CN101942196A - CdSe quantum dot-containing silicone base composite material and preparation method and application thereof - Google Patents
CdSe quantum dot-containing silicone base composite material and preparation method and application thereof Download PDFInfo
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- CN101942196A CN101942196A CN2009100892188A CN200910089218A CN101942196A CN 101942196 A CN101942196 A CN 101942196A CN 2009100892188 A CN2009100892188 A CN 2009100892188A CN 200910089218 A CN200910089218 A CN 200910089218A CN 101942196 A CN101942196 A CN 101942196A
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Abstract
The invention relates to a CdSe quantum dot-containing silicone base composite material, which is a nanometer composite material consisting of a colorless and transparent silicone and CdSe quantum dot particles uniformly dispersed in the silicone, and the mass ratio of the CdSe quantum dot to the silicone in the composite material is 0.1-10. The preparation method of the composite material comprises the following steps of: dissolving the CdSe quantum dot particles with different particle diameters into an organic solvent to obtain a CdSe quantum dot solution; meanwhile dissolving the silicone into a proper solution to obtain a silicone solution; and then uniformly mixing the corresponding CdSe quantum dot solution with the silicone solution according to the CdSe content in the composite material, vacuumizing to completely volatilize the solvent, then placing into a baking oven, and solidifying and forming to obtain the CdSe quantum dot-containing silicone composite material. The composite material has a certain transparence and favorable luminescent property and is suitable for surface package of photoelectric devices, LED solid lighting device or outdoor neon lights.
Description
Technical field
The present invention relates to a kind of silicone resin nano composite material and method for making and purposes, more particularly, the present invention relates to a kind of silicon resin base composite material and method for making and purposes of the CdSe of containing quantum dot.
Background technology
Photodiode (Light Emitting Diode, i.e. LED) is a kind of be expected to the replace a large amount of at present practical fluorescent tube bulbs or high-performance solid light source of bulb.Tradition LED realizes that the white light technology is a coating fluorescent powder and then encapsulate with Resins, epoxy on led chip, and the scattering of light effect meeting of fluorescent material is quickened the aging of potting resin material and the work-ing life of shortening LED, simultaneously, the restriction of encapsulating structure usually causes the uneven problem of LED space colourity.
Quantum dot (Quantum Dots, i.e. QD) particle diameter is very little, has only several nanometers, can avoid the caused scattering of light effect of conventional fluorescent powder fully, and can produce the monochromatic ray of different colours according to dimensional change, even white light, this is that the conventional fluorescent powder can't be realized at all.Quantum dot is added in the body material, not only can increase the stability of quantum dot, and can avoid fluorescent material to apply uneven and colourity uneven problem in space that cause.
CdSe is important a member of II-VI family semiconductor material, and the energy gap of its body phase is 1.72eV, so the CdSe quantum dot is along with the variation of particle diameter, and its radiative wavelength can cover from indigo plant to red almost whole visible region.And silicone resin is compared with Resins, epoxy, and good fast light thermal ageing can be arranged, and therefore, the silicone resin composite material that preparation contains the CdSe quantum dot has great importance.
Summary of the invention
The silicone resin composite material that the purpose of this invention is to provide a kind of CdSe of containing quantum dot.
Another object of the present invention provides a kind of method for preparing the silicone resin composite material of the above-mentioned CdSe of containing quantum dot.
A further object of the present invention provides a kind of purposes of silicone resin composite material of the above-mentioned CdSe of containing quantum dot.
Technical scheme of the present invention is as follows:
The silicone resin composite material that contains the CdSe quantum dot provided by the invention, it is made up of water white silicone resin and the CdSe quantum dot that is dispersed in this water white silicone resin; Described CdSe quantum dot content is the 0.1-10wt% of described silicone resin composite material.
The particle diameter of described CdSe quantum dot is 1.5-9nm.Described silicone resin is solvent-borne type silicone resin or no-solvent type silicone resin, and its transmittance at visible region is 85%-99.9%.
The preparation method who contains CdSe quantum dot particulate silicone resin composite material provided by the invention, its step is as follows:
1) CdSe quantum dot particle is dissolved in the organic solvent that must contain the CdSe quantum dot in the organic solvent; Described organic solvent is normal hexane, toluene, chloroform or methylene dichloride;
2) water white silicone resin is dissolved in the organic solvent silicon resin solution; Described organic solvent is ethanol, acetone or toluene;
3) then the step 1) gained is contained the organic solvent and the step 2 of CdSe quantum dot) gained silicon resin solution uniform mixing, under the vacuum organic solvent is volatilized fully, place baking oven afterwards, curing molding obtains containing the silicone resin composite material of CdSe quantum dot; Described CdSe quantum dot content is the 0.1-10wt% of described silicone resin composite material.
The particle diameter of described CdSe quantum dot is 1.5-9nm.Described silicone resin is solvent-borne type silicone resin or no-solvent type silicone resin, and its transmittance at visible region is 85%-99.9%.
The silicone resin composite material of the CdSe of containing quantum dot of the present invention is used for the surface encapsulation of photoelectric device, LED solid state lighting device or outdoor neon.
Compared with prior art, the present invention has following advantage:
1, silicone resin composite material that contains the CdSe quantum dot of the present invention and preparation method thereof contains the matrix material of organic/inorganic nano light-emitting particles by preparation, has realized the photoluminescence of material.
2, the CdSe quantum dot particulate silicone resin composite material that contains of method preparation provided by the invention has certain transparency at visible region.
Need not to use fluorescent material when 3, the silicone resin composite material that contains the CdSe quantum dot of method provided by the invention preparation is used for the encapsulation of LED, can avoid the caused scattering of light effect of conventional fluorescent powder, prolong the work-ing life of LED; Improve the homogeneity of space colourity simultaneously; And the present invention preparation to contain the method for silicone resin composite material of CdSe quantum dot simple, easy to operate.
Embodiment
Further describe the present invention below in conjunction with embodiment (but being not limited to illustrated embodiment):
Embodiment 1
With the 0.01g particle diameter be the CdSe quantum dot particles dispersed of 1.5nm in the 2mL normal hexane, must contain the hexane solution of CdSe quantum dot; With the 10g transmittance is that 99% no-solvent type silicone resin (DOW CORNING OE6665) is dissolved in 2mL acetone and gets the silicone resin acetone soln; With behind above-mentioned two kinds of solution uniform mixing, make solvent evaporates complete under the vacuum then, place baking oven then, 150 ℃ solidify the 1h moulding down, obtain containing the silicone resin composite material (its fluorescent emission position is in blue region) of CdSe quantum dot;
The silicone resin composite material that contains the CdSe quantum dot that present embodiment makes, CdSe quantum dot content are the 0.1wt% of the silicone resin composite material that contains the CdSe quantum dot that makes;
The silicone resin composite material of the above-mentioned CdSe of the containing quantum dot before uncured is injected led die can encapsulate near ultraviolet light-emitting diode chip for backlight unit based on InGaN/GaN, 150 ℃ solidify 1h down after, obtain the photodiode that can emit white light.
Embodiment 2
With the 0.05g particle diameter be the CdSe quantum dot particles dispersed of 3nm in 2mL toluene, the chloroformic solution of CdSe quantum dot; With the 10g transmittance is that 85% solvent-borne type silicone resin (promise FJN-9802 is praised in Changzhou) is dissolved in 2mL acetone and gets the silicone resin acetone soln; Then with behind above-mentioned two kinds of solution uniform mixing, film, after solvent evaporates is complete, dry 1h down for 180 ℃, obtain containing the silicone resin composite material (CdSe quantum dot content is the 0.5wt% of the silicone resin composite material that contains the CdSe quantum dot that makes) of CdSe quantum dot, its fluorescent emission position is in blue region.
The silicone resin composite material of the above-mentioned CdSe of the containing quantum dot before uncured is coated on the spectral filter, and ambient cure then adopts this filter plate can realize that UV-light arrives the light source conversion of blue light.
Embodiment 3
With the 0.2g particle diameter be the CdSe quantum dot particles dispersed of 4nm in the 5mL chloroform, the chloroformic solution of CdSe quantum dot; With the 10g transmittance is that 95% non-solvent silicone resin (KE560 of Guangzhou Kang Erjia organosilicon material company limited) is dissolved in 5mL ethanol and gets the silicone resin acetone soln; Then with behind above-mentioned two kinds of solution uniform mixing, after vacuum makes solvent evaporates fully, the ambient cure moulding, obtain containing the silicone resin composite material (CdSe quantum dot content is that the silicone resin composite material that contains the CdSe quantum dot that makes is 2wt%) of CdSe quantum dot, its fluorescent emission position is in the green glow zone.
The silicone resin composite material of the above-mentioned CdSe of the containing quantum dot before uncured is coated on the spectral filter, and ambient cure then adopts this filter plate can realize that UV-light arrives green light source conversion.
Embodiment 4
With the 0.5g particle diameter be the CdSe quantum dot particles dispersed of 5nm in 2mL toluene, the chloroformic solution of CdSe quantum dot; With the 8g transmittance is that 85% solvent-borne type silicone resin (Shenzhen peace product AP-268) is dissolved in 2mL toluene, toluene solution that must silicone resin; Then with behind above-mentioned two kinds of solution uniform mixing, film, after solvent evaporates is complete, 160 ℃ solidify 15min down, obtain containing the silicone resin composite material (CdSe quantum dot content is that the silicone resin composite material that contains the CdSe quantum dot that makes is 5wt%) of CdSe quantum dot, its fluorescent emission position is in the gold-tinted zone.
The silicone resin composite material of the above-mentioned CdSe of the containing quantum dot before uncured evenly is coated on the glass tube walls of ultraviolet neon light, and 160 ℃ solidify 15min down, obtain the gold-tinted neon light.
Embodiment 5
With the 0.5g particle diameter be the CdSe quantum dot particles dispersed of 9nm in the 3mL methylene dichloride, the dichloromethane solution of CdSe quantum dot; With the 5g transmittance is that 90% solvent-borne type silicone resin (Hangzhou Lexus LZ5301) is dissolved in 3mL ethanol, the acetone soln of silicone resin; Then above-mentioned two kinds of solution are mixed, vacuum makes solvent evaporates solidify the 1h curing molding for back fully 150 ℃, obtain containing the silicone resin composite material (CdSe quantum dot content is that the silicone resin composite material that contains the CdSe quantum dot that makes is 10wt%) of CdSe quantum dot, its fluorescent emission position is in the ruddiness zone.
The silicone resin composite material of the above-mentioned CdSe of the containing quantum dot before uncured evenly is coated on the glass tube walls of ultraviolet neon light, and 150 ℃ solidify 1h, obtain the ruddiness neon light.
Claims (7)
1. silicone resin composite material that contains the CdSe quantum dot, it is made up of water white silicone resin and the CdSe quantum dot that is dispersed in this water white silicone resin; Described CdSe quantum dot content is the 0.1-10wt% of described silicone resin composite material.
2. by the described silicone resin composite material that contains the CdSe quantum dot of claim 1, it is characterized in that the particle diameter of described CdSe quantum dot is 1.5-9nm.
3. by the described CdSe quantum dot particulate silicone resin composite material that contains of claim 1, it is characterized in that described silicone resin is solvent-borne type silicone resin or no-solvent type silicone resin, its transmittance at visible region is 85%-99.9%.
4. described preparation method who contains CdSe quantum dot particulate silicone resin composite material of claim 1, its step is as follows:
1) CdSe quantum dot particle is dissolved in the organic solvent that must contain the CdSe quantum dot in the organic solvent; Described organic solvent is normal hexane, toluene, chloroform or methylene dichloride;
2) water white silicone resin is dissolved in the organic solvent silicon resin solution; Described organic solvent is ethanol, acetone or toluene;
3) then the step 1) gained is contained the organic solvent and the step 2 of CdSe quantum dot) gained silicon resin solution uniform mixing, under the vacuum organic solvent is volatilized fully, place baking oven afterwards, curing molding obtains containing the silicone resin composite material of CdSe quantum dot; Described CdSe quantum dot content is the 0.1-10wt% of described silicone resin composite material.
5. by the described preparation method who contains CdSe quantum dot particulate silicone resin composite material of claim 4, it is characterized in that the particle diameter of described CdSe quantum dot is 1.5-9nm.
6. by the described preparation method who contains CdSe quantum dot particulate silicone resin composite material of claim 4, it is characterized in that described silicone resin is solvent-borne type silicone resin or no-solvent type silicone resin, its transmittance at visible region is 85%-99.9%.
7. the silicone resin composite material of the described CdSe of the containing quantum dot of claim 1 is used for the surface encapsulation of photoelectric device, LED solid state lighting device or outdoor neon.
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| CN2009100892188A CN101942196B (en) | 2009-07-09 | 2009-07-09 | CdSe quantum dot-containing silicone base composite material and preparation method and application thereof |
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| CN2009100892188A CN101942196B (en) | 2009-07-09 | 2009-07-09 | CdSe quantum dot-containing silicone base composite material and preparation method and application thereof |
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| CN101942196B CN101942196B (en) | 2012-06-13 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618035A (en) * | 2011-01-26 | 2012-08-01 | 中国科学院理化技术研究所 | CdSe quantum dot silicon resin composite material emitting white fluorescence and preparation method thereof |
| CN103343005A (en) * | 2013-07-13 | 2013-10-09 | 上海洞舟实业有限公司 | High-stability carbon nanometer fluorescence dye |
| US9594203B2 (en) | 2011-07-14 | 2017-03-14 | Lg Innotek Co., Ltd. | Optical member, display device having the same and method for fabricating the same |
| CN108922958A (en) * | 2018-08-01 | 2018-11-30 | 苏州星烁纳米科技有限公司 | White light LEDs and display device |
| CN111273484A (en) * | 2020-03-11 | 2020-06-12 | 宁波东旭成新材料科技有限公司 | Barrier-free diaphragm quantum dot film |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101338187B (en) * | 2007-07-05 | 2011-08-31 | 中国科学院理化技术研究所 | Photoluminescent transparent epoxy nanometer composite material, preparation method and application thereof |
-
2009
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618035A (en) * | 2011-01-26 | 2012-08-01 | 中国科学院理化技术研究所 | CdSe quantum dot silicon resin composite material emitting white fluorescence and preparation method thereof |
| CN102618035B (en) * | 2011-01-26 | 2013-10-16 | 中国科学院理化技术研究所 | CdSe quantum dot silicon resin composite material emitting white fluorescence and preparation method thereof |
| US9594203B2 (en) | 2011-07-14 | 2017-03-14 | Lg Innotek Co., Ltd. | Optical member, display device having the same and method for fabricating the same |
| TWI647522B (en) * | 2011-07-14 | 2019-01-11 | Ｌｇ伊諾特股份有限公司 | Optical member, display device having the same and method for fabricating the same |
| CN103343005A (en) * | 2013-07-13 | 2013-10-09 | 上海洞舟实业有限公司 | High-stability carbon nanometer fluorescence dye |
| CN103343005B (en) * | 2013-07-13 | 2015-05-13 | 上海洞舟实业有限公司 | High-stability carbon nanometer fluorescence dye |
| CN108922958A (en) * | 2018-08-01 | 2018-11-30 | 苏州星烁纳米科技有限公司 | White light LEDs and display device |
| CN108922958B (en) * | 2018-08-01 | 2024-03-15 | 苏州星烁纳米科技有限公司 | White light LED and display device |
| CN111273484A (en) * | 2020-03-11 | 2020-06-12 | 宁波东旭成新材料科技有限公司 | Barrier-free diaphragm quantum dot film |
| CN111273484B (en) * | 2020-03-11 | 2023-08-22 | 宁波东旭成新材料科技有限公司 | Non-resistance diaphragm quantum dot film |
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| CN101942196B (en) | 2012-06-13 |
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