CN107799742A - A kind of lithium battery load porous carbon negative pole material of silicon bio-based N doping and preparation method thereof - Google Patents
A kind of lithium battery load porous carbon negative pole material of silicon bio-based N doping and preparation method thereof Download PDFInfo
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- CN107799742A CN107799742A CN201710899887.6A CN201710899887A CN107799742A CN 107799742 A CN107799742 A CN 107799742A CN 201710899887 A CN201710899887 A CN 201710899887A CN 107799742 A CN107799742 A CN 107799742A
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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
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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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- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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 lithium battery load porous carbon negative pole material of silicon bio-based N doping and preparation method thereof.It is using bio-based N doping porous carbon as carrier, and, the specific surface area of the bio-based N doping porous carbon is 100~3000 m by monocrystalline silicon nanometer particle load on this carrier2/ g, nitrogen element content are 0.1~10.0 wt.%.The present invention upsets carbon atom ∏ conjugated electron systems by using the porous carbon materials rich in a large amount of N elements, there is provided bigger electrochemical surface area and avtive spot, collaboration promote electric charge transfer between carbon atom and hetero atom, lift carbon layer material conductance and specific capacity;Monocrystalline silicon nano used is semi-conducting material; poorly conductive itself; and porous carbon materials can be used as excellence conductor; the present invention is by monocrystalline silicon nanometer particle load on bio-based N doping porous carbon support; substantially increase electric conductivity; because its preparation technology is simple, be advantageous to large-scale production application.
Description
Technical field
The present invention relates to new energy battery material technical field, specifically a kind of lithium battery load silicon bio-based N doping
Porous carbon negative pole material and preparation method thereof.
Background technology
Different from the traditional energy based on fossil energy, with solar energy, geothermal energy, wind energy etc. for representative new energy in work(
There is larger randomness with intermittent in rate output, be otherwise known as the intermittent renewable energy.It is above-mentioned renewable in order to realize
Grid-connected application, energy stores and the conversion of the energy, growth-promoting is using safe efficient, environment-friendly secondary cell system as label
Chemical energy storage technology by academia extensive concern and Innovation Input.Wherein, lithium ion battery is because capacity is big, operating voltage
It is high, self discharge is low, it is safe, have extended cycle life, small volume, it is in light weight, than can high, memory-less effect, a not leaded mercury huge sum of money
Category etc. activity beneficial, firmly occupy the existing market principal status of public economy, be widely used in Aero-Space, communications and transportation, household electrical appliances, office,
The fields such as mobile communication.Current commercial li-ion battery embedded type graphite-like carbon negative pole material specific capacity is low(372 mAh·g-1),
It can not meet in the high-power high-current device requirement such as electric automobile, ship, electric tool.Therefore, Fabrication of High Specific Capacitance of new generation is explored
Amount, high-energy-density, the negative material of high circulation life-span and high rate performance have become study hotspot.
Silicon materials are up to 4200 mAhg because of it-1Theoretical specific capacity, 9700 mAhcm-1Volume and capacity ratio, 1.1 eV
Energy gap, 0-0.4 V operating potentials and 250 DEG C of operating temperatures, turn into most promising lithium ion battery of future generation and bear
One of pole material.In addition, silicon material resources reserve is enriched, mature preparation process, it is adapted to exploitation to be born for commercial li-ion battery
Pole material.Though silicon has many advantages, such as the above as negative material, some inevitable defects itself are still suffered from:1)Silicon is
A kind of semi-conducting material, intrinsic resistivity 2.3*105 Ω cm, dielectric constant 11.9, electrical conductivity is relatively low;2)In charge and discharge cycles
During, thus Li+ constantly embedded and abjection, silicon materials Volume Changes produce a series of problems up to 400%.Such as:Silicon
Particle crushes or Materials Fracture is so as to destroy electrode structure, conductive contact is deteriorated, causes capacity to decline.It is circulated throughout in electrochemistry
Cheng Zhong, uneven polarization caused by along the electrochemical reaction in thickness of electrode direction triggers the rupture of electrode stratiform and peeled off, and then goes out
Existing conductive network collapse and electrode failure;3)Li+Solid-electrolyte interface film is concatenated to form during insertion-abjection
(SEI), after multiple charge and discharge cycles, SEI thickness increases ultimately result in Si materials and lose electro-chemical activity, cause capacitance loss.
To solve the above problems, improving silicon materials negative material performance, C@Si composite nano materials are prepared as negative material, are being ensured
On the basis of silicon materials height ratio capacity and energy density, reduce active material cracking or peel off the electrode failure triggered, suppress SEI
Formed, increase electric conductivity, improve charge-discharge performance.In a word, around high performance lithium ion battery application demand, further
Carbon silicon-based nano negative material is designed and prepared, improves the charge-discharge performance of lithium ion battery negative material, is still that the field has
Important scientific issues to be solved.
The content of the invention
It is an object of the present invention to provide a kind of lithium battery porous carbon negative pole material of load silicon bio-based N doping and its preparation
Method, it is raw material that biomass porous carbon material, which takes natural bamboo or bamboo shoots, and preparation technology is simple, can large-scale industry metaplasia
Production, the porous carbon negative pole material of load silicon bio-based N doping being prepared have excellent chemical property.
Described a kind of lithium battery load porous carbon negative pole material of silicon bio-based N doping, it is characterised in that with bio-based
N doping porous carbon is carrier, by monocrystalline silicon nanometer particle load on this carrier, the ratio of the bio-based N doping porous carbon
Surface area is 100~3000 m2/ g, nitrogen element content are 0.1~10.0 wt.%.
A kind of described lithium battery load porous carbon negative pole material of silicon bio-based N doping, it is characterised in that bio-based nitrogen
Doping porous carbon is one or both of bamboo carbon, bamboo shoots carbon mixture.
A kind of described lithium battery load porous carbon negative pole material of silicon bio-based N doping, it is characterised in that load monocrystalline
The particle diameter of silicon nano is 5~500 nm.
The preparation method of the described lithium battery load porous carbon negative pole material of silicon bio-based N doping, it is characterised in that will
Monocrystalline silicon nano is scattered in organic solvent for ultrasonic to being uniformly dispersed, and adds bio-based N doping porous carbon and continues ultrasound,
Carry out high speed centrifugation after ultrasound structure, then wash through deionized water, lithium battery load silicon bio-based nitrogen is obtained after oven drying
Adulterate porous carbon negative pole material.
The preparation method of the described lithium battery load porous carbon negative pole material of silicon bio-based N doping, it is characterised in that have
Solvent is tetrahydrofuran.
The preparation method of the described lithium battery load porous carbon negative pole material of silicon bio-based N doping, it is characterised in that sulphur
It is 20-40 minutes, preferably 30 minutes to change molybdenum nano-particle to be scattered in the organic solvent for ultrasonic time.
The preparation method of the described lithium battery load porous carbon negative pole material of silicon bio-based N doping, it is characterised in that raw
Thing base N doping porous carbon continues ultrasonic 10-30 minutes, preferably 20 minutes.
The electrode storage lithium performance characterization method of the described lithium battery load porous carbon negative pole material of silicon bio-based N doping
It is as follows:Using the button-shaped half-cells of CR2025, the lithium battery load porous Carbon anode of silicon bio-based N doping of mass fraction 80%
Material(Abbreviation C@Si composites), 10% binding agent Kynoar, 10% conductive agent acetylene carbon black is dissolved in N- methylpyrroles
In alkanone and coated on copper foil, vacuum drying, 6 MPa, which are compressed, is used as negative pole stand-by, is lithium piece to electrode, barrier film uses poly- third
The how empty barrier film of alkene-polyethylene-polypropylene, 1M lithium hexafluoro phosphates(LiPF6)Dimethyl carbonate and ethylene carbonate by volume
1:1 prepares electrolyte, and encapsulation carries out half-cell test.
Ben Faken uses Land CT2001A(Wuhan is blue rich)Constant current charge-discharge test is carried out to battery, filled by record
The data such as time, voltage, electric current, capacity in discharge process, characterize the data such as electrode material cycle life and charge and discharge platform.
Using Arbin MSTAT4(U.S. A Bin)Cyclic voltammetry is carried out to battery(CV), it is anti-to obtain the specific electrochemistry of electrode generation
Current potential is answered, analyzes sample electrochemical reaction process and mechanism, electrochemical reaction material category is participated in auxiliary checking.Using
CHI660D(Shanghai Chen Hua)Electrochemical impedance test is carried out, to comparative sample charge transfer resistance size.
By using above-mentioned technology, compared with prior art, the present invention has following have the beneficial effect that:
1)The porous carbon raw material of bio-based N doping of the present invention is obtained, it adds by using natural bamboo or bamboo shoots by processing
Work technique is simple, and gained porous carbon materials are highly cross-linked network structure, high-specific surface area and are easy to ion to transmit rich in mesoporous,
Its specific surface area is 100~3000 m2/ g, nitrogen element content are 0.1~10.0 wt.%, and limit porous carbon by this loads with silicon
For obtained negative material compared with commercial carbons negative material, Si has more height ratio capacity and energy density, operating potential 0-
Between 0.4V, lithium ion battery negative material, and rich reserves are suitable as, are easily obtained;
2)A large amount of N elements are rich in the porous carbon materials that the present invention uses, upset carbon atom ∏ conjugated electron systems, there is provided bigger
Electrochemical surface area and avtive spot, collaboration promote electric charge transfer between carbon atom and hetero atom, lift carbon layer material conductance
And specific capacity;
3)The monocrystalline silicon nano of the present invention is semi-conducting material, poorly conductive itself, and porous carbon materials can be used as it is excellent
Monocrystalline silicon nanometer particle load on bio-based N doping porous carbon support, is substantially increased electric conductivity by conductor, the present invention, by
It is simple in its preparation technology, be advantageous to large-scale production application.
Brief description of the drawings
Fig. 1 is bio-based porous carbon materials scanning electron microscope (SEM) photograph of the present invention;
Fig. 2 is load silicon bio-based N doping porous carbon scanning electron microscope (SEM) photograph prepared by embodiment 1;
Fig. 3 is load silicon bio-based N doping porous carbon cathode material lithium ion battery charge-discharge cycle prepared by embodiment 1
Can comparison diagram.
Embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention
Content is not limited solely to the following examples.
Embodiment 1:
A kind of lithium battery load porous carbon negative pole material of silicon bio-based N doping, it is characterised in that described bio-based N doping
Porous carbon is bamboo carbon, and the specific surface area of carbon material is 500 m2/ g, nitrogen element content are 1.0 wt.%.
Described load monocrystalline silicon nano, particle diameter are 50 nm.
5 g monocrystalline silicon nanos are scattered in ultrasound 30 minutes in tetrahydrofuran solvent, after being uniformly dispersed, added
100 g porous carbons continue ultrasound 20 minutes, high speed centrifugation, deionized water washing, obtain loading silicon biology after 40 DEG C of oven dryings
Base N doping porous carbon, assemble battery as lithium ion battery negative material and test its charge-discharge performance.
Embodiment 2:
A kind of lithium battery load porous carbon negative pole material of silicon bio-based N doping, it is characterised in that described bio-based N doping
Porous carbon is bamboo carbon, and the specific surface area of carbon material is 1000 m2/ g, nitrogen element content are 3.0 wt.%.
Described load monocrystalline silicon nano, particle diameter are 50 nm.
5 g monocrystalline silicon nanos are scattered in ultrasound 30 minutes in tetrahydrofuran solvent, after being uniformly dispersed, added
100 g porous carbons continue ultrasound 20 minutes, high speed centrifugation, deionized water washing, obtain loading silicon biology after 40 DEG C of oven dryings
Base N doping porous carbon, assemble battery as lithium ion battery negative material and test its charge-discharge performance.
Embodiment 3:
A kind of lithium battery load porous carbon negative pole material of silicon bio-based N doping, it is characterised in that described bio-based N doping
Porous carbon is bamboo carbon, and the specific surface area of carbon material is 1500 m2/ g, nitrogen element content are 5.0 wt.%.
Described load monocrystalline silicon nano, particle diameter are 50 nm.
5 g monocrystalline silicon nanos are scattered in ultrasound 30 minutes in tetrahydrofuran solvent, after being uniformly dispersed, added
100 g porous carbons continue ultrasound 20 minutes, high speed centrifugation, deionized water washing, obtain loading silicon biology after 40 DEG C of oven dryings
Base N doping porous carbon, assemble battery as lithium ion battery negative material and test its charge-discharge performance.
Embodiment 4:
A kind of lithium battery load porous carbon negative pole material of silicon bio-based N doping, it is characterised in that described bio-based N doping
Porous carbon is bamboo carbon, and the specific surface area of carbon material is 2000 m2/ g, nitrogen element content are 8.0 wt.%.
Described load monocrystalline silicon nano, particle diameter are 50 nm.
5 g monocrystalline silicon nanos are scattered in ultrasound 30 minutes in tetrahydrofuran solvent, after being uniformly dispersed, added
100 g porous carbons continue ultrasound 20 minutes, high speed centrifugation, deionized water washing, obtain loading silicon biology after 40 DEG C of oven dryings
Base N doping porous carbon, assemble battery as lithium ion battery negative material and test its charge-discharge performance.
In 100 mAg-1Under current density, test respectively its first, 50 charge and discharge cycles specific capacities, concrete numerical value sees below
Shown in table 1:
Table 1 loads the porous carbon negative pole material charge and discharge cycles specific capacity of silicon bio-based N doping
The load silicon bio-based N doping porous carbon of the preparation it can be seen from the data of table 1 is first as lithium ion battery negative material
Secondary charge and discharge cycles specific capacity is up to 3315 mAhg-1, far above 370 mAhg of the carbon material negative pole material commercially used-1,
And still there are 1569 mAhg after 50 charge and discharge cycles of experience-1Specific capacity value, equally far above commercial carbon material negative pole material
Material.Therefore, it can have extensive commercial value and answer as the alternative materials of conventional commercial carbon negative electrode material of lithium ion cell
Use prospect.
Claims (8)
1. a kind of lithium battery load porous carbon negative pole material of silicon bio-based N doping, it is characterised in that more with bio-based N doping
Hole carbon is carrier, and, the specific surface area of the bio-based N doping porous carbon is by monocrystalline silicon nanometer particle load on this carrier
100~3000 m2/ g, nitrogen element content are 0.1~10.0 wt.%.
2. a kind of lithium battery according to claim 1 load porous carbon negative pole material of silicon bio-based N doping, its feature
It is bio-based N doping porous carbon for one or both of bamboo carbon, bamboo shoots carbon mixture.
3. a kind of lithium battery according to claim 1 load porous carbon negative pole material of silicon bio-based N doping, its feature
The particle diameter for being to load monocrystalline silicon nano is 5~500 nm.
A kind of 4. preparation side of the lithium battery according to claim 1 load porous carbon negative pole material of silicon bio-based N doping
Method, it is characterised in that monocrystalline silicon nano is scattered in organic solvent for ultrasonic to being uniformly dispersed, adds bio-based N doping
Porous carbon continues ultrasound, carries out high speed centrifugation after ultrasound structure, then washs through deionized water, lithium battery is obtained after oven drying uses
Load the porous carbon negative pole material of silicon bio-based N doping.
5. the lithium battery according to claim 4 preparation method of the load porous carbon negative pole material of silicon bio-based N doping,
It is characterized in that organic solvent is tetrahydrofuran.
6. the lithium battery according to claim 4 preparation method of the load porous carbon negative pole material of silicon bio-based N doping,
It is characterized in that it is 20-40 minutes, preferably 30 minutes that molybdenum sulfide nano-particle, which is scattered in the organic solvent for ultrasonic time,.
7. the lithium battery according to claim 4 preparation method of the load porous carbon negative pole material of silicon bio-based N doping,
It is characterized in that bio-based N doping porous carbon continues ultrasonic 10-30 minutes, preferably 20 minutes.
8. the electrode storage lithium of the lithium battery according to claim 1 load porous carbon negative pole material of silicon bio-based N doping
Energy characterizing method is as follows:Using the button-shaped half-cells of CR2025, the lithium battery load silicon bio-based N doping of mass fraction 80%
Porous carbon negative pole material, 10% binding agent Kynoar, 10% conductive agent acetylene carbon black are dissolved in 1-METHYLPYRROLIDONE simultaneously
Coated on copper foil, vacuum drying, 6 MPa, which are compressed, is used as negative pole stand-by, is lithium piece to electrode, barrier film uses polypropylene-poly- second
The how empty barrier film of alkene-polypropylene, the dimethyl carbonate and ethylene carbonate of 1M lithium hexafluoro phosphates by volume 1:1 prepares electrolyte,
Encapsulation carries out half-cell test.
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Cited By (3)
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CN111634909A (en) * | 2020-05-22 | 2020-09-08 | 上海应用技术大学 | Preparation method and application of nitrogen-doped porous carbon material based on trichloro-aza-acene fused-ring aromatic hydrocarbon |
CN112110436A (en) * | 2020-09-18 | 2020-12-22 | 昆明理工大学 | Preparation method of nitrogen-doped carbon-silicon negative electrode material of lithium ion battery |
EP4120393A4 (en) * | 2020-03-11 | 2023-11-08 | Ningde Amperex Technology Limited | Anode plate and manufacturing method therefor, battery using anode plate, and electronic apparatus |
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EP4120393A4 (en) * | 2020-03-11 | 2023-11-08 | Ningde Amperex Technology Limited | Anode plate and manufacturing method therefor, battery using anode plate, and electronic apparatus |
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