CN101759946A - High-performance quantum dot-polymer fluorescent nano composite material and preparation method thereof - Google Patents
High-performance quantum dot-polymer fluorescent nano composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-performance quantum dot-polymer fluorescent nano composite material and a preparation method thereof. The high-performance quantum dot-polymer fluorescent nano composite material comprises polymer and quantum dot which has fluorescent property and is hybridized by silicon dioxide. The method comprises the following steps of: firstly, dissolving 1g of polymer by using a solvent or heating 1g of polymer into a molten state, then adding 0.0002-0.08g of quantum dot which has the particle diameter of 5-30 nanometers, is not modified or is modified by using silane coupling agent and is hybridized by the silicon dioxide and removing the solvent or cooling naturally after stirring for 2min-24hr to obtain the quantum dot-polymer nano composite material. The nano composite material has very strong photoinduced fluorescent property, and the mechanical property of the nano composite material is also enhanced greatly in comparison with that of a corresponding straight polymer. The high-performance quantum dot-polymer fluorescent nano composite material has simple preparation and is suitable for mass production. The invention has very good application prospect in the aspects of preparing an optical device and an optical material, replacing a traditional polymer material and the like.
Description
Technical field
What the present invention relates to is inorganic-polymer nanocomposites field, specifically is a kind of high-performance quantum dot point-polymer fluorescent nano composite material and preparation method thereof
Background technology
Quantum dot is because its unique size relies on luminescent properties, and wide excitation peak and narrow characteristics such as emission peak are at biomarker, optics, and aspects such as solar cell have obtained using widely.But the surface of quantum dot is very fragile in use destroyed easily and cause losing luminescent properties, with quantum dot and polymkeric substance is compound not only can keep the characteristic of quantum dot but also can have good processing properties and mechanical property (J.Mater.Chem., 2008,18,214-220; J.Am.Chem.Soc.2007,129,12828-12833; Langmuir2007,23,850-854).Current compound existing more report about quantum dot and polymkeric substance, but these reports all lay particular emphasis on quantum dot and the polymkeric substance luminescent properties after compound, for compound back quantum dot to the influence of polymkeric substance mechanical property do not appear in the newspapers so far (Chem.Mater.2004,16,1240-1243; Chem.Mater.2007,19,2930-2936; Macromolecules 2002,35,8400-8404).Undoubtedly, the mechanical property of matrix material is very important for its practical application.Because the size of quantum dot is less, itself is exactly a kind of good inorganic nano additive, obtain a kind of high-performance quantum dot point-polymer fluorescent nano composite material that had not only had strong mechanical performance but also had luminescent properties after being expected to add in the polymkeric substance.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of high-performance quantum dot point-polymer fluorescent nano composite material and preparation method thereof is provided, this quantum dot-polymer nanocomposites not only has strong mechanical performance but also have excellent luminescent properties.
High-performance quantum dot point-polymer fluorescent nano composite material is made up of polymkeric substance and the quantum dot with SiO 2 hybrid of fluorescence property.Its described quantum dot is Cadmium Sulfide, cadmium selenide, cadmium telluride, zinc sulphide, zinc selenide, zinc telluridse or lead sulfide.Its described polymkeric substance is polymethylmethacrylate, poly hydroxy ethyl acrylate, polyvinyl alcohol, polystyrene, polyacrylamide, nylon 6, nylon 66, NYLON610, polyethylene, polypropylene or polyethylene terephthalate.
The preparation method of high-performance quantum dot point-polymer fluorescent nano composite material is:
Earlier maybe will be heated to molten state with dissolution with solvents to the 1g polymkeric substance, add 0.0002～0.08g particle diameter again and be the quantum dot of SiO 2 hybrid unmodified or that modify with silane coupling agent of 5～30 nanometers, after stirring 2min～24hr, remove and desolvate or naturally cooling, obtain quantum dot-polymer nanocomposites.
Described silane coupling agent is a 3-sulfydryl propyl trimethoxy silicane, 3-sulfydryl propyl-triethoxysilicane, the 3-aminopropyl trimethoxysilane, the 3-aminopropyl triethoxysilane, the octadecyl trichlorosilane, the octadecyl Trimethoxy silane, octadecyltriethoxy silane, the hexadecyl Trimethoxy silane, the hexadecyl triethoxyl silane, propyl trimethoxy silicane, propyl-triethoxysilicane, the octyl group Trimethoxy silane, octyltri-ethoxysilane or methyl-prop diluted acid-3-(trimethoxy is silica-based) propyl ester.The quantum dot of SiO 2 hybrid its described unmodified or that modify with silane coupling agent and the mass ratio of polymkeric substance are 0.05～4: 100.
Prepared quantum dot-the polymer nanocomposites of the present invention has been tested its absorption and through performance with ultraviolet spectrometer, tested its luminescent properties with fluorescence spectrophotometer, tested the dispersiveness of quantum dot in polymkeric substance with transmission electron microscope, mechanical property has been tested with universal testing machine.The result shows that resulting quantum dot-polymer nanocomposites has excellent luminescent properties and mechanical property.Compare with corresponding straight polymer, the quantum dot of the SiO 2 hybrid of interpolation is to the almost not influence of the transparency of polymkeric substance, and tensile break strength and Young's modulus all improve a lot, and elongation at break does not significantly reduce even increases to some extent.This strong mechanical performance and quantum dot-polymer nanocomposites that can be luminous are at display material, there is good application prospects aspect such as luminescent device and anti-fake material, because its preparation method is simple, aspect alternative traditional polymer materials very big potentiality are being arranged also in addition.
Description of drawings
Fig. 1 is the transmission electron microscope figure that adds gained film behind the cadmium telluride quantum dot of SiO 2 hybrid that particle diameter that methyl-prop diluted acid-3-(trimethoxy is silica-based) propyl ester of 8wt% modifies is 12 nanometers in the polymethylmethacrylate.
Fig. 2 is that to add content in the polystyrene be 0wt%, and the particle diameter that the propyl-triethoxysilicane of 0.15wt% or 0.5wt% is modified is the stress-strain curve that test obtains behind the CdSe quantum dots of SiO 2 hybrid of 20 nanometers.
Fig. 3 is that to add content in the polyvinyl alcohol be 0wt%, and the particle diameter of 0.25wt% or 0.5wt% unmodified is the stress-strain curve that test obtains behind the cadmium telluride quantum dot of SiO 2 hybrid of 8 nanometers.
Fig. 4 is that to add content in the polymethylmethacrylate be 0.1wt%, and 0.2wt%, the particle diameter that 0.5wt% or 1.0wt% octadecyl trichlorosilane are modified are the fluorescence spectrum figure that test obtains behind the CdSe quantum dots of SiO 2 hybrid of 13 nanometers.
Embodiment
The patent that the quantum dot of the SiO 2 hybrid of unmodified of the present invention has been applied for reference to us (number of patent application: CN 200910156964.4) preparation.The quantum dot of the SiO 2 hybrid of modifying with silane coupling agent of the present invention prepares as follows:
The quantum dot that in flask, adds the SiO 2 hybrid of 0.1～10g unmodified, 10～100mL dehydrated alcohol, 0.1～30g silane coupling agent, behind 20～60 ℃ of stirring 1～48hr, centrifugation obtains the quantum dot of the SiO 2 hybrid of silane coupling agent modification.
The following examples are to further specify of the present invention, rather than limit the scope of the invention.
Embodiment 1:
The 1g polymethylmethacrylate with acetic acid ethyl dissolution after, adding the particle diameter that 0.08g modifies with methyl-prop diluted acid-3-(trimethoxy is silica-based) propyl ester again is the cadmium telluride quantum dot of the SiO 2 hybrid of 12 nanometers, after stirring 5hr, naturally place and remove ethyl acetate, obtain cadmium telluride-polymethyl methacrylate nano matrix material.The transmission electron microscope figure of its film as shown in Figure 1, the cadmium telluride quantum dot of the SiO 2 hybrid that methyl-prop diluted acid-3-(trimethoxy is silica-based) propyl ester is modified is uniformly dispersed in poly-methylpropanoic acid methyl esters, high resolution transmission electron microscopy confirms that the crystalline structure of cadmium telluride quantum dot has obtained good maintenance, and therefore the film that obtains not only has the very strong transparency but also have excellent luminescent properties.
Embodiment 2:
The 1g polystyrene is heated to 150 ℃, and adding the particle diameter that 0.005g modifies with propyl-triethoxysilicane again is the CdSe quantum dots of the SiO 2 hybrid of 20 nanometers, stir 1hr after, naturally cooling obtains cadmium selenide-polystyrene nano composite material.Its tensile stress-strain curve as shown in Figure 2, comparing its Young's modulus with pure polystyrene has increased by 42%, elongation at break has increased by 6%.
Embodiment 3:
Embodiment 3 is with embodiment 2, and just the particle diameter that propyl-triethoxysilicane is modified is that the add-on of CdSe quantum dots of the SiO 2 hybrid of 20 nanometers changes 0.0015g into, obtains cadmium selenide-polystyrene nano composite material.Its tensile stress-strain curve as shown in Figure 2, comparing its tensile break strength with pure polystyrene has increased by 11%, Young's modulus has increased by 33%, elongation at break has increased by 12%.
Embodiment 4:
The 1g polyvinyl alcohol with water dissolution after, adding 0.0002g again is the cadmium telluride quantum dot of the SiO 2 hybrid of 8 nanometers with the particle diameter of unmodified, stir 1hr after, remove moisture, obtain cadmium telluride-polyvinyl alcohol nano matrix material.
Embodiment 5:
Embodiment 5 is with embodiment 4, is the particle diameter of unmodified that the amount of cadmium telluride quantum dot of the SiO 2 hybrid of 8 nanometers changes 0.005g into just, obtains cadmium telluride-polyvinyl alcohol nano matrix material.Its tensile stress-strain curve as shown in Figure 3, comparing its tensile break strength with pure polyvinyl alcohol has increased by 16%.
Embodiment 6:
Embodiment 6 is with embodiment 4, is the particle diameter of unmodified that the amount of cadmium telluride quantum dot of the SiO 2 hybrid of 8 nanometers changes 0.0025g into just, obtains cadmium telluride-polyvinyl alcohol nano matrix material.Its tensile stress-strain curve as shown in Figure 3, comparing its tensile break strength with pure polyvinyl alcohol has increased by 22%.
Embodiment 7:
The 1g polymethylmethacrylate is heated to 130 ℃, adding the particle diameter that 0.01g modifies with the octadecyl trichlorosilane again is the CdSe quantum dots of the SiO 2 hybrid of 13 nanometers, after stirring 2hr, naturally cooling obtains cadmium selenide-polymethyl methacrylate nano matrix material.Its fluorogram as shown in Figure 4, luminous very strong, emission peak is sharp-pointed.
Embodiment 8:
Embodiment 8 is with embodiment 7, is the particle diameter of octadecyl trichlorosilane modification that the amount of CdSe quantum dots of the SiO 2 hybrid of 13 nanometers changes 0.005g into just, obtains cadmium selenide-polymethyl methacrylate nano matrix material.Its fluorogram as shown in Figure 4, luminous very strong, emission peak is sharp-pointed.
Embodiment 9:
Embodiment 9 is with embodiment 7, is the particle diameter of octadecyl trichlorosilane modification that the amount of CdSe quantum dots of the SiO 2 hybrid of 13 nanometers changes 0.002g into just, obtains cadmium selenide-polymethyl methacrylate nano matrix material.Its fluorogram as shown in Figure 4, luminous stronger, emission peak is sharp-pointed.
Embodiment 10:
Embodiment 10 is with embodiment 7, is the particle diameter of octadecyl trichlorosilane modification that the amount of CdSe quantum dots of the SiO 2 hybrid of 13 nanometers changes 0.001g into just, obtains cadmium selenide-polymethyl methacrylate nano matrix material.Its fluorogram as shown in Figure 4, luminous stronger, emission peak is sharp-pointed.
Embodiment 11:
Embodiment 11 is with embodiment 7, just the particle diameter that 0.01g octadecyl trichlorosilane is modified is that the particle diameter that the CdSe quantum dots of the SiO 2 hybrid of 13 nanometers changes the modification of 0.0005g octadecyl trichlorosilane into is the cadmiumsulfide quantum dot of the SiO 2 hybrid of 30 nanometers, Heating temperature changes 200 ℃ into, polymethylmethacrylate changes polyethylene terephthalate into, obtains Cadmium Sulfide-polyethylene terephthalate nano composite material.
Embodiment 12:
Embodiment 12 is with embodiment 7, just the particle diameter that 0.01g octadecyl trichlorosilane is modified is that the particle diameter that the CdSe quantum dots of the SiO 2 hybrid of 13 nanometers changes the SiO 2 hybrid of 0.04g 3-aminopropyl triethoxysilane modification into is the zinc selenide quantum dot of 5 nanometers, Heating temperature changes 210 ℃ into, polymethylmethacrylate changes NYLON610 into, obtains zinc selenide-NYLON610 nano composite material.
Embodiment 13:
Embodiment 13 is with embodiment 7, just the particle diameter that the octadecyl trichlorosilane is modified is that the particle diameter that the CdSe quantum dots of the SiO 2 hybrid of 13 nanometers changes the SiO 2 hybrid of octyl group Trimethoxy silane modification into is the zinc telluride quantum dot of 15 nanometers, polymethylmethacrylate changes polystyrene into, obtains zinc telluridse-polystyrene nano composite material.
Claims (5)
1. high-performance quantum dot point-polymer fluorescent nano composite material, the quantum dot that it is characterized in that comprising polymkeric substance He have the SiO 2 hybrid of fluorescence property; Described quantum dot is Cadmium Sulfide, cadmium selenide, cadmium telluride, zinc sulphide, zinc selenide, zinc telluridse or lead sulfide.
2. a kind of high-performance quantum dot point-polymer fluorescent nano composite material according to claim 1 is characterized in that described polymkeric substance is polymethylmethacrylate, poly hydroxy ethyl acrylate, polyvinyl alcohol, polystyrene, polyacrylamide, nylon 6, nylon 66, NYLON610, polyethylene, polypropylene or polyethylene terephthalate.
3. preparation method of high-performance quantum dot point-polymer fluorescent nano composite material according to claim 1, it is characterized in that: maybe will be heated to molten state with dissolution with solvents earlier to the 1g polymkeric substance, add 0.0002～0.08g particle diameter again and be the quantum dot of SiO 2 hybrid unmodified or that modify with silane coupling agent of 5～30 nanometers, after stirring 2min～24hr, remove and desolvate or naturally cooling, obtain quantum dot-polymer nanocomposites.
4. the preparation method of a kind of high-performance quantum dot point-polymer fluorescent nano composite material according to claim 3 is characterized in that described silane coupling agent is a 3-sulfydryl propyl trimethoxy silicane, 3-sulfydryl propyl-triethoxysilicane, the 3-aminopropyl trimethoxysilane, the 3-aminopropyl triethoxysilane, the octadecyl trichlorosilane, the octadecyl Trimethoxy silane, octadecyltriethoxy silane, the hexadecyl Trimethoxy silane, the hexadecyl triethoxyl silane, propyl trimethoxy silicane, propyl-triethoxysilicane, the octyl group Trimethoxy silane, octyltri-ethoxysilane or methyl-prop diluted acid-3-(trimethoxy is silica-based) propyl ester.
5. the preparation method of a kind of high-performance quantum dot point-polymer fluorescent nano composite material according to claim 3, it is characterized in that described unmodified or the SiO 2 hybrid modified with silane coupling agent the quantum dot and the mass ratio of polymkeric substance are 0.05～4: 100.
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