CN108511201A - A kind of ultra-thin MoS2Nanometer sheet/CNT composite material and preparation methods - Google Patents
A kind of ultra-thin MoS2Nanometer sheet/CNT composite material and preparation methods Download PDFInfo
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- CN108511201A CN108511201A CN201711489880.3A CN201711489880A CN108511201A CN 108511201 A CN108511201 A CN 108511201A CN 201711489880 A CN201711489880 A CN 201711489880A CN 108511201 A CN108511201 A CN 108511201A
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- 239000002131 composite material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 18
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 6
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 5
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 229910015667 MoO4 Inorganic materials 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 239000003643 water by type Substances 0.000 claims description 3
- 229910004619 Na2MoO4 Inorganic materials 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 2
- 239000011684 sodium molybdate Substances 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- 238000007792 addition Methods 0.000 claims 1
- 238000005253 cladding Methods 0.000 claims 1
- 239000004570 mortar (masonry) Substances 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 230000005540 biological transmission Effects 0.000 abstract description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract 2
- 239000005864 Sulphur Substances 0.000 abstract 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 abstract 1
- 239000003792 electrolyte Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 abstract 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 abstract 1
- 230000009257 reactivity Effects 0.000 abstract 1
- 239000007772 electrode material Substances 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for 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
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Nanotechnology (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of ultra-thin MoS2Nanometer sheet/carbon nanotube（CNT）Composite material and preparation method.The present invention is prepared using hydro-thermal method, this method has many advantages, such as simple for process, flexible to operation, morphology controllable, which uses inorganic sulphur source, keeps the sulphur source utilization rate in the reaction larger, and environmentally harmful hydrogen sulfide gas is not will produce, it is a kind of environmentally friendly preparation method.The MoS of two-dimensional ultrathin structure2With larger specific surface area, the contact area with electrolyte can be increased, more surface-active sites are provided, the reactivity of material surface is improved.And the CNT of one-dimensional perforation keeps being used as MoS in the case of complete structure in the reaction2Growh framework；On the other hand, one-dimensional CNT pipelines can improve the power density of material as the quick transmission path of ion and electronics, make its cycle charge-discharge under high current density, can significantly improve the chemical property of material.
Description
Technical field
The present invention relates to a kind of MoS2The functional composite material and preparation method of/CNT.It is prepared by one step hydro thermal method
MoS2The functional composite material of/CNT.The material has good chemical property, and preparation process is environmentally protective, as accumulator
The electrode material of part, it will there is great application in electronic device fields such as ultracapacitor, lithium ion batteries.
Background technology
As the decaying of world's crude oil energy storage and Global Greenhouse Effect aggravate, people are to large power long time stable power-supplying
Energy storage device more stringent requirements are proposed.Therefore to the performance of ultracapacitor, higher requirements are also raised, super capacitor
Device has larger power density and good stable circulation performance as a kind of Utopian electrochemical energy storing device, makees
An important factor for influence performance of the supercapacitor, electrode material has been obtained for the extensive research of people.
MoS2As the two-dimensional layer material of a type graphene, there is the lattice symmetry structure and electricity similar with graphene
Energy subband structure, MoS2Unique texture with S-Mo-S " sandwich ", MoS2Pass through weaker Van der Waals force between atomic layer
It links together, is inserted into the methods of stripping by liquid phase stripping or ion, the 1T metal phase structures of single layer, the knot can be prepared
There is structure good electric conductivity, band gap can be reduced after stripping, and two-dimensional layered structure can promote the quick of electronics
Transfer and transmission, while it also has larger specific surface area, good flexibility and chemical stability, to make it in energy storage
The fields such as field, biologic medical, photocatalysis and water electrolysis hydrogen production have a wide range of applications.
Carbon material is used as a kind of electrode material for super capacitor the most widely used now, has larger specific surface
Product, the physical and chemical properties stablized and abundance are cheap, receive much attention.The carbon of one-dimensional perforation is received
Mitron, on the one hand can be as the Growh framework of material, in the continuous of electrode material as a kind of carbon material with good conductivity
In cyclic process, the stabilization of material can be kept, its broken and dusting is prevented, improves material structure stability；Another aspect CNT
As good conductive material, the electric conductivity of composite material can also be enhanced, improve the power density of material.
Invention content
The invention aims to provide a kind of compound patterns of the 1D/2D of stabilization, and MoS can be significantly improved2Monomer
The MoS of specific capacitance2/ CNT composite materials.The stable structure of products obtained therefrom, and the functionality with good chemical property is compound
Material.
MoS in the present invention2/ CNT have it is stable equal and compound pattern, MoS2It is one-dimensional with ultra-thin lamellar structure
The carbon nanotube of perforation is uniformly through MoS2Between nanometer sheet, as illustrated in fig. 1 and 2.
The MoS of the present invention2/ CNT composite materials have good chemical property, in MoS2The basis of monomer has certain
Raising.In test voltage range -0.8-0.2 V, sweep speed is in the CV loop tests of 10 to 50 mV/s, MoS2/CNT
Functional composite material shows outstanding chemical property.As shown in Figure 3.
Realize that the technical solution adopted in the present invention is：A kind of MoS2/ CNT functional composite materials, pass through one step hydro thermal method
From growing, have technique environmentally protective, the advantages of operation is simple and feasible, the carbon nanotube of gained is uniformly applied in two dimension
MoS2Nanometer sheet surface, and excellent chemical property is shown, preparation process is as follows：
（1）Utilize the HNO of debita spissitudo3Solution carries out moditied processing to carbon nano tube surface, weighs the CNT of 100 mg
A concentration of 60% HNO is added3In solution, under conditions of being heated to boiling, continuing magnetic force stirs 2 h, then 1 h of sonic oscillation,
To make CNT be uniformly dispersed.The mixed solution that will be prepared is transferred in 60 DEG C of vacuum drying chamber, is ground with agate after drying
Alms bowl grinds 30 min, and collection is used as carbon source；
（2）Weigh step（1）In 10 mg of surface treated CNT, be added in 100 ml deionized waters, further
2 h of sonic oscillation makes CNT full and uniform dispersions, and 0.241 g Na are added2MoO4·2H2In O to CNT solution, and stir at room temperature
1 h is mixed, 0.291 g KSCN are added, stirs 30 min.Acquired solution is transferred in the reaction kettle of 150 ml, at 180 DEG C
Under reaction temperature, 12 h are reacted, MoS is made2It is fully compound to be preferably grown in CNT.Room temperature is naturally cooled to after reaction, is used
Deionized water and absolute ethyl alcohol repeatedly wash centrifugation, and dry in vacuum drying chamber；
Step（1）In 60% HNO3Concentration refers to the volume ratio of concentrated nitric acid and deionized water；
Step（2）Middle Na2MoO4·2H2O:KSCN=1:3（Molar ratio）；
Step（3）Middle centrifuge washing process is first to be cleaned 2 times with deionized water, then with washes of absolute alcohol 2 times, centrifuge
Rotating speed be 5000rpm, time 5min.
Description of the drawings
Fig. 1 is MoS2The SEM of/CNT composite materials.
Fig. 2 is MoS2The TEM of/CNT composite materials.
Fig. 3 is MoS2The CV curve graph of/CNT composite materials under different surface sweeping rates.
Specific embodiment
（1）Utilize the HNO of debita spissitudo3Solution carries out moditied processing to carbon nano tube surface, weighs the CNT of 100 mg
A concentration of 60% HNO is added3In solution, under conditions of being heated to boiling, continuing magnetic force stirs 2 h, then 1 h of sonic oscillation,
To make CNT be uniformly dispersed.The mixed solution that will be prepared is transferred in 60 DEG C of vacuum drying chamber, is ground with agate after drying
Alms bowl grinds 30 min, and collection is used as carbon source.
（2）Weigh step（1）In 10 mg of surface treated CNT, be added in 100 ml deionized waters, further
2 h of sonic oscillation makes CNT full and uniform dispersions, and 0.241 g Na are added2MoO4·2H2In O to CNT solution, and stir at room temperature
1 h is mixed, 0.291 g KSCN are added, stirs 30 min.Acquired solution is transferred in the reaction kettle of 150 ml, at 180 DEG C
Under reaction temperature, 12 h are reacted, MoS is made2It is fully compound to be preferably grown in CNT.Room temperature is naturally cooled to after reaction, is used
Deionized water and absolute ethyl alcohol repeatedly wash centrifugation, and dry in vacuum drying chamber.
Claims (5)
1. a kind of ultra-thin MoS2Nanometer sheet/CNT composite materials, it is characterised in that：The composite material is by ultra-thin MoS2Nanometer sheet
It is formed with two kinds of Material claddings of CNT of one-dimensional perforation, there is two dimensional surface shape characteristic.
2. a kind of ultra-thin MoS2The preparation method of nanometer sheet/CNT composite materials, it is characterised in that including following preparation process：
（1）Utilize the HNO of debita spissitudo3Solution carries out moditied processing to carbon nano tube surface, and the CNT additions for weighing 100 mg are dense
The HNO that degree is 60%3In solution, under conditions of being heated to boiling, continuing magnetic force stirs 2h, then sonic oscillation 1h, to make
CNT is uniformly dispersed；The mixed solution that will be prepared is transferred in 60 DEG C of vacuum drying chamber, is ground with agate mortar after drying
30min, collection are used as carbon source；
（2）Weigh step（1）In surface treated CNT10mg, be added in 100ml deionized waters, further ultrasound is shaken
Swinging 2h makes CNT full and uniform dispersions, and 0.241 g Na are added2MoO4·2H2In O to CNT solution, and 1h is stirred at room temperature, then
0.291 g KSCN are added, stir 30min；Acquired solution is transferred in the reaction kettle of 150ml, under 180 DEG C of reaction temperature,
12h is reacted, MoS is made2It is fully compound to be preferably grown in CNT；
（3）Room temperature is naturally cooled to after reaction, repeatedly washs centrifugation with deionized water and absolute ethyl alcohol, and be dried in vacuo
It is dry in case.
3. a kind of ultra-thin MoS as described in claim 12The preparation method of nanometer sheet/CNT composite materials, it is characterised in that：Institute
State step step（1）In 60% HNO3Concentration refers to the volume ratio of concentrated nitric acid and deionized water.
4. a kind of ultra-thin MoS as described in claim 12The preparation method step of nanometer sheet/CNT composite materials（2）In
Na2MoO4·2H2O:KSCN=1:3（Molar ratio）.
5. a kind of ultra-thin MoS as described in claim 12The preparation method step of nanometer sheet/CNT composite materials（3）Middle centrifugation is washed
It is first clean 2 times with deionized water, then with washes of absolute alcohol 2 times, the rotating speed of centrifuge is 5000rpm to wash process, and the time is
5min。
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| CN201711489880.3A CN108511201A (en) | 2017-12-29 | 2017-12-29 | A kind of ultra-thin MoS2Nanometer sheet/CNT composite material and preparation methods |
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| CN201711489880.3A CN108511201A (en) | 2017-12-29 | 2017-12-29 | A kind of ultra-thin MoS2Nanometer sheet/CNT composite material and preparation methods |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110380028A (en) * | 2019-07-08 | 2019-10-25 | 武汉理工大学 | A kind of CNT/MoS2Lithium ion battery negative material and preparation method thereof |
| CN111223682A (en) * | 2020-03-19 | 2020-06-02 | 桂林理工大学 | Electrode composite material of flexible supercapacitor and preparation method thereof |
| CN112509818A (en) * | 2020-10-20 | 2021-03-16 | 厦门大学 | Mixed-phase molybdenum sulfide-multiwalled carbon nanotube composite material, preparation method and application |
| CN112992557A (en) * | 2021-02-05 | 2021-06-18 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | Molybdenum disulfide-carbon nanotube/graphene electrode material and preparation method and application thereof |
| CN113952964A (en) * | 2021-10-20 | 2022-01-21 | 北华大学 | Preparation method and application of molybdenum disulfide/indium oxide nanocomposite material with 2D/3D structure |
-
2017
- 2017-12-29 CN CN201711489880.3A patent/CN108511201A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110380028A (en) * | 2019-07-08 | 2019-10-25 | 武汉理工大学 | A kind of CNT/MoS2Lithium ion battery negative material and preparation method thereof |
| CN110380028B (en) * | 2019-07-08 | 2022-09-09 | 武汉理工大学 | CNT/MoS 2 Lithium ion battery cathode material and preparation method thereof |
| CN111223682A (en) * | 2020-03-19 | 2020-06-02 | 桂林理工大学 | Electrode composite material of flexible supercapacitor and preparation method thereof |
| CN111223682B (en) * | 2020-03-19 | 2021-07-16 | 桂林理工大学 | Electrode composite material of flexible supercapacitor and preparation method thereof |
| CN112509818A (en) * | 2020-10-20 | 2021-03-16 | 厦门大学 | Mixed-phase molybdenum sulfide-multiwalled carbon nanotube composite material, preparation method and application |
| CN112992557A (en) * | 2021-02-05 | 2021-06-18 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | Molybdenum disulfide-carbon nanotube/graphene electrode material and preparation method and application thereof |
| CN113952964A (en) * | 2021-10-20 | 2022-01-21 | 北华大学 | Preparation method and application of molybdenum disulfide/indium oxide nanocomposite material with 2D/3D structure |
| CN113952964B (en) * | 2021-10-20 | 2023-11-17 | 北华大学 | Preparation method and application of 2D/3D structured molybdenum disulfide/indium oxide nanocomposite |
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