CN107834040A - A kind of lithium battery porous carbon negative pole material of bio-based N doping of load molybdenum disulfide and preparation method thereof - Google Patents
A kind of lithium battery porous carbon negative pole material of bio-based N doping of load molybdenum disulfide and preparation method thereof Download PDFInfo
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- CN107834040A CN107834040A CN201710899878.7A CN201710899878A CN107834040A CN 107834040 A CN107834040 A CN 107834040A CN 201710899878 A CN201710899878 A CN 201710899878A CN 107834040 A CN107834040 A CN 107834040A
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- 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
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- 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
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- H—ELECTRICITY
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- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
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Abstract
The invention discloses a kind of lithium battery load porous carbon negative pole material of molybdenum disulfide bio-based N doping and preparation method thereof, it is using bamboo carbon, the one or two of bamboo shoots carbon as bio-based N doping porous carbon, molybdenum disulfide nano particle is scattered in after ultrasonic disperse is uniform in tetrahydrofuran solvent, add high speed centrifugation after porous carbon continues ultrasound uniformly, deionized water is washed, obtain loading molybdenum disulfide bio-based N doping porous carbon after oven drying, as cathode material of lithium ion battery, the button-shaped half-cells of assembling CR2025 simultaneously test its chemical property.The negative material of the present invention is in 100 mAg‑1Under current density, first charge-discharge circulation specific capacity is up to 1650 mAhg‑1, far above 370 mAhg of the carbon material negative pole material commercially used‑1, and still there are 782 mAhg after 50 charge and discharge cycles‑1Specific capacity value, equally far above commercial carbon material negative pole material.Therefore, it can have extensive commercial value and application prospect as the alternative materials of conventional commercial carbon negative electrode material of lithium ion cell.
Description
Technical field
The present invention relates to new energy battery material technical field, the biology of specifically a kind of lithium battery load molybdenum disulfide
Porous carbon negative pole material of base N doping 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.
Molybdenum disulfide material is up to 1800 mAhg because of it-1Theoretical specific capacity, 4300 mAhcm-1Volume and capacity ratio,
1.1 eV energy gaps, 0-0.4 V operating potentials and 250 DEG C of operating temperatures, turn into most promising lithium-ion electric of future generation
One of pond negative material.In addition, molybdenum disulfide raw material resources deposit enriches, mature preparation process, it is commercial lithium to be adapted to exploitation
Ion battery cathode material.Though molybdenum disulfide has many advantages, such as the above as negative material, some itself are still suffered from not
Defect can be avoided:1)Molybdenum disulfide is a kind of semi-conducting material, intrinsic resistivity 1.9*105 Ω .cm, dielectric constant 8.7, conductance
Rate is relatively low;2)During charge and discharge cycles, Li+It is constantly embedded and deviate from, the change of molybdenum disulfide material volume is reachable
400%, thus produce a series of problems.Such as:Molybdenum disulfide particles crush or Materials Fracture is so as to destroy electrode structure, make conduction
Contact is deteriorated, and causes capacity to decline.It is uneven caused by along the electrochemical reaction in thickness of electrode direction in electrochemistry cyclic process
Even polarization triggers the rupture of electrode stratiform and peeled off, and then conductive network collapse and electrode failure occurs;3)Li+Insertion-abjection
During be concatenated to form solid-electrolyte interface film(SEI), after multiple charge and discharge cycles, SEI thickness increases ultimately result in Si materials
Material loses electro-chemical activity, causes capacitance loss.To solve the above problems, molybdenum disulfide material negative material performance is improved, system
Standby C@MoS2Composite nano materials are ensureing the basis of molybdenum disulfide material height ratio capacity and energy density as negative material
On, reduce active material cracking or peel off the electrode failure triggered, suppress SEI and formed, increase electric conductivity, improve charge and discharge cycles
Performance.In a word, around high performance lithium ion battery application demand, further design and prepare carbon@molybdenum-disulfide radical nanometers and bear
Pole material, improve the charge-discharge performance of lithium ion battery negative material, be still that the field there are important scientific issues to be solved.
The content of the invention
For the above-mentioned problems in the prior art, it is an object of the present invention to provide a kind of lithium battery load molybdenum disulfide
Porous carbon negative pole material of N doping of bio-based and preparation method thereof, the biomass porous carbon material take natural bamboo or bamboo shoots
For raw material, preparation technology is simple, can large-scale industrial production, the load molybdenum disulfide bio-based N doping being prepared is porous
Carbon negative pole material has excellent chemical property.
A kind of porous carbon negative pole material of bio-based N doping of described lithium battery load molybdenum disulfide, it is characterised in that
Using bio-based N doping porous carbon as carrier, by the load of molybdenum disulfide nano particle on this carrier, the bio-based N doping
The specific surface area of porous carbon is 100~3000 m2/ g, nitrogen element content are 0.1~10.0 wt.%, and the bio-based N doping is more
A diameter of 2-50nm of hole on the carbon of hole.
Described a kind of lithium battery load porous carbon negative pole material of molybdenum disulfide bio-based N doping, it is characterised in that negative
The particle diameter for carrying molybdenum disulfide nano particle is 5~500 nm.
Described a kind of lithium battery load porous carbon negative pole material of molybdenum disulfide bio-based N doping, it is characterised in that raw
Thing base N doping porous carbon is bamboo carbon, the one or two of bamboo shoots carbon, and the preparation technology of bio-based porous carbon exists
201610340621.3 application for a patent for invention file in disclose.
The described lithium battery preparation method of the load porous carbon negative pole material of molybdenum disulfide bio-based N doping, its feature
It is molybdenum disulfide nano particle being scattered in organic solvent for ultrasonic to after being uniformly dispersed, adds bio-based N doping porous carbon
Continue ultrasound, carry out high speed centrifugation after ultrasound structure, then wash through deionized water, lithium battery is obtained after oven drying load two
The porous carbon negative pole material of molybdenum sulfide bio-based N doping.
The described lithium battery preparation method of the load porous carbon negative pole material of molybdenum disulfide bio-based N doping, its feature
It is tetrahydrofuran to be organic solvent.
The described lithium battery preparation method of the load porous carbon negative pole material of molybdenum disulfide bio-based N doping, its feature
It is 20-40 minutes, preferably 30 minutes to be that molybdenum disulfide nano particle is scattered in the organic solvent for ultrasonic time.
The described lithium battery preparation method of the load porous carbon negative pole material of molybdenum disulfide bio-based N doping, its feature
It is that bio-based N doping porous carbon continues ultrasonic 10-30 minutes, preferably 20 minutes.
The electrode storage lithium performance table of the described lithium battery load porous carbon negative pole material of molybdenum disulfide bio-based N doping
Sign method is as follows:Using the button-shaped half-cells of CR2025, the lithium battery of mass fraction 80% is mixed with load molybdenum disulfide bio-based nitrogen
Miscellaneous porous carbon negative pole material, 10% binding agent Kynoar, 10% conductive agent acetylene carbon black are dissolved in 1-METHYLPYRROLIDONE
And coated on copper foil, vacuum drying, 6 MPa compress stand-by as negative pole, be lithium piece to electrode, barrier film is using polypropylene-gather
The how empty barrier film of ethylene-polypropylene, the dimethyl carbonate and ethylene carbonate of 1M lithium hexafluoro phosphates by volume 1:1 prepares electrolysis
Liquid, encapsulation carry out half-cell test.
The present invention 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 beneficial effect:
1)The present invention is using natural bamboo or bamboo shoots as the porous carbon raw material of bio-based N doping, and its processing technology is simple, gained
The specific surface area of porous carbon materials is 100~3000 m2/ g, nitrogen element content are 0.1~10.0 wt.%, and it is a kind of height
Cross-linked structure, there is high-specific surface area and rich in mesoporous(I.e. the hole diameter of porous carbon is in 2-50 nm), it is easy to ion to pass
It is defeated, because it is rich in a large amount of N elements contain, upset carbon atom ∏ conjugated electron systems, can provide bigger electrochemical surface area with
Avtive spot, collaboration promote electric charge transfer between carbon atom and hetero atom, lift carbon layer material conductance and specific capacity;
2)The molybdenum disulfide of the present invention is semi-conducting material, poorly conductive, and bio-based nitrogen-doped porous carbon material is as excellent
Conductor, both are complementary, improve electric conductivity;
3)The present invention loads to molybdenum disulfide nano particle on bio-based N doping porous carbon, molybdenum disulfide rich reserves, former
Expect the porous carbon negative pole material of N doping of load molybdenum disulfide bio-based simple and easy to get, to obtain and commercial carbons negative material phase
Than because molybdenum disulfide has more height ratio capacity and an energy density, between its operating potential 0-0.4V, being more suitable for lithium ion
Cell negative electrode material, its preparation technology is simple, is advantageous to scale application.
Brief description of the drawings
Fig. 1 is the bio-based porous carbon materials scanning electron microscope (SEM) photograph of the present invention;
Fig. 2 is the bio-based N doping porous carbon scanning electron microscope (SEM) photograph of load molybdenum disulfide prepared by embodiment 1;
Fig. 3 is the lithium of the load porous carbon negative pole material of molybdenum disulfide bio-based N doping and commercial carbon material prepared by embodiment 1
Ion battery charge-discharge performance 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 molybdenum disulfide bio-based N doping, uses bamboo carbon as bio-based N doping
Porous carbon, the specific surface area of the carbon material is 500m2/ g, nitrogen element content are 1.0 wt.%.
The particle diameter of the molybdenum disulfide nano particle of load is 50 nm, and its preparation method is as follows:
5 g molybdenum disulfide nano particles are scattered in ultrasound 30 minutes in tetrahydrofuran solvent, after being uniformly dispersed, add 100
G bio-based N dopings porous carbon continues ultrasound 20 minutes, at a high speed(Both are efficiently separated, namely height of the prior art
Speed)Centrifugation, deionized water are washed, and obtain loading molybdenum disulfide bio-based N doping porous carbon after 40 DEG C of oven dryings, as lithium
Ion battery cathode material assembles battery and tests its charge-discharge performance.
Embodiment 2:
A kind of lithium battery load porous carbon negative pole material of molybdenum disulfide bio-based N doping, bio-based N doping porous carbon is bamboo
Carbon, the specific surface area of the carbon material is 1000 m2/ g, nitrogen element content are 3.0 wt.%.
The particle diameter of described load molybdenum disulfide nano particle is 50 nm, and its preparation method is as follows:
5 g molybdenum disulfide nano particles are scattered in ultrasound 30 minutes in tetrahydrofuran solvent, after being uniformly dispersed, add 100
G porous carbons continue ultrasound 20 minutes, high speed centrifugation, deionized water washing, obtain loading molybdenum disulfide life after 40 DEG C of oven dryings
Thing 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 molybdenum disulfide bio-based N doping, bio-based N doping porous carbon is bamboo
Carbon, the specific surface area of carbon material is 1500 m2/ g, nitrogen element content are 5.0 wt.%.
Described load molybdenum disulfide nano particle, particle diameter are 50 nm, and its preparation method is as follows:
5 g molybdenum disulfide nano particles are scattered in ultrasound 30 minutes in tetrahydrofuran solvent, after being uniformly dispersed, add 100
G porous carbons continue ultrasound 20 minutes, high speed centrifugation, deionized water washing, obtain loading molybdenum disulfide life after 40 DEG C of oven dryings
Thing 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 molybdenum disulfide bio-based N doping, bio-based N doping porous carbon is bamboo
Carbon, the specific surface area of carbon material is 2000 m2/ g, nitrogen element content are 8.0 wt.%.
The particle diameter of described load molybdenum disulfide nano particle is 50 nm.
5 g molybdenum disulfide nano particles 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 curing after 40 DEG C of oven dryings
Molybdenum bio-based N doping porous carbon, assemble battery as lithium ion battery negative material and test its charge-discharge performance.
Load molybdenum disulfide bio-based N doping porous carbon composite electrode storage lithium performance characterization uses CR2025 buttons
Formula half-cell, the load molybdenum disulfide bio-based N doping porous carbon composite of mass fraction 80%(Abbreviation C@Si composite woods
Material), 10% binding agent Kynoar(PVDF), 10% conductive agent acetylene carbon black is dissolved in 1-METHYLPYRROLIDONE(NMP)In 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, 1M lithium hexafluoro phosphates(LiPF6)Dimethyl carbonate(DMC)And ethylene carbonate(EC)By volume
Than 1:1 prepares electrolyte, and encapsulation carries out half-cell test.
Using Land CT2001A(Wuhan is blue rich)Constant current charge-discharge test is carried out to battery, by recording discharge and recharge
The data such as time, voltage, electric current, capacity in journey, 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), obtain electrode and specific electrochemical reaction electricity occur
Position, analyzes sample electrochemical reaction process and mechanism, and electrochemical reaction material category is participated in auxiliary checking;Using CHI660D(On
Hai Chenhua)Electrochemical impedance test is carried out, to comparative sample charge transfer resistance size.
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 molybdenum disulfide bio-based N doping
The load molybdenum disulfide bio-based N doping porous carbon conduct that it can be seen from the data of table 1 prepared by 1-4 of the embodiment of the present invention
Lithium ion battery negative material first charge-discharge circulation specific capacity is up to 1650 mAhg-1More than, far above the carbon materials commercially used
Expect 370 mAhg of negative material-1, and still there are 782 mAhg after undergoing 50 charge and discharge cycles-1Specific capacity value, it is same remote
Higher than commercial carbon material negative pole material.Therefore, it can have extensive as the alternative materials of commercial li-ion cell negative electrode material
Commercial value and application prospect.
The load porous carbon negative pole material of molybdenum disulfide bio-based N doping that the embodiment of the present invention 1 obtains passes through with commercial carbon material
The specific capacity value contrast of 50 charge and discharge cycles is gone through as shown in figure 3, from figure 3, it can be seen that the load curing that the present invention obtains
The specific capacity for the carbon material negative pole material that the specific capacity of the porous carbon negative pole material of molybdenum bio-based N doping significantly larger than commercially uses
Value, it can have extensive commercial value and application prospect as the alternative materials of commercial li-ion cell negative electrode material.
Claims (8)
1. a kind of lithium battery porous carbon negative pole material of bio-based N doping of load molybdenum disulfide, it is characterised in that with bio-based
N doping porous carbon is carrier, by the load of molybdenum disulfide nano particle on this carrier, the bio-based N doping porous carbon
Specific surface area is 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 molybdenum disulfide bio-based N doping,
It is characterized in that the particle diameter of load molybdenum disulfide nano particle is 5~500 nm.
3. a kind of lithium battery according to claim 1 load porous carbon negative pole material of molybdenum disulfide bio-based N doping,
It is characterized in that bio-based N doping porous carbon is bamboo carbon, the one or two of bamboo shoots carbon.
A kind of 4. lithium battery according to claim 1 load porous carbon negative pole material of molybdenum disulfide bio-based N doping
Preparation method, it is characterised in that molybdenum disulfide nano particle is scattered in organic solvent for ultrasonic to after being uniformly dispersed, adds life
Thing base N doping porous carbon continues ultrasound, carries out high speed centrifugation after ultrasound structure, then washs through deionized water, after oven drying
To the lithium battery load porous carbon negative pole material of molybdenum disulfide bio-based N doping.
5. the lithium battery according to claim 4 preparation of the load porous carbon negative pole material of molybdenum disulfide bio-based N doping
Method, it is characterised in that organic solvent is tetrahydrofuran.
6. the lithium battery according to claim 4 preparation of the load porous carbon negative pole material of molybdenum disulfide bio-based N doping
Method, it is characterised in that it is 20-40 minutes, preferably 30 points that molybdenum disulfide nano particle, which is scattered in the organic solvent for ultrasonic time,
Clock.
7. the lithium battery according to claim 4 preparation of the load porous carbon negative pole material of molybdenum disulfide bio-based N doping
Method, it is characterised in that bio-based N doping porous carbon continues ultrasonic 10-30 minutes, preferably 20 minutes.
8. the lithium battery according to claim 1 electrode of the load porous carbon negative pole material of molybdenum disulfide bio-based N doping
It is as follows to store up lithium performance characterization method:Using the button-shaped half-cells of CR2025, the lithium battery load molybdenum disulfide of mass fraction 80%
The porous carbon negative pole material of bio-based N doping, 10% binding agent Kynoar, 10% conductive agent acetylene carbon black are dissolved in N- methyl
In pyrrolidones 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
The how empty barrier film of polypropylene-polyethylene-polypropylene, the dimethyl carbonate and ethylene carbonate of 1M lithium hexafluoro phosphates by volume 1:1
Electrolyte is prepared, encapsulation carries out half-cell test.
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Cited By (6)
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CN109273691A (en) * | 2018-09-25 | 2019-01-25 | 岭南师范学院 | A kind of molybdenum disulfide/nitrogen-doped carbon composite material and preparation method and application |
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CN112786865A (en) * | 2021-01-29 | 2021-05-11 | 西北工业大学宁波研究院 | MoS2Preparation method and application of quasi-quantum dot/nitrogen-sulfur co-doped biomass carbon composite nano material |
CN112599770A (en) * | 2021-03-04 | 2021-04-02 | 湖南镕锂新材料科技有限公司 | Lithium/sodium ion battery negative electrode material and preparation method thereof |
CN112599770B (en) * | 2021-03-04 | 2022-02-18 | 湖南镕锂新材料科技有限公司 | Lithium/sodium ion battery negative electrode material and preparation method thereof |
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