CN110669521A - Synthesis method of quantum dots - Google Patents
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Abstract
A method for synthesizing quantum dots comprises the following steps: dissolving zinc carboxylate and/or chromium carboxylate, fatty amine, sulfur powder or mercaptan into 1-octadecene or liquid paraffin, and uniformly mixing to form a shell precursor solution; adding 1-octadecene into the synthesized quantum dot core for dilution, heating to the temperature of 310-. By adding the carboxylate of chromium and zinc into the shell precursor, the chromium oxide and the zinc oxide can uniformly form a compact protective film on the surface of the material to prevent the material from being further oxidized, the quantum dot shell can resist water-oxygen corrosion by utilizing the principle, excessive purification processes are not needed, the crystallinity of the quantum dot is improved by cladding at a higher temperature, and the stability and the optical performance of the quantum dot are further improved.
Description
Technical Field
The invention relates to a method for synthesizing quantum dots.
Background
Quantum dots have physical and chemical properties different from those of bulk materials because of their relatively small size, diameter of only a few nanometers, less than the bohr radius of excitons. The quantum dot as a fluorescent substance has the characteristics of small size, narrow half-peak width, high quantum yield and continuously adjustable wavelength, and is widely applied to the optical field and the biological detection field. In order to improve the optical properties of the quantum dots, the quantum dots need to be cladded to improve the stability, increase the quantum yield, and suppress fluorescence flicker. Common shell materials include cadmium sulfide, zinc selenide and the like, and the scheme is mature, but the quantum dots are still sensitive to water and oxygen, such as patents CN 108659817A and CN 106893577A. Some of the quantum dots are coated with silica continuously on the basis of the coating of the shell materials, and the water and oxygen resistance of the whole quantum dot is improved by utilizing the high barrier property of the silica. The silicon coating method mostly uses a reverse microemulsion method, quantum dots are dissolved in a polar solvent by using a dispersing agent to form emulsion, then TEOS or TMOS is added, ammonia water is continuously added to catalyze hydrolysis, and a silicon dioxide layer is formed on the surface of emulsion droplets through condensation. This scheme is cumbersome in steps, too long in duration, and quantum dots lose a certain quantum yield. The silicon-coated quantum dots also have certain problems in use, and particularly in the field of optical films, the silicon dioxide-coated quantum dots have poor compatibility with acrylic resin due to high polarity and large size. The prepared quantum dots can be gathered and deposited at the bottom of the bottle after a long time, and the uniformity of the quantum dot film is seriously influenced in the coating process. Meanwhile, the barrier film of the quantum dot film is high in cost, the cost of the quantum dot film can be further reduced by researching and developing novel water-oxygen-resistant quantum dots, and the competitiveness of the product is improved.
Disclosure of Invention
In order to overcome the defects of the conventional quantum dot, the invention provides a synthetic method of the quantum dot, wherein the quantum dot shell can resist water and oxygen corrosion and improve the optical performance of the quantum dot.
The technical scheme for solving the technical problem is as follows: a method for synthesizing quantum dots comprises the following steps:
dissolving zinc carboxylate and/or chromium carboxylate, fatty amine, sulfur powder or mercaptan into 1-octadecene or liquid paraffin, and uniformly mixing to form a shell precursor solution;
adding 1-octadecene into the synthesized quantum dot core for dilution, heating to the temperature of 310-.
Preferably, the cation of the quantum dot core is Cd ion and/or Zn ion, and the anion of the quantum dot core is Se ion and/or S ion.
Preferably, the concentration of zinc ions ranges from 0.1mol/L to 1mol/L, and the concentration of chromium ions ranges from 0.01mol/L to 0.1 mol/L.
Preferably, the fatty amine is octylamine and/or oleylamine, and the addition amount is 10-15% of the volume of 1-octadecene or liquid paraffin.
Preferably, the whole reaction is carried out under nitrogen atmosphere during the dropping of the shell layer precursor solution.
Preferably, the sulfur powder or mercaptan concentration is in the range of 0.1mol/L to 1 mol/L.
Preferably, the mercaptan is octyl mercaptan or dodecyl mercaptan.
Preferably, the carboxylate of zinc is a formate or acetate of zinc and the carboxylate of chromium is a formate or acetate of chromium.
The invention has the beneficial effects that: by adding the carboxylate of chromium and zinc into the shell precursor, the chromium oxide and the zinc oxide can uniformly form a compact protective film on the surface of the material to prevent the material from being further oxidized, the quantum dot shell can resist water-oxygen corrosion by utilizing the principle, excessive purification processes are not needed, the crystallinity of the quantum dot is improved by cladding at a higher temperature, and the stability and the optical performance of the quantum dot are further improved.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments.
Example one
Putting 0.183g of zinc acetate, 0.023g of chromium acetate and 0.035g of sulfur powder into a 25ml round-bottom flask, adding 1ml of oleylamine and 9ml of 1-octadecene, carrying out ultrasonic dissolution to obtain a shell layer precursor solution, taking a 10ml syringe, and pumping the solution into the syringe pump for later use.
1ml of 1-octadecene solution of CdSe core quantum dots with synthesis pl =550nm and fwhm =25nm (about 3X 10-7mmol of a quantum dot core), addAnd (3) putting the mixture into a 50ml three-neck flask, injecting 5ml of liquid paraffin for dilution, connecting the three-neck flask into a single exhaust pipe, exhausting oxygen by nitrogen for 10 minutes, heating to 330 ℃, injecting a shell precursor solution by using an injection pump, controlling the injection speed to be 5ml/h, keeping small airflow of the single exhaust pipe to exhaust the nitrogen, monitoring the reaction after injecting for about 30 minutes, stopping injecting the shell precursor, cooling to 290 ℃, preserving the temperature for 30 minutes, closing the heating, and finishing the curing.
As a result: PL =590nm, FWHM =27nm, quantum yield = 88%.
The quantum yield is 87% under the conditions of 240h, 60 ℃ and 90% humidity, and the pl peak is maintained at 590 nm.
Example two
Putting 0.183g of zinc acetate, 0.030g of chromium acetate and 0.19g of octanethiol into a 25ml round-bottom flask, adding 1ml of oleylamine and 9ml of 1-octadecene, carrying out ultrasonic dissolution to obtain a shell layer precursor solution, taking a 10ml syringe, and pumping the solution into the syringe pump for later use.
Taking 1ml of synthesized CdZnSe core quantum dot 1-octadecene solution with PL =526nm and FWHM =31nm (containing about 2X 10 of the total weight)-7mmol quantum dot core), put into a 50ml three-neck flask, and diluted by injecting 6ml of 1-octadecene. And (3) connecting the three-neck flask with a single exhaust pipe, exhausting air for 10 minutes by using nitrogen after the single exhaust pipe, heating the reaction to 310 ℃, injecting a shell precursor by using an injection pump, keeping the speed at 8ml/h, taking a small amount of reaction liquid by using an injector after injecting for about 40 minutes, and detecting the reaction, wherein the fluorescence of the quantum dots reaches the expected peak position. Stopping injecting the shell precursor, cooling to 260 ℃, preserving heat for 30 minutes, and turning off heating to finish curing.
As a result: PL =536nm, FWHM =24nm, quantum yield = 94%.
The quantum yield of the test sample is 93% under the conditions of 240h and 60 ℃ and 90% humidity, and the pl peak is maintained at 536 nm.
EXAMPLE III
A method for synthesizing quantum dots comprises the following steps:
dissolving zinc formate, octylamine and sulfur powder in 1-octadecene, and performing ultrasonic dissolution to obtain a shell precursor solution. The concentration range of zinc ions in the shell precursor solution is 0.2mol/L, the concentration of sulfur powder is 0.2mol/L, and the addition amount of octylamine is 15% of the volume of 1-octadecene.
Adding 1-octadecene into the synthesized quantum dot core, diluting, heating to 310 ℃, dropwise adding a shell precursor solution at a speed of 8ml/h until the wavelength of the quantum dot is within a given range, stopping dropwise adding, and keeping the temperature at 265 ℃ for 1h and then stopping heating. In this embodiment, the quantum dot core is CdZnSe.
And the whole reaction is carried out under the protection of nitrogen atmosphere in the dropping process of the shell layer precursor solution.
Example four
A method for synthesizing quantum dots comprises the following steps:
dissolving chromium formate, oleylamine and octyl mercaptan in liquid paraffin, and dissolving by ultrasonic to obtain a shell precursor solution. The concentration range of chromium ions in the shell layer precursor solution is 0.03mol/L, the concentration of octyl mercaptan is 0.4mol/L, and the addition amount of oleylamine is 11% of the volume of the liquid paraffin.
Adding 1-octadecene into the synthesized quantum dot core, diluting, heating to 330 ℃, dropwise adding a shell precursor solution at a speed of 5ml/h until the wavelength of the quantum dot is within a given range, stopping dropwise adding, and keeping the temperature at 270 ℃ for 1.5h, and stopping heating. In this embodiment, the quantum dot core is CdSe.
And the whole reaction is carried out under the protection of nitrogen atmosphere in the dropping process of the shell layer precursor solution.
EXAMPLE five
A method for synthesizing quantum dots comprises the following steps:
mixing chromium acetate and a mixture of chromium acetate and chromium acetate in a volume ratio of 1: dissolving oleylamine, octylamine and dodecyl mercaptan of 1 in 1-octadecene, and performing ultrasonic dissolution to obtain a shell precursor solution. The concentration range of chromium ions in the shell layer precursor solution is 0.01mol/L, the concentration of dodecyl mercaptan is 0.5mol/L, and the addition amount of oleylamine and octylamine is 11% of the volume of 1-octadecene.
Adding 1-octadecene into the synthesized quantum dot core, diluting, heating to 328 ℃, dropwise adding a shell precursor solution at the speed of 6ml/h until the wavelength of the quantum dot is within a given range, stopping dropwise adding, and keeping the temperature at 260 ℃ for 0.5h, and stopping heating. The quantum dot core in this embodiment is CdS.
And the whole reaction is carried out under the protection of nitrogen atmosphere in the dropping process of the shell layer precursor solution.
EXAMPLE six
A method for synthesizing quantum dots comprises the following steps:
mixing zinc acetate and a solvent with the volume ratio of 1: dissolving the oleylamine, the octylamine and the octylmercaptan in the liquid paraffin, and performing ultrasonic dissolution to obtain a shell precursor solution. The concentration range of zinc ions in the shell precursor solution is 0.5mol/L, the concentration of octyl mercaptan is 0.1mol/L, and the addition amount of oleylamine and octyl amine is 10% of the volume of the liquid paraffin.
Adding 1-octadecene into the synthesized quantum dot core, diluting, heating to 320 ℃, dropwise adding a shell precursor solution at a speed of 10ml/h until the wavelength of the quantum dot is within a given range, stopping dropwise adding, and keeping the temperature at 290 ℃ for 0.7h, and stopping heating. The quantum dot core in this example is CdZnS.
And the whole reaction is carried out under the protection of nitrogen atmosphere in the dropping process of the shell layer precursor solution.
EXAMPLE seven
A method for synthesizing quantum dots comprises the following steps:
zinc formate, and the volume ratio is 2: dissolving oleylamine, octylamine and dodecyl mercaptan of 1 in 1-octadecene, and performing ultrasonic dissolution to obtain a shell precursor solution. The concentration range of zinc ions in the shell precursor solution is 1mol/L, the concentration of dodecyl mercaptan is 1mol/L, and the addition amount of oleylamine and octylamine is 13% of the volume of 1-octadecene.
Adding 1-octadecene into the synthesized quantum dot core, diluting, heating to 315 ℃, dropwise adding a shell precursor solution at the speed of 9ml/h until the wavelength of the quantum dot is within a given range, stopping dropwise adding, and keeping the temperature of 285 ℃ for 2h and stopping heating. In this embodiment, the quantum dot core is CdZnSeS.
And the whole reaction is carried out under the protection of nitrogen atmosphere in the dropping process of the shell layer precursor solution.
Example eight
A method for synthesizing quantum dots comprises the following steps:
dissolving zinc formate, chromium acetate, oleylamine and octyl mercaptan in liquid paraffin, and dissolving by ultrasonic to obtain a shell precursor solution. The concentration of zinc ions in the shell precursor solution is 0.1mol/L, the concentration of chromium ions is 0.04mol/L, the concentration of octyl mercaptan is 0.7mol/L, and the addition amount of oleylamine is 12% of the volume of the liquid paraffin.
Adding 1-octadecene into the synthesized quantum dot core, diluting, heating to 325 ℃, dropwise adding a shell precursor solution at a speed of 5.5ml/h until the wavelength of the quantum dot is within a given range, stopping dropwise adding, and keeping the temperature at 275 ℃ for 1.8h, and stopping heating. The quantum dot core in this example is CdZnS.
And the whole reaction is carried out under the protection of nitrogen atmosphere in the dropping process of the shell layer precursor solution.
Example nine
A method for synthesizing quantum dots comprises the following steps:
dissolving zinc formate, chromium formate, oleylamine and dodecyl mercaptan in 1-octadecene, and performing ultrasonic dissolution to obtain a shell precursor solution. The concentration of zinc ions in the precursor solution of the shell layer is 0.8mol/L, the concentration of chromium ions is 0.09mol/L, the concentration of dodecyl mercaptan is 0.45mol/L, and the addition amount of oleylamine is 15.5 percent of the volume of 1-octadecene.
Adding 1-octadecene into the synthesized quantum dot core, diluting, heating to 332 ℃, dropwise adding a shell precursor solution at a speed of 7ml/h until the wavelength of the quantum dot is within a given range, stopping dropwise adding, and keeping the temperature at 280 ℃ for 1.2h, and stopping heating. The quantum dot core in this example is ZnS.
And the whole reaction is carried out under the protection of nitrogen atmosphere in the dropping process of the shell layer precursor solution.
Example ten
A method for synthesizing quantum dots comprises the following steps:
dissolving zinc formate, chromium acetate, octylamine and octylmercaptan in liquid paraffin, and performing ultrasonic dissolution to obtain a shell precursor solution. The concentration of zinc ions in the precursor solution of the shell layer is 0.6mol/L, the concentration of chromium ions is 0.06mol/L, the concentration of octyl mercaptan is 0.25mol/L, and the addition amount of octyl amine is 10.5 percent of the volume of the liquid paraffin.
Adding 1-octadecene into the synthesized quantum dot core, diluting, heating to 315 ℃, dropwise adding a shell precursor solution at a speed of 8.5ml/h until the wavelength of the quantum dot is within a given range, stopping dropwise adding, and keeping the temperature at 263 ℃ for 0.9h, and stopping heating. In this embodiment, the quantum dot core is ZnSe.
And the whole reaction is carried out under the protection of nitrogen atmosphere in the dropping process of the shell layer precursor solution.
EXAMPLE eleven
A method for synthesizing quantum dots comprises the following steps:
dissolving zinc acetate, chromium acetate, octylamine and sulfur powder in 1-octadecene, and performing ultrasonic dissolution to obtain a shell precursor solution. The concentration of zinc ions in the precursor solution of the shell layer is 0.55mol/L, the concentration of chromium ions is 0.1mol/L, the concentration of sulfur powder is 0.6mol/L, and the addition amount of octylamine is 14 percent of the volume of 1-octadecene.
Adding 1-octadecene into the synthesized quantum dot core, diluting, heating to 335 ℃, dropwise adding a shell precursor solution at a speed of 8ml/h until the wavelength of the quantum dot is within a given range, stopping dropwise adding, and keeping the temperature at 280 ℃ for 0.6h, and stopping heating. In this embodiment, the quantum dot core is CdSe.
And the whole reaction is carried out under the protection of nitrogen atmosphere in the dropping process of the shell layer precursor solution.
Claims (9)
1. A method for synthesizing quantum dots is characterized in that:
dissolving zinc carboxylate and/or chromium carboxylate, fatty amine, sulfur powder or mercaptan into 1-octadecene or liquid paraffin, and uniformly mixing to form a shell precursor solution;
adding 1-octadecene into the synthesized quantum dot core for dilution, heating to the temperature of 310-.
2. A method of synthesizing a quantum dot as claimed in claim 1, wherein: the positive ions of the quantum dot cores are Cd ions and/or Zn ions, and the negative ions of the quantum dot cores are Se ions and/or S ions.
3. A method of synthesizing a quantum dot as claimed in claim 1 or 2, wherein: the concentration range of zinc ions is 0.1-1 mol/L, and the concentration range of chromium ions is 0.01-0.1 mol/L.
4. A method of synthesizing a quantum dot as claimed in claim 1 or 2, wherein: the fatty amine is octylamine and/or oleylamine, and the addition amount is 10-15% of the volume of 1-octadecene or liquid paraffin.
5. A method of synthesizing a quantum dot as claimed in claim 1 or 2, wherein: the whole reaction is carried out under nitrogen atmosphere in the dropping process of the shell layer precursor solution.
6. A method of synthesizing a quantum dot as claimed in claim 1 or 2, wherein: the concentration range of the sulfur powder or the mercaptan is 0.1mol/L-1 mol/L.
7. The method of synthesizing a quantum dot of claim 6, wherein: the mercaptan is octyl mercaptan or dodecyl mercaptan.
8. A method of synthesizing a quantum dot as claimed in claim 1 or 2, wherein: the carboxylate of zinc is formate or acetate of zinc, and the carboxylate of chromium is formate or acetate of chromium.
9. A method of synthesizing a quantum dot as claimed in claim 1 or 2, wherein: the carboxylate of zinc is formate or acetate of zinc, and the carboxylate of chromium is formate or acetate of chromium.
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| CN110129055A (en) * | 2019-05-20 | 2019-08-16 | 上海交通大学 | The preparation of CdSeZnS/ZnS/ZnS core shell/shell quantum dot |
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- 2019-09-20 CN CN201910894287.XA patent/CN110669521A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103582690A (en) * | 2011-06-07 | 2014-02-12 | 拜耳技术工程（上海）有限公司 | Preparation methods of core-shell nanoparticles and solution thereof |
| CN103113882A (en) * | 2013-02-20 | 2013-05-22 | 杭州纳晶科技有限公司 | Nanocrystalline quantum dot with core-shell structure and preparation method of nanocrystalline quantum dot |
| CN108913142A (en) * | 2018-06-29 | 2018-11-30 | 纳晶科技股份有限公司 | Quantum dot, preparation method and the application of coated metal oxide |
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