CN102618035A - CdSe quantum dot silicon resin composite material emitting white fluorescence and preparation method thereof - Google Patents
CdSe quantum dot silicon resin composite material emitting white fluorescence and preparation method thereof Download PDFInfo
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- CN102618035A CN102618035A CN2011100281302A CN201110028130A CN102618035A CN 102618035 A CN102618035 A CN 102618035A CN 2011100281302 A CN2011100281302 A CN 2011100281302A CN 201110028130 A CN201110028130 A CN 201110028130A CN 102618035 A CN102618035 A CN 102618035A
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Abstract
The invention relates to a quantum dot silicon composite material emitting white fluorescence, which comprises a silicon resin which is colorless and transparent in a visible light region and a CdSe quantum dot white light mixture uniformly dispersed in the silicon resin, wherein the weight ratio of the CdSe quantum dot white light mixture to the silicon resin which is colorless and transparent in the visible light region in the quantum dot silicon composite material emitting white fluorescence is 1-8:99-92. A preparation method of the composite material comprises the following steps: preparing a CdSe quantum dot white light mixture solution; adding the CdSe quantum dot white light mixture solution with a volume corresponding to the content of a white fluorescent material in the composite material to the silicon resin; uniformly mixing, extracting a solvent; uniformly coating the solvent on a smooth glass sheet; and cure-molding to obtain the quantum dot silicon composite material emitting white fluorescence. The composite material can emit white lights under the excitation of ultraviolet lights, the photoluminescent spectrum is continuous, spectral peaks are smooth, and the peak type is similar to the solar spectrum, so the composite material is suitable for luminescent materials of electro-optical devices and white LED solid illuminating devices.
Description
Invention field
The present invention relates to a kind of quantum dot silicone resin composite material and method for making and purposes, particularly a kind of preparation method and purposes.
Background technology
White light emitting diode (White light emitting diodes; Be called for short WLED); It is a kind of novel solid cold light source;, vibration resistance, shock resistance little, energy-conservation with pollution-free, long lifetime, volume also can reflect the characteristics such as true colors of irradiating object preferably, are regarded as the emerging product that is expected most in the LED industry.Scientific research at present finds that photoaging is not resin foreigner's a sole cause among the WLED, and the Another reason that causes the WLED life-span to reduce is the scattering process of fluorescent material.In the WLED practical application, avoid causing that by the fluorescent material scattering resin aged way mainly is to make phosphor powder layer as far as possible away from led chip.Though but this method can alleviate the negative impact that the fluorescent material scattering of light is caused to a certain extent, can not settle the matter once and for all.Want to address this problem just to need to use and do not produce the fluorescent material of scattering of light.
In recent years, also be applied to white light LED part at the luminous II-VI family semiconductor-quantum-point of visible light wave range as splendid alternative materials.Semiconductor-quantum-point is the zero-dimension nano material, and its size on three dimensions is all close with electron mean free path, has unique discrete energy levels system, and artificial atom therefore is otherwise known as.Because quantum size effect, quantum dot is that example is compared with the conventional fluorescent powder and had following characteristics with CdSe: only need the size of control CdSe, just can obtain the fluorescence that emission wavelength almost covers whole visible light wave range; The blue-ray LED of different emission can excite the CdSe nano material.These character all are that the conventional fluorescent powder can't be realized at all.
Utilize the blue purple LED of InGaN/GaN of Metalorganic chemical vapor deposition method (MOCVD) growth to get into the stage of commercially producing; Thereby be substrate with the blue purple LED of InGaN/GaN; Spin coating green glow and red light quantum point fluorescent material utilize the photoluminescence property of quantum dot to realize that white light parts is a kind of good selection.In recent years, Demir etc. has obtained a series of important successes in this respect.Wherein exciting progress is exactly the realization of the warm light source of white, selects red (613nm), green (555nm), blue (452nm) three look quantum dots to constitute white light.Regulate the component content of three look quantum dots, just can obtain the white light LEDs emmission spectrum, but in spectrum, lack blue green light and the gold-tinted about 580nm about 520nm.
Summary of the invention
The object of the present invention is to provide a kind of CdSe quantum dot silicone resin composite material of launching white fluorescent;
Another object of the present invention is to provide the said preparation method who launches the CdSe quantum dot silicone resin composite material of white fluorescent;
A purpose more of the present invention is to provide said purposes of launching the CdSe quantum dot silicone resin composite material of white fluorescent.
Technical scheme of the present invention is following:
The CdSe quantum dot silicone resin composite material of emission white fluorescent provided by the invention, it is made up of silicone resin and the CdSe quantum dot mixture that is dispersed in this silicone resin; The weight part proportioning of said CdSe quantum dot mixture and said silicone resin is 1~8: 99~92;
Said silicone resin is greater than 85% transparent silicon resin at the visible region transmittance;
Said CdSe quantum dot mixture is made up of the CdSe quantum dot of photoluminescence wavelength 455nm, the CdSe quantum dot of photoluminescence wavelength 490nm, the CdSe quantum dot of photoluminescence wavelength 523nm, the CdSe quantum dot of photoluminescence wavelength 546nm, the CdSe quantum dot of photoluminescence wavelength 575nm and the CdSe quantum dot of photoluminescence wavelength 623nm.CdSe quantum point grain diameter in the said CdSe quantum dot mixture is less than 5nm.
The preparation method who launches the CdSe quantum dot silicone resin composite material of white fluorescent provided by the invention, the gas preparation process is following:
(1) takes by weighing six kinds of CdSe quantum dots of different-grain diameter respectively, and be added to respectively in the normal hexane, obtain the CdSe quantum dot normal hexane clear solution that six kinds of CdSe quantum dot concentration are 0.1mol/L through abundant ultra-sonic dispersion;
Said six kinds of CdSe quantum dot normal hexane clear solutions contain the CdSe quantum dot of photoluminescence wavelength 455nm and a CdSe quantum dot normal hexane clear solution of normal hexane respectively; Contain the CdSe quantum dot of photoluminescence wavelength 490nm and the 2nd CdSe quantum dot normal hexane clear solution of normal hexane; Contain the CdSe quantum dot of photoluminescence wavelength 523nm and the 3rd CdSe quantum dot normal hexane clear solution of normal hexane; The CdSe quantum dot and normal hexane the 4th CdSe quantum dot normal hexane clear solution that contain photoluminescence wavelength 546nm; Contain photoluminescence wavelength 575nm CdSe quantum dot and normal hexane the 5th CdSe quantum dot normal hexane clear solution and contain CdSe quantum dot and normal hexane the 6th CdSe quantum dot normal hexane clear solution of photoluminescence wavelength 623nm;
(2) with a said CdSe quantum dot normal hexane clear solution, the 2nd CdSe quantum dot normal hexane clear solution, the 3rd CdSe quantum dot normal hexane clear solution, the 4th CdSe quantum dot normal hexane clear solution, the 5th CdSe quantum dot normal hexane clear solution and the 6th CdSe quantum dot normal hexane clear solution be 1: 1: 1~2: 2~8: 2~8 ratio thorough mixing by volume, obtain containing the CdSe quantum dot mixture normal hexane clear solution of six kinds of CdSe quantum dots;
(3) the CdSe quantum dot mixture normal hexane clear solution and the silicone resin that contain six kinds of CdSe quantum dots that step (2) are obtained mix; Extract normal hexane solvent wherein out; Afterwards it evenly is coated on the smooth glass sheet; 150 ℃ solidify 1h, obtain launching the CdSe quantum dot silicone resin composite material of white fluorescent, and this CdSe quantum dot mixture and the weight part proportioning of silicone resin that can launch in the CdSe quantum dot silicone resin composite material of white fluorescent is 1~8: 99~92; Described silicone resin is greater than 85% silicone resin at the visible region transmittance.CdSe quantum point grain diameter in the described CdSe quantum dot mixture is all less than 5nm.
The application of CdSe quantum dot silicone resin composite material on the luminescent material that is used for electro-optical device, white light LEDs solid state lighting device of launching white fluorescent provided by the invention.
Compared with prior art, the present invention has following advantage:
1, the present invention matches colors through the CdSe quantum dot that adopts six kinds of emission wavelengths and obtains the fluorescent material of emission white light, has realized the photic white light of material.
2, the quantum dot silicone resin composite material of the emission white fluorescent of the inventive method preparation has higher thermotolerance, does not go bad because of the rising of envrionment temperature; Photoluminescence spectra is continuous under the exciting of UV-light, and the spectrum peak is level and smooth, approaches solar spectrum.
3, the quantum dot silicone resin composite material of the emission white fluorescent of the inventive method preparation only contains CdSe quantum dot and silicone resin, and other doping is not arranged.
4, the CdSe quantum dot uncoated in the quantum dot silicone resin composite material of the emission white fluorescent of the inventive method preparation.
5, the present invention preparation method of launching the quantum dot silicone resin composite material of white fluorescent prepares simply, and Production Time is short, favorable repeatability, and toxicity is little, and cost is low.
6, the starting material of the inventive method are easy to buy from market or processing obtains, and particularly control emission wavelength through regulating CdSe quantum dot size, have good color developing, do not need carefully balanced various fluorescence.
7, the quantum dot silicone resin composite material of emission white fluorescent of the present invention can be used for white light LEDs and replaces fluorescent material, can avoid the caused scattering of light effect of conventional fluorescent powder, prolongs the work-ing life of white light LEDs; Improve the homogeneity of space colourity simultaneously.
Embodiment:
Further describe the present invention below in conjunction with embodiment (but being not limited to the embodiment that lifts):
Embodiment 1
(1) takes by weighing the CdSe quantum dot of six kinds of different-grain diameters of 0.76g (4mmol) respectively; And add respectively in the 40ml normal hexane; Ultra-sonic dispersion fully disperseed it in 15 minutes, obtained the CdSe quantum dot normal hexane clear solution that six kinds of CdSe quantum dot concentration are 0.1mol/L; These six kinds of CdSe quantum dot normal hexane clear solution emission different wavelengths of light;
CdSe quantum point grain diameter in above-mentioned six kinds of solution is respectively: 2.31 ± 0.04nm, 2.92 ± 0.04nm, 3.35 ± 0.12nm, 3.68 ± 0.06nm, 4.23 ± 0.12nm, 4.74 ± 0.23nm; In fact the CdSe quantum point grain diameter is as long as all can less than 5nm.
(2) measure 10ml CdSe quantum dot normal hexane clear solution a respectively; 10ml CdSe quantum dot normal hexane clear solution b; 10ml CdSe quantum dot normal hexane clear solution c, 20mlCdSe quantum dot normal hexane clear solution d, 20ml CdSe quantum dot normal hexane clear solution e; With 20ml CdSe quantum dot normal hexane clear solution f, above-mentioned six kinds of CdSe quantum dot normal hexane clear solution thorough mixing are obtained launching the CdSe quantum spot white light mixture solution of white light;
(3) after CdSe quantum spot white light mixture solution and the 38.2g silicone resin (Dow Corning OE-6550) of getting the emission white light of preparation in the 20ml step (2) mixes; Extract normal hexane solvent wherein out; Afterwards it evenly is coated on the smooth glass sheet; 150 ℃ solidify 1h, can obtain launching the CdSe quantum dot silicone resin composite material of white fluorescent, and the CdSe quantum spot white light mixture wherein and the weight part proportioning of silicone resin are 1: 99; Silicone resin is greater than 85% silicone resin at the visible region transmittance.The matrix material of present embodiment preparation excites under the 365nm uv lamp can launch white fluorescent.
Embodiment 2
(1) takes by weighing the CdSe quantum dot of six kinds of different-grain diameters of 0.76g (4mmol) respectively; And add respectively in the 40ml normal hexane; Ultra-sonic dispersion fully disperseed it in 15 minutes, obtained the CdSe quantum dot normal hexane clear solution that six kinds of CdSe quantum dot concentration are 0.1mol/L; These six kinds of CdSe quantum dot normal hexane clear solution emission different wavelengths of light;
CdSe quantum point grain diameter in above-mentioned six kinds of solution is respectively: 2.31 ± 0.04nm, 2.92 ± 0.04nm, 3.35 ± 0.12nm, 3.68 ± 0.06nm, 4.23 ± 0.12nm, 4.74 ± 0.23nm; In fact the CdSe quantum point grain diameter is as long as all can less than 5nm.
(2) measure 10ml CdSe quantum dot normal hexane clear solution a respectively; 10ml CdSe quantum dot normal hexane clear solution b; 20ml CdSe quantum dot normal hexane clear solution c, 20mlCdSe quantum dot normal hexane clear solution d, 40ml CdSe quantum dot normal hexane clear solution e; With 40ml CdSe quantum dot normal hexane clear solution f, above-mentioned six kinds of CdSe quantum dot normal hexane clear solution thorough mixing are obtained launching the CdSe quantum spot white light mixture solution of white light;
(3) after CdSe quantum spot white light mixture solution and the 7.6g silicone resin (Dow Corning OE-6550) of getting the emission white light of preparation in the 20ml step (2) mixes; Extract normal hexane solvent wherein out; Afterwards it evenly is coated on the smooth glass sheet; 150 ℃ solidify 1h, can obtain launching the CdSe quantum dot silicone resin composite material of white fluorescent, and the CdSe quantum spot white light mixture wherein and the weight part proportioning of silicone resin are 5: 95; Silicone resin is greater than 85% silicone resin at the visible region transmittance.The matrix material of present embodiment preparation excites under the 365nm uv lamp can launch white fluorescent.
Embodiment 3
(1) takes by weighing the CdSe quantum dot of six kinds of different-grain diameters of 0.76g (4mmol) respectively; And add respectively in the 40ml normal hexane; Ultra-sonic dispersion fully disperseed it in 15 minutes, obtained the CdSe quantum dot normal hexane clear solution that six kinds of CdSe quantum dot concentration are 0.1mol/L; These six kinds of CdSe quantum dot normal hexane clear solution emission different wavelengths of light;
CdSe quantum point grain diameter in above-mentioned six kinds of solution is respectively: 2.31 ± 0.04nm, 2.92 ± 0.04nm, 3.35 ± 0.12nm, 3.68 ± 0.06nm, 4.23 ± 0.12nm, 4.74 ± 0.23nm; In fact the CdSe quantum point grain diameter is as long as all can less than 5nm.
(2) measure 10ml CdSe quantum dot normal hexane clear solution a respectively; 10ml CdSe quantum dot normal hexane clear solution b; 20ml CdSe quantum dot normal hexane clear solution c, 40mlCdSe quantum dot normal hexane clear solution d, 80ml CdSe quantum dot normal hexane clear solution e; With 80ml CdSe quantum dot normal hexane clear solution f, above-mentioned six kinds of CdSe quantum dot normal hexane clear solution thorough mixing are obtained launching the CdSe quantum spot white light mixture solution of white light;
(3) after CdSe quantum spot white light mixture solution and the 4.5g silicone resin (Dow Corning OE-6550) of getting the emission white light of preparation in the 20ml step (2) mixes; Extract normal hexane solvent wherein out; Afterwards it evenly is coated on the smooth glass sheet; 150 ℃ solidify 1h, can obtain launching the CdSe quantum dot silicone resin composite material of white fluorescent, and the CdSe quantum spot white light mixture wherein and the weight part proportioning of silicone resin are 8: 92; Silicone resin is greater than 85% silicone resin at the visible region transmittance.The matrix material of present embodiment preparation excites under the 365nm uv lamp can launch white fluorescent.
Claims (5)
1. the CdSe quantum dot silicone resin composite material that can launch white fluorescent, it is made up of silicone resin and the CdSe quantum dot mixture that is dispersed in this silicone resin; The weight part proportioning of said CdSe quantum dot mixture and said silicone resin is 1~8: 99~92;
Said silicone resin is greater than 85% transparent silicon resin at the visible region transmittance;
Said CdSe quantum dot mixture is made up of the CdSe quantum dot of photoluminescence wavelength 455nm, the CdSe quantum dot of photoluminescence wavelength 490nm, the CdSe quantum dot of photoluminescence wavelength 523nm, the CdSe quantum dot of photoluminescence wavelength 546nm, the CdSe quantum dot of photoluminescence wavelength 575nm and the CdSe quantum dot of photoluminescence wavelength 623nm.
2. by the CdSe quantum dot silicone resin composite material of the described emission white fluorescent of claim 1, it is characterized in that the CdSe quantum point grain diameter in the said CdSe quantum dot mixture is less than 5nm.
3. the preparation method of the CdSe quantum dot silicone resin composite material of the described emission white fluorescent of claim 1 may further comprise the steps:
(1) takes by weighing six kinds of CdSe quantum dots of different-grain diameter respectively, and be added to respectively in the normal hexane, obtain the CdSe quantum dot normal hexane clear solution that six kinds of CdSe quantum dot concentration are 0.1mol/L through abundant ultra-sonic dispersion;
Said six kinds of CdSe quantum dot normal hexane clear solutions contain the CdSe quantum dot of photoluminescence wavelength 455nm and a CdSe quantum dot normal hexane clear solution of normal hexane respectively; Contain the CdSe quantum dot of photoluminescence wavelength 490nm and the 2nd CdSe quantum dot normal hexane clear solution of normal hexane; Contain the CdSe quantum dot of photoluminescence wavelength 523nm and the 3rd CdSe quantum dot normal hexane clear solution of normal hexane; The CdSe quantum dot and normal hexane the 4th CdSe quantum dot normal hexane clear solution that contain photoluminescence wavelength 546nm; Contain photoluminescence wavelength 575nm CdSe quantum dot and normal hexane the 5th CdSe quantum dot normal hexane clear solution and contain CdSe quantum dot and normal hexane the 6th CdSe quantum dot normal hexane clear solution of photoluminescence wavelength 623nm;
(2) with a said CdSe quantum dot normal hexane clear solution, the 2nd CdSe quantum dot normal hexane clear solution, the 3rd CdSe quantum dot normal hexane clear solution, the 4th CdSe quantum dot normal hexane clear solution, the 5th CdSe quantum dot normal hexane clear solution and the 6th CdSe quantum dot normal hexane clear solution be 1: 1: 1~2: 2~8: 2~8 ratio thorough mixing by volume, obtain containing the CdSe quantum dot mixture normal hexane clear solution of six kinds of CdSe quantum dots;
(3) the CdSe quantum dot mixture normal hexane clear solution and the silicone resin that contain six kinds of CdSe quantum dots that step (2) are obtained mix; Extract normal hexane solvent wherein out; Afterwards it evenly is coated on the smooth glass sheet; 150 ℃ solidify 1h, obtain launching the CdSe quantum dot silicone resin composite material of white fluorescent, and this CdSe quantum dot mixture and the weight part proportioning of silicone resin that can launch in the CdSe quantum dot silicone resin composite material of white fluorescent is 1~8: 99~92; Described silicone resin is greater than 85% silicone resin at the visible region transmittance.
4. by the described preparation method who launches the CdSe quantum dot silicone resin composite material of white fluorescent of claim 3, it is characterized in that the CdSe quantum point grain diameter in the described CdSe quantum dot mixture is all less than 5nm.
5. the described application of CdSe quantum dot silicone resin composite material on the luminescent material that is used for electro-optical device, white light LEDs solid state lighting device of launching white fluorescent of claim 1.
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CN115011329A (en) * | 2022-06-29 | 2022-09-06 | 苏州科技大学 | Ultra-wideband high-brightness green environment-friendly short-wave infrared emission light source material and preparation method and application thereof |
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