CN110684534B - Method for preparing near-infrared cadmium telluride quantum dots in hydrothermal mode - Google Patents
Method for preparing near-infrared cadmium telluride quantum dots in hydrothermal mode Download PDFInfo
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- CN110684534B CN110684534B CN201910884329.1A CN201910884329A CN110684534B CN 110684534 B CN110684534 B CN 110684534B CN 201910884329 A CN201910884329 A CN 201910884329A CN 110684534 B CN110684534 B CN 110684534B
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Abstract
The invention discloses a method for preparing near-infrared cadmium telluride quantum dots in a hydrothermal mode, which comprises the following steps: respectively adding a cadmium salt solution and a sulfhydryl ligand into an aqueous solution, and uniformly mixing to obtain a mixed solution, wherein the molar ratio of the sulfhydryl ligand to the cadmium salt is 2-4: 1; adjusting the pH value of the mixed solution to 9-11, introducing nitrogen for more than 30 minutes, then adding a sodium hydrogen telluride aqueous solution, and uniformly mixing to obtain a cadmium telluride precursor solution, wherein the molar ratio of sodium hydrogen telluride to cadmium ions is 0.1-0.2: 1; heating the cadmium telluride precursor solution for 5 minutes, adding a precipitator, centrifuging, removing supernatant, and adding water for re-dissolving; and adding a cadmium salt solution and a sulfhydryl ligand into the dissolved cadmium telluride quantum dots, wherein the molar ratio of mercaptopropionic acid to cadmium chloride is 2-4: 1, adjusting the pH value of the mixed solution to 9-11, and heating for a period of time to obtain the near-infrared luminescent cadmium telluride quantum dots. The method can be used for preparing the near-infrared cadmium telluride quantum dots, and the obtained cadmium telluride quantum dots have good lattice structures.
Description
Technical Field
The invention relates to the field of preparation of water-soluble quantum dots, in particular to a method for preparing near-infrared cadmium telluride quantum dots in a hydrothermal mode.
Background
The cadmium telluride quantum dot belongs to a nanocrystal consisting of II-VI group elements, and is a spherical crystal with the diameter of less than 10 nanometers. As a luminescent material, the cadmium telluride quantum dot has good optical stability, wide excitation spectrum, narrow emission spectrum and luminescent wavelength in a visible light region (400-700 nm), and can be widely applied to various fields. But in the fields of fluorescent labeling of biological cells, in vivo imaging of animals, etc., biological compounds and tissues specifically absorb and scatter incident light to varying degrees. Only near infrared light (700-900 nm) wave band has higher spatial resolution, deeper depth penetrating biological matrix and lower optical absorption and scattering. Thus, biomarkers and imaging must work in specific regions of the electromagnetic spectrum to improve imaging.
The traditional method for preparing the cadmium telluride quantum dots by a hydrothermal method is influenced by the boiling point of solvent water, the energy obtained by a reaction system is relatively low, the quantum dots have long growth time and do not emit light after reaching a certain size, so that the near-infrared light-emitting water-soluble cadmium telluride quantum dots are difficult to obtain. In order to prepare the near-infrared luminescent cadmium telluride quantum dot, the prior art generally provides additional energy for the preparation process by technical means such as auxiliary microwave, ultrasonic, UV irradiation and the like, and the complexity of the preparation process is increased to a certain extent.
Therefore, in order to overcome the above-mentioned drawbacks of the prior art, there is a need to provide a simple and convenient solution for preparing a near-infrared luminescent cadmium telluride quantum dot without using additional reactants and auxiliary means.
Disclosure of Invention
The invention aims to provide a hydrothermal preparation method of a near-infrared luminescent cadmium telluride quantum dot, which solves the problem of limitation of the luminescent range of the traditional preparation method of water-soluble quantum dots.
In order to solve the problems, the invention adopts the following technical scheme:
step one, respectively adding a cadmium salt solution and a sulfhydryl ligand into an aqueous solution, and uniformly mixing to obtain a mixed solution, wherein the molar ratio of the sulfhydryl ligand to cadmium ions is 2-4: 1;
step two, adjusting the pH value of the mixed solution obtained in the step one to 9-11, introducing nitrogen for more than 30 minutes, then adding a sodium hydrogen telluride aqueous solution, and uniformly mixing to obtain a cadmium telluride precursor solution, wherein the molar ratio of sodium hydrogen telluride to cadmium ions is 0.1-0.2: 1;
step three, heating the cadmium telluride precursor solution for 5 minutes, adding a precipitator, centrifuging, removing supernatant, adding water, and dispersing again;
and step four, adding a cadmium salt solution and a sulfhydryl ligand into the dispersed cadmium telluride quantum dots, adjusting the pH value to 9-11, and heating for a period of time to obtain the near-infrared luminous cadmium telluride quantum dots, wherein the molar ratio of the sulfhydryl ligand to cadmium chloride is 2-4: 1.
By adopting the technical scheme, the small-size quantum dot solution is centrifugally redispersed, the monomer (Cd-SR) remained in the solution is removed, and then the monomer is added again, so that the electrostatic repulsion among the quantum dots is reduced, the Ostwald ripening growth of the quantum dots is promoted, and the near-infrared luminescent cadmium telluride quantum dots are obtained.
Further, the cadmium salt solution is prepared from water-soluble cadmium salt, and the water-soluble cadmium salt is any one of cadmium chloride, cadmium bromide or cadmium nitrate.
Further, the sulfhydryl ligand is one or more of thioglycolic acid, mercaptopropionic acid, mercaptobutyric acid, thioglycolate, mercaptopropionate or mercaptobutyrate.
Further, in the second step and the fourth step, the pH value of the mixed solution is adjusted by adopting a sodium hydroxide aqueous solution or a potassium hydroxide aqueous solution.
Further, in the second step, the preparation method of the sodium hydrogen telluride aqueous solution comprises the following steps: dissolving sodium borohydride in deionized water, and rapidly adding tellurium powder; sealing the reaction vessel by a rubber plug, wherein the rubber plug is provided with a small pinhole communicated with the outside so as to release hydrogen generated by the reaction; in the reaction process, the system is cooled by using an ice-water bath, then black tellurium powder disappears and white sodium borate crystals are generated, and the upper clear light purple solution is a sodium hydrogen telluride aqueous solution.
Furthermore, in the third step, one or more of ethanol, isopropanol, potassium salt or sodium salt is used as a precipitator.
The invention has the beneficial effects that:
1. different from the microwave-assisted method adopted in the prior art, the invention can prepare cadmium telluride quantum dots by a hydrothermal method, removes the residual monomer (Cd-SR) in the solution by centrifugally re-dispersing the small-size quantum dot solution, then re-adds the monomer, reduces the electrostatic repulsion among the quantum dots, promotes the Ostwald ripening growth of the quantum dots, and thus obtains the near-infrared luminescent cadmium telluride quantum dots.
2. The water-soluble cadmium telluride quantum dot obtained by the method has a good lattice structure. The cadmium telluride quantum dots are in a polydisperse spherical-like particle shape and have a regular crystal form.
3. The method has the advantages of simple equipment, low energy consumption, easy operation, no danger, convenient raw material supply and low raw material price.
Drawings
FIG. 1 shows fluorescence peak positions of quantum dots obtained in example 1 by heating for different times.
FIG. 2 is a graph showing the relationship between the heating time and the fluorescence peak position in example 1.
Detailed Description
The invention is explained in more detail below with reference to exemplary embodiments and the accompanying drawings. The following examples are not intended to limit the present invention in any way, and all technical solutions obtained by means of equivalent substitution or equivalent transformation are within the scope of the present invention.
In order to overcome the defects in the prior art, the invention provides a method for preparing near-infrared cadmium telluride quantum dots in a hydrothermal mode, which comprises the following steps:
step one, respectively adding a cadmium salt solution and a sulfhydryl ligand into an aqueous solution, and uniformly mixing to obtain a mixed solution, wherein the molar ratio of the sulfhydryl ligand to cadmium ions is 2-4: 1;
step two, adjusting the pH value of the mixed solution obtained in the step one to 9-11, introducing nitrogen for more than 30 minutes, then adding a sodium hydrogen telluride aqueous solution, and uniformly mixing to obtain a cadmium telluride precursor solution, wherein the molar ratio of sodium hydrogen telluride to cadmium ions is 0.1-0.2: 1;
step three, heating the cadmium telluride precursor solution for 5 minutes, adding a precipitator, centrifuging, removing supernatant, adding water, and dispersing again;
and step four, adding a cadmium salt solution and a sulfhydryl ligand into the dispersed cadmium telluride quantum dots, adjusting the pH value to 9-11, and heating for a period of time to obtain the near-infrared luminous cadmium telluride quantum dots, wherein the molar ratio of the sulfhydryl ligand to cadmium chloride is 2-4: 1.
By adopting the technical scheme, the small-size quantum dot solution is centrifugally redispersed, the monomer (Cd-SR) remained in the solution is removed, and then the monomer is added again, so that the electrostatic repulsion among the quantum dots is reduced, the Ostwald ripening growth of the quantum dots is promoted, and the near-infrared luminescent cadmium telluride quantum dots are obtained.
The technical solution of the present invention is described in detail below with reference to specific examples.
Example 1
a. 0.5mL of 0.1M aqueous solution of cadmium chloride and 10uL of mercaptopropionic acid solution were added to 4.5mL of water, and stirred uniformly.
b. The pH of the mixed solution was adjusted to 9.1 with an aqueous solution of sodium hydroxide having a concentration of 1.0M, and then nitrogen gas was introduced for 30 minutes. 15uL of the prepared 0.667M sodium hydrogen telluride solution is injected to obtain the precursor solution of cadmium telluride. In the embodiment, the molar ratio of the cadmium chloride to the mercaptopropionic acid to the sodium hydrogen telluride is 1:2.4:0.2, and the concentration of cadmium ions is 10 mM.
c. And heating the precursor solution for five minutes, adding 3mL of isopropanol, mixing, centrifuging, removing a supernatant, and dispersing the precipitated quantum dots in 200mL of deionized water.
d. 0.5mL of a cadmium chloride solution and 10uL of a mercaptopropionic acid solution were added, and the pH of the mixed solution was adjusted to 9.1 with a 1.0M aqueous solution of sodium hydroxide. Heating for 4 hours to obtain the water-soluble cadmium telluride quantum dots with the fluorescence peak position of 700nm, and continuously heating to obtain the near-infrared luminous water-soluble cadmium telluride quantum dots with different fluorescence peak positions. Specifically, refer to fig. 1 and fig. 2, where fig. 1 is a fluorescence peak position of the quantum dot obtained by heating in this embodiment for different time. FIG. 2 is a graph showing the relationship between the heating time and the fluorescence peak position in this example.
Example 2
a. 5mL of 0.1M aqueous cadmium chloride solution and 0.1mL of mercaptopropionic acid solution were added to 45mL of water and stirred uniformly.
b. The pH of the mixed solution was adjusted to 9.1 with an aqueous solution of sodium hydroxide having a concentration of 1.0M, and then nitrogen gas was introduced for 30 minutes. And injecting 0.15mL of the just prepared 0.667M sodium hydrogen telluride solution to obtain a precursor solution of cadmium telluride. In the embodiment, the molar ratio of the cadmium chloride to the mercaptopropionic acid to the sodium hydrogen telluride is 1:2.4:0.2, and the concentration of cadmium ions is 10 mM.
c. And heating the precursor solution for five minutes, adding 30mL of isopropanol, mixing, centrifuging, removing a supernatant, and dispersing the precipitated quantum dots in 200mL of deionized water.
d. 6.8mL of a cadmium chloride solution and 140uL of a mercaptopropionic acid solution were added, and the pH of the mixed solution was adjusted to 9.1 with a 1.0M aqueous solution of sodium hydroxide. Heating for 3.5 hours to obtain the water-soluble cadmium telluride quantum dots with the fluorescence peak position of 700nm, and continuously heating to obtain the near-infrared luminous water-soluble cadmium telluride quantum dots with different fluorescence peak positions. Specifically, refer to fig. 1 and fig. 2, where fig. 1 is a fluorescence peak position of the quantum dot obtained by heating in this embodiment for different time. FIG. 2 is a graph showing the relationship between the heating time and the fluorescence peak position in this example.
Example 3
a. 10mL of 0.1M aqueous solution of cadmium chloride and 140uL of thioglycolic acid were added to 50mL of water, and the mixture was stirred well.
b. The pH of the mixed solution was adjusted to 11 with an aqueous solution of sodium hydroxide having a concentration of 1.0M, and then nitrogen gas was introduced for 30 minutes. After 150uL of the just prepared 0.667M sodium hydrogen telluride solution is injected, the precursor solution of cadmium telluride can be obtained. In the embodiment, the molar ratio of the cadmium chloride to the thioglycolic acid to the sodium hydrogen telluride is 1:2:0.1, and the concentration of cadmium ions is 16.7 mM.
c. And heating the precursor solution for five minutes, adding 40mL of isopropanol, mixing, centrifuging, removing a supernatant, and dispersing the precipitated quantum dots in 200mL of deionized water.
d. 5mL of a cadmium chloride solution and 70uL of a mercaptopropionic acid solution were added, and the pH of the mixed solution was adjusted to 11 with a 1.0M aqueous solution of sodium hydroxide. Heating for 20 hours to obtain the water-soluble cadmium telluride quantum dot with the fluorescence peak position of 700 nm. Specifically, refer to fig. 1 and fig. 2, where fig. 1 is a fluorescence peak position of the quantum dot obtained by heating in this embodiment for different time. FIG. 2 is a graph showing the relationship between the heating time and the fluorescence peak position in this example.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. The method for preparing the near-infrared cadmium telluride quantum dot by the hydrothermal method is characterized by comprising the following steps:
step one, respectively adding a cadmium salt solution and a sulfhydryl ligand into an aqueous solution, and uniformly mixing to obtain a mixed solution, wherein the molar ratio of the sulfhydryl ligand to cadmium ions is 2-4: 1;
step two, adjusting the pH value of the mixed solution obtained in the step one to 9-11, introducing nitrogen for more than 30 minutes, then adding a sodium hydrogen telluride aqueous solution, and uniformly mixing to obtain a cadmium telluride precursor solution, wherein the molar ratio of sodium hydrogen telluride to cadmium ions is 0.1-0.2: 1;
step three, heating the cadmium telluride precursor solution for 5 minutes, adding a precipitator, centrifuging, removing supernatant, adding water, and dispersing again;
and step four, adding a cadmium salt solution and a sulfhydryl ligand into the dispersed cadmium telluride quantum dots, adjusting the pH value to 9-11, and heating for a period of time to obtain the near-infrared luminous cadmium telluride quantum dots, wherein the molar ratio of the sulfhydryl ligand to cadmium chloride is 2-4: 1.
2. The hydrothermal preparation method of near-infrared cadmium telluride quantum dots as claimed in claim 1, wherein the cadmium salt solution is prepared by using water-soluble cadmium salt, and the water-soluble cadmium salt is any one of cadmium chloride, cadmium bromide or cadmium nitrate.
3. The hydrothermal method for preparing near-infrared cadmium telluride quantum dots according to claim 1, wherein the mercapto ligand is one or more of thioglycolic acid, mercaptopropionic acid, mercaptobutyric acid, thioglycolate, mercaptopropionate or mercaptobutyrate.
4. The hydrothermal preparation method of near-infrared cadmium telluride quantum dots according to claim 1 wherein in step two and step four, sodium hydroxide aqueous solution or potassium hydroxide aqueous solution is used to adjust the pH value of the mixed solution.
5. The hydrothermal preparation method of near-infrared cadmium telluride quantum dots as claimed in claim 1, wherein in the second step, the preparation method of the sodium hydrogen telluride aqueous solution comprises the following steps: dissolving sodium borohydride in deionized water, and rapidly adding tellurium powder; sealing the reaction vessel by a rubber plug, wherein the rubber plug is provided with a small pinhole communicated with the outside so as to release hydrogen generated by the reaction; in the reaction process, the system is cooled by using an ice-water bath, then black tellurium powder disappears and white sodium borate crystals are generated, and the upper clear light purple solution is a sodium hydrogen telluride aqueous solution.
6. The hydrothermal method for preparing near-infrared cadmium telluride quantum dots according to claim 1, wherein one or more of ethanol, isopropanol, potassium salt or sodium salt is adopted as a precipitant in the third step.
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