CN107248573A - Polyphosphazene is combined the preparation method of carbon composite electrode material for the molybdenum disulfide of carbon source - Google Patents

Polyphosphazene is combined the preparation method of carbon composite electrode material for the molybdenum disulfide of carbon source Download PDF

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Publication number
CN107248573A
CN107248573A CN201710491605.9A CN201710491605A CN107248573A CN 107248573 A CN107248573 A CN 107248573A CN 201710491605 A CN201710491605 A CN 201710491605A CN 107248573 A CN107248573 A CN 107248573A
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mos
molybdenum disulfide
warming
polyphosphazene
electrode material
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周泽平
魏晓娟
陈枫
赵正平
范萍
杨晋涛
钟明强
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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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
    • 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
    • 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
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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 provides a kind of preparation method of lithium battery composite carbon electrode material.The present invention is raw material using hexachlorocyclotriph,sphazene (HCCP) and 4,4' dihydroxydiphenylsulisomer (BPS), with triethylamine (TEA) for acid binding agent, is prepared under ultrasonication by a step precipitation polymerization method and is coated with MoS2Polyphosphazene microspheres, MoS is obtained after high temperature cabonization2@C composites, available for electrode material.The invention has the advantages that：The MoS being made2The features such as@C composites have high-specific surface area, good circulation and large current density electrical stability, high specific capacitance.

Description

Polyphosphazene is combined the preparation method of carbon composite electrode material for the molybdenum disulfide of carbon source
(1) technical field
The present invention relates to the preparation method that a kind of polyphosphazene is combined carbon composite electrode material for the molybdenum disulfide of carbon source.
(2) background technology
In recent years, for the research of lithium ion battery electrode material, raising efficiency for charge-discharge is concentrated mainly on, electricity is improved In terms of pond service life and the specific surface area of raising material.Research now, is mainly modified on the surface of carbon material, including Surface attachment nanometer phase, surface form nanometer micropore and the application of some other nanometer technology.The achievement of research is a lot of, also opens up Show that the development prospect of lithium ion battery is very considerable.
Molybdenum disulfide (MoS2) be used as lithium ion battery negative material theoretical capacity it is very big, be a kind of electricity of great prospect Pole material selection；Functional polyalkylene phosphonitrile micro Nano material has template-mediated self assembly, carbonization mesoporous material precursor, molecule knot The characteristics such as structure designability, are a kind of carbon sources of the porous carbon materials of great prospect.
So far, also there is the MoS synthesized using hydro-thermal method2Nanometer sheet be made electrode report [《Materials Research Bulletin》,2009,44(9):1811-1815], specific capacitance is up to 748m Ah/g.But the electrode remains unchanged and deposited Trigger MoS in the embedding de- process of lithium ion2The problem of change of volume, it is not stabilization to cause its actual chemical property.It is porous Carbon material lignin micro Nano material is a kind of good and with the electrode material of actual use value, steady with good structure It is qualitative, by itself and MoS2It is compound to be expected to have both advantages concurrently.
(3) content of the invention
It is an object of the present invention to provide a kind of constitutionally stable MoS2The preparation method of@C composites.
The technical solution adopted by the present invention is：
A kind of polyphosphazene is the MoS of carbon source2The preparation method of@C combination electrode materials, methods described includes：
(1) hexachlorocyclotriph,sphazene (HCCP) and 4,4' dihydroxydiphenyl sulfone (BPS) are added in advance through ultrasonic disperse In molybdenum disulfide acetonitrile solution, then ultrasonic disperse；
(2) step (1) dispersion liquid is slowly added to triethylamine (TEA) in ultrasound, continues ultrasonic disperse after 3~5 hours, from The heart is simultaneously washed 3 times with ethanol and deionization, obtains powder product；
(3) step (2) 60~80 DEG C of powder product vacuum drying 24~36 hours, obtains dry MoS2@polyphosphazenes-sulfone (PZS) nanoparticle powder；
(4) the drying MoS for obtaining step (3)2@polyphosphazenes-sulfone nanoparticle powder is placed in N2Forged in atmosphere through tube furnace Burn, obtain MoS2@C combination electrode materials.
Further, the ratio between the hexachlorocyclotriph,sphazene, 4,4'- dihydroxydiphenylsulisomers, molybdenum disulfide quality consumption are：340 ~350：580~600：50~250, preferably 345:595:64.
Further, calcine technology is in the step (4)：Be warming up to 300 DEG C with 5 DEG C/min speed, then with 2 DEG C/ Min speed is warming up to after 500 DEG C, insulation 1h, 900 DEG C is warming up to 5 DEG C/min, with 6 DEG C/min speed after being incubated through 1h 300 DEG C are cooled to, then cools to the furnace after 100 DEG C and takes out.
It is preferably 6000r/min, 5min/ times that step (2) centrifugation, which is set,.
Molybdenum disulfide described in the step (1) is preferably lamellar structure.
Molybdenum disulfide acetonitrile solution concentration is preferably 0.1~0.5g/L described in the step (1).
The rate of addition of triethylamine is preferably 15mL/h in the step (2).
Ultrasonic power is preferably 300~500W in the step (2).
In the present invention, described hexachlorocyclotriph,sphazene (HCCP) and 4,4'- dihydroxydiphenylsulisomer (BPS), in ultrasonication Scattered molybdenum disulfide (the MoS of condensation methods cladding is precipitated by a step down2), obtain being coated with MoS2Polyphosphazene-sulfone (PZS) receive Meter Wei Qiu.
The MoS that the present invention is provided2@C composites have coreshell type structure, specific surface area is higher, it is to avoid molybdenum disulfide Volume Changes.
The invention provides the MoS2As a result@C composites show as the application of lithium ion battery negative material, The features such as it has good circulation and large current density electrical stability, high specific capacitance.
The beneficial effects are mainly as follows：
1、MoS2PZS microballoons have successfully been coated, have been core shell structure, specific surface area is big, is 5.5m2/ g or so.It is this poly- Phosphonitrile, which is combined sulfur materials, can combine polyphosphazene and MoS2Both outstanding chemical properties.
2nd, the carbon material that PZS complex microspheres are obtained through high temperature cabonization still keeps spherical, a diameter of 550nm or so, and particle is equal It is even, and because the distillation effusion of PZS small moleculars forms porous type, aperture is 0~100nm, and these ducts can realize MoS2With Lithium ion contact in electrolyte, and further improve the contact area of material and electrolyte.
3、MoS2@C composites have higher specific capacitance (1080mAh/g), and still have good under multiple circulation Retention, shows the chemical property of good and stable circulation.
(4) illustrate
Fig. 1 is MoS prepared by embodiment 32The SEM figures of@C composites；
Fig. 2 is MoS prepared by embodiment 32The desorption absorption figure and size distribution figure of the nitrogen of@C composites；
Fig. 3 is MoS prepared by embodiment 32The cyclic voltammogram of@C composite electrode materials；
Fig. 4 is the MoS prepared using embodiment 32The constant current charge-discharge diagram of@C composite electrode materials；
Fig. 5 is the MoS prepared using embodiment 32The specific capacitance figure of@C composite electrode materials.
(5) embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in This：
Embodiment 1：
Take 0.064g MoS2In 500ml acetonitrile solutions, then the ultrasound 1h in ultrasonic cell disrupte machine turns solution Move on in 500ml round-bottomed flasks, the ultrasound 30min in ultra sonic bath.0.345g HCCP and 0.595g are added into round-bottomed flask again BPS, the ultrasound 30min in ultra sonic bath.50ml TEA are slowly added dropwise and shake, addition finish after under 300w power ultrasound 5h. The solution obtained after ultrasound is centrifuged into (6000r/min, 5min/ times) in supercentrifuge, obtained solid is through absolute ethyl alcohol Wash centrifugation three times respectively with deionized water, product is placed in vacuum drying chamber (60 DEG C) and dried after 24h in tube furnace (with 5 DEG C/min speed is warming up to 300 DEG C, then is warming up to 2 DEG C/min speed after 500 DEG C, insulation 1h, heated up with 5 DEG C/min To 900 DEG C, 300 DEG C are cooled to 6 DEG C/min speed after being incubated through 1h, then cools to the furnace after 100 DEG C and takes out) calcine To MoS2@C composites.Gained MoS2Preferably, its particle diameter is 280~550nm to@C composites particle dispersibility.
Embodiment 2：
Other are same as Example 1, and difference is that the ultrasonic power reacted is 400w.Gained MoS2@C composite woods Expect particle dispersibility preferably, a diameter of 275-385nm.
Embodiment 3：
Other are same as Example 1, and difference is that the ultrasonic power reacted is 500w.Its SEM figure is referring to Fig. 1, nitrogen The desorption absorption figure and size distribution figure of gas are referring to Fig. 2, as seen from the figure, gained MoS2@C composites particle dispersibility compared with Good, there is back stagnant ring in a diameter of 483-502nm, curve, illustrates that material has pore passage structure, and specific surface area is 5.5m2/ g, pore volume For 0.035cm3/g。
Embodiment 4：Comparative example 1
Other are same as Example 1, and difference is to be added without MoS2.As a result show that its specific capacitance of discharging only has 596mAh/g。
Embodiment 5：Application Example 1
By MoS made from embodiment 32@C composites and conductive agent (acetylene black), polytetrafluoroethylene PTFE (binding agent) By 8：1：1 ratio mixing, is equably coated in the nickel foam of precise, working electrode is made, and makees to join with Ag/AgCl electrodes Than electrode, it is that electrolyte constitutes three-electrode system that platinized platinum, which is used as auxiliary electrode and potassium hydroxide solution, for testing electrochemistry Energy.
The MoS prepared using the present invention2The cyclic voltammogram of@C composite electrode materials is referring to Fig. 3, constant current charge-discharge Figure is referring to Fig. 4 (figure line is 0.1~0.005V respectively from top to bottom), and specific capacitance figure is referring to Fig. 5, and as seen from the figure, prepared by the present invention MoS2@C composites have preferable discharge and recharge invertibity, with higher specific capacitance (1080mAh/g), and multiple Still there is good retention under circulation, show the chemical property of good and stable circulation.

Claims (8)

1. a kind of polyphosphazene is the MoS of carbon source2The preparation method of@C combination electrode materials, methods described includes：
(1) that hexachlorocyclotriph,sphazene and 4,4' dihydroxydiphenyl sulfone are added into the prior molybdenum disulfide acetonitrile through ultrasonic disperse is molten In liquid, then ultrasonic disperse；
(2) step (1) dispersion liquid is slowly added to triethylamine in ultrasound, continues ultrasonic disperse after 3~5 hours, centrifuges and use second Alcohol and deionization are washed 3 times, obtain powder product；
(3) step (2) 60~80 DEG C of powder product vacuum drying 24~36 hours, obtains dry MoS2@polyphosphazenes-sulfone nanoparticle Powder；
(4) the drying MoS for obtaining step (3)2@polyphosphazenes-sulfone nanoparticle powder is placed in N2Calcined in atmosphere through tube furnace, Obtain MoS2@C combination electrode materials.
2. the method as described in claim 1, it is characterised in that：The hexachlorocyclotriph,sphazene, 4,4' dihydroxydiphenyl sulfone, two The ratio between molybdenum sulfide quality consumption is：340~350：580~600：50~250.
3. the method as described in claim 1, it is characterised in that calcine technology is in the step (4)：With 5 DEG C/min speed 300 DEG C are warming up to, then is warming up to 2 DEG C/min speed after 500 DEG C, insulation 1h, 900 DEG C is warming up to 5 DEG C/min, is protected through 1h 300 DEG C are cooled to 6 DEG C/min speed after temperature, then cools to the furnace after 100 DEG C and takes out.
4. the method as described in claim 1, it is characterised in that step (2) centrifugation is set to 6000r/min, 5min/ times.
5. the method as described in claim 1, it is characterised in that the molybdenum disulfide described in the step (1) is lamellar structure.
6. the method as described in claim 1, it is characterised in that molybdenum disulfide acetonitrile solution concentration is described in the step (1) 0.1~0.5g/L.
7. the method as described in claim 1, it is characterised in that the rate of addition of triethylamine is 15mL/h in the step (2).
8. the method as described in claim 1, it is characterised in that ultrasonic power is 300~500W in the step (2).
CN201710491605.9A 2017-06-26 2017-06-26 Polyphosphazene is combined the preparation method of carbon composite electrode material for the molybdenum disulfide of carbon source Pending CN107248573A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109137144A (en) * 2018-08-06 2019-01-04 浙江工业大学 The preparation method of molybdenum disulfide composite hollow carbon nano-fiber materials
CN109161023A (en) * 2018-08-06 2019-01-08 浙江工业大学 Polyphosphazene microspheres are the preparation method of the molybdenum disulfide composite material of carbon source
CN110416621A (en) * 2019-06-12 2019-11-05 中国科学院化学研究所 A method of inorganic solid electrolyte is handled using phosphorus-containing matter
CN110474062A (en) * 2019-08-02 2019-11-19 北京化工大学常州先进材料研究院 A kind of preparation and application of efficient MXene titanium carbide cell catalyst
CN110729135A (en) * 2019-09-11 2020-01-24 江苏大学 Preparation method of molybdenum disulfide/polyphosphazene/ferroferric oxide electrode material
CN112086638A (en) * 2019-06-12 2020-12-15 中国科学院化学研究所 Method for reducing alkalinity of positive electrode material by using phosphorus-containing organic matter
CN113540447A (en) * 2021-06-29 2021-10-22 暨南大学 Preparation and application of ultra-long cycle polyatomic doping hollow carbon electrode material
CN115010537A (en) * 2022-05-06 2022-09-06 广州大丘有机农产有限公司 Fermentation treatment process of agricultural and forestry waste

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CN105047914A (en) * 2015-05-28 2015-11-11 东南大学 Lithium-ion battery anode material molybdenum disulfide/carbon and preparation method thereof

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CN105047914A (en) * 2015-05-28 2015-11-11 东南大学 Lithium-ion battery anode material molybdenum disulfide/carbon and preparation method thereof

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109137144A (en) * 2018-08-06 2019-01-04 浙江工业大学 The preparation method of molybdenum disulfide composite hollow carbon nano-fiber materials
CN109161023A (en) * 2018-08-06 2019-01-08 浙江工业大学 Polyphosphazene microspheres are the preparation method of the molybdenum disulfide composite material of carbon source
CN110416621A (en) * 2019-06-12 2019-11-05 中国科学院化学研究所 A method of inorganic solid electrolyte is handled using phosphorus-containing matter
CN112086638A (en) * 2019-06-12 2020-12-15 中国科学院化学研究所 Method for reducing alkalinity of positive electrode material by using phosphorus-containing organic matter
CN112086638B (en) * 2019-06-12 2021-12-21 中国科学院化学研究所 Method for reducing alkalinity of positive electrode material by using phosphorus-containing organic matter
CN110474062A (en) * 2019-08-02 2019-11-19 北京化工大学常州先进材料研究院 A kind of preparation and application of efficient MXene titanium carbide cell catalyst
CN110729135A (en) * 2019-09-11 2020-01-24 江苏大学 Preparation method of molybdenum disulfide/polyphosphazene/ferroferric oxide electrode material
CN113540447A (en) * 2021-06-29 2021-10-22 暨南大学 Preparation and application of ultra-long cycle polyatomic doping hollow carbon electrode material
CN115010537A (en) * 2022-05-06 2022-09-06 广州大丘有机农产有限公司 Fermentation treatment process of agricultural and forestry waste

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