CN104192909B - A kind of method of preparing Wolfram disulfide nano bar - Google Patents
A kind of method of preparing Wolfram disulfide nano bar Download PDFInfo
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- CN104192909B CN104192909B CN201410379340.XA CN201410379340A CN104192909B CN 104192909 B CN104192909 B CN 104192909B CN 201410379340 A CN201410379340 A CN 201410379340A CN 104192909 B CN104192909 B CN 104192909B
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Abstract
The invention discloses a kind of method of preparing Wolfram disulfide nano bar, comprise the following steps: a. adds tungsten disulfide powder in the mixed solvent of water and ethanol, carries out hydrothermal synthesis reaction; B. more reacted solution is carried out ultrasonic, centrifugally, obtain Wolfram disulfide nano bar. This preparation method's mild condition, reaction is green, agents useful for same is novel and simple, is applicable to a large amount of preparations and suitability for industrialized production, is a kind of method that has application prospect.
Description
Technical field
The invention belongs to nano material preparing technical field, relate in particular to a kind of method of preparing Wolfram disulfide nano bar.
Background technology
WS2That the curing of the interactional stratiform transition metal of Van der Waals force occurs between one typically has layer by layerThing. The WS of nanostructured2There is the light conduction and the excellent frictional behaviour that strengthen catalytic performance, excellence, can be used for tooIn sun energy battery, field-effect transistor. WS2Nanometer rods with the method for sonochemistry have bibliographical information (Nikotenko, SI,J.Mater.Chem.2002,12,1450-1452.), it is to use W (Co)6In dimethylamino benzophenone alkane solvents excess of sulfur inertiaUnder condition, react.
Through retrieval, the Chinese invention patent that publication number is CN1793304A, discloses " as two of antifriction additiveTungsten sulfide nanometer rods and preparation method thereof ". It is characterized in that comprising the following steps: adopt planetary high-energy ball mill, willThe tungsten disulfide powder of common micron order layer structure and micron order sulphur powder mixing and ball milling, acquisition nanometer layer sheet formPresoma, then, in reactor, adds dispersant polyethylene glycol, at 200～260 DEG C of temperature, rotating speed 200～400r/minLower insulation is naturally cooling after 10～30 hours, because solvent heat inducing action causes structural change, obtains tungsten disulfide and receivesRice rod. Planetary high-energy ball mill production efficiency is low, and the method is not suitable for large-scale industrial production.
Publication number is the Chinese invention patent of CN102701283A, discloses " a kind of Wolfram disulfide nano bar of preparingMethod ". It is characterized in that comprising the following steps: (1) obtain solution: by (NH4)2WO4、CS(NH2)2、NH2OHHCl and surfactant are soluble in water, dissolve and obtain solution, then by the pH value of acid-conditioning solution be5～6.5; (2), after solution step (1) being obtained stirs, move into stainless steel cauldron, sealing, after isothermal reaction,Be cooled to room temperature, obtain product; (3) separate above-mentioned product, washing, dry, obtains tungsten disulfide and receivesRice rod. The Wolfram disulfide nano bar uniform particle diameter for preparing by the method for the invention, controlled. The method is to formerMaterial requires harsh, is not suitable for large-scale industrial production.
Therefore, those skilled in the art is devoted to develop a kind of Wolfram disulfide nano of applicable large-scale industrial productionRod preparation method.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of new method of preparing Wolfram disulfide nano bar, to be applicable toLarge-scale industrial production.
In order to solve the problems of the technologies described above, a kind of method of preparing Wolfram disulfide nano bar is provided, comprise the following steps:
A. tungsten disulfide powder is added in the mixed solvent of water and ethanol, carry out hydrothermal synthesis reaction;
B. more reacted solution is carried out ultrasonic, centrifugally, centrifugal gained precipitation is Wolfram disulfide nano bar.
Preferably, in step a, the quality of tungsten disulfide powder is 1mg～1kg.
Preferably, in step a, the mixed solvent of water and ethanol is water: ethanol=1:1～1:100 by water and ethanol by volumeConfiguration forms.
More preferably, water and ethanol volume ratio are water: ethanol=1:1～7:13.
Preferably, in step a, the volume of water is 5～1000ml.
Preferably, in step a, the volume of ethanol is 5～1000ml.
Preferably, in step a, the reaction temperature of hydrothermal synthesis reaction is 80～220 DEG C, and the reaction time is 5～48h.
Preferably, in step b, the ultrasonic time is 0.5～50h, and ultrasonic power is 100～600W.
Preferably, in step b, centrifugal speed is 100～10000rpm, and centrifugation time is 10～360min.
The present invention also provides the Wolfram disulfide nano bar of preparing according to said method.
This invention mild condition, reaction is green, agents useful for same is novel and simple, is applicable to a large amount of preparations and suitability for industrialized production,It is a kind of method that has application prospect.
Below with reference to accompanying drawing, the technique effect of design of the present invention, concrete structure and generation is described further, withUnderstand fully object of the present invention, feature and effect.
Brief description of the drawings
Fig. 1 is the low resolution transmission electron microscope image of the Wolfram disulfide nano bar prepared of the embodiment of the present invention 1;
Fig. 2 is the high-resolution transmission electron microscope image of the Wolfram disulfide nano bar prepared of the embodiment of the present invention 1;
Fig. 3 is preparation method's schematic diagram of the present invention.
Detailed description of the invention
Embodiment 1
A method of preparing Wolfram disulfide nano bar, specifically comprises the following steps:
A. be that water and ethanol are configured to mixed solvent by water: ethanol=7:13 according to volume ratio; By 30mg curing tungsten powderBody adds in the above-mentioned mixed solvent of 20ml, carries out hydrothermal synthesis reaction 10h at 200 DEG C;
B. again by reacted solution ultrasonic 1h under power 400W, by the centrifugal 30min of 500rpm, obtain twoTungsten sulfide nanometer rods.
Fig. 1 is the low resolution transmission electron microscope image of the Wolfram disulfide nano bar prepared of the present embodiment, can from Fig. 1The length of knowing Wolfram disulfide nano bar prepared by the present embodiment is about 100～1000nm. Fig. 2 be the present embodiment prepare twoThe high-resolution transmission electron microscope image of tungsten sulfide nanometer rods, the tungsten disulfide that as can be known from Fig. 2 prepared by the present embodiment is receivedThe width of rice rod is about 20nm. Fig. 3 is preparation method's schematic diagram of the present invention.
Embodiment 2
A method of preparing Wolfram disulfide nano bar, specifically comprises the following steps:
A. be that water and ethanol are configured to mixed solvent by water: ethanol=7:13 according to volume ratio; By 30mg curing tungsten powderBody adds in the above-mentioned mixed solvent of 20ml, carries out hydrothermal synthesis reaction 15h at 180 DEG C;
B. again by reacted solution ultrasonic 1h under power 400W, by the centrifugal 30min of 500rpm, obtain twoTungsten sulfide nanometer rods.
Embodiment 3
A method of preparing Wolfram disulfide nano bar, specifically comprises the following steps:
A. be that water and ethanol are configured to mixed solvent by water: ethanol=1:1 according to volume ratio; By 30mg tungsten disulfide powderAdd in the above-mentioned mixed solvent of 20ml, carry out hydrothermal synthesis reaction 10h at 200 DEG C;
B. again by reacted solution ultrasonic 1h under power 400W, by the centrifugal 30min of 500rpm, obtain twoTungsten sulfide nanometer rods.
Embodiment 4
A method of preparing Wolfram disulfide nano bar, specifically comprises the following steps:
A. be that water and ethanol are configured to mixed solvent by water: ethanol=1:1 according to volume ratio; By 30mg tungsten disulfide powderAdd in the above-mentioned mixed solvent of 20ml, carry out hydrothermal synthesis reaction 5h at 220 DEG C;
B. again by reacted solution ultrasonic 50h under power 100W, by the centrifugal 360min of 100rpm, obtainWolfram disulfide nano bar.
Embodiment 5
A method of preparing Wolfram disulfide nano bar, specifically comprises the following steps:
A. be that water and ethanol are configured to mixed solvent by water: ethanol=1:100 according to volume ratio; By 30mg curing tungsten powderBody adds in the above-mentioned mixed solvent of 20ml, carries out hydrothermal synthesis reaction 48h at 80 DEG C;
B. again by reacted solution ultrasonic 0.5h under power 600W, by the centrifugal 10min of 10000rpm, obtainTo Wolfram disulfide nano bar.
More than describe preferred embodiment of the present invention in detail. Should be appreciated that those of ordinary skill in the art withoutNeed creative work just can design according to the present invention make many modifications and variations. Therefore, in the art allTechnical staff under this invention's idea on the basis of existing technology can by logical analysis, reasoning, or a limited experimentWith the technical scheme obtaining, all should be in by the determined protection domain of claims.
Claims (7)
1. a method of preparing Wolfram disulfide nano bar, is characterized in that, it comprises the following steps:
A. tungsten disulfide powder is added in the mixed solvent of water and ethanol, carry out hydrothermal synthesis reaction; Described waterFor configuring, water: ethanol=1:1～1:100 formed by volume by water and ethanol with the mixed solvent of ethanol; Described waterThe reaction temperature of thermal synthesis reaction is 80～220 DEG C, and the reaction time is 5～48h;
B. more reacted solution is carried out ultrasonic, centrifugally, centrifugal gained precipitation is Wolfram disulfide nano bar.
2. the method for preparing Wolfram disulfide nano bar according to claim 1, is characterized in that step aDescribed in the quality of tungsten disulfide powder be 1mg～1kg.
3. the method for preparing Wolfram disulfide nano bar according to claim 1, is characterized in that, water and secondAlcohol volume ratio is water: ethanol=1:1～7:13.
4. the method for preparing Wolfram disulfide nano bar according to claim 1, is characterized in that step aDescribed in the volume of water be 5～1000mL.
5. the method for preparing Wolfram disulfide nano bar according to claim 1, is characterized in that step aDescribed in the volume of ethanol be 5～1000mL.
6. the method for preparing Wolfram disulfide nano bar according to claim 1, is characterized in that step bDescribed in the ultrasonic time be 0.5～50h, described ultrasonic power is 100～600W.
7. the method for preparing Wolfram disulfide nano bar according to claim 1, is characterized in that step bDescribed in centrifugal speed be 100～10000rpm, centrifugation time is 10～360min.
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| CN104993140B (en) * | 2015-06-08 | 2017-10-27 | 陕西科技大学 | A kind of fibrous WS2The preparation method of nanometer anode material |
| CN104925866B (en) * | 2015-06-08 | 2016-08-24 | 陕西科技大学 | A kind of bar-shaped WS of high length-diameter ratio2nanocrystalline preparation method |
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| CN1793304A (en) * | 2006-01-17 | 2006-06-28 | 浙江大学 | Wolfram disulfide nano bar used as friction reducing additive and preparation process thereof |
| CN102583547B (en) * | 2012-03-07 | 2013-12-04 | 长安大学 | Preparation method of monolayer MoS2 nano-sheet solution |
| CN103771521B (en) * | 2014-02-26 | 2015-02-25 | 新疆大学 | Method for preparing tungsten disulfide nano sheet |
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