SEM figure of four vanadic sulfide of nano bar-shape of comparative example 1 of the present invention preparation.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
It takes in 5mmol thioacetamide (TAA) plus 70mL dehydrated alcohol, then dissolves it all with magnetic agitation 1h；
1mmol ammonium metavanadate is added under magnetic stirring later, and continues stirring 1h and makes it completely dissolved；It is stirred continuously lower addition 1mL
Dilute hydrochloric acid, stirring 0.5h form clear solution；Above-mentioned stirring rate is 300r/min~400r/min, by the mixed of above-mentioned acquisition
It closes liquid to go in the polytetrafluoroethyllining lining of 100mL stainless steel autoclave, seal stainless steel autoclave and is put
Enter air dry oven to react for 24 hours at 180 DEG C；After cooled to room temperature, with anhydrous dehydrated alcohol centrifuge washing products therefrom
Four times, deionized water centrifuge washing products therefrom four times is simultaneously dried in vacuo 12h to get four vanadic sulfide powder of nano bar-shape.Fig. 1 is
The SEM of four vanadic sulfide of nano bar-shape manufactured in the present embodiment schemes.Confirm VS manufactured in the present embodiment4With more neat shape
Looks, higher purity and crystallinity and substantially without unordered stacking the phenomenon that.
In order to further demonstrate that beneficial effects of the present invention, four vanadic sulfide of nano bar-shape prepared by embodiment 1 is as lithium
Ion battery cathode material carries out electric conductivity and electrochemical property test:
Firstly, being 8:1:1 dissolution by mass fraction ratio by four vanadic sulfide of nano bar-shape, acetylene black and polyvinylidene fluoride
In N-Methyl pyrrolidone, uniform slurry is stirred into, is coated on copper foil, 80 DEG C of air drying 0.5h, 110 DEG C of vacuum
Middle dry 12h, then slice compacting is used as the working electrode of lithium ion battery；CR2032 button electricity is assembled in pure argon atmosphere
Lithium piece is used as to electrode by pond, and polypropylene screen (Celgard 2400) is used as diaphragm, the ethylene carbonate of 1.0M lithium hexafluoro phosphate
Ester/diethyl carbonate/dimethyl carbonate (volume ratio 1:1:1) is used as electrolyte；By ion battery in LAND test macro
On tested, charging/discharging voltage range be 0.01V-3V, lithium ion battery test charging and discharging currents density be 200mA/g.
Fig. 2 is electrochemical impedance spectrogram, and the frequency range of test is 0.01Hz~100KHz, Charge-transfer resistance (Rct)
Half circular diameter of high frequency region is shown as, the relative size of Warburg impedance (Zw) shows as the slope of low frequency range straight line.It confirms
Nano bar-shape VS prepared by the present invention4Cathode has lesser Rct value, about 100ohm, and has lesser Zw value, this meaning
Nano bar-shape VS4Cathode has good electric conductivity and high rate capability.
Fig. 3 is the chemical property figure that four vanadic sulfide of nano bar-shape is used as lithium ion battery negative material.Confirm utilization
Nano bar-shape VS prepared by the present invention4Under the current density of 200mA/g, first discharge specific capacity reaches the lithium ion battery of production
574.3mAh g is arrived-1, after long circulating 120 encloses, reversible remaining specific capacity can still remain into 439.3mAh g-1, can still account for head
The 76.5% of secondary specific capacity, as can be seen from Figure 3 the volume change of negative electrode material is small, battery has extended cycle life.
Embodiment 2
It takes in 4mmol thioacetamide (TAA) plus 60mL dehydrated alcohol, then dissolves it all with magnetic agitation 2h；
0.5mmol ammonium metavanadate is added under magnetic stirring later, and continues stirring 2h and makes it completely dissolved；It is stirred continuously lower addition
1mL dilute hydrochloric acid, stirring 1h form clear solution；Above-mentioned stirring rate is 300r/min~400r/min, by above-mentioned acquisition
Mixed liquor is gone in the polytetrafluoroethyllining lining of 100mL stainless steel autoclave, seal stainless steel autoclave and by its
It is put into air dry oven and reacts 23h at 190 DEG C；After cooled to room temperature, produced obtained by anhydrous dehydrated alcohol centrifuge washing
Object four times, deionized water centrifuge washing products therefrom four times is simultaneously dried in vacuo 12h to get four vanadic sulfide powder of nano bar-shape.
Comparative example 1
It takes in 5mmol thioacetamide (TAA) plus 70mL dehydrated alcohol, then dissolves it all with magnetic agitation 1h；
1mmol ammonium metavanadate is added under magnetic stirring later, and continues stirring 1h and makes it completely dissolved；It is stirred continuously lower addition
0.75mL dilute hydrochloric acid, stirring 0.5h form clear solution；The mixed liquor of above-mentioned acquisition is gone into 100mL stainless steel autoclave
Polytetrafluoroethyllining lining in, seal stainless steel autoclave and put it into air dry oven and reacted for 24 hours at 180 DEG C；
After cooled to room temperature, with anhydrous dehydrated alcohol centrifuge washing products therefrom four times, deionized water centrifuge washing products therefrom
Four times and 12h is dried in vacuo to get four vanadic sulfide powder of nano bar-shape.Fig. 4 is that the nano bar-shape four of this comparative example preparation vulcanizes
The SEM of vanadium schemes.Confirm the part nano bar-shape VS of comparative example preparation4There is bending growth and size is non-uniform existing
As this affects VS to a certain extent4Crystallinity.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other
The difference of embodiment, the same or similar parts in each embodiment may refer to each other.For device disclosed in embodiment
For, since it is corresponded to the methods disclosed in the examples, so being described relatively simple, related place is said referring to method part
It is bright.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (9)
1. a kind of four vanadic sulfide raw powder's production technology of nano bar-shape, which comprises the following steps:
(1) it takes thioacetamide to dissolve in dehydrated alcohol, stirs to whole dissolutions, obtain mixture A；
(2) ammonium metavanadate is added in mixture A, stirs to whole dissolutions, obtains mixture B；
(3) dilute hydrochloric acid is instilled in mixture B under agitation, forms clear solution, obtains mixture C；
(4) mixture C is gone in hydrothermal reaction kettle, 24~25h of hydro-thermal reaction；
(5) natural cooling after reaction, centrifuge washing for several times after, be dried in vacuo to get four vanadic sulfide powder of nano bar-shape.
2. four vanadic sulfide raw powder's production technology of a kind of nano bar-shape according to claim 1, which is characterized in that the sulphur
For acetamide: ammonium metavanadate: dehydrated alcohol: dilute hydrochloric acid=(4~5) mmol:(0.5~1) mmol:(60~70) mL:1mL.
3. four vanadic sulfide raw powder's production technology of a kind of nano bar-shape according to claim 1, which is characterized in that the sulphur
For acetamide: ammonium metavanadate: dehydrated alcohol: dilute hydrochloric acid=5mmol:1mmol:70mL:1mL.
4. four vanadic sulfide raw powder's production technology of a kind of nano bar-shape according to claim 1-3, feature exist
In the dilute hydrochloric acid concentration is 20wt%.
5. four vanadic sulfide raw powder's production technology of a kind of nano bar-shape according to claim 4, which is characterized in that the water
The temperature of thermal response is controlled at 180~190 DEG C.
6. four vanadic sulfide raw powder's production technology of a kind of nano bar-shape according to claim 5, which is characterized in that the step
Suddenly (1), step (2), the middle stirring of step (3) are magnetic agitation, and stirring rate is 300r/min~400r/min, step
(1) mixing time is 1~2h, step (2) mixing time is 1~2h, step (3) mixing time is 0.5~1h.
7. four vanadic sulfide raw powder's production technology of a kind of nano bar-shape according to claim 6, which is characterized in that the step
Suddenly (5) specifically: natural cooling after reaction, with anhydrous dehydrated alcohol centrifuge washing four times, deionized water centrifuge washing four
It is secondary, it is dried in vacuo 12~13h.
8. a kind of utilize four vanadic sulfide powder of nano bar-shape made from any one of the claim 1-7 preparation method, feature
It is, which is the nano bar-shape structure that diameter is 20~60nm, length is 1~2um.
9. four vanadic sulfide powder of nano bar-shape as claimed in claim 8 is preparing sodium-ion battery, lithium ion battery, magnesium ion electricity
Application in pond or photochemical catalyst.
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| WO2022172963A1 (en) * | 2021-02-10 | 2022-08-18 | 国立研究開発法人産業技術総合研究所 | Coated metal sulfide layer and method for producing same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022172963A1 (en) * | 2021-02-10 | 2022-08-18 | 国立研究開発法人産業技術総合研究所 | Coated metal sulfide layer and method for producing same |
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