CN103043718A - Preparation method of zirconia quantum dots - Google Patents
Preparation method of zirconia quantum dots Download PDFInfo
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- CN103043718A CN103043718A CN2013100047836A CN201310004783A CN103043718A CN 103043718 A CN103043718 A CN 103043718A CN 2013100047836 A CN2013100047836 A CN 2013100047836A CN 201310004783 A CN201310004783 A CN 201310004783A CN 103043718 A CN103043718 A CN 103043718A
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Abstract
The invention belongs to the technical field of quantum dots, and relates to a preparation method of zirconia quantum dots, in particular to a preparation method of zirconia quantum dots with a high-temperature oil phase. The method comprises the steps of 1) dissolving a metal zirconium compound A into a solvent B to form a solution C, 2) adding a ligand D into a solution C to form a solution E, 3) conducting vacuum-pumping on a solution E, filling in nitrogen gas, heating to a required temperature, stirring for required time, cooling the solution to the room temperature, and repeating procedures of vacuum-pumping and nitrogen gas filling according to requirements, and 4) conducting centrifugation washing on the solution E obtained in Step 3), dispersing in a solvent F, and obtaining a zirconia quantum dot solution. The method is simple and environment-friendly, and can prepare the zirconia quantum dots on a large scale.
Description
Technical field
The present invention relates to a kind of preparation method of zirconium white quantum dot, especially adopt the high temperature oil phase to prepare the method for zirconium white quantum dot, belong to the technology of quantum dots field.
Background technology
Quanta point material is because its quantum confined effect, and electronics and hole be by quantum confinement, and when quantum spot size during less than Bohr radius, the energy level distribution of quantum dot will be transformed into discrete energy levels by continuous energy level.The performance of quantum dot can be regulated by changing particle size and chemical composition.Just because of the many good characteristics of quantum dot, it is had a wide range of applications in fields such as photochemical catalysis, photoelectric device, biological chemistry, molecular biology.
Zirconia material has high rigidity, high strength, high tenacity, the physical and chemical performance that high wear resistance and chemical resistance etc. are good, zirconium white obtain to use widely in pottery, refractory materials, machinery, electronics, optics, opticfiber communication, aerospace, biology, chemistry etc. various fields.The zirconium white quantum dot also becomes one of focus of present research, at aspects such as photochemical catalysis, biology, photoelectricity important application prospect is arranged.
Because zirconium dioxide has higher fusing point and boiling point, what therefore the zirconium dioxide of present preparation high-crystallinity adopted usually is high temperature sintering.High-temperature sintering process not only energy consumption is high, and particle size is large, is difficult to obtain size, the uniform quantum dot of pattern.Therefore, seek a kind of simple, less energy-consumption, environmental friendliness, degree of crystallinity is high, appearance and size is controlled and the method that can prepare on a large scale the zirconium dioxide quantum dot seems very important.
Summary of the invention
The objective of the invention is in order to propose a kind of method for preparing the zirconium white quantum dot.
The objective of the invention is to be achieved through the following technical solutions.
The preparation method of a kind of zirconium white quantum dot of the present invention, concrete steps are:
1) the metal zirconium compd A is dissolved among the solvent B forms solution C;
2) will form solution E in the part D adding solution C;
3) solution E is vacuumized and inflated with nitrogen, after then being warming up to temperature required and stirring required time, treat that solution is cooled to room temperature; Can repeat as required to vacuumize and the inflated with nitrogen process;
4) to step 3) solution E that obtains carries out eccentric cleaning, and be scattered in and obtain the zirconium white quantum dot solution among the solvent F.
Above-mentioned steps 1) the metal zirconium compd A is a kind of in the following material in: Zircosol ZN, basic zirconium chloride, zirconium acetate, methyl ethyl diketone zirconium, zirconyl carbonate, zirconium chloride, zirconium-n-propylate, zirconium-n-butylate;
Above-mentioned steps 1) the solvent B in is a kind of in the following material: Yelkin TTS, polysorbate, glycerin fatty acid ester, oleic acid, lauric acid, the trolamine soap, the dioctyl sodium sulfosuccinate, cetyl trimethylammonium bromide, dodecyl mercaptans, amino dodecane, tri octyl phosphine, oleyl amine, stearylamine, n-caprylic acid, oleic acid, sad, trolamine, diethanolamine, polyethylene, polyvinyl chloride, polyvinylpyrrolidone, polypropylene, polyacrylic acid, polyvinyl alcohol, polyoxyethylene glycol, the polyethylene formicester, polyacrylamide, polyoxyethylene, urethane, trioctyl phosphine oxide;
Above-mentioned steps 2) the part D in is a kind of in the following material: Yelkin TTS, polysorbate, glycerin fatty acid ester, oleic acid, lauric acid, the trolamine soap, the dioctyl sodium sulfosuccinate, cetyl trimethylammonium bromide, dodecyl mercaptans, amino dodecane, tri octyl phosphine, oleyl amine, stearylamine, n-caprylic acid, oleic acid, sad, trolamine, diethanolamine, polyethylene, polyvinyl chloride, polyvinylpyrrolidone, polypropylene, polyacrylic acid, polyvinyl alcohol, polyoxyethylene glycol, the polyethylene formicester, polyacrylamide, polyoxyethylene, urethane, trioctyl phosphine oxide;
Above-mentioned steps 4) the solvent F in is a kind of in the following solvent: normal hexane, toluene, hexanaphthene, octane, methylene dichloride, trichloromethane, pyridine, toluene dichloride;
Above-mentioned steps 1) in the solution C concentration of metal zirconium compd A be 0.01mM to 1M.
Above-mentioned steps 2) in the solution E concentration of part D be 0.01mM to 1M.
Above-mentioned steps 3) temperature required in is that 150 degree are to 320 degree.
Above-mentioned steps 3) required time in is 10 minutes to 10 hours.
Beneficial effect
Method of the present invention is simple, environmental friendliness and can prepare on a large scale the sulfide quantum dot.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the zirconium white quantum dot that obtains of embodiment 1.
Embodiment
Embodiment 1
With 10mmol ZrO (NO
3)
2Be dissolved in the 100ml trioctyl phosphine oxide, form solution C.Then the 20mmol lauric acid is dissolved in the solution C, forms solution E.Solution E is vacuumized and inflated with nitrogen, 3 times and so forth, then be warming up to 200 degree and stirred 2 hours, treat that solution is cooled to room temperature; And then eccentric cleaning, and be scattered in and obtain the zirconium white quantum dot solution in the toluene, its electromicroscopic photograph is as shown in Figure 1.
Embodiment 2
With 8mmol ZrOCl
2Be dissolved in the 100ml trioctyl phosphine oxide, form solution C.Then 20mmol oleic acid is dissolved in the solution C, forms solution E.Solution E is vacuumized and inflated with nitrogen, 3 times and so forth, then be warming up to 240 degree and stirred 4 hours, treat that solution is cooled to room temperature; And then eccentric cleaning, and be scattered in and obtain the zirconium white quantum dot solution in the normal hexane.
Embodiment 3
With 10mmol ZrO (NO
3)
2Be dissolved in the 100ml trioctyl phosphine oxide, form solution C.Then 20mmol oleic acid is dissolved in the solution C, forms solution E.Solution E is vacuumized and inflated with nitrogen, 3 times and so forth, then be warming up to 200 degree and stirred 3 hours, treat that solution is cooled to room temperature; And then eccentric cleaning, and be scattered in and obtain the zirconium white quantum dot solution in the toluene.
Embodiment 4
With 10mmol ZrCl
4Be dissolved in the 100ml trioctyl phosphine oxide, form solution C.Then the 15mmol lauric acid is dissolved in the solution C, forms solution E.Solution E is vacuumized and inflated with nitrogen, 3 times and so forth, then be warming up to 270 degree and stirred 2 hours, treat that solution is cooled to room temperature; And then eccentric cleaning, and be scattered in and obtain the zirconium white quantum dot solution in the toluene.
With 10mmol ZrO (NO
3)
2Be dissolved in the 100ml trioctyl phosphine oxide, form solution C.Then the 20mmol oleyl amine is dissolved in the solution C, forms solution E.Solution E is vacuumized and inflated with nitrogen, 3 times and so forth, then be warming up to 260 degree and stirred 2 hours, treat that solution is cooled to room temperature; And then eccentric cleaning, and be scattered in and obtain the zirconium white quantum dot solution in the toluene.
Embodiment 6
With 10mmol ZrO (NO
3)
2Be dissolved in the 100ml tri octyl phosphine, form solution C.Then the 16mmol amino dodecane is dissolved in the solution C, forms solution E.Solution E is vacuumized and inflated with nitrogen, 3 times and so forth, then be warming up to 220 degree and stirred 1 hour, treat that solution is cooled to room temperature; And then eccentric cleaning, and be scattered in and obtain the zirconium white quantum dot solution in the toluene.
Embodiment 7
With 10mmol ZrO (NO
3)
2Be dissolved in the 100ml tri octyl phosphine, form solution C.Then the 18mmol lauric acid is dissolved in the solution C, forms solution E.Solution E is vacuumized and inflated with nitrogen, 3 times and so forth, then be warming up to 200 degree and stirred 8 hours, treat that solution is cooled to room temperature; And then eccentric cleaning, and be scattered in and obtain the zirconium white quantum dot solution in the toluene dichloride.
Embodiment 8
The 10mmol zirconium acetate is dissolved in the 100ml trioctyl phosphine oxide, forms solution C.Then the 20mmol lauric acid is dissolved in the solution C, forms solution E.Solution E is vacuumized and inflated with nitrogen, 3 times and so forth, then be warming up to 200 degree and stirred 2 hours, treat that solution is cooled to room temperature; And then eccentric cleaning, and be scattered in and obtain the zirconium white quantum dot solution in the toluene.
Embodiment 9
The 5mmol zirconium acetate is dissolved in the 100ml tri octyl phosphine, forms solution C.Then the 15mmol lauric acid is dissolved in the solution C, forms solution E.Solution E is vacuumized and inflated with nitrogen, 3 times and so forth, then be warming up to 280 degree and stirred 1.5 hours, treat that solution is cooled to room temperature; And then eccentric cleaning, and be scattered in and obtain the zirconium white quantum dot solution in the toluene.
Embodiment 10
The 8mmol zirconium acetate is dissolved in the 100ml trioctyl phosphine oxide, forms solution C.Then the 16mmol lauric acid is dissolved in the solution C, forms solution E.Solution E is vacuumized and inflated with nitrogen, 3 times and so forth, then be warming up to 300 degree and stirred 1 hour, treat that solution is cooled to room temperature; And then eccentric cleaning, and be scattered in and obtain the zirconium white quantum dot solution in the toluene.
Claims (10)
1. the preparation method of a zirconium white quantum dot is characterized in that concrete steps are:
1) the metal zirconium compd A is dissolved among the solvent B forms solution C;
2) will form solution E in the part D adding solution C;
3) solution E is vacuumized and inflated with nitrogen, after then being warming up to temperature required and stirring required time, treat that solution is cooled to room temperature;
4) to step 3) solution E that obtains carries out eccentric cleaning, and be scattered in and obtain the zirconium white quantum dot solution among the solvent F.
2. the preparation method of a kind of zirconium white quantum dot according to claim 1 is characterized in that: repeat to vacuumize and inflated with nitrogen process 3 times.
3. the preparation method of a kind of zirconium white quantum dot according to claim 1 is characterized in that: step 1) in the metal zirconium compd A be a kind of in the following material: Zircosol ZN, basic zirconium chloride, zirconium acetate, methyl ethyl diketone zirconium, zirconyl carbonate, zirconium chloride, zirconium-n-propylate, zirconium-n-butylate.
4. the preparation method of a kind of zirconium white quantum dot according to claim 1 is characterized in that: step 1) in solvent B be a kind of in the following material: Yelkin TTS, polysorbate, glycerin fatty acid ester, oleic acid, lauric acid, the trolamine soap, the dioctyl sodium sulfosuccinate, cetyl trimethylammonium bromide, dodecyl mercaptans, amino dodecane, tri octyl phosphine, oleyl amine, stearylamine, n-caprylic acid, oleic acid, sad, trolamine, diethanolamine, polyethylene, polyvinyl chloride, polyvinylpyrrolidone, polypropylene, polyacrylic acid, polyvinyl alcohol, polyoxyethylene glycol, the polyethylene formicester, polyacrylamide, polyoxyethylene, urethane, trioctyl phosphine oxide.
5. the preparation method of a kind of zirconium white quantum dot according to claim 1 is characterized in that: step 2) in part D be a kind of in the following material: Yelkin TTS, polysorbate, glycerin fatty acid ester, oleic acid, lauric acid, the trolamine soap, the dioctyl sodium sulfosuccinate, cetyl trimethylammonium bromide, dodecyl mercaptans, amino dodecane, tri octyl phosphine, oleyl amine, stearylamine, n-caprylic acid, oleic acid, sad, trolamine, diethanolamine, polyethylene, polyvinyl chloride, polyvinylpyrrolidone, polypropylene, polyacrylic acid, polyvinyl alcohol, polyoxyethylene glycol, the polyethylene formicester, polyacrylamide, polyoxyethylene, urethane, trioctyl phosphine oxide.
6. the preparation method of a kind of zirconium white quantum dot according to claim 1 is characterized in that: step 4) in solvent F be a kind of in the following solvent: normal hexane, toluene, hexanaphthene, octane, methylene dichloride, trichloromethane, pyridine, toluene dichloride.
7. the preparation method of a kind of zirconium white quantum dot according to claim 1 is characterized in that: step 1) in the solution C concentration of metal zirconium compd A be 0.01mM to 1M.
8. the preparation method of a kind of zirconium white quantum dot according to claim 1 is characterized in that: step 2) in the solution E concentration of part D be 0.01mM to 1M.
9. the preparation method of a kind of zirconium white quantum dot according to claim 1 is characterized in that: step 3) in temperature required be 150 the degree to 320 the degree.
10. the preparation method of a kind of zirconium white quantum dot according to claim 1 is characterized in that: step 3) in required time be 10 minutes to 10 hours.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588247A (en) * | 2013-11-05 | 2014-02-19 | 北京理工大学 | Novel method for carrying out solvothermal synthesis to obtain monodisperse high-crystallinity zirconia quantum dots |
| CN107055608A (en) * | 2016-10-21 | 2017-08-18 | 华南农业大学 | A kind of transparent dispersion liquid of nano zirconium dioxide and preparation method and application |
| CN108486710A (en) * | 2018-01-17 | 2018-09-04 | 南通富尊纺织科技有限公司 | A kind of production technology of high energy jewel bio wave health yarn |
| US11133468B2 (en) | 2018-06-25 | 2021-09-28 | Samsung Electronics Co., Ltd. | Semiconductor nanocrystal-ligand composite and device including composite |
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| CN1271174C (en) * | 2003-03-05 | 2006-08-23 | 韩国化学研究院 | Method for continuous preparation of nanometer-sized hydrous zirconia sol using microwave |
| CN1290771C (en) * | 2003-03-07 | 2006-12-20 | 韩国化学研究院 | Method for continuous preparation of nanometer-sized hydrous zirconia sol |
| CN101157851A (en) * | 2007-08-28 | 2008-04-09 | 华中师范大学 | Preparation method of quantum dot self-assembling nano structural material |
| CN101585515A (en) * | 2009-06-15 | 2009-11-25 | 中国医药城泰州纳米生命医学研究院 | Prepartion method of ternary system quantum dots containing Cd*Zn*Se |
| CN101961626B (en) * | 2010-09-20 | 2012-11-07 | 浙江大学 | Method for preparing ZrO2 aerogel |
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2013
- 2013-01-07 CN CN2013100047836A patent/CN103043718A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1271174C (en) * | 2003-03-05 | 2006-08-23 | 韩国化学研究院 | Method for continuous preparation of nanometer-sized hydrous zirconia sol using microwave |
| CN1290771C (en) * | 2003-03-07 | 2006-12-20 | 韩国化学研究院 | Method for continuous preparation of nanometer-sized hydrous zirconia sol |
| CN101157851A (en) * | 2007-08-28 | 2008-04-09 | 华中师范大学 | Preparation method of quantum dot self-assembling nano structural material |
| CN101585515A (en) * | 2009-06-15 | 2009-11-25 | 中国医药城泰州纳米生命医学研究院 | Prepartion method of ternary system quantum dots containing Cd*Zn*Se |
| CN101961626B (en) * | 2010-09-20 | 2012-11-07 | 浙江大学 | Method for preparing ZrO2 aerogel |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588247A (en) * | 2013-11-05 | 2014-02-19 | 北京理工大学 | Novel method for carrying out solvothermal synthesis to obtain monodisperse high-crystallinity zirconia quantum dots |
| CN103588247B (en) * | 2013-11-05 | 2016-01-20 | 北京理工大学 | A kind of method of novel dissolvent thermal synthesis monodisperse high-crystallinity zirconium white quantum dot |
| CN107055608A (en) * | 2016-10-21 | 2017-08-18 | 华南农业大学 | A kind of transparent dispersion liquid of nano zirconium dioxide and preparation method and application |
| CN108486710A (en) * | 2018-01-17 | 2018-09-04 | 南通富尊纺织科技有限公司 | A kind of production technology of high energy jewel bio wave health yarn |
| US11133468B2 (en) | 2018-06-25 | 2021-09-28 | Samsung Electronics Co., Ltd. | Semiconductor nanocrystal-ligand composite and device including composite |
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Application publication date: 20130417 |