CN110304612A - A kind of two ferrous selenide nanometer sheets for lithium ion battery negative material - Google Patents
A kind of two ferrous selenide nanometer sheets for lithium ion battery negative material Download PDFInfo
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- CN110304612A CN110304612A CN201910559127.XA CN201910559127A CN110304612A CN 110304612 A CN110304612 A CN 110304612A CN 201910559127 A CN201910559127 A CN 201910559127A CN 110304612 A CN110304612 A CN 110304612A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M10/052—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
- 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
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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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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- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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 present invention discloses a kind of two ferrous selenide nanometer sheet materials and preparation method thereof for energy storage devices such as lithium ion batteries.Two ferrous selenide nanometer sheets synthesize a step solvent-thermal method, are not necessarily to template and surfactant.Two ferrous selenide of nanometer sheet of synthesis is as negative electrode material and lithium piece as cathode assembling at lithium ion half-cell, test structure is shown, the nano-electrode material is under the multiplying power of 1C, initial capacity is up to 400mAh/g after recycling third circle, its first circle coulombic efficiency is up to 78.23%, and in 250 circle of circulation, coulombic efficiency is close to 100%, and there is good cyclical stability, and its internal resistance is only 2.6 ohm.Two ferrous selenides nanometer sheet negative electrode material prepared by the present invention is with good performance, and preparation method is easy to operate, environmentally protective, and low cost is conducive to industrialization.
Description
Technical field
The invention belongs to nano materials and energy field, and in particular to a kind of negative electrode material of lithium ion battery.
Background technique
With economic growth, the energy crisis and problem of environmental pollution of 21 century is increasingly serious, in order to meet us not
The energy demand come, it should clean energy resource is developed to substitute traditional fossil fuel, for example, solar energy, wind energy, nuclear energy, biology
The novel environmentally friendly energy such as energy and tide energy.However these novel energy are unstable, can not directly for used in the people,
Energy storage device is needed to store conversion output be stable can be the energy that people directly use.Rechargeable lithium ion batteries because
Its high-energy density, long circulation life and environment friendly are studied and apply extensively.
The further development of lithium ion battery depends on searching and is significantly better than cobalt acid lithium yin applied currently on the market
The material of pole and graphite anode.In 2000, it has been found that transition metal oxide (iron oxide, nickel oxide, tin oxide and oxidation
Cobalt etc.) reversible electrochemical reaction can occur with lithium metal, and theoretical specific capacity is much higher than the theoretical specific capacity of graphite
(372mAh/g), wherein the theoretical specific capacity of iron oxide is up to 1000mAh/g or so, and therefore, transition metal oxide is expected to replace
Become next-generation lithium ion battery negative material for graphite-based negative electrode material.Although there is transition-metal oxide to have high specific volume
Amount, but its initial irreversible capacity is big and electronic conductivity is low.Transition metal selenides has higher than transition metal oxide
Conductivity, or even there is metalline, this characteristic is very beneficial for it applied to lithium ion battery material, is expected to become new
The lithium ion battery negative material of a generation haveing excellent performance.
Currently, transition metal selenides is in superconduction, photoelectric device, catalysis, fuel sensitization solar battery and super electricity
The fields such as container are widely used, and two ferrous selenides rely on its extensive source of iron reserves and the cost of lower synthesis more
Cause the concern of researcher, but it is still less in terms of the research in terms of lithium battery.The present invention, which designs one kind, can be used for
Two ferrous selenide nanometer sheets of lithium ion battery negative material have high specific capacity and high rate performance, be a kind of excellent lithium from
Sub- cell anode electrodes material.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of two ferrous selenides for lithium ion battery negative material to receive
Rice piece and preparation method, the lithium ion battery negative material that the present invention is prepared have high specific capacity and high rate performance；
Preparation method is simple, and process is short, does not need complex device, low in cost, is conducive to industrialization.
The present invention provides a kind of two ferrous selenide nanometer sheet materials for lithium ion battery negative material, the nanometer sheet is thick
Degree be about 10 ~ 50nm, length and width are about 5 ~ 20 μm, and in the nanometer sheet it is irregular be scattered with it is tiny.
Further, the two ferrous selenides nanometer sheet, shows excellent cycle performance in lithium ion battery, the nanometer
Piece is used as the negative electrode material of lithium ion battery, and under the multiplying power of 1C, initial capacity is first up to 400mAh/g after recycling third circle
Circle coulombic efficiency is up to 78.23%, recycles in 250 circles, and coulombic efficiency has good cyclical stability close to 100%, and its
Internal resistance is only 2.6 Ω.
The present invention also provides the preparation methods of two ferrous selenide nanometer sheets of above-mentioned lithium ion battery negative material, comprising:
(1) selenium powder and source of iron are added in ptfe autoclave according to the ratio of molar ratio 1:1；
(2) the Standard entertion ethanol amine of 12 ~ 18mL is added according to every 1mmol selenium powder
As reducing agent, magnetic agitation is to being uniformly mixed；
(3) aforesaid reaction vessel is placed at 120 DEG C -200 DEG C and keeps the temperature 8-24h, progress solvent thermal reaction, natural cooling, obtain-molten
Agent hot；
(4) the obtained product of (3) step is used into deionized water and ethyl alcohol eccentric cleaning several times respectively, obtains two after vacuum drying
Ferrous selenide nanometer sheet.
Source of iron is FeSO in the step (1)47H20.
The method of two ferrous selenide nanometer sheets of preparation of the invention further includes following preferred embodiment:
Ethanol amine adds the Standard entertion of 12mL according to every 1mmol selenium powder in preferred scheme.
The magnetic agitation time is 0.5h in preferred scheme.
Solvent thermal reaction temperature is 160 ~ 180 DEG C in preferred scheme.
The solvent thermal reaction time is 8 ~ 12h in preferred scheme.
The beneficial achievement of invention is:
(1) the two ferrous selenide nanometer sheet materials for lithium ion battery that method of the invention is prepared, apparent colour are black
Color or taupe, chemical stability is good, and the high conductivity characteristic with transition metal selenides, is conducive to electrode material electricity
The transmitting of lotus can become excellent lithium ion battery negative material.
(2)) the two ferrous selenide nanometer sheet materials for supercapacitor that method of the invention is prepared, not only have
High specific surface area and good conductivity, and the lithium ion battery prepared has good cyclical stability and excellent multiplying power
Performance.
(3) method that the present invention uses solvent-thermal process, source of iron is cheap and easy to get, at low cost, and the technological operation is simple, stream
Journey is short, and synthesis temperature is low, and the time is short, environmentally protective, is conducive to industrialization.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) figure of two ferrous selenide nanometer sheets prepared by the embodiment of the present invention 1.
Fig. 2 is two ferrous selenide nanometer sheet XRD diagram prepared by the embodiment of the present invention 1.
Fig. 3 is the cycle performance figure of two ferrous selenide nanometer sheets prepared by the embodiment of the present invention 1.
Fig. 4 is the charging and discharging curve figure of two ferrous selenide nanometer sheets prepared by the embodiment of the present invention 1.
Fig. 5 is the ac impedance spectroscopy of two ferrous selenide nanometer sheets prepared by the embodiment of the present invention 1.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated, is best understood from this hair with those skilled in the art
It is bright, but the present invention is not limited to following embodiment.
Embodiment 1
Raw material 2.5mmol selenium powder, 2.5mmol green vitriol are placed in 50mL ptfe autoclave, are added
Magnetic agitation 0.5h obtains uniform mixed solution to 30mL ethanol amine at room temperature, and polytetrafluoroethyllining lining is packed into the anti-of stainless steel
It answers in kettle and seals, the reaction kettle is then placed in baking oven progress solvent-thermal process reaction, reaction temperature is 160 DEG C, when reaction
Between be 12 hours, cool to room temperature with the furnace, with ethyl alcohol and deionized water difference eccentric cleaning three times after, dry 12 is small at 60 DEG C
When obtain final two selenizing ferrum nano material of product.
Embodiment 2
Raw material 2.5mmol selenium powder, 2.5mmol green vitriol are placed in 50mL ptfe autoclave, are added
Magnetic agitation 0.5h obtains uniform mixed solution to 30mL ethanol amine at room temperature, and polytetrafluoroethyllining lining is packed into the anti-of stainless steel
It answers in kettle and seals, the reaction kettle is then placed in baking oven progress solvent-thermal process reaction, reaction temperature is 140 DEG C, when reaction
Between be 12 hours, cool to room temperature with the furnace, with ethyl alcohol and deionized water difference eccentric cleaning three times after, dry 12 is small at 60 DEG C
When obtain final two selenizing ferrum nano material of product.
Embodiment 3
Raw material 2.5mmol selenium powder, 2.5mmol green vitriol are placed in 50mL ptfe autoclave, are added
Magnetic agitation 0.5h obtains uniform mixed solution to 30mL ethanol amine at room temperature, and polytetrafluoroethyllining lining is packed into the anti-of stainless steel
It answers in kettle and seals, the reaction kettle is then placed in baking oven progress solvent-thermal process reaction, reaction temperature is 120 DEG C, when reaction
Between be 24 hours, cool to room temperature with the furnace, with ethyl alcohol and deionized water difference eccentric cleaning three times after, dry 12 is small at 60 DEG C
When obtain final two selenizing ferrum nano material of product.
Embodiment 4
Raw material 2.5mmol selenium powder, 2.5mmol green vitriol are placed in 50mL ptfe autoclave, are added
Magnetic agitation 0.5h obtains uniform mixed solution to 30mL ethanol amine at room temperature, and polytetrafluoroethyllining lining is packed into the anti-of stainless steel
It answers in kettle and seals, the reaction kettle is then placed in baking oven progress solvent-thermal process reaction, reaction temperature is 200 DEG C, when reaction
Between be 8 hours, cool to room temperature with the furnace, with ethyl alcohol and deionized water difference eccentric cleaning three times after, dry 12 is small at 60 DEG C
When obtain final two selenizing ferrum nano material of product.
Embodiment 5
Raw material 2.5mmol selenium powder, 2.5mmol green vitriol are placed in 50mL ptfe autoclave, are added
Magnetic agitation 0.5h obtains uniform mixed solution to 45mL ethanol amine at room temperature, and polytetrafluoroethyllining lining is packed into the anti-of stainless steel
It answers in kettle and seals, the reaction kettle is then placed in baking oven progress solvent-thermal process reaction, reaction temperature is 140 DEG C, when reaction
Between be 12 hours, cool to room temperature with the furnace, with ethyl alcohol and deionized water difference eccentric cleaning three times after, dry 12 is small at 60 DEG C
When obtain final two selenizing ferrum nano material of product.
Performance test:
1) SEM is tested: the various embodiments described above being prepared finally obtained sample and are observed under a scanning electron microscope.Fig. 1 is real
Sample microscopic appearance made from example 1 is applied, there it can be seen that the nanometer sheet thickness is uniform, but not of uniform size, nanometer sheet thickness is about
10 ~ 50nm, length and width are about 5 ~ 20 μm, and irregular in the nanometer sheet are scattered with tiny nano particle.
2) XRD is tested: the various embodiments described above being prepared finally obtained sample and carry out XRD test, if Fig. 2 is embodiment 1
Obtained sample X-ray diffractogram, X-Ray map show that two ferrous selenides of solvent-thermal process are rhombic system, embodiment sample
The diffraction maximum of product and the characteristic peak of the PDF card (79-1892) of two ferrous selenides are corresponding one by one, and embodiment is without other diffraction
Peak illustrates that product is two ferrous selenides of pure phase.
3) electrochemical property test: the lithium-ion electric that two ferrous selenide nanometer sheet materials made from the various embodiments described above are assembled
The test of pond progress chemical property.
The lithium ion half-cell process of two ferrous selenides nanometer sheet composition prepared by the present invention is as follows, and two ferrous selenides of preparation are received
Rice piece and super p and polyvinylidene fluoride are ground according to mass ratio for 7:2:1 and the mixing of suitable N-N dimethyl pyrrolidone
It is ground to no granular sensation, is uniformly coated on copper foil, 12h is dried in vacuo, the copper foil dried is cut into each diameter with tablet press machine
For the sequin of 16mm, then load capacity 1-1.5mg/cm2 assembles lithium ion battery in glove box again.Using micropore poly- third
Alkene film is as diaphragm, the LiPF6(ethylene carbonate of 1M: dimethyl carbonate=1:1 volume ratio) it is used as electrolyte, lithium metal is
To electrode.After assembled battery places 12h, chemical property, voltage range 0.1 are tested with blue electricity and electrochemical workstation
~3V。
Such as the cycle performance figure obtained under multiplying power of the attached drawing 3 for sample 1C made from embodiment 1；Fig. 4 is made for embodiment 1
Sample at 1C before the charging and discharging curve that recycles three times, the platform of apparent charge and discharge as we can see from the figure；In times of 1C
Under rate, for initial capacity up to 400mAh/g, first circle coulombic efficiency is up to 78.23% after recycling third circle, recycles in 250 circles,
Coulombic efficiency has good cyclical stability close to 100%.
Fig. 5 is the AC impedance figure of sample made from embodiment 1, it can be deduced that material resistance is only 2.6 ohm, is shown
The good electric conductivity of material.
Claims (5)
1. a kind of two ferrous selenide nanometer sheets for lithium ion battery negative material, it is characterised in that: the two ferrous selenides nanometer
Piece, thickness about 10 ~ 50nm, length and width are between 5 ~ 20 μm；And irregular in the nanometer sheet it is scattered with tiny nano particle.
2. a kind of two ferrous selenide nanometer sheets for lithium ion battery negative material according to claim 1, feature exist
In: under the multiplying power of 1C, initial capacity reaches 400mAh/g after recycling third circle, and first circle coulombic efficiency is up to 78.23%；250 circle of circulation
Interior, for coulombic efficiency close to 100%, internal resistance is 2.6 ohm.
3. preparing a kind of two ferrous selenide nanometers for lithium ion battery negative material described in any one of claims 1 to 2
Piece, it is characterised in that comprise the following steps that
1) selenium powder and source of iron are added in ptfe autoclave；1:1 is added in molar ratio for selenium powder and source of iron；
2) ethanol amine is continuously added in reaction kettle as reducing agent, is stirred to uniformly mixed；According to every 1mmol selenium powder addition 12 ~
The Standard entertion ethanol amine of 18mL；
3) aforesaid reaction vessel is placed in baking oven, carries out solvent thermal reaction；
4) reaction product uses deionized water and ethyl alcohol eccentric cleaning three times respectively, and dry 12-24h, obtains described two at 60 DEG C
Ferrous selenide nanometer sheet.
4. a kind of preparation method of the two ferrous selenide nanometer sheets for lithium ion battery negative material according to claim 3,
It is characterized by: source of iron is FeSO in the step 1)47H20。
5. a kind of preparation method of the two ferrous selenide nanometer sheets for lithium ion battery negative material according to claim 3,
It is characterized by: solvent thermal reaction temperature is 120 DEG C -200 DEG C in the step 3), reaction time 8-24h.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113991185A (en) * | 2021-10-29 | 2022-01-28 | 世一国际新能源有限公司 | Energy storage lithium ion battery based on nano electrode and preparation method thereof |
| CN113991062A (en) * | 2021-10-29 | 2022-01-28 | 世一国际新能源有限公司 | High-capacity energy storage lithium ion battery and preparation method thereof |
| CN114368765A (en) * | 2021-08-20 | 2022-04-19 | 山东泰普锂业科技有限公司 | Morphology control process and method of lithium carbonate nanosheet with smooth surface for lithium supplement of positive electrode in lithium ion battery |
| CN114671414A (en) * | 2022-03-25 | 2022-06-28 | 浙江大学 | Iron-copper-tin ternary selenide nano material for sodium ion battery and preparation method thereof |
| CN114725351A (en) * | 2022-04-29 | 2022-07-08 | 信阳师范学院 | Alkaline battery negative electrode material and preparation method thereof |
| US11600453B1 (en) * | 2022-01-25 | 2023-03-07 | University Of Sharjah | All transition metal selenide composed high-energy solid-state hybrid supercapacitor |
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| CN105060261A (en) * | 2015-09-23 | 2015-11-18 | 广东工业大学 | Method for preparing ferrum diselenide self-assembled microflowers |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114368765A (en) * | 2021-08-20 | 2022-04-19 | 山东泰普锂业科技有限公司 | Morphology control process and method of lithium carbonate nanosheet with smooth surface for lithium supplement of positive electrode in lithium ion battery |
| CN114368765B (en) * | 2021-08-20 | 2023-09-22 | 山东泰普锂业科技有限公司 | Morphology control method of smooth-surface lithium carbonate nanosheets for lithium supplementing of positive electrode in lithium ion battery |
| CN113991185A (en) * | 2021-10-29 | 2022-01-28 | 世一国际新能源有限公司 | Energy storage lithium ion battery based on nano electrode and preparation method thereof |
| CN113991062A (en) * | 2021-10-29 | 2022-01-28 | 世一国际新能源有限公司 | High-capacity energy storage lithium ion battery and preparation method thereof |
| US11600453B1 (en) * | 2022-01-25 | 2023-03-07 | University Of Sharjah | All transition metal selenide composed high-energy solid-state hybrid supercapacitor |
| CN114671414A (en) * | 2022-03-25 | 2022-06-28 | 浙江大学 | Iron-copper-tin ternary selenide nano material for sodium ion battery and preparation method thereof |
| CN114725351A (en) * | 2022-04-29 | 2022-07-08 | 信阳师范学院 | Alkaline battery negative electrode material and preparation method thereof |
| CN114725351B (en) * | 2022-04-29 | 2024-02-27 | 信阳师范学院 | Alkaline battery cathode material and preparation method thereof |
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