CN113105707A - Nano-silver loaded graphene and quantum dot co-doped polymer and application - Google Patents

Nano-silver loaded graphene and quantum dot co-doped polymer and application Download PDF

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CN113105707A
CN113105707A CN202010801318.5A CN202010801318A CN113105707A CN 113105707 A CN113105707 A CN 113105707A CN 202010801318 A CN202010801318 A CN 202010801318A CN 113105707 A CN113105707 A CN 113105707A
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CN113105707B (en
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王颖
王志文
曹明轩
张彦军
杜大明
乐庆胜
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Shenzhen Wanzhida Enterprise Management Co ltd
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Abstract

The invention relates to a nano-silver loaded graphene and quantum dot co-doped polymer and a preparation method thereof, wherein the nano-silver loaded graphene and quantum dot co-doped polymer is prepared from the following components in parts by mass: 1-3.5 parts of nano-silver loaded graphene; 5-20 parts of semiconductor quantum dots; 20-74 parts of photosensitive polymer; 1-5 parts of a photoinitiator. The invention also relates to application of the obtained nano-silver loaded graphene and quantum dot co-doped polymer in a random laser. The raw materials are simple and easy to obtain, and the cost is low; and the obtained random laser has the characteristics of short preparation period, simple preparation process, low production cost, higher emitted light intensity and low threshold value, so that the random laser has wide application prospect.

Description

Nano-silver loaded graphene and quantum dot co-doped polymer and application
Technical Field
The invention belongs to the field of quantum dots, and particularly relates to a nano-silver loaded graphene and quantum dot co-doped polymer, and a preparation method and application of the nano-silver loaded graphene and quantum dot co-doped polymer.
Background
Laser technology has been widely used in many fields such as industry, medicine and communication. Random lasers are a subject of constant relevance and importance, particularly in the development of new low-cost and mirrorless laser technologies. The random laser core component comprises a pumping source, a working medium and a resonant cavity. The light with certain frequency and consistent direction is selected by the resonant cavity to be amplified in the highest priority, and the light with other frequencies and directions is inhibited to form standing wave oscillation and finally emitted in the form of laser. The random laser uses a strong scattering, disordered and aperiodic medium as a resonant cavity, has the characteristics of low threshold, small size, no resonant cavity structure, simple process, short preparation period, low manufacturing cost and the like, and has wide application prospect in the aspects of photonic integration, optical sensing, optical fiber communication, tumor detection, wearable devices and the like.
Recent developments in graphene-based random lasers have highlighted the role of graphene in implementing novel RLs suitable for designing high-performance optoelectronic and nanoelectronic devices. The graphene is sp2Two-dimensional honeycomb lattices of hybridized carbon atoms, the remarkable properties of which are well known, can be doped chemicallyImpurities, external magnetic fields and applied voltages. In recent studies on stochastic lasing of graphene, highly porous vertical graphene wall networks are used to scatter the emitted light of perovskite nanocrystals and provide important optical feedback for achieving stochastic lasing and ultra-low threshold energy densities.
On the other hand, in view of the continuous development of related bio-imaging and bio-sensing applications, development of quantum dots with low toxicity and higher photo-stability is required. As such, graphene quantum dots are emerging carbon-based quantum dots that have received much attention due to their unique properties and wide applications. They are more photostable, biocompatible and environmentally friendly than some conventional scatterers. Due to their excellent properties, they are promising alternatives to noble metal doped quantum dots in many applications, including light emitting diodes, solar cells, bio-imaging, biosensing and photocatalysis. The dye is a common laser gain medium, and the corresponding dispersed liquid crystal structure formed is a dye-doped polymer dispersed liquid crystal structure. Random laser defects of dye-doped polymer dispersed liquid crystals are: the laser emission threshold is high, the full width of the half peak is large, the light stability is poor, the synthesis process is complex, the light-emitting wave band is not easy to change, the production period is long and the cost is high; at dispersible concentrations in the polymer dispersed liquid crystal structure, it is not convenient to prepare random lasers; and the noble metal doped quantum dots have high cost and great environmental pollution, and the finished solution is easy to have cluster precipitation and has poor stability. So from a practical point of view, it seems interesting to develop a random laser based on graphene quantum dots, but there is little research on the use of graphene quantum dots in a random laser. The preparation of random laser by using nano-silver loaded graphene and quantum dot co-doped polymer is not studied, so that the research and study are worth.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a nano-silver loaded graphene and quantum dot co-doped polymer and application thereof in a random laser, and can overcome the defects of the noble metal doped random laser.
An object of the present invention is to provide a graphene and quantum dot co-doped polymer, which is achieved by the following technical means.
The polymer codoped by nano-silver loaded graphene and quantum dots is characterized by being prepared from the following components in parts by mass:
Figure BDA0002627486240000021
further, the semiconductor quantum dots are selected from ZnCdSeS/ZnS quantum dots or perovskite semiconductor quantum dots,
the perovskite semiconductor quantum dot is CsPbX3Perovskite semiconductor quantum dots, X is selected from Cl, Br or I.
Further, the photosensitive polymer is selected from one or more of polymethyl methacrylate, polymethyl acrylate, polyethyl acrylate, polyamino acrylate, poly hydroxypropyl acrylate or polyurethane acrylate.
Further, the photoinitiator is selected from one or more of phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide, 2-hydroxy-methyl phenyl propane-1-one, 1-hydroxy cyclohexyl phenyl ketone, benzoin dimethyl ether, 2-phenyl benzyl-2-dimethyl amine-1- (4-morpholine benzyl phenyl) butanone and 2-isopropyl thioxanthone.
Another object of the present invention is to provide a preparation method of the nano-silver loaded graphene and quantum dot co-doped polymer, which includes the following steps:
(1) blending a photosensitive polymer and a photoinitiator to form a mixed solution;
(2) adding the semiconductor quantum dots into the mixed solution, and stirring to obtain a solution A;
(3) adding the nano-silver loaded graphene into the mixed solution A, and stirring to obtain a solution B;
(4) and (3) carrying out ultraviolet curing on the solution B by using ultraviolet light.
Further, in the above (2) and (3), the stirring method is: the ultrasound is performed first, and then the mechanical agitation is performed.
Further, the wavelength of the ultraviolet light is 200-365 nm.
Further, the ultraviolet curing time is more than or equal to 5 seconds.
Further, the steps (1) to (4) are carried out under protection from light.
The invention also aims to provide application of the nano-silver loaded graphene and quantum dot co-doped polymer in a random laser.
The invention has the following beneficial effects:
1. the invention provides a nano-silver loaded graphene and quantum dot co-doped polymer and a preparation method thereof, wherein the raw materials are common chemicals and are simple and easy to obtain; the preparation process is simple and the cost is low; the required preparation environment is loose, and the method has good industrialization prospect.
2. The random laser of the nano-silver loaded graphene and quantum dot co-doped polymer has the characteristics of short preparation period, simple preparation process, low production cost, higher emitted light intensity and low threshold value, and has the advantages of low driving voltage, high sensing precision, high communication quality and the like in the aspects of photonic integration, optical sensing, optical fiber communication, tumor detection, wearable devices and the like.
Drawings
Fig. 1 is an optical microscope image of the nano-silver loaded graphene and quantum dot co-doped polymer in example 1.
Fig. 2 is an optical microscope image of the nano-silver loaded graphene and quantum dot co-doped polymer in example 2.
Fig. 3 is an optical microscope image of the nano-silver loaded graphene and quantum dot co-doped polymer in example 3.
Fig. 4 is a schematic structural diagram of a random laser in which nano-silver loaded graphene and quantum dots are co-doped with a polymer in embodiment 4.
The designations in the drawings include: 1-pump laser; 2-working medium and resonant cavity; 3-a spectrometer; 4-spectrometer probe; 5-random laser; 6-a focusing lens; 7-pump laser.
Detailed Description
The nano-silver loaded graphene and quantum dot co-doped polymer, the preparation method thereof and the related random laser structure are specifically described in the following with reference to specific embodiments. The scope of the invention is not limited to the embodiments.
In the embodiment of the present invention, the first and second substrates,
the method for loading the graphene by the nano silver comprises the following steps: the material of the nano-silver loaded graphene is a mixed heating method. Mixing the graphene and the acetate of the metal silver in a manual or mechanical ball milling mode, further heating in a segmented mode, keeping the temperature for a period of time when the temperature reaches the acetate decomposition temperature of the metal silver, and forming metal silver nano particles on the surface of the graphene by utilizing the characteristic that the acetate of the metal silver is heated and decomposed.
The nano-silver loaded graphene is purchased from chemical society and has the model of GRSP 50;
ZnCdSeS/ZnS semiconductor quantum dot and CsPbBr3Perovskite semiconductor quantum dots are all purchased from Guangdong Pujiafu optoelectronic technologies, Inc.
Example 1
A nano-silver loaded graphene and quantum dot co-doped polymer is prepared from the following components in parts by mass:
Figure BDA0002627486240000041
the nano-silver loaded graphene and quantum dot co-doped polymer is prepared by the following method:
(1) and (3) stirring the photosensitive polymer polymethyl methacrylate and the photoinitiator phenylbis (2,4, 6-trimethylbenzoyl) phosphine oxide in parts by mass at 50 ℃ in a dark place for 5min to form a mixed solution.
(2) And adding the ZnCdSeS/ZnS semiconductor quantum dots into the mixed solution according to the mass parts, firstly performing ultrasonic dispersion for 2 hours, and then mechanically stirring for 1 hour at 50 ℃ in a dark place to obtain a solution A.
(3) Adding the nano-silver loaded graphene into the mixed solution A according to the mass parts, firstly performing ultrasonic dispersion for 2 hours, and then mechanically stirring for 1 hour at 50 ℃ in a dark place to obtain a solution B;
(4) and (3) carrying out ultraviolet curing on the solution B by using ultraviolet light with the wavelength of 200nm, wherein the curing time is 5 seconds.
Fig. 1 shows an optical microscope image of a nano-silver loaded graphene and quantum dot co-doped polymer, the obtained morphology is consistent with expectations, the nano-silver loaded graphene can be well embedded in a polymer matrix under ultraviolet light curing, and the nano-silver loaded graphene distribution is seen to have no clustering phenomenon and is relatively good in distribution.
Example 2
Figure BDA0002627486240000042
The nano-silver loaded graphene and quantum dot co-doped polymer is prepared by the following method:
(1) and (2) stirring the photosensitive polymer polymethyl acrylate and the photoinitiator 2-hydroxy-methyl phenyl propane-1 ketone in parts by mass at 50 ℃ in a dark place for 10min to form a mixed solution.
(2) Reacting CsPbBr3Adding the perovskite semiconductor quantum dots into the mixed solution according to the mass parts, firstly performing ultrasonic dispersion for 2 hours, and then mechanically stirring for 3 hours at 50 ℃ in a dark place to obtain a solution A.
(3) Adding the nano-silver loaded graphene into the mixed solution A according to the mass parts, firstly performing ultrasonic dispersion for 2 hours, and then mechanically stirring for 1 hour at 50 ℃ in a dark place to obtain a solution B;
(4) and (3) carrying out ultraviolet curing on the solution B by using ultraviolet light with the wavelength of 365nm, wherein the curing time is 5 seconds.
Fig. 2 shows an optical microscope image of the nano-silver loaded graphene and quantum dot co-doped polymer, the obtained morphology is consistent with expectations, the polymer structure formed by co-doping the nano-silver loaded graphene and the quantum dot is better overall, and as can be seen by comparing fig. 1, the nano-silver loaded graphene in fig. 2 begins to appear clusters, which indicates that the kind of the semiconductor quantum dot and the doping amount of the nano-silver loaded graphene both affect the polymer structure.
Example 3
Figure BDA0002627486240000051
The nano-silver loaded graphene and quantum dot co-doped polymer is prepared by the following method:
(1) and stirring the photosensitive polymer polyethylacrylate and the photoinitiator benzoin dimethyl ether in parts by weight at 50 ℃ in a dark place for 5min to form a mixed solution.
(2) And adding the ZnCdSeS/ZnS semiconductor quantum dots into the mixed solution according to the mass parts, firstly performing ultrasonic dispersion for 4 hours, and then mechanically stirring for 2 hours at 50 ℃ in a dark place to obtain a solution A.
(3) Adding the nano-silver loaded graphene into the mixed solution A according to the mass parts, firstly performing ultrasonic dispersion for 2 hours, and then mechanically stirring for 1 hour at 50 ℃ in a dark place to obtain a solution B;
(4) and (3) carrying out ultraviolet curing on the solution B by using ultraviolet light with the wavelength of 300nm, wherein the curing time is 5 seconds.
Fig. 3 shows an optical microscope image of the nano-silver loaded graphene and quantum dot co-doped polymer, and the obtained morphology is consistent with expectations, when the doping amount of the nano-silver loaded graphene is too large, a structure formed by the nano-silver loaded graphene and the quantum dot co-doped polymer may have a large number of clusters of the nano-silver loaded graphene.
Example 4
The embodiment relates to application of nano-silver loaded graphene and quantum dot co-doped polymer in a random laser.
(1) The structure and the working principle of the random laser of the nano-silver loaded graphene and quantum dot co-doped polymer.
The structural schematic diagram of the random laser of the nano-silver loaded graphene and quantum dot co-doped polymer is shown in fig. 4. The respective parts function as follows:
pump laser 1: the pump light energy is provided for the nano-silver loaded graphene and quantum dot co-doped polymer, the population inversion occurs in the working medium, and an atomic system needs to be de-excited by a certain method, so that the population at the upper energy level is increased, and laser radiation is generated.
Working medium and resonant cavity 2: the laser generation must be carried out with the selection of a suitable working medium, which may be a gas, a liquid, a solid or a semiconductor. Population inversion can be achieved in such media to create the necessary conditions for obtaining laser light. According to the invention, perovskite semiconductor quantum dots in the nano-silver loaded graphene and quantum dot co-doped polymer are used as working media; and the polymer microdroplet in the nano-silver loaded graphene and quantum dot co-doped polymer is used as a resonant cavity.
Spectrometer 3 and spectrometer probe 4: collecting the spectral information of the emergent laser.
Random laser 5: the scattering effect of the polymer droplets increases the travel of photons in the working medium and there is a certain probability that the optical circuit is closed by the travel. The photons are continuously excited and radiated in the closed optical loop, the light intensity is continuously enhanced, and finally the light intensity exceeds the laser threshold value, and the stroke is random laser radiation.
The focusing lens 6: and focusing the emission light spot to enable the light energy irradiated on the surface of the nano-silver loaded graphene and quantum dot co-doped polymer to be more concentrated.
Pump laser 7: pump laser light 1 is generated.
The working principle of the random laser is as follows: the pump laser 1 generated by the pump laser 7 is an ultraviolet pulse laser, the pulse frequency is 1Hz-1000Hz, and the pulse energy is more than 1 muJ. The pump laser 1 is focused by the focusing lens 6, and the pump light spot is reduced. Through the pumping action of the pump laser 1, the quantum dots in the working medium and the resonant cavity 2 emit fluorescence. The fluorescence is strongly scattered by the working medium and the polymer microdroplets in the resonant cavity 2 to form a random closed resonant cavity, and random laser 5 radiation is generated after the laser threshold is reached. The emission spectrum information can be collected by the spectrometer 3 and the spectrometer probe 4.
(2) Random laser correlation test of nano-silver loaded graphene and quantum dot co-doped polymer
Using the given structure of the random laser of FIG. 4, examples 1 to 3, and comparative samples 1 to 5, respectively, were subjected to performance tests under 0.5mJ/cm2At the pumping intensity of (c).
Wherein the content of the first and second substances,
the comparative sample 1 and the example 2 have the same component types, the same component parts, and the same preparation methods, but do not contain the nano-silver-loaded graphene.
The comparative sample 2 and example 2 were identical in the kinds of components, the parts by mass of the components, and the preparation method, and the difference was that CsPbCl was used in the comparative sample 2 in an equal part by mass3Perovskite semiconductor quantum dots instead of CsPbBr as described in example 23The perovskite semiconductor quantum dots are doped with polymers, and do not contain nano-silver loaded graphene.
The comparative sample 3 and example 2 were identical in the kind of components, the parts by mass of the components, and the preparation method, and the difference was that CsPbI was used in the comparative sample 2 in an equal part by mass3Perovskite semiconductor quantum dots instead of CsPbBr as described in example 23The perovskite semiconductor quantum dots are doped with polymers, and do not contain nano-silver loaded graphene.
The comparative sample 4 and example 1 have the same component types, component parts by mass, and preparation methods, but do not contain nano-silver-loaded graphene.
The relevant data are shown in table 1. The quantum dot doped polymer without the nano-silver loaded graphene, namely the comparative samples 1-4, does not have random laser under the pumping intensity, which indicates that the threshold value is higher than 0.5mJ/cm2. As can be seen from the data in the table, the emission light intensity and the random laser threshold of the nano-silver loaded graphene and quantum dot co-doped polymer have significant advantages compared with those of the quantum dot doped polymer.
Table 1 examples 1-3, and comparative samples 1-4 were applied to random lasers, the emitted light intensity of which and the random laser threshold
Figure BDA0002627486240000071

Claims (10)

1. The polymer codoped by nano-silver loaded graphene and quantum dots is characterized by being prepared from the following components in parts by mass:
Figure FDA0002627486230000011
2. the nano-silver loaded graphene and quantum dot co-doped polymer according to claim 1, wherein the semiconductor quantum dot is selected from ZnCdSeS/ZnS quantum dot or perovskite semiconductor quantum dot,
the perovskite semiconductor quantum dot is CsPbX3Perovskite semiconductor quantum dots, X is selected from Cl, Br or I.
3. The nano-silver loaded graphene and quantum dot co-doped polymer according to claim 1, wherein the photosensitive polymer is selected from one or more of polymethyl methacrylate, polymethyl acrylate, polyethyl acrylate, polyaminoacrylate, poly hydroxypropyl acrylate or polyurethane acrylate.
4. The polymer co-doped with the nano-silver-supported graphene and the quantum dot according to claim 1, wherein the photoinitiator is selected from one or more of phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide, 2-hydroxy-methylphenylpropane-1 one, 1-hydroxycyclohexyl phenyl ketone, benzoin bis methyl ether, 2-phenylbenzyl-2-dimethylamine-1- (4-morpholinebenzylphenyl) butanone and 2-isopropyl thioxanthone.
5. The preparation method of the nano-silver loaded graphene and quantum dot co-doped polymer according to any one of claims 1 to 4, characterized by comprising the following steps:
(1) blending a photosensitive polymer and a photoinitiator to form a mixed solution;
(2) adding the semiconductor quantum dots into the mixed solution, and stirring to obtain a solution A;
(3) adding the nano-silver loaded graphene into the mixed solution A, and stirring to obtain a solution B;
(4) and (3) carrying out ultraviolet curing on the solution B by using ultraviolet light.
6. The preparation method of the nano-silver loaded graphene and quantum dot co-doped polymer according to claim 5, wherein in the steps (2) and (3), the stirring method comprises the following steps: the ultrasound is performed first, and then the mechanical agitation is performed.
7. The method for preparing the nano-silver loaded graphene and quantum dot co-doped polymer according to claim 5, wherein the wavelength of the ultraviolet light is 200-365 nm.
8. The preparation method of the nano-silver loaded graphene and quantum dot co-doped polymer according to claim 5, wherein the ultraviolet curing time is not less than 5 seconds.
9. The preparation method of the nano-silver loaded graphene and quantum dot co-doped polymer according to claim 5, wherein the steps (1) to (4) are performed under the condition of avoiding light.
10. The application of the nano-silver loaded graphene and quantum dot co-doped polymer according to any one of claims 1 to 4 in a random laser.
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