CN109768151B - Multi-color LED for illumination and display and preparation method thereof - Google Patents
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Abstract
The invention discloses a multicolor light-emitting diode (LED) for illumination and display and a preparation method thereof, wherein the multicolor LED comprises a blue LED chip and a multicolor luminescent material which is coated on the surface of the blue LED chip and is based on a metal organic framework and loaded with fluorescent molecules, wherein the multicolor luminescent material comprises the following components: 96.5-99.98wt% of metal organic framework, 0.01-1.5wt% of 3- (2-benzothiazolyl) -N, N-diethylbenzenamine, 0.005-1wt% of methyl 2- (6-amino-3-imino-3H-xanthen-9-yl) benzoate, and 0.005-1wt% of 9- (2-carboxyphenyl) -2,3,6,7,12,13,16, 17-octahydro-1H, 5H,11H, 15H-xanthene [2,3,4-IJ:5,6,7-I 'J' ] biquinoline-18-ammonium chloride. The invention is based on the high-efficiency energy transfer of various fluorescent molecules in the metal organic framework, and the prepared multicolor LED has wide color gamut and high efficiency. The invention improves the problems of narrow color gamut, poor color rendering, difficult multi-chip transfer in the micro-display field and the like of the conventional commercial white light LED, and can be used in the fields of white light illumination and full-color display.
Description
Technical Field
The invention relates to the scientific fields of organic-inorganic hybrid material science, physical optics, solid luminescent materials and the like, in particular to a multicolor LED for illumination and display and a preparation method thereof.
Background
The white light LED has the advantages of high efficiency, energy conservation, environmental protection, quick response, strong reliability, shock impact resistance, no mercury pollution and the like, and is considered to be an ideal lighting product for replacing the traditional lighting source. Currently, commercially available white LEDs mainly include blue LEDs and yellow YAG: ce3+The fluorescent powder is obtained by combination, and the LED packaging structure has the advantages of simple packaging process, easiness in batch production, mature blue LED manufacturing technology and capability of providing high lumen efficiency. However, the white light obtained by combining the blue light (450-. Therefore, the search and design for preparing phosphors that can be effectively excited by commercial blue LEDs, have as broad a spectral coverage as possible, and have a spectrum with sufficient red light content has been the focus and focus of research.
micro-LED chip (micro-LED) is a technology for making traditional LED chip into micro-matrix, the size of traditional LED is generally larger than 200 μm, and the micro-LED is reduced to be within 100 μm, and each pixel point can be individually addressed, driven and lighted through matrix arrangement, compared with traditional TFT-LCD, OLED display technology which develops faster in recent years, micro-LED has the advantages of high contrast, high brightness and low power consumption, can self-illuminate as OLED without backlight element, but has longer service life than OLED, and can be used as display device of head-wearing display equipment, mobile phone, micro-projection, high-end TV and the like. In order to achieve the display effect of wide color gamut, three-primary-color micro-LEDs (R-G-B) need to be grown on an array substrate to provide light-emitting units with different colors, but the method is very complicated and difficult to operate, and a method of coating a wide-spectrum multicolor light-emitting material on a substrate by using a more mature blue micro-LED and adding a color filter layer in the light-emitting direction to realize full-color display is easier to realize, so that the development of an excellent wide-spectrum multicolor light-emitting material is needed.
The metal organic framework is a novel three-dimensional porous crystalline material formed by metal ions or metal ion clusters and polydentate organic ligands in a bridging mode, and the material has the characteristics of ordered pore channel structures, adjustable pore channel sizes, large specific surface area and the like. The organic fluorescent molecules have strong luminescence but aggregation quenching effect, and the luminescence in a solid state is weak, but the aggregation quenching of the fluorescent molecules can be effectively reduced or even avoided by introducing the fluorescent molecules into the pore channels of the metal organic framework, because the pore channel structure of the metal organic framework can greatly limit the intra-molecular rotation motion, the structural rigidity is improved, the probability of non-radiative transition is reduced, and the luminous efficiency and the stability are improved. Based on the purpose of wide-spectrum multicolor luminescence, several fluorescent molecules emitting different light need to be introduced into the system at the same time, but the fluorescent molecules emitting different light characteristics under single excitation light influence the spectrum structure and the output efficiency of the whole system due to insufficient excitation, and when the overlapping degree of the emission spectrum of one molecule and the absorption spectrum of another molecule is large, the former will generate energy transfer to the latter, so that the wide-spectrum efficient luminescence of several fluorescent molecules can be realized under the excitation of single excitation light.
Disclosure of Invention
The invention aims to provide a multicolor LED for illumination and display and a preparation method thereof, which overcome the defects of lack of red light components, poor color rendering of obtained white light and high color temperature of the existing commercial white light LED, can obtain warm color light with high color rendering index and higher lumen efficiency when being applied to the field of white light LEDs, has better color purity and spectral width when being applied to the display field, and can be used for full-color display.
The object of the invention is achieved by:
a multicolor LED for illumination and display comprises a blue LED chip and a multicolor luminescent material coated on the surface of the blue LED chip, wherein a metal organic framework carries fluorescent molecules, and the multicolor luminescent material comprises the following components: 96.5-99.98wt% of metal organic framework, 0.01-1.5wt% of 3- (2-benzothiazolyl) -N, N-diethylbenzenamine, 0.005-1wt% of methyl 2- (6-amino-3-imino-3H-xanthen-9-yl) benzoate, and 0.005-1wt% of 9- (2-carboxyphenyl) -2,3,6,7,12,13,16, 17-octahydro-1H, 5H,11H, 15H-xanthene [2,3,4-IJ:5,6,7-I 'J' ] biquinoline-18-ammonium chloride. Wherein the 3- (2-benzothiazolyl) -N, N-diethylbenzenamine generates the maximum absorption in the blue light region of 440-470nm, which is in accordance with the good light-emitting wavelength (450-470nm) of the commercial blue LED chip, the emission is the broad-spectrum green light of 510-550nm, the maximum absorption 520-560nm of the methyl 2- (6-amino-3-imino-3H-xanthene-9-yl) benzoate just overlaps with the maximum absorption, and is excited to emit the yellow green light of 540-580nm, and the light-emitting range is in accordance with the absorption range (550-580nm) of 9- (2-carboxyphenyl) -2,3,6,7,12,13,16, 17-octahydro-1H, 5H,11H, 15H-xanthene [2,3,4-IJ:5,6,7-I 'J' ] biquinoline-18-ammonium chloride The fluorescence molecules emitting light with long wavelength in the system can be effectively excited by the fluorescence molecules emitting light with short wavelength under the excitation of single blue light, so that high quantum efficiency can be ensured when wide-spectrum multicolor output is ensured.
The invention discloses a preparation method of a multicolor LED for illumination and display, which comprises the following two steps:
the first method comprises the following steps:
step one, preparing multicolor luminescent material of metal organic framework loaded fluorescent molecules by in-situ one-step method
Dissolving a polydentate carboxylic acid organic ligand and a metal salt hydrate in a mass ratio of 1:0.2-1:5 in 30-100mL of an organic solvent or a mixed solution of the organic solvent and water, adding 0.5-10mg of 3- (2-benzothiazolyl) -N, N-diethylbenzenamine, 0.2-5mg of methyl 2- (6-amino-3-imino-3H-xanthen-9-yl) benzoate and 0.2-10mg of 9- (2-carboxyphenyl) -2,3,6,7,12,13,16, 17-octahydro-1H, 5H,11H, 15H-xanthene [2,3,4-IJ:5,6,7-I 'J' ] biquinoline-18-ammonium chloride into the mixed solution, adjusting the pH value to 5-7, performing ultrasonic dispersion, filling the reaction solution after ultrasonic treatment into a reaction kettle with a polytetrafluoroethylene lining, reacting at 80-160 ℃ for 10-48h, filtering after the reaction is finished, washing with N, N-dimethylformamide and ethanol, and drying at 30-100 ℃ to obtain the multicolor luminescent material with the metal organic framework loaded with fluorescent molecules;
step two, preparation of multicolor LED
Grinding the multicolor luminescent material of the metal organic framework loaded with the fluorescent molecules prepared in the step one to the particle size of 120-230 meshes, mixing and stirring the multicolor luminescent material with high-transparency organic silica gel according to the mass ratio of 1:2-1:5, defoaming in vacuum, coating the surface of a blue light LED chip, and curing for 0.5-3h at 100 ℃ to obtain the multicolor LED.
The second method comprises the following steps:
step one, preparation of metal organic framework
Dissolving a polydentate carboxylic acid organic ligand and a metal salt hydrate in a mass ratio of 1:0.2-1:5 in 30-100mL of organic solvent or a mixed solution of the organic solvent and water, adjusting the pH value to 5-7, filling the adjusted reaction solution into a reaction kettle with a polytetrafluoroethylene lining, reacting at 80-160 ℃ for 10-48h, filtering after the reaction is finished, washing with N, N-dimethylformamide and ethanol, and drying at 30-100 ℃ to obtain a metal organic framework;
step two, loading fluorescent molecules on metal organic framework
Grinding a metal organic framework to a particle size of 120-230 meshes, preparing a fluorescent molecule mixed solution by 0.5-10mg of 3- (2-benzothiazolyl) -N, N-diethylbenzenamine, 0.2-5mg of 2- (6-amino-3-imino-3H-xanthene-9-yl) methyl benzoate, 0.2-10mg of 9- (2-carboxyphenyl) -2,3,6,7,12,13,16, 17-octahydro-1H, 5H,11H, 15H-xanthene [2,3,4-IJ:5,6,7-I 'J' ] biquinoline-18-ammonium chloride and 1-10mL of N, N-dimethylformamide, adding 10-500mg of the ground metal organic framework into the fluorescent molecule mixed solution, loading by diffusion loading or ion exchange reaction, soaking at 30-90 deg.C for 5-36h, filtering, washing with N, N-dimethylformamide and ethanol to obtain colorless supernatant, and oven drying at 30-100 deg.C to obtain multicolor luminescent material with metal organic frame loaded with fluorescent molecules.
Step three, preparation of multicolor LED
And (3) mixing and stirring the multicolor luminescent material of the metal organic framework loaded with fluorescent molecules prepared in the step two with high-transparency organic silica gel according to the mass ratio of 1:2-1:5, defoaming in vacuum, uniformly coating on the surface of a blue light LED chip, and curing at 100 ℃ for 0.5-3h to obtain the multicolor LED.
In the two preparation methods, the organic ligand of the polydentate carboxylic acid is biphenyl dicarboxylic acid, 5 '- (4-carboxyphenyl) - [1, 1': 3 ', 1 "-triphenyl ] -4, 4" -dicarboxylic acid, 4', 4 "- (phenyl-1, 3, 5-trioxo) -benzoic acid, 2-methyl terephthalic acid, or 1,2,4, 5-tetrakis (4-carboxyphenyl) benzene.
The metal salt hydrate is zinc salt hydrate, such as zinc nitrate hexahydrate, zinc sulfate heptahydrate, zinc acetate dihydrate and the like; zirconium salt hydrates such as zirconyl chloride octahydrate, zirconyl nitrate hydrate, zirconium chloride and the like; indium salt hydrates such as indium trichloride tetrahydrate, indium nitrate hydrate, indium sulfate and the like.
The organic solvent is one or a mixture of more of N, N-dimethylformamide, N-dimethylacetamide, N-diethylformamide, dimethyl sulfoxide, methanol, ethanol, dioxane and acetone.
The pH value is adjusted by using one or more of hydrochloric acid, nitric acid, sulfuric acid, glacial acetic acid and fluoboric acid as acid.
The multicolor LED for illumination and display is connected to a printed circuit board by welding, and the printed circuit board is connected with a radiator by welding and can be applied to white LED illumination.
The multicolor LED for illumination and display is provided with the color filter layers in the light emitting direction, comprises the red light filter layer, the green light filter layer and the blue light filter layer, and can be applied to full-color micro-display.
The invention has the beneficial effects that:
1. three kinds of fluorescent molecules are simultaneously introduced into a metal organic framework, the overlapping degree of absorption spectrum and emission spectrum among the fluorescent molecules is large, and the fluorescent molecules which emit light with short wavelength inside a pore channel can efficiently transfer energy to the fluorescent molecules which emit light with long wavelength while receiving exciting light by virtue of proper distribution distance after entering the pore channel of the same material, so that the efficient output of the whole energy of the multicolor light-emitting material is ensured;
2. on the basis of ensuring that a luminescent material system has higher quantum efficiency (80%), the peak range of the material luminescence spectrum is remarkably widened through the superposition of the luminescence of three fluorescent agents, so that a multicolor LED obtained by combining a multicolor luminescent material and a blue LED can give out white light emission with high color rendering index;
3. the micro light-emitting LED chip has huge market potential with excellent brightness and efficiency, but the current problem of applying the micro light-emitting LED chip to the field of full-color micro display is the batch production of R, G, B three-primary-color micro-LED arrays and the transfer to a substrate, the problem can be well solved by adopting the multi-color LED formed by combining the multi-color light-emitting material and a single blue-light LED, and a full-color micro-display device can be obtained based on the mature technology of the micro blue-light diode and the addition of a color filter layer;
4. the pore structure of the metal organic framework can effectively limit the intramolecular rotation motion of the fluorescent molecule, so that the probability of non-radiative transition is reduced, the luminous efficiency of the fluorescent molecule is improved, the influence of environmental factors on the organic fluorescent molecule can be reduced due to the isolation effect of the pore, and the stability of the organic fluorescent molecule is improved;
4. the multicolor LED based on the metal organic framework has simple preparation process, can flexibly adjust the light-emitting characteristic of the multicolor LED by adjusting the types and the loading content of fluorescent molecules in the metal organic framework according to the result requirement, and has the advantages of flexibility and adjustability.
Drawings
FIG. 1 is an effect diagram of a white light fixture packaged with multi-color LEDs;
fig. 2 is a spectral composition of a multicolor LED.
Detailed Description
Example 1:
step one, preparing multicolor luminescent material of metal organic framework loaded fluorescent molecules by in-situ one-step method
Reacting 5 '- (4-carboxyphenyl) - [1, 1': 300mg of 3 ', 1 ' -triphenyl ] -4,4 ' -dicarboxylic acid and 350mg of zinc nitrate hexahydrate are dissolved in 70mL of a mixed solution of N, N-dimethylformamide and 10mL of water, 1.2mg of 3- (2-benzothiazolyl) -N, N-diethylbenzylamine, 0.5mg of methyl 2- (6-amino-3-imino-3H-xanthen-9-yl) benzoate and 1mg of 9- (2-carboxyphenyl) -2,3,6,7,12,13,16, 17-octahydro-1H, 5H,11H, 15H-xanthene [2,3,4-IJ:5,6,7-I ' J ' ] biquinoline-18-ammonium chloride are added to the above mixed solution, hydrochloric acid is added to adjust the pH to 6.4, performing ultrasonic dispersion, filling the reaction solution after ultrasonic treatment into a reaction kettle with a polytetrafluoroethylene lining, reacting for 36 hours at 100 ℃, filtering after the reaction is finished, washing with N, N-dimethylformamide and ethanol, and drying at 70 ℃ to obtain the multicolor luminescent material of the metal organic framework loaded with fluorescent molecules;
step two, preparation of multicolor LED
Grinding the multicolor luminescent material of the metal organic framework loaded with the fluorescent molecules prepared in the step one to the particle size of 120-170 meshes, mixing and stirring the multicolor luminescent material with high-transparency organic silica gel according to the mass ratio of 1:2, defoaming in vacuum, uniformly coating the mixture on the surface of a blue light LED chip, and curing for 1h at the temperature of 100 ℃ to obtain the multicolor LED.
The multicolor LED can emit wide-spectrum light covering 450-700nm, wherein the quantum efficiency of the multicolor luminescent material of the metal organic framework is more than 80 percent, the multicolor LED can emit white light with the color rendering index of 85, the color temperature of 4500K, the CIE color coordinate of (0.342,0.351), the lumen efficiency of 110lm/W under 20mA driving current, the R9 value of 90, the temperature of 60 ℃ and the temperature of 120A/cm2Under the aging condition, the light attenuation is only 0.17%, the service life is relatively ideal, and the spectrum and the packaged lamp are shown in the attached figure 1 of the specification andfig. 2.
The multicolor LED prepared by combining the minitype light-emitting LED chip with 70 mu m is characterized in that the minitype blue light LED chip is firstly transferred to a glass substrate and is arranged in a dot matrix manner, a multicolor light-emitting material of which a metal organic framework is loaded with fluorescent molecules is coated in the light-emitting direction of the multicolor LED, the multicolor LED based on the metal organic framework is obtained, and a colorful filter layer is arranged on the light-emitting side of the multicolor light-emitting material, and comprises a red light filter layer, a green light filter layer and a blue light filter layer, so that the full color display with high brightness and low power consumption is realized, and the multicolor.
Example 2:
step one, preparation of metal organic framework material
Dissolving 450mg of 1,2,4, 5-tetra (4-carboxyphenyl) benzene and 600mg of indium trichloride tetrahydrate in a mixed solution of 60mL of N, N-dimethylformamide and 10mL of ethanol, adding nitric acid to adjust the pH value to 6, filling the adjusted reaction solution into a reaction kettle with a polytetrafluoroethylene lining, reacting for 24 hours at 160 ℃, filtering after the reaction is finished, washing with N, N-dimethylformamide and ethanol, and drying at 70 ℃ to obtain a metal organic framework material;
step two, loading fluorescent molecules on metal organic framework
Grinding a metal organic framework to a particle size of 140 meshes to 230 meshes, preparing a fluorescent molecule mixed solution by taking 2mg of 3- (2-benzothiazolyl) -N, N-diethylbenzenamine, 1mg of methyl 2- (6-amino-3-imino-3H-xanthen-9-yl) benzoate, 1.5mg of 9- (2-carboxyphenyl) -2,3,6,7,12,13,16, 17-octahydro-1H, 5H,11H, 15H-xanthene [2,3,4-IJ:5,6,7-I 'J' ] biquinoline-18-ammonium chloride and 10mL of N, N-dimethylformamide, adding 100mg of the ground metal organic framework into the fluorescent molecule mixed solution, loading through diffusion loading or ion exchange reaction, soaking at 60 ℃ for 24h, filtering, washing with N, N-dimethylformamide and ethanol until the supernatant is colorless, and drying at 70 ℃ to obtain the multicolor luminescent material with the metal organic framework loaded with fluorescent molecules.
Step three, preparation of multicolor LED
And (3) mixing and stirring the multicolor luminescent material of the metal organic framework loaded with fluorescent molecules prepared in the step two with high-transparency organic silica gel according to the mass ratio of 1:3, defoaming in vacuum, uniformly coating on the surface of a blue light LED chip, and curing for 2 hours at 100 ℃ to obtain the multicolor LED.
The color rendering index of white light emitted by the multicolor LED reaches 89, the color temperature is 4300K, the CIE color coordinate is (0.337,0.359), the lumen efficiency reaches 108lm/W under the drive current of 20mA, and the value of R9 is 92. And the full-color display can be realized by additionally arranging the color filter layer.
Example 3:
step one, preparation of metal organic framework
Dissolving 200mg of 4,4 '- (phenyl-1, 3, 5-trioxo) -benzoic acid and 600mg of 4, 4' - (phenyl-1, 3, 5-trioxo) -benzoic acid in a mixed solution of 90mLN, N-dimethylformamide and 10mL of water, adding nitric acid to adjust the pH value to 6, putting the adjusted reaction solution into a reaction kettle with a polytetrafluoroethylene lining, reacting at 160 ℃ for 24 hours, filtering after the reaction is finished, washing with N, N-dimethylformamide and ethanol, and drying at 70 ℃ to obtain a metal organic framework material;
step two, loading fluorescent molecules on metal organic framework
Grinding a metal organic framework to a particle size of 120-170 meshes, preparing a fluorescent molecule mixed solution from 7mg of 3- (2-benzothiazolyl) -N, N-diethylbenzenamine, 1.2mg of methyl 2- (6-amino-3-imino-3H-xanthen-9-yl) benzoate, 2.5mg of 9- (2-carboxyphenyl) -2,3,6,7,12,13,16, 17-octahydro-1H, 5H,11H, 15H-xanthene [2,3,4-IJ:5,6,7-I 'J' ] biquinoline-18-ammonium chloride and 8mL of N, N-dimethylformamide, adding 200mg of the ground metal organic framework into the fluorescent molecule mixed solution, loading through diffusion loading or ion exchange reaction, soaking at 80 ℃ for 12h, filtering, washing with N, N-dimethylformamide and ethanol until the supernatant is colorless, and drying at 80 ℃ to obtain the multicolor luminescent material with the metal organic framework loaded with fluorescent molecules.
Step three, preparation of multicolor LED
And (3) mixing and stirring the multicolor luminescent material of the metal organic framework loaded with fluorescent molecules prepared in the step two with high-transparency organic silica gel according to the mass ratio of 1:2, defoaming in vacuum, uniformly coating on the surface of a blue light LED chip, and curing for 3 hours at 100 ℃ to obtain the multicolor LED.
The color rendering index of white light emitted by the multicolor LED reaches 86, the color temperature 4452K and the CIE color coordinates are (0.346 and 0.361), the lumen efficiency reaches 120lm/W under 20mA driving current, and the R9 value is 89. And the full-color display can be realized by additionally arranging the color filter layer.
Claims (8)
1. A multi-color LED for illumination and display, characterized by: the LED fluorescent material comprises a blue LED chip and a multicolor luminescent material which is coated on the surface of the blue LED chip and is formed by loading fluorescent molecules on a metal organic framework, wherein the multicolor luminescent material comprises the following components in percentage by mass: 96.5-99.98wt% of metal organic framework, 0.01-1.5wt% of 3- (2-benzothiazolyl) -N, N-diethylbenzenamine, 0.005-1wt% of methyl 2- (6-amino-3-imino-3H-xanthen-9-yl) benzoate, and 0.005-1wt% of 9- (2-carboxyphenyl) -2,3,6,7,12,13,16, 17-octahydro-1H, 5H,11H, 15H-xanthene [2,3,4-IJ:5,6,7-I 'J' ] biquinoline-18-ammonium chloride.
2. A method of manufacturing a multi-color LED for illumination and display according to claim 1,
the method comprises the following steps:
step one, preparing multicolor luminescent material of metal organic framework loaded fluorescent molecules by in-situ one-step method
Dissolving a polydentate carboxylic acid organic ligand and a metal salt hydrate in a mass ratio of 1:0.2-1:5 in 30-100mL of an organic solvent or a mixed solution of the organic solvent and water, adding 0.5-10mg of 3- (2-benzothiazolyl) -N, N-diethylbenzenamine, 0.2-5mg of methyl 2- (6-amino-3-imino-3H-xanthen-9-yl) benzoate and 0.2-10mg of 9- (2-carboxyphenyl) -2,3,6,7,12,13,16, 17-octahydro-1H, 5H,11H, 15H-xanthene [2,3,4-IJ:5,6,7-I 'J' ] biquinoline-18-ammonium chloride into the mixed solution, adjusting the pH value to 5-7, performing ultrasonic dispersion, filling the reaction solution after ultrasonic treatment into a reaction kettle with a polytetrafluoroethylene lining, reacting at 80-160 ℃ for 10-48h, filtering after the reaction is finished, washing with N, N-dimethylformamide and ethanol, and drying at 30-100 ℃ to obtain the multicolor luminescent material with the metal organic framework loaded with fluorescent molecules;
step two, preparation of multicolor LED
Grinding the multicolor luminescent material of the metal organic framework loaded with fluorescent molecules prepared in the step one to the particle size of 120-230 meshes, mixing and stirring the multicolor luminescent material with high-transparency organic silica gel according to the mass ratio of 1:2-1:5, defoaming in vacuum, uniformly coating the mixture on the surface of a blue light LED chip, and curing for 0.5-3h at 100 ℃ to obtain a multicolor LED;
alternatively, the method comprises the following steps:
step one, preparation of metal organic framework material
Dissolving a polydentate carboxylic acid organic ligand and a metal salt hydrate in a mass ratio of 1:0.2-1:5 in 30-100mL of an organic solvent or a mixed solution of the organic solvent and water, adjusting the pH value to 5-7, filling the adjusted reaction solution into a reaction kettle with a polytetrafluoroethylene lining, reacting at 80-160 ℃ for 10-48h, filtering after the reaction is finished, washing with N, N-dimethylformamide and ethanol, and drying at 30-100 ℃ to obtain a metal organic framework material;
step two, loading fluorescent molecules on metal organic framework
Grinding a metal organic framework material to a particle size of 120-230 meshes, preparing a fluorescent molecule mixed solution by 0.5-10mg of 3- (2-benzothiazolyl) -N, N-diethylbenzenamine, 0.2-5mg of 2- (6-amino-3-imino-3H-xanthen-9-yl) methyl benzoate, 0.2-10mg of 9- (2-carboxyphenyl) -2,3,6,7,12,13,16, 17-octahydro-1H, 5H,11H, 15H-xanthene [2,3,4-IJ:5,6,7-I 'J' ] biquinoline-18-ammonium chloride and 1-10mL of N, N-dimethylformamide, adding 10-500mg of the ground metal organic framework into the fluorescent molecule mixed solution, loading by diffusion loading or ion exchange reaction, soaking at 30-90 deg.C for 5-36h, filtering, washing with N, N-dimethylformamide and ethanol to obtain colorless supernatant, and oven drying at 30-100 deg.C to obtain multicolor luminescent material with metal organic frame loaded with fluorescent molecules;
step three, preparation of multicolor LED
And (3) mixing and stirring the multicolor luminescent material of the metal organic framework loaded with fluorescent molecules prepared in the step two with high-transparency organic silica gel according to the mass ratio of 1:2-1:5, defoaming in vacuum, uniformly coating the surface of the blue LED chip, and curing at 100 ℃ for 0.5-3h to obtain the multicolor LED.
3. The method of making a multi-color LED for illumination and display of claim 2, wherein: the polydentate carboxylic acid organic ligand is biphenyl dicarboxylic acid, 5 '- (4-carboxyphenyl) - [1, 1': 3 ', 1 "-triphenyl ] -4, 4" -dicarboxylic acid, 4', 4 "- (phenyl-1, 3, 5-trioxo) -benzoic acid, 2-methyl terephthalic acid, or 1,2,4, 5-tetrakis (4-carboxyphenyl) benzene.
4. The method of making a multi-color LED for illumination and display of claim 2, wherein: the metal salt hydrate is zinc salt hydrate, zirconium salt hydrate or indium salt hydrate.
5. The method of making a multi-color LED for illumination and display of claim 2, wherein: the organic solvent is one or a mixture of more of N, N-dimethylformamide, N-dimethylacetamide, N-diethylformamide, dimethyl sulfoxide, methanol, ethanol, dioxane and acetone.
6. The method of making a multi-color LED for illumination and display of claim 2, wherein: the pH value is adjusted to 5-7, and the acid is one or a mixture of more of hydrochloric acid, nitric acid, sulfuric acid, glacial acetic acid and fluoboric acid.
7. Use of a multicolored LED for illumination and display purposes, characterized in that the multicolored LED for illumination and display purposes as claimed in claim 1 is connected by soldering to a printed circuit board, which is provided with a heat sink for white LED illumination.
8. Use of a multicolored LED for illumination and display purposes, characterized in that a colour filter layer, comprising a red filter layer, a green filter layer and a blue filter layer, is produced in the light exit direction of a multicolored LED for illumination and display purposes according to claim 1 for the full colour display area.
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| FR2991325B1 (en) * | 2012-05-31 | 2015-01-16 | Centre Nat Rech Scient | IMPROVED INORGANIC ORGANIC HYBRID SOLID WITH MODIFIED EXTERNAL SURFACE |
| CN103740361B (en) * | 2013-12-24 | 2015-04-15 | 浙江大学 | Dye/metal-organic framework composite material for white light emission and preparation method thereof |
| EP3081616B1 (en) * | 2015-04-17 | 2018-06-06 | Universidad de Castilla La Mancha | White light emitting zirconium-based mofs |
| CN105419785B (en) * | 2015-12-15 | 2017-06-16 | 浙江大学 | Multi-photon polarization laser material being combined based on metal organic frame host and guest build and preparation method thereof |
| CN105694849A (en) * | 2016-02-26 | 2016-06-22 | 浙江大学 | Rare-earth-free fluorescent powder for white light LED and preparation method of rare-earth-free fluorescent powder |
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