CN110116992A - A kind of preparation method and application of two selenizing niobium of sodium ion battery electrode material - Google Patents
A kind of preparation method and application of two selenizing niobium of sodium ion battery electrode material Download PDFInfo
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- CN110116992A CN110116992A CN201910379103.6A CN201910379103A CN110116992A CN 110116992 A CN110116992 A CN 110116992A CN 201910379103 A CN201910379103 A CN 201910379103A CN 110116992 A CN110116992 A CN 110116992A
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- niobium
- ion battery
- electrode material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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 preparation method and application of two selenizing niobium of sodium ion battery electrode material, the method includes being uniformly mixed selenium source and niobium source, it in non-oxidizing atmosphere or vacuum, is sintered at a certain temperature, two selenizing niobium material of pure phase is made after natural cooling.The features such as material of the present invention has small investment, preparation process flow and equipment to be simple and convenient to operate, product purity is high and has a safety feature.When the two selenizing niobium materials that the present invention is prepared are applied to sodium ion battery electrode material, there is excellent stable circulation performance and outstanding high rate performance.
Description
Technical field
The invention belongs to energy storage materials and technical field of chemical power, more particularly, to a kind of sodium ion battery electrode material
The preparation method and application of two selenizing niobiums.
Background technique
As part indispensable in new energy system, requirement of the people to energy storage device is continuously improved.Lithium ion
Since secondary cell self-discovery, the advantages that due to high-energy density, long circulation life, lesser self-discharge phenomenon, by very big
Concern and be rapidly developed.With the large-scale application of lithium ion secondary battery, the price of cobalt acid lithium is caused to rise year by year.
Due to sodium resource reserve it is big, it is widely distributed, be easy to the features such as refining so that sodium-ion battery can be used as the substitution of lithium ion battery
One of selection.Due to the radius of sodium ionGreater than the radius of lithium ionSo that sodium ion is in insert material
It is more difficult during crystal structure, therefore, research and probe height ratio capacity, long circulation life electrode material become develop sodium from
The key of sub- battery.
In terms of sodium-ion battery positive material research, the Na of stratified material containing sodiumxMO2(M=Co, Ni, Fe, Mn, V etc.) tool
There is reversible ionic deintercalation performance, is widely used in secondary battery electrode material.Early in 1981, the researchs such as Delmas synthesized difference
The Na of phasexCoO2, and their electrochemistry storage sodium behavior (Solid State Ionics, 1981,165,3-4) has been probed into, due to
Sodium ion improves material and is conducive to improving its dynamic performance in the deintercalation relative difficulty of stratiform transition metal oxide material
Improve the chemical property of sodium-ion battery.For olivine-type NaMPO4(M=Fe, Mn etc.) material, Sun etc. are utilized
Pechini method is successfully prepared NaFePO4Material, lower (the Materials science and of capacity retention ratio
Engineering B, 2012,1-6).For Nasicon class NaxM2(PO4)3(M=V, Ti etc.) has Three-dimensional Open ion defeated
Wan access is a kind of fast ion conducting material.
In terms of anode material of lithium-ion battery research, in carbon material research, since sodium ion radius is larger, Bu Neng
Reversible deintercalation is carried out in graphite linings, non-graphite carbon material mainly includes two class of hard carbon and soft carbon, and wherein hard carbon material exists not
The problems such as reversible capacity is big, high rate performance difference and fast decaying.For metal and alloy materials, Xiao etc. uses high-energy ball milling
Method is prepared for SnSb/C nano-complex, and first week reversible storage sodium capacity is 544mAh/g, be demonstrated by preferable cyclical stability with
High rate performance maintains 435mAh/g (Chemical communications, 2012,48,3321) after 50 weeks circulations.For
Such material, in charge and discharge process, the electrode material microstructural damage as caused by electrode volume expansion, battery capacity meeting
Rapid decay, to limit its application range.Using suitable preparation method or inert substance is introduced as structural support means
To alleviate the development priority that its volume change in charge and discharge process is alloy material.In addition, there is a considerable amount of document reports
Road metal oxide, titanate, organic matter etc. also can be used as anode material of lithium-ion battery.
As people constantly rise up into sodium-ion battery energy storage exploration, researcher, which thirsts for exploitation, has high security, height
The new material of the excellent electrochemical performances such as specific capacity, excellent high rate performance, to meet the development of the following sodium-ion battery energy storage
Demand.
Summary of the invention
The object of the present invention is to provide a kind of preparation method and application of two selenizing niobium of sodium ion battery electrode material.
In order to achieve the above object, the present invention also provides the preparation sides of above-mentioned two selenizing niobium of sodium ion battery electrode material
Method characterized by comprising selenium powder and niobium powder are uniformly mixed, is placed under non-oxidizing atmosphere or vacuum condition and is sintered,
Two selenizing niobium of sodium ion battery electrode material is made after cooling.
Preferably, the niobium powder and the molar ratio of niobium and selenium in selenium powder are 1:2~3.
It is highly preferred that the molar ratio of niobium and selenium is 1:.2.1~2.3 in the niobium powder and selenium powder.
Preferably, the niobium powder and selenium powder are equal by magnetic agitation, hand-ground, wet ball grinding or dry ball milling mixing
Even, incorporation time is 1~20h.
It is highly preferred that the niobium powder and selenium powder are uniformly mixed by hand-ground or wet ball grinding, incorporation time 2
~4h.
Preferably, the non-oxidizing atmosphere is nitrogen, argon gas or hydrogen.
It is highly preferred that the non-oxidizing atmosphere is argon gas.
Preferably, heating rate is 1~20 DEG C/min in the sintering process, and sintering temperature is 500~1000 DEG C, sintering
Soaking time is 1~48h.
It is highly preferred that heating rate is 2~10 DEG C/min in the sintering process, sintering temperature is 600~850 DEG C, is burnt
Knot soaking time is 2~10h.
Application of the two selenizing niobium of sodium ion battery electrode material of above method preparation in sodium-ion battery, feature exist
In, which is characterized in that the working electrode of the sodium-ion battery is two selenizing niobiums.
Detailed description of the invention
Fig. 1 is the surface sweeping electron microscope for the two selenizing niobium materials that embodiment 2 is prepared；
Fig. 2 is the XRD spectrum for the two selenizing niobium materials that embodiment 2 is prepared；
Fig. 3 is the 1st time, the 2nd time and the 10th time charging and discharging curve figure of the two selenizing niobium materials that embodiment 2 is prepared；
Fig. 4 is cycle performance figure of the two selenizing niobium materials that are prepared of embodiment 2 under 100mA/g current density；
Fig. 5 is high rate performance figure of the two selenizing niobium materials that are prepared of embodiment 2 under different electric current densities.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Two selenizing niobium materials, conductive carbon black and binder sodium carboxymethylcellulose (CMC) that the method for the present invention synthesizes are pressed
Mass ratio 8:1:1 is uniformly mixed, and is coated on copper foil, after being dried in vacuo for 24 hours at 100 DEG C, is struck out electrode slice.
It is to electrode, with 1mol/LNaClO with metallic sodium4(solvent is the ethylene carbonate that mass ratio is 1:1 to solution
(EC) mixed solution of/dimethyl carbonate (DMC)) it is used as electrolyte, button cell is assembled into argon gas glove box.
Electrochemical property test is carried out using the blue electricity CT2001A type cell tester in Wuhan, charging/discharging voltage range is
0.01V~3.0V (vs.Na+/Na), test temperature are 25 DEG C.
Embodiment 1
The niobium powder of 1g is uniformly mixed with the selenium powder of 2g by dry ball milling, incorporation time 4h, under the conditions of argon atmosphere
It is sintered in tube furnace, after being warming up to 650 DEG C and constant temperature holding 2h with 5 DEG C/min rate, cooled to room temperature is obtained
Two selenizing niobium of product sodium ion battery electrode material.
Embodiment 2
The niobium powder of 0.93g is uniformly mixed with the selenium powder of 1.975g by hand-ground, incorporation time 2h, in vacuum condition
Under be sintered in tube furnace, be warming up to after 750 DEG C and constant temperature keeps 3h with 10 DEG C/min rate, cooled to room temperature obtains
To two selenizing niobium of product sodium ion battery electrode material.
Fig. 1 is the XRD spectrum of two selenizing niobium materials, it can be seen from the figure that the peak position of the XRD spectrum of material is good
With on standard card (JCPDS No.72-0864) peak position and peak intensity match, illustrate that the ingredient of material obtained is pure phase
NbSe2.
Fig. 2 is the 1st time, the 2nd time and the 10th time charging and discharging curve figure of two selenizing niobium materials, as shown, following in difference
There is similar curve in the discharge process of ring, i.e., one in 2.0V or so significantly long discharge platform and 1.5~1.0V's
One shorter more inclined platform；In the charging process of different circulations, different curves have similar shape, that is, occur one
In the apparent voltage platform of 2.0~2.2V.
Fig. 3 is cycle performance figure of the two selenizing niobium materials under 100mA/g current density, discharge capacity after 100 circulations
It is the 84.7% of the 2nd cyclic discharge capacity for 98.8mAh/g；Illustrate that the material has excellent cyclical stability.
Fig. 4 is circulating ratio figure of the two selenizing niobium materials under different discharge currents.As shown, 0.01-3.0V's
Within the scope of charging/discharging voltage, when discharge current be increased to 100mA/g, 200mA/g, 500mA/g, 1000mA/g, 2000mA/g,
When 4000mA/g, the capacity of two selenizing niobium electrodes remain respectively 114.1mAh/g, 104.7mAh/g, 94.7mAh/g,
88.1mAh/g, 83.9mAh/g, 76.8mAh/g illustrate that the material of invention has excellent high rate performance.
Embodiment 3
The niobium powder of 1.1g is uniformly mixed with the selenium powder of 2.2g by magnetic force, incorporation time 2h, under the conditions of argon atmosphere
It is sintered in tube furnace, after being warming up to 800 DEG C and constant temperature holding 10h with 15 DEG C/min rate, cooled to room temperature is obtained
To two selenizing niobium of product sodium ion battery electrode material.
Embodiment 4
The niobium powder of 1.86g is uniformly mixed with the selenium powder of 4g by wet ball grinding, incorporation time 2h, in argon atmosphere condition
Under be sintered in tube furnace, be warming up to after 700 DEG C and constant temperature keeps 7h with 7 DEG C/min rate, cooled to room temperature obtains
To two selenizing niobium of product sodium ion battery electrode material.
Embodiment 5
The niobium powder of 2.5g is uniformly mixed with the selenium powder of 5.02g by wet ball grinding, incorporation time 3h, in nitrogen atmosphere item
It is sintered in tube furnace under part, after being warming up to 750 DEG C and constant temperature holding 5h with 3 DEG C/min rate, cooled to room temperature
Obtain two selenizing niobium of product sodium ion battery electrode material.
Embodiment 6
The niobium powder of 3g is uniformly mixed with the selenium powder of 6.21g by wet ball grinding, incorporation time 2h, in argon atmosphere condition
Under be sintered in tube furnace, be warming up to after 850 DEG C and constant temperature keeps 2h with 1 DEG C/min rate, cooled to room temperature obtains
To two selenizing niobium of product sodium ion battery electrode material.
Claims (8)
1. a kind of preparation method of two selenizing niobium of sodium ion battery electrode material characterized by comprising mix selenium powder and niobium powder
It closes uniformly, is placed under non-oxidizing atmosphere or vacuum condition and is sintered, obtain two selenium of sodium ion battery electrode material after cooling
Change niobium.
2. the preparation method of two selenizing niobium of sodium ion battery electrode material as described in claim 1, which is characterized in that the niobium powder
It is 1:2~3 with the molar ratio of niobium in selenium powder and selenium.
3. the preparation method of two selenizing niobium of sodium ion battery electrode material as described in claim 1, which is characterized in that the niobium powder
It is 1:.2.1~2.3 with the molar ratio of niobium in selenium powder and selenium.
4. the preparation method of two selenizing niobium of sodium ion battery electrode material as described in claim 1, which is characterized in that the niobium source
It is uniformly mixed with selenium source by magnetic agitation, hand-ground, wet ball grinding or dry ball milling, incorporation time is 1~20h.
5. the preparation method of two selenizing niobium of sodium ion battery electrode material as described in claim 1, which is characterized in that described non-oxygen
The property changed atmosphere is nitrogen, argon gas or hydrogen.
6. the preparation method of two selenizing niobium of sodium ion battery electrode material as described in claim 1, which is characterized in that the sintering
Heating rate is 1~20 DEG C/min in the process, and sintering temperature is 500~1000 DEG C, and the sintered heat insulating time is 1~48h.
7. the preparation method of two selenizing niobium of sodium ion battery electrode material as claimed in claim 6, which is characterized in that the sintering
Heating rate is 2~10 DEG C/min in the process, and sintering temperature is 600~850 DEG C, and the sintered heat insulating time is 2~10h.
8. the two selenizing niobium of sodium ion battery electrode material of any one of claim 1~7 the method preparation is in sodium-ion battery
In application, which is characterized in that the working electrode of the sodium-ion battery be two selenizing niobiums.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111422837A (en) * | 2020-03-31 | 2020-07-17 | 上海电力大学 | Preparation and application of lithium ion battery electrode material |
| CN111422838A (en) * | 2020-03-31 | 2020-07-17 | 上海电力大学 | Preparation and application of potassium ion battery electrode material |
| CN113860270A (en) * | 2021-09-27 | 2021-12-31 | 曲阜师范大学 | Cubic phase Cu3NbSe4Nano material and preparation method and application thereof |
| CN115285947A (en) * | 2022-08-12 | 2022-11-04 | 深圳博磊达新能源科技有限公司 | Selenide negative electrode material for sodium ion battery, preparation method of selenide negative electrode material and sodium ion battery |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111422837A (en) * | 2020-03-31 | 2020-07-17 | 上海电力大学 | Preparation and application of lithium ion battery electrode material |
| CN111422838A (en) * | 2020-03-31 | 2020-07-17 | 上海电力大学 | Preparation and application of potassium ion battery electrode material |
| CN113860270A (en) * | 2021-09-27 | 2021-12-31 | 曲阜师范大学 | Cubic phase Cu3NbSe4Nano material and preparation method and application thereof |
| CN115285947A (en) * | 2022-08-12 | 2022-11-04 | 深圳博磊达新能源科技有限公司 | Selenide negative electrode material for sodium ion battery, preparation method of selenide negative electrode material and sodium ion battery |
| CN115285947B (en) * | 2022-08-12 | 2023-06-16 | 深圳博磊达新能源科技有限公司 | Selenide anode material for sodium ion battery, preparation method of selenide anode material and sodium ion battery |
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Application publication date: 20190813 |