CN110228821A - A kind of preparation method that carbon dots doping induces 1T phase molybdenum disulfide and the application in energy storage material - Google Patents
A kind of preparation method that carbon dots doping induces 1T phase molybdenum disulfide and the application in energy storage material Download PDFInfo
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 82
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000004146 energy storage Methods 0.000 title claims abstract description 12
- 239000011232 storage material Substances 0.000 title claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 20
- 239000011733 molybdenum Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000005864 Sulphur Substances 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- 230000006698 induction Effects 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- LTUDISCZKZHRMJ-UHFFFAOYSA-N potassium;hydrate Chemical group O.[K] LTUDISCZKZHRMJ-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical group NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- 239000007772 electrode material Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 150000004685 tetrahydrates Chemical class 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 20
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 239000012071 phase Substances 0.000 description 33
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 21
- 102100030310 5,6-dihydroxyindole-2-carboxylic acid oxidase Human genes 0.000 description 19
- 101000773083 Homo sapiens 5,6-dihydroxyindole-2-carboxylic acid oxidase Proteins 0.000 description 19
- 101000761220 Streptomyces clavuligerus Clavaminate synthase 2 Proteins 0.000 description 19
- 238000000034 method Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 8
- 239000013078 crystal Substances 0.000 description 6
- 238000001069 Raman spectroscopy Methods 0.000 description 5
- 101000898746 Streptomyces clavuligerus Clavaminate synthase 1 Proteins 0.000 description 5
- 241000446313 Lamella Species 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002372 labelling Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000000502 dialysis Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000012456 homogeneous solution Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002077 nanosphere Substances 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 description 1
- 241001138444 Globularia alypum Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000001453 impedance spectrum Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
-
- 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
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- 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
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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
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Abstract
The preparation method for adulterating induction 1T phase molybdenum disulfide the invention discloses a kind of carbon dots and the application in energy storage material are that the molybdenum source of certain mol proportion, sulphur source, carbon source and water are sufficiently mixed to stirring to uniform solution, obtain precursor solution；Gained precursor solution is transferred in autoclave, high-temperature high-voltage reaction, after reaction by reaction solution filtration washing, the 1T molybdenum disulfide powder of carbon dots doping is obtained after dry.1T phase molybdenum disulfide hybrid material obtained by the present invention shows good chemical property and catalysis absorbing property, the potentiality with wide industrial applications.
Description
Technical field
The present invention relates to the preparation of energy storage material and applications, and in particular to a kind of carbon dots doping induction 1T phase curing
The preparation method of molybdenum and the application in energy storage material.
Background technique
Molybdenum disulfide (MoS2) belong to a kind of cheap transition metal, the special property with semiconductor material.Curing
There are three types of the crystal structures of form, respectively the 2H phase of triangular prism-shaped, the 1T phase of octahedral figure and rhombohedron knot for molybdenum tool
The 3R phase of structure.Industrially extracts and obtain usually from molybdenite concentrate, and it is the molybdenum disulfide of 2H phase that prepared by general industry method, by
In the tightly packed of molybdenum disulfide lamellar structure, the active site exposed is less, and electrochemical properties are poor, seriously limits two sulphur
Change the application of molybdenum.And the molybdenum disulfide of 1T metal phase, lamella pile up pine, interlamellar spacing is big, have good electro-chemical activity and compared with
High electric conductivity significantly improves the electrochemical properties of molybdenum disulfide, to widen it in energy storage field and catalysis
Inhale the application in wave field.Supercapacitor is a kind of energy storage devices of novel and high-efficiency, it is between traditional capacitor and electric power storage
Between pond, but possess bigger energy density and higher power density than traditional capacitor, this makes it in terms of energy reserve
Possess unique advantage, to play big advantage in fields such as communication, national defence, traffic, instrument and meter and electronic devices.
Existing patent report come out be mostly 2H phase molybdenum disulfide, and 1T phase molybdenum disulfide report it is less.It is known that
The 1T phase molybdenum disulfide of metalline has stronger electric conductivity than the 2H phase molybdenum disulfide of semiconductor property, and it is in energy
The fields such as storage, catalytic degradation and microwave absorption have potential application prospect.1T phase molybdenum disulfide preparation difficulty is big at present, system
Standby technique lacks.Such as patent of invention 201810354978.6 is prepared for 1T phase molybdenum disulfide as substrate by carbon fiber, uses
In electrode material for super capacitor, 1000 charge-discharge tests are carried out under the low current density of 2A/g, capacitor retains 79%, property
Can be unsatisfactory, while lacking the share that the tests such as Raman, XPS prove and detect 1T crystal form and its occupy.Patent of invention
201811581233.X being substrate using Nano tube array of titanium dioxide, by molybdenum disulfide nano sheet hydrothermal growth in nanotube
On, and the catalytic degradation for being applied to pollutant is studied, but the proof foundation as 1T phase molybdenum disulfide is only tested using XRD, and
Without convincingness.For another example conducting polymer and molybdenum disulfide are combined together by patent 201610417561.0, and purpose is to obtain
The mixing material of high capacitance is obtained, however specific capacitance only reaches 307F/g under the current density of 1A/g.1T gold prepared by the present invention
Symbolic animal of the birth year molybdenum disulfide method is simple and easy, and material structure is clear, after carbon dots doping introduces, than electricity under the current density of 0.5A/g
Appearance has reached 513F/g, has been higher by much than above-mentioned two end number mixing material specific capacitance.Therefore the preparation method is simple, at low cost
Honest and clean, data characterization is complete, is real 1T phase molybdenum disulfide.
Summary of the invention
The present invention provides a kind of preparation side of carbon dots induction 1T phase molybdenum disulfide for the problems of prior art
Method and the application in energy storage material, main purpose be solve the problems, such as carbon dots doping removing 1T molybdenum disulfide, thus
It is widened in the application in the fields such as energy storage and catalytic degradation.
The present invention solves 1T metal phase molybdenum disulfide and synthesizes difficult, low output, and at high cost and chemical property difference etc. is difficult
Topic, and then it is applied to the electrode material of supercapacitor, increase substantially the chemical property of molybdenum disulfide.
The preparation method of carbon dots doping induction 1T phase molybdenum disulfide of the present invention, is by the molybdenum source, sulphur source, carbon of certain mol proportion
Source and water, which are sufficiently mixed, is stirred until homogeneous solution, obtains precursor solution；Gained precursor solution is transferred to autoclave
In, high-temperature high-voltage reaction obtains carbon dots doping 1T molybdenum disulfide powder after reaction by reaction solution filtration washing after dry.
Specifically comprise the following steps:
Step 1: the preparation of presoma
Molybdenum source, sulphur source, carbon source and deionized water are sufficiently mixed the uniform precursor solution of stirring to obtain；
In step 1, the molybdenum source be seven Ammonium paramolybdate tetrahydrates, the sulphur source be thiocarbamide, the molar ratio 2:1 of sulphur source and molybdenum source,
Quality is respectively 2.28 and 1.24g；The carbon source is monohydrate potassium, and the additive amount of quality 2.48g, deionized water are
50mL。
The preparation of step 2:1T molybdenum disulfide
Precursor solution is transferred in autoclave, and reaction kettle is moved in baking oven, in 220 DEG C of high temperature and pressure
Lower reaction 10h；It is using ethyl alcohol and deionized water that the black liquor filtration washing of reaction kettle is multiple to after reaction, finally
40 DEG C are dried to obtain carbon dots doping 1T molybdenum disulfide powder.
The application of carbon dots doping induction 1T phase molybdenum disulfide prepared by the present invention, is to be applied to energy storage material
In.
Further, the application of carbon dots doping induction 1T phase molybdenum disulfide prepared by the present invention, is as supercapacitor
Electrode material use, with excellent chemical property and catalysis absorbing property.
In the present invention, hydro-thermal method is prepared for the 1T molybdenum disulfide CDs@1T-MoS that carbon dots are adulterated first2, wherein sample
CAS2 after 2000 charge-discharge tests, still maintains initial capacitance value (513F/g) under 5A/g current density
85%, show outstanding chemical property and stable recycling performance.
The beneficial effects of the present invention are embodied in:
The present invention is prepared for the 1T phase molybdenum disulfide of carbon dots doping induction, experiment using a kind of simple and easy hydro-thermal method
Mild condition, controllability are preferable.Raman test confirms the acquisition of carbon dots doping induction 1T metal phase molybdenum disulfide, wherein 1T phase
Account for 78%.
Compared with the methods of Traditional liquid phase removing, ultrasound removing, mechanical stripping molybdenum disulfide stratiform, the carbon of this method preparation
Point doping 1T phase molybdenum disulfide prevents lamella from growing aggregation, and peeling effect is good, and maximum lamella distance reaches 0.84nm, XRD test
In (002) crystal face it is obviously mobile to low-angle, interplanar distance increases.This method yield is high, and method is simple, low in cost, and electricity
Chemical property is excellent.
Present invention carbon dots obtained adulterate 1T phase molybdenum disulfide, morphology controllable, compound with regular structure, the life of carbon dots induction 1T phase
At, and successfully removed 1T phase molybdenum disulfide lamella and piled up, interlamellar spacing is wider, to expose more active sites, is conducive to
The transmitting of electronics, to show high specific capacitance, good cyclical stability can be used as good electrode material in energy storage material
Material.
Carbon dots doping 1T molybdenum disulfide material prepared by the present invention has inhales wave and catalytic degradation performance well.
Detailed description of the invention
Fig. 1 is the Raman figure of molybdenum disulfide and carbon dots doping 1T molybdenum disulfide hybrid material.
Fig. 2 is the scanning electron microscope of (a) molybdenum disulfide and (b) carbon dots doping 1T molybdenum disulfide hybrid material CAS2
Figure.
Fig. 3 is the X diffraction pattern of molybdenum disulfide and carbon dots doping 1T molybdenum disulfide hybrid material CAS2.
Fig. 4 is the transmission electron microscopy of molybdenum disulfide (a, b) and carbon dots doping 1T molybdenum disulfide hybrid material CAS2 (c, d)
Mirror figure.
Fig. 5 is the X-ray electronic chart of molybdenum disulfide and carbon dots doping 1T molybdenum disulfide hybrid material CAS2.Wherein a figure is
Total spectrogram of CAS1 and CAS2, b are the sulphur spectrogram of CAS2, and c is the molybdenum spectrogram of CAS2.
Fig. 6 is the electrochemical property test figure of molybdenum disulfide and carbon dots doping 1T molybdenum disulfide hybrid material CAS2.Wherein a
For the charge and discharge electrograph of CAS2, b is the cyclic voltammogram of CAS2, and c is impedance spectra, and d is 2000 charge and discharge cycles figures.
Specific embodiment
Elaborate below to the embodiment of the present invention, following embodiments under the premise of the technical scheme of the present invention into
Row is implemented, and the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following realities
Apply example.
Embodiment 1:
Molybdenum source in the present embodiment, sulphur source are not added, and carbon source monohydrate potassium content is 2.48g, product labelling obtained
For CAS0.It takes monohydrate potassium 2.48g to be dissolved in being sufficiently mixed in 50mL deionized water and be stirred until homogeneous solution, obtains presoma
Solution；Precursor solution is poured into polytetrafluoroethylene (PTFE) autoclave, and reaction kettle is moved in baking oven, it is anti-at 220 DEG C
Answer 10h；After reaction, reaction kettle is removed from baking oven, by the filter 23 at reduced pressure conditions of the brown color liquid in reaction kettle
Aqueous filter membrane that is secondary, the use of aperture being 0.22 μm.The bag filter for the use of molecular cut off being 500 is average to filtrate dialysis treatment
Every 10h changes a water, and dialysis procedure continues 72h.By the liquid removal in bag filter, extra water is removed using Rotary Evaporators
Point, the concentrate of yellow is obtained, is put into -10 DEG C of refrigerator-freezer and freezes into ice cube；Ice cube after above-mentioned frost is put into freeze dryer
Middle removing moisture, obtains yellowish-brown carbon quantum dot powder, and sample is labeled as CAS0.
Embodiment 2:
The present embodiment prepares carbon dots doping 1T molybdenum disulfide as follows:
1, the preparation of presoma
By the molybdenum source of certain mol proportion, sulphur source, the carbon source and water of certain mass are sufficiently mixed stirring to uniform solution, obtain
Presoma.Wherein, molybdenum source uses seven Ammonium paramolybdate tetrahydrates, and sulphur source uses thiocarbamide, the molar ratio 2:1 of sulphur source and molybdenum source, quality difference
For 2.28 and 1.24g；Carbon source uses monohydrate potassium, and the quality of monohydrate potassium is 0g, and water uses deionized water 50mL.
2, the preparation of carbon dots doping 1T molybdenum disulfide
Presoma is poured into autoclave, 220 DEG C of reaction 10h, to after reaction, use ethyl alcohol and deionized water
The adopting dark liquid filtration washing of reaction kettle is multiple, and last 40 DEG C are dried to obtain carbon dots doping 1T molybdenum disulfide powder, are obtained
Product labelling be CAS1.
Embodiment 3:
The molar ratio 2:1 of the present embodiment sulphur source and molybdenum source, quality are respectively 2.28 and 1.24g, carbon source monohydrate potassium
2.48g, other are same as Example 2, and product labelling obtained is CAS2.
Specific preparation parameter in embodiment 1-3 is as follows:
Fig. 1 is that molybdenum disulfide and carbon dots adulterate 1T molybdenum disulfide hybrid material Raman figure, and sample CAS2 is in 147 (J1),
196,219(J2),280(E1g) and 327 (J3)cm-1The Raman peaks for showing apparent 1T crystal form are only shown different from CAS1
E1 2gAnd A1gThe two typical Raman peaks, this is typical 2H molybdenum disulfide.This shows the carbon dots of citric acid generation induction of two
The generation of molybdenum sulfide 1T phase crystal structure.This is because citric acid enters among the lamellar structure of molybdenum disulfide, two sulphur are expanded
Change molybdenum layer spacing, while the carbon quantum dot that citric acid is formed effectively prevents the accumulation of molybdenum disulfide lamellar structure, to generate
The molybdenum disulfide of 1T metal phase.
Fig. 2 is the scanning electron microscope diagram that molybdenum disulfide CAS1 and carbon dots adulterate 1T molybdenum disulfide hybrid material CAS2,
It is clearly seen from figure, curing molybdenum sheet is easy to be piled into flower-like nanometer ball, and diameter is about 5 μm.The addition of citric acid, so that two
The diameter of molybdenum sulfide nanosphere is reduced rapidly.This is to be attributed to the fact that citric acid is formed after carbon quantum dot, and the doping of carbon quantum dot lures
Molybdenum disulfide nano sphere volume is led to lesser Long-term change trend.Sample CAS2 accumulation globe daisy is too small and very irregular, this be by
Caused by the effect of the limit removing of carbon dots.
Fig. 3 is that molybdenum disulfide and carbon dots are adulterated in the XRD of 1T molybdenum disulfide hybrid material, (002) peak point of sample CAS2
Two peaks are turned to, between this can prove the carbon dots perfection insertion molybdenum disulfide lamellar structure that citric acid generates, expand interlamellar spacing,
Induction of the generation of 1T phase molybdenum disulfide.
Fig. 4 is that molybdenum disulfide and carbon dots adulterate 1T molybdenum disulfide hybrid material TEM figure, with the promotion of citric acid content, two
Molybdenum sulfide lamellar structure is reduced, and sample CAS2 shows single layer structure, and there are spacings of lattice in its single layer structure is
The carbon quantum dot of 0.24nm, it was demonstrated that carbon quantum dot successfully introduces.Meanwhile (100) and (110) crystal face of 1T molybdenum disulfide is also in
Reveal and.
Fig. 5 is the XPS figure that molybdenum disulfide and carbon dots adulterate 1T molybdenum disulfide hybrid material, and XPS discloses 1T phase curing
The element of molybdenum and 2H phase molybdenum disulfide, the peak intensity of C1s is significantly raised in CAS2, it is meant that citric acid water thermal cracking is for carbon amounts
Sub- point.
Fig. 6 is that molybdenum disulfide and carbon dots adulterate 1T molybdenum disulfide hybrid material electrochemical property test figure, sample CAS1 and
The CV curve of CAS2 demonstrates the storage mechanism of electric double layer, is existed by the molybdenum disulfide that charge and discharge result can calculate 1T phase
Specific capacitance has reached 513F/g under the current density of 0.5A/g.And pass through 2000 charge and discharge under the electric current current density of 5A/g
After test, 85% capacitance is still maintained, shows good chemical property.
Claims (5)
1. a kind of preparation method of carbon dots doping induction 1T phase molybdenum disulfide, it is characterised in that:
The molybdenum source of certain mol proportion, sulphur source, carbon source and water are sufficiently mixed stirring to uniform solution, obtain precursor solution；It will
Gained precursor solution is transferred in autoclave, high-temperature high-voltage reaction, dry after reaction by reaction solution filtration washing
After obtain carbon dots doping 1T molybdenum disulfide powder.
2. preparation method according to claim 1, it is characterised in that include the following steps:
Step 1: the preparation of presoma
Molybdenum source, sulphur source, carbon source and deionized water are sufficiently mixed the uniform precursor solution of stirring to obtain；
The preparation of step 2:1T molybdenum disulfide
Precursor solution is transferred in autoclave, and reaction kettle is moved in baking oven, it is anti-under 220 DEG C of high temperature and pressure
Answer 10h；It is using ethyl alcohol and deionized water that the black liquor filtration washing of reaction kettle is multiple to after reaction, last 40 DEG C
It is dried to obtain carbon dots doping 1T molybdenum disulfide powder.
3. preparation method according to claim 2, it is characterised in that:
In step 1, the molybdenum source is seven Ammonium paramolybdate tetrahydrates, and the sulphur source is thiocarbamide, the molar ratio 2:1 of sulphur source and molybdenum source, quality
Respectively 2.28 and 1.24g；The carbon source is monohydrate potassium, and the additive amount of quality 2.48g, deionized water are
50mL reacts 10h under 220 DEG C of high temperature and pressure.
4. a kind of application for the carbon dots doping 1T phase molybdenum disulfide that any preparation method is prepared in claim 1,2 or 3,
It is characterized by: being used as energy storage material.
5. application according to claim 4, it is characterised in that:
It is the electrode material use as supercapacitor, there is excellent chemical property performance.
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| CN111115686A (en) * | 2019-12-31 | 2020-05-08 | 吉林大学 | Metal phase molybdenum disulfide, electrode, preparation method, electrocatalyst and energy storage element |
| CN113461060A (en) * | 2021-05-07 | 2021-10-01 | 电子科技大学 | Preparation method and application of interlayer spacing expanded nano spherical 1T phase molybdenum disulfide |
| CN116443856A (en) * | 2023-03-28 | 2023-07-18 | 上海大学 | Carbon quantum dot/MoS 2 Nanosheet composite material and preparation method thereof |
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