CN106830050B - A kind of extra small silver sulfide quantum dot and preparation method thereof - Google Patents
A kind of extra small silver sulfide quantum dot and preparation method thereof Download PDFInfo
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- CN106830050B CN106830050B CN201710181199.6A CN201710181199A CN106830050B CN 106830050 B CN106830050 B CN 106830050B CN 201710181199 A CN201710181199 A CN 201710181199A CN 106830050 B CN106830050 B CN 106830050B
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Abstract
The invention discloses a kind of extra small silver sulfide quantum dot, the average-size of the silver sulfide quantum dot is less than 2nm.Nano silver grain is dissolved in nonpolar solvent by the present invention, and mercaptan is added and is placed on illumination reaction under ultraviolet light, removes solvent after reaction, then centrifuge washing is dried to obtain silver sulfide quantum dot.Method of the invention is obtained with extra small silver sulfide quantum dot at room temperature, and method is simple, and reproducibility is high, can be used for the extra small silver sulfide quantum dot of large scale preparation.
Description
Technical field
The present invention relates to technology of quantum dots fields.More particularly, to a kind of extra small silver sulfide quantum dot and its preparation side
Method.
Background technique
Quantum dot (size is in 100nm particle below), because of its quantum size confinement effect, with its body phase material phase
Than having unique physicochemical properties, gathering around and have broad application prospects in terms of catalysis, luminous and photoelectric device.Currently, amount
The synthesis of son point mainly uses high temperature oil phase or hydro-thermal reaction to prepare, and reaction temperature is high, substantially increases the complexity of synthesis
And cost.
Gradually go deep into as people are knowable to nanometer sized materials unique physico-chemical, field of nanometer material technology development
Rapidly, wherein being again most with nano semiconductor material.Sulfide semiconductor material nanoscale embody structure abundant with
The adjustability of property, therefore the extensive concern by researcher.Silver sulfide is as a kind of stable structure that nature is widely present
Semiconductor material, quantum dot have can modulation it is near-infrared luminous, to have wide application prospect in bio-imaging.
In recent years, the controllable quantum dot of dimensional structure how is prepared to become the focus of people's research.It is often adopted in conventional method
High temperature oil phase or hydrothermal method, the formation of quantum dot follow nucleating growth mechanism.Under this mechanism, need to reaction
Order is added in temperature, reactant concentration, reactant, reactant is added a large amount of experiment condition such as speed and carries out accuracy controlling,
It is possible to ensure that the controllability and repeatability of experimental result.Such method has the experimental level of operator high
It is required that being unfavorable for extension and the procedure of production.In addition, the extremely difficult acquisition size 2nm quantum dot below of conventional method, because
In nucleating growth mechanism, the nucleation of explosion type is difficult to carry out accuracy controlling, this is the defect of this method inherently.
Therefore, the present invention provides a kind of extra small silver sulfide quantum dot, the method for converting Nano silver grain by ultraviolet light, will
The size Control of the silver sulfide quantum dot of synthesis is in 2nm or less.
Summary of the invention
It is an object of the present invention to provide a kind of extra small silver sulfide quantum dots.Silver sulfide quantum dot ruler in the present invention
It is very little to be less than 2nm, there is apparent quantum size effect.
It is another object of the present invention to provide a kind of preparation methods of extra small silver sulfide quantum dot.The present invention passes through purple
Outer illumination converts oil-soluble Nano silver grain, has synthesized extra small silver sulfide quantum in nonpolar solvent under mercaptan existence condition
Point.
It is another object of the present invention to provide a kind of preparation methods of extra small silver sulfide quantum dot.
In order to achieve the above first purpose, the present invention adopts the following technical solutions:
A kind of extra small silver sulfide quantum dot, the silver sulfide quantum dot average-size are less than 2nm.Quantum dot of the invention
Small, luminous efficiency is high, and surface exposure active site is more.
To reach above-mentioned second purpose, the present invention is adopted the following technical solutions:
A kind of preparation method of extra small silver sulfide quantum dot, includes the following steps:
1) Nano silver grain is dissolved in nonpolar solvent and obtains solution A；
2) mercaptan is added into solution A and obtains solution B；
3) solution B is placed in illumination reaction under ultraviolet light；
4) ultraviolet lighting removes solvent after reaction, then centrifuge washing is dried to obtain silver sulfide quantum dot.
Preferably, Nano silver grain described in step 1) is oil-soluble Nano silver grain.It is a discovery of the invention that oil-soluble silver is received
Rice corpuscles favorable solubility in nonpolar solvent, so that guarantee reactant concentration can modulation.
Preferably, nonpolar solvent described in step 1) is selected from one of toluene, hexamethylene, n-hexane.The present invention adopts
Nonpolar solvent all has good dispersibility to various reactants, and keeps stablizing in illumination reaction.
Preferably, the concentration of solution A described in step 1) is 8 μm of ol/ml or less.It is a discovery of the invention that the concentration of solution A≤
When 8 μm of ol/ml, abundant illumination is can be obtained in entire reaction system, to guarantee that there is no differences inside same reaction system.
It is highly preferred that the concentration of solution A described in step 1) is 4~8 μm of ol/ml.It is a discovery of the invention that in the concentration model
In enclosing, batch reaction yield and product quality are more satisfactory.
Preferably, mercaptan described in step 2) is 2- ethyl thiophenol, in 4- isopropylbenzene thiophenol, 4- tert .- butylthiophenol
One kind.The feature of heretofore described mercaptan be its compound for being formed with monovalence silver as the intermediate reacted both topographically
With 1-dimention nano cable architecture, this structure ensures the generation of subsequent extra small silver sulfide quantum dot.
Preferably, the molar ratio of mercaptan described in step 2) and silver is 20:1 or more.It is a discovery of the invention that molar ratio >=20:1
When guarantee reaction sufficiently carry out, obtain final product silver sulfide quantum dot.
It is highly preferred that the molar ratio of mercaptan described in step 2) and silver is 20~70:1.It is a discovery of the invention that at described mole
Than in range, guaranteeing to save mercaptan usage amount while reaction sufficiently obtain target product.
Preferably, ultraviolet source described in step 3) is arbitrarily to have the light source of transmitting in wavelength 300-400nm range.This hair
Ultraviolet light within the scope of bright discovery wavelength 300-400nm being capable of induced chemical reaction progress.
Preferably, illumination reaction described in step 3) carries out under stiring, present invention discover that the lower reaction of stirring can make instead
It should quickly be sufficiently carried out.
Preferably, the time of illumination reaction described in step 3) is adjusted according to different light sources.Such as according to the present invention
Preferred embodiment, the ultraviolet source described in the step 3) is when including the 500W mercury lamp light source of 365nm bandpass filter, instead
Between seasonable for 12~for 24 hours, present invention discover that the reaction time, which is less than the range, then cannot get silver sulfide quantum under the light source
Point becomes larger greater than the range silver sulfide quantum dot average-size.
Preferably, the reagent that use is washed described in step 4) includes but is not limited to methanol.The reagent pair that the present invention uses
Reaction product is insoluble, and eliminates the organic by-products generated in reaction and extra mercaptan.
Preferably, solvent removing method described in step 4) is rotary evaporation mode.It is a discovery of the invention that rotary evaporation mode
Sufficiently eliminate low-boiling organic reaction solvent.
Preferably, drying temperature described in step 4) is 40-60 DEG C, and drying time is greater than 4h.The present invention is using described dry
Dry temperature and time sufficiently removes low boiling point organic solvent therein under the premise of product does not change.
The present invention is based on basic principle be that thiol molecule corrodes Nano silver grain under ultraviolet light and generates one-dimensional knot
The mercaptan of structure and argintous compound, the hydrogen sulfide effect which further generates with mercaptan under light illumination generate extra small
Silver sulfide quantum dot, therefore the selection of suitable light source and Suitable base is extremely important, while the proportion of raw material in the present invention,
The control of the technological parameters such as reaction time is all the technological difficulties for needing to solve.
The present invention is existed the size Control of the silver sulfide quantum dot of synthesis by the method that ultraviolet light converts Nano silver grain
2nm or less.This method is obtained with extra small silver sulfide quantum dot at room temperature, and method is simple, and reproducibility is high, can be used for advising greatly
Mould prepares extra small silver sulfide quantum dot.
In addition, unless otherwise specified, any range documented by the present invention includes any number between end value and end value
Any subrange that any number between value and end value or end value is constituted.
Beneficial effects of the present invention are as follows:
(1) present invention converts Nano silver grain under ultraviolet light and is prepared for size less than 2nm by light reaction method
Silver sulfide quantum dot.
(2) present invention is obtained with extra small silver sulfide quantum dot at room temperature, and method is simple, and reproducibility is high, can be used for
The extra small silver sulfide quantum dot of large scale preparation, and provided for the exploration of the performance of super-small silver sulfide quantum dot and application study
It may.
Detailed description of the invention
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing.
Fig. 1 shows the high-resolution-ration transmission electric-lens figure of the silver sulfide quantum dot in the embodiment of the present invention 1.
Fig. 2 shows the selection electron diffraction diagrams of the silver sulfide quantum dot in the embodiment of the present invention 1.
Fig. 3 shows the transmission electron microscope picture of the silver sulfide quantum dot in the embodiment of the present invention 1.
Fig. 4 shows the dimension analysis figure of the silver sulfide quantum dot in the embodiment of the present invention 1.
Specific embodiment
In order to illustrate more clearly of the present invention, the present invention is done further below with reference to preferred embodiments and drawings
It is bright.Similar component is indicated in attached drawing with identical appended drawing reference.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
In the description of the present invention, unless otherwise indicated, the meaning of " plurality " is two or more；Term " on ",
The orientation or positional relationship of the instructions such as "lower", "left", "right", "inner", "outside", " front end ", " rear end ", " head ", " tail portion " is
It is based on the orientation or positional relationship shown in the drawings, is merely for convenience of description of the present invention and simplification of the description, rather than instruction or dark
Show that signified device or element must have a particular orientation, be constructed and operated in a specific orientation, therefore should not be understood as pair
Limitation of the invention.
Embodiment 1
A kind of extra small silver sulfide quantum dot, preparation step are as follows:
1) oil-soluble Nano silver grain is dissolved in the solution A that toluene is configured to 5 μm of ol/ml；
2) it takes 6ml solution A to be put into the quartz ampoule of 15ml capacity, adds 100 μ l 4- tert .- butylthiophenols, obtain molten
Liquid B；
3) 500W mercury lamp light source is used to solution B, and it is anti-to reaction system progress illumination to install 365nm bandpass filter additional
It answers, reaction carries out under constant stirring, reaction time 18h；
4) solvent is removed using rotary evaporation mode after illumination reaction, after residue uses methanol centrifuge washing 4 times
Dry, drying temperature is 60 DEG C, and drying time 4h can obtain final product.
Characterize to material: Fig. 1 is the high-resolution-ration transmission electric-lens figure of silver sulfide quantum dot made from the above method.By scheming
1 it is found that gained silver sulfide quantum dot crystallinity is good, it can be observed that significantly belonging to the crystalline substance of (- 103) and (103) crystal face
Interplanar distance.Fig. 2 is the selection electron diffraction diagram of silver sulfide quantum dot made from the above method, show it is apparent correspond to (-
103) diffraction ring of crystal face.Fig. 3 is the electron microscope of gained silver sulfide quantum dot, is figure to the analysis of quantum dot size according to the figure
4, show that the average-size of gained silver sulfide quantum dot is less than the extra small silver sulfide quantum dot of 2nm.
Embodiment 2~4
A kind of extra small silver sulfide quantum dot, preparation step the difference is that only with embodiment 1:
The concentration of solution A is respectively 2 μm of ol/ml, 4 μm of ol/ml, 8 μm of ol/ml in step 1).
The average-size of obtained silver sulfide quantum dot such as table 1:
The size for the silver sulfide quantum dot being prepared under 1 different solutions A concentration of table
| Embodiment 2 | Embodiment 3 | Embodiment 1 | Embodiment 4 | Comparative example 1 | |
| Concentration (μm ol/ml) | 2 | 4 | 5 | 8 | 10 |
| Average-size (nm) | 1.6 | 1.7 | 1.7 | 1.7 | 2.8 |
As known from Table 1, when the concentration range≤8 μm ol/ml of solution A, the silver sulfide quantum dot average-size that is prepared
Less than 2nm, there is the particle of larger size to generate beyond the range, average-size is made to become larger.
Comparative example 1
A kind of extra small silver sulfide quantum dot, preparation step the difference is that only with embodiment 1:
The concentration of solution A is 10 μm of ol/ml in step 1).
The average-size of obtained silver sulfide quantum dot is listed in table 1.
Embodiment 5~7
A kind of extra small silver sulfide quantum dot, preparation step the difference is that only with embodiment 1:
The molar ratio of mercaptan and silver is 30:1,40:1,50:1 in step 2).
The average-size of obtained silver sulfide quantum dot such as table 2:
The size for the silver sulfide quantum dot being prepared under the molar ratio of the different mercaptan of table 2 and silver
| Comparative example 2 | Embodiment 1 | Embodiment 5 | Embodiment 6 | Embodiment 7 | |
| Molar ratio | 10:1 | 20:1 | 30:1 | 40:1 | 50:1 |
| Average-size (nm) | - | 1.7 | 1.7 | 1.7 | 1.7 |
As known from Table 1, when molar ratio range >=20:1 of mercaptan and silver, the silver sulfide quantum dot average-size that is prepared
Less than 2nm, can not be carried out completely beyond range reaction, product is not silver sulfide quantum dot.
Comparative example 2
A kind of extra small silver sulfide quantum dot, preparation step the difference is that only with embodiment 1:
The molar ratio of mercaptan and silver is 10:1 in step 2)
The average-size of obtained product is listed in table 1.
Embodiment 8~10
A kind of extra small silver sulfide quantum dot, preparation step the difference is that only with embodiment 1:
The reaction time is 12h, 16h, 22h in step 3).
The average-size of obtained silver sulfide quantum dot such as table 2:
The size for the silver sulfide quantum dot that table is prepared under 2 differential responses time
| Comparative example 3 | Embodiment 1 | Embodiment 8 | Embodiment 9 | Embodiment 10 | Comparative example 4 | |
| Reaction time (h) | 8 | 18 | 12 | 16 | 22 | 30 |
| Average-size (nm) | - | 1.7 | 1.7 | 1.7 | 1.7 | 4.8 |
As known from Table 1, in 12-24h, the silver sulfide quantum dot average-size being prepared is less than reaction time range
2nm then reacts less than the range and is unable to fully carry out, cannot get silver sulfide quantum dot, is greater than the range silver sulfide quantum dot and sends out
Raw a degree of aggregation, average-size become larger.
Comparative example 3~4
A kind of extra small silver sulfide quantum dot, preparation step the difference is that only with embodiment 1:
The reaction time is 8h, 30h in step 3)
The average-size of obtained silver sulfide quantum dot is listed in table 1.
Embodiment 11~12
A kind of extra small silver sulfide quantum dot, preparation step the difference is that only with embodiment 1:
The nonpolar solvent used in step 1) is respectively hexamethylene, n-hexane.
Finally obtained silver sulfide quantum dot size is similar with embodiment 1.
Embodiment 13~14
A kind of extra small silver sulfide quantum dot, preparation step the difference is that only with embodiment 1:
The mercaptan used in step 2) is respectively 2- ethyl thiophenol, 4- isopropylbenzene thiophenol.
Finally obtained silver sulfide quantum dot size is similar with embodiment 1.
Embodiment 15
A kind of extra small silver sulfide quantum dot, preparation step the difference is that only with embodiment 1:
Light source described in step 3) is the 300W mercury lamp light source for including 365nm bandpass filter, reaction time 48h.
Finally obtained silver sulfide quantum dot size is similar with embodiment 1.
Embodiment 16
A kind of extra small silver sulfide quantum dot, preparation step the difference is that only with embodiment 1:
Light source described in step 3) is 500W mercury lamp light source, reaction time 7h.
Finally obtained silver sulfide quantum dot size is similar with embodiment 1.
The present invention is experimentally confirmed, and ultraviolet source is to obtain arbitrarily when wavelength 300-400nm range has the light source of transmitting
The silver sulfide quantum dot average-size arrived is less than 2nm.
Comparative example 5
A kind of extra small silver sulfide quantum dot, preparation step the difference is that only with embodiment 1:
Nano silver grain described in step 1) is water-soluble silver nanoparticle
Final Nano silver grain is unable to fully be distributed in solvent, and reaction can not carry out.
Comparative example 6
A kind of extra small silver sulfide quantum dot, preparation step the difference is that only with embodiment 1:
Light source described in step 3) is the 500W mercury lamp light source for including 240nm bandpass filter.
System can not occur without significant change, reaction in the final 72h illumination reaction time.
Comparative example 7
A kind of extra small silver sulfide quantum dot, preparation step the difference is that only with embodiment 1:
Light source described in step 3) be include 500W mercury lamp light source that 400nm above band filters out optical filter.
System can not occur without significant change, reaction in the final 72h illumination reaction time.
Conclusion: the present invention passes through matching between the suitable ultraviolet source of selection, oil-soluble Nano silver grain, each raw material of adjustment
Than and control the reaction time, mutually coordinated, mating reaction, realize average-size less than 2nm silver sulfide quantum dot room temperature
Synthesis, product have good dimensional homogeneity, have achieved the effect that conventional method can not obtain.In product of the invention in life
Object imaging etc. all has the effect of excellent.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention may be used also on the basis of the above description for those of ordinary skill in the art
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is all to belong to this hair
The obvious changes or variations that bright technical solution is extended out are still in the scope of protection of the present invention.
Claims (3)
1. a kind of preparation method of extra small silver sulfide quantum dot, which is characterized in that the average-size of the silver sulfide quantum dot is small
In 2 nm；The preparation method of the extra small silver sulfide quantum dot includes the following steps:
1) oil-soluble Nano silver grain is dissolved in nonpolar solvent and obtains solution A；
2) 2- ethyl thiophenol or 4- isopropylbenzene thiophenol is added into solution A or 4- tert .- butylthiophenol obtains solution B；
3) solution B is placed in illumination reaction under ultraviolet light；
4) ultraviolet lighting removes solvent after reaction, then centrifuge washing is dried to obtain silver sulfide quantum dot；
Ultraviolet source is 500 W mercury lamp light sources of 365 nm bandpass filters in step 3), and the reaction time is 12 ~ 24 h；
The concentration of solution A described in step 1) is 8 μm of ol/ml hereinafter, the nonpolar solvent is in hexamethylene, n-hexane
One kind；
2- ethyl thiophenol described in step 2,4- isopropylbenzene thiophenol or 4- tert .- butylthiophenol and silver-colored molar ratio are all
20:1 or more.
2. a kind of preparation method of extra small silver sulfide quantum dot according to claim 1, which is characterized in that institute in step 3)
Illumination reaction is stated to carry out under stiring.
3. a kind of preparation method of extra small silver sulfide quantum dot according to claim 1, which is characterized in that institute in step 4)
Stating the reagent that washing uses includes methanol；Solvent removing method is rotary evaporation mode；Drying temperature is 40-60 DEG C, when dry
Between be greater than 4 h.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103991895A (en) * | 2014-05-23 | 2014-08-20 | 南京师范大学 | Preparation method of aptamer-induced Ag2S quantum dots |
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| CN103991895A (en) * | 2014-05-23 | 2014-08-20 | 南京师范大学 | Preparation method of aptamer-induced Ag2S quantum dots |
Non-Patent Citations (1)
| Title |
|---|
| "Thiolate-Mediated Photoinduced Synthesis of Ultrafine Ag2S Quantum Dots from Silver Nanoparticles";Yitao Cao et al.;《Angew. Chem. Int. Ed.》;20161027;第55卷;第14952 –14957页 * |
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