CN108933257A - Cu as lithium ion battery electrode material2-xSe nano material and preparation method thereof - Google Patents
Cu as lithium ion battery electrode material2-xSe nano material and preparation method thereof Download PDFInfo
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- CN108933257A CN108933257A CN201811010049.XA CN201811010049A CN108933257A CN 108933257 A CN108933257 A CN 108933257A CN 201811010049 A CN201811010049 A CN 201811010049A CN 108933257 A CN108933257 A CN 108933257A
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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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- 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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- 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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- 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
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- 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
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Abstract
The present invention discloses a kind of copper selenide nanometer material and preparation method thereof as lithium ion battery electrode material, which is flake nano structure.The Cu2‑xSe nano material uses the synthetic method of a step hydro-thermal, with SeO2For selenium source, CuCl2·2H2O is copper source, a step hydrothermal synthesis Cu2‑xSe.The Cu of preparation2‑xSe nano material shows the characteristic that structural purity is high, pattern is uniform, granule size is different.It is assembled into lithium ion battery in this, as electrode material, carries out electrochemical property test, initial specific capacities beginning specific capacity is up to 345.75mAh/g, and very close theoretical value 376mAh/g, Charge-transfer resistance can be down to 1.32 Ω/cm2.Copper selenide nano-electrode material prepared by the present invention has the characteristics that specific capacitance is high, impedance is low, preparation method is simple, at low cost.
Description
Technical field
The present invention relates to lithium ion battery electrode material more particularly to the electrodes of the selenides lithium ion battery of nanostructure
Material Field.
Background technique
In recent years, with the appearance of the energy conservation measure of reply global warming, secondary cell, fuel cell, supercapacitor
Etc. new energy resources systems be expected to be used for reduce CO2 emission.In particular, traffic and transportation sector accounts for the 24% of energy consumption, dioxy
Change the 20% of carbon emission amount, lead, nickel-metal hydride battery have been applied to mixed power electric car (Hev) and electric car (EV).Secondary electricity
The energy of lithium ion battery and power density highest in pond, be in the secondary battery it is most light, therefore, lithium ion battery is suitable for
For the power source of the vehicles such as electric vehicle, car, energy-saving effect can be improved using secondary cell on railway.Chargeable lithium
Ion battery (LIB) with its energy density height, is followed as most promising one of electrochemical energy conversion/memory device
The features such as ring is good, memory-less effect, low self-discharge, high security, in various portable electronic products and emerging electronic vapour
It is widely used in vehicle.But high-energy, high power density, long circulation life and low manufacturing cost lithium-ion electric
Pond is just becoming higher and higher and traditional graphite-based material and has been unable to meet people to compel high-energy density and extensive energy storage
It highly necessary asks, because its theoretical capacity is low.Therefore, new anode material is found to replace graphite to become urgent.
In this respect, copper chalcogenide is due to its low cost, good electric conductivity and high capacity and be considered as have it is uncommon
The candidate of prestige.And it is also fresh to attempt using selenides as electrode material, recently it is found that CuxSey(copper-based selenides) is in electricity
All there is advantage, it will be a kind of very promising lithium ion battery electrode material on capacity and electric conductivity.The selenium of nanostructure
Change copper due to large specific surface area, pore structure abundant and be capable of increasing the advantages such as its capacitance and be particularly subject to researcher
Favor.In the case where electrode material composition is selected, reasonable structure design can effectively improve the electrochemistry of electrode
Performance, for example obtain higher specific surface area and can increase the contact area of electrode active material and electrolyte, thus effectively
The utilization rate for improving active material, then improves energy density.In addition seek the electrode material preparation of low cost, methods simplification
Method, the industrialization for lithium ion battery are also very necessary.
Bibliography:
[1] H. Ozawa and T. Ogihara, Running Test of Contact wireless Tramcar
Using Lithium Ion Battery, IEEJ Trans Elec Electron Eng, 2008, 3, 360-362.
[2] W. Wang, I. Ruiz, K. Ahmed, H. H. Bay, A. S. George, J. Wang, J.
Butler, M. Ozkan, and C. S. Ozkan, Silicon Decorated Cone Shaped Carbon
Nanotube Clusters for Lithium Ion Battery Anodes, Small, 2014, 10, 3389-3396.
[3] Z.H. Wang, Q. Sha, F.W. Zhang, J. Pu and W. Zhang, Synthesis of
polycrystalline cobalt selenide nanotubes and their catalytic and capacitive
behaviors, CrystEngComm, 2013, 15, 5928–5934。
Summary of the invention
A kind of exploration of lithium ion battery electrode material as excellent properties, the present invention is directed to micro- by reasonable material
Structure design realizes Cu using a kind of easy to operate, inexpensive preparation method2-xSe nanometers of multidimensional structure, it is effective to improve
The specific surface area and space utilization rate of electrode material, to promote the specific capacity and electric conductivity of electrode material.
The present invention provides a kind of Cu as lithium ion battery electrode material2-xSe nano material, the Cu2-xSe nanometers
Material is regular laminated structure, and single nanoscale twins are interlaced and form the laminated structure intensively reunited, with hexagon sheet
It is collected as rolling into a ball for unit, the sheet subunit structure that layer that is thin and folding interweaves is towards different.The present invention passes through reasonable material
Microstructure design, and the nanostructure being realized to, the nanostructure of multidimensional increases the ratio of electrode using feasible preparation method
The attaching space of surface area and electrode material and electrolyte reaches the effect of the electric conductivity and specific capacity that effectively improve electrode material
Fruit.
Further, the Cu2-xThe nanometer sheet thickness of Se nano material is between 90~150nm.
Further, the Cu2-xThe diameter of Se nano lamellar material is several hundred nanometers to several microns.The diameter of nanometer sheet
Control, cladding thickness on a current collector and specific surface area, cover when being directly related to the material as lithium ion cell electrode
The increase of lid thickness and specific surface area directly increases the load thickness of electrode active material, this will undoubtedly improve electrode material
Electric conductivity can play remarkable result for improving lithium ion battery specific capacity.
The present invention also provides prepare above-mentioned Cu2-xThe method of Se nano material, includes the following steps:
With SeO2For selenium source, CuCl2·2H2O is copper source, using the method for a step hydrothermal synthesis.By raw material SeO2、CuCl2·
2H2O is dissolved in deionized water, stirs evenly be placed in reaction kettle at room temperature, is later added to reducing agent molten in reaction kettle
In liquid, then the reaction kettle is placed in baking oven and carries out hydrothermal synthesis reaction, obtains Cu2-xSe powder, after water, ethyl alcohol rinse,
It is collected by filtration, up to Cu after drying2-xSe nano material.
Further, the temperature that reaction kettle carries out hydrothermal synthesis reaction in an oven in step is 160 DEG C, and the reaction time is
8-12 hours.Reaction time is directly related to the control to form nanotopography.Time is too short, and nanometer sheet forming amount is very few, and straight
Diameter is smaller, cannot reach the loading demand for meeting active material of lithium ion battery electrode；And the reaction time is too long, nanometer sheet knot
Structure can also change, and size significantly increases, to reduce specific surface area.
Further, in step in raw material, reducing agent is hydrazine hydrate, and hydrazine hydrate, copper chloride dihydrate, SeO2And deionization
The usage ratio strict control of water is 2mL:1mmol:1mmol:30mL.The proportion of these three raw materials is controlled, can just grow needs
The Cu wanted2-xThe nanotopography of Se nano material and needs and guarantee are subsequently formed the bigger serface structure electricity of high-energy density
Pole material.
Further, drying procedure is in step, dries 4 hours for 80 DEG C in air.
Further, the above-mentioned Cu of the present invention2-xSe nano material is applied in lithium ion battery as electrode material, in lithium
In the test of ion battery cycle performance, initial specific capacities can reach 345.75mAh/g, close to its theoretical specific capacity (376mAh/
G), there is very high specific capacity, also there is low Charge-transfer resistance, test value can be down to 1.32 Ω/cm2。
Beneficial achievement of the invention is:
1) present invention is designed by reasonable material microstructure, and the preparation method that use is easy to operate, inexpensive realizes Cu2-xSe
The multidimensional structure of nano material, Cu obtained2-xThe distribution of Se nano material is fine and close, nanometer sheet diameter in several hundred nanometers to several micro-
Rice, nanometer sheet is interlaced and forms the laminated structure intensively reunited, structural purity is high, pattern is uniform, granule size is different and
Stepped distribution provides excellent channel for the diffusion and migration of ion, also can increase the ratio of the nano structure electrode
The attaching space of surface area and electrode material and electrolyte reaches the effect of the electric conductivity and specific capacity that effectively improve electrode material
Fruit.
2) Cu prepared by the present invention2-xSe nano material is shown in the electro-chemical test for being applied to lithium ion battery
Initial specific capacities, in cycle performance of lithium ion battery test, initial specific capacities can reach 345.75mAh/g, wherein theoretical
Specific capacity is 376mAh/g, has extraordinary specific capacity；It has also been found that Charge-transfer resistance can when carrying out testing impedance to it
Down to 1.32 Ω/cm2, ion-diffusibility is strong.
3) method that the present invention uses a step hydrothermal synthesis, raw material is easy to get, equipment cost is low, easy to operate, is very suitable to
In industrialized batch production.
3) present invention is with SeO2For selenium source, CuCl2·2H2O is copper source, using the method for a step hydrothermal synthesis.Raw material is easy
, equipment cost it is low, easy to operate, preparation method is very simple and economical and practical, is very suitable for industrialized batch production.
Detailed description of the invention
Fig. 1 is Cu made from embodiment 12-xScanning electron microscope (SEM) figure of Se nanometer sheet.
Fig. 2 is Cu made from embodiment 22-xScanning electron microscope (SEM) figure of Se nanometer sheet.
Fig. 3 is Cu made from embodiment 12-xTransmission electron microscope (TEM) figure of Se nano material.
Fig. 4 is Cu made from embodiment 22-xTransmission electron microscope (TEM) figure of Se nano material.
Fig. 5 is Cu made from embodiment 12-xThe X-ray diffraction (XRD) figure of Se nano material.
Fig. 6 is Cu made from embodiment 22-xThe X-ray diffraction (XRD) figure of Se nano material.
Fig. 7 is Cu made from embodiment 12-xThe CV curve of Se nano material.
Fig. 8 is Cu made from embodiment 22-xThe CV curve of Se nano material.
Fig. 9 is Cu made from embodiment 12-xThe cyclic curve of Se nano material.
Figure 10 is Cu made from embodiment 22-xThe cyclic curve of Se nano material.
Figure 11 is Cu made from embodiment 1,22-xThe EIS curve of Se nano material.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
(1) in 100ml polytetrafluoroethylene (PTFE) autoclave (pre-add 30mL deionized water), addition 1mmol copper chloride dihydrate,
1mmolSeO2, 2ml hydrazine hydrate makees reducing agent.
(2) it was stirred by ultrasonic by 10 minutes, reaction kettle is sealed in stainless steel autoclave, 160 DEG C of progress hydro-thermal reactions, is protected
It holds 8 hours.
(3) cooled to room temperature, product are collected by filtration after water, ethyl alcohol rinse, and dry 4 hours at 80 DEG C to get arriving
Target product.
Embodiment 2
(1) in 100ml polytetrafluoroethylene (PTFE) autoclave (pre-add 30mL deionized water), addition 1mmol copper chloride dihydrate,
1mmolSeO2, 2ml hydrazine hydrate makees reducing agent.
(2) it was stirred by ultrasonic by 10 minutes, reaction kettle is sealed in stainless steel autoclave, 160 DEG C of progress hydro-thermal reactions, is protected
It holds 12 hours.
(3) cooled to room temperature, product are collected by filtration after water, ethyl alcohol rinse, and dry 4 hours at 80 DEG C to get arriving
Target product.
Performance test:
1) SEM is tested: by Cu made from the various embodiments described above preparation step2-xSe nanometer sheet is seen under SEM scanning electron microscope
It examines, it can be seen that the powder of acquisition is that sample is agglomerating with bulk aggregation, and most of nanometer blocks particle is smaller, looks under Electronic Speculum
The most of powder arrived regular lamellar growth, the group of being collected as unit of hexagon sheet, to advantageously form high energy
The bigger serface structure electrode material of metric density.If attached drawing 1 is Cu made from embodiment 12-xThe scanning electron microscope of Se nanometer sheet
(SEM) figure；Fig. 2 is Cu made from embodiment 22-xScanning electron microscope (SEM) figure of Se nanometer sheet.Cu2-xSe nano material is shown
Purity is high, pattern is uniform, granule size is different and the characteristic of distribution gradient.Cu2-xThe nanometer sheet thickness of Se nano material is 90
Between~150nm, diameter is several hundred nanometers to several microns.Sheet subunit structure that layer that is thin and folding interweaves and towards each
It is different.
2) TEM is tested: by Cu made from the various embodiments described above preparation step2-xSe nanometer sheet at transmission electron microscope (TEM) into
Row observation, acceleration voltage 200kV, it can be seen that even across decentralized processing, powder sample also has reunion and stacks phenomenon.
Under transmission electron microscope it can be seen that powder sample sample random display it is thin and fold layer interweave sheet subunit structure and court
To different, granularity is simultaneously uneven, but pattern meets Cu2-xThe characteristics of S hexagonal phase.Attached drawing 3 is Cu made from embodiment 12-xSe receives
Transmission electron microscope (TEM) figure of rice material；Fig. 4 is Cu made from embodiment 22-xTransmission electron microscope (TEM) figure of Se nano material.
3) XRD is tested: by the final Cu obtained of the various embodiments described above preparation step2-xSe nano material carries out X-ray diffraction
(XRD) it tests, XRD test uses the K of CuaLine (λ=1.5406) is used as x-ray source, and test angle is 5 ° -85 °.Attached drawing 5,
Fig. 6 is respectively Cu made from embodiment 1,22-xThe X-ray diffractogram that Se nanometer sheet sample test obtains, the XRD diffraction maximum of sample
It can explicitly indicate that as Cu2-xThe hexagonal phase (JCPDS number 06-0680) of Se is strong at 2 θ=26.7 °, 44.6 ° and 52.9 °
Diffraction maximum can clearly belong to Cu respectively2-x(111), (220) and (311) face of Se.It therefore deduces that, two embodiments
Nano material is by pure Cu2-xSe phase composition.
4) CV is tested: by the last Cu obtained of the various embodiments described above2-xLithium ion cell electrode is respectively prepared in Se nano material
Piece is simultaneously assembled into progress cyclic voltammetry test after complete battery, and voltage range is 0.01V ~ 3V, rate 0.5mV/s.Such as
Fig. 7, Fig. 8 are respectively Cu made from embodiment 1,22-xThe CV curve of Se nano material.Reduction peak at 1.90V and 1.40V can
It is attributed to from Cu2-xSe to LixCu2-xThe phase transformation of Se, is then further converted into Cu2Se.And the broad peak centered on 0.60 V
It is related with the formation of solid electrolyte interface (SEI) film with weak peak.
5) cycle performance is tested: by Cu made from the various embodiments described above2-xLithium ion battery battery is respectively prepared in Se nano material
Pole piece is simultaneously assembled into progress cycle performance test after complete battery, the Cu as made from the respectively embodiment 1,2 of attached drawing 9,102- xThe cyclic curve of Se nano material, Cu made from embodiment 12-xSe nano material initial charge specific capacity and specific discharge capacity point
Not Wei 291.5mAh/g and 345.75mAh/g, starting efficiency 84.3%, Cu made from embodiment 22-xSe nano material is initially filled
Electric specific capacity and specific discharge capacity are respectively 124.5mAh/g and 122.25mAh/g, starting efficiency 45.5%.
6) ac impedance spectroscopy is tested: by Cu made from the various embodiments described above2-xLithium ion battery is respectively prepared in Se nano material
Electrode slice is simultaneously assembled into progress electrochemical alternate impedance spectrum test after complete battery, as shown in Fig. 11, for the system of embodiment 1,2
The Cu obtained2-xThe AC impedance spectroscopy of Se nano material electrode, illustration are model of fit.From the figure, it can be seen that hydrothermal synthesis
Sample has small charge transfer resistance, can be down to 1.32 Ω/cm2。
Claims (7)
1. a kind of Cu as lithium ion battery electrode material2-xSe nano material, it is characterised in that: the Cu2-xSe nanometers of materials
Material is regular laminated structure, and single nanoscale twins are interlaced and form the laminated structure intensively reunited, and is with hexagon sheet
Unit is collected as rolling into a ball, the sheet subunit structure that layer that is thin and folding interweaves and towards different.
2. a kind of Cu as lithium ion battery electrode material according to claim 12-xSe nano material, feature exist
In: the Cu2-x90~150nm of thickness of the hexagon piece of Se nano material, diameter is in several hundred nanometers between several microns.
3. preparing a kind of Cu as lithium ion battery electrode material described in any one of claims 1 to 22-xSe nanometers of materials
The method of material, it is characterised in that: with SeO2For selenium source, CuCl2·2H2O is copper source, using the method for a step hydrothermal synthesis, including
Following steps, by raw material SeO2、CuCl2·2H2O is dissolved in deionized water, stirs evenly be placed in reaction kettle at room temperature, later
Reducing agent is added in the solution in reaction kettle, then the reaction kettle is placed in baking oven and carries out hydrothermal synthesis reaction, is obtained
Cu2-xSe powder is collected by filtration after water, ethyl alcohol rinse, up to Cu after drying2-xSe nano material.
4. according to a kind of Cu as lithium ion battery electrode material of claim 32-xThe preparation method of Se nano material, it is special
Sign is: the temperature that reaction kettle carries out hydrothermal synthesis reaction in an oven is 160 DEG C, and the reaction time is 8-12 hours.
5. according to a kind of Cu as lithium ion battery electrode material of claim 32-xThe preparation method of Se nano material, it is special
Sign is: in the feed, reducing agent is hydrazine hydrate, and hydrazine hydrate, copper chloride dihydrate, SeO2It is tight with the usage ratio of deionized water
Lattice control is 2mL:1mmol:1mmol:30mL.
6. according to a kind of Cu as lithium ion battery electrode material of claim 32-xThe preparation method of Se nano material, it is special
Sign is: the drying is dried 4 hours for 80 DEG C in air.
7. according to Cu made from any one of claim 3 to 6 preparation method2-xSe nano material is in lithium ion cell electrode
Application in material, it is characterised in that: the Cu2-xIn performance of lithium ion battery test, initial specific capacities reach Se nano material
To 345.75mAh/g, Charge-transfer resistance is down to 1.32 Ω/cm2。
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| CN112700967A (en) * | 2020-11-30 | 2021-04-23 | 电子科技大学 | Cu with high specific capacity2-xNegative electrode material of Se super capacitor |
| CN113086953A (en) * | 2021-04-20 | 2021-07-09 | 郑州大学 | KCu4Se8Preparation and application of nano-rod |
| CN114039046A (en) * | 2021-11-02 | 2022-02-11 | 远景动力技术(江苏)有限公司 | Sodium ion battery and preparation method thereof |
| CN114122388A (en) * | 2021-11-16 | 2022-03-01 | 信阳师范学院 | CuSe nano material for sodium ion battery and preparation method thereof |
| CN115548287A (en) * | 2022-09-14 | 2022-12-30 | 武汉大学 | Negative electrode active material, zinc ion battery and electronic device |
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