CN104449698A - Quantum dot/titanium dioxide composite nanodot array having visible-light response and preparation method of quantum dot/titanium dioxide composite nanodot array - Google Patents
Quantum dot/titanium dioxide composite nanodot array having visible-light response and preparation method of quantum dot/titanium dioxide composite nanodot array Download PDFInfo
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Abstract
The invention discloses a quantum dot/titanium dioxide composite nanodot array having visible-light response. On the surface of a substrate, each nanodot in the composite nanodot array is composed of titanium dioxide covered visible-light response quantum dots; the dimension of the composite nanodots ranges from 50-200nm and the density of the composite nanodots ranges from 0.31*10<10> to the power of 10 to 3.01*10<10> to the power of 10 cm<-2>. The preparation process is a one-step method and specifically comprises the following steps: adding the quantum dots while preparing a spin-coating solution, applying the spin-coating solution to the surface of the substrate by use of a sol-gel spin-coating method, and preparing the quantum dot/titanium dioxide composite nanodot array by use of a hydrothermal method or direct annealing; the process is simple and easy to implement. The response and the utilization rate of the composite nanodot array to light can be regulated by regulating the types of the quantum dots and the excitation waveforms of the quantum dots; besides, the hydrophobicity and the hydrophilicity of the surface of the material can be changed by use of visible light different in wavelength, and therefore, later cell detachment is realized and the visible light can be possibly used for cell detachment.
Description
Technical field
The invention belongs to bio-medical film applications, quantum dot/titanium dioxide composite Nano lattice array being specifically related to visible light-responded performance and preparation method thereof.
Background technology
In recent years, due to the limitation of existing Method of Tissue Engineering, cell sheets tissue engineering technique gets more and more people's extensive concerning.Traditional TS obtains cell sheets technical development rapidly by changing temperature, but defect possible there is remaining of toxic chemical substance.The electric charge and the hydrophilic and hydrophobic that change surface can realize Cell detachment.Therefore, utilizing light to change the hydrophilic and hydrophobic of certain material surface, is a kind of method of more excellent acquisition cell sheets.Titanium dioxide is nontoxic, has excellent biocompatibility and chemical stability.The energy gap of anatase titanium dioxide is 3.2 eV, and UV-light can change the hydrophilic and hydrophobic of material surface.So, cell sheets (Yi Hong successfully can be obtained with UV365 nm rayed titanium dioxide nanometer points film, Mengfei Yu, Wenjian Weng, et al. Light-induced cell detachment for cell sheet technology, Biomaterials, 34 (2013) 11-18).But there is certain toxicity to cell and may cause transgenation in UV-light, therefore this method also exists certain defect.Therefore, visible ray desorption cell receives publicity.
Quantum dot has very strong photoluminescence, has the fluorescent characteristic of upper conversion and lower conversion simultaneously, and electronics give body and acceptor property.In quantum dot/titanium dioxide composite Nano lattice array system, the up-conversion fluorescence characteristic of quantum dot and the body/acceptor performance of giving of electronics can improve the visible light-responded property of titanium dioxide, for it provides possibility at visible ray desorption cell field.
Quantum dot is doped with in titanium dioxide nanometer points system, by being separated, quantum dot is wrapped in nano dot, formed visible light-responded biomaterial, composite Nano lattice array structure and the response to visible ray is regulated and controled by changing the kind of quantum dot, excitation wavelength and preparation technology, research cell and material or the interaction between cell and cell, the development for cell sheets desorption, organizational project, cell biological sensor etc. has important meaning.
Summary of the invention
The object of this invention is to provide a kind of visible light-responded quantum dot/titanium dioxide composite Nano lattice array and preparation method thereof.
Of the present invention have visible light-responded quantum dot/titanium dioxide composite Nano lattice array at substrate surface, each nano dot in composite Nano lattice array wraps up visible light-responded quantum dot by titanium dioxide and forms, composite Nano point is of a size of 50 ~ 200 nm, and density is 0.31 × 10
10~ 3.01 × 10
10cm
-2.
Above-mentioned substrate can be silica glass, silicon chip, tantalum piece or medical titanium metal and alloy thereof.
The C quantum dot of described visible light-responded quantum dot to be excitation wavelength be 360 ~ 500 nm, CdS quantum dot, CdSe/ZnS quantum dot or CdS/ZnS quantum dot.
The preparation method with visible light-responded quantum dot/titanium dioxide composite Nano lattice array of the present invention, has following two schemes:
Scheme 1
There is the preparation method of visible light-responded quantum dot/titanium dioxide composite Nano lattice array, comprise the following steps:
1) in 5 ~ 10 mL ethanol, 5 ~ 100 μ L methyl ethyl diketones are added successively, 1 ~ 100 μ L deionized water, 30 ~ 300 μ L concentration are the quantum dot solution of 5 μ g/mL, 100 ~ 1000 μ L tetrabutyl titanates, 0.1 ~ 0.5 g polyvinylpyrrolidone, stirred at ambient temperature, ethanol is settled to 10 mL, obtains precursor sol;
2) get 10 ~ 20 μ L precursor sols and be spin-coated on substrate surface with the speed of 4000 ~ 10000 rpm, then this sample is placed in retort furnace, keep 0.5 ~ 10 h at 400 ~ 700 DEG C, take out, deionized water rinsing, drying; Or after sample room temperature ageing 2 ~ 24 h, put into water heating kettle inner bag, add the deionized water of water heating kettle inner bag volume 60 ~ 95%, at 100 ~ 300 DEG C, keep 1 ~ 20 h, take out, deionized water rinsing, drying.
Scheme 2
There is the preparation method of visible light-responded quantum dot/titanium dioxide composite Nano lattice array, comprise the following steps:
1) in 1 ~ 5 mL ethanol, add 100 ~ 1000 μ L tetrabutyl titanates and 30 ~ 300 μ L concentration is that the quantum dot solution of 5 μ g/mL carries out premix, obtains premixed liquid;
2) in 1 ~ 10 mL ethanol, 5 ~ 100 μ L methyl ethyl diketones are added successively, 1 ~ 100 μ L deionized water, step 1) obtained premixed liquid, 0.1 ~ 0.5 g polyvinylpyrrolidone, stirred at ambient temperature, ethanol is settled to 10 mL, obtains precursor sol;
3) get 10 ~ 20 μ L precursor sols and be spin-coated on substrate surface with the speed of 4000 ~ 10000 rpm, then this sample is placed in retort furnace, 400 ~ 700 DEG C keep 0.5 ~ 10 h, take out, deionized water rinsing, drying; Or after sample room temperature ageing 2 ~ 24 h, put into water heating kettle inner bag, add the deionized water of water heating kettle inner bag volume 60 ~ 95%, at 100 ~ 300 DEG C, keep 1 ~ 20 h, take out, deionized water rinsing, drying.
The present invention improves the responsiveness of titanium dioxide to visible ray by titanium dioxide and quantum dot compound: preparation process of the present invention is single stage method, namely quantum dot is added when preparing spin coating liquid, be spun on substrate surface by sol-gel spin-coating method, quantum dot/titanium dioxide composite Nano lattice array is prepared in hydrothermal method or directly annealing.By kind and the excitation wavelength thereof of quantum point, adjustable composite Nano lattice array is to the responsiveness of light and utilization ratio; And utilize the visible ray of different wave length to change the hydrophilic and hydrophobic of material surface, thus realize the Cell detachment in later stage.Therefore, preparation method of the present invention is simple, is easy to realize, for visible ray desorption cell provides possibility.
Accompanying drawing explanation
Fig. 1 is the SEM figure of titanium dioxide nanometer points array.
The SEM figure of Fig. 2 to be excitation wavelength be C quantum dot/titanium dioxide composite Nano lattice array of 360 nm.
The SEM figure of Fig. 3 to be excitation wavelength be C quantum dot/titanium dioxide composite Nano lattice array of 470 nm.
Fig. 4 is the UV-Vis curve of embodiment 1, embodiment 2 and embodiment 3.
Embodiment
Describe the present invention in detail below in conjunction with embodiment and accompanying drawing, but the present invention is not limited to this.
Embodiment 1
1) in 5 mL ethanol, add 62 μ L methyl ethyl diketones successively, 36 μ L deionized waters, 100 μ L tetrabutyl titanates, 0.4 g polyvinylpyrrolidone, stirred at ambient temperature, ethanol is settled to 10 mL, obtains precursor sol.
2) get the above-mentioned precursor sol of 20 μ L and be spin-coated on Quartz glass surfaces with the speed of 8000 rpm; This sample is placed in retort furnace, takes out after 500 DEG C of maintenance 1 h, deionized water rinsing, drying, obtain titanium dioxide nanometer points array (see figure 1).Its UV-Vis curve is shown in Fig. 4 solid line, absorbs and is limited to 401 nm.
Embodiment 2
1) in 5 mL ethanol, 100 μ L methyl ethyl diketones are added successively, 1 μ L deionized water, the C quantum dot that 36 μ L excitation wavelengths are 360 nm, concentration is 5 μ g/mL, 680 μ L tetrabutyl titanates, 0.1 g polyvinylpyrrolidone, stirred at ambient temperature, ethanol is settled to 10 mL, obtains precursor sol.
2) get the above-mentioned precursor sol of 15 μ L and be spin-coated on silicon metallic substrate surfaces with the speed of 6000 rpm; This sample is placed in retort furnace, and take out after 700 DEG C of maintenance 0.5 h, deionized water rinsing, drying, obtain C quantum dot/titanium dioxide composite Nano lattice array (see Fig. 2).Wherein titanium dioxide nanometer points size range is at 70 ~ 200 nm.The UV-Vis curve of Fig. 4 deshed line to be excitation wavelength be C quantum dot/titanium dioxide composite Nano lattice array of 360 nm, its absorption is limited to 419 nm, does not compare obvious red shift occurs with embodiment 1 containing the titanium dioxide nanometer points array of visible light-responded quantum dot.
Embodiment 3
1) in 5 mL ethanol, 62 μ L methyl ethyl diketones are added successively, 100 μ L deionized waters, the C quantum dot that 30 μ L excitation wavelengths are 470 nm, concentration is 5 μ g/mL, 1000 μ L tetrabutyl titanates, 0.5 g polyvinylpyrrolidone, stirred at ambient temperature, ethanol is settled to 10 mL, obtains precursor sol.
2) get the above-mentioned precursor sol of 10 μ L and be spin-coated on tantalum metallic substrate surfaces with the speed of 10000 rpm; This sample is placed in retort furnace, and take out after 400 DEG C of maintenance 10 h, deionized water rinsing, drying, obtain C quantum dot/titanium dioxide composite Nano lattice array (Fig. 3).Wherein titanium dioxide nanometer points size range is at 70 ~ 200 nm.The UV-Vis curve of Fig. 4 dotted line to be excitation wavelength be C quantum dot/titanium dioxide composite Nano lattice array of 470 nm, its absorption is limited to 431 nm, compares obvious red shift occurs with embodiment 1 titanium dioxide nanometer points array.
Embodiment 4
1) in 5 mL ethanol, 5 μ L methyl ethyl diketones are added successively, 36 μ L deionized waters, the CdS quantum dot that 300 μ L excitation wavelengths are 450 nm, concentration is 5 μ g/mL, 680 μ L tetrabutyl titanates, 0.5 g polyvinylpyrrolidone, stirred at ambient temperature, ethanol is settled to 10 mL, obtains precursor sol.
2) get the above-mentioned precursor sol of 15 μ L and be spin-coated on medical titanium metallic substrate surfaces with the speed of 4000 rpm; After this sample room temperature ageing 6 h, put into the water heating kettle of polytetrafluoroethylliner liner, add the deionized water of inner bag volume 80%, take out after 100 DEG C of maintenance 20 h, obtain CdS quantum dot/titanium dioxide composite Nano lattice array.
Embodiment 5
1) in 3 mL ethanol, add the CdSe/ZnS quantum dot that 36 μ L excitation wavelengths are 500 nm, concentration is 5 μ g/mL and 680 μ L tetrabutyl titanate premixs; In 4 mL ethanol, add 62 μ L methyl ethyl diketones, 36 μ L deionized waters, above-mentioned premixed liquid and 0.4 g polyvinylpyrrolidone successively, stirred at ambient temperature, ethanol is settled to 10 mL, obtains precursor sol.
2) get the above-mentioned precursor sol of 15 μ L and be spin-coated on medical titanium alloy substrate surface with the speed of 8000 rpm; After this sample room temperature ageing 2 h, put into the water heating kettle of polytetrafluoroethylliner liner, add the deionized water of inner bag volume 60%, take out after 120 DEG C of maintenance 2 h, obtain CdSe/ZnS quantum dot/titanium dioxide composite Nano lattice array.
Embodiment 6
1) in 3 mL ethanol, add the CdS/ZnS quantum dot that 72 μ L excitation wavelengths are 500 nm, concentration is 5 μ g/mL and 680 μ L tetrabutyl titanate premixs; In 4mL ethanol, add 62 μ L methyl ethyl diketones, 100 μ L deionized waters, above-mentioned premixed liquid and 0.4 g polyvinylpyrrolidone successively, stirred at ambient temperature, ethanol is settled to 10 mL, obtains precursor sol.
2) get the above-mentioned precursor sol of 15 μ L and be spin-coated on tantalum metallic substrate surfaces with the speed of 8000 rpm; After this sample room temperature ageing 24 h, put into the water heating kettle of polytetrafluoroethylliner liner, add the deionized water of inner bag volume 95%, take out after 300 DEG C of maintenance 3 h, obtain CdS/ZnS quantum dot/titanium dioxide composite Nano lattice array.
Embodiment 7
1) in 5 mL ethanol, 5 μ L methyl ethyl diketones are added successively, 36 μ L deionized waters, the CdS quantum dot that 36 μ L excitation wavelengths are 450 nm, concentration is 5 μ g/mL, 680 μ L tetrabutyl titanates, 0.5 g polyvinylpyrrolidone, stirred at ambient temperature, ethanol is settled to 10 mL, obtains precursor sol.
2) get the above-mentioned precursor sol of 15 μ L and be spin-coated on Quartz glass surfaces with the speed of 8000 rpm; By this sample room temperature ageing 2 h, put into the water heating kettle of polytetrafluoroethylliner liner, add the deionized water of inner bag volume 60%, take out after 120 DEG C of maintenance 2 h, deionized water rinsing, drying, obtain CdS quantum dot/titanium dioxide composite Nano lattice array.
Embodiment 8
1) in 5 mL ethanol, 5 μ L methyl ethyl diketones are added successively, 36 μ L deionized waters, the C quantum dot that 36 μ L excitation wavelengths are 360 nm, concentration is 5 μ g/mL, 680 μ L tetrabutyl titanates, 0.5 g polyvinylpyrrolidone, stirred at ambient temperature, ethanol is settled to 10 mL, obtains precursor sol.
2) get the above-mentioned precursor sol of 15 μ L and be spin-coated on Quartz glass surfaces with the speed of 8000 rpm; By this sample room temperature ageing 24 h, put into the water heating kettle of polytetrafluoroethylliner liner, add the deionized water of inner bag volume 95%, take out after 300 DEG C of maintenance 3 h, deionized water rinsing, drying, obtain C quantum dot/titanium dioxide composite Nano lattice array.
Embodiment 9
1) in 5 mL ethanol, 5 μ L methyl ethyl diketones are added successively, 36 μ L deionized waters, the C quantum dot that 36 μ L excitation wavelengths are 470 nm, concentration is 5 μ g/mL, 680 μ L tetrabutyl titanates, 0.5 g polyvinylpyrrolidone, stirred at ambient temperature, ethanol is settled to 10 mL, obtains precursor sol.
2) get the above-mentioned precursor sol of 15 μ L and be spin-coated on Quartz glass surfaces with the speed of 8000 rpm; By this sample room temperature ageing 24 h, put into the water heating kettle of polytetrafluoroethylliner liner, add the deionized water of inner bag volume 80%, take out after 300 DEG C of maintenance 3 h, deionized water rinsing, drying, obtain C quantum dot/titanium dioxide composite Nano lattice array.
Embodiment 10
In 3 mL ethanol, add that 36 μ L excitation wavelengths are 500 nm, concentration is 5 μ g/mL CdSe/ZnS quantum dot and 680 μ L tetrabutyl titanate premixs; In 4mL ethanol, add 62 μ L methyl ethyl diketones successively, 36 μ L deionized waters, above-mentioned premixed liquid and 0.4 g polyvinylpyrrolidone, stirred at ambient temperature, ethanol is settled to 10 mL, obtains precursor sol.
2) get the above-mentioned precursor sol of 15 μ L and be spin-coated on metal titanium substrate surface with the speed of 8000 rpm; By this sample room temperature ageing 24 h, put into the water heating kettle of polytetrafluoroethylliner liner, add the deionized water of inner bag volume 80%, take out after 120 DEG C of maintenance 3 h, deionized water rinsing, drying, obtain CdS/ZnS quantum dot/titanium dioxide composite Nano lattice array.
Embodiment 11
36 μ L excitation wavelengths are 500 nm, concentration is 5 μ g/mL CdS/ZnS quantum dot and 680 μ L tetrabutyl titanate premixs is added in 3 mL ethanol; In 4mL ethanol, add 62 μ L methyl ethyl diketones (AcAc) successively, 36 μ L deionized waters, above-mentioned premixed liquid and 0.4 g polyvinylpyrrolidone, stirred at ambient temperature, ethanol is settled to 10 mL, obtains precursor sol.
2) get the above-mentioned precursor sol of 15 μ L and be spin-coated on titanium alloy substrate surface with the speed of 8000 rpm; By above-mentioned sample ageing 24 h, put into the water heating kettle of polytetrafluoroethylliner liner, add the deionized water of inner bag volume 80%, take out after 120 DEG C of maintenance 2 h, deionized water rinsing, drying, obtain CdS/ZnS quantum dot/titanium dioxide composite Nano lattice array.
Claims (5)
1. there is visible light-responded quantum dot/titanium dioxide composite Nano lattice array, it is characterized in that this composite Nano lattice array is at substrate surface, each nano dot in composite Nano lattice array wraps up visible light-responded quantum dot by titanium dioxide and forms, composite Nano point is of a size of 50 ~ 200 nm, and density is 0.31 × 10
10~ 3.01 × 10
10cm
-2.
2. according to claim 1 have visible light-responded quantum dot/titanium dioxide composite Nano lattice array, it is characterized in that described substrate is silica glass, silicon chip, tantalum piece or medical titanium metal and alloy thereof.
3. according to claim 1 have visible light-responded quantum dot/titanium dioxide composite Nano lattice array, it is characterized in that described visible light-responded quantum dot to be excitation wavelength be the C quantum dot of 360 ~ 500 nm, CdS quantum dot, CdSe/ZnS quantum dot or CdS/ZnS quantum dot.
4. prepare the method with visible light-responded quantum dot/titanium dioxide composite Nano lattice array according to claim 1, comprise the following steps:
1) in 5 ~ 10 mL ethanol, 5 ~ 100 μ L methyl ethyl diketones are added successively, 1 ~ 100 μ L deionized water, 30 ~ 300 μ L concentration are the quantum dot solution of 5 μ g/mL, 100 ~ 1000 μ L tetrabutyl titanates, 0.1 ~ 0.5 g polyvinylpyrrolidone, stirred at ambient temperature, ethanol is settled to 10 mL, obtains precursor sol;
2) get 10 ~ 20 μ L precursor sols and be spin-coated on substrate surface with the speed of 4000 ~ 10000 rpm, then this sample is placed in retort furnace, keep 0.5 ~ 10 h at 400 ~ 700 DEG C, take out, deionized water rinsing, drying; Or after sample room temperature ageing 2 ~ 24 h, put into water heating kettle inner bag, add the deionized water of water heating kettle inner bag volume 60 ~ 95%, at 100 ~ 300 DEG C, keep 1 ~ 20 h, take out, deionized water rinsing, drying.
5. prepare the method with visible light-responded quantum dot/titanium dioxide composite Nano lattice array according to claim 1, comprise the following steps:
1) in 1 ~ 5 mL ethanol, add 100 ~ 1000 μ L tetrabutyl titanates and 30 ~ 300 μ L concentration is that the quantum dot solution of 5 μ g/mL carries out premix, obtains premixed liquid;
2) in 1 ~ 10 mL ethanol, 5 ~ 100 μ L methyl ethyl diketones are added successively, 1 ~ 100 μ L deionized water, step 1) obtained premixed liquid, 0.1 ~ 0.5 g polyvinylpyrrolidone, stirred at ambient temperature, ethanol is settled to 10 mL, obtains precursor sol;
3) get 10 ~ 20 μ L precursor sols and be spin-coated on substrate surface with the speed of 4000 ~ 10000 rpm, then this sample is placed in retort furnace, 400 ~ 700 DEG C keep 0.5 ~ 10 h, take out, deionized water rinsing, drying; Or after sample room temperature ageing 2 ~ 24 h, put into water heating kettle inner bag, add the deionized water of water heating kettle inner bag volume 60 ~ 95%, at 100 ~ 300 DEG C, keep 1 ~ 20 h, take out, deionized water rinsing, drying.
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| CN107326001A (en) * | 2017-07-26 | 2017-11-07 | 浙江大学 | A kind of photoresponse extracellular matrix laminated film and preparation method thereof |
| CN109762517A (en) * | 2019-02-01 | 2019-05-17 | 浙江大学 | A kind of graphene/titanium dioxide/Si substrate and preparation method thereof of ultraviolet/visible light response |
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| CN106085948A (en) * | 2016-06-16 | 2016-11-09 | 浙江大学 | A kind of method of the cell/cell thin utilizing radiation of visible light to obtain In vitro culture |
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| CN107326001A (en) * | 2017-07-26 | 2017-11-07 | 浙江大学 | A kind of photoresponse extracellular matrix laminated film and preparation method thereof |
| CN107326001B (en) * | 2017-07-26 | 2020-06-16 | 浙江大学 | Photoresponse extracellular matrix composite film and preparation method thereof |
| CN109762517A (en) * | 2019-02-01 | 2019-05-17 | 浙江大学 | A kind of graphene/titanium dioxide/Si substrate and preparation method thereof of ultraviolet/visible light response |
| CN109762517B (en) * | 2019-02-01 | 2020-10-16 | 浙江大学 | Ultraviolet/visible light responsive graphene/titanium dioxide/Si substrate and preparation method thereof |
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