CN107195883A - A kind of preparation method of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium ion composite nano materials - Google Patents

A kind of preparation method of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium ion composite nano materials Download PDF

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Publication number
CN107195883A
CN107195883A CN201710400707.5A CN201710400707A CN107195883A CN 107195883 A CN107195883 A CN 107195883A CN 201710400707 A CN201710400707 A CN 201710400707A CN 107195883 A CN107195883 A CN 107195883A
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molybdenum disulfide
preparation
nitrogen
doped carbon
sodium
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CN201710400707.5A
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张文玲
刘敬权
冯红彬
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Qingdao University
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Qingdao University
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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
    • H01M4/366—Composites as layered products
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • 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
    • 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
    • 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 preparation method of sodium-ion battery negative active core-shell material, more particularly to a kind of preparation method of nitrogen-doped carbon nanosphere/molybdenum disulfide anode material of lithium-ion battery, 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；Its preparation method is simple, environmental protection and effectively；Melanin is extracted 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, is conducive to commercially producing and applies.

Description

A kind of preparation of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium ion composite nano materials Method
Technical field：
The invention belongs to battery preparation technology field, it is related to a kind of preparation method of sodium-ion battery negative active core-shell material, The preparation method of more particularly to a kind of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium anode material of lithium-ion battery, by natural One layer of class graphene transition metal molybdenum disulfide has been wrapped up on melanin nanosphere, carbon ball/molybdenum disulfide of N doping is prepared (MoS2)(carbon spheres,CS)(CS/MoS2) material.
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 preparation method of nitrogen-doped carbon nanosphere/molybdenum disulfide anode material of lithium-ion battery, With reference to the high theoretical specific capacity of molybdenum disulfide and the advantage of N doping carbon ball high conductivity, there is high charge-discharge specific volume for preparing The sodium-ion battery of amount, good high rate performance 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 The preparation method of sodium anode material of lithium-ion battery, by having wrapped up one layer of class graphene transition on natural black pigment nanosphere Metal dithionite molybdenum, prepares the material of carbon ball/molybdenum disulfide of N doping.
To achieve these goals, nitrogen-doped carbon nanosphere of the present invention/molybdenum disulfide sodium sodium-ion battery negative pole The primary raw material parts by weight of material are：1-5 parts of natural black pigment, 1-20 parts of sodium molybdate, 8-40 parts of thioacetamide.
The preparation technology tool of the nitrogen-doped carbon nanosphere that the present embodiment is related to/molybdenum disulfide sodium anode material of lithium-ion battery 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 progress washing is dried to obtain nitrogen-doped carbon nanosphere/molybdenum disulfide sodium sodium-ion battery and born Pole material powder.
Compared with prior art, its preparation method is simple, environmental protection and effectively by the present invention；The present invention is from natural inkfish juice Middle extraction melanin, molybdenum disulfide is wrapped up by hydro-thermal method on its surface, because the main component of melanin is poly-dopamine, water It is changed into the carbon ball of N doping in thermal process, molybdenum disulfide nano sheet is uniformly coated on Nano carbon balls, is formed between nanometer sheet Laod network, serves good conductive network；By the CS/MoS of preparation2Material is used as the negative material of sodium-ion battery, carries The high stability of negative pole structure and interface, improves the cyclical stability of negative pole, is conducive to commercially producing and applies；This hair The CS/MoS of bright preparation2Negative pole stores up sodium, in 80mA g-1First discharge specific capacity under current density is up to 794mAh g-1； 1000mA g-1Under high current density, 343mAh g are remained at-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 80mA g-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 weight of the nitrogen-doped carbon nanosphere that the present embodiment is related to/molybdenum disulfide sodium anode material of lithium-ion battery Measuring part is：1-5 parts of natural black pigment, 1-20 parts of sodium molybdate, 8-40 parts of thioacetamide.
The preparation technology tool of the nitrogen-doped carbon nanosphere that the present embodiment is related to/molybdenum disulfide sodium anode material of lithium-ion battery 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 progress washing is dried to obtain nitrogen-doped carbon nanosphere/molybdenum disulfide sodium sodium-ion battery and born Pole material powder.
Embodiment 2：
The present embodiment is related to a kind of preparation method of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium-ion battery negative plate, its Primary raw material parts by weight are：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；Wherein day Right melanin is derived from inkfish capsule, and remaining is commercially available prod.
The present embodiment further relates to a kind of preparation technology of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium-ion battery negative plate, Specifically include：
By the CS/MoS of preparation2Composite nano materials powder, Super P (conductive black) and PVDF (being dissolved in NMP) according to Weight ratio is 15:5:2 ratio, which is put into mortar, grinds to form uniform slurry, then slurry is coated on copper foil, by copper foil It is placed under the infrared baking lamp that temperature is 60 DEG C and bakes to dry tack free, then copper foil of the lamp after roasting is placed in vacuum drying oven 100-120 DEG C of baking 8-10h, then by the copper foil roll-in after baking and is cut to a diameter of 12mm electrode slice and gets product.
Sodium-ion battery negative plate, metallic sodium piece, electrolyte made from the present embodiment are assembled into sodium-ion battery, are used for Constant current charge-discharge test is carried out, electrolyte is NaClO4It is 1 to be dissolved in volume ratio:1 ethylene carbonate (EC) and propene carbonate (PC) in, and 5vol% fluorinated ethylene carbonate (FEC) is added；The voltage range of cyclic voltammetric (CV) test is 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 80mA g 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. the preparation method of a kind of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium ion composite nano materials, it is characterised in that it is made Standby technique is specifically included：
(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.
2. a kind of preparation of nitrogen-doped carbon nanosphere/molybdenum disulfide anode material of lithium-ion battery according to claim 1 Method, it is characterised in that the primary raw material parts by weight of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium ion composite nanometre powder are：My god Right 1-5 parts of melanin, 1-20 parts of sodium molybdate, 8-40 parts of thioacetamide.
CN201710400707.5A 2017-05-31 2017-05-31 A kind of preparation method of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium ion composite nano materials Pending CN107195883A (en)

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Cited By (6)

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CN107673348A (en) * 2017-09-30 2018-02-09 青岛海澄知识产权事务有限公司 A kind of biomass-based porous agraphitic carbon nanosphere sodium-ion battery
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
CN110357161A (en) * 2019-07-03 2019-10-22 山东省分析测试中心 A kind of MCHS@molybdenum disulfide nano-composite material and its preparation method and application based on core-shell structure
CN111477855A (en) * 2020-04-24 2020-07-31 喻明兵 Mesoporous carbon coated MoS2The negative electrode material of the sodium ion battery and the preparation method thereof
CN114976007A (en) * 2022-06-08 2022-08-30 中国科学院化学研究所 Method for controllably constructing sulfide coating layer
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 (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107673348A (en) * 2017-09-30 2018-02-09 青岛海澄知识产权事务有限公司 A kind of biomass-based porous agraphitic carbon nanosphere sodium-ion battery
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
CN110357161A (en) * 2019-07-03 2019-10-22 山东省分析测试中心 A kind of MCHS@molybdenum disulfide nano-composite material and its preparation method and application based on core-shell structure
CN110357161B (en) * 2019-07-03 2021-09-28 山东省分析测试中心 MCHS @ molybdenum disulfide nanocomposite based on core-shell structure and preparation method and application thereof
CN111477855A (en) * 2020-04-24 2020-07-31 喻明兵 Mesoporous carbon coated MoS2The negative electrode material of the sodium ion battery and the preparation method thereof
CN114976007A (en) * 2022-06-08 2022-08-30 中国科学院化学研究所 Method for controllably constructing sulfide coating layer
CN114976007B (en) * 2022-06-08 2024-02-20 中国科学院化学研究所 Method for controllably constructing sulfide coating layer
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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Application publication date: 20170922