CN106824230A - The method that quantum dot aids in synthesis of carbon/molybdenum disulfide - Google Patents
The method that quantum dot aids in synthesis of carbon/molybdenum disulfide Download PDFInfo
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- CN106824230A CN106824230A CN201710140933.4A CN201710140933A CN106824230A CN 106824230 A CN106824230 A CN 106824230A CN 201710140933 A CN201710140933 A CN 201710140933A CN 106824230 A CN106824230 A CN 106824230A
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 42
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 24
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 19
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 19
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 26
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011733 molybdenum Substances 0.000 claims abstract description 25
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 24
- 239000010703 silicon Substances 0.000 claims abstract description 24
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- 230000008859 change Effects 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 239000003643 water by type Substances 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- 235000010378 sodium ascorbate Nutrition 0.000 claims description 6
- 229960005055 sodium ascorbate Drugs 0.000 claims description 6
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims description 6
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 claims description 6
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims description 4
- 239000011609 ammonium molybdate Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 230000015556 catabolic process Effects 0.000 abstract description 8
- 238000006731 degradation reaction Methods 0.000 abstract description 8
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 abstract description 7
- 229940012189 methyl orange Drugs 0.000 abstract description 7
- 230000006378 damage Effects 0.000 abstract description 5
- 230000036541 health Effects 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 4
- 239000000975 dye Substances 0.000 abstract description 4
- 238000001228 spectrum Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- 230000003595 spectral effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 14
- 150000004770 chalcogenides Chemical class 0.000 description 7
- 239000010410 layer Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 229910052723 transition metal Inorganic materials 0.000 description 6
- 150000003624 transition metals Chemical class 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- 239000012855 volatile organic compound Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 241000446313 Lamella Species 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 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
- 229910016001 MoSe Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003124 biologic agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001048 orange dye Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000003348 petrochemical agent Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- -1 sensor Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Water Supply & Treatment (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Toxicology (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The method that quantum dot aids in synthesis of carbon/molybdenum disulfide, it is related to a kind of preparation method of photochemical catalyst.Serious destruction is not only caused to environment the present invention is to solve VOC (VOC), and the health of the mankind oneself or even life is subject to the technical problem of serious threat.This method is as follows:First, Hydrothermal Synthesiss silicon quantum dot;2nd, silicon quantum dot auxiliary synthesis of carbon/molybdenum disulfide.Silicon quantum dot of the present invention and molybdenum bisuphide construct a kind of new mixed structure, and its spectral absorption characteristics there has also been greatly change.The absorption of full spectrum has reached 95%, can effectively absorb solar energy.Silicon quantum dot of the invention and molybdenum bisuphide mixed structure are greatly improved to the degradation rate of methyl orange organic dyestuff.Under visible light, compared to existing most fast degradation time 150min, the degradation time of silicon quantum dot of the present invention and molybdenum bisuphide structure is up to 90min.The invention belongs to the preparation field of photochemical catalyst.
Description
Technical field
The present invention relates to a kind of preparation method of photochemical catalyst.
Background technology
Van der Waals crystal is the material that a class has layer structure, including Graphene, metal oxide, chalcogenide and
Phosphate etc., their different chemical compositions and crystal structure result in different performances, such as wherein existing conductor has again
Insulator.Although each material has differences, these materials all present one it is common the characteristics of --- big Van der Waals layer
Spacing and weak interaction force.The interlamellar spacing of Van der Waals crystal is in several rans, there is provided certain reaction condition, can with gram
Take the weak interaction force of its interlayer it is reversible by some functional moleculars, ion and atom etc. insert its bedding void, formed class
It is similar to a layer column structure.Wherein Graphene has been widely used in pencil-lead, motor as Van der Waals material of greatest concern
The industry such as electrode and dry lubricant.Another very typical two dimension Van der Waals semiconductor --- the chalcogenide of transition metal two
(TMDs).Such compound molecule formula is generally MX2(wherein M=Mo, W, Nb, Ta, Ti;X=S, Se, Te).Transition metal two
Chalcogenide presence stable in the air, the block materials electronic structure with their own is entirely different.With MoSe2As a example by,
The MoSe of two dimension2Nanometer sheet has thickness, larger band gap width, carrier activity high and the abundant table of atomic level
The features such as face dangling bonds.Different from grapheme material natural zero band gap the characteristics of, the chalcogenide of transition metal two is naturally deposited
Enable that the material is widely used in semicon industry in band gap, be described as the another revolutionary electronic device after silicon materials
Material, can continue the Moore's Law of development of electronic devices.
The chalcogenide of nano level transition metal two (TMDs) is cashed compared with its block materials as electronic structure is different,
Including:(1) density of states (2) for increasing covalent bond shortens the diffusion length in light induced electron-hole pair.And, performance also has very big
Change, including (1) with good photocatalysis performance (2) with effective redox reaction catalytic performance.In addition, may be used also
Some properties are obtained with by adjusting chemical composition or structure, with multi-field application prospect.Molybdenum bisuphide (MoS2)
It is a kind of very typical chalcogenide of transition metal two, but block molybdenum bisuphide is due to its poorly conductive, energy gap
The defect such as big.Limit its extensive use.
In order to improve the electric conductivity of molybdenum bisuphide, shorten energy gap, except towards the ultra-thin molybdenum bisuphide of synthesis individual layer
The direction of nanometer sheet can also be carried out outside making great efforts by changing the methods such as phase transformation.Ultra-thin two-dimension sheet layer material is special due to its
Structure, possesses unprecedented physics, and chemistry, electrical and optical performance has potential application value, example in numerous areas
Such as electrode material, photoelectric material, sensor, catalyst, material for water treatment and biological agent.This also imply that molybdenum bisuphide
Have a extensive future.
Molybdenum bisuphide is used as a kind of chalcogenide of transition metal two the most typical, lamellar structure and energy with uniqueness
Band structure, scene effect semiconductor, photo luminescent devices, DSSC, ultracapacitor, lithium ion battery,
The numerous areas such as electrocatalytic decomposition hydrogen manufacturing have potential application prospect.For the intrinsic poorly conductive of molybdenum bisuphide, band gap knot
The problems such as structure is wide, lamella is easily piled up, common method is that the material good with electric conductivity is combined, and synthesizes individual layer or several layers of
Ultrathin nanometer lamella and the method such as different atom of insertion in lamella.
In the society of 21 century, energy and environment problem has become the theme of World Focusing, how to reduce pollution, protection
The ecological balance, solves environmental issue, has caused the great attention of each government decision department and academic research department.When current
In generation, we are greatly developing social productive forces, while advancing in living standard, serious destruction are also result in environment, seriously
Threaten our existence.Nowadays, water and air has been increasingly subject to pay attention to as the most valuable resource of the mankind.In particular with
The quickening of industrial process, has been discharged substantial amounts of waste water, waste gas in water and air, wherein containing substantial amounts of toxic organicses
Can be enriched with human body, the health care belt to the mankind carrys out huge threat.And in these compounds, there is part of compounds to use flat
Normal processing method is difficult to be degraded.Chinese scholar Jin Qi front yards et al. are found by studying observation:Many organic compounds
Anaerobe can be made to produce obvious toxic action.By experimental result as can be seen that these organic compounds must be by one
A little other abiotic degradation techniques are removed.In our daily life, there is substantial amounts of VOC
(volatile organic compound, VOC) is discharged into the environment of our lives, and not only environment is caused seriously
Destruction, and make the mankind oneself health so that life be subject to it is serious threaten, for example, various petrochemicals
And interior/exterior decoration product, the daily living article of toxic gas, the construction material that particularly interior decoration is commonly used can be produced
As paint, coating etc., these compounds cause serious pollution to environment, and the health to the mankind causes serious prestige to do harm to.Therefore,
Develop a kind of simple and effective method to come pollution control of water and atmosphere pollution is one urgent problem of human society.Though
So there are many governing measures at present, but the technology of photocatalysis treatment organic pollution is inexpensive due to its, nontoxic, energy-conservation,
Efficient advantage is increasingly becoming the emphasis of people from all walks of life's research, and light-catalysed research and development also suddenly become current world popular research neck
One of domain.
Methyl orange dye is that one kind common are organic pollutants, non-volatility, and is decomposed with a relatively high anti-direct light
With the ability of oxidation;Its concentration can use spectrophotometry, and method is easy, is often used as the model reaction of light-catalyzed reaction
Thing.It belongs to azo dyes, this kind of dyestuff be dyestuff it is all kinds of in most one kind, account for 50% or so of whole dyestuffs.According to
Existing experimental analysis, methyl orange is the organic matter compared with difficult degradation, thus representative as research object using it.
The content of the invention
Serious destruction is not only caused to environment the present invention is to solve VOC (VOC), and is made
The health or even life of the mankind oneself are subject to the technical problem of serious threat, there is provided a kind of quantum dot auxiliary synthesis curing
The method of molybdenum.
The method of quantum dot auxiliary synthesis of carbon/molybdenum disulfide is followed the steps below:
First, Hydrothermal Synthesiss silicon quantum dot:
The sodium ascorbate of 0.040g-0.060g is dissolved in the deionized water of 10ml and places 20min, obtain mixed liquor,
The mixed liquor of 1.25ml is dissolved in 1ml trimethyoxysilanes, adds deionized water to be made into the solution that concentration is 20g/l, and
Solution is poured into hydrothermal reaction kettle and is heated to 200 DEG C of reaction 24h, obtain silicon quantum dot;
2nd, silicon quantum dot auxiliary synthesis of carbon/molybdenum disulfide:
5mmol-7mmol ammonium molybdates and 17mmol-19mmol thiocarbamides are dissolved in 20ml deionized waters, are added
The silicon quantum dot of 0.025mmol purifying, then pours into hydrothermal reaction kettle mixed mixture, under conditions of 150 DEG C
Reaction 12h, natural cooling collects black deposit, is washed with ethanol and deionized water, then is dried in 60 DEG C of baking oven, obtains
To molybdenum bisuphide.
Silicon quantum dot of the present invention and molybdenum bisuphide construct a kind of new mixed structure, because quantum dot belongs to semiconductor
Material, and the recombination energy of molybdenum bisuphide plays synergy, improves the level structure of molybdenum bisuphide, its spectral absorption characteristics
There is great change.The absorption of full spectrum has reached 95%, can effectively absorb solar energy.Silicon quantum dot of the invention and curing
Molybdenum mixed structure is greatly improved to the degradation rate of methyl orange organic dyestuff.Under visible light, compared to existing most fast degraded
The degradation time of time 150min, silicon quantum dot of the present invention and molybdenum bisuphide structure is up to 90min.
Brief description of the drawings
Fig. 1 is the structural representation for testing the molybdenum bisuphide of quantum dot auxiliary synthesis in one;
Fig. 2 is the electromicroscopic photograph for testing the molybdenum bisuphide of quantum dot auxiliary synthesis in one.
Specific embodiment
Technical solution of the present invention is not limited to act specific embodiment set forth below, also including between each specific embodiment
Any combination.
Specific embodiment one:The method of present embodiment quantum dot auxiliary synthesis of carbon/molybdenum disulfide is entered according to following steps
OK:
First, Hydrothermal Synthesiss silicon quantum dot:
The sodium ascorbate of 0.040g-0.060g is dissolved in the deionized water of 10ml and places 20min, obtain mixed liquor,
The mixed liquor of 1.25ml is dissolved in 1ml trimethyoxysilanes, adds deionized water to be made into the solution that concentration is 20g/l, and
Solution is poured into hydrothermal reaction kettle and is heated to 200 DEG C of reaction 24h, obtain silicon quantum dot;
2nd, silicon quantum dot auxiliary synthesis of carbon/molybdenum disulfide:
5mmol-7mmol ammonium molybdates and 17mmol-19mmol thiocarbamides are dissolved in 20ml deionized waters, are added
The silicon quantum dot of 0.025mmol purifying, then pours into hydrothermal reaction kettle mixed mixture, under conditions of 150 DEG C
Reaction 12h, natural cooling collects black deposit, is washed with ethanol and deionized water, then is dried in 60 DEG C of baking oven, obtains
To molybdenum bisuphide.
Specific embodiment two:Present embodiment from step one unlike specific embodiment one by 0.0594g's
Sodium ascorbate places 20min in being dissolved in the deionized water of 10ml.Other are identical with specific embodiment one.
Specific embodiment three:Present embodiment from step 2 unlike specific embodiment one or two by 5mmol
Ammonium molybdate and 17mmol thiocarbamides are dissolved in 20ml deionized waters.Other are identical with specific embodiment one or two.
Specific embodiment four:Will in step 2 unlike one of present embodiment and specific embodiment one to three
5.5mmol ammonium molybdates and 17.5mmol thiocarbamides are dissolved in 20ml deionized waters.Other phases one of with specific embodiment one to three
Together.
Specific embodiment five:Will in step 2 unlike one of present embodiment and specific embodiment one to four
6mmol ammonium molybdates and 18mmol thiocarbamides are dissolved in 20ml deionized waters.Other are identical with one of specific embodiment one to four.
Specific embodiment six:Specific embodiment four:One of present embodiment and specific embodiment one to five difference
Be 6.5mmol ammonium molybdates and 18.5mmol thiocarbamides to be dissolved in 20ml deionized waters in step 2.Other and specific embodiment party
One of formula one to five is identical.
Specific embodiment seven:Specific embodiment four:One of present embodiment and specific embodiment one to six difference
Be 7mmol ammonium molybdates and 19mmol thiocarbamides to be dissolved in 20ml deionized waters in step 2.Other and specific embodiment one
It is identical to one of six.
Using following experimental verifications effect of the present invention:
Experiment one:
The method of quantum dot auxiliary synthesis of carbon/molybdenum disulfide is followed the steps below:
First, Hydrothermal Synthesiss silicon quantum dot:
The sodium ascorbate of 0.0594g is dissolved in the deionized water of 10ml and places 20min, obtain mixed liquor, will
The mixed liquor of 1.25ml is dissolved in 1ml trimethyoxysilanes, adds deionized water to be made into the solution that concentration is 20g/l, and will
Solution pours into hydrothermal reaction kettle how long be heated to 200 DEG C of reactions, obtain silicon quantum dot;
2nd, silicon quantum dot auxiliary synthesis of carbon/molybdenum disulfide:
6mmol ammonium molybdates and 18mmol thiocarbamides are dissolved in 20ml deionized waters, the silicon quantum of 0.025mmol purifying is added
Point, then pours into hydrothermal reaction kettle mixed mixture, and 12h is reacted under conditions of 150 DEG C, and natural cooling is collected
Black deposit, is washed with ethanol and deionized water, then is dried in 60 DEG C of baking oven, obtains molybdenum bisuphide.
Photo-catalytic degradation of methyl-orange is tested:
The methyl orange solution of 10mg/l is prepared, the molybdenum bisuphide for weighing 0.025g is poured into methyl orange mixed solution.First
Adsorption desorption balance 5min is set up in the dark, then converts xenon source (250-2500nm) catalytic reaction of different wave length, respectively
The catalytic degradation methyl orange under visible ray (400-760nm) and ultraviolet light (250-400nm) and full spectrum.
(1) under ultraviolet light, above-mentioned catalytic reaction is carried out, 40min is degradable into colourless inorganic matter.
(2) under visible light, above-mentioned catalytic reaction is carried out, 90min is degradable into colourless inorganic matter.
(3) under full spectrum, above-mentioned catalytic reaction is carried out, 30min is degradable into colourless inorganic matter.
It can be seen that determining existing two sulphur of molybdenum bisuphide of synthesis according to the spacing between lattice from the electromicroscopic photograph of Fig. 2
Change molybdenum (0.942nm) and also contain Si quantum dots (0.30nm).
Claims (7)
1. quantum dot aid in synthesis of carbon/molybdenum disulfide method, it is characterised in that quantum dot auxiliary synthesis of carbon/molybdenum disulfide method according to
Following steps are carried out:
First, Hydrothermal Synthesiss silicon quantum dot:
The sodium ascorbate of 0.040g-0.060g is dissolved in the deionized water of 10ml and places 20min, obtain mixed liquor, will
The mixed liquor of 1.25ml is dissolved in 1ml trimethyoxysilanes, adds deionized water to be made into the solution that concentration is 20g/l, and will
Solution is poured into hydrothermal reaction kettle and is heated to 200 DEG C of reaction 24h, obtains silicon quantum dot;
2nd, silicon quantum dot auxiliary synthesis of carbon/molybdenum disulfide:
5mmol-7mmol ammonium molybdates and 17mmol-19mmol thiocarbamides are dissolved in 20ml deionized waters, add 0.025mmol pure
The silicon quantum dot of change, then pours into hydrothermal reaction kettle mixed mixture, and 12h is reacted under conditions of 150 DEG C, natural
Cooling, collects black deposit, is washed with ethanol and deionized water, then is dried in 60 DEG C of baking oven, obtains molybdenum bisuphide.
2. the method that quantum dot aids in synthesis of carbon/molybdenum disulfide according to claim 1, it is characterised in that will in step one
The sodium ascorbate of 0.0594g places 20min in being dissolved in the deionized water of 10ml.
3. the method that quantum dot aids in synthesis of carbon/molybdenum disulfide according to claim 1, it is characterised in that by 5mmol in step 2
Ammonium molybdate and 17mmol thiocarbamides are dissolved in 20ml deionized waters.
4. the method that quantum dot aids in synthesis of carbon/molybdenum disulfide according to claim 1, it is characterised in that will in step 2
5.5mmol ammonium molybdates and 17.5mmol thiocarbamides are dissolved in 20ml deionized waters.
5. the method that quantum dot aids in synthesis of carbon/molybdenum disulfide according to claim 1, it is characterised in that by 6mmol in step 2
Ammonium molybdate and 18mmol thiocarbamides are dissolved in 20ml deionized waters.
6. the method that quantum dot aids in synthesis of carbon/molybdenum disulfide according to claim 1, it is characterised in that will in step 2
6.5mmol ammonium molybdates and 18.5mmol thiocarbamides are dissolved in 20ml deionized waters.
7. the method that quantum dot aids in synthesis of carbon/molybdenum disulfide according to claim 1, it is characterised in that by 7mmol in step 2
Ammonium molybdate and 19mmol thiocarbamides are dissolved in 20ml deionized waters.
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CN113479901A (en) * | 2021-07-06 | 2021-10-08 | 哈尔滨工业大学 | Preparation method for synthesizing special-morphology 13X molecular sieve by assistance of silicon quantum dots |
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CN108520832A (en) * | 2018-04-02 | 2018-09-11 | 哈尔滨工业大学 | SiQDs-MoS2/ rGO composite material and preparation methods and application |
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CN110875150A (en) * | 2019-11-27 | 2020-03-10 | 长安大学 | Si/MoS2Preparation method of electrode material |
CN113479901A (en) * | 2021-07-06 | 2021-10-08 | 哈尔滨工业大学 | Preparation method for synthesizing special-morphology 13X molecular sieve by assistance of silicon quantum dots |
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