CN108598450A - A kind of CoP/ nitrogen-doped carbons/graphene nanocomposite material and preparation method thereof - Google Patents
A kind of CoP/ nitrogen-doped carbons/graphene nanocomposite material and preparation method thereof Download PDFInfo
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- CN108598450A CN108598450A CN201810699809.6A CN201810699809A CN108598450A CN 108598450 A CN108598450 A CN 108598450A CN 201810699809 A CN201810699809 A CN 201810699809A CN 108598450 A CN108598450 A CN 108598450A
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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
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5805—Phosphides
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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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
Abstract
The invention discloses a kind of CoP/ nitrogen-doped carbons/graphene nanocomposite materials and preparation method thereof, the composite material is with graphene oxide, cabaltous nitrate hexahydrate, a hydration sodium hypophosphite, 4,4' bipyridyls and 1,3,5 trimesic acids are raw material, are prepared using simple hydro-thermal method and low temperature phosphor method.The method of the present invention is simple, of low cost, and prepared CoP/ nitrogen-doped carbons/graphene composite material is three-dimensional porous structure, can be applied to lithium/anode material of lithium-ion battery and presents good chemical property.
Description
Technical field
The invention belongs to field of electrochemical power source, and in particular to a kind of CoP/ nitrogen-doped carbons/stone of excellent electrochemical performance
Black alkene nanocomposite and preparation method thereof.
Background technology
It is also all very rapid in industry, agricultural and various economic developments with the development of new century, therefore the mankind are to energy
The demand in source is also continuously increased, and the non-renewable resources such as traditional energy such as oil, coal bring huge pollution to environment, this
And green, health, the theory of sustainable development that the mankind pursue in the new century are not met.In recent years, the mankind have been devoted to visit
Suo Qingjie, the exploitation of regenerative resource, utilization and energy storage problem.And lithium ion battery is as a kind of efficient, easily storage
Electric energy storage device have received widespread attention and study.Compared with lithium ion battery, sodium-ion battery system is provided due to sodium
The advantages that abundant, cheap, higher current potential in source has been since lithium-ion battery system most before researching value and application
The secondary cell system of scape.
Anode material of lithium-ion battery is one of the important indicator for weighing sodium-ion battery performance.Wherein negative material electrode
In can change with the sodium material of reaction include 3d transition metal oxides, sulfide, phosphide etc..And actually mostly
There are actual capacities for several electrode materials well below theoretical capacity, high rate performance is poor, reversible capacity decaying is fast, cycle life
Short, the problems such as charge and discharge potential polarization is big, energy loss is big.And these problems are caused by following reason：(1) electrode material shape
The variation of looks and micro-structure；(2) on electrode active material volume change, this eventually results in the crushing of active material and electrode
Machinery disintegrate；(3) poorly conductive causes its utilization rate to substantially reduce.In addition with 3d transition metal oxides, testing sulphide ratio,
Metal phosphide polarization is minimum, and capacity is high, and voltage platform is low.Importantly, transition metal phosphide has smaller
Volume expansion, and the feature of its metalloid also implies that the electric conductivity of transition metal phosphide is relatively preferable.Therefore, it seeks
The high-energy and power for looking for novel anode material or design and assembly novel anode material structure to realize lithium/sodium-ion battery are close
Degree, long circulation life, low cost and high safety performance demand are the targets that scientist pursues always, it has also become the forward position heat of research
Point.
Invention content
Regarding the issue above, the present invention provides a kind of with height ratio capacity, big multiplying power and long-life and steady
CoP/ nitrogen-doped carbons/graphene composite material of qualitative good storage lithium/sodium performance, and provide a kind of side of preparation for the composite material
Method.
For above-mentioned purpose, CoP/ of the invention nitrogen-doped carbon/graphene nanocomposite material is prepared by following methods
It arrives：By graphene oxide ultrasonic disperse in n,N-Dimethylformamide, add cabaltous nitrate hexahydrate, 4,4'- bipyridyls and
1,3,5- trimesic acid is stirred at room temperature 0.5~1 hour, then gained suspension is transferred in autoclave, at 110~130 DEG C
Lower reaction 5~8 hours naturally cools to room temperature, centrifugation, washing, drying；Gained desciccate and a waterside sodium phosphate press quality
Than being 10~20:1 is placed in argon gas atmosphere, is calcined 1~3 hour at 300~400 DEG C, obtains CoP/ nitrogen-doped carbons/graphene
Nanocomposite.
In above-mentioned preparation method, preferably quality-volume ratio of graphene oxide and n,N-Dimethylformamide be 0.5~
0.9mg:The mass ratio of 1mL, graphene oxide and cabaltous nitrate hexahydrate is 1:15~30, cabaltous nitrate hexahydrate and 4,4'- joins pyrrole
Pyridine, 1,3,5- trimesic acids molar ratio be 1:1:1.
In above-mentioned preparation method, preferably gained suspension is transferred in autoclave, is reacted 6 hours at 120 DEG C.
In above-mentioned preparation method, further preferably gained desciccate and a waterside sodium phosphate are 15~18 in mass ratio:1
It is placed in argon gas atmosphere, is calcined 2 hours at 320~350 DEG C.
The present invention utilizes solvent-thermal method that cobalt -4,4'- bipyridyl -1,3,5- trimesic acids and graphene is compound for the first time
To cobalt -4,4'- bipyridyl -1,3, then 5- trimesic acids/graphene composite material obtain cellular by low temperature phosphor
CoP/ nitrogen-doped carbons/graphene nanocomposite material.The present invention is equal by nano Co P particles by simple, low-cost method
It is dispersed in evenly on nitrogen-doped carbon/graphene nanocomposite material, and compound with CoP/ nitrogen-doped carbons/graphene nano of the present invention
Material does cell negative electrode material, shows superior storage lithium/sodium performance.
Description of the drawings
Fig. 1 be nitrogen mix graphene, CoP/ nitrogen-doped carbons, embodiment 1 prepare CoP/ nitrogen-doped carbons/graphene nano it is compound
The X-ray powder diffraction of material is composed.
Fig. 2 is the SEM figures of CoP/ nitrogen-doped carbons/graphene nanocomposite material prepared by embodiment 1.
Fig. 3 is the TEM figures of CoP/ nitrogen-doped carbons/graphene nanocomposite material prepared by embodiment 1.
Fig. 4 be nitrogen mix graphene, CoP/ nitrogen-doped carbons, embodiment 1 prepare CoP/ nitrogen-doped carbons/graphene nano it is compound
The storage lithium cycle performance figure of material.
Fig. 5 be nitrogen mix graphene, CoP/ nitrogen-doped carbons, embodiment 1 prepare CoP/ nitrogen-doped carbons/graphene nano it is compound
The storage lithium high rate performance figure of material.
Fig. 6 is the storage sodium cycle performance figure of CoP/ nitrogen-doped carbons/graphene nanocomposite material prepared by embodiment 1.
Fig. 7 is the storage sodium high rate performance figure of CoP/ nitrogen-doped carbons/graphene nanocomposite material prepared by embodiment 1.
Specific implementation mode
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to
These embodiments.
Embodiment 1
35mg graphene oxides (GO) are added to 70mLN, ultrasound 2 hours in dinethylformamide (DMF) are made equal
One, the GO/DMF suspensions disperseed, then by 1.0186g (3.5mmol) cabaltous nitrate hexahydrate, 0.5466g (3.5mmol) 4,4'-
Bipyridyl and 0.7355g (3.5mmol) 1,3,5- trimesic acids, which are added in above-mentioned GO/DMF suspensions, to be stirred 0.5 hour
It to purple suspension, is then transferred in 100mL autoclaves, is reacted 6 hours at 120 DEG C, naturally cool to room temperature, from
The heart, washing, drying.By gained desciccate and a hydration sodium hypophosphite with mass ratio for 20:1 is placed in argon gas atmosphere,
It is calcined 2 hours at 350 DEG C, obtains CoP/ nitrogen-doped carbons/graphene nanocomposite material.
Embodiment 2
49mg graphene oxides are added to ultrasound 2 hours in 70mL DMF, it is suspended that uniform, dispersion GO/DMF is made
Liquid, then by 1.0186g (3.5mmol) cabaltous nitrate hexahydrate, 0.5466g (3.5mmol) 4,4'- bipyridyls and 0.7355g
(3.5mmol) 1,3,5- trimesic acid, which is added to stir 0.5 hour in above-mentioned GO/DMF suspensions, obtains purple suspension, so
It is transferred to afterwards in 100mL autoclaves, room temperature, centrifugation, washing, drying is naturally cooled to after being reacted 5 hours at 110 DEG C.It will
Gained desciccate and one is hydrated sodium hypophosphite with mass ratio as 15:1 is placed in argon gas atmosphere, and it is small that 2 are calcined at 300 DEG C
When, obtain CoP/ nitrogen-doped carbons/graphene nanocomposite material.
Embodiment 3
63mg graphene oxides are added to ultrasound 2 hours in 70mL DMF, it is suspended that uniform, dispersion GO/DMF is made
Liquid, then by 1.0186g (3.5mmol) cabaltous nitrate hexahydrate, 0.5466g (3.5mmol) 4,4'- bipyridyls and 0.7355g
(3.5mmol) 1,3,5- trimesic acid, which is added to stir 0.5 hour in above-mentioned GO/DMF suspensions, obtains purple suspension, so
It is transferred to afterwards in 100mL autoclaves, room temperature, centrifugation, washing, drying is naturally cooled to after being reacted 8 hours at 130 DEG C.It will
Gained desciccate and one is hydrated sodium hypophosphite with mass ratio as 18:1 is placed in argon gas atmosphere, and it is small that 2 are calcined at 320 DEG C
When, obtain CoP/ nitrogen-doped carbons/graphene nanocomposite material.
Inventor carries out structure to 1 gained sample of embodiment respectively using X-ray diffractometer, scanning electron microscope and transmission electron microscope
And morphology characterization, the result is shown in Figure 1~3.As seen from Figure 1, the XRD spectrum of sample contains the diffraction maximum of CoP and graphene, from Fig. 2
SEM figures as can be seen that having a large amount of CoP particles and CoP nano particles are evenly dispersed in nitrogen-doped carbon/graphene in sample
It is upper formed three-dimensional structure composite material, also can prove that from Fig. 3 extra small CoP nano particles be dispersed in nitrogen-doped carbon/
In graphene sheet layer structure, the diameter of CoP particles is in 5nm or so.In addition, the X-ray of 3 products obtained therefrom of embodiment 2 and embodiment
Powder diffraction spectrum is same as Example 1, and SEM figures and TEM figures show embodiment 2 and 3 gained sample of embodiment and 1 sample of embodiment
Pattern it is similar, be porous material composite material.
In order to prove that beneficial effects of the present invention, inventor sample the composite material of above-described embodiment 1~3, prepare respectively
At working electrode, it is then assembled into lithium ion battery and sodium-ion battery respectively, it is specific to try to the electrochemical property test of battery
It is as follows to test situation：
(1) preparation of working electrode
By powdered composite material and acetylene black prepared in above-described embodiment, Kynoar with mass ratio for 8:1:
1 is uniformly mixed；Then excessive N-Methyl pyrrolidone is instilled to stir evenly batch mixing；Uniformly mixed slurry is uniformly coated
In nickel foam circular piece, it is placed on 80 DEG C of dryings in vacuum drying chamber；It finally places it under tablet press machine and flattens, weighs.Root
The quality that active material in electrode is obtained according to rate of charge is 1.8 ± 0.1mg/cm2。
(2) lithium ion battery assembles
Using the pole piece prepared by above-mentioned steps (1) as working electrode, simple metal Li is used as to electrode and reference electrode, every
Film is commercialized polypropylene porous film, and used electrolyte is a concentration of 1mol/L LiPF6/ ethylene carbonate-carbonic acid two
Methyl esters-methyl ethyl carbonate (volume ratio 1:1:1).
(3) sodium-ion battery assembles
Using the pole piece prepared by above-mentioned steps (1) as working electrode, simple metal Na is used as to electrode and reference electrode, every
Film is commercialized polypropylene porous film, and electrolyte is 1mol/L NaClO4/ propene carbonate-ethylene carbonate (volume ratio 1:
1, and the fluorinated ethylene carbonate containing 5vol%).
Above-mentioned assembling overall process is completed in the glove box full of Ar atmosphere, finally sealing machine is used to seal.
(4) electrochemical property test
The electrochemical property test of lithium/sodium-ion battery is to be used as test device by the CR2025 button cells of assembling.
Specific capacity, stable circulation performance and high rate performance are completed by the blue electricity CT2001A cell testers test in Wuhan, test result
See Fig. 4~7.
Fig. 4 illustrates made in nitrogen-doped graphene, CoP/ nitrogen-doped carbons composite material and embodiment 1 by way of contrast
Standby CoP/ nitrogen-doped carbons/graphene nanocomposite material is 0.2A g in current density-1Under storage lithium cycle performance.From figure
To see, reversible specific capacity is up to 634mAh/g after CoP/ nitrogen-doped carbons/graphene nanocomposite material charge and discharge 100 times, and
Coulombic efficiency is about 99%.However, nitrogen-doped graphene and CoP/ nitrogen-doped carbon composite materials occur it is lasting, significantly decline
Subtract phenomenon, reversible specific capacity is only 287 and 129mAh/g after charge and discharge 100 times.Fig. 5 be above-mentioned material current density from
0.25 to 4A/g returns the high rate performance figure of 0.25A/g.It is obvious that CoP/ nitrogen-doped carbons/graphene prepared by embodiment 1 is received
The average reversible specific capacity of nano composite material is 755,639,576,541 and 507mAh/g respectively.When circulating current is reduced to
When 0.25A/g, the averaged discharge specific capacitance of the composite material can still be restored to 647mAh/g.Under identical current density, nitrogen
Doped graphene and CoP/ nitrogen-doped carbons composite material but show poor high rate performance.It can be seen that this from Figure 4 and 5
CoP/ nitrogen-doped carbons/graphene nanocomposite material prepared by inventive embodiments 1 shows outstanding storage lithium performance.After tested,
The storage lithium performance of embodiment 2 and embodiment 3 gained CoP/ nitrogen-doped carbons/graphene nanocomposite material compared with Example 1, than
The difference of capacity is only ± 3%.
Fig. 6 is that CoP/ nitrogen-doped carbons/graphene nanocomposite material prepared by embodiment 1 in current density is 0.1A g-1
Under storage sodium cycle performance.See from figure, it is reversible after CoP/ nitrogen-doped carbons/graphene nanocomposite material charge and discharge 100 times
Specific capacity is up to 555mAh/g, and coulombic efficiency is about 99%.Fig. 7 is that CoP/ nitrogen-doped carbons/graphene prepared by embodiment 1 is received
Nano composite material returns the high rate performance figure of 0.1A/g in current density from 0.1 to 3.2A/g.It is obvious that CoP/ N dopings
The average reversible specific capacity of carbon graphite alkene nanocomposite is 680,588,497,434,380 and 337mAh/g respectively.When following
When circular current is reduced to 0.1A/g, the averaged discharge specific capacitance of the composite material can still be restored to 563mAh/g.It can from Fig. 6 and 7
To find out, CoP/ nitrogen-doped carbons/graphene composite material prepared by the embodiment of the present invention 1 shows outstanding storage sodium performance.Through
Test, storage lithium performance and 1 phase of embodiment of embodiment 2 and embodiment 3 gained CoP/ nitrogen-doped carbons/graphene nanocomposite material
Than the difference of specific capacity is only ± 4%.
Claims (6)
1. a kind of preparation method of CoP/ nitrogen-doped carbons/graphene composite material, it is characterised in that：By graphene oxide ultrasound point
It dissipates in n,N-Dimethylformamide, adds cabaltous nitrate hexahydrate, 4,4'- bipyridyls and 1,3,5- trimesic acids, room temperature
Gained suspension, is then transferred in autoclave, is reacted 5~8 hours at 110~130 DEG C by stirring 0.5~1 hour, naturally cold
But room temperature, centrifugation, washing, drying are arrived；Gained desciccate and a waterside sodium phosphate are 10~20 in mass ratio:1 is placed in argon gas
In atmosphere, is calcined 1~3 hour at 300~400 DEG C, obtain CoP/ nitrogen-doped carbons/graphene nanocomposite material.
2. the preparation method of CoP/ nitrogen-doped carbons/graphene nanocomposite material according to claim 1, feature exist
In：Quality-volume ratio of the graphene oxide and N,N-dimethylformamide is 0.5~0.9mg:1mL.
3. the preparation method of CoP/ nitrogen-doped carbons/graphene nanocomposite material according to claim 2, feature exist
In：The mass ratio of the graphene oxide and cabaltous nitrate hexahydrate is 1:15~30, cabaltous nitrate hexahydrate and 4,4'- bipyridyls,
The molar ratio of 1,3,5- trimesic acids is 1:1:1.
4. the preparation method of CoP/ nitrogen-doped carbons/graphene nanocomposite material according to claim 1, feature exist
In：Gained suspension is transferred in autoclave, is reacted 6 hours at 120 DEG C.
5. the preparation method of CoP/ nitrogen-doped carbons/graphene nanocomposite material according to claim 1, feature exist
In：Gained desciccate and a waterside sodium phosphate are 15~18 in mass ratio:1 is placed in argon gas atmosphere, at 320~350 DEG C
Calcining 2 hours.
6. CoP/ nitrogen-doped carbons/graphene nanocomposite material that Claims 1 to 5 any one method is prepared.
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| CN109967099A (en) * | 2019-03-11 | 2019-07-05 | 浙江大学 | A kind of Co with hollow nanostructures2P@C composite and its preparation method and application |
| CN111039268A (en) * | 2019-12-19 | 2020-04-21 | 河南省人民医院 | CoP/C nano composite material, preparation method and application |
| CN112552902A (en) * | 2020-11-20 | 2021-03-26 | 扬州大学 | Graphene quantum dot assembly with foam structure and preparation method thereof |
| CN112981446A (en) * | 2021-02-07 | 2021-06-18 | 西安交通大学 | Multi-stage catalytic structure composite material for efficient water electrolysis hydrogen evolution and preparation method thereof |
| CN113896177A (en) * | 2021-10-08 | 2022-01-07 | 宁德师范学院 | Novel battery negative electrode material and preparation method thereof, negative electrode and novel lithium ion battery |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109411736A (en) * | 2018-12-04 | 2019-03-01 | 重庆文理学院 | A kind of phosphatization cobalt/graphene/N doped carbon composite material and preparation method |
| CN109967099A (en) * | 2019-03-11 | 2019-07-05 | 浙江大学 | A kind of Co with hollow nanostructures2P@C composite and its preparation method and application |
| CN111039268A (en) * | 2019-12-19 | 2020-04-21 | 河南省人民医院 | CoP/C nano composite material, preparation method and application |
| CN112552902A (en) * | 2020-11-20 | 2021-03-26 | 扬州大学 | Graphene quantum dot assembly with foam structure and preparation method thereof |
| CN112981446A (en) * | 2021-02-07 | 2021-06-18 | 西安交通大学 | Multi-stage catalytic structure composite material for efficient water electrolysis hydrogen evolution and preparation method thereof |
| CN113896177A (en) * | 2021-10-08 | 2022-01-07 | 宁德师范学院 | Novel battery negative electrode material and preparation method thereof, negative electrode and novel lithium ion battery |
| CN114045500A (en) * | 2021-11-19 | 2022-02-15 | 北京科技大学 | Preparation method of self-supporting multi-level structure electrode |
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