CN108878159A - 2D/1D structure molybdenum disulfide/bismuth sulfide nano composite material and preparation method thereof - Google Patents

2D/1D structure molybdenum disulfide/bismuth sulfide nano composite material and preparation method thereof Download PDF

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Publication number
CN108878159A
CN108878159A CN201810500406.4A CN201810500406A CN108878159A CN 108878159 A CN108878159 A CN 108878159A CN 201810500406 A CN201810500406 A CN 201810500406A CN 108878159 A CN108878159 A CN 108878159A
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preparation
composite material
mos
molybdenum disulfide
nano composite
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严学华
王静静
沙大巍
周辰
王琼
王东风
潘建梅
程晓农
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Jiangsu University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/24Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Power Engineering (AREA)
  • Materials Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Composite Materials (AREA)
  • Manufacturing & Machinery (AREA)
  • Electric Double-Layer Capacitors Or The Like (AREA)

Abstract

The present invention relates to electrode material for super capacitor, refer in particular to a kind of 2D/1D structure molybdenum disulfide/bismuth sulfide nano composite material and preparation method thereof.Bi is weighed in proportion2S3Nanometer rods, Na2MoO4·2H2O and thiocarbamide are dissolved in deionized water, and magnetic agitation 1h is allowed to evenly dispersed at room temperature.Gained mixture is transferred in 50mL reaction kettle, is reacted for 24 hours at 210 DEG C, is made Na2MoO4·2H2O is with thiocarbamide fully reacting and in Bi2S3Nanorod surfaces generate MoS2Nanometer sheet.It takes out and is cooled to room temperature after reaction, be centrifuged with deionized water and ethanol wash, and dry in a vacuum drying oven, MoS can be obtained2/Bi2S3Nanocomposite.

Description

2D/1D structure molybdenum disulfide/bismuth sulfide nano composite material and preparation method thereof
Technical field
The present invention relates to electrode material for super capacitor, and it is compound to refer in particular to a kind of 2D/1D structure molybdenum disulfide/bismuth sulfide nano Material preparation method.Molybdenum disulfide/bismuth sulfide nano composite material is prepared by two one-step hydrothermals.The material is with higher Specific capacitance and preferable cyclical stability, and preparation process is simple, environmentally protective, as novel molybdenum-disulfide radical electrode material, There is application prospect in energy storage fields such as supercapacitor, lithium batteries.
Background technique
The getting worse of energy crisis and environmental problem has caused people to the great research enthusiasm of energy storage device.Newly Type energy-storage travelling wave tube plays a crucial role the efficient and sustainable use of the energy such as the appearance of supercapacitor (SC). Compared with traditional rechargeable battery and capacitor, SC has bigger power density and energy density.According to charge storage mechanism Difference, the electrode material of SC can be divided into double layer capacitor (EDLC) electrode material and fake capacitance electrode material.With EDLC Electrode material is compared, and fake capacitance electrode material is because occurring in the faraday's reaction on electrode/electrolyte surface ratio with higher Capacitor.
In recent years, sulfide is as electrode material, because of its own intrinsic physical property and chemical property, in energy field Attract extensive attention.Greatly, and the covalent radius (60pm) of O compares S to electronegativity (2.58) of the electronegativity (3.44) of O than S (104pm's) is small, therefore is compared to M-O key, and the M-S bond resultant force that transition metal and sulphur anion are formed is weaker, transition gold Belong to sulfide to be easier that redox reaction occurs.Compared with traditional carbon material, most of sulfide all have than carbon electrode It is higher by several times of specific capacitance.And compared with metal oxide, sulfide also has more good lead other than with high specific capacitance Electrically, and cheap, it is resourceful, it is convieniently synthesized, thus it is considered to have bigger market value and bigger application is dived The electrode material of energy.
Transition-metal dichalcogenide MoS with class graphene layer structure2, the specific surface area of Yin Qigao, good Electrochemical electrical conductivity and preferable chemical stability, become the research emphasis of energy storage material.MoS2Two S atom folders in layer A miscellaneous Mo atom in the layer structure of sandwich type, and is then between the layers faint Van der Waals force connection.By stripping From two-dimensional layer nanometer MoS2With biggish specific surface area and have preferable absorption property, convenient for charge aggregation and deposit Storage.Monodimension nano stick bismuth sulfide Bi2S3With narrow direct band gap and quick electronics transfer.In MoS2Nanometer sheet is grown in Bi2S3During in nanometer rods, composite material forms heterojunction boundary abundant under the action of Van der Waals epitaxial growth, By the advantage of the two, i.e. Bi2S3Swift electron transfer and MoS2Biggish surface area combines, and can be improved composite material Specific capacitance and cyclical stability.
Summary of the invention
It is a kind of with the stable compound pattern of 2D/1D the invention aims to provide, and MoS can be improved2Monomer is than electricity Hold the MoS with cyclical stability2/Bi2S3Composite material.Products obtained therefrom is a kind of stable structure and has good chemical property Functional composite material.
MoS in the present invention2/Bi2S3Composite material has stable, uniform microscopic appearance, MoS2Nanometer sheet homoepitaxial In Bi2S3Nanorod surfaces.As shown in Figure 1 and Figure 2.
MoS in the present invention2/Bi2S3Composite material has good chemical property, in MoS2On the basis of nanometer sheet It is obviously improved.In test voltage -0.2~0.8V of range, scanning speed is 10 to 100mV s-1CV loop test in, MoS2/Bi2S3Composite material exhibits go out excellent chemical property, in 10mV s-1Sweep speed under, specific capacity reaches 125.1F g-1, as shown in Figure 3.Electrode material is 1A g in current density-1After Shi Xunhuan 2000 times, capacity retention ratio is 83.2%, as shown in Figure 4.
Realize the technical scheme adopted by the invention is as follows:A kind of MoS2/Bi2S3Nanocomposite, by two-step method system , have many advantages, such as simple process, low in cost, green non-pollution, two-dimentional MoS2Nanometer sheet homoepitaxial is in one-dimensional Bi2S3It receives Rice stick surface, and excellent chemical property is shown, preparation step is as follows:
(1) one-dimensional Bi is prepared first2S3Nanometer rods.Weigh 0.38g Bi (NO3)3·5H2O and 0.19g thiocarbamide is dissolved in In 30mL deionized water, 30min is stirred.Acquired solution is transferred in 50mL reaction kettle, is reacted at 200 DEG C for 24 hours, reaction terminates It takes out and is cooled to room temperature afterwards, be centrifuged with deionized water and ethanol wash, and dry in a vacuum drying oven, Bi can be obtained2S3It receives Rice stick.
(2) above-mentioned gained Bi is weighed in proportion2S3Nanometer rods, Na2MoO4·2H2O and thiocarbamide are dissolved in deionized water, room The lower magnetic agitation 1h of temperature is allowed to evenly dispersed.Bi2S3Nanometer rods, Na2MoO4·2H2O, the mass volume ratio of thiocarbamide and deionized water For:0.27g:0.045g:0.0425g:40mL.Gained mixture is transferred in 50mL reaction kettle, is reacted for 24 hours, is made at 210 DEG C Na2MoO4·2H2O is with thiocarbamide fully reacting and in Bi2S3Nanorod surfaces generate MoS2Nanometer sheet.Cooling is taken out after reaction It to room temperature, is centrifuged with deionized water and ethanol wash, and dried in a vacuum drying oven, MoS can be obtained2/Bi2S3Nanometer is multiple Condensation material.
Detailed description of the invention
Fig. 1 is MoS2/Bi2S3The scanning electron microscope (SEM) photograph of composite material.
Fig. 2 is MoS2/Bi2S3The transmission electron microscope picture of composite material.
Fig. 3 is MoS2/Bi2S3CV curve graph of the composite material under different scanning rates.
Fig. 4 is MoS2/Bi2S3Composite material is 1A g in current density-1When cycle performance.
Specific embodiment
Embodiment of the present invention is a kind of simple process, low in cost, environmentally protective preparation method, passes through hydro-thermal method Prepare MoS2/Bi2S3Composite material, the compound shape characteristic with 2D/1D, in MoS2Than electricity on the basis of nanometer sheet monomer Hold and cyclical stability has biggish promotion.
MoS in the present invention2/Bi2S3Composite material has good chemical property.Test voltage range -0.2~ 0.8V, scanning speed are 10 to 100mV s-1CV loop test in, MoS2/Bi2S3Composite material exhibits go out excellent electrochemistry Performance, in 10mV s-1Sweep speed under, specific capacity has reached 125.1F g-1.Electrode material is 1Ag in current density-1When After circulation 2000 times, capacity retention ratio 83.2%.
The present invention relates to excellent chemical property MoS2/Bi2S3The preparation method of composite material, includes the following steps:
(1) one-dimensional Bi is prepared first2S3Nanometer rods weigh 0.38g Bi (NO3)3·5H2O and 0.19g thiocarbamide is dissolved in In 30mL deionized water, 30min is stirred.Acquired solution is transferred in 50mL reaction kettle, is reacted at 200 DEG C for 24 hours, reaction terminates It takes out and is cooled to room temperature afterwards, be centrifuged with deionized water and ethanol wash, and dry in a vacuum drying oven, Bi can be obtained2S3It receives Rice stick.
(2) above-mentioned 0.27g Bi is weighed2S3Nanometer rods, 0.045g Na2MoO4·2H2O and 0.0425g thiocarbamide is dissolved in In 40mL deionized water, magnetic agitation 1h is allowed to evenly dispersed at room temperature.Gained mixture is transferred in 50mL reaction kettle, It is reacted at 210 DEG C for 24 hours, makes Na2MoO4·2H2O is with thiocarbamide fully reacting and in Bi2S3Nanorod surfaces generate MoS2Nanometer sheet. It takes out and is cooled to room temperature after reaction, be centrifuged with deionized water and ethanol wash, and dry in a vacuum drying oven.

Claims (5)

1.2D/1D structure molybdenum disulfide/bismuth sulfide nano composite material and preparation method thereof, the material is by MoS2Nanometer sheet and Bi2S3 Two kinds of Material claddings of nanometer rods form, the shape characteristic with 2D/1D;Wherein two dimension MoS2Nanometer sheet homoepitaxial is one-dimensional Bi2S3Nanorod surfaces avoid two-dimensional material and reunite during the preparation process, provide more activity for electrochemical reaction Reaction site;One-dimensional material while promoting electronic and ionic quickly to transmit, answer by the part born in electrochemical reaction process Power effect, is conducive to the holding of composite structure, improves cyclical stability of the electrode material when long-time uses, special Sign is that the preparation method is as follows:Bi is weighed in proportion2S3Nanometer rods, Na2MoO4·2H2O and thiocarbamide are dissolved in deionized water In, magnetic agitation is allowed to evenly dispersed at room temperature;Gained mixture, which is transferred in reaction kettle, carries out hydro-thermal reaction, makes Na2MoO4· 2H2O is with thiocarbamide fully reacting and in Bi2S3Nanorod surfaces generate MoS2Nanometer sheet is taken out be cooled to room temperature after reaction, It is centrifuged with deionized water and ethanol wash, and dried in a vacuum drying oven, 2D/1D structure MoS can be obtained2/Bi2S3Nanometer Composite material.
2. 2D/1D structure molybdenum disulfide/bismuth sulfide nano composite material and preparation method thereof as described in claim 1, feature exist In the time of the magnetic agitation is 1h.
3. 2D/1D structure molybdenum disulfide/bismuth sulfide nano composite material and preparation method thereof as described in claim 1, feature exist In the Bi2S3Nanometer rods, Na2MoO4·2H2O, thiocarbamide and the mass volume ratio of deionized water are:0.27g:0.045g: 0.0425g:40mL。
4. 2D/1D structure molybdenum disulfide/bismuth sulfide nano composite material and preparation method thereof as described in claim 1, feature exist In the reaction condition is to react for 24 hours at 210 DEG C.
5. 2D/1D structure molybdenum disulfide/bismuth sulfide nano composite material purposes of method preparation as described in claim 1, Molybdenum-disulfide radical electrode material is used as in supercapacitor, lithium battery energy storage battery field.
CN201810500406.4A 2018-05-23 2018-05-23 2D/1D structure molybdenum disulfide/bismuth sulfide nano composite material and preparation method thereof Withdrawn CN108878159A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110180560A (en) * 2019-05-28 2019-08-30 广州大学 A kind of nano bar-shape bismuth doping molybdenum sulfide sphere multiphase Fenton catalyst and its preparation method and application
CN110289416A (en) * 2019-06-26 2019-09-27 中南大学 A kind of preparation method of anode material of lithium-ion battery bismuth molybdenum bimetallic sulfide
CN110380042A (en) * 2019-08-08 2019-10-25 山东大学 Aluminum secondary battery positive electrode, battery and preparation method
CN113735181A (en) * 2021-09-06 2021-12-03 安徽工业大学 Antimony-cobalt sulfide-carbon composite nanorod and preparation method and application thereof
CN113735168A (en) * 2021-09-06 2021-12-03 安徽工业大学 Antimony-molybdenum sulfide-carbon composite material and preparation method and application thereof
CN114094078A (en) * 2021-11-16 2022-02-25 中国科学院深圳先进技术研究院 Nitrogen-doped carbon-coated metal sulfide heterojunction material, preparation method and battery application
WO2023087148A1 (en) * 2021-11-16 2023-05-25 中国科学院深圳先进技术研究院 Sulfide composite material for metal-ion battery, preparation method therefor, and application thereof

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CN103641169A (en) * 2013-11-12 2014-03-19 江苏大学 Synthetic method of Bi2S3-MoS2 nanometer heterostructure
CN104491888A (en) * 2014-12-18 2015-04-08 中国科学院上海硅酸盐研究所 Multifunctional diagnosis and treatment agent based on MoS2/Bi2S3-PEG nanosheet as well as preparation method and application of multifunctional diagnosis and treatment agent
CN107681142A (en) * 2017-09-29 2018-02-09 合肥工业大学 A kind of molybdenum disulfide cladding carbon nano-fiber as lithium ion battery negative material and preparation method thereof
CN107978742A (en) * 2017-11-17 2018-05-01 齐鲁工业大学 A kind of C doping flowered-spherical titanium dioxide/molybdenum disulfide composite materials formed by nanometer sheet and preparation method thereof

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WO2011149991A1 (en) * 2010-05-24 2011-12-01 The Regents Of The University Of California Inorganic nanostructure-organic polymer heterostructures useful for thermoelectric devices
CN103641169A (en) * 2013-11-12 2014-03-19 江苏大学 Synthetic method of Bi2S3-MoS2 nanometer heterostructure
CN104491888A (en) * 2014-12-18 2015-04-08 中国科学院上海硅酸盐研究所 Multifunctional diagnosis and treatment agent based on MoS2/Bi2S3-PEG nanosheet as well as preparation method and application of multifunctional diagnosis and treatment agent
CN107681142A (en) * 2017-09-29 2018-02-09 合肥工业大学 A kind of molybdenum disulfide cladding carbon nano-fiber as lithium ion battery negative material and preparation method thereof
CN107978742A (en) * 2017-11-17 2018-05-01 齐鲁工业大学 A kind of C doping flowered-spherical titanium dioxide/molybdenum disulfide composite materials formed by nanometer sheet and preparation method thereof

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110180560A (en) * 2019-05-28 2019-08-30 广州大学 A kind of nano bar-shape bismuth doping molybdenum sulfide sphere multiphase Fenton catalyst and its preparation method and application
CN110180560B (en) * 2019-05-28 2022-02-15 广州大学 Nano-rod bismuth-doped molybdenum sulfide sphere multiphase Fenton catalyst and preparation method and application thereof
CN110289416A (en) * 2019-06-26 2019-09-27 中南大学 A kind of preparation method of anode material of lithium-ion battery bismuth molybdenum bimetallic sulfide
CN110289416B (en) * 2019-06-26 2022-02-01 中南大学 Preparation method of bismuth-molybdenum bimetallic sulfide as negative electrode material of sodium-ion battery
CN110380042A (en) * 2019-08-08 2019-10-25 山东大学 Aluminum secondary battery positive electrode, battery and preparation method
CN110380042B (en) * 2019-08-08 2021-01-15 山东大学 Anode material of aluminum secondary battery, battery and preparation method
CN113735181A (en) * 2021-09-06 2021-12-03 安徽工业大学 Antimony-cobalt sulfide-carbon composite nanorod and preparation method and application thereof
CN113735168A (en) * 2021-09-06 2021-12-03 安徽工业大学 Antimony-molybdenum sulfide-carbon composite material and preparation method and application thereof
CN114094078A (en) * 2021-11-16 2022-02-25 中国科学院深圳先进技术研究院 Nitrogen-doped carbon-coated metal sulfide heterojunction material, preparation method and battery application
WO2023087148A1 (en) * 2021-11-16 2023-05-25 中国科学院深圳先进技术研究院 Sulfide composite material for metal-ion battery, preparation method therefor, and application thereof
CN114094078B (en) * 2021-11-16 2024-01-26 中国科学院深圳先进技术研究院 Nitrogen-doped carbon-coated metal sulfide heterojunction material, preparation method and battery application

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