CN111117615B - Quantum dot material, preparation method and application thereof, and light-emitting device - Google Patents
Quantum dot material, preparation method and application thereof, and light-emitting device Download PDFInfo
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- H10K50/115—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers comprising active inorganic nanostructures, e.g. luminescent quantum dots
Abstract
The invention discloses an alkali metal doped indium phosphide quantum dot with higher luminous efficiency, a preparation method and application thereof and a luminescent device. The preparation method of the alkali metal doped indium phosphide quantum dot comprises the following steps: dissolving indium acetate and alkali metal acetate in a mixed solution of acetic acid and n-butyl alcohol to obtain a solution I; mixing a phosphorus source with a mixed solution of acetic acid and n-butyl alcohol to obtain a solution II; mixing the solution I and the solution II, and then carrying out microwave reaction to obtain an intermediate product; and purifying and drying the intermediate product to obtain the alkali metal doped indium phosphide quantum dot. The alkali metal doped indium phosphide-based luminescent material with the perovskite structure is obtained by doping the alkali metal elements into the InP quantum dots, and the quantum dot material has ultrahigh luminescent efficiency and can meet the requirement of being used in luminescent devices.
Description
Technical Field
The invention relates to the technical field of quantum dots, in particular to a quantum dot material, a preparation method and application thereof, and a light-emitting device.
Background
The quantum dot material can be combined into a plurality of photoelectric devices, and the properties of the quantum dot material depend on the composition, the shape and the size of the quantum dot material, so that the quantum dot material has wide application prospect in the photoelectric devices. In order to fully utilize the potential of the quantum dot material, the quantum dot material needs to meet the following standards when used: narrow and symmetric emission spectra, high Photoluminescence (PL) Quantum Yield (QY), high optical stability, eco-friendly and low cost mass production method. The earliest research on quantum dots focused mostly on materials containing cadmium, mercury or lead elements. But the toxicity and the pollution to the ecological environment cannot be ignored. Therefore, quantum dot production without the above materials needs to be attempted.
Besides the characteristics of nano materials, the quantum dots based on indium phosphide also have other unique excellent characteristics: (1) the lattice structure of the material is similar to that of diamond, belongs to a zinc blende structure, and is a direct forbidden band semiconductor material, and the forbidden band width is 1.35eV at room temperature; (2) the exciton Bohr radius is 14nm, and thus has a stronger amountA sub-confinement effect; (3) the transition probability is high, and the absorption rate of photons with the forbidden band width larger than that of the photons is high; (4) the electron mobility is higher; (5) high thermal conductivity and high radiation resistance. The characteristics make InP quantum dots have good prospects in the field of photoelectric devices. However, the application of the method is limited due to the problems of multiple surface defects, uneven size and the like. Researchers have further found that quantum dots can exhibit a range of more excellent characteristics through doping of metal ions, for example, Zn2+The in (zn) P alloy quantum dots formed by doping have absorption and blue shift of fluorescence spectrum, but the luminous efficiency is still insufficient, so that there is a need to provide a quantum dot material with higher luminous efficiency.
Disclosure of Invention
The invention aims to provide a quantum dot material with higher luminous efficiency, a preparation method and application thereof, and a luminescent device.
According to a first aspect of the present invention, there is provided a quantum dot material, according to an embodiment of the present invention, the alkali gold quantum dot material has the following general formula: a. the3In2P3And A is selected from any one of Li, Na, K, Rb and Cs, namely the invention provides an alkali metal doped indium phosphide quantum dot material.
According to a second aspect of the invention, there is provided a method of preparing the quantum dot material, the method comprising, according to an embodiment of the invention, the steps of:
dissolving indium salt and alkali metal salt in a mixed solution of low-alcohol and acid to obtain a solution I;
mixing a phosphorus source with a mixed solution of low-valent alcohol and acid to obtain a solution II;
mixing the solution I and the solution II, and then carrying out microwave reaction to obtain an intermediate product;
and washing and drying the intermediate product to obtain the alkali metal doped indium phosphide quantum dots.
Wherein, the phosphorus source refers to a material which provides phosphorus element in the reaction, and a non-limiting example of the material can be P (TMS) commonly used in InP quantum dot synthesis3I.e. tris (trimethylsilyl) -A phosphine; p [ N (CH) may also be selected3)2]3Or P [ N (CH)3CH2)2]3I.e., tris (dimethylamino) -phosphine or tris (diethylamino) -phosphine, as the phosphorus source used in the present invention. The indium salt is preferably a soluble indium salt having a certain solubility in a mixed solution of a lower alcohol and an acid, and specifically may be indium hydrochloride, indium sulfate, indium nitrate, indium acetate, or the like. The alkali metal salt is preferably a soluble alkali metal salt having a certain solubility in a mixed solution of a lower alcohol and an acid, and may specifically be a hydrochloride, a sulfate, a nitrate, an acetate, or the like. The alkali metal is at least one of lithium, sodium, potassium, rubidium and cesium. By lower alcohols is meant straight-chain or straight-chain aliphatic C having not more than 4-OH groups substituted onto carbon atoms1-10An alcohol.
According to the examples of the present invention, the anion corresponding to the indium salt is the same as the anion corresponding to the alkali metal salt.
According to the embodiment of the invention, the anion corresponding to the indium salt and the anion corresponding to the alkali metal correspond to acid, and in the mixed solution of the lower alcohol and the acid, the acid is dilute acid solution.
According to an embodiment of the present invention, the indium salt and the alkali metal salt are present in a ratio of 2:3 in a molar ratio.
According to the embodiment of the invention, the concentration of the phosphorus source in the second solution is 6-15 mmol/L.
Preferably, the concentration of the phosphorus source in the second solution is 8-12 mmol/L.
According to the embodiment of the invention, the microwave reaction is carried out for 3-6h under the conditions of 100-140 ℃.
According to the embodiment of the present invention, the volume fraction of the acid and the oligohydric alcohol in the mixed solution of the acid and the oligohydric alcohol is 50%.
According to an embodiment of the present invention, the first solution and the second solution are mixed by dropping the solutions into the second solution which is stirred at a high speed.
According to the embodiment of the invention, the intermediate product can be purified by washing specifically by heating it to elevated temperature (which may be under vacuum condition to accelerate liquid volatilization), removing 60-80% of liquid, and adding 1:1:1 to 60-80% of the volume before heating, centrifuging and retaining the upper liquid.
According to the embodiment of the present invention, the drying may be specifically performed by heating the mixture to a colloidal state at 100-140 ℃ (which may be performed under vacuum condition to accelerate the volatilization of the liquid).
According to a third aspect of the invention, the invention provides an application of the alkali metal doped indium phosphide quantum dot in preparing an optical product. Among them, non-limiting examples of the optical product may be a light emitting device, a display device, a lighting device, and the like.
According to a fourth aspect of the present invention, there is provided a light emitting device comprising, according to an embodiment of the present invention, a light emitting layer comprising the above-described alkali metal doped indium phosphide quantum dots or the quantum dot material prepared according to the above-described method.
According to the embodiment of the invention, the light-emitting device further comprises a conductive film layer connected with the light-emitting layer, wherein the conductive film layer is a nano silver wire-graphene composite conductive film.
The term "connected" means that there is a connection relationship between the light-emitting layer and the conductive film layer, and the connection relationship may be between the light-emitting layer and the conductive film layer or indirectly connected, and a non-limiting example of indirect connection may be that a hole function layer (including a hole transport layer and/or a hole injection layer) or an electron function layer (including an electron transport layer and/or an electron injection layer) is further provided between the conductive film layer and the light-emitting layer.
According to an embodiment of the present invention, the light emitting device may be a structure including a conductive film layer as an anode layer, a hole function layer, a quantum dot layer, an electron function layer, and a cathode layer, which are sequentially disposed, wherein the hole function layer includes one of a hole injection layer stacked and combined with the anode layer, a hole transport layer stacked and combined with the quantum dot layer, or two layers stacked and combined with each other; the electron function layer includes one of an electron injection layer laminated with the cathode layer, an electron transport layer laminated with the quantum dot layer, or two layers laminated with each other.
According to the embodiment of the invention, the weight ratio of the nano silver wires to the graphene in the nano silver wire-graphene composite conductive film is 4: 1 (1-16).
According to the embodiment of the invention, the diameter of the nano silver wire is less than or equal to 50nm, and the length of the nano silver wire is more than or equal to 500 mu m.
The silver nanowire can be prepared by the following steps:
and reducing the silver salt in the ethylene glycol solution to obtain a nano silver wire seed crystal, re-dispersing the obtained nano silver wire seed crystal into the ethylene glycol solution for re-growth, and repeating the steps for multiple times to obtain the ultra-long nano silver wire.
The single nano silver wire conductive film has the problems that the mutual contact point resistance is greatly increased and a breakpoint is easy to exist, and the single graphene conductive film has the problem that the sheet resistance is too high. According to the invention, the one-dimensional ultra-long nano silver wire and the two-dimensional graphene nanosheet are lapped by adding the nano silver wire-graphene composite conductive film, so that the problem of single material is solved, and the conductive film has the advantages of low sheet resistance, uniformity and no breakpoint.
The invention has the beneficial effects that:
compared with the original InP quantum dots, the crystal form change of the InP quantum dots can effectively prevent electron quenching, so that more electrons are transited to a valence band to emit light, the luminous efficiency of the quantum dot material is improved, and the use of the quantum dot material in a luminous device can be met.
Drawings
Fig. 1 is a schematic structural view of a light emitting device of an embodiment of the present invention.
Fig. 2 is an etched mirror view of a light emitting device according to an embodiment of the present invention.
Fig. 3 is a result of performance test of a light emitting device according to an embodiment of the present invention.
Detailed Description
The conception, the specific structure, and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below, so that the objects, the features, and the effects of the present invention can be fully understood. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
Example 1
A preparation method of a sodium-doped indium phosphide quantum dot specifically comprises the following steps:
(1) dissolving 0.1mmol of anhydrous indium acetate and 0.15mmol of anhydrous sodium acetate in acetic acid/n-butyl alcohol solution (the mass fraction of glacial acetic acid is 50%) to obtain a solution I;
(2) dispersing tris (trimethylsilyl) -phosphine in an acetic acid/n-butyl alcohol solution (the mass fraction of glacial acetic acid is 50%) at a concentration of 10mmol/L to obtain a solution II;
(3) dropping the solution into a second solution under the state of high-speed stirring (400-;
(4) pouring the uniformly mixed solution into a microwave reaction kettle, putting the microwave reaction kettle into a microwave reactor, and carrying out microwave reaction for 5 hours at the temperature of 120 ℃;
(5) and cooling, taking out the reaction kettle, placing the reaction kettle into a vacuum oven, vacuumizing, heating to 120 ℃, heating, pouring ethylene glycol/n-butanol/acetonitrile in a ratio of 1:1:1 to 3/4 liquid level after 3/4 volume of liquid is evaporated, centrifuging the mixture in a centrifuge at 5000rpm for 30min, pouring the upper layer liquid into a sample bottle, and heating to a colloidal state at 120 ℃ in the vacuum oven to obtain the sodium-doped indium phosphide quantum dot.
Fig. 1 is a schematic structural diagram of a light-emitting device according to an embodiment of the present invention, and as shown in fig. 1, the light-emitting device includes, from bottom to top, a transparent conductive anode layer 1, a hole injection layer 2, a hole transport layer 3, a quantum dot layer 4, an electron injection layer 5, an electron transport layer 5, and a cathode layer 6, which are sequentially disposed. The transparent conductive anode layer 1 is a nano silver wire-graphene composite conductive film, the hole injection layer 2 is PEDOT, the PSS layer, the hole transport layer 3 is a PVK layer, the quantum dot layer 4 is an alkali metal doped indium phosphide quantum dot layer, the electron injection layer 5 is a TPBi layer, the electron transport layer 5 is a LiF layer, and the cathode layer 6 is Al.
The preparation method of the light-emitting device specifically comprises the following steps:
1. synthesis of nano silver wire-graphene composite conductive film
1.1 preparation of silver nanowire seeds
(1) Putting ethylene glycol into a reaction kettle, heating to 151.5 ℃, keeping the temperature for 1h to ensure that the temperature of the ethylene glycol fully reaches the required temperature and keeps unchanged, wherein the stirring speed of the reaction kettle is 280 rpm.
(2) Adding a prepared copper chloride glycol solution into a reaction kettle, heating to a specified temperature for 15min, adding a polyvinylpyrrolidone glycol solution, and adding a silver nitrate solution after 15 min. And (3) in the process of adding the nitrate into the solution, using a peristaltic pump to realize uniform and slow dripping, controlling the dripping speed to be 0.1mL/min, reacting for 3 hours, taking out the mixed solution, and centrifugally collecting the nano silver wire seed crystal.
1.2 repeated growth of silver nanowires
Ultrasonically dispersing the collected nano silver wire seed crystal into an ethylene glycol solution, repeating the reaction step, and in the process, reducing silver nitrate into simple substance silver to enable the nano silver wire to continuously grow, repeating the reaction step for many times to obtain the ultra-long nano silver wire with the diameter of less than or equal to 50nm and the length of more than or equal to 500 mu m.
1.3 pulverization and refinement of graphene
And (3) crushing the graphene through a high-speed stirring and shearing device, filtering and collecting the crushed graphene through a filter screen with the aperture of 50nm to obtain graphene powder with the particle size of less than or equal to 50 nm.
1.4 preparation of nano silver wire-graphene ink
(1) And (3) mixing the prepared ultra-long nano silver wire and graphene powder according to the weight ratio of 20: dispersing 80 weight percent of the mixture into isopropanol solution, and performing ultrasonic dispersion for 30 min;
(2) adding 0.5 mass percent of thickening agent hydroxypropyl cellulose, 0.1 mass percent of dispersing agent polyvinylpyrrolidone and 0.3 mass percent of flatting agent TRITON-X into the solution, and uniformly mixing the solution in a mode of combining ultrasonic stirring and mechanical stirring to obtain the nano silver wire-graphene ink.
1.5 preparation of nano silver wire-graphene composite conductive film
And (3) coating the nano silver wire-graphene ink on the PET film, and drying to obtain the nano silver wire-graphene composite conductive film.
2. Preparation of light emitting devices
(1) Spin-coating a PEDOT (PSS) solution (with the solid content of 1%) on the nano silver wire-graphene composite conductive film at the initial speed of 500rpm, the subsequent speed of 4000rpm for 1min, and then baking at 120 ℃ for 5min to solidify the nano silver wire-graphene composite conductive film to form a hole injection layer;
(2) spin-coating a PVK chlorobenzene solution with the concentration of 5mg/mL on the hole injection layer at the initial speed of 500rpm and the subsequent speed of 4000rpm for 1min, and then baking the hole injection layer for 15min at 80 ℃ under a vacuum condition to obtain a hole transport layer;
(3) spin-coating the alkali metal-doped indium phosphide quantum dot colloid on the hole transport layer at the spin-coating speed of 1500rpm for 30s, and drying to obtain a quantum dot layer;
(4) sequentially depositing TPBi and LiF/Al on the quantum dot layer by using vacuum thermal evaporation equipment to form an electron injection layer, an electron transport layer and a cathode layer, wherein the thickness of TPBi is 30nm, the thickness of LiF is 1nm, and in the evaporation process, the vacuum degree is controlled to be 1 multiplied by 10-3Pa, the evaporation temperature is 300 ℃ and 350 ℃, and a crystal oscillator plate is used as a thickness reference; a light emitting device is obtained.
Fig. 2 is an etched mirror view of a light emitting device according to an embodiment of the present invention. As shown in FIG. 2, the device has very uniform structural distribution, and electrode layers formed by the top silver nanowire-graphene composite conductive film are crossed and compact and are uniformly distributed, so that the device has a very good application prospect.
Fig. 3 is a result of performance test of a light emitting device according to an embodiment of the present invention. The upper curve of the two curves represents the change in current efficiency with luminous intensity, and the lower curve represents the change in external quantum efficiency with luminous intensity. The results in fig. 3 show that the light emitting device provided by the present embodiment has high external quantum efficiency (which can reach 16%) and current efficiency, which is greatly improved compared to the external quantum efficiency of no more than 15% in the prior art. The result shows that the quantum dot and the light-emitting device prepared by the quantum dot have high luminous efficiency.
Example 2
A light emitting device was distinguished from example 1 in that the obtained silver nanowire-graphene composite conductive film was cut, a circuit was etched, a solder resist was applied, an IC chip and a resistive element were packaged with epoxy resin, and finally, a light emitting composite layer (a hole injection layer, a hole transport layer, a quantum dot layer, an electron injection layer, and an electron transport layer) was applied and then a frame was sealed with epoxy resin.
Example 3
The cesium-doped indium phosphide quantum dot has a structural formula of Cs3In2P3。
The preparation method of the quantum dot material comprises the following steps:
(1) dissolving 0.1mmol of anhydrous indium acetate and 0.15mmol of anhydrous cesium acetate in 50% acetic acid/n-butanol solution to obtain a first solution;
(2) dispersing tris (trimethylsilyl) -phosphine in a 50% acetic acid/n-butanol solution at a concentration of 10mmol to give solution two;
(3) dripping the solution I into a solution II in a high-speed stirring state, and then stirring at a high speed for 2 hours;
(4) pouring the uniformly mixed solution into a microwave reaction kettle, putting the microwave reaction kettle into a microwave reactor, and carrying out microwave reaction for 5 hours at the temperature of 120 ℃;
(5) and cooling, taking out the reaction kettle, placing the reaction kettle into a vacuum oven, vacuumizing, heating to 120 ℃, heating, pouring ethylene glycol/n-butanol/acetonitrile in a ratio of 1:1:1 to 3/4 liquid level after 3/4 volume of liquid is evaporated, centrifuging the mixture in a centrifuge at 5000rpm for 30min, pouring the upper layer of liquid into a sample bottle, and heating to a colloid state at 120 ℃ in the vacuum oven to obtain the cesium-doped indium phosphide quantum dot.
Example 4
A potassium-doped indium phosphide quantum dot with a structural formula of K3In2P3。
The preparation method of the quantum dot material comprises the following steps:
(1) dissolving 0.1mmol of indium sulfate and 0.15mmol of potassium sulfate in a sulfuric acid/ethylene glycol solution (the mass fraction of sulfuric acid is 10%) to obtain a solution I;
(2) dispersing tris (trimethylsilyl) -phosphine in a sulfuric acid/ethylene glycol solution (the mass fraction of sulfuric acid is 10%) at a concentration of 10mmol to obtain a solution two;
(3) dripping the solution I into a solution II in a high-speed stirring state, and then stirring at a high speed for 2 hours;
(4) pouring the uniformly mixed solution into a microwave reaction kettle, putting the microwave reaction kettle into a microwave reactor, and carrying out microwave reaction for 4 hours at the temperature of 110 ℃;
(5) and cooling, taking out the reaction kettle, placing the reaction kettle into a vacuum oven, vacuumizing, heating to 110 ℃, heating, pouring ethylene glycol/n-butanol/acetonitrile in a ratio of 1:1:1 to 3/4 liquid level after 3/4 volume of liquid is evaporated, centrifuging the mixture in a centrifuge at 5000rpm for 25min, pouring the upper layer of liquid into a sample bottle, and heating to a colloidal state at 110 ℃ in the vacuum oven to obtain the potassium-doped indium phosphide quantum dot.
While the preferred embodiments of the present invention have been illustrated and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A quantum dot material having the formula: a. the3In2P3And A is selected from any one of Li, Na, K, Rb and Cs.
2. The method for preparing a quantum dot material according to claim 1, comprising the steps of:
dissolving indium salt and alkali metal salt in a mixed solution of low-alcohol and acid to obtain a solution I;
mixing a phosphorus source with a mixed solution of low-valent alcohol and acid to obtain a solution II;
mixing the solution I and the solution II, and then carrying out microwave reaction to obtain an intermediate product;
and washing and drying the intermediate product to obtain the alkali metal doped indium phosphide quantum dot.
3. The method of claim 2 wherein said indium salt and said alkali metal salt are mixed in a molar ratio of 2: 3.
4. The method according to claim 2, wherein the concentration of the phosphorus source in the second solution is 6 to 15 mmol/L.
5. The method as claimed in claim 2, wherein the microwave reaction is carried out at 140 ℃ for 3-6 h.
6. Use of the quantum dot material of claim 1 in the manufacture of an optical product.
7. A light-emitting device comprising a light-emitting layer, wherein the light-emitting layer comprises the quantum dot material according to claim 1 or comprises the quantum dot material prepared by the preparation method according to any one of claims 2 to 5.
8. The light-emitting device according to claim 7, further comprising a conductive film layer connected to the light-emitting layer, wherein the conductive film layer is a nano silver wire-graphene composite conductive film.
9. The light-emitting device according to claim 8, wherein a weight ratio of the silver nanowires to the graphene in the silver nanowire-graphene composite conductive film is 4: (1-16).
10. The light-emitting device according to claim 9, wherein the diameter of the nano silver wire is less than or equal to 50nm, and the length of the nano silver wire is greater than or equal to 500 μm.
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