CN111849484B - SnSe 2 Preparation method of quantum dot and SnSe 2 Quantum dots - Google Patents
SnSe 2 Preparation method of quantum dot and SnSe 2 Quantum dots Download PDFInfo
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Abstract
The application discloses a SnSe 2 Preparation method of quantum dot and SnSe 2 Quantum dot of the SnSe 2 The preparation method of the quantum dot comprises the following steps: snSe 2 Crushing the powder to obtain SnSe 2 Microparticles; adding SnSe into polyethylene glycol 2 Micron particles to form an initial mixed solution with a preset concentration; carrying out ultrasonic pretreatment on the initial mixed solution to obtain a pretreated mixed solution; carrying out ultrasonic crushing on the pretreated mixed solution to obtain an ultrasonic mixed solution; centrifuging the ultrasonic mixed solution, and collecting the centrifuged supernatant to obtain SnSe dispersed in polyethylene glycol 2 And (4) quantum dots. The preparation method is simple and easy to operate. SnSe prepared by the preparation method 2 The quantum dots have fluorescent properties.
Description
Technical Field
The application relates to the technical field of quantum dots, in particular to SnSe 2 Preparation method of quantum dot and SnSe 2 And (4) quantum dots.
Background
Quantum Dots (QDs) are a kind of semiconductor nanomaterial with a special structure in which carriers are restricted in three dimensions, and different from a two-dimensional semiconductor nanomaterial with only one dimension in a nanometer scale, when the dimensions of the semiconductor nanomaterial in the three dimensions are smaller than the bohr exciton radius, the movement of electrons and holes in the three-dimensional space is restricted by the Quantum confinement effect, and a continuous energy band structure becomes a discrete energy level structure with molecular characteristics. At present, quantum dots have wide application prospects in the fields of solar cells, luminescent devices, biomedicine and the like.
The two-dimensional material has abundant electrical properties, and the electrical conductivity of the two-dimensional material comprises insulators, semiconductors, semimetals and metals. Has wide application in the fields of electronics, energy, catalysis and the like. As shown in FIG. 1, two-dimensional (2D) Transition Metal Dichalcogenides (TMDs) refer to compounds of X-M-X type "sandwich" structure formed by Transition Metal elements (M) and chalcogen nonmetal elements (X), such as MoS 2 ，MoSe 2 ，MoTe 2 ，WS 2 ，WSe 2 ，WTe 2 ，TiS 2 ，TaS 2 VS, etc. Similar to graphene, 2D TMDs have a two-dimensional layered structure in which metal atoms within a layer are covalently bonded to chalcogen non-metal atoms, while weak van der waals forces exist between layers. There has been still less research associated with quasi-zero-dimensional nanostructured two-dimensional transition metal chalcogenide quantum dot (2D-TMD QDs) materials with geometric dimensions that are within the quantum confinement effect range in three dimensions. TMDs have a unique electronic structure, so that the TMDs have potential application values in the fields of electronic devices, photonic devices, catalysis, energy sources, environment and the like; meanwhile, TMDs materials have good biocompatibility, so 2D-TMD QDs are expected to become a new generation of low-toxicity quantum dots and are widely applied to the fields of fluorescence labeling, medical diagnosis, biological imaging, biosensing and the like.
SnSe 2 Has the same as MoS 2 A similar structure, in which a Sn layer is sandwiched between two Se layers to form a stable "tri-layer" structure. SnSe 2 Belongs to the IVA-VIA family, and has rich earth resources, environmental protection and low cost. However, at present SnSe 2 The preparation method of the quantum dots is relatively complicated and complex.
Disclosure of Invention
The application provides a SnSe 2 Preparation method of quantum dot and SnSe 2 Quantum dot, and aims at providing one simple and easy-to-operate preparation process of preparing SnSe with fluorescent characteristic 2 And (4) quantum dots.
In one aspect, the present application provides a SnSe 2 A method of making a quantum dot, comprising:
SnSe 2 Powder is subjected toCrushing to obtain SnSe 2 Microparticles;
adding the SnSe into polyethylene glycol 2 Micron particles to form an initial mixed solution with a preset concentration;
carrying out ultrasonic pretreatment on the initial mixed solution to obtain a pretreated mixed solution;
carrying out ultrasonic crushing on the pretreated mixed solution to obtain an ultrasonic mixed solution;
centrifuging the ultrasonic mixed solution, and collecting the centrifuged supernatant to obtain SnSe dispersed in the polyethylene glycol 2 And (4) quantum dots.
In the preparation method of the present application, the SnSe is 2 The powder is crushed, comprising: snSe by mortar pair 2 Grinding the powder to obtain SnSe 2 The powder is crushed.
In the preparation method of the present application, the polyethylene glycol includes PEG 200 、PEG 400 And PEG 600 At least one of (1).
In the preparation method of the present application, the predetermined concentration is 0.6mg/ml to 1.3mg/ml.
In the preparation method of the present application, the performing ultrasonic pretreatment on the initial mixed solution includes: and carrying out ultrasonic pretreatment on the initial mixed solution for a preset time by using a water bath ultrasonic instrument.
In the preparation method of the present application, the ultrasonication of the pretreated mixed solution includes: and under the preset ultrasonic condition, carrying out ultrasonic crushing on the pretreated mixed liquid by adopting an ultrasonic cell crusher.
In the preparation method of the present application, the preset ultrasonic conditions include: the crushing power of the ultrasonic cell crusher is 450W-550W; and/or the working cycle of the probe of the ultrasonic cell crusher is 2S-6S and 4S-8S, and the total crushing time is 8h-12h; and/or the distance that the probe of the ultrasonic cell crusher extends into the liquid level of the pretreatment mixed liquid is 1.2cm-1.8cm; and/or, sonication with an ice bath.
In the production method of the present application, the conditions of the centrifugation treatment include: the centrifugal speed is 8500-9500 r/min, and the centrifugal time is 25-35 min.
In the preparation method of the present application, the preparation method further comprises: to the SnSe 2 And carrying out heat treatment on the quantum dots.
On the other hand, the application also provides SnSe 2 Quantum dot of said SnSe 2 The quantum dot is prepared by the preparation method.
The embodiment of the application provides SnSe 2 A preparation method of quantum dots by reacting SnSe 2 Crushing the powder to obtain SnSe 2 Microparticles; adding the SnSe into polyethylene glycol 2 Micron particles to form an initial mixed solution with a preset concentration; carrying out ultrasonic pretreatment on the initial mixed liquor to obtain a pretreated mixed liquor; carrying out ultrasonic crushing on the pretreated mixed solution to obtain an ultrasonic mixed solution; centrifuging the ultrasonic mixed solution, and collecting the centrifuged supernatant to obtain SnSe dispersed in the polyethylene glycol 2 And (4) quantum dots. The preparation method is simple and easy to operate. SnSe prepared by the preparation method 2 The quantum dots have fluorescent properties.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a schematic representation of the crystal structure of a two-dimensional transition metal chalcogenide;
fig. 2 is SnSe provided in an embodiment of the present application 2 A schematic flow diagram of a method of preparing quantum dots;
FIG. 3 (a) is an exemplary SnSe substrate 2 TEM pictures of quantum dots;
FIG. 3 (b) is an exemplary embodiment of the present disclosure showing an exemplary SnSe 2 The particle diameter of the quantum dots is largeA small statistical distribution map;
FIG. 3 (c) is an exemplary embodiment of the present disclosure showing an exemplary SnSe 2 High power TEM pictures of quantum dots;
FIG. 3 (d) is an exemplary embodiment of the present disclosure showing an exemplary SnSe 2 A quantum dot selective area diffraction (SAED) pattern;
FIG. 4 (a) is an exemplary SnSe substrate 2 AFM pictures of quantum dots;
FIG. 4 (b) is an exemplary embodiment of the present disclosure showing an exemplary SnSe 2 A highly schematic view of quantum dots;
fig. 5 is SnSe provided in an embodiment of the present application 2 Ultraviolet-visible absorption spectra of quantum dots;
fig. 6 is SnSe provided in an embodiment of the present application 2 Fluorescence spectra of the quantum dots under different heating times, wherein the heating temperature is 160 ℃;
fig. 7 is SnSe provided in an embodiment of the present application 2 A schematic flow diagram of a method of preparing quantum dots;
fig. 8 is SnSe provided in an embodiment of the present application 2 A schematic diagram of a preparation method of the quantum dots;
FIG. 9 is an exemplary embodiment of SnSe provided herein 2 Fluorescence spectra of the quantum dots at different heating temperatures, wherein the heating time is 10h;
FIG. 10 is an exemplary embodiment of SnSe provided herein 2 Fluorescence spectra of the quantum dots under different excitation wavelengths, wherein the heating time is 10h, and the heating temperature is 160 ℃;
FIG. 11 is an exemplary embodiment of SnSe provided herein 2 Schematic diagram of quantum dot fluorescence enhancement.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some, but not all, of the embodiments of the present application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It is also to be understood that the terminology used in the description of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in the specification of the present application and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
It should be further understood that the term "and/or" as used in this specification and the appended claims refers to any and all possible combinations of one or more of the associated listed items and includes such combinations.
The application provides a SnSe 2 Preparation method of quantum dot and SnSe 2 The preparation method of the quantum dot is simple and easy to operate.
Referring to fig. 2, fig. 2 is a schematic diagram of SnSe according to an embodiment of the present application 2 Schematic flow diagram of a method for preparing quantum dots. As shown in FIG. 2, the SnSe 2 The method for preparing the quantum dot includes steps S101 to S105.
S101, snSe 2 Crushing the powder to obtain SnSe 2 Micron particles.
S102, adding the SnSe into polyethylene glycol 2 Micron particles to form an initial mixed liquid with a preset concentration.
S103, carrying out ultrasonic pretreatment on the initial mixed liquor to obtain a pretreated mixed liquor.
And S104, carrying out ultrasonic crushing on the pretreated mixed solution to obtain an ultrasonic mixed solution.
S105, centrifuging the ultrasonic mixed solution, and collecting the centrifuged supernatant to obtain SnSe dispersed in the polyethylene glycol 2 And (4) quantum dots.
In some embodiments, the SnSe is 2 The powder is crushed, including: snSe by mortar pair 2 Grinding the powder to obtain SnSe 2 The powder is crushed.
Illustratively, 50mg of SnSe is taken 2 High purity powder, grinding with mortarSo that SnSe 2 The high purity powder can be broken down into micron sized particles.
In some embodiments, the sample after grinding is SnSe 2 The microparticles were added to 50ml of polyethylene glycol to obtain an initial mixture of 1 mg/ml. Understandably, the above-mentioned SnSe 2 The dosage of the high-purity powder and the polyethylene glycol can be selected according to actual requirements, so that initial mixed liquid with preset concentration is obtained. Illustratively, the predetermined concentration is 0.6mg/ml to 1.3mg/ml, i.e., the predetermined concentration may be any one of 0.6mg/ml, 1.3mg/ml, and 0.6mg/ml to 1.3mg/ml.
It will be appreciated that any suitable molecular weight polyethylene glycol may be used. Illustratively, the polyethylene glycol comprises PEG 200 、PEG 400 And PEG 600 At least one of (1). In some embodiments, the polyethylene glycol is PEG 400 。
In some embodiments, the subjecting the initial mixture to ultrasonic pretreatment comprises: and carrying out ultrasonic pretreatment on the initial mixed solution for a preset time by using a water bath ultrasonic instrument. The preset time can be set according to actual requirements, for example, 20h-28 h. Illustratively, the initial mixture is pre-sonicated in a water bath sonicator for 24h. It can be understood that the initial mixed liquid is subjected to ultrasonic pretreatment by using a water bath ultrasonic instrument, and the ultrasonic pretreatment is performed by using a water bath so as to absorb at least part of heat generated in the ultrasonic process, so that the temperature of the pretreated liquid is constant, and the crushing efficiency is improved.
In some embodiments, the sonicating the pre-treated mixed liquor comprises: and under the preset ultrasonic condition, carrying out ultrasonic crushing on the pretreated mixed liquid by adopting an ultrasonic cell crusher.
Wherein, the preset ultrasonic condition can be designed according to actual requirements. Illustratively, the preset ultrasound conditions include: the crushing power of the ultrasonic cell crusher is 450W-550W; and/or the working cycle of the probe of the ultrasonic cell crusher is 2S-6S and 4S-8S; and/or the distance that the probe of the ultrasonic cell crusher extends into the liquid level of the pretreatment mixed liquid is 1.2cm-1.8cm; and/or, sonication with an ice bath.
In some embodiments, the pretreatment mixture is placed in an ultrasonic cell disruptor for further disruption. The distance that the probe of ultrasonic cell crusher stretches into the liquid level of preliminary treatment mixed liquid is 1.5cm, the crushing power of ultrasonic cell crusher is 500W, the duty cycle of the probe of ultrasonic cell crusher is 4 seconds of work, stops for 6 seconds, and the total time of breakage is 10h. An ice bath is adopted in the whole ultrasonic process to absorb heat generated in the ultrasonic process and keep the temperature of the ultrasonic liquid constant. Specifically, ultrasonication employs an ice bath such that the temperature of the sonicated liquid is less than or equal to 30 ℃.
In some embodiments, the centrifuging the ultrasonic mixture specifically includes: and (3) centrifuging the ultrasonic mixed solution at the rotating speed of 8500-9500 r/min for 25-35 min.
Illustratively, the ultrasound mixture is placed in a centrifuge tube and then centrifuged. Wherein, the centrifugal speed is 9000 r/min, and the centrifugal time is 30 min. Collecting the supernatant after centrifugation in a centrifuge tube to obtain SnSe dispersed in the polyethylene glycol 2 And (4) quantum dots.
The organic solvent used to prepare the two-dimensional (2D) Transition Metal chalcogenides (TMDs) is typically N-methylpyrrolidone (NMP), whereas SnSe prepared from N-methylpyrrolidone 2 Quantum dots do not have significant fluorescence phenomena and cannot be further surface functionalized. Due to PEG 400 Is a non-ionic surfactant. In the preparation process, PEG 400 The molecule being capable of adsorbing to SnSe 2 On the surface of the quantum dots, so that they can be directly dispersed, and also prevent them from aggregating. In addition, PEG 400 Is a polymer with good biocompatibility and can be used for SnSe 2 Surface functionalization of quantum dots.
Thus, in some embodiments, polyethylene glycol is PEG 400 The above preparation is adopted as the organic solventMethod for preparing SnSe 2 Quantum dot and the prepared SnSe 2 The quantum dots are characterized, and the adopted characterization means comprise Transmission Electron Microscope (TEM), atomic Force Microscope (AFM), ultraviolet visible absorption spectrum and fluorescence spectrum.
Referring to FIGS. 3 (a) and 3 (b), snSe prepared by the examples of the present application 2 The quantum dots have uniform particle size and SnSe 2 The particle size of the quantum dots is less than 10nm, the average size is about 7nm, and the quantum dots have good dispersibility. Referring to FIG. 3 (c), snSe prepared by the examples of the present application 2 Lattice spacing of quantum dots is 0.201nm, and SnSe 2 The (003) crystal planes of (c) are completely coincident. Diffraction Pattern surface in FIG. 3 (d), snSe prepared in examples of the present application 2 Quantum dots are polycrystalline in nature.
To study SnSe 2 Thickness of quantum dots, snSe according to an embodiment of the present application 2 The quantum dots were subjected to AFM characterization. Referring to FIGS. 4 (a) and 4 (b), snSe along the black line in FIG. 4 (a) 2 The quantum dot height has been shown in FIG. 4 (b), and it can be seen that SnSe is shown 2 The height of the quantum dots was about 7nm, consistent with TEM characterization data. Thus, the preparation method provided by the embodiment successfully prepares SnSe 2 And (4) quantum dots.
The ultraviolet-visible absorption spectrometry is a commonly used spectrometry for analysis based on an absorption spectrum generated by electronic transition in a sample to be detected under the irradiation of light. The absorption of molecules in the uv-vis is closely related to their electronic structure. Different electronic transitions correspond to different energies (wavelengths), and are reflected in an ultraviolet-visible absorption spectrum diagram, and an absorption peak with certain intensity is arranged at a certain position. The structural information of the material can be judged by the position of the absorption peak, the purity of the material is checked, the concentration of the suspension is compared, the size of the nano-sheet in the suspension is estimated, the stability of the suspension is detected, and the like, namely the SnSe is checked 2 One of the important means for the success of quantum dot preparation. Referring to FIG. 5, it can be seen that SnSe 2 The quantum dots have a distinct absorption band at 300 nm. In addition, snSe 2 Variation of quantum dot absorption rangeNarrow, showing weak or even no absorption after 400nm, which is a sign of the formation of small particles, a phenomenon in SnS 2 Quantum dots and MoS 2 Quantum dots have also been observed to be primarily caused by quantum confinement effects and edge defects.
MoS 2 The quantum dots have the property of photoluminescence, so the embodiment of the application tests SnSe 2 Whether fluorescence is present in the quantum dots. In some embodiments, excitation is performed using ultraviolet light, visible light, and a weak fluorescence signal is detected in the visible light, as shown in particular in fig. 6. Specifically, as can be seen from FIG. 6, when SnSe 2 When the quantum dots are in normal temperature environment, i.e. SnSe 2 When the quantum dots are heated for 0h, a weak fluorescence signal can be detected under the visible light. The reason for this phenomenon may be due to the SnSe produced 2 The quantum dots have a few-layer structure, and are not single-layer structures, so the band gap is also an indirect band gap, not a direct band gap.
SnSe of the above embodiment 2 A preparation method of quantum dots by reacting SnSe 2 Crushing the powder to obtain SnSe 2 Microparticles; adding the SnSe into polyethylene glycol 2 Micron particles to form an initial mixed solution with a preset concentration; carrying out ultrasonic pretreatment on the initial mixed solution to obtain a pretreated mixed solution; carrying out ultrasonic crushing on the pretreated mixed solution to obtain an ultrasonic mixed solution; centrifuging the ultrasonic mixed solution, and collecting the centrifuged supernatant to obtain SnSe dispersed in the polyethylene glycol 2 And (4) quantum dots. The preparation method is simple and easy to operate. SnSe prepared by the preparation method 2 The quantum dots have fluorescent properties.
Referring to fig. 7, fig. 7 is a schematic diagram of SnSe according to an embodiment of the present disclosure 2 Schematic flow diagram of a method for preparing quantum dots. As shown in fig. 7 and 8, the SnSe 2 The preparation method of the quantum dot includes steps S201 to S206.
S201, snSe 2 Crushing the powder to obtain SnSe 2 Micron particles.
S202, adding the SnSe into polyethylene glycol 2 Micron particles to form a predetermined concentration of the initial mixture.
S203, carrying out ultrasonic pretreatment on the initial mixed liquor to obtain a pretreated mixed liquor.
And S204, carrying out ultrasonic crushing on the pretreated mixed solution to obtain an ultrasonic mixed solution.
S205, centrifuging the ultrasonic mixed solution, and collecting the centrifuged supernatant to obtain SnSe dispersed in the polyethylene glycol 2 And (4) quantum dots.
S206, aiming at the SnSe 2 And carrying out heat treatment on the quantum dots.
Steps S201-S205 can refer to steps S101-S105, which are not described herein.
To increase SnSe 2 Fluorescent characteristics of quantum dots, an embodiment of the present application is directed to the SnSe prepared in step S205 2 The quantum dots are heat treated to increase SnSe 2 The fluorescence intensity of the quantum dots is further expanded, and the SnSe is further expanded 2 The quantum dots are applied to the fields of optical devices, lighting devices and the like, and the method is simple and easy to operate. Specifically, the SnSe prepared in step S205 2 The quantum dots are placed in a constant-temperature air-blast drying oven for heat treatment, and the heating temperature and the heating time can be set according to actual requirements. For example, the heating temperature is 120 ℃ to 180 ℃, i.e., 120 ℃, 180 ℃, and any other suitable temperature between 120 ℃ to 180 ℃. The heating time is 0-12h, i.e. 0h,12h and any other suitable heating time between 0-12h. That is, the heating temperature of the heat treatment is 120 ℃ to 180 ℃. The heating time of the heat treatment is 0-12h.
In some embodiments, the SnSe prepared is 2 The quantum dots are divided into six groups of test groups, and the six groups of test groups are put into a constant-temperature air-blowing drying box for heat treatment, wherein the heating temperature is 160 ℃, and the heating time is 0h,4h,6h,8h,10h and 10 2h respectively. In addition, this embodiment also deals with pure PEG 400 The solution was heated at 160 ℃ for 12h and used as a control. The excitation wavelength was 370nm for each test and control group, and all test conditions were the same. Of samples from six test and control groupsThe fluorescence spectrum is shown in FIG. 6.
As can be seen from FIG. 6, as the heating time increases, snSe 2 The fluorescence intensity of the quantum dots gradually increases. SnSe after heating for 12h 2 The fluorescence intensity of the quantum dots is compared with that of SnSe after being heated for 10h 2 The fluorescence intensity of the quantum dots was significantly reduced without significant shift in peak position, probably due to PEG in the sample 400 The functional group in (1) has reached saturation already at 10h. During the heating process, the fluorescence peak position gradually red-shifted with the increase of the heating time, which may be too short, only part of SnSe 2 Quantum dot quilt PEG 400 Functional group modification in (1). Comparing SnSe after heating for 12h 2 Quantum dots and PEG 400 It can be found that the peak positions of the fluorescence spectra of the two are obviously different, and the intensity difference is very large, thus proving that the SnSe is obtained 2 The fluorescence enhancement of the quantum dots is SnSe 2 Nanoparticle coated PEG 400 As a result of the medium functional group modification, the fluorescence intensity increased by about 10 times.
In addition, the embodiment of the application also researches the heating temperature to SnSe 2 The heating time is 10h due to the influence of the fluorescence characteristics of the quantum dots. Exemplarily, snSe is shown in fig. 9 2 The quantum dots are heated for 10h at 120 ℃, 140 ℃, 160 ℃ and 180 ℃ respectively. As can be seen from FIG. 9, snSe heated at 160 deg.C 2 The fluorescent properties of quantum dots are best.
Referring to FIG. 10, the SnSe is heat-treated at 160 ℃ for 10h 2 Fluorescence spectra of quantum dots at different excitation wavelengths. As can be seen from FIG. 10, the SnSe after the heat treatment changes from 370nm to 450nm in the excitation wavelength 2 The emission peak wavelength of the quantum dots is changed from 450nm to 535nm, and the emission is maximum under the excitation of 406 nm. The quantum dot fluorescence peak shows a red shift with increasing excitation wavelength. Furthermore, by this method, snSe can be significantly increased 2 Fluorescence intensity of quantum dots, this pair of investigated fluorescent SnSe 2 The quantum dots have a guiding function.
Please refer to fig. 11, snse 2 The reason for the fluorescence enhancement of quantum dots is: the heat treatment may be at PEG 400 In a solventForming a thermodynamic state, the ultrasonically exfoliated nanoparticles are heated to a plasma state, and then the surface defects of the nanoparticles may be associated with PEG 400 Further reaction of the fragment molecules of (a) may further result in the presence of carboxylate groups on the surface of the nanoparticles.
The above embodiment provides SnSe 2 A preparation method of quantum dots by reacting SnSe 2 Crushing the powder to obtain SnSe 2 Microparticles; adding the SnSe into polyethylene glycol 2 Micron particles to form an initial mixed solution with a preset concentration; carrying out ultrasonic pretreatment on the initial mixed solution to obtain a pretreated mixed solution; carrying out ultrasonic crushing on the pretreated mixed solution to obtain an ultrasonic mixed solution; centrifuging the ultrasonic mixed solution, and collecting the centrifuged supernatant to obtain SnSe dispersed in the polyethylene glycol 2 Quantum dots; to the SnSe 2 And carrying out heat treatment on the quantum dots. The preparation method is simple and easy to operate. After heat treatment, the SnSe can be remarkably increased 2 The fluorescent property of the quantum dot enables the SnSe prepared by the preparation method 2 The quantum dot has strong fluorescence property, and is further SnSe 2 The quantum dots are widely applied in the fields of optical devices, lighting devices and the like.
An embodiment of the present application further provides a SnSe 2 Quantum dot of said SnSe 2 The quantum dot is prepared by the preparation method.
While the invention has been described with reference to specific embodiments, the scope of the invention is not limited thereto, and those skilled in the art can easily conceive various equivalent modifications or substitutions within the technical scope of the invention. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.
Claims (9)
1. SnSe 2 The preparation method of the quantum dot is characterized by comprising the following steps:
SnSe 2 Crushing the powder to obtain SnSe 2 Microparticles;
adding the SnSe into polyethylene glycol 2 Micron particles to form an initial mixed solution with a preset concentration;
carrying out ultrasonic pretreatment on the initial mixed solution to obtain a pretreated mixed solution;
carrying out ultrasonic crushing on the pretreated mixed solution to obtain an ultrasonic mixed solution;
centrifuging the ultrasonic mixed solution, and collecting the centrifuged supernatant to obtain SnSe dispersed in the polyethylene glycol 2 Quantum dots;
to the SnSe 2 And carrying out heat treatment on the quantum dots.
2. The SnSe of claim 1 2 The preparation method of the quantum dot is characterized in that the SnSe is prepared by reacting SnSe with a catalyst 2 The powder is crushed, comprising:
SnSe by mortar pair 2 Grinding the powder to obtain SnSe 2 The powder is crushed.
3. The SnSe of claim 1 2 The preparation method of the quantum dot is characterized in that the polyethylene glycol comprises PEG 200 、PEG 400 And PEG 600 At least one of (1).
4. The SnSe of claim 1 2 The preparation method of the quantum dot is characterized in that the preset concentration is 0.6-1.3 mg/ml.
5. The SnSe of claim 1 2 The preparation method of the quantum dot is characterized in that the ultrasonic pretreatment is carried out on the initial mixed solution, and comprises the following steps:
and carrying out ultrasonic pretreatment on the initial mixed solution for preset time by using a water bath ultrasonic instrument.
6. The SnSe of claim 5 2 The preparation method of the quantum dots is characterized in that the pretreated mixed solution is subjected to ultrasonic crushingThe method comprises the following steps:
and under the preset ultrasonic condition, carrying out ultrasonic crushing on the pretreated mixed liquid by adopting an ultrasonic cell crusher.
7. The SnSe of claim 6 2 The preparation method of the quantum dot is characterized in that the preset ultrasonic conditions comprise:
the crushing power of the ultrasonic cell crusher is 450W-550W; and/or the working cycle of the probe of the ultrasonic cell crusher is 2S-6S and 4S-8S, and the total crushing time is 8h-12h; and/or the distance that the probe of the ultrasonic cell crusher extends into the liquid level of the pretreatment mixed liquid is 1.2cm-1.8cm; and/or, sonication with an ice bath.
8. The SnSe of claim 1 2 The preparation method of the quantum dot is characterized in that the centrifugal treatment conditions comprise: the centrifugal speed is 8500-9500 r/min, and the centrifugal time is 25-35 min.
9. SnSe 2 Quantum dot, characterized in that said SnSe 2 The quantum dot is prepared by the preparation method of any one of claims 1 to 8.
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| CN102863955A (en) * | 2012-10-12 | 2013-01-09 | 上海交通大学 | Polyethylene glycol/stannic sulfide intercalation quantum dot and hydrothermal synthesis method |
| CN105600773A (en) * | 2015-12-18 | 2016-05-25 | 上海交通大学 | Preparation method of graphene quantum point by using graphite nanoparticle liquid phase stripping |
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| SnSe2 Quantum Dots: Facile Fabrication and Application in Highly Responsive UV-Detectors;Xiangyang Li et al.;《Nanomaterials》;20190915;第9卷;第1324页 * |
| 基于层状材料量子点/石墨烯复合结构的光电探测器研究;李向阳;《中国优秀博硕士学位论文全文数据库(硕士) 工程科技Ⅰ辑》;20211015(第10期);第B015-23页 * |
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