CN110217824A - Molybdenum disulfide quantum dot and its preparation method and application and photoelectric device, sensor, catalyst or lubricant - Google Patents
Molybdenum disulfide quantum dot and its preparation method and application and photoelectric device, sensor, catalyst or lubricant Download PDFInfo
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Abstract
The present invention provides a kind of molybdenum disulfide quantum dot and its preparation method and application and photoelectric device, sensor, catalyst or lubricants, it is related to field of material technology, the preparation method includes: to mix molybdenum disulfide, tannic acid and ionic liquid, obtains mixed liquor；The mixed liquor is ultrasonically treated and is heated, to obtain the molybdenum disulfide quantum dot.This method is simple, convenient, it is easy to accomplish, it is time-consuming short, consume low, yield is high, favorable repeatability, is suitble to large-scale production and without secondary pollution to environment, the molybdenum disulfide quantum dot size being prepared is smaller and of uniform size, and the number of plies is less, good dispersion.
Description
Technical field
The present invention relates to field of material technology, in particular to a kind of molybdenum disulfide quantum dot and preparation method thereof and
Purposes and photoelectric device, sensor, catalyst or lubricant.
Background technique
With the development of science and technology, non-environmental-pollution, friction durability length, low friction, solid lubricant are as lubrication
The most promising developing direction in field, pays close attention to by common people.Solid self lubricant material greatly breaches tradition in performance
The operating limit of material is widely applied to the high-tech areas such as electronics, biology, space flight and aviation.The solid of layer structure moistens
Lubrication prescription such as molybdenum disulfide (MoS2) it is ideal vacuum lubricant, irreplaceable work is played in space flight lubricating area
With.Since solid molybdenum disulfide is difficult to be dispersed into uniform colloidal sol, the molybdenum disulfide powder of micron order bulky grain be easy to cause filter
The blocking of oil-piping or the bottom for being deposited on grease-box decline its lubricity acutely, limit its application significantly and promote.
Currently, the preparation method of molybdenum disulfide quantum dot mainly has two major classes: top-to-bottom method and from bottom to top
Method, including mechanical stripping method, liquid phase stripping method, chemical synthesis, chemical gaseous phase lamination, electron beam etching method etc..It is mechanical
Stripping method prepares that molybdenum disulfide quantum dot yield is extremely low, time-consuming, and is difficult to that molybdenum disulfide quantum dot is prepared；Chemical synthesis
The molybdenum disulfide quantum dot surface of method preparation usually contains a variety of organic ligands, is not easy to eliminate, hinders subsequent some uses；
Chemical gaseous phase lamination, electron beam etching method can not on a large scale and high efficiency prepares molybdenum disulfide quantum dot；Liquid phase stripping method is
A kind of preferable preparation method, however the yield of molybdenum disulfide quantum dot is still lower.Develop a kind of high yield, prepare with scale
The preparation method of molybdenum disulfide quantum dot is extremely urgent.
In view of this, the present invention is specifically proposed.
Summary of the invention
One of the objects of the present invention is to provide a kind of simple, convenient, it is easy to accomplish, consumption is low, and yield is high, can weigh
Renaturation is good, is suitble to large-scale production or the method for preparing molybdenum disulfide quantum dot without secondary pollution to environment, utilizes the party
The molybdenum disulfide quantum dot size that method is prepared is smaller and of uniform size, and the number of plies is less, good dispersion.
The second object of the present invention is to provide a kind of size smaller and of uniform size, and the number of plies is less, and the two of good dispersion
Molybdenum sulfide quantum dot.
In order to realize above-mentioned purpose of the invention, the following technical scheme is adopted:
A kind of preparation method of molybdenum disulfide quantum dot, comprising: molybdenum disulfide, tannic acid and ionic liquid are mixed, obtained
Obtain mixed liquor；The mixed liquor is ultrasonically treated and is heated, to obtain the molybdenum disulfide quantum dot.
Further, for the mixed liquor by pretreatment, the pretreatment includes: to carry out at grinding to the mixed liquor
Reason；
Preferably, the time of the grinding is 10-30min, preferably 15-20min.
Further, the mass ratio of the molybdenum disulfide, tannic acid and ionic liquid is 2:1:(2-8)；Preferably 2:1:
5。
Further, the ionic liquid includes 1- butyl -3- methylimidazole hexafluorophosphate；
Preferably, the partial size of the molybdenum disulfide is 2-10 microns.
Further, after carrying out the milled processed to the mixed liquor, before being ultrasonically treated and being heated,
Further include the steps that being diluted processing to the mixed liquor using solvent；
Preferably, the mass volume ratio of the molybdenum disulfide and solvent is (0.1-1) g:50-100mL, preferably 0.5g:
50mL；
Preferably, the solvent includes N-Methyl pyrrolidone and/or n,N-Dimethylformamide, preferably N- methyl pyrrole
Pyrrolidone.
Further, the ultrasonic treatment and/or the heat treatment are repeated to the mixed liquor；
Preferably, the mixed liquor is repeated alternately to be ultrasonically treated and heat；
Preferably, the number for repeating the alternately described ultrasonic treatment and the heat treatment is 1-3 times；
Preferably, the power of the ultrasonic treatment is 200-300W, and the time is 0.5-2 hours；
Preferably, the temperature of the heat treatment is 110-140 DEG C, and the time is 0.5-2 hours.
Further, which further includes withering to the product of the ultrasonic treatment and heat treatment
Step, the drying carry out under vacuum conditions；
Preferably, the preparation method further include: the product after the drying is dissolved in after polar solvent freeze and is done
Dry step.
A kind of molybdenum disulfide quantum dot is prepared using mentioned-above preparation method；
Preferably, the molybdenum disulfide quantum dot is layer structure, and the size of the molybdenum disulfide quantum dot is 2-4nm；
Preferably, the molybdenum disulfide quantum dot with a thickness of 0.7-1.2nm.
A kind of mentioned-above molybdenum disulfide quantum dot is in production photoelectric device, sensor, catalyst or lubricant
Purposes.
A kind of photoelectric device, sensor, catalyst or lubricant, including mentioned-above molybdenum disulfide quantum dot.
Compared with prior art, the invention has the benefit that
In the present invention, the interlayer Van der Waals force that the energy that ultrasonic wave provides when ultrasonic treatment can weaken molybdenum disulfide makes its stripping
From and obtain few layer nanometer sheet, heat offer energy can make molybdenum disulfide nano sheet isolated into smaller size to
Gradually form quantum dot；Moreover, the surface of ionic liquid closely can can effectively be cut with the surface of molybdenum disulfide
Weak interlayer Van der Waals force, and then can efficiently remove molybdenum disulfide at multi-layer nano piece, the knot of tannic acid and molybdenum disulfide
Closing can greatly inhibit the nanometer sheet removed compound for 75.95eV much larger than the combination energy of the interlayer of molybdenum disulfide,
So that molybdenum disulfide are efficiently processed into the quantum dot that size is smaller, the number of plies is less, and quantum dot using the above method
Yield it is higher, can be more than 80%；In addition, the above method is simple, convenient, it is easy to accomplish, it is time-consuming short, consume low, cost
Low, yield is high, favorable repeatability, is suitble to large-scale production or without secondary pollution to environment.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, is also possible to obtain other drawings based on these drawings.
Fig. 1 is the ultraviolet-visible absorption spectroscopy of molybdenum disulfide quantum dot in deionized water in embodiment 1；
Fig. 2 is the low power transmission electron microscope image (TEM) of molybdenum disulfide quantum dot in embodiment 1；
Fig. 3 is the high power transmission electron microscope image (HRTEM) of molybdenum disulfide quantum dot in embodiment 1；
Fig. 4 is the atomic force microscope image (AFM) of molybdenum disulfide quantum dot in embodiment 1.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.
In one aspect of the invention, the present invention provides a kind of preparation method of molybdenum disulfide quantum dot, this method packets
It includes:
S100: molybdenum disulfide, tannic acid and ionic liquid are mixed, and obtain mixed liquor.
In certain embodiments of the present invention, for the mixed liquor by pretreatment, the pretreatment includes: to described mixed
Liquid is closed to be ground.The milled processed can remove molybdenum disulfide to multilayer nanometer sheet, conducive to subsequent step as a result,
It carries out, and also helps tannic acid and mixed with the uniform of molybdenum disulfide.
In some preferred embodiments of the invention, time of the grinding be 10-20min (such as 10min,
12min, 14min, 16min, 18min or 20min etc.).Milling time is suitable as a result, can effectively remove molybdenum disulfide
To multilayer nanometer sheet, tannic acid mixes relatively uniform with molybdenum disulfide.In certain embodiments of the present invention, the grinding
It can be carried out in mortar (such as agate mortar etc.), it is simple, convenient, it is easy to accomplish.
In certain embodiments of the present invention, the mass ratio of the molybdenum disulfide, tannic acid and ionic liquid is 2:1:
(2-8), such as the mass ratio of molybdenum disulfide, tannic acid and ionic liquid can be 2:1:(2/3/4/5/6/7/8).It is red as a result,
The dosage of peaceful acid and ionic liquid is suitable, conducive to molybdenum disulfide to be removed to the lamellar structure less at the number of plies when subsequent processing.Phase
For above-mentioned amount ranges, when the mass ratio of tannic acid and molybdenum disulfide is excessive, then reagent waste is caused, increase molybdenum disulfide
The preparation cost of quantum dot is then difficult to molybdenum disulfide carrying out stratiform stripping when the mass ratio of tannic acid and molybdenum disulfide is too small
From being unfavorable for obtaining molybdenum disulfide quantum dot；When the mass ratio of ionic liquid and molybdenum disulfide is excessive, then cause reagent unrestrained
Take, the preparation cost for increasing molybdenum disulfide quantum dot is then difficult to obtain when the mass ratio of ionic liquid and molybdenum disulfide is too small
The slurries of molybdenum disulfide dispersion, to increase grinding difficulty.
In some preferred embodiments of the invention, the mass ratio of molybdenum disulfide, tannic acid and ionic liquid is 2:1:
5.It is more advantageous to as a result, and molybdenum disulfide is removed to the lamellar structure less at the number of plies.
In certain embodiments of the present invention, the ionic liquid includes 1- butyl -3- methylimidazole hexafluorophosphate.
Material source is extensive as a result, can be closer with the surface of molybdenum disulfide, conducive to more efficiently to molybdenum disulfide removed with
Obtain few layer molybdenum disulfide.
In certain embodiments of the present invention, other surface tension and molybdenum disulfide interlayer power also can be selected in ionic liquid
It is close, the reagent that can be dispersed in DMF (n,N-Dimethylformamide) or NMP (N-Methyl pyrrolidone) equal solvent.At this
In some preferred embodiments of invention, the partial size of the molybdenum disulfide is 2-10 microns.It is conducive to save preparation curing as a result,
The time of molybdenum quantum dot.For example, the partial size of molybdenum disulfide is 2,3,4,5,6,7,8,9 or 10 microns.
In certain embodiments of the present invention, it after carrying out the milled processed to the mixed liquor, carries out at ultrasound
Before reason and heat treatment, further include the steps that being diluted processing to the mixed liquor using solvent.Thus, it is possible to reduce mixed
The concentration of liquid is closed, the mobility of enhancing molybdenum disulfide in the solution, being more advantageous to will grind under subsequent ultrasonic and/or heat effect
Molybdenum disulfide after mill in mixed liquor is further removed and isolates into smaller size of molybdenum disulfide quantum dot.Of the invention one
In a little embodiments, above-mentioned dilution processing can be carried out in closed container, such as processing can be diluted in serum bottle,
Thus, it is possible to provide good space for dilution, the volatilization loss of solvent is hardly caused.
In some preferred embodiments of the invention, the mass volume ratio of the molybdenum disulfide and solvent is (0.1-1)
G:(50-100) mL, preferably 0.5g:50mL.The effect for diluting mixed liquor as a result, is preferable.
In some preferred embodiments of the invention, the solvent includes N-Methyl pyrrolidone, N, N- dimethyl methyl
At least one of amide, preferably N-Methyl pyrrolidone.Material source is extensive as a result, and price is lower, molybdenum disulfide, pellet
Peaceful acid and ionic liquid are preferable in dispersion effect wherein.
In some preferred embodiments of the invention, the mixed liquor is ultrasonically treated and is heated, so as to
Obtain the molybdenum disulfide quantum dot.
In certain embodiments of the present invention, the power of the ultrasonic treatment be 200-300W (such as 200W, 220W,
240W, 260W, 280W perhaps 300W etc.) time is 0.5-2 hours (such as 0.5 hour, 1 hour, 1.5 hours or 2 hours
Deng).The energy that ultrasonic wave provides as a result, can overcome the interlayer Van der Waals force of molybdenum disulfide to make its piece layer open, thus by lamella
Further removing.When the power of ultrasonic treatment is excessive or the overlong time of ultrasonic treatment, then lead to the waste of the energy, increases
The preparation cost of molybdenum disulfide quantum dot is then removed when the power of ultrasonic treatment is too small or the time of ultrasonic treatment is too short
The effect of molybdenum disulfide is relatively poor, and the yield of molybdenum disulfide quantum dot is lower.
In certain embodiments of the present invention, the temperature of the heat treatment is 110-140 DEG C of (such as 110 DEG C, 115
DEG C, 120 DEG C, 125 DEG C, 130 DEG C, 135 DEG C or 140 DEG C etc.), the time be 0.5-2 hours (such as 0.5 hour, 1 hour, it is 1.5 small
When or 2 hours etc.).The energy that above-mentioned temperature provides as a result, can make molybdenum disulfide nano sheet isolated into smaller size from
And gradually form quantum dot.When the temperature of heat treatment is excessively high or overlong time, then it is easy to that molybdenum disulfide is caused to be oxidized,
It influences and the function of molybdenum disulfide quantum dot, while will cause energy waste, when the temperature of heat treatment is too low or time mistake
In short-term, then the effect for isolating molybdenum disulfide nano sheet is relatively poor, and the yield of molybdenum disulfide quantum dot is lower.
In some preferred embodiments of the invention, the ultrasonic treatment and/or institute are repeated to the mixed liquor
State heat treatment.It is conducive to obtain smaller molybdenum disulfide quantum dot as a result,；When repeat be ultrasonically treated and heat
When, due to both being ultrasonically treated and heating alternately, molybdenum disulfide can be made to be alternately carried out removing and crushing,
The quantum dot being adsorbed on molybdenum disulfide nano sheet can also be made to fall off, conducive to reduce molybdenum disulfide quantum dot the number of plies, and benefit
In the uniformity for improving molybdenum disulfide quantum dot size, the yield of molybdenum disulfide quantum dot is significantly improved.
In some preferred embodiments of the invention, repeat the number of the ultrasonic treatment and the heat treatment
Respectively 1-3 times (such as 1 time, 2 times or 3 times).Thus, it is possible to significantly improve the yield of molybdenum disulfide quantum dot.When repetition
When the number for being ultrasonically treated and being heated is excessive, the effect for improving the yield of molybdenum disulfide quantum dot is relatively unobvious,
The cost is relatively high, and the production cycle is relatively long.
In certain embodiments of the present invention, which further includes the production to the ultrasonic treatment and heat treatment
The withering step of object, the drying carry out under vacuum conditions.Drying efficiency is high as a result, in drying process
Molybdenum disulfide quantum dot is hardly reunited, and molybdenum disulfide good dispersion further increases the yield of molybdenum disulfide quantum dot.
In certain embodiments of the present invention, the preparation method further include: the product after the drying is dissolved in pole
The step of being freeze-dried after property solvent.
In certain specific embodiments of the invention, the molybdenum disulfide after drying can be redissolved in deionized water, second
Alcohol, N-Methyl pyrrolidone or n,N-Dimethylformamide isopolarity solvent, without fines means such as ultrasound, grindings
Reach the preferable dispersion liquid of dispersion effect, greatly expands its use scope.When polar solvent is water, the dispersion liquid of acquisition can
Stablize preservation 1 year or more, and the concentration of molybdenum disulfide quantum dot is 12g/L or more in the dispersion liquid, overcomes and contain two at present
The low defect of solid content in the dispersion liquid of molybdenum sulfide quantum dot.
After product after drying is dissolved in polar solvent, cryogenic vacuum Refrigeration Technique can be used, removed in the way of distillation
The fabulous molybdenum disulfide quantum dot powder of ultra-dispersed property is made in polar solvent and partial organic substances (such as mentioned-above solvent)
Body.
In certain specific embodiments of the invention, prepare the method for molybdenum disulfide quantum dot the following steps are included:
(1) the tannic acid powder of the molybdenum disulfide powder of 500mg and 250mg are placed in mortar, 0.5-2g ion is added
Liquid simultaneously grinds 15min in mortar, obtains the first dispersion liquid；
(2) the first dispersion liquid is diluted using 50mL solvent and is transferred to closed glass container (such as 250mL serum bottle etc.),
Obtain the second dispersion liquid；
(3) by the closed glass container equipped with the second dispersion liquid, it is small to be placed in processing 0.5-2 in supersonic wave cleaning machine
When, it is subsequently transferred in baking oven be heat-treated 0.5-2 hours at 120 DEG C；
(4) it repeats described in (3) step 1-3 times；
(5) gained mixture in (4) is evaporated under vacuum conditions, obtains molybdenum disulfide quantum dot powder；This powder can
It is redissolved in the segment polarities solvent such as deionized water easily, obtains third dispersion liquid.
In the above method, the alternately removing and fragmentation to molybdenum disulfide assists liquid phase stripping method compared to current electrochemistry
(having a lithium ion residual, complex process, equipment cost is high) and chemical synthesis (remain organic group, dangerous not environmentally) etc.
Method has apparent advantage, can overcome molybdenum disulfide quantum dot low yield obtained in the prior art, diameter of particle unevenness, divide
From the defects of difficult, powder is easy to reunite；Method and process of the invention is simple, time-consuming short, safety and environmental protection, and at low cost, yield height (can
More than 80%), favorable repeatability, molybdenum disulfide quantum dot can be separated with solvent easily, can get good dispersion, of uniform size
Molybdenum disulfide quantum dot, realize from molybdenum disulfide block to quantum dot extensive industrialization preparation, be molybdenum disulfide amount
Application of the son point in fields such as photoelectric device, sensor, catalysis, battery, storage and lubricants lays the foundation, and easily realizes low cost
Industrialization production.And the molybdenum disulfide quantum dot being prepared using method of the invention can easy distribution in polar solvent
In, substantially increase its application range.
In another aspect of this invention, the present invention provides a kind of molybdenum disulfide quantum dots.The molybdenum disulfide quantum dot is
It is prepared using mentioned-above preparation method.
In certain embodiments of the present invention, the molybdenum disulfide quantum dot is layer structure, the molybdenum disulfide amount
The size of son point is 2-4nm.Molybdenum disulfide quantum dot size is uniform as a result, good dispersion, can be applied to self-replenishing solid profit
Sliding coating.It should be noted that the length of molybdenum disulfide quantum dot refers to flaky molybdenum disulfide quantum dot perpendicular to thickness
On direction between any two points the distance of line maximum value.
In certain embodiments of the present invention, molybdenum disulfide quantum dot is layer structure, and is round or similar round,
Size refers to round or similar round diameter.
In certain embodiments of the present invention, the molybdenum disulfide quantum dot with a thickness of 0.7-1.2nm.As a result, two
The thinner thickness of molybdenum sulfide quantum dot, closer to single layer structure, dispersibility is more preferable, is more suitable for self-replenishing solid lubrication and applies
Layer.
Molybdenum disulfide quantum dot size provided by the invention is smaller, and specific surface area is larger, on the surface of the material adhesion with cover
Lid degree all significantly improves, and the molybdenum disulfide quantum dot of smaller size has extremely strong quantum confined effect and boundary effect,
Meanwhile in the case where identical in quality, the granule number of the molybdenum disulfide quantum dot of smaller size increases severely, and antiwear and reducing friction performance obtains
Exponential raising, so that it has more application prospect in terms of Nanotribology；In addition, the molybdenum disulfide of super-small be easier to
The problem of water or organic binder uniformly mix, and improve bulk molybdenum disulfide bad dispersibility advantageously forms fine and close solid
Lubricant coating.
In another aspect of this invention, the present invention provides a kind of mentioned-above molybdenum disulfide quantum dots in production photoelectricity
Purposes in device, sensor, catalyst or lubricant.
It should be noted that the molybdenum disulfide quantum dot has mentioned-above all feature and advantage, herein not after
It repeats more.
In another aspect of this invention, the present invention provides a kind of photoelectric device, sensor, catalyst or lubricant,
Including mentioned-above molybdenum disulfide quantum dot.
It should be noted that the molybdenum disulfide quantum dot has mentioned-above all feature and advantage, herein not after
It repeats more.
In certain embodiments of the present invention, photoelectric device in addition to include mentioned-above molybdenum disulfide quantum dot it
It outside, further include photo resistance, photodiode etc.；The type of sensor can be gas sensor, in addition to front institute
Except the molybdenum disulfide quantum dot stated, further includes the structure that conventional gas sensors should have, no longer excessively repeat herein.
Present invention will be further explained by specific examples below, it should be understood, however, that, these embodiments are only
It is used, is but should not be understood as present invention is limited in any form for being described in more detail.
Embodiment 1
The preparation method of molybdenum disulfide quantum dot, includes the following steps:
(1) the tannic acid powder of the molybdenum disulfide powder of 500mg and 250mg are placed in mortar, 2g ionic liquid is added
And 15min is ground in mortar, obtain the first dispersion liquid；
(2) the first dispersion liquid is diluted using 50mLNMP and is transferred to closed glass container, obtain the second dispersion liquid；
(3) by the closed glass container equipped with the second dispersion liquid, it is placed in the supersonic wave cleaning machine that power is 240W
Middle processing 0.5 hour, is subsequently transferred in baking oven be heat-treated 0.5 hour at 120 DEG C；
(4) step 2 time described in (3) is repeated；
(5) gained mixture in (4) is evaporated under vacuum conditions, obtains molybdenum disulfide quantum dot.
The resulting molybdenum disulfide quantum dot of the present embodiment is more stable, can store at room temperature 1 year or more.By the present embodiment
1 resulting molybdenum disulfide quantum dot is characterized, as a result as shown in 1-4 figure.
Molybdenum disulfide quantum dot shows apparent absorption characteristic, absorption spectra in the region 250-450nm as can be seen from Figure 1
Show apparent similar quantum point type absorption curve, it was demonstrated that the present invention obtains molybdenum disulfide quantum dot really；It can from Fig. 2
To find out, molybdenum disulfide quantum dot monodispersity is good, of uniform size, and length is in 3nm or so；It can clearly be seen that from Fig. 3
The lattice fringe of molybdenum disulfide quantum dot atomic layer, wherein spacing of lattice 0.27nm；Obtained by as can be seen from Figure 4
Molybdenum disulfide quantum dot corresponds to single layer molybdenum disulfide with a thickness of 0.7nm.
Embodiment 2
The present embodiment prepares the method for molybdenum disulfide quantum dot with embodiment 1, the difference is that ionic liquid dosage is
0.5g。
Embodiment 3
The present embodiment prepares the method for molybdenum disulfide quantum dot with embodiment 1, the difference is that ionic liquid dosage is
2g。
Embodiment 4
The present embodiment prepares the method for molybdenum disulfide quantum dot with embodiment 1, the difference is that ionic liquid dosage is
1.5g。
Embodiment 5
The present embodiment prepares the method for molybdenum disulfide quantum dot with embodiment 1, the difference is that ionic liquid dosage is
0.2g。
Embodiment 6
The present embodiment prepares the method for molybdenum disulfide quantum dot with embodiment 1, the difference is that ionic liquid dosage is
5g。
Embodiment 7
The present embodiment prepares the method for molybdenum disulfide quantum dot with embodiment 1, the difference is that tannic acid dosage is
500mg。
Embodiment 8
The present embodiment prepares the method for molybdenum disulfide quantum dot with embodiment 1, the difference is that tannic acid dosage is
100mg。
Embodiment 9
The present embodiment prepares the method for molybdenum disulfide quantum dot with embodiment 1, the difference is that not carrying out to step (3)
It repeats.
Embodiment 10
The present embodiment prepares the method for molybdenum disulfide quantum dot with embodiment 1, the difference is that: in step (3), no
The step of repeating to be ultrasonically treated, only repeating baking oven heat treatment.
Embodiment 11
The preparation method of molybdenum disulfide quantum dot, includes the following steps:
(1) the tannic acid powder of the molybdenum disulfide powder of 500mg and 250mg are placed in mortar, 0.5g ionic liquid is added
Body simultaneously grinds 10min in mortar, obtains the first dispersion liquid；
(2) the first dispersion liquid is diluted using 50mL solvent and is transferred to closed glass container, obtain the second dispersion liquid；
(3) by the closed glass container equipped with the second dispersion liquid, it is placed in the supersonic wave cleaning machine that power is 200W
Middle processing 0.5 hour, is subsequently transferred in baking oven be heat-treated 0.5 hour at 110 DEG C；
(4) step 3 time described in (3) is repeated；
(5) gained mixture in (4) is evaporated under vacuum conditions, obtains molybdenum disulfide quantum dot.
Embodiment 12
The preparation method of molybdenum disulfide quantum dot, includes the following steps:
(1) the tannic acid powder of the molybdenum disulfide powder of 500mg and 250mg are placed in mortar, 2g ionic liquid is added
And 20min is ground in mortar, obtain the first dispersion liquid；
(2) the first dispersion liquid is diluted using 100mL solvent and is transferred to closed glass container, obtain the second dispersion liquid；
(3) by the closed glass container equipped with the second dispersion liquid, it is placed in the supersonic wave cleaning machine that power is 300W
Middle processing 2 hours, is subsequently transferred in baking oven be heat-treated 2 hours at 140 DEG C；
(4) step 3 time described in (3) is repeated；
(5) gained mixture in (4) is evaporated under vacuum conditions, obtains molybdenum disulfide quantum dot.
Comparative example 1
In this comparative example, the method for molybdenum disulfide quantum dot is prepared with embodiment 1, the difference is that in step (1) not
Use tannic acid.
Wherein, embodiment 1,11 and the specific type of 12 intermediate ion liquid, solvent see the table below 1:
Table 1
The size of the molybdenum disulfide quantum dot obtained using the preparation method of embodiment 1-12 and comparative example 1, yield are shown in
The following table 2:
Table 2
| Average-size/nm | Average thickness/nm | Yield/% | |
| Embodiment 1 | 3 | 0.8 | 88% |
| Embodiment 2 | 3 | 0.8 | 42% |
| Embodiment 3 | 3 | 0.8 | 87% |
| Embodiment 4 | 3 | 0.8 | 87% |
| Embodiment 5 | 3 | 0.8 | 15% |
| Embodiment 6 | 3 | 0.8 | 86% |
| Embodiment 7 | 3 | 0.8 | 84% |
| Embodiment 8 | 3 | 0.8 | 56% |
| Embodiment 9 | 3 | 0.8 | 21% |
| Embodiment 10 | 3 | 0.8 | 24% |
| Embodiment 11 | 3 | 0.8 | 82% |
| Embodiment 12 | 3 | 0.8 | 86% |
| Comparative example 1 | 3 | 0.8 | 4% |
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from of the invention
Many other change and modification can be made in the case where spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. a kind of preparation method of molybdenum disulfide quantum dot characterized by comprising
Molybdenum disulfide, tannic acid and ionic liquid are mixed, mixed liquor is obtained；
The mixed liquor is ultrasonically treated and is heated, the molybdenum disulfide quantum dot is obtained.
2. preparation method according to claim 1, which is characterized in that the mixed liquor is by pretreatment, the pretreatment
It include: to be ground to the mixed liquor；
Preferably, the time of the grinding is 10-30min, preferably 15-20min.
3. preparation method according to claim 1 or 2, which is characterized in that the molybdenum disulfide, tannic acid and ionic liquid
Mass ratio be 2:1:(2-8)；Preferably 2:1:5.
4. preparation method according to claim 1 or 2, which is characterized in that the ionic liquid includes 1- butyl -3- methyl
Limidazolium hexafluorophosphate；
Preferably, the partial size of the molybdenum disulfide is 2-10 microns.
5. preparation method according to claim 2, which is characterized in that after being ground to the mixed liquor, utilize
Solvent is diluted the mixed liquor, then carries out the ultrasonic treatment and heat treatment；
Preferably, the mass volume ratio of the molybdenum disulfide and solvent is (0.1-1) g:(50-100) mL, preferably 0.5g:
50mL；
Preferably, the solvent includes N-Methyl pyrrolidone and/or n,N-Dimethylformamide, preferably N- crassitude
Ketone.
6. preparation method according to claim 1-5, which is characterized in that repeat to the mixed liquor described
Ultrasonic treatment and/or the heat treatment；
Preferably, the mixed liquor is repeated alternately to be ultrasonically treated and heat；
Preferably, it repeats the alternately described ultrasonic treatment and the heat treatment is 1-3 times；
Preferably, the power of the ultrasonic treatment is 200-300W, and the time is 0.5-2 hours；
Preferably, the temperature of the heat treatment is 110-140 DEG C, and the time is 0.5-2 hours.
7. according to claim 1, preparation method described in 2,5 or 6, which is characterized in that further include to it is described ultrasonic treatment and
The withering step of the product of heat treatment, the drying carry out under vacuum conditions；
Preferably, further includes: the product after the drying is dissolved in the step of being freeze-dried after polar solvent.
8. a kind of molybdenum disulfide quantum dot, which is characterized in that prepared using the described in any item preparation methods of claim 1-7
It obtains；
Preferably, the molybdenum disulfide quantum dot is layer structure, and the size of the molybdenum disulfide quantum dot is 2-4nm；
Preferably, the molybdenum disulfide quantum dot with a thickness of 0.7-1.2nm.
9. a kind of molybdenum disulfide quantum dot according to any one of claims 8 is in production photoelectric device, sensor, catalyst or lubricant
In purposes.
10. a kind of photoelectric device, sensor, catalyst or lubricant, which is characterized in that including according to any one of claims 8 two
Molybdenum sulfide quantum dot.
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