CN105524617A - Preparation method of molybdenum selenide quantum dots - Google Patents
Preparation method of molybdenum selenide quantum dots Download PDFInfo
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- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
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- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/00—Particle morphology
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- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a preparation method of molybdenum selenide quantum dots; the selenium molybdenum quantum dots are synthesized by a two-step method, and the preparation method comprises the concrete implementation method: firstly, dispersing molybdenum oxide and a selenium powder in a hydrazine hydrate aqueous solution, carrying out hydrothermal ion exchange reaction to obtain molybdenum selenide crystals; and then, dispersing the molybdenum selenide crystals in a mixed solution of water and isopropanol, then transferring the obtained solution into a stirring barrel, dissociating molybdenum selenide by a liquid shearing force produced by high-speed rotation of blades, and thus obtaining a molybdenum selenide quantum dot dispersion liquid. The preparation method of the selenium molybdenum quantum dots has the advantages of low cost, large-scale preparation, high efficiency and short production cycle.
Description
Technical field
The present invention relates to a kind of preparation method of selenizing molybdenum quantum dot, the method Bound moisture thermal ion exchange and liquid phase shearing force dissociating method obtain selenizing molybdenum quantum dot dispersion liquid, belong to technical field prepared by nano material.
Background technology
Two-dimension nano materials, as Graphene, transient metal sulfide etc., shows outstanding application potential electronics, sensing and photoelectric device etc. are multi-field with the physics of its excellence and structural performance.Wherein, Graphene is widely studied as the representational two-dimensional material of most.It has the carrier mobility of superelevation, but shortage band gap seriously hinders Graphene at logic semiconductor devices as the application in field-effect transistor.And as the line-up of delegates of transient metal sulfide semi-conductor family, molybdenumdisulphide (MoS
2) there is obvious band gap, and in n-type transistor, show excellent on-off ratio characteristic (>10
8).But, MoS
2there is the reduction that may cause electronic mobility in middle textural defect, thus affects its electric property.Therefore many methods are used for introducing band gap in Graphene by trial, are such as cut into nano belt, introduce defect and prepare quantum dot.
In recent years, selenizing molybdenum, with its good electrical transport factor and higher electro catalytic activity, becomes the potential important two-dimensional semiconductor material being applicable to high-performance optical electron device and energy field of tool gradually.With graphite-like seemingly, be also mutually stacking by faint interlaminar action power between the atomic shell of selenizing molybdenum, and this reactive force has Van der Waals force feature, can obtain few layer of selenizing molybdenum nanometer sheet by mechanically peel or ultrasonic stripping.Nearest report confirms that selenizing molybdenum shows the current density of hydrogen-evolution overpotential lower than moly-sulfide and Geng Gao in electrocatalytic hydrogen evolution reaction.In addition, along with the structural transfer of selenizing molybdenum from block to nanometer sheet, more avtive spot and lower hydrogen-evolution overpotential will be shown.For very thin selenizing molybdenum nanometer sheet when being limited to zero dimension, quantum effect and edge action can be more outstanding, and these will cause interesting physical properties.But still theory stage is rested on for the research of selenizing molybdenum quantum dot, preparation experimentally is not also implemented.For this reason, develop a kind of simple preparation method and for widening the industrial scale applications of selenizing molybdenum in photoelectron and electrocatalysis field, there is important value to the selenizing molybdenum quantum dot obtaining size uniform.
Summary of the invention
Goal of the invention: in order to overcome the deficiencies in the prior art; the invention provides a kind of preparation method of selenizing molybdenum quantum dot; the selenizing molybdenum of the high liquid phase shearing force dissociate water thermal synthesis utilizing high speed rotating cutter head to produce; can realize selenizing molybdenum quantum dot simple, prepare fast, there is low cost, potential prepared by mass-producing.
Technical scheme: for achieving the above object, the technical solution used in the present invention is:
A preparation method for selenizing molybdenum quantum dot, adopt two step synthesis selenizing molybdenum quantum dot, concrete methods of realizing is: first, is dispersed in hydrazine hydrate aqueous solution by molybdenum oxide and selenium powder, is obtained by reacting selenizing molybdenum crystal by hydrothermal solvent; Then, by crystalline dispersion for selenizing molybdenum in water and isopropyl alcohol mixture, transfer in agitation vat, the liquid phase shearing force produced by high-speed revolving blade makes selenizing molybdenum dissociate, and can obtain selenizing molybdenum quantum dot dispersion liquid.
The method specifically comprises the steps:
(1) first hydrazine hydrate aqueous solution is configured; Take molybdenum oxide and selenium powder respectively again, the mol ratio of molybdenum oxide and selenium powder is 1:2; Then the selenium powder taken is sprinkled in the hydrazine hydrate aqueous solution of configuration, stirs and form selenium powder dispersion liquid; Finally the molybdenum oxide taken is sprinkled in selenium powder dispersion liquid, stirs and form molybdenum oxide and selenium powder dispersion liquid; In hydrazine hydrate aqueous solution, the volume ratio of hydrazine hydrate and water is 1:40 ~ 1:10, and every 50mL hydrazine hydrate aqueous solution is sprinkled into 0.1 ~ 1g selenium powder;
(2) molybdenum oxide and selenium powder dispersion liquid are transferred in stainless steel cauldron carry out hydrothermal solvent reaction, after hydrothermal solvent has reacted, first throw out is filtered out, re-use second alcohol and water to rinse throw out, then baking oven throw out being placed in 45 ~ 55 DEG C is dried, and obtains selenizing molybdenum crystal; The temperature of reaction of hydrothermal solvent reaction is 140 ~ 220 DEG C, and the reaction times is 6 ~ 18h;
(3) by crystalline dispersion for selenizing molybdenum in water and isopropyl alcohol mixture, stir and form selenizing molybdenum dispersion liquid, be transferred in agitation vat by selenizing molybdenum dispersion liquid, the liquid phase shearing force produced by high-speed revolving blade makes selenizing molybdenum crystal dissociate, and can obtain selenizing molybdenum quantum dot dispersion liquid; In water and isopropyl alcohol mixture, the volume ratio of water and Virahol is 1:10 ~ 1:1, every 200 ~ 500mL water and isopropyl alcohol mixture dispersion 0.05 ~ 1g selenizing molybdenum crystal, and the rotating speed of high-speed revolving blade is 15000 ~ 25000rpm, and Dissociation time is 0.5 ~ 2h;
(4) by the centrifugation under 6000 ~ 10000rpm rotating speed of selenizing molybdenum quantum dot dispersion liquid, get supernatant liquid and be stable selenizing molybdenum quantum dot dispersion liquid, lateral size of dots is between 2 ~ 5nm.
Described agitation vat is household kitchen processor, such as soybean milk maker or Fresh Juice machine.
Beneficial effect: the preparation method of selenizing molybdenum quantum dot provided by the invention, shears in conjunction with hydrothermal method and liquid phase and dissociates, can realize selenizing molybdenum quantum dot simple, prepare fast, there is low cost, potential prepared by mass-producing.First this preparation method utilizes hydrothermal method to carry out ion-exchange and obtains selenizing molybdenum, can realize extensive preparation; The liquid phase shearing force produced by household kitchen processor cutter head high speed rotating is again dissociated selenizing molybdenum, and this liquid phase shearing mechanism also can be amplified to industrially scalableization further and produce, and thus the method has extendability and the applicability widely of height.Profit can obtain size uniform and the selenizing molybdenum quantum dot of high dispersing in this way, and this not only compensate for the deficiency of existing selenizing molybdenum nanostructure, also for the preparation of other two-dimensional material quantum dots provides possibility.
Accompanying drawing explanation
Fig. 1 is optical photograph and crystalline diffraction (XRD) collection of illustrative plates of selenizing molybdenum crystal prepared by the inventive method; Wherein, 1 (a) is the optical photograph of selenizing molybdenum crystal, the XRD figure that 1 (b) is selenizing molybdenum is composed, and the X-coordinate of 1 (b) is diffraction angle 2 θ (unit: degree), and the ordinate zou of 1 (b) is diffraction relative intensity (zero dimension);
Fig. 2 is scanning electron microscope (SEM) figure of selenizing molybdenum crystal prepared by the inventive method; Wherein, 2 (a) is low power SEM figure, and 2 (b) is high power SEM figure;
Fig. 3 is transmission electron microscope (TEM) figure of selenizing molybdenum crystal prepared by the inventive method; Wherein, 3 (a) is low power TEM figure, and 3 (b) is high power TEM figure;
Fig. 4 is the TEM figure of selenizing molybdenum quantum dot prepared by the inventive method; Wherein, 4 (a) is low power TEM figure, and 4 (b) is high power TEM figure;
Fig. 5 is the optical photograph of the Tyndall effect of selenizing molybdenum quantum dot prepared by the inventive method;
Fig. 6 is absorption spectrum and the luminescent spectrum of selenizing molybdenum crystal selenizing molybdenum quantum dot prepared by the inventive method; Wherein, 6 (a) is low power absorption spectrum, 6 (b) is luminescent spectrum, the X-coordinate of 6 (a) and 6 (b) is wavelength (unit: nm), and the ordinate zou of 6 (a) and 6 (b) is relative intensity (zero dimension).
Embodiment
Below in conjunction with accompanying drawing, the present invention is further described.
Embodiment 1
(1) prepare 50mL hydrazine hydrate aqueous solution, in hydrazine hydrate aqueous solution, hydrazine hydrate and water volume ratio are 1:20; Take molybdenum oxide and selenium powder respectively again, the mol ratio of molybdenum oxide and selenium powder is 1:2, and selenium powder quality is 0.2g; The selenium powder taken is sprinkled in the hydrazine hydrate aqueous solution of configuration, stirs and form selenium powder dispersion liquid; The molybdenum oxide taken is sprinkled in selenium powder dispersion liquid, stirs and form molybdenum oxide and selenium powder dispersion liquid;
(2) molybdenum oxide and selenium powder dispersion liquid are transferred to capacity is in the stainless steel cauldron of 80mL, carries out hydrothermal solvent reaction 6h under 140 DEG C of conditions; After hydrothermal solvent has reacted, first filter out throw out, re-use second alcohol and water and rinse throw out, the baking oven then throw out being placed in 50 DEG C is dried, and obtains selenizing molybdenum crystal;
(3) take in the crystalline dispersion water to 300mL of 0.1g selenizing molybdenum and isopropyl alcohol mixture, in water and isopropyl alcohol mixture, the volume ratio of water and Virahol is 1:1; Be transferred in the cooking machine of kitchen by selenizing molybdenum dispersion liquid, the liquid phase shearing force produced by high-speed revolving blade makes selenizing molybdenum crystal dissociate, and can obtain selenizing molybdenum quantum dot dispersion liquid; The rotating speed of high-speed revolving blade is 17000rpm, and Dissociation time is 1h;
(4) by the centrifugation under 6000rpm rotating speed of selenizing molybdenum quantum dot dispersion liquid, get supernatant liquid and be stable selenizing molybdenum quantum dot dispersion liquid, lateral size of dots is between 2 ~ 5nm.
Embodiment 2
(1) prepare 50mL hydrazine hydrate aqueous solution, in hydrazine hydrate aqueous solution, hydrazine hydrate and water volume ratio are 1:40; Take molybdenum oxide and selenium powder respectively again, the mol ratio of molybdenum oxide and selenium powder is 1:2, and selenium powder quality is 0.1g; The selenium powder taken is sprinkled in the hydrazine hydrate aqueous solution of configuration, stirs and form selenium powder dispersion liquid; The molybdenum oxide taken is sprinkled in selenium powder dispersion liquid, stirs and form molybdenum oxide and selenium powder dispersion liquid;
(2) molybdenum oxide and selenium powder dispersion liquid are transferred to capacity is in the stainless steel cauldron of 80mL, carries out hydrothermal solvent reaction 12h under 160 DEG C of conditions; After hydrothermal solvent has reacted, first filter out throw out, re-use second alcohol and water and rinse throw out, the baking oven then throw out being placed in 50 DEG C is dried, and obtains selenizing molybdenum crystal;
(3) take in the crystalline dispersion water to 200mL of 0.05g selenizing molybdenum and isopropyl alcohol mixture, in water and isopropyl alcohol mixture, the volume ratio of water and Virahol is 1:3; Be transferred in the cooking machine of kitchen by selenizing molybdenum dispersion liquid, the liquid phase shearing force produced by high-speed revolving blade makes selenizing molybdenum crystal dissociate, and can obtain selenizing molybdenum quantum dot dispersion liquid; The rotating speed of high-speed revolving blade is 23000rpm, and Dissociation time is 1.5h;
(4) by the centrifugation under 9000rpm rotating speed of selenizing molybdenum quantum dot dispersion liquid, get supernatant liquid and be stable selenizing molybdenum quantum dot dispersion liquid, lateral size of dots is between 2 ~ 5nm.
Embodiment 3
(1) prepare 50mL hydrazine hydrate aqueous solution, in hydrazine hydrate aqueous solution, hydrazine hydrate and water volume ratio are 1:12; Take molybdenum oxide and selenium powder respectively again, the mol ratio of molybdenum oxide and selenium powder is 1:2, and selenium powder quality is 0.5g; The selenium powder taken is sprinkled in the hydrazine hydrate aqueous solution of configuration, stirs and form selenium powder dispersion liquid; The molybdenum oxide taken is sprinkled in selenium powder dispersion liquid, stirs and form molybdenum oxide and selenium powder dispersion liquid;
(2) molybdenum oxide and selenium powder dispersion liquid are transferred to capacity is in the stainless steel cauldron of 80mL, carries out hydrothermal solvent reaction 8h under 180 DEG C of conditions; After hydrothermal solvent has reacted, first filter out throw out, re-use second alcohol and water and rinse throw out, the baking oven then throw out being placed in 50 DEG C is dried, and obtains selenizing molybdenum crystal;
(3) take in the crystalline dispersion water to 500mL of 0.2g selenizing molybdenum and isopropyl alcohol mixture, in water and isopropyl alcohol mixture, the volume ratio of water and Virahol is 1:1; Be transferred in the cooking machine of kitchen by selenizing molybdenum dispersion liquid, the liquid phase shearing force produced by high-speed revolving blade makes selenizing molybdenum crystal dissociate, and can obtain selenizing molybdenum quantum dot dispersion liquid; The rotating speed of high-speed revolving blade is 20000rpm, and Dissociation time is 2h;
(4) by the centrifugation under 10000rpm rotating speed of selenizing molybdenum quantum dot dispersion liquid, get supernatant liquid and be stable selenizing molybdenum quantum dot dispersion liquid, lateral size of dots is between 2 ~ 5nm.
Fig. 1 is optical photograph and the crystalline diffraction collection of illustrative plates of selenizing molybdenum crystal prepared by the present embodiment, and Fig. 2 is the scanning electron microscope (SEM) photograph of selenizing molybdenum crystal prepared by the present embodiment, and Fig. 3 is the transmission electron microscope picture of selenizing molybdenum crystal prepared by the present embodiment; More than characterize the sufficient proof successful preparation of selenizing molybdenum.Fig. 4 is the TEM figure of selenizing molybdenum quantum dot prepared by the present embodiment, and can know and see, the quantum dot of size uniform is successfully prepared.Fig. 5 is the optical photograph of the Tyndall effect of selenizing molybdenum quantum dot prepared by the present embodiment, demonstrates the dispersiveness that selenizing molybdenum quantum dot is stable.Fig. 6 is absorption spectrum and the luminescent spectrum of the selenizing molybdenum crystal prepared of the present embodiment and selenizing molybdenum quantum dot; Can see, selenizing molybdenum quantum dot has stronger UV luminescent characteristics than selenizing molybdenum powder body, embodies the superiority of quantum dot.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (4)
1. the preparation method of a selenizing molybdenum quantum dot, it is characterized in that: adopt two step synthesis selenizing molybdenum quantum dot, concrete methods of realizing is: first, is dispersed in hydrazine hydrate aqueous solution by molybdenum oxide and selenium powder, is obtained by reacting selenizing molybdenum crystal by hydrothermal solvent; Then, by crystalline dispersion for selenizing molybdenum in water and isopropyl alcohol mixture, transfer in agitation vat, the liquid phase shearing force produced by high-speed revolving blade makes selenizing molybdenum dissociate, and can obtain selenizing molybdenum quantum dot dispersion liquid.
2. the preparation method of selenizing molybdenum quantum dot according to claim 1, is characterized in that: the method specifically comprises the steps:
(1) first hydrazine hydrate aqueous solution is configured; Take molybdenum oxide and selenium powder respectively again, the mol ratio of molybdenum oxide and selenium powder is 1:2; Then the selenium powder taken is sprinkled in the hydrazine hydrate aqueous solution of configuration, stirs and form selenium powder dispersion liquid; Finally the molybdenum oxide taken is sprinkled in selenium powder dispersion liquid, stirs and form molybdenum oxide and selenium powder dispersion liquid; In hydrazine hydrate aqueous solution, the volume ratio of hydrazine hydrate and water is 1:40 ~ 1:10, and every 50mL hydrazine hydrate aqueous solution is sprinkled into 0.1 ~ 1g selenium powder;
(2) molybdenum oxide and selenium powder dispersion liquid are transferred in stainless steel cauldron carry out hydrothermal solvent reaction, after hydrothermal solvent has reacted, first throw out is filtered out, re-use second alcohol and water to rinse throw out, then baking oven throw out being placed in 45 ~ 55 DEG C is dried, and obtains selenizing molybdenum crystal; The temperature of reaction of hydrothermal solvent reaction is 140 ~ 220 DEG C, and the reaction times is 6 ~ 18h;
(3) by crystalline dispersion for selenizing molybdenum in water and isopropyl alcohol mixture, stir and form selenizing molybdenum dispersion liquid, be transferred in agitation vat by selenizing molybdenum dispersion liquid, the liquid phase shearing force produced by high-speed revolving blade makes selenizing molybdenum crystal dissociate, and can obtain selenizing molybdenum quantum dot dispersion liquid; In water and isopropyl alcohol mixture, the volume ratio of water and Virahol is 1:10 ~ 1:1, every 200 ~ 500mL water and isopropyl alcohol mixture dispersion 0.05 ~ 1g selenizing molybdenum crystal, and the rotating speed of high-speed revolving blade is 15000 ~ 25000rpm, and Dissociation time is 0.5 ~ 2h;
(4) by the centrifugation under 6000 ~ 10000rpm rotating speed of selenizing molybdenum quantum dot dispersion liquid, get supernatant liquid and be stable selenizing molybdenum quantum dot dispersion liquid, lateral size of dots is between 2 ~ 5nm.
3. the preparation method of selenizing molybdenum quantum dot according to claim 1, is characterized in that: described agitation vat is household kitchen processor.
4. the preparation method of selenizing molybdenum quantum dot according to claim 3, is characterized in that: described household kitchen processor is soybean milk maker or Fresh Juice machine.
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| CN110079317A (en) * | 2019-04-17 | 2019-08-02 | 安徽理工大学 | The synthetic method and application of molybdenum disulfide fluorescence quantum |
| CN110079317B (en) * | 2019-04-17 | 2022-09-16 | 安徽理工大学 | Synthesis method and application of molybdenum disulfide fluorescent quantum dots |
| CN111747384A (en) * | 2020-06-29 | 2020-10-09 | 西安交通大学医学院第一附属医院 | Method for preparing low-toxicity molybdenum diselenide by ultrasonic wave |
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Application publication date: 20160427 |