CN114381269A - Size-controllable water-soluble PbS/PbSe/ZnS core-shell structure quantum dot and preparation method thereof - Google Patents
Size-controllable water-soluble PbS/PbSe/ZnS core-shell structure quantum dot and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a size-controllable water-soluble PbS/PbSe/ZnS core-shell structure quantum dot and a preparation method thereof, wherein the preparation method comprises the following steps: s1: adding a stabilizer into a lead source aqueous solution, adjusting the pH value, and injecting a sulfur source aqueous solution to generate PbS quantum dots with hydrophilic ligands; s2: adding a selenium source water solution into the step S1, and reacting the selenium source with the unreacted stabilizer and the lead source in the step S1 to obtain PbS/PbSe core-shell structure quantum dots; s3: and (3) injecting the quantum dot solution obtained in the step S2 into a zinc source aqueous solution, finally adding a stabilizer and a sulfur source aqueous solution, heating for reacting for a certain time, cooling to room temperature, and performing precipitation, centrifugal separation and freeze drying to form the water-soluble PbS/PbSe/ZnS core-shell structure quantum dot with the surface coated with the hydrophilic ligand. The water-soluble quantum dot prepared by the method has the characteristics of uniform particle size, controllable size, wide absorption spectrum, good stability and the like, can simultaneously realize the detection of near infrared light and mid-infrared light, and is an infrared light detection material with high practicability.
Description
Technical Field
The invention relates to the technical field of quantum dot materials, in particular to a size-controllable water-soluble PbS/PbSe/ZnS core-shell structure quantum dot and a preparation method thereof.
Background
The quantum dots are also called semiconductor nanocrystals, and because the dimensions of the three dimensions are in the nanometer level, the quantum dots show unique optical and electrical properties, such as surface effect, quantum size effect, dielectric confinement effect and macroscopic quantum tunneling effect, and particularly have excellent spectral properties, photochemical stability and electrochemical properties, so that the quantum dots show great application prospects in the research fields of photoelectric detection, illumination display, clinical detection, molecular biology and the like, and become a great research hotspot in recent years.
The PbS quantum dot has a larger Bohr radius (18nm) and a narrower forbidden bandwidth (0.41eV), and the absorption spectrum and the fluorescence emission spectrum of the PbS quantum dot can cover the whole near-infrared band (900-1600 nm) easily by controlling the size of the PbS quantum dot, so the PbS quantum dot has wide application prospect in the fields of photoelectric detectors, communication, biological fluorescence labeling and the like. At present, the mainstream technology for synthesizing PbS quantum dots by a chemical method is an organic metal pyrolysis method. PbO was dissolved into oleic acid with heating (150 ℃) in an argon atmosphere to form a lead oleate precursor as a lead source. Bis-trimethylsilyl sulfur was dissolved in octadecene as a sulfur source. And (3) putting a sulfur source into a lead source, and heating to react to generate the PbS quantum dots. Oleic acid as a coordination solvent can be adsorbed on the surface of the quantum dot to prevent the quantum dot from accumulating and growing.
However, the organometallic pyrolysis method requires the preparation of PbS quantum dots at higher temperatures, and the quantum dot synthesis occurs in organic solution, which has a certain impact on the environment. Under the condition of industrial production, the quantum dots of different batches are required to keep good consistency, which requires that the synthesis of the quantum dots has good repeatability, but the uniformity of the particle size of the quantum dots synthesized by the method is poor, which causes difficulty in controlling the positions of optical absorption peaks and emission peaks of the quantum dots, and is also a main reason for high cost when the quantum dots are applied on a large scale.
Secondly, the absorption spectrum of PbS quantum dots is narrow. Meanwhile, due to the fact that a large number of dangling bonds and defects exist on the surface of the PbS quantum dot prepared by the organic metal pyrolysis method, and due to the fact that the surface of the quantum dot is not passivated sufficiently by common organic ligands (such as oleic acid), photo-oxidation, photo-bleaching and photo-degradation reactions occur on the surface of the quantum dot, and the stability of the quantum dot is greatly reduced. Due to the existence of Pb heavy metal ions in the quantum dots, heavy metal ions are separated out much, so that the safety of the quantum dots becomes the bottleneck of application.
Disclosure of Invention
In view of the shortcomings of the prior art, the invention aims to provide a size-controllable water-soluble PbS/PbSe/ZnS core-shell structure quantum dot and a preparation method thereof. The preparation method adopts a hydrothermal method, synthesizes PbS/PbSe/ZnS quantum dots at a lower temperature, can avoid Ostwald Ripening from occurring in the quantum dots at a higher reaction temperature, and has the advantages of mild reaction conditions, simple method, good experimental repeatability and the like. The introduction of PbSe widens the detectable waveband to mid-infrared light, and meanwhile, the uniform PbSe/ZnS double-layer spherical shell coating ensures the long-term stability of the quantum dots and reduces the precipitation of heavy metal ions.
In order to solve the technical problems, the invention adopts the following technical scheme:
according to a first technical scheme, the size-controllable water-soluble PbS/PbSe/ZnS core-shell structure quantum dot is characterized in that PbS is taken as a core, PbSe and ZnS are taken as shell layers, the surface of the core-shell structure quantum dot is wrapped by a hydrophilic ligand, and the hydrophilic ligand comprises at least one of thioglycolic acid, mercaptopropionic acid, L-cysteine, N-acetyl-L-cysteine, monothioglycerol, dithioglycerol, glutathione and sodium citrate.
According to a second technical scheme of the invention, a preparation method of a size-controllable water-soluble PbS/PbSe/ZnS core-shell structure quantum dot is provided, which comprises the following steps:
s1, adding a stabilizer into the lead source aqueous solution, uniformly mixing to obtain a first mixed solution, adjusting the pH value of the first mixed solution, deoxidizing, and then injecting the sulfur source aqueous solution under magnetic stirring to react to form a PbS quantum dot solution with hydrophilic ligands;
s2, adding a selenium source aqueous solution into the PbS quantum dot solution to obtain a second mixed solution, heating the second mixed solution in an inert gas atmosphere, after the selenium source and a stabilizer and a lead source in the PbS quantum dot solution are reacted, rapidly cooling to room temperature, performing post-treatment to obtain PbS/PbSe core-shell structure quantum dots, and dissolving the PbS/PbSe core-shell structure quantum dots in water to obtain a PbS/PbSe quantum dot aqueous solution;
and S3, injecting the aqueous solution of PbS/PbSe quantum dots into the aqueous solution of zinc source, stirring and heating, finally injecting a stabilizer and an aqueous solution of sulfur source, reacting for a certain time, cooling to room temperature, and performing precipitation, centrifugal separation and freeze drying to form the water-soluble PbS/PbSe/ZnS core-shell structure quantum dots with the surfaces wrapped by hydrophilic ligands.
Further, the lead source water solution is prepared by dissolving a lead source in water, wherein the lead source comprises one of lead acetate, lead nitrate, lead oxide or a mixture thereof.
Further, the stabilizer (i.e., hydrophilic ligand) includes one or a mixture of thioglycolic acid, mercaptopropionic acid, L-cysteine, N-acetyl-L-cysteine, monothioglycerol, dithioglycerol, glutathione, sodium citrate.
Further, the adjusting the pH of the first mixed solution includes:
and adjusting the pH value of the first mixed solution to 8-12 by using a pH adjusting agent, wherein the pH adjusting agent comprises one of sodium hydroxide solution, triethylamine, ammonia water and a combination thereof.
Further, the sulfur source water solution is prepared by dissolving a sulfur source in water, wherein the sulfur source comprises one or a mixture of sodium sulfide, sulfur powder and sulfur powder.
Further, the selenium source water solution is prepared by dissolving a selenium source in water, wherein the selenium source comprises one or a mixture of selenium powder, sodium selenosulfate and selenium oxide.
Further, the zinc source aqueous solution is prepared by dissolving a zinc source in water, wherein the zinc source comprises one of zinc acetate, zinc nitrate, zinc chloride and zinc sulfate or a mixture thereof.
Further, the steps S1-S3 all provide ultraviolet lamps as reaction media, the wavelength provided by the ultraviolet lamps is 320nm, and the ultraviolet lamps are annularly arranged around the reaction equipment and used for avoiding incomplete reaction of partial quanta through observation and identification in the reaction process.
Further, the molar ratio of lead to sulfur in the step S1 is: 1-5:1, the molar ratio of sulfur in step S1 to selenium in step S2 is: 1-6:1, the molar ratio of zinc in step S3 to selenium in step S2 is: 1:1-5.
Compared with the prior art, the invention has the beneficial effects that:
the water-soluble PbS/PbSe/ZnS core-shell structure quantum dot prepared by the invention is synthesized in water on the basis of a hydrothermal method, and has the advantages of simple preparation experiment operation and good process repeatability. The quantum dot has the characteristics of uniform particle size, controllable size, wide absorption spectrum, good stability, less heavy metal ion precipitation and the like, can simultaneously realize the detection of near infrared light and mid-infrared light, and is an infrared light detection material with high practicability.
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In the drawings, which are not necessarily drawn to scale, like reference numerals may describe similar components in different views. Like reference numerals having letter suffixes or different letter suffixes may represent different instances of similar components. The drawings illustrate various embodiments generally by way of example and not by way of limitation, and together with the description and claims serve to explain the disclosed embodiments. The same reference numbers will be used throughout the drawings to refer to the same or like parts, where appropriate. Such embodiments are illustrative, and are not intended to be exhaustive or exclusive embodiments of the present apparatus or method.
Fig. 1 shows a structural diagram of a size-controllable water-soluble PbS/PbSe/ZnS core-shell structure quantum dot according to an embodiment of the present invention.
Fig. 2 shows a transmission electron microscope image of the PbS/PbSe/ZnS core-shell structure quantum dot prepared by the preparation method of the size-controllable water-soluble PbS/PbSe/ZnS core-shell structure quantum dot in the embodiment of the invention.
Description of reference numerals: 1-PbS core, 2-PbSe shell and 3-ZnS shell.
Detailed Description
The following examples are given for the purpose of illustration of the present invention, and the present invention is not limited to the examples. Therefore, those skilled in the art can make insubstantial modifications and adaptations of the embodiments based on the above disclosure, and apply other embodiments within the scope of the invention.
Fig. 1 shows a structural diagram of a size-controllable water-soluble PbS/PbSe/ZnS core-shell structure quantum dot according to an embodiment of the present invention. As shown in fig. 1, the embodiment of the invention provides a size-controllable water-soluble PbS/PbSe/ZnS core-shell structure quantum dot. The core-shell structure quantum dot sequentially comprises the following components from inside to outside: the surface of the PbS core 1, the PbSe shell 2 and the ZnS shell 3 is wrapped with a hydrophilic ligand, and the hydrophilic ligand comprises at least one of thioglycolic acid, mercaptopropionic acid, L-cysteine, N-acetyl-L-cysteine, monothioglycerol, dithioglycerol, glutathione and sodium citrate and a combination thereof.
The embodiment of the invention also provides a preparation method of the size-controllable water-soluble PbS/PbSe/ZnS core-shell structure quantum dot. The preparation method starts at step S1: adding a stabilizer into a lead source aqueous solution, uniformly mixing, adjusting the pH value of the solution by using a pH regulator, introducing inert gas to remove oxygen for 20 minutes, quickly injecting a sulfur source aqueous solution under magnetic stirring, and reacting to form a PbS quantum dot solution with a hydrophilic ligand.
In some embodiments, the lead source is dissolved in water to prepare a solution with a concentration of 0.01-0.35mol/L, 1-20mL of stabilizer is added for stirring and mixing, the pH value is adjusted to 8-12, after inert gas is introduced for deoxygenation for 20 minutes, a sulfur source aqueous solution with a concentration of 0.01-0.25mol/L is rapidly injected under magnetic stirring, and the reaction is carried out for 1-10 minutes at a temperature of 25-40 ℃ to form the PbS quantum dot solution with the hydrophilic ligand.
In step S2: dissolving a selenium (Se) source in water to prepare a selenium source aqueous solution, adding the selenium source aqueous solution into the PbS quantum dot solution with the hydrophilic ligand formed in the step S1, heating the mixed solution in an inert gas atmosphere, quickly cooling to room temperature after the selenium source and the unreacted stabilizer and the lead source in the step S1 complete the reaction, carrying out post-treatment on the reaction stock solution to obtain the high-purity PbS/PbSe core-shell structure quantum dot, and dissolving the quantum dot in water for later use.
In some embodiments, the selenium source aqueous solution with the concentration of 0.05 to 0.5mol/L is added into the step S1, the mixed solution is heated to 30 to 120 ℃ under the inert gas atmosphere, the temperature is rapidly reduced to room temperature after the reaction is carried out for 1 to 10 minutes, the reaction stock solution is post-processed to obtain the high-purity PbS/PbSe core-shell structure quantum dots, and the quantum dots are dispersed in 20ml of water for later use.
And finally, in step S3, preparing a zinc source aqueous solution, injecting the quantum dot aqueous solution obtained in step S2 into the zinc source aqueous solution, stirring and heating the solution, finally injecting a stabilizer and a sulfur source aqueous solution, reacting the solution for a certain time, cooling the reaction product to room temperature, and performing precipitation, centrifugal separation and freeze drying on the reaction product to form the water-soluble PbS/PbSe/ZnS core-shell structure quantum dot with the surface coated with the hydrophilic ligand.
In some embodiments, 0.001-0.6mol/L of zinc source aqueous solution is prepared, the quantum dot aqueous solution obtained in the step S2 is injected into the zinc source aqueous solution, stirring and heating are carried out, 1-20mL of stabilizer and 0.01-0.25mol/L of sulfur source aqueous solution are finally injected, the mixture is reacted at the temperature of 60-100 ℃ for 1-4 hours and then cooled to the room temperature, and the water-soluble PbS/PbSe/ZnS core-shell structure quantum dot with the surface coated with the hydrophilic ligand is formed through precipitation, centrifugal separation and freeze drying.
Specific experiments will be carried out by using the preparation methods provided by the embodiments of the present invention, and specific experimental data are combined to further illustrate the feasibility and the progress of the embodiments of the present invention.
Example 1:
preparing the size-controllable water-soluble PbS/PbSe/ZnS core-shell structure quantum dot according to the following steps:
s1: dissolving 0.2mmol of lead acetate in 5mL of water to prepare a solution with the concentration of 0.04mol/L, adding 2mL of mercaptopropionic acid, stirring and mixing, adjusting the pH value of the solution to 11 by adopting triethylamine, introducing argon to remove oxygen for 20 minutes, quickly injecting 5mL of sodium sulfide aqueous solution with the concentration of 0.02mol/L under magnetic stirring, and reacting for 5 minutes at normal temperature to form a PbS quantum dot solution with a hydrophilic ligand;
s2: adding 1mL of sodium selenosulfate aqueous solution with the concentration of 0.1mol/L into the step S1, heating the mixed solution to 100 ℃ in an argon atmosphere, reacting for 1 minute, rapidly cooling to room temperature, carrying out post-treatment on the reaction stock solution to obtain high-purity PbS/PbSe core-shell structure quantum dots, and dispersing the quantum dots in 20mL of water for later use;
s3: preparing 2mL of zinc acetate aqueous solution with the concentration of 0.01mol/L, injecting the quantum dot aqueous solution obtained in the step S2 into the zinc acetate aqueous solution, stirring and heating, finally injecting 1mL of mercaptopropionic acid and 1mL of sodium sulfide aqueous solution with the concentration of 0.02mol/L, reacting at 80 ℃ for 1 hour, cooling to room temperature, and carrying out precipitation, centrifugal separation and freeze drying to form the water-soluble PbS/PbSe/ZnS core-shell structure quantum dot with the surface coated with the hydrophilic ligand, wherein FIG. 2 is a transmission electron microscope picture (the average particle size is 5nm) of the synthesized quantum dot. It was dispersed in 6ml of water and stored at 4 ℃ in a dark place.
Example 2:
preparing the size-controllable water-soluble PbS/PbSe/ZnS core-shell structure quantum dot according to the following steps:
s1: dissolving 0.2mmol of lead nitrate in 5mL of water to prepare a solution with the concentration of 0.04mol/L, adding 2mL of thioglycollic acid, stirring and mixing, adjusting the pH value of the solution to 10 by adopting sodium hydroxide, introducing nitrogen to remove oxygen for 20 minutes, quickly injecting 5mL of sodium sulfide aqueous solution with the concentration of 0.02mol/L under magnetic stirring, and reacting for 6 minutes at normal temperature to form a PbS quantum dot solution with a hydrophilic ligand;
s2: adding 1mL of sodium selenosulfate aqueous solution with the concentration of 0.1mol/L into the step S1, heating the mixed solution to 100 ℃ in the nitrogen atmosphere, reacting for 2 minutes, rapidly cooling to room temperature, carrying out post-treatment on the reaction stock solution to obtain high-purity PbS/PbSe core-shell structure quantum dots, and dispersing the quantum dots in 20mL of water for later use;
s3: preparing 2mL of zinc sulfate aqueous solution with the concentration of 0.01mol/L, injecting the quantum dot aqueous solution obtained in the step S2 into the zinc sulfate aqueous solution, stirring and heating, finally injecting 1mL of thioglycolic acid and 1mL of sodium sulfide aqueous solution with the concentration of 0.02mol/L, reacting at 100 ℃ for 2 hours, cooling to room temperature, carrying out precipitation, centrifugal separation and freeze drying to form the water-soluble PbS/PbSe/ZnS core-shell structure quantum dot with the surface coated with the hydrophilic ligand, dispersing the quantum dot in 6mL of water, and keeping the quantum dot in a dark place at 4 ℃ for sealed storage.
The above description is intended to be illustrative and not restrictive. For example, the above-described examples (or one or more versions thereof) may be used in combination with each other. For example, other embodiments may be used by those of ordinary skill in the art upon reading the above description. In addition, in the foregoing detailed description, various features may be grouped together to streamline the disclosure. This should not be interpreted as an intention that a disclosed feature not claimed is essential to any claim. Rather, inventive subject matter may lie in less than all features of a particular disclosed embodiment. Thus, the following claims are hereby incorporated into the detailed description as examples or embodiments, with each claim standing on its own as a separate embodiment, and it is contemplated that these embodiments may be combined with each other in various combinations or permutations. The scope of the invention should be determined with reference to the appended claims, along with the full scope of equivalents to which such claims are entitled.
Claims (10)
1. The size-controllable water-soluble PbS/PbSe/ZnS core-shell structure quantum dot is characterized in that the core-shell structure quantum dot takes PbS as a core and PbSe and ZnS as shell layers, the surface of the core-shell structure quantum dot is wrapped by a hydrophilic ligand, and the hydrophilic ligand comprises at least one of thioglycolic acid, mercaptopropionic acid, L-cysteine, N-acetyl-L-cysteine, monothioglycerol, dithioglycerol, glutathione and sodium citrate.
2. A preparation method of a size-controllable water-soluble PbS/PbSe/ZnS core-shell structure quantum dot is characterized by comprising the following steps:
s1, adding a stabilizer into the lead source aqueous solution, uniformly mixing to obtain a first mixed solution, adjusting the pH value of the first mixed solution, deoxidizing, and then injecting the sulfur source aqueous solution under magnetic stirring to react to form a PbS quantum dot solution with hydrophilic ligands;
s2, adding a selenium source aqueous solution into the PbS quantum dot solution to obtain a second mixed solution, heating the second mixed solution in an inert gas atmosphere, after the selenium source and a stabilizer and a lead source in the PbS quantum dot solution are reacted, rapidly cooling to room temperature, performing post-treatment to obtain PbS/PbSe core-shell structure quantum dots, and dissolving the PbS/PbSe core-shell structure quantum dots in water to obtain a PbS/PbSe quantum dot aqueous solution;
and S3, injecting the aqueous solution of PbS/PbSe quantum dots into the aqueous solution of zinc source, stirring and heating, finally injecting a stabilizer and an aqueous solution of sulfur source, reacting for a certain time, cooling to room temperature, and performing precipitation, centrifugal separation and freeze drying to form the water-soluble PbS/PbSe/ZnS core-shell structure quantum dots with the surfaces wrapped by hydrophilic ligands.
3. The preparation method of the core-shell structure quantum dot according to claim 2, wherein the lead source aqueous solution is prepared by dissolving a lead source in water, and the lead source comprises one of lead acetate, lead nitrate, lead oxide or a mixture thereof.
4. The preparation method of the quantum dot with the core-shell structure according to claim 2, wherein the stabilizer comprises one of thioglycolic acid, mercaptopropionic acid, L-cysteine, N-acetyl-L-cysteine, monothioglycerol, dithioglycerol, glutathione, sodium citrate or a mixture thereof.
5. The preparation method of the core-shell quantum dot according to claim 2, wherein the adjusting the pH value of the first mixed solution comprises:
and adjusting the pH value of the first mixed solution to 8-12 by using a pH adjusting agent, wherein the pH adjusting agent comprises one of sodium hydroxide solution, triethylamine, ammonia water and a combination thereof.
6. The preparation method of the core-shell structure quantum dot according to claim 2, wherein the sulfur source aqueous solution is prepared by dissolving a sulfur source in water, and the sulfur source comprises one of sodium sulfide, sulfur powder or a mixture thereof.
7. The preparation method of the core-shell structure quantum dot according to claim 2, wherein the selenium source aqueous solution is prepared by dissolving a selenium source in water, and the selenium source comprises one or a mixture of selenium powder, sodium selenosulfate and selenium oxide.
8. The preparation method of the core-shell quantum dot according to claim 2, wherein the zinc source aqueous solution is prepared by dissolving a zinc source in water, and the zinc source comprises one of zinc acetate, zinc nitrate, zinc chloride, zinc sulfate or a mixture thereof.
9. The preparation method of the core-shell structure quantum dot according to claim 2, wherein the steps S1-S3 all provide an ultraviolet lamp as a reaction medium, the wavelength of the ultraviolet lamp is 320nm, and the ultraviolet lamp is annularly arranged on the periphery of the reaction equipment and is used for avoiding partial quantum reaction incomplete condition through observation and identification in the reaction process.
10. The method for preparing the core-shell quantum dot according to claim 2, wherein the molar ratio of lead to sulfur in the step S1 is: 1-5:1, the molar ratio of sulfur in step S1 to selenium in step S2 is: 1-6:1, the molar ratio of zinc in step S3 to selenium in step S2 is: 1:1-5.
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| CN104297306A (en) * | 2014-09-30 | 2015-01-21 | 江南大学 | Multifunctional photoelectrochemical sensor based on G-tetrahedron/hemin |
| CN110878202A (en) * | 2019-11-12 | 2020-03-13 | 重庆大学 | In-situ synthesis method of PbS/ZnS core-shell structure quantum dots |
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|---|---|---|---|---|
| CN104297306A (en) * | 2014-09-30 | 2015-01-21 | 江南大学 | Multifunctional photoelectrochemical sensor based on G-tetrahedron/hemin |
| CN110878202A (en) * | 2019-11-12 | 2020-03-13 | 重庆大学 | In-situ synthesis method of PbS/ZnS core-shell structure quantum dots |
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