CN101734616B - Method for preparing silicon dioxide hybridized quantum dot by using one-pot method - Google Patents
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Abstract
The invention discloses a method for preparing silicon dioxide hybridized quantum dot by using a one-pot method. The invention comprises the following steps of: adding a non-metal ion source needed for preparing quantum dots to a quantum dot metal ion source containing mercapto stabilizer in a water phase system, getting the precursor liquid of quantum dot under the protection of a nitrogen atmosphere, then adding the silicon dioxide to the precursor liquid of quantum dot and reacting the silicon dioxide with the precursor liquid of quantum dot to obtain the silicon dioxide hybridized quantum dot. The silicon dioxide hybridized quantum dot obtained in the invention has the advantages of good dissolubility, excellent luminous performance and optical stability, good biocompatibility and biological stability, and good prospect of application in the aspects of biomarker and function materials.
Description
Technical field
That the present invention relates to is the preparation method of field of nanometer technology, a kind of method of method for preparing silicon dioxide hybridized quantum dot by using one-pot specifically,
Background technology
The wavelength of fluorescence of quantum dot or glow color can be regulated by particle diameter at an easy rate, luminous quantum efficiency is high, have narrow and symmetrical emission spectrum and wide and continuous absorption spectrum, these characteristics are so that quantum dot demonstrates wide application prospect in fields such as biomarker, luminescent device, composite, solar cells.However, synthetic quantum dot also has some serious shortcomings such as luminous to stablize not, be difficult to a large amount of preparations, toxicity large etc., thereby makes quantum dot be difficult to be used widely.In order to solve these shortcomings, can coat layer of silicon dioxide on the surface of quantum dot.Silica has good optics and chemical stability, both can protect quantum dot can also do not improved the anti-environment capacity of quantum dot by photooxidation.Simultaneously, the good biocompatibility of silica can reduce the toxicity of quantum dot greatly, is conducive to its biologic applications.In addition, the raw material of preparation silica is cheap, is conducive to a large amount of preparations.Thereby preparation quantum dot-silica hybrid material is subject to the extensive concern of academia.The people such as Rogach synthesize first CdTe, CdSe, CdSe/CdS quantum dot, and the recycling sol-gel process on quantum dot, obtains quantum dot (Chem.Mater.2000,12 (9): 2676-2685) of SiO 2 hybrid with coated with silica.The people such as Gao at first prepare water miscible CdTe quantum dot, then utilize the method for reverse micro emulsion successfully to prepare silica-cadmium telluride hybrid particle (Adv.Mater.2005,17 (19): 2354-2357).The people such as Ying have reported that quantum efficiency is the preparation of the CdSe quantum dot of 20% SiO 2 hybrid, its synthetic method is to prepare first oil-soluble CdSe quantum dot, then hydrophily is modified to increase in its surface, the method of recycling reverse micro emulsion is wrapped up silica (Adv.Mater.2005,17 (13): 1620-1625).
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of one kettle way to prepare the method for the quantum dot of SiO 2 hybrid.
The method that one kettle way prepares the quantum dot of SiO 2 hybrid may further comprise the steps:
Step (a): metal ion source and sulfhydryl compound are dissolved in the deionized water, the concentration of metal ion source is 0.01～300 mM every liter, the mol ratio of sulfydryl sulfhydryl compound and metal ion source is 1～6: 1, adding hydroxide regulator solution pH value is 7～10, makes quantum dot metal ion precursor solution;
Step (b): logical nitrogen and the temperature of solution is raised to 90～100 ℃ in the quantum dot metal ion precursor solution, the nonmetallic ion source aqueous solution is injected this metal ion precursor solution, the mol ratio of nonmetallic ion source and metal ion source is 0.6～1.3: 1, makes the front body fluid of quantum dot;
Step (c): silica source is injected in the front body fluid of quantum dot, the mol ratio of silica source and metal ion source is 0.5～800: 1,85～100 ℃ of lower reactions 0.2～108 hour, makes the quantum dot of SiO 2 hybrid.
Metal ion source described in the step (a) is zinc chloride, caddy, lead chloride, zinc bromide, cadmium iodide, zinc chlorate, cadmium chlorate, zinc perchlorate, cadmium perchlorate, zinc nitrate, cadmium nitrate, plumbi nitras, zinc acetate, cadmium acetate, lead acetate, zinc sulfate or cadmium sulfate.Sulfhydryl compound comprises TGA, mercaptopropionic acid, mercaptoethanol, mercaprol, mercapto glycerol, mercaptoethylmaine, sulfydryl propylamine, sulfydryl butylamine or glutathione described in the step (a).The mol ratio of sulfydryl stabilizing agent and metal ion source is 2～5: 1 described in the step (a).The concentration of quantum dot metal ion source is 0.01～200 mM every liter in the step (a).Hydroxide comprises NaOH, potassium hydroxide described in the step (a); The pH value of quantum dot metal ion prerequisite solution is 7.5～10.The nonmetal source of the preparation quantum dot described in the step (b) comprises vulcanized sodium, potassium sulfide, sodium hydrogen telluride, hydrogen telluride potassium, sodium hydrogen selenide or selenium hydrofining.The mol ratio of the metal ion source in the step (b) in nonmetallic ion source and the step (a) is 0.7～1.2: 1.Used silica source comprises methyl silicate, ethyl orthosilicate, silicic acid four butyl esters or silicon tetrachloride in the step (c); The mol ratio of the metal ion source in silica source and the step (a) is 1～600: 1.The reaction time is 0.5～72 hour in the step (c).
The optical characteristics of the quantum dot of the SiO 2 hybrid that the present invention obtains is tested with absorption spectrometer and XRF, pattern is analyzed with the transmission electron microscope (TEM) of high power, toxicity adopts the cytotoxicity experiment test, and the quantum dot of SiO 2 hybrid also adopts x-ray diffractometer, x-ray photoelectron power spectrum, infrared spectrum etc. to characterize in addition.
The quantum dot of SiO 2 hybrid prepared in accordance with the present invention has fabulous dissolubility, is conducive to carry out further modification; Have excellent luminescent properties, and emission wavelength can regulate and control by the kind of reaction time and sulfydryl stabilizing agent, can satisfy different luminous demands; Fluorescent stability is strong, and toxicity is low, suitable biomarker, lighting function material, the solar cell etc. of being applied to; Ultra-fine particle diameter, can be used for doing the additive of polymer composites, be expected to improve when giving the polymerization luminescent properties mechanical property of polymer, in addition, the quantum dot that utilizes the present invention to prepare is also having good application prospect aspect anti-fake material and the luminous printing ink.
Description of drawings
Fig. 1 utilizes mercapto glycerol to be the fluorescence spectrum figure of the CdTe quantum dot of the SiO 2 hybrid of stabilizing agent preparation;
Fig. 2 utilizes mercaptopropionic acid to be the fluorescence spectrum figure of the CdTe quantum dot of the SiO 2 hybrid of stabilizing agent preparation;
Fig. 3 is the transmission electron microscope figure of the CdTe quantum dot of SiO 2 hybrid.
The specific embodiment
The following examples are to further specify of the present invention, rather than limit the scope of the invention.
Embodiment 1:
Take the source metal of cadmium acetate as the preparation quantum dot, the mercaptopropionic acid stabilizing agent, sodium hydrogen selenide is the nonmetal source of preparation quantum dot, ethyl orthosilicate is silica source, the CdSe quantum dot of preparation SiO 2 hybrid.
Step (a): in 2 liters reaction bulb, adding 1.33 gram cadmium acetates and 2.55 gram mercaptopropionic acids in 1.5 liters of deionized waters, is 8.0 with sodium hydrate regulator solution pH value, makes the cadmium ion precursor solution.
Step (b): the temperature of solution is elevated to 100 ℃ when logical nitrogen in the reaction bulb, then adds 4 milliliters of aqueous solution that contain 0.41 gram sodium hydrogen selenide, make the front body fluid of CdSe quantum dot.
Step (c): 20.8 gram ethyl orthosilicates are injected in the front body fluid of CdSe quantum dot, 100 ℃ of lower reactions 48 hours, make the CdSe quantum dot of SiO 2 hybrid.The CdSe quantum dot of the SiO 2 hybrid that makes issues fluorescent orange at 365 nanometer uviol lamps.
Embodiment 2:
Take the source metal of cadmium acetate as the preparation quantum dot, the mercaptopropionic acid stabilizing agent, the selenium hydrofining is the nonmetal source of preparation quantum dot, ethyl orthosilicate is silica source, the CdSe quantum dot of preparation SiO 2 hybrid.
Step (a): in 2 liters reaction bulb, adding 0.27 gram cadmium acetate and 0.65 gram mercaptopropionic acid in 1.5 liters of deionized waters, is 10.0 with sodium hydrate regulator solution pH value, makes the cadmium ion precursor solution.
Step (b): the temperature of solution is elevated to 90 ℃ when logical nitrogen in the reaction bulb, then adds 4 milliliters of aqueous solution that contain 0.1 gram selenium hydrofining, make the front body fluid of CdSe quantum dot.
Step (c): 20.8 gram ethyl orthosilicates are injected in the front body fluid of CdSe quantum dot, 90 ℃ of lower reactions 72 hours, make the CdSe quantum dot of SiO 2 hybrid.The CdSe quantum dot of the SiO 2 hybrid that makes issues red fluorescence at 365 nanometer uviol lamps.
Embodiment 3:
Take the source metal of cadmium acetate as the preparation quantum dot, the TGA stabilizing agent, sodium hydrogen selenide is the nonmetal source of preparation quantum dot, ethyl orthosilicate is silica source, the CdSe quantum dot of preparation SiO 2 hybrid.
Step (a): in 2 liters reaction bulb, adding 4.1 gram cadmium acetates and 4.4 gram TGAs in 1.5 liters of deionized waters, is 7.5 with sodium hydrate regulator solution pH value, makes the cadmium ion precursor solution.
Step (b): the temperature of solution is elevated to 100 ℃ when logical nitrogen in the reaction bulb, then adds 4 milliliters of aqueous solution that contain 0.96 gram sodium hydrogen selenide, make the front body fluid of CdSe quantum dot.
Step (c): 150 gram ethyl orthosilicates are injected in the front body fluid of CdSe quantum dot, 100 ℃ of lower reactions 24 hours, make the CdSe quantum dot of SiO 2 hybrid.The CdSe quantum dot of the SiO 2 hybrid that makes issues yellow fluorescence at 365 nanometer uviol lamps.
Embodiment 4:
Take the source metal of cadmium acetate as the preparation quantum dot, the mercaptopropionic acid stabilizing agent, sodium hydrogen selenide is the nonmetal source of preparation quantum dot, ethyl orthosilicate is silica source, the CdSe quantum dot of preparation SiO 2 hybrid.
Step (a): in 2 liters reaction bulb, adding 1.33 gram cadmium acetates and 2.55 gram mercaptopropionic acids in 1.5 liters of deionized waters, is 9.0 with sodium hydrate regulator solution pH value, makes the cadmium ion precursor solution.
Step (b): the temperature of solution is elevated to 98 ℃ when logical nitrogen in the reaction bulb, then adds 4 milliliters of aqueous solution that contain 0.41 gram sodium hydrogen selenide, make the front body fluid of CdSe quantum dot.
Step (c): 45.6 gram ethyl orthosilicates are injected in the front body fluid of CdSe quantum dot, 98 ℃ of lower reactions 0.5 hour, make the CdSe quantum dot of SiO 2 hybrid.The CdSe quantum dot of the SiO 2 hybrid that makes issues green fluorescence at 365 nanometer uviol lamps.
Embodiment 5:
Take the source metal of cadmium nitrate as the preparation quantum dot, the mercaptopropionic acid stabilizing agent, the selenium hydrofining is the nonmetal source of preparation quantum dot, ethyl orthosilicate is silica source, the CdSe quantum dot of preparation SiO 2 hybrid.
Step (a): in 2 liters reaction bulb, adding 1.03 gram cadmium nitrates and 2.15 gram mercaptopropionic acids in 1.5 liters of deionized waters, is 9.0 with sodium hydrate regulator solution pH value, makes the cadmium ion precursor solution.
Step (b): the temperature of solution is elevated to 98 ℃ when logical nitrogen in the reaction bulb, then adds 4 milliliters of aqueous solution that contain 0.41 gram selenium hydrofining, make the front body fluid of CdSe quantum dot.
Step (c): 40.2 gram ethyl orthosilicates are injected in the front body fluid of CdSe quantum dot, 98 ℃ of lower reactions 18 hours, make the CdSe quantum dot of SiO 2 hybrid.The CdSe quantum dot of the SiO 2 hybrid that makes is fluorescent orange under 365 nanometer uviol lamps.
Embodiment 6:
Take the source metal of caddy as the preparation quantum dot, the mercapto glycerol stabilizing agent, sodium hydrogen telluride is the nonmetal source of preparation quantum dot, ethyl orthosilicate is silica source, the CdTe quantum dot of preparation SiO 2 hybrid.
Step (a): in 10 liters reaction bulb, adding 5.49 gram caddies and 11.66 gram mercapto glycerols in removing 7 liters of ionized waters, is 9.3 with potassium hydroxide regulator solution pH value, makes the cadmium ion precursor solution.
Step (b): the temperature of solution is elevated to 97 ℃ when logical nitrogen in the reaction bulb, then adds 12 milliliters of aqueous solution that contain 3.17 gram sodium hydrogen tellurides, make the front body fluid of CdTe quantum dot.
Step (c): 624.7 gram ethyl orthosilicates are injected in the front body fluid of CdTe quantum dot, 97 ℃ of lower reactions 24 hours, make the CdTe quantum dot of SiO 2 hybrid.The CdTe quantum dot of the SiO 2 hybrid that makes issues yellow-green fluorescence at 365 nanometer uviol lamps.
The spectrofluorimetry of the CdTe quantum dot of the SiO 2 hybrid that embodiment 6 makes is as shown in Figure 1: emission peak is sharp-pointed and narrow, shows that the products therefrom luminescent properties is fine.
Embodiment 7:
Take the source metal of caddy as the preparation quantum dot, mercaptopropionic acid is stabilizing agent, and sodium hydrogen telluride is the nonmetal source of preparation quantum dot, and ethyl orthosilicate is silica source, the CdTe quantum dot of preparation SiO 2 hybrid.
Step (a): in 2 liters reaction bulb, adding 1.83 gram caddies and 4.24 gram mercaptopropionic acids in 1.3 liters of deionized waters, is 9.0 with sodium hydrate regulator solution pH value, makes the cadmium ion precursor solution.
Step (b): the temperature of solution is elevated to 98 ℃ when logical nitrogen in the reaction bulb, then adds 5 milliliters of aqueous solution that contain 1.21 gram sodium hydrogen tellurides, make the front body fluid of CdTe quantum dot.
Step (c): 88.8 gram ethyl orthosilicates are injected in the front body fluid of CdTe quantum dot, 98 ℃ of lower reactions 12 hours, make the CdTe quantum dot of SiO 2 hybrid.The CdTe quantum dot of the SiO 2 hybrid that makes issues yellow fluorescence at 365 nanometer uviol lamps.
The spectrofluorimetry of the CdTe quantum dot of the SiO 2 hybrid that embodiment 7 makes is as shown in Figure 2: emission peak is sharp-pointed and narrow, shows that the products therefrom luminescent properties is fine.
The transmission electron micrograph of the CdTe quantum dot of the SiO 2 hybrid that embodiment 7 makes as shown in Figure 3, the grain diameter homogeneous, average-size is about 10 nanometers.
Embodiment 8:
Embodiment 8 just changes the caddy among the embodiment 7 into zinc chloride with embodiment 7.
Embodiment 9:
Embodiment 9 just changes the caddy among the embodiment 7 into cadmium iodide with embodiment 7, and mercaptopropionic acid changes TGA into.
Embodiment 9:
Embodiment 9 just changes the caddy among the embodiment 7 into cadmium perchlorate with embodiment 7, and sodium hydrogen telluride changes hydrogen telluride potassium into, and mercaptopropionic acid changes mercaptoethylmaine into.
Embodiment 10:
Embodiment 10 just changes the caddy among the embodiment 7 into cadmium sulfate with embodiment 7, and mercaptopropionic acid changes the sulfydryl propylamine into.
Claims (10)
1. an one kettle way prepares the method for the quantum dot of SiO 2 hybrid, it is characterized in that specifically may further comprise the steps:
Step (a): metal ion source and sulfhydryl compound are dissolved in the deionized water, the concentration of metal ion source is 0.01～300 mM every liter, the mol ratio of sulfhydryl compound and metal ion source is 1～6: 1, adding hydroxide regulator solution pH value is 7～10, makes quantum dot metal ion precursor solution;
Step (b): logical nitrogen and the temperature of solution is raised to 90～100 ℃ in the quantum dot metal ion precursor solution, the nonmetallic ion source aqueous solution is injected this metal ion precursor solution, the mol ratio of nonmetallic ion source and metal ion source is 0.6～1.3: 1, makes the front body fluid of quantum dot;
Step (c): silica source is injected in the front body fluid of quantum dot, the mol ratio of silica source and metal ion source is 0.5～800: 1,85～100 ℃ of lower reactions 0.2～108 hour, makes the quantum dot of SiO 2 hybrid.
2. a kind of one kettle way according to claim 1 prepares the method for the quantum dot of SiO 2 hybrid, it is characterized in that the metal ion source described in the step (a) is zinc chloride, caddy, lead chloride, zinc bromide, cadmium iodide, zinc chlorate, cadmium chlorate, zinc perchlorate, cadmium perchlorate, zinc nitrate, cadmium nitrate, plumbi nitras, zinc acetate, cadmium acetate, lead acetate, zinc sulfate or cadmium sulfate.
3. a kind of one kettle way according to claim 1 prepares the method for the quantum dot of SiO 2 hybrid, it is characterized in that sulfhydryl compound comprises TGA, mercaptopropionic acid, mercaptoethanol, mercaprol, mercapto glycerol, mercaptoethylmaine, sulfydryl propylamine, sulfydryl butylamine or glutathione described in the step (a).
4. a kind of one kettle way according to claim 1 prepares the method for the quantum dot of SiO 2 hybrid, it is characterized in that the mol ratio of sulfhydryl compound described in the step (a) and metal ion source is 2～5: 1.
5. a kind of one kettle way according to claim 1 prepares the method for the quantum dot of SiO 2 hybrid, it is characterized in that the concentration of quantum dot metal ion source in the step (a) is 0.01～200 mM every liter.
6. a kind of one kettle way according to claim 1 prepares the method for the quantum dot of SiO 2 hybrid, it is characterized in that hydroxide comprises NaOH, potassium hydroxide described in the step (a); The pH value of quantum dot metal ion precursor solution is 7.5～10.
7. a kind of one kettle way according to claim 1 prepares the method for the quantum dot of SiO 2 hybrid, it is characterized in that the nonmetal source of the preparation quantum dot described in the step (b) comprises vulcanized sodium, potassium sulfide, sodium hydrogen telluride, hydrogen telluride potassium, sodium hydrogen selenide or selenium hydrofining.
8. a kind of one kettle way according to claim 1 prepares the method for the quantum dot of SiO 2 hybrid, it is characterized in that the mol ratio of the metal ion source in the middle nonmetallic ion source of step (b) and the step (a) is 0.7～1.2: 1.
9. a kind of one kettle way according to claim 1 prepares the method for the quantum dot of SiO 2 hybrid, it is characterized in that used silica source comprises methyl silicate, ethyl orthosilicate, silicic acid four butyl esters or silicon tetrachloride in the step (c); The mol ratio of the metal ion source in silica source and the step (a) is 1～600: 1.
10. a kind of one kettle way according to claim 1 prepares the method for the quantum dot of SiO 2 hybrid, it is characterized in that the reaction time is 0.5～72 hour in the step (c).
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