CN110951478A - Double-emission fluorescent material, preparation method thereof and application thereof in LED device - Google Patents
Double-emission fluorescent material, preparation method thereof and application thereof in LED device Download PDFInfo
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- CN110951478A CN110951478A CN201911106133.6A CN201911106133A CN110951478A CN 110951478 A CN110951478 A CN 110951478A CN 201911106133 A CN201911106133 A CN 201911106133A CN 110951478 A CN110951478 A CN 110951478A
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- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
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Abstract
The invention discloses a dual-emission fluorescent material, a preparation method thereof and application thereof in an LED device, wherein the dual-emission fluorescent material comprises the following components, by mass, 10-18% of silicon quantum dots and 82-90% of polysiloxane; the preparation method comprises the steps of mixing a silicon source, a chelating agent and deionized water, and carrying out hydrothermal reaction at 180-250 ℃ to obtain the dual-emission fluorescent material. The dual-emission fluorescent material is 2-D polysiloxane inlaid with silicon quantum dots, is dual-emission of blue-green light, and has excellent thermal stability and temperature resistance; the double-emission fluorescent material and an ultraviolet or purple light LED chip are packaged to form a warm white light LED without UV emission, and the LED is an ideal eye-protecting LED light source; or packaging the LED chip with a blue LED chip to form a positive white LED device which can be commercially applied.
Description
Technical Field
The invention relates to the field of luminescent materials, in particular to a dual-emission fluorescent material, a preparation method thereof and application thereof in an LED device.
Background
Light Emitting diodes (abbreviated as LEDs) have become the most promising new generation of Light sources, which utilize solid semiconductor chips as Light Emitting materials, and when a forward voltage is applied across the two terminals, minority carriers injected into the semiconductor are combined with the majority carriers, and excess energy is released in the form of Light, thereby directly converting electrical energy into Light energy. The mainstream of the LED lighting source is a high-brightness white LED, and most of the commercialized white LEDs at present have two wavelengths, namely, a blue light single chip and YAG yellow fluorescent powder are mixed to generate white light; the human eye has strong adaptability to natural light and good visual effect, so that an eye protection LED light source capable of providing the most natural light needs to be found.
The silicon quantum dots are novel silicon nano materials and have wide application prospects in the fields of photoelectrons, catalysis, sensing and the like, however, the silicon quantum dots can achieve higher fluorescence quantum efficiency only when existing in a solvent, and if the solid quantum dots are obtained through post-treatment, the fluorescence can be remarkably reduced or quenched, and the application of the silicon quantum dots in an LED (light-emitting diode) lighting source cannot be achieved. For this reason, silicon quantum dots are assembled into organic or inorganic matrixes to realize solid luminescence, but the problem of thermal/optical stability of the quantum dots cannot be solved, the problem of low fluorescence quantum efficiency also faces, and the application of the quantum dots in LED illumination light sources cannot be met. Therefore, up to now, there has been no report that silicon quantum dots or composite materials thereof are used as light emitting materials for LED illumination light sources.
Disclosure of Invention
In order to overcome the above disadvantages, the present invention provides a dual emission fluorescent material emitting blue-green light.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
the dual-emission fluorescent material comprises, by mass, 10-18% of silicon quantum dots and 82-90% of polysiloxane.
Preferably, the dual emission fluorescent material has a two-dimensional thin film structure in which silicon quantum dots are embedded on polysiloxane.
Preferably, the absorption wavelength range of the dual-emission fluorescent material is 250-500 nm, and the emission wavelength range of the dual-emission fluorescent material is 400-600 nm.
Preferably, the quantum efficiency of the dual-emission fluorescent material reaches 40-85% under the excitation of ultraviolet rays with the wavelength of 350-400 nm.
Preferably, the silicon quantum dots and the polysiloxane are prepared by taking 1- [3- (trimethoxysilyl) propyl ] urea as a silicon source.
The invention also aims to provide a preparation method of the dual-emission fluorescent material.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
the preparation method of the dual-emission fluorescent material comprises the following steps:
and mixing a silicon source, a chelating agent and deionized water, and carrying out hydrothermal reaction at 180-250 ℃ to obtain the dual-emission fluorescent material.
Preferably, the dosage ratio of the silicon source, the chelating agent and the deionized water is (1-2.5) ml to 1g (20-30) ml.
Preferably, the silicon source is 1- [3- (trimethoxysilyl) propyl ] urea, and the chelating agent is sodium citrate and/or a mixture of citric acid and sodium hydroxide.
Preferably, the hydrothermal reaction time is 5-15 h.
The invention also aims to provide an application of the dual-emission fluorescent material or the dual-emission fluorescent material obtained by the preparation method in an LED device.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
the double-emission fluorescent material or the double-emission fluorescent material prepared by the preparation method is applied to an LED device, and the double-emission fluorescent material and organic silicon are uniformly mixed according to the mass ratio of 1: 3-10 and then coated on an LED chip.
Preferably, the coating is coated on an LED chip with the dominant wavelength of 350-420 nm, and the warm white LED device is obtained after curing.
Preferably, the coating is coated on an LED chip with the dominant wavelength of 440-480 nm, and the positive white light LED device is obtained after curing.
Another object of the present invention is to provide a white LED device.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
a white light LED device comprises a dual-emission fluorescent material or the dual-emission fluorescent material obtained by the preparation method.
The invention provides a dual-emission fluorescent material which is 2-D polysiloxane inlaid with silicon quantum dots, and the material is of a sheet structure. The dual-emission fluorescent material is blue-green light dual-emission, and the quantum efficiency is 75%; the absorption wavelength range is 250-500 nm, and the emission wavelength range is 400-600 nm. The dual-emission fluorescent material also has excellent thermal stability and temperature resistance. The dual-emission fluorescent material can be synthesized by only one step, and the method is simple and low in cost. The double-emission fluorescent material and the ultraviolet or purple light LED chip are packaged to form a warm white light LED without UV emission, and the LED is an ideal eye-protecting LED light source; or packaging the LED chip with a blue LED chip to form a positive white LED device which can be commercially applied.
Drawings
FIG. 1 is an HRTEM image of a dual emission fluorescent material of example 1 of the present invention.
FIG. 2 is a graph showing an excitation spectrum of a dual emission fluorescent material according to example 1 of the present invention.
FIG. 3 is a graph showing the emission spectra of the dual emission fluorescent material of example 1 under UV excitation and blue excitation.
FIG. 4 is a graph of emission spectra of the dual emission fluorescent material of example 1 of the present invention at an excitation wavelength of 390nm after being processed at different temperatures.
FIG. 5 is a graph of the emission spectrum of a warm white LED based on UV LED chips in accordance with example 1 of the present invention.
Fig. 6 is a white LED emission spectrum based on a blue LED chip according to embodiment 1 of the present invention.
Detailed Description
The invention is described in detail below with reference to the attached drawing figures:
example 1
(1) Dual-emission fluorescent material
The dual emission fluorescent material 1 of the present example includes 12.5% by mass of silicon quantum dots and 87.5% by mass of polysiloxane.
1.5ml of 1- [3- (trimethoxysilyl) propyl ] urea is weighed, 1.2g of sodium citrate is weighed and added into 28ml of deionized water, and the mixture is fully and uniformly mixed by magnetic stirring for 30min to obtain a mixed solution. And then, transferring the mixed solution into a hydrothermal reaction kettle, and reacting for 5 hours at 200 ℃ to obtain the dual-emission fluorescent material 1. The dual-emission fluorescent material is a two-dimensional film structure with silicon quantum dots embedded in the surface of polysiloxane, and is shown in figure 1. The quantum efficiency of the material is 75% under the excitation of ultraviolet light with the wavelength of 380nm through experiments. In the invention, the two-dimensional film structure of the silicon quantum dot embedded polysiloxane is synthesized by a one-step method, the method is simple and convenient, and the subsequent application of the material is not influenced.
As shown in FIGS. 2 to 3, the absorption wavelength range of the dual emission fluorescent material 1 is 250 to 500nm, and the emission wavelength range thereof is 400 to 600 nm; wherein, under the excitation of UV with the wavelength of 395nm, the main peak of the luminescence of the material is about 480nm (shown as a curve a), and under the excitation of blue light with the wavelength of 460nm, the main peak of the luminescence of the material is about 520nm (shown as a curve b), which shows that the dual-emission fluorescent material has blue-green light dual emission.
After the dual-emission fluorescent material 1 obtained in the embodiment 1 is treated at the temperature of 0-250 ℃ for the same time, emission spectrograms obtained under the excitation of UV with the wavelength of 390nm are sequentially emission peaks of curves a to f from top to bottom, the emission peaks of curves a, b and c are obtained from the material treated at the temperature of 0 ℃, 100 ℃ and 150 ℃, the emission peak intensities of the emission spectrograms are basically the same, the emission peak intensity of the emission spectrograms is slightly reduced after the material is treated at the temperature of 200 ℃, but the intensity value is still very high, the curve e is obtained when the temperature is increased to 225 ℃, the emission peak intensity is reduced, and the emission peak intensity of the curve f obtained from the material treated at the temperature of 250 ℃ is obviously reduced, as shown in fig. 4, which proves that the dual-emission fluorescent material has excellent thermal stability and heat resistance, and the heat resistance temperature can be up to 200 ℃.
(2) Warm white LED device
Weighing the dual-emission fluorescent material 1 and the epoxy resin according to the mass ratio of 1:3, fully stirring and uniformly mixing the materials, coating the mixture on an LED chip with the dominant wavelength of 395nm, and curing to obtain the warm white LED without UV emission. When a layer of dual-emission fluorescent material 1 is coated on an ultraviolet LED chip, as shown in fig. 5, the obtained warm white LED device has a light emission spectrum range of 450 to 650nm and no light emission with a wavelength of 395 nm. The dual-emission fluorescent material can be matched with an ultraviolet or purple light LED chip, and the color temperature measured by the obtained warm white light LED device is about 3000K; because the silicon quantum dots in the dual-emission fluorescent material have a strong UV absorption function, the dual-emission fluorescent material and an ultraviolet or purple LED chip can be packaged to form a warm white LED device without UV emission. The warm white LED device not only avoids the light emission from an ultraviolet or purple LED chip, but also overcomes the harm of blue light, and is an ideal eye-protecting LED light source.
(3) Positive white light LED device
Weighing the dual-emission fluorescent material 1 and the silica gel according to the mass ratio of 1:3.1, fully stirring and uniformly mixing the materials, coating the mixture on an LED chip with the main wavelength of 460nm, and curing to obtain the white light LED. Part of the blue light emitted by the LED chip is absorbed by the dual-emission fluorescent material 1, and the other part of the blue light is mixed with the green light with the wavelength of about 520nm emitted by the dual-emission fluorescent material 1 to obtain white light, and fig. 6 shows that the light-emitting spectrum range of the positive white light LED device is 420-650 nm. The positive white light LED device packaged by the dual-emission fluorescent material and the blue light LED chip has the color coordinates of (0.332,0.334), the color rendering index of 82 and the color temperature of 6500K, can replace YAG (yttrium aluminum garnet): Ce yellow fluorescent powder, and achieves the index of commercial application.
Example 2
The dual emission fluorescent material 2 of the present example includes 10% by mass of silicon quantum dots and 90% by mass of polysiloxane.
1.1ml of 1- [3- (trimethoxysilyl) propyl ] urea is measured, 1.2g of sodium citrate is measured and added into 25ml of deionized water, and the mixture is fully and uniformly mixed by magnetic stirring for 30min to obtain a mixed solution. And then, transferring the mixed solution into a hydrothermal reaction kettle, and reacting for 8 hours at 180 ℃ to obtain the dual-emission fluorescent material 2. The quantum efficiency of the dual emission fluorescent material 2 is measured to be 60% by experiments under the excitation of ultraviolet rays with the wavelength of 370 nm.
The dual-emission fluorescent material 2 and the silica gel in the embodiment are weighed according to the mass ratio of 1:4, fully stirred and uniformly mixed, coated on an LED chip with the main wavelength of 350nm, and cured to obtain the warm white LED without UV emission.
The dual-emission fluorescent material 2 and the epoxy resin are weighed according to the mass ratio of 1:4.5, fully stirred and uniformly mixed, coated on an LED chip with the main wavelength of 440nm, and cured to obtain the white light LED.
Example 3
The dual emission fluorescent material 3 of the present embodiment includes 15% by mass of silicon quantum dots and 85% by mass of polysiloxane.
1.8ml of 1- [3- (trimethoxysilyl) propyl ] urea is measured, 1.2g of a mixture of sodium citrate, citric acid and sodium hydroxide is weighed, added into 30ml of deionized water, and fully and uniformly mixed by magnetic stirring for 30min to obtain a mixed solution. And then, transferring the mixed solution into a hydrothermal reaction kettle, and reacting for 10 hours at 200 ℃ to obtain the dual-emission fluorescent material 3. The quantum efficiency of the dual emission fluorescent material 3 was measured to be 53% by an experiment under the excitation of ultraviolet rays having a wavelength of 360 nm.
The dual-emission fluorescent material 3 and the epoxy resin are weighed according to the mass ratio of 1:5, fully stirred and uniformly mixed, coated on an LED chip with the main wavelength of 380nm, and cured to obtain the warm white LED without UV emission.
The dual-emission fluorescent material 3 and the silica gel are weighed according to the mass ratio of 1:6.3, fully stirred and uniformly mixed, coated on an LED chip with the main wavelength of 450nm, and cured to obtain the white light LED.
Example 4
The dual emission fluorescent material 4 of the present embodiment includes 17% by mass of silicon quantum dots and 83% by mass of polysiloxane.
2.2ml of 1- [3- (trimethoxysilyl) propyl ] urea is measured, 1.2g of a mixture of citric acid and sodium hydroxide is weighed, added into 32ml of deionized water, and fully and uniformly mixed by magnetic stirring for 30min to obtain a mixed solution. And then, transferring the mixed solution into a hydrothermal reaction kettle, and reacting for 13 hours at 220 ℃ to obtain the dual-emission fluorescent material 4. The quantum efficiency of the dual emission fluorescent material 4 was experimentally measured to be 40% under the excitation of ultraviolet rays having a wavelength of 350 nm.
The dual-emission fluorescent material and the silica gel are weighed according to the mass ratio of 1:7, fully stirred and uniformly mixed, coated on an LED chip with the main wavelength of 400nm, and cured to obtain the warm white LED without UV emission.
The dual-emission fluorescent material and the epoxy resin are weighed according to the mass ratio of 1:8.4, fully stirred and uniformly mixed, coated on an LED chip with the main wavelength of 470nm, and cured to obtain the white light LED.
Example 5
The dual emission fluorescent material 5 of the present example includes 18% by mass of silicon quantum dots and 82% by mass of polysiloxane.
2.5ml of 1- [3- (trimethoxysilyl) propyl ] urea is measured, 1.2g of sodium citrate is measured and added into 35ml of deionized water, and the mixture is fully and uniformly mixed by magnetic stirring for 30min to obtain a mixed solution. And then, transferring the mixed solution into a hydrothermal reaction kettle, and reacting for 15 hours at 250 ℃ to obtain the dual-emission fluorescent material 5. The quantum efficiency of the dual emission fluorescent material 5 was found to be 85% by experiment under the excitation of ultraviolet rays having a wavelength of 400 nm.
The dual-emission fluorescent material and the silica gel are weighed according to the mass ratio of 1:9.8, fully stirred and uniformly mixed, coated on an LED chip with the main wavelength of 420nm, and cured to obtain the warm white LED without UV emission.
The dual-emission fluorescent material and the epoxy resin are weighed according to the mass ratio of 1:10, fully stirred and uniformly mixed, coated on an LED chip with the main wavelength of 480nm, and cured to obtain the white light LED.
The transmission electron microscope images of the dual emission fluorescent materials 2 to 5 obtained in the examples 2 to 5 show the thin film structure, and through experimental detection, the material structure, the absorption wavelength range and the emission wavelength range of the dual emission fluorescent materials 2 to 5 obtained in the examples 2 to 5 are basically consistent, and the dual emission fluorescent materials also show excellent temperature resistance and stability. Similarly, the dual-emission fluorescent materials 2-5 can be matched with ultraviolet or purple light LED or blue light LED chips, and can be packaged into warm white LED devices with the color temperature of 3000K or positive white LED devices with the color temperature of 6500K.
The embodiments of the present invention are merely illustrative, and not restrictive, of the scope of the claims, and other substantially equivalent alternatives may occur to those skilled in the art and are within the scope of the present invention.
Claims (13)
1. The dual-emission fluorescent material is characterized by comprising the following components, by mass, 10% -18% of silicon quantum dots and 82% -90% of polysiloxane.
2. The dual emission phosphor of claim 1, having a two-dimensional thin film structure of silicon quantum dots embedded on polysiloxane.
3. The dual-emission fluorescent material of claim 1, wherein the absorption wavelength range of the dual-emission fluorescent material is 250 to 500nm, and the emission wavelength range of the dual-emission fluorescent material is 400 to 600 nm.
4. The dual-emission fluorescent material of claim 1, wherein the quantum efficiency of the dual-emission fluorescent material is 40-85% under the excitation of ultraviolet rays with a wavelength of 350-400 nm.
5. The dual emission fluorescent material of claim 1, wherein the silicon quantum dots and the polysiloxane are prepared by using 1- [3- (trimethoxysilyl) propyl ] urea as a silicon source.
6. The method for preparing a dual emission fluorescent material of any one of claims 1 to 5, comprising the steps of: and mixing a silicon source, a chelating agent and deionized water, and carrying out hydrothermal reaction at 180-250 ℃ to obtain the dual-emission fluorescent material.
7. The method for preparing a dual emission fluorescent material of claim 6, wherein the silicon source, the chelating agent and the deionized water are used in a ratio of (1-2.5) ml to 1g (20-30) ml.
8. The method of claim 6, wherein the silicon source is 1- [3- (trimethoxysilyl) propyl ] urea, and the chelating agent is sodium citrate and/or a mixture of citric acid and sodium hydroxide.
9. The method for preparing a dual emission fluorescent material according to claim 6, wherein the hydrothermal reaction time is 5-15 h.
10. The use of the dual-emission fluorescent material according to any one of claims 1 to 5 or the dual-emission fluorescent material obtained by the preparation method according to any one of claims 6 to 9 in an LED device is characterized in that the dual-emission fluorescent material and organic silicon are uniformly mixed according to a mass ratio of 1:3 to 10 and then coated on an LED chip.
11. The application of the white-light LED device as claimed in claim 10, wherein the white-light LED device is obtained by coating the white-light LED device on an LED chip with a dominant wavelength of 350-420 nm and curing the LED chip.
12. The application of the white light LED device as claimed in claim 10, wherein the white light LED device is obtained by coating the white light LED device on an LED chip with a dominant wavelength of 440-480 nm and curing the LED chip.
13. A white light LED device, characterized in that, the white light LED device comprises the dual-emission fluorescent material of any one of claims 1 to 5 or the dual-emission fluorescent material obtained by the preparation method of any one of claims 6 to 9.
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Application publication date: 20200403 |
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