CN106981647A - A kind of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium-ion battery negative plate - Google Patents
A kind of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium-ion battery negative plate Download PDFInfo
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- CN106981647A CN106981647A CN201710400706.0A CN201710400706A CN106981647A CN 106981647 A CN106981647 A CN 106981647A CN 201710400706 A CN201710400706 A CN 201710400706A CN 106981647 A CN106981647 A CN 106981647A
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- molybdenum disulfide
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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
- H01M10/054—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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
- H01M4/5815—Sulfides
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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
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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 belongs to battery preparation technology field, it is related to a kind of sodium-ion battery negative plate, more particularly to a kind of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium-ion battery negative plate, by having wrapped up one layer of class graphene transition metal molybdenum disulfide on natural black pigment nanosphere, carbon ball/molybdenum disulfide material of N doping is prepared, and is prepared into battery；It extracts melanin from natural inkfish juice, molybdenum disulfide is wrapped up on its surface by hydro-thermal method, because the main component of melanin is poly-dopamine, it is changed into the carbon ball of N doping in water-heat process, molybdenum disulfide nano sheet is uniformly coated on Nano carbon balls, laod network is formed between nanometer sheet, good conductive network is served；By the CS/MoS of preparation2Material is used as the negative material of sodium-ion battery, improves the stability at negative pole structure and interface, improves the cyclical stability of negative pole, is conducive to commercially producing and applies.
Description
Technical field：
The invention belongs to battery preparation technology field, it is related to a kind of sodium-ion battery negative plate, more particularly to a kind of nitrogen is mixed
Miscellaneous Nano carbon balls/molybdenum disulfide sodium-ion battery negative plate, by having wrapped up one layer of class graphite on natural black pigment nanosphere
Alkene transition metal molybdenum disulfide, prepares carbon ball/molybdenum disulfide (MoS of N doping2)(carbon spheres,CS)(CS/
MoS2) material, and it is prepared into battery.
Background technology：
Sodium-ion battery is because abundance, preparation technology are simple, pollution-free, cheap and are distributed in nature
Wide the advantages of, be considered as the preferable substitute of lithium ion battery always.More anode material of lithium-ion battery is studied at present
Mainly various carbon-based materials, such as graphite, carbonaceous mesophase spherules, hard carbon, the chemical property of carbon-based material have with its structure
Substantial connection, meanwhile, metal_based material, due to higher theoretical capacity, is also the preferable anode material of lithium-ion battery of a class,
It wherein common are metal alloy, metal oxide and metal sulfide etc..Two-dimentional transient metal sulfide have low cost and
The characteristics of high theoretical specific capacity, the study hotspot as sode cell negative material；Because interlamellar spacing is big, interlaminar action power compares
Weak, two-dimentional transient metal sulfide is easily achieved the reversible electrochemical deintercalation of sodium ion；Wherein, molybdenum disulfide is a kind of typical case
Two-dimentional transient metal sulfide, have the advantages that theoretical capacity is high, but its electric conductivity is poor, causes its high rate performance to be paid no attention to
Think.Therefore the present invention is intended to provide a kind of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium-ion battery negative plate, with reference to molybdenum disulfide
The advantage of high theoretical specific capacity and N doping carbon ball high conductivity, for preparing with high charge-discharge specific capacity, good forthright again
The sodium-ion battery of energy and long circulation life, with good economic benefit and social benefit.
The content of the invention：
The present invention is in order to overcome the shortcomings of the prior art, seek to design a kind of nitrogen-doped carbon nanosphere/molybdenum disulfide
Sodium-ion battery negative plate, by having wrapped up one layer of class graphene transition metal molybdenum disulfide on natural black pigment nanosphere,
The material of carbon ball/molybdenum disulfide of N doping is prepared, and is prepared into battery.
To achieve these goals, nitrogen-doped carbon nanosphere of the present invention/molybdenum disulfide sodium-ion battery negative plate
Primary raw material parts by weight be：1-5 parts of natural black pigment, 1-20 parts of sodium molybdate, 8-40 parts of thioacetamide, conductive black 5-20
Part, 0.001-0.1 parts of PVDF (Kynoar), 1-2 parts of NMP (1-METHYLPYRROLIDONE), 20-200 parts of copper foil；It is wherein natural
Melanin is derived from inkfish capsule, and remaining is commercially available prod.
The invention further relates to nitrogen-doped carbon nanosphere/molybdenum disulfide sodium-ion battery negative plate preparation technology, specifically
Including：
(1) the inkfish capsule of select is broken and is taken out black liquor, be then added in ultra-pure water and centrifuged
Washing 2-10 time after, then by the melanin after centrifugation be put into bag filter progress dialysis purification, then the melanin after purification is entered
Row freeze-drying obtains natural black pigment powder standby to powder；
(2) according to weight proportion take natural black pigment powder be distributed to 25-35 times of weight than ultra-pure water in, carry out ultrasound
The finely dispersed natural black pigment aqueous solution is prepared after 10 minutes；
(3) take sodium molybdate and thioacetamide to be added in the ultra-pure water of 20-30 times of weight ratio according to weight proportion, carry out
Ultrasonic disperse is added to after 10-60 minutes in the natural black pigment aqueous solution of step (2) preparation, continues 10-60 points of magnetic agitation
Mixed dispersion liquid is obtained after clock；
(4) mixed dispersion liquid for obtaining step (3) is placed in ptfe autoclave, is entered at 150-200 DEG C
Water-filling thermal response 24-36 hours, then carries out washing and is dried to obtain nitrogen-doped carbon nanosphere/molybdenum disulfide sodium ion composite Nano
Material powder.
(5) CS/MoS for preparing step (4)2Composite nano materials powder and Super P (conductive black) and PVDF are (molten
In NMP) according to weight ratio be 15:5:2 ratio, which is put into mortar, grinds to form uniform slurry, and slurry then is coated on into copper foil
On, copper foil is placed under the infrared baking lamp that temperature is 60 DEG C and baked to dry tack free, then copper foil of the lamp after roasting is placed on vacuum
8-10h is toasted at 100-120 DEG C in baking oven, then by the copper foil roll-in after baking and a diameter of 12mm electrode slice is cut to and produces
Finished product.
Compared with prior art, it extracts melanin to the present invention from natural inkfish juice, is wrapped by hydro-thermal method on its surface
Molybdenum disulfide is wrapped up in, because the main component of melanin is poly-dopamine, is changed into the carbon ball of N doping, molybdenum disulfide in water-heat process
Nanometer sheet is uniformly coated on Nano carbon balls, and laod network is formed between nanometer sheet, serves good conductive network；Will system
Standby CS/MoS2Material is used as the negative material of sodium-ion battery, improves the stability at negative pole structure and interface, improves negative
The cyclical stability of pole, is conducive to commercially producing and applies；CS/MoS prepared by the present invention2Sodium-ion battery, in 80mA g-1
First discharge specific capacity under current density is up to 794mAh g-1；In 1000mA g-1Under high current density, remain at
343mAh g-1。
Brief description of the drawings：
The CS/MoS that Fig. 1 is prepared for the present invention2Composite nano materials scanning electron microscope (SEM) photograph.
The transmission electron microscope picture for the natural black pigment that Fig. 2 extracts for the present invention.
The CS/MoS that Fig. 3 is prepared for the present invention2Sodium-ion battery is in 80mAg-1Current density under cycle performance and storehouse
Human relations efficiency chart.
Fig. 4 is CS/MoS prepared by the embodiment of the present invention2The high rate performance of sodium-ion battery.
Embodiment：
It is described further below by embodiment and with reference to accompanying drawing.
Embodiment 1：
The primary raw material parts by weight of the nitrogen-doped carbon nanosphere that the present embodiment is related to/molybdenum disulfide sodium-ion battery negative plate
For：1-5 parts of natural black pigment, 1-20 parts of sodium molybdate, 8-40 parts of thioacetamide, 5-20 parts of conductive black, PVDF (polyvinylidene fluorides
Alkene) 0.001-0.1 parts, 1-2 parts of NMP (1-METHYLPYRROLIDONE), 20-200 parts of copper foil；Wherein natural black pigment is derived from inkfish capsule
In, remaining is commercially available prod.
The preparation technology of the nitrogen-doped carbon nanosphere that the present embodiment is further related to/molybdenum disulfide sodium-ion battery negative plate, tool
Body includes：
(1) the inkfish capsule of select is broken and is taken out black liquor, be then added in ultra-pure water and centrifuged
Washing 2-10 time after, then by the melanin after centrifugation be put into bag filter progress dialysis purification, then the melanin after purification is entered
Row freeze-drying obtains natural black pigment powder standby to powder；
(2) according to weight proportion take natural black pigment powder be distributed to 25-35 times of weight than ultra-pure water in, carry out ultrasound
The finely dispersed natural black pigment aqueous solution is prepared after 10 minutes；
(3) take sodium molybdate and thioacetamide to be added in the ultra-pure water of 20-30 times of weight ratio according to weight proportion, carry out
Ultrasonic disperse is added to after 10-60 minutes in the natural black pigment aqueous solution of step (2) preparation, continues 10-60 points of magnetic agitation
Mixed dispersion liquid is obtained after clock；
(4) mixed dispersion liquid for obtaining step (3) is placed in ptfe autoclave, is entered at 150-200 DEG C
Water-filling thermal response 24-36 hours, then carries out washing and is dried to obtain nitrogen-doped carbon nanosphere/molybdenum disulfide sodium ion composite Nano
Material powder.
(5) CS/MoS for preparing step (4)2Composite nano materials powder and Super P (conductive black) and PVDF are (molten
In NMP) according to weight ratio be 15:5:2 ratio, which is put into mortar, grinds to form uniform slurry, and slurry then is coated on into copper foil
On, copper foil is placed under the infrared baking lamp that temperature is 60 DEG C and baked to dry tack free, then copper foil of the lamp after roasting is placed on vacuum
8-10h is toasted at 100-120 DEG C in baking oven, then by the copper foil roll-in after baking and a diameter of 12mm electrode slice is cut to and produces
Finished product.
Sodium-ion battery negative plate made from the present embodiment and metallic sodium piece and electrolyte are assembled into sodium-ion battery, used
In carrying out constant current charge-discharge test, electrolyte is NaClO4It is 1 to be dissolved in volume ratio:1 ethylene carbonate (EC) and propylene carbonate
In ester (PC), and add 5vol% fluorinated ethylene carbonate (FEC)；Cyclic voltammetric (CV) test voltage range be
0.01V-3V, sweep speed is 0.1mVs-1, tester is CHI610E electrochemical workstations, and test result is as follows：
As shown in figure 3, CS/MoS2The 80mAg in sodium-ion battery-1Current density under cycle performance.Discharge first
Specific capacity is 794mAh g-1, initial charge specific capacity is 535mAh g-1, preceding 34 circle specific capacity is always growth state, to 34
Circle specific discharge capacity reaches 600mAh g-1, then there is downward trend, 80 circle specific discharge capacities remain at 288mAh g-1It is left
It is right.Fig. 4 is CS/MoS2High rate performance, in 20,40,80,320,640,1000mA g-1Current density under its discharge specific volume
Amount is respectively 468,465,439,397,369,342mAh g-1.Illustrate that material has good high rate performance, this may be with biology
There is provided good electric charge transmission channel is relevant for the good electric conductivity of matter carbon ball.
Claims (2)
1. a kind of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium-ion battery negative plate, it is characterised in that its primary raw material parts by weight
For：1-5 parts of natural black pigment, 1-20 parts of sodium molybdate, 8-40 parts of thioacetamide, 5-20 parts of conductive black, PVDF (polyvinylidene fluorides
Alkene) 0.001-0.1 parts, 1-2 parts of NMP (1-METHYLPYRROLIDONE), 20-200 parts of copper foil；Wherein natural black pigment is derived from inkfish capsule
In, remaining is commercially available prod.
2. a kind of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium-ion battery negative plate according to claim 1, its feature exists
Specifically included in the preparation technology of the nitrogen-doped carbon nanosphere/molybdenum disulfide sodium-ion battery negative plate：
(1) the inkfish capsule of select is broken and is taken out black liquor, be then added in ultra-pure water and carry out centrifuge washing
After 2-10 times, then by the melanin after centrifugation be put into bag filter carry out dialysis purification, then by after purification melanin carry out it is cold
It is lyophilized dry to powder, obtain natural black pigment powder standby；
(2) according to weight proportion take natural black pigment powder be distributed to 25-35 times of weight than ultra-pure water in, carry out ultrasound 10 points
The finely dispersed natural black pigment aqueous solution is prepared after clock；
(3) take sodium molybdate and thioacetamide to be added in the ultra-pure water of 20-30 times of weight ratio according to weight proportion, carry out ultrasound
In the natural black pigment aqueous solution that step (2) preparation is added to after scattered 10-60 minutes, continue magnetic agitation after 10-60 minutes
Obtain mixed dispersion liquid；
(4) mixed dispersion liquid for obtaining step (3) is placed in ptfe autoclave, and water-filling is entered at 150-200 DEG C
Thermal response 24-36 hours, then carries out washing and is dried to obtain nitrogen-doped carbon nanosphere/molybdenum disulfide sodium ion composite nano materials
Powder.
(5) CS/MoS for preparing step (4)2Composite nano materials powder (is dissolved in Super P (conductive black) and PVDF
NMP it is) 15 according to weight ratio:5:2 ratio, which is put into mortar, grinds to form uniform slurry, and slurry then is coated on into copper foil
On, copper foil is placed under the infrared baking lamp that temperature is 60 DEG C and baked to dry tack free, then copper foil of the lamp after roasting is placed on vacuum
8-10h is toasted at 100-120 DEG C in baking oven, then by the copper foil roll-in after baking and a diameter of 12mm electrode slice is cut to and produces
Finished product.
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Cited By (8)
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| CN107611428A (en) * | 2017-08-01 | 2018-01-19 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of battery molybdenum disulfide cathode size preparation method and products thereof and application |
| CN107697912A (en) * | 2017-09-30 | 2018-02-16 | 青岛大学 | A kind of preparation method of biomass-based porous agraphitic carbon nanosphere electrode material |
| CN107799757A (en) * | 2017-10-31 | 2018-03-13 | 青岛大学 | A kind of MoS2/ nitrogen-doped carbon pipe composite and its preparation method and application |
| 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 |
| CN109279583A (en) * | 2018-09-25 | 2019-01-29 | 岭南师范学院 | One kind two selenizing molybdenums/nitrogen-doped carbon composite nano materials and the preparation method and application thereof |
| CN109713258A (en) * | 2018-12-06 | 2019-05-03 | 盐城工学院 | A kind of cobalt doped molybdenum sulfide-graphene-carbon composite and its preparation method and application |
| US20210074992A1 (en) * | 2016-09-16 | 2021-03-11 | Pacesetter, Inc. | Battery Electrode And Methods Of Making |
| CN117613264A (en) * | 2024-01-23 | 2024-02-27 | 吉林嘉能钠电科技有限责任公司 | Molybdenum sulfide composite carbon sphere and preparation method and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20210074992A1 (en) * | 2016-09-16 | 2021-03-11 | Pacesetter, Inc. | Battery Electrode And Methods Of Making |
| US11735706B2 (en) * | 2016-09-16 | 2023-08-22 | Pacesetter, Inc. | Methods of making battery electrodes with tubes, optimized solvent to powder weight ratios, and specified calendar roller diameters |
| CN107611428A (en) * | 2017-08-01 | 2018-01-19 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of battery molybdenum disulfide cathode size preparation method and products thereof and application |
| CN107697912A (en) * | 2017-09-30 | 2018-02-16 | 青岛大学 | A kind of preparation method of biomass-based porous agraphitic carbon nanosphere electrode material |
| CN107799757A (en) * | 2017-10-31 | 2018-03-13 | 青岛大学 | A kind of MoS2/ nitrogen-doped carbon pipe composite and its preparation method and application |
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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 |
| CN109279583A (en) * | 2018-09-25 | 2019-01-29 | 岭南师范学院 | One kind two selenizing molybdenums/nitrogen-doped carbon composite nano materials and the preparation method and application thereof |
| CN109713258A (en) * | 2018-12-06 | 2019-05-03 | 盐城工学院 | A kind of cobalt doped molybdenum sulfide-graphene-carbon composite and its preparation method and application |
| CN117613264A (en) * | 2024-01-23 | 2024-02-27 | 吉林嘉能钠电科技有限责任公司 | Molybdenum sulfide composite carbon sphere and preparation method and application thereof |
| CN117613264B (en) * | 2024-01-23 | 2024-04-05 | 吉林嘉能钠电科技有限责任公司 | Molybdenum sulfide composite carbon sphere and preparation method and application thereof |
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