CN112063380A - Composite material with metal nanowires wrapped by organic luminescent material and preparation method thereof - Google Patents
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Abstract
The invention relates to the field of core-shell structure nano materials, in particular to a composite material of an organic luminescent material wrapping metal nanowires and a preparation method thereof. The method comprises the steps of firstly synthesizing a pure metal nanowire by a hydrothermal method, and then wrapping an organic luminescent material on the surface of the metal nanowire to form a core-shell structure, so that the core-shell structure of the metal-organic luminescent material composite is realized on a single one-dimensional metal nanowire. The novel nano material with the core-shell structure integrates organic luminescent materials and metals, can be used for manufacturing nano-level luminescent devices, further realizes the nano-level luminescent devices similar to OLED structures, and brings unprecedented new application to the field of photoelectric information; not only overcomes the problem of high cost, but also meets the characteristic requirement of flexibility of the light-emitting device.
Description
Technical Field
The invention relates to the field of core-shell structure nano materials, in particular to a composite material of an organic luminescent material wrapping metal nanowires and a preparation method thereof.
Background
The OLED is an electroluminescent device based on a multilayer organic thin film structure, and has the advantages of low power consumption, high response speed, good low-temperature characteristic, small quality, capability of realizing soft screen and the like. Among them, the soft screen can be realized because the OLED substrate material has a very wide range of alternatives.
The transparent electrode is one of important components of photoelectric devices which are widely applied in daily life of people, and is continuously researched by researchers. An organic electroluminescent device and a preparation method thereof with application number of CN201710024541.1, wherein the publication date is 2018, 08 and 28, and the organic electroluminescent device comprises: a cathode metal layer; irradiating the cleaned transparent electrode ITO with ultraviolet rays; the organic functional layer is positioned between the cathode metal layer and the transparent electrode ITO; in the organic functional layer, the following layers are sequentially laid along the electron transmission direction from the transparent electrode ITO to the cathode metal layer: a hole injection layer; a light-emitting layer which is made of 8-hydroxyquinoline aluminum doped with dye and is subjected to microwave low-temperature annealing treatment; a hole buffer layer made of an Ag-doped ZnS thin film. Said invention not only can raise the conductivity of light-emitting layer of organic electroluminescent device, but also can raise the density of current carrier.
However, the traditional transparent electrode material ITO is high in price, and the ITO material has the problem of easy breakage, so that the ITO material cannot be used for a flexible photoelectric device.
Disclosure of Invention
In order to solve the problems of high cost and no flexibility of the transparent electrode material, the invention provides a composite material of an organic light-emitting material wrapped metal nanowire, wherein the composite material is a core-shell structure nanowire, the metal nanowire is used as an inner core, and the surface of the metal nanowire is wrapped with the organic light-emitting material to form a core-shell structure.
On the basis of the above scheme, further, the metal nanowire comprises at least one metal nanowire of copper, silver, gold, aluminum, nickel, zinc, platinum, titanium and vanadium.
On the basis of the above scheme, further, the organic luminescent material comprises Alq3、Znq2、Liq、Beq2、Gaq3One or more of (a).
The invention provides a preparation method of a composite material of organic luminescent material wrapped metal nanowires, which comprises the following steps:
(1) synthesizing a metal nanowire;
(2) treating residues attached to the metal nanowires with an acid;
(3) and (3) placing the metal nanowires in the step (2) in a clarified solution of an organic light-emitting material to enable the organic light-emitting material to wrap the metal nanowires, so as to obtain the composite material of the organic light-emitting material wrapped with the metal nanowires.
On the basis of the above scheme, further, the acid used for treating the residue attached to the metal nanowire in the step (2) includes one or more of an acetic acid solution, a lactic acid solution, and a formic acid solution. The invention selects the specific acid solutions, can effectively remove residues, does not influence the quality of the nano wire, and can ensure that the organic luminescent material is effectively coated on the nano wire.
On the basis of the scheme, the metal nanowire is further synthesized by adopting a liquid phase method of aqueous solution/organic solution.
On the basis of the scheme, further, in the synthesis process, high-purity nitrogen is continuously introduced to avoid the oxidation of the metal nanowires.
On the basis of the scheme, further, the preparation method of the clear solution of the organic luminescent material comprises the following steps: the organic luminescent material is placed in a solvent, after three steps of stirring, ultrasound and stirring, the supernatant is centrifuged to obtain a clear solution without particle suspension, the polarity of the selected solvent is consistent with that of the selected organic luminescent material, and the solvent of the organic luminescent material can be fully dissolved.
On the basis of the scheme, the stirring is carried out for 10-20min, the centrifugation time is 5-10min, and Alq is avoided3Presence of suspended particles in solution.
On the basis of the scheme, further, the metal nanowires synthesized in the step (1) are dispersed in a dispersing agent, and are circulated for 3-4 times through ultrasonic and centrifugal steps, wherein the ultrasonic time is 3-5min each time, and the centrifugal time is 5-10min, so that impurity ions and organic matters remained in the reaction are removed, and then the metal nanowires are stored in the dispersing agent for later use, wherein the dispersing agent is a solvent which effectively disperses the nanowires and avoids the nanowires from agglomerating; in the step (3), the metal nanowires are placed in a clear solution of an organic luminescent material and are subjected to magnetic stirring or dip-coating treatment.
The invention provides a composite material of organic luminescent material wrapping metal nano-wire and a preparation method thereof, compared with the prior art, the composite material has the following advantages:
the invention relates to a one-dimensional core-shell structure nano material, which is characterized in that pure metal nanowires with excellent quality are synthesized by a hydrothermal method, and then an organic luminescent material (such as Alq) is added3、Znq2、Liq、Beq2、Gaq3And the like) are directly wrapped on the surface of the metal nanowire to form a core-shell structure, so that the metal-organic luminescent material composite core-shell structure is realized on a single one-dimensional metal nanowire. The invention firstly and creatively integrates the organic luminescent material and metal together to prepare the nano material with the core-shell structure, realizes the direct contact of the electrode material and the organic luminescent material on the microscopic level, can be used for manufacturing nano-level luminescent devices, further realizes the nano-level luminescent devices similar to OLED structures, and brings unprecedented new application to the field of photoelectric information.
The composite core-shell structure material can be made into a nano-grade luminescent device, not only overcomes the problems of harsh preparation conditions, complex process and high cost of the traditional luminescent device (such as OLED), but also meets the characteristic requirement of flexibility of the luminescent device.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a flow chart of the preparation of core-shell structure nanowires of copper-organic light-emitting materials according to the invention;
FIG. 2 shows a copper-organic light emitting material Alq according to an embodiment of the present invention3SEM image of core-shell structure nanowire;
FIG. 3 shows a copper-organic light emitting material Alq according to an embodiment of the present invention3AES spectrogram of the core-shell structure nanowire sample at 0 nm;
FIG. 4 shows a copper-organic light emitting material Alq according to an embodiment of the present invention3IR spectrogram of the core-shell structure nanowire;
FIG. 5 shows a copper-organic light emitting material Alq according to an embodiment of the present invention3PL luminescence spectrum of core-shell structure nano-wire.
FIG. 6 shows a copper-organic light emitting material Alq according to an embodiment of the present invention3And (3) a bending effect graph of core-shell structure nanowires transferred on a PET substrate.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. 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 invention.
The invention also provides the examples shown in the following table:
as shown in fig. 1, the preparation method of the composite material of the organic light emitting material wrapped metal nanowire of the present invention comprises the following steps:
(1) synthesizing a metal nanowire;
(2) acid-treating residues attached to the metal nanowires;
(3) and (3) placing the metal nanowires in the step (2) in a clarified solution of an organic luminescent material to obtain uniform nanowires with a core-shell structure, wherein the metal nanowires are wrapped by the organic luminescent material.
The specific steps are as follows:
1. firstly, growing a copper nanowire by a hydrothermal method, obtaining a pure copper nanowire through ultrasonic and centrifugal processes, and then storing the pure copper nanowire in a dispersing agent for later use.
Respectively weighing 0.8mmol of copper chloride powder, 0.4mmol of nickel acetylacetonate powder and 10ml of oleylamine by using an analytical balance, mixing in a three-neck flask, and placing the whole three-neck flask reaction device on a constant-temperature heating magnetic stirrer. The whole reaction device is heated to 80 ℃ for 10min, and then the temperature is raised to 185 ℃ for 4 h. Meanwhile, the whole reaction device is kept to continuously pass 50sccm of high-purity nitrogen gas, so that the grown copper nanowires are prevented from being oxidized by doping oxygen in the reaction process.
In the reaction process, copper chloride is used as an oxidant, nickel acetylacetonate is used as a catalyst, and oleylamine is used as a reducing agent, a structure directing agent and a dispersing agent. Oleylamine as a reducing agent reduces divalent copper ions into copper atoms, as a structure directing agent enables the reduced copper atoms to grow along a certain direction, and as a dispersing agent enables various reaction substances to fully react in a solution.
After the copper nanowires grow, the constant temperature button is closed, and the reaction device is naturally cooled to room temperature under the conditions of stirring and introducing high-purity nitrogen. And dispersing the taken copper nanowires in a normal hexane dispersing agent, transferring the copper nanowires into a centrifugal tube, carrying out ultrasonic treatment for 3-5min, placing the centrifugal tube into a centrifugal machine, and centrifuging for 5min at the rotating speed of 10000 r/min. And repeating the steps of ultrasonic treatment and centrifugation for 3-4 times to obtain the copper nanowire, and placing the copper nanowire in n-hexane dispersion liquid for later use.
2. And carrying out acid treatment on the copper nanowires to remove organic residues attached to the single nanowires.
This step can be considered mainly from the following two processing methods:
a) and carrying out acid treatment on the copper nanowires on the filter membrane. And (3) ultrasonically oscillating the copper nanowire solution to uniformly disperse the copper nanowires in the normal hexane, and performing suction filtration on the uniformly dispersed copper nanowires on the filter membrane by using a vacuum suction filtration device. Preparing deionized water: the acetic acid is 10: 1, placing the filter membrane attached with the copper nanowires in the diluted acid solution, taking out the filter membrane after 30s, cleaning the filter membrane in deionized water for 30s, replacing the deionized water, and then cleaning for 3-5min to remove residual acid in the copper nanowires and avoid the residual acid from corroding the surfaces of the copper nanowires.
b) And carrying out acid treatment on the copper nanowires on the silicon substrate. Imprinting a copper nanowire on a silicon substrate by using a nanowire imprinting technology, and preparing deionized water: the acetic acid is 10: 1, placing the silicon substrate attached with the copper nanowires in the diluted acid solution, taking out after 30s, and drying by using nitrogen.
The copper nanowire with the organic residue on the surface removed can be obtained by the two ways.
3. Placing a certain amount of organic luminescent material in a solvent, and centrifuging and taking supernatant liquid to obtain a clear solution without particle suspension after three steps of stirring, ultrasound and stirring.
With an organic light-emitting material Alq3Is an embodiment. Because of Alq3Is a polar material, a polar solvent should be selected for dissolution. Acetonitrile is a common polar organic solvent, so acetonitrile is chosen as the solvent in this example. 0.02g of Alq are weighed3Placed in 20ml acetonitrile. Adding Alq3Magnetically stirring in acetonitrile for 10min to obtain Alq3Dissolving, and then subjecting to ultrasonic treatment for 10min to obtain undissolved granular Alq3Dispersing, and magnetically stirring for 10min to obtain Alq dissolved in acetonitrile3And (3) solution. In order to obtain clarified Alq3Solution of Alq3The solution was transferred to a centrifuge tube for centrifugation. Centrifuging at 10000r/min for 5min, and collecting supernatant. This step may further avoid Alq3The existence of suspended particles in the solution, thereby reducing the organic luminescent materialThe appearance of a residue of the particulate organic light emitting material in the wrapped copper nanowire.
4. And (3) placing the metal nanowires subjected to acid treatment in a clarified solution of the organic luminescent material, and performing a magnetic stirring process or a dip-coating process to obtain the uniform composite material with the metal nanowires wrapped by the organic luminescent material shell.
With an organic light-emitting material Alq3Wrapping copper nanowires is an embodiment that can be considered primarily from two processing methods:
a) magnetic stirring method. After acid treatment on the filter membrane, taking down the copper nanowires on the filter membrane, and putting the copper nanowires into Alq3In the clear solution, the ultrasonic oscillation is carried out until the copper nanowire is in Alq3The solution was uniformly dispersed, followed by a magnetic stirring process. The rotating speed of magnetic stirring is 600r/min, the mixed solution after stirring is transferred to a centrifuge tube for centrifugation after 20 hours, the supernatant is poured out after centrifugation, and only the nanowires at the lower layer are left. Adding acetonitrile into a centrifuge tube, carrying out ultrasonic treatment for 3-5min, centrifuging for 5min at the rotating speed of 10000r/min, pouring out the supernatant again, and only leaving the nanowires at the lower layer. Then, adding normal hexane into the centrifugal tube, repeating the steps of ultrasonic treatment and centrifugation for 3-4 times to obtain the organic luminescent material Alq3A composite material wrapping the copper nanowire.
b) And (4) dip coating. After the silicon substrate is treated by acid, the silicon substrate imprinted with the copper nanowire is immersed into Alq3The solution was clarified, blown dry with nitrogen and washed in pure acetonitrile to remove residual Alq3Repeating the dipping process once to obtain Alq3Wrapped copper nanowires.
The organic luminescent material Alq can be realized by adopting the method3It should be noted that the selection of specific parameters in the present embodiment, such as the amount of reagent and the operation time, is not meant to limit the scope of the claims, and the embodiment is only a preferred option (which itself has corresponding inventive step) under the inventive concept, and those skilled in the art can select the core-shell structure for wrapping the copper nanowires according to the present inventionThe design idea of the invention is to correspondingly select specific parameters and steps so as to achieve or basically achieve the purpose of the invention of the technical scheme.
The organic luminescent material Alq prepared by the embodiment of the invention3The copper-wrapped nanowires are characterized, and the analysis results are as follows:
FIG. 2 shows the copper-Alq obtained in the experiment3Scanning electron microscope image of core-shell structure nanowire wrapped with organic luminescent material Alq3Then, the surface of the nanowire is changed from the original flat and smooth surface to a slightly rough surface, which indicates that the surface of the copper nanowire is actually coated with a layer of material.
FIG. 3 shows copper-Alq3AES spectrogram of the core-shell structure nanowire sample at 0nm shows that Al, C, O and N elements exist on the surface of the nanowire sample. As can be seen from the SEM image of fig. 2, the sample consists of the nanowires, and therefore, the detected Al, C, O, and N elements only come from the surface of the nanowires. Thus, it was confirmed that the organic light-emitting material Alq3Has been wrapped onto copper nanowires.
FIG. 4 shows copper-Alq3And (3) an infrared spectrogram of the core-shell structure nanowire. Alq3The functional group contains C-N, C-O and the like. For 1000-2000 cm-1Is analyzed in the wave number range of 1690-1500 cm-1The peak in the range is the stretching vibration of C ═ N bond, 1475-1500 cm-1The peak in the range is C-O stretching vibration. And compared with the pure copper nanowire, the pure copper nanowire has no peaks in the two ranges, thereby also proving that the organic luminescent material Alq is coated on the nanowire3。
In conclusion, the organic light-emitting material Alq coated on the surface of the nanowire is proved from two aspects of element analysis and functional group characterization3。
Therefore, the preparation of the core-shell structure nano material prepared by wrapping the metal nanowire with the organic luminescent material can be effectively and successfully realized through a specific preparation process, and the nano material can be used as a nano-level luminescent device.
FIG. 5 shows copper-Alq3Photoluminescence (PL) spectra of core-shell structured nanowires. It can be seen that after the acetic acid treatmentThen 1mg/ml of Alq3Solution synthesized copper-Alq3The core-shell structure nanowire has a luminescence peak at 520nm, the copper nanowire has no luminescence peak at the waveband, and Alq3The band has a luminous peak, thereby proving that the organic luminous material Alq is coated on the nano-wire3And successfully has the luminescence property. Wherein, it is necessary to remove the residual organic matter on the surface of the original copper nanowire by adopting the acetic acid treatment process, and the copper-Alq synthesized by the acetic acid treatment process is not adopted3The core-shell structure nanowire has almost no luminescence peak at the position of 520nm and has no luminescence property. Meanwhile, Alq with lower concentration of 0.25mg/ml is adopted3Solution synthesis of copper-Alq3Core-shell structured nanowires are feasible, but the luminescence peak intensity at 250nm is relatively reduced. In addition, the effect of using two acids, lactic acid solution and formic acid solution, is also consistent with acetic acid. In summary, the specific weak acid treatment in the invention can successfully coat the organic light-emitting material on the nanowire, and simultaneously ensure the light-emitting performance, thereby solving the problem of how to coat the organic light-emitting material on the nanowire and preparing the nano-level light-emitting device with the organic light-emitting material coated on the nanowire for the first time.
The composite material prepared by wrapping the metal nanowire with the organic light-emitting material has flexibility, as shown in fig. 6, wherein fig. 6 is copper-Alq3The bending effect of the core-shell structure nanowire transferred on the PET substrate, and after the bending and twisting tests, the copper-Alq3The core-shell structure nanowire still keeps the original linear form and is not changed.
The simple preparation method of the core-shell structure nanowire luminescent material is used for integrating an organic luminescent material and metal together, so that the electrode material is directly contacted with the organic luminescent material on a microscopic level, and further can be used for manufacturing a nano-level luminescent device and realizing the nano-level luminescent device similar to an OLED structure.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A composite material of organic luminescent material wrapping metal nano-wire is characterized in that: the composite material is a core-shell structure nanowire, the metal nanowire is used as an inner core, and the surface of the metal nanowire is coated with an organic light-emitting material to form a core-shell structure.
2. The organic light-emitting material-wrapped metal nanowire composite material according to claim 1, wherein: the metal nanowire comprises at least one metal nanowire of copper, silver, gold, aluminum, nickel, zinc, platinum, titanium and vanadium.
3. The organic light-emitting material-wrapped metal nanowire composite material according to claim 1, wherein: the organic luminescent material comprises Alq3、Znq2、Liq、Beq2、Gaq3One or more of (a).
4. The method for preparing the organic light-emitting material-wrapped metal nanowire composite material according to claim 1, comprising the following steps:
(1) synthesizing a metal nanowire;
(2) treating residues attached to the metal nanowires with an acid;
(3) and (3) placing the metal nanowires in the step (2) in a clarified solution of an organic light-emitting material to enable the organic light-emitting material to wrap the metal nanowires, so as to obtain the composite material of the organic light-emitting material wrapped with the metal nanowires.
5. The method for preparing the composite material of organic light-emitting material wrapped metal nanowire according to claim 4, wherein: the acid used for treating the residue attached to the metal nanowire in the step (2) includes one or more of an acetic acid solution, a lactic acid solution, and a formic acid solution.
6. The method for preparing the composite material of organic light-emitting material wrapped metal nanowire according to claim 4, wherein: the metal nanowire is synthesized by adopting a liquid phase method of aqueous solution/organic solution.
7. The method for preparing the composite material of organic light-emitting material wrapped metal nanowire according to claim 6, wherein: and in the synthesis process, high-purity nitrogen is continuously introduced to avoid the oxidation of the metal nanowires.
8. The method for preparing the composite material of organic light-emitting material wrapped metal nanowire according to claim 4, wherein the method for preparing the clear solution of organic light-emitting material comprises the following steps: placing the organic luminescent material in a solvent, carrying out three steps of stirring, ultrasonic treatment and stirring, then centrifuging and taking supernatant to obtain a clear solution without particle suspension, wherein the polarity of the selected solvent is consistent with that of the selected organic luminescent material.
9. The method for preparing the composite material of organic light-emitting material wrapped metal nanowire according to claim 8, wherein: the stirring and ultrasonic time is 10-20min, and the centrifugal time is 5-10 min.
10. The method for preparing the composite material of organic light-emitting material wrapped metal nanowire according to claim 4, wherein:
dispersing the metal nanowires synthesized in the step (1) in a dispersing agent, circulating for 3-4 times through ultrasonic and centrifugal steps, wherein the ultrasonic time is 3-5min each time, and the centrifugal time is 5-10min to remove impurity ions and organic matters remained in the reaction, and then storing the metal nanowires in the dispersing agent for later use;
in the step (3), the metal nanowires are placed in a clear solution of an organic luminescent material and are subjected to magnetic stirring or dip-coating treatment.
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