CN111739995A - White light LED based on dual-waveband white light perovskite quantum dots and preparation method - Google Patents
White light LED based on dual-waveband white light perovskite quantum dots and preparation method Download PDFInfo
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
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- H—ELECTRICITY
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Abstract
A white light LED based on dual-band white light perovskite quantum dots and a preparation method thereof, the white light LED comprises an insulating base, a bowl-shaped reflector, an ultraviolet LED chip and a lens, wherein the bowl-shaped reflector is arranged on the insulating base, a heat conducting fin is arranged between the bowl-shaped reflector and the insulating base, the ultraviolet LED chip is fixed in the bowl-shaped reflector, the blue light LED chip is covered with the dual-band white light perovskite quantum dots, the lens is arranged outside the bowl-shaped reflector, and the lens is filled with a transparent silicon resin packaging material; by Hbr and MnCl2Auxiliary oil bath reaction to obtain Mn2+Doped CsPb (Cl/Br)3The double-waveband white-light perovskite quantum dots accurately allocate the position relative intensity of two wavelengths, the double-waveband white-light perovskite quantum dots are coated on an ultraviolet light LED chip and cured, and a lens is placed outside the bowl-shaped reflector and filled with a transparent packaging material. The invention is beneficial to improving the stability and the application range of the perovskite material in the white light LED.
Description
Technical Field
The invention relates to a white light LED and a preparation method thereof, in particular to a white light LED prepared by exciting dual-waveband white light perovskite quantum dots through an ultraviolet LED, and belongs to the field of semiconductor illumination and display.
Background
As a new generation solid light source, the semiconductor LED has the advantages of energy saving, environmental protection, firmness, durability, high energy density, small volume and the like, has been widely applied to the fields of liquid crystal display backlight sources, large color display screens, landscape lighting, automotive lamps, landscape decoration and the like, and is a research hotspot in the fields of photoelectron, lighting and the like.
The common preparation method of the white light LED comprises the combination of blue light LED excitation fluorescent powder, ultraviolet LED excitation fluorescent powder and red, green and blue LED chips, and various methods generate multicolor light to be mixed to form white light, wherein the blue light LED excitation fluorescent powder, the ultraviolet LED excitation fluorescent powder and the red, green and blue LED chips are the mainstream technology for obtaining the white light LED at present. For example, an InGaN blue LED chip is used for exciting yellow rare earth fluorescent powder to form white light, and the defect is that the spectrum of the yellow rare earth fluorescent powder lacks red components, so that the color rendering index of a white LED is not high; or the InGaN blue LED chip is used for exciting the red light and the green light fluorescent powder to form the tricolor white light, and the defect is that the fluorescent efficiency of the red light fluorescent powder is not high, so that the luminous efficiency of the white light LED is not high. The traditional fluorescent powder is usually synthesized by a high-temperature solid-phase method, the reaction temperature is high, and the energy consumption and the cost are high. Meanwhile, the fluorescent powder material is solid opaque particles with the magnitude of micron or dozens of microns, so that the problem of light scattering and light blocking is serious, and the light is not uniform. And the fluorescent powder is dispersed in the packaging adhesive in a suspension form during the assembly of the white light LED, so that the problem of sedimentation exists, the fluorescent powder is not uniformly coated, and the light emission is not uniform.
Therefore, it is necessary to develop a fluorescent conversion material with small particle size, wide color gamut, high color rendering index, low cost, good stability and easy uniform dispersion to prepare a white LED to solve the problems and disadvantages of the prior art. At present, perovskite quantum dots serving as a class of potential fluorescent conversion materials become research hotspots, and have the advantages of adjustable luminescence wavelength, high quantum efficiency and the like, but perovskite has a strong ion exchange phenomenon, so that the perovskite quantum dots with two or more luminescence wavelengths can rapidly generate an ion exchange chemical reaction after being mixed, new perovskite quantum dots with intermediate luminescence wavelengths are generated, and the application of various perovskite quantum dots in preparing white light and preparing white light LEDs is severely limited.
Disclosure of Invention
Aiming at the problems of the prior art for blending white light LED by perovskite quantum dots, the invention provides Mn2+Doped CsPb (Cl/Br)3Stable single perovskite quantum dot emitting cyan-red double-waveband white light, and Mn excited by ultraviolet LED2+:CsPb(Cl/Br)3A white light LED manufactured by dual-band white light stable perovskite quantum dot luminescence is used for avoiding the problem of anion exchange reaction in the process of blending various perovskite quantum dots when the perovskite quantum dots are applied to the white light LED. The invention also provides a preparation method of the white light LED.
The invention discloses a white light LED of ultraviolet light excited double-waveband white light perovskite quantum dots, which adopts the following technical scheme:
the white light LED comprises an insulating base, a bowl-shaped reflector, an ultraviolet light LED chip and a lens, wherein the bowl-shaped reflector is arranged on the insulating base, a heat conducting sheet is arranged between the bowl-shaped reflector and the insulating base, the ultraviolet light LED chip is fixed in the bowl-shaped reflector, and the ultraviolet light LED chip is covered with dispersed Mn2+:CsPb(Cl/Br)3The silicon resin of two wave band white light perovskite quantum dots is provided with two electrodes of being connected with the ultraviolet LED chip on the insulating base, and the outside of bowl shape speculum is covered with lens, fills transparent silicon resin packaging material in the lens, wraps up electrode bonding wire, bowl shape speculum, two wave band white light perovskite quantum dots and ultraviolet LED chip on the insulating base.
The emission wavelength of the ultraviolet LED chip is 350-430 nm.
The Mn is2+:CsPb(Cl/Br)3The double-waveband white-light perovskite quantum dot is prepared by the conventional CsPb (Cl/Br)3HBr and MnCl are added on the basis of quantum dot oil bath reaction2Obtaining the quantum dot solid powder by accurate reaction and centrifuging the reaction solution; the Mn is2 +:CsPb(Cl/Br)3The perovskite quantum dot is a nano-scale, uniform-size and stable luminescent material with double wave bands for emitting white light.
The Mn is2+:CsPb(Cl/Br)3The two emission peak wavelengths of the two-waveband white-light perovskite quantum dot are near 480nm and 600nm, the corresponding colors of the two wavelengths are complementary colors, the white light is modulated by controlling the relative intensities of the two wavebands, the spectral range of the white light is wider, the white light covers cyan, yellow-green, yellow, orange and red, the spectrums are mixed to form white light, and Mn is excited by an ultraviolet LED (light-emitting diode)2+:CsPb(Cl/Br)3The dual-band white perovskite quantum dots form a white LED.
The preparation method of the white light LED comprises the following steps:
(1) preparation of Mn2+Doped CsPb (Cl/Br)3Dual-band white-light perovskite quantum dots: preparing a cesium oleate precursor solution, namely adding 0.1-0.5g of cesium carbonate into a 50mL three-necked bottle, adding 5-20mL of octadecene and 0.1-5mL of oleic acid, introducing high-purity nitrogen for protection, magnetically stirring, bubbling for 0.5-5 hours by using nitrogen, then heating to 110-; weighing raw materials with a Cl/Br raw material molar ratio of 7:3 and a Mn/Pb molar ratio of 1:5, adding the raw materials into a 50mL three-neck flask filled with 5-20mL of octadecene, 0.1-5mL of oleic acid and 0.2-0.5mL of oleylamine, magnetically stirring, introducing high-purity nitrogen for protection, heating to 110-130 ℃ for stirring for 1 hour after a nitrogen bubble is 0.5-5 hours, then adjusting the temperature to 170-220 ℃, immediately injecting 0.2-5mL of cesium oleate precursor solution after reaching the specified temperature, reacting for 10 seconds-10 minutes, transferring to ice water, cooling and cooling. The stock solution is transferred into a centrifuge tube and centrifuged for 3-30 minutes at high speed (4000-2+Doped CsPb (Cl/Br)3Dual-band white-light perovskite quantum dots;
(2) fixing a heat-conducting plate on the insulating base, fixing the bowl-shaped reflector on the heat-conducting plate,
(3) fixing an ultraviolet LED chip with the emission wavelength of 350-430nm in a bowl-shaped reflector, respectively placing two electrodes on two sides of an insulating base, and respectively welding the two electrodes with a P electrode and an N electrode of the blue LED chip together through gold wires;
(4) 0.1-0.2 g of Mn prepared in the step (1)2+Doped CsPb (Cl/Br)3Uniformly mixing the double-waveband white-light perovskite quantum dot powder and the silicon resin A/B glue, coating the mixture on a fixed ultraviolet LED chip connected with an electrode, and naturally curing the mixture at the normal temperature of 25 ℃;
(5) fixing a lens outside the bowl-shaped reflector, connecting the two electrodes with gold wires, the bowl-shaped reflector, and Mn2+Doped CsPb (Cl/Br)3The double-waveband white light perovskite quantum dot/silicon resin mixture and the ultraviolet LED chip are wrapped on the insulating base, transparent silicon resin A/B glue is filled in the lens to be uniformly mixed and packaged, and the white light LED is obtained after the silicon resin is cured.
The invention utilizes ultraviolet light to excite the white light LED which emits light by the double-waveband white light perovskite quantum dots, avoids the problem of anion exchange reaction in the process of blending various perovskite quantum dots when the perovskite quantum dots are applied to the white light LED, and promotes the application of the perovskite quantum dot material in the white light LED.
Drawings
FIG. 1 is a schematic structural diagram of a white light LED emitting light by ultraviolet excitation of dual-band white light perovskite quantum dots.
FIG. 2 shows Mn prepared according to the present invention2+Doped CsPb (Cl/Br)3High-resolution TEM images of two-band white-light perovskite quantum dots.
FIG. 3 is a graph of the luminescence spectrum of a white LED prepared according to the present invention.
FIG. 4 is a chromaticity diagram of a white LED prepared according to the present invention.
Wherein: 1. the LED lamp comprises an insulating base, 2 parts of a heat conducting pad, 3 parts of a bowl-shaped reflector, 4 parts of an ultraviolet LED chip, 5 parts of a positive electrode, 6 parts of a negative electrode, 7 parts of a gold wire, 8 parts of Mn2+Doped CsPb (Cl/Br)3The double-waveband white light perovskite quantum dot, 9, silicone, 10, lens.
Detailed Description
As shown in fig. 1, the ultraviolet light excited dual-band white light perovskite quantum dot light emitting white light LED of the present invention comprises an insulating base 1, a heat conducting pad 2, a bowl-shaped reflector 3, an ultraviolet light LED chip 4, a positive electrode 5, a negative electrode 6, a gold wire 7, a dual-band white light perovskite quantum dot 8, a silicon resin 9, and a lens 10; the heat conducting pad 2 is connected with the bowl-shaped reflector 3 and is arranged in the center of the insulating base 1, the ultraviolet LED chip 4 is fixed in the center of the bowl-shaped reflector 3, the positive electrode 5 and the negative electrode 6 are arranged on two sides of the insulating base 1 and are connected with the P electrode and the N electrode of the ultraviolet LED chip 4 through gold threads 7, the ultraviolet LED chip 4 is coated with double-waveband white-light perovskite quantum dots 8, the insulating base is covered with the lens 10, and the high-light-transmission silicon resin packaging material 9 is filled between the insulating base and the lens. Wherein the emission wavelength of the ultraviolet LED chip 5 is 350nm-430 nm.
The preparation method of the white light LED comprises the following steps:
(1) preparation of Mn2+Doped CsPb (Cl/Br)3Dual-band white perovskite quantum dots 8: preparing a cesium oleate precursor solution, namely adding 0.203g of cesium carbonate powder into a 50mL three-necked bottle, adding 10mL of octadecene and 1mL of oleic acid, magnetically stirring, raising the temperature to 120 ℃ after bubbling with nitrogen for 2 hours, stirring for 1 hour, and raising the temperature to 150 ℃ until a clear cesium oleate precursor solution is obtained; 0.0623g PbCl2，0.0345g PbBr2And 0.0080g MnCl2Adding the powder into a 50mL three-necked bottle filled with 10mL of octadecene, 1mL of oleic acid and 1mL of oleylamine, magnetically stirring, bubbling with nitrogen for 2 hours, heating to 120 ℃, stirring for 1 hour, heating to 180 ℃, immediately injecting 1mL of cesium oleate precursor solution, reacting for 30 seconds, transferring into ice water, cooling, transferring the stock solution into a centrifuge tube, centrifuging at the rotating speed of 6000rpm/min for 5min, removing the supernatant, and separating out a precipitate, wherein the precipitate is Mn2+Doped CsPb (Cl/Br)3Dual-band white-light perovskite quantum dots 8;
(2) a heat conducting fin 2 is fixed on an insulating base 1, a bowl-shaped reflector 3 is fixed on the heat conducting fin 2,
(3) an ultraviolet LED chip 4 with the emission wavelength of 370nm is fixed in a bowl-shaped reflector 3, a positive electrode 5 and a negative electrode 6 are respectively arranged on two sides of an insulating base 1 and are respectively welded with a P electrode and an N electrode of the ultraviolet LED chip 4 through gold wires 7.
(4) Uniformly mixing 0.2g of the dual-waveband white-light perovskite quantum dots 8 prepared in the step (1) with silicon resin A/B glue 9, coating the mixture on a fixed ultraviolet LED chip 4 connected with an electrode, and naturally curing at the normal temperature of 25 ℃;
(5) fixing a lens 10 on an insulating substrate 1, exhausting gas in the lens 10, filling the high-light-transmission silicon resin 9A/B mixed glue, and naturally curing for 5 hours at normal temperature to obtain the white light LED, wherein the silicon resin 9 protects a bowl-shaped reflector 3, a blue light LED chip 4, a gold wire 7 and a two-waveband white light perovskite quantum dot 8 layer between the lens 11 and the insulating substrate 1.
The luminescence spectrogram and chromaticity coordinate graph of the white light LED obtained by adopting the ultraviolet LED chip with the emission wavelength of 370nm and the double-waveband white light perovskite quantum dot according to the method are shown in fig. 3 and fig. 4, and the color rendering index of the white light LED is 62.4, the chromaticity coordinate is (0.31,0.34) and the color temperature is 6376K.
Claims (2)
1. The utility model provides a white light LED based on dual waveband white light perovskite quantum dot, includes insulator foot, bowl shape speculum, ultraviolet ray LED chip and lens, and bowl shape speculum setting is characterized by on insulator foot: the bowl-shaped reflector is arranged on the insulating base, the heat conducting fins are arranged between the bowl-shaped reflector and the insulating base, the ultraviolet LED chip is fixed in the bowl-shaped reflector, the ultraviolet LED chip is covered with two-waveband white light perovskite quantum dots, the insulating base is provided with two electrodes connected with the ultraviolet LED chip, the outside of the bowl-shaped reflector is provided with a lens, and the lens is filled with a transparent packaging material. Wherein, the emission wavelength of the ultraviolet LED chip is 350-430 nm. The double-waveband white-light perovskite quantum dot is prepared from HBr and MnCl2Mn obtained by auxiliary oil bath reaction2+Doped CsPb (Cl/Br)3The green-red dual-band white light is emitted to stabilize the perovskite quantum dots, the position relative intensity of two wavelengths is accurately adjusted, and white light is obtained.
2. The method for preparing the white light LED based on the dual-band white light perovskite quantum dot in claim 1 is characterized by comprising the following steps: the method comprises the following steps:
(1) preparation of Mn2+Doped CsPb (Cl/Br)3Dual-band white-light perovskite quantum dots: preparation of Cesium oleate precursor solution, adding 0.1-0.5g Cesium carbonate into a 50mL three-necked bottle, addingAdding 5-20mL of octadecene and 0.1-5mL of oleic acid, introducing high-purity nitrogen for protection, magnetically stirring, bubbling the nitrogen for 0.5-5 hours, then heating to 110-; weighing raw materials with a Cl/Br raw material molar ratio of 7:3 and a Mn/Pb molar ratio of 1:5, adding the raw materials into a 50mL three-neck flask filled with 5-20mL of octadecene, 0.1-5mL of oleic acid and 0.2-0.5mL of oleylamine, magnetically stirring, introducing high-purity nitrogen for protection, heating to 110-130 ℃ for stirring for 1 hour after a nitrogen bubble is 0.5-5 hours, then adjusting the temperature to 170-220 ℃, immediately injecting 0.2-5mL of cesium oleate precursor solution after reaching the specified temperature, reacting for 10 seconds-10 minutes, transferring to ice water, cooling and cooling. The stock solution is transferred into a centrifuge tube and centrifuged for 3-30 minutes at high speed (4000-2+Doped CsPb (Cl/Br)3Dual-band white-light perovskite quantum dots;
(2) fixing a heat-conducting plate on the insulating base, fixing the bowl-shaped reflector on the heat-conducting plate,
(3) fixing an ultraviolet LED chip with the emission wavelength of 350-430nm in a bowl-shaped reflector, respectively placing two electrodes on two sides of an insulating base, and respectively welding the two electrodes with a P electrode and an N electrode of the blue LED chip together through gold wires;
(4) 0.1-0.2 g of Mn prepared in the step (1)2+Doped CsPb (Cl/Br)3Uniformly mixing the double-waveband white-light perovskite quantum dot powder and the silicon resin A/B glue, coating the mixture on a fixed ultraviolet LED chip connected with an electrode, and naturally curing the mixture at the normal temperature of 25 ℃;
(5) fixing a lens outside the bowl-shaped reflector, connecting the two electrodes with gold wires, the bowl-shaped reflector, and Mn2 +Doped CsPb (Cl/Br)3The double-waveband white light perovskite quantum dot/silicon resin mixture and the ultraviolet LED chip are wrapped on the insulating base, transparent silicon resin A/B glue is filled in the lens to be uniformly mixed and packaged, and the white light LED is obtained after the silicon resin is cured.
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