CN112877062B - Near-infrared silver copper sulfur quantum dot and preparation method and application thereof - Google Patents
Near-infrared silver copper sulfur quantum dot and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a near-infrared silver copper sulfur quantum dot and a preparation method and application thereof. The preparation method comprises the following steps: reacting a first mixed reaction system containing a silver source, mercaptan and a selectively added or not added weak polar solvent in a closed environment to prepare a precursor solution of silver; and carrying out solvothermal reaction on a second mixed reaction system containing the silver precursor solution and the copper source at 180-255 ℃ to obtain the near-infrared silver copper sulfur quantum dots, wherein the wavelength of a fluorescence emission peak of the near-infrared silver copper sulfur quantum dots is 800-1160 nm. The silver-copper-sulfur quantum dot is prepared by a simple high-temperature solvothermal method, the synthesis process is simple and controllable, the yield is high, the large-scale preparation can be realized, the fluorescence emission is near infrared, the quantum efficiency is high, the light stability is excellent, and the silver-copper-sulfur quantum dot has wide application prospects in the fields of biological imaging, near infrared devices and the like.
Description
Technical Field
The invention relates to a near-infrared quantum dot and a preparation method thereof, in particular to a near-infrared silver-copper-sulfur quantum dot and a preparation method and application thereof, belonging to the technical field of material science.
Background
In-vivo noninvasive imaging plays an increasingly important role in biomedical research and clinical practice, wherein the fluorescence imaging technology has the advantages of non-contact, visual image, real-time performance, high sensitivity, economy, convenience, no radiation hazard and the like, and has wide application prospect in the field of biomedicine, particularly in the aspect of fluorescence image surgical navigation.
The visible fluorescence imaging wavelength range (400-650 nm) has serious biological autofluorescence interference, and living tissues (including skin, blood, fat and the like) have strong absorption and scattering effects on photons in the wave band, so that the extremely limited penetration depth (less than 3 mm) and spatial resolution (about 1000 μm) cannot meet the imaging requirement under deep tissues. In comparison, biological tissues have weak absorption and scattering effects on near infrared light and strong penetration capability, so that near infrared fluorescence imaging technology has attracted much attention in recent years.
The quantum dot as an excellent near-infrared fluorescent probe has the following characteristics in vivo imaging research: high biocompatibility, high quantum efficiency, tunable excitation and emission wavelengths and easy surface functionalization. Therefore, the development of the high-quality near-infrared quantum dot with simple process, high fluorescence intensity and adjustable spectrum is very important, so that the high-quality near-infrared quantum dot can be applied to the field of biological or fluorescent devices and has important significance.
Disclosure of Invention
The invention mainly aims to provide a near-infrared silver copper sulfur quantum dot and a preparation method thereof, thereby overcoming the defects in the prior art.
The invention also aims to provide application of the near-infrared silver copper sulfur quantum dots.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a preparation method of near-infrared silver, copper and sulfur quantum dots, which comprises the following steps:
reacting a first mixed reaction system containing a silver source, mercaptan and a selectively added or not added weak polar solvent in a closed environment to prepare a precursor solution of silver;
and carrying out solvothermal reaction on the precursor solution containing silver and a second mixed reaction system of a copper source at 180-255 ℃ to obtain the near-infrared silver-copper-sulfur quantum dots.
In some embodiments, the preparation method specifically comprises: uniformly mixing a silver source, mercaptan and a weak polar solvent to form the first mixed reaction system, and then heating the first mixed reaction system to 80-120 ℃ in a closed environment to react for less than 1h to prepare a silver precursor solution.
In some embodiments, the method of making specifically comprises: under the condition of continuous stirring, adding a copper source into the silver precursor solution with the temperature of 80-120 ℃ to form the second mixed reaction system, and then heating to 180-255 ℃ to perform solvothermal reaction for 2-600 min to obtain the near-infrared silver copper sulfur quantum dots.
The embodiment of the invention also provides the near-infrared silver copper sulfur quantum dot prepared by the method.
Furthermore, the diameter of the near-infrared silver copper sulfur quantum dot is 2-25 nm, and the size distribution is uniform.
Furthermore, the wavelength of the fluorescence emission peak of the near-infrared silver copper sulfur quantum dot is 800-1160 nm.
The embodiment of the invention also provides application of any near-infrared silver copper sulfur quantum dot in the fields of biological imaging, biomedicine or near-infrared devices (such as near-infrared light-emitting diodes) and the like.
Compared with the prior art, the invention has the beneficial effects that:
1) The preparation process of the near-infrared silver copper sulfur quantum dots provided by the invention is a solvothermal reaction, the steps are simple, the experimental conditions are controllable, the used reagents are simple and easy to obtain, the yield of the final product is high, and the preparation method is suitable for large-scale production;
2) The final product near-infrared silver copper sulfur fluorescent quantum dots prepared by the method disclosed by the invention are uniform in size distribution, the fluorescence emission is 800-1160 nm, and the fluorescent quantum dots do not contain any toxic heavy metal element, have higher quantum efficiency and superior light stability, and have wide application prospects in the fields of biological imaging, near-infrared devices and the like;
3) The preparation process can be expanded to other preparation processes of near-infrared fluorescent quantum dots, and is high in yield and easy to amplify reaction scale.
Drawings
In order to more clearly illustrate the technical solutions of the present invention, the drawings used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings described below are only used as some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a TEM image of the NIR silver-copper-sulfur fluorescent quantum dots in example 1 of the present invention;
FIG. 2 is a fluorescence emission spectrum of the near-infrared silver-copper-sulfur fluorescent quantum dots in example 2 of the present invention.
Detailed Description
As mentioned above, in view of the defects of the prior art, the present inventors have made extensive studies and practice to propose the technical solution of the present invention, which mainly comprises: taking a silver source, mercaptan and a copper source as reactants, and carrying out nucleation and growth in a reaction system with surfactants with different coordination characteristics to obtain the silver-copper-sulfur quantum dot, wherein the mercaptan provides a sulfur source and can be used as a solvent and the surfactant. The technical solution of the present invention will be explained in more detail as follows.
Specifically, the process of the invention comprises the following steps: mixing a silver source, mercaptan and a proper surfactant, placing the mixture in a closed device, and heating the mixture to a proper temperature until the mixture is clear and transparent; and then, quickly adding a copper source to a proper temperature for a proper time of reaction, then cooling, adding excessive ethanol or acetone, centrifuging and washing to obtain the silver-copper-sulfur quantum dot. Then mixing the prepared hydrophobic silver copper sulfur quantum dots, a certain amount of hydrophilic reagent (such as mercaptopropionic acid) containing sulfydryl and ethanol, stirring, shaking or ultrasonically reacting the hydrophobic silver copper sulfur quantum dots, performing centrifugal washing by using water to obtain the low-toxicity near-infrared silver copper sulfur quantum dots with high fluorescence yield and good biocompatibility, and finally performing biological imaging.
As one aspect of the technical scheme of the invention, the related preparation method of the near-infrared silver copper sulfur quantum dot comprises the following steps:
reacting a first mixed reaction system containing a silver source, mercaptan and a selectively added or not added weak polar solvent in a closed environment to prepare a precursor solution of silver;
and carrying out solvothermal reaction on the second mixed reaction system containing the silver precursor solution and the copper source at 180-255 ℃ to obtain the near-infrared silver copper sulfur quantum dots.
In some embodiments, the method of making consists essentially of: and uniformly mixing a silver source, mercaptan and a weak polar solvent to prepare a clear silver precursor solution, and then adding a copper source into the silver precursor solution to prepare the silver-copper-sulfur quantum dots, wherein the wavelength of a fluorescence emission peak of the quantum dots is 800-1160 nm.
In some preferred embodiments, the preparation method of the near-infrared silver copper sulfur quantum dot may specifically include:
heating a mixed reaction system containing a silver source, mercaptan and a weak polar solvent to 80-120 ℃ in a closed environment to prepare a precursor solution of silver;
and adding a copper source into the silver precursor solution at 80-120 ℃ under stirring, and heating to 180-255 ℃ for reaction to obtain the silver-copper-sulfur fluorescent quantum dot.
Further, the preparation method may specifically include: taking a mixed system of a silver source, mercaptan and a weak polar solvent, and carrying out ultrasonic uniform dispersion; then adding the mixed system to 80-120 ℃ until the solution is transparent and clear; and then quickly adding a copper source into the mixed solution, heating to 180-255 ℃ and reacting for a proper time to obtain the silver-copper-sulfur fluorescent quantum dots with the diameter of 2-25 nm, wherein the fluorescence emission peak of the silver-copper-sulfur fluorescent quantum dots is 800-1160 nm.
In some embodiments, the method of preparation may specifically comprise: uniformly mixing a silver source, mercaptan and a weak-polarity solvent to form the first mixed reaction system, and then heating the first mixed reaction system to 80-120 ℃ in a closed environment to react for 1 hour, thereby preparing a precursor solution of silver.
In some embodiments, the molar ratio of the silver source to the thiol is from 1:1 to 1000000.
In some embodiments, the preparation method may specifically include: under the condition of continuous stirring, adding a copper source into the silver precursor solution with the temperature of 80-120 ℃ to form the second mixed reaction system, and then heating to 180-255 ℃ to perform solvothermal reaction for 2-600 min to obtain the near-infrared silver copper sulfur quantum dots.
In some embodiments, the method of making further comprises: and after the reaction is finished, adding a polar amphoteric solvent, washing and centrifuging to obtain the silver-copper-sulfur fluorescent quantum dots.
In some embodiments, the molar ratio of the silver source to the copper source is from 0.8:1 to 1: 0.65.
In some embodiments, the silver salt includes any one or a combination of two or more of silver nitrate, silver acetate, silver trifluoroacetate, silver diethyldithiocarbamate, and the like, but is not limited thereto.
In some embodiments, the thiol includes any one or a combination of two or more of dodecanethiol, octanethiol, octadecanethiol, and the like, but is not limited thereto.
In some embodiments, the weakly polar solvent includes any one or a combination of two or more of oleylamine, oleic acid, octadecene, octadecylamine, dodecylamine, tetradecylamine, and the like, or the weakly polar solvent is selected not to be added, but is not limited thereto.
In some embodiments, the copper source includes any one or a combination of two or more of copper nitrate, copper chloride, copper sulfate, copper acetate, copper diethyldithiocarbamate, and the like, but is not limited thereto.
As a more specific embodiment, the preparation method of the near-infrared silver-copper-sulfur quantum dot may include the following steps:
I. taking a mixed system of a silver source, mercaptan and a weak polar solvent, and carrying out ultrasonic uniform dispersion;
II. Then adding the mixed system to 80-120 ℃ until the solution is transparent and clear;
III, quickly adding a copper source into the mixed solution, and heating to 180-255 ℃ for reacting for a proper time, preferably 2-600 min;
IV, separating a product obtained by the solvothermal reaction in the step III, cleaning and drying to obtain the near-infrared silver-copper-sulfur quantum dots.
The final product near-infrared silver copper sulfur fluorescent quantum dots prepared by the method disclosed by the invention are uniform in size distribution, the emission peak wavelength is 800-1160 nm, the quantum efficiency is higher, and the final product near-infrared silver copper sulfur fluorescent quantum dots do not contain any toxic heavy metal elements. And the yield of the final product is high, and the preparation process is easy to enlarge the reaction scale.
Furthermore, the preparation process of the near-infrared silver copper sulfur quantum dot is a solvothermal reaction, the steps are simple, the experimental conditions are controllable, the used reagents are simple and easy to obtain, the yield of the final product is high, the method is suitable for large-scale production, the preparation method can be expanded to other preparation processes of near-infrared fluorescent quantum dots, the yield is high, and the reaction scale is easy to amplify.
As another aspect of the technical scheme, the invention also relates to the near-infrared silver copper selenium fluorescent quantum dot prepared by the method.
Furthermore, the diameter of the near-infrared silver copper sulfur quantum dot is 2-25 nm, and the size distribution is uniform.
Furthermore, the fluorescence emission peak of the near-infrared silver copper sulfur fluorescence quantum dot is positioned between 800 and 1160nm.
As another aspect of the technical scheme, the invention also provides a near-infrared silver-copper-selenium fluorescent quantum dot which is uniform in appearance and size, high in absolute quantum yield, free of any toxic heavy metal element and has important application prospects in the fields of biological imaging, biomedicine or near-infrared devices and the like.
Another aspect of the embodiments of the present invention also provides a use of any one of the aforementioned near-infrared silver-copper-selenium quantum dots in fields of biological imaging, biomedicine, or near-infrared devices, and the like.
Further, the near infrared device may be a near infrared light emitting diode, but is not limited thereto.
Further, the use comprises: mixing the prepared hydrophobic silver copper sulfur quantum dots, a certain amount of hydrophilic reagent (such as mercaptopropionic acid) containing sulfydryl and ethanol, stirring, shaking or ultrasonically reacting the hydrophobic silver copper sulfur quantum dots, performing centrifugal washing by using water to obtain the high-fluorescence-yield near-infrared silver copper sulfur quantum dots with low toxicity and good biocompatibility, and finally performing biological imaging.
In conclusion, by the technical scheme, the silver-copper-sulfur quantum dots are prepared by a simple high-temperature solvothermal method, the synthesis process is simple and controllable, the yield is high, the silver-copper-sulfur quantum dots can be prepared in a large scale, the fluorescence emission is near infrared, the quantum efficiency is high, the light stability is excellent, and the silver-copper-sulfur quantum dots have wide application prospects in the fields of biological imaging, near infrared devices and the like.
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention are further described in detail with reference to some preferred embodiments, but the present invention is not limited to the following embodiments, and those skilled in the art can make insubstantial improvements and modifications within the spirit of the present invention and still fall within the scope of the present invention. Unless otherwise specified, various reagents used in the following examples are well known to those skilled in the art and can be obtained by means of commercial sources and the like. However, the experimental methods in the following examples, in which specific conditions are not specified, are generally performed under conventional conditions or under conditions recommended by the manufacturers.
Example 1
Mixing 0.1mmol of silver acetate, 5mmol of octanethiol and 10mL of octadecene, ultrasonically dispersing uniformly, slowly heating to 80 ℃ for reaction for 1h to obtain a clear and transparent silver precursor solution, then adding 0.065mmol of copper diethyldithiocarbamate, heating to 230 ℃ for reaction for 2h to obtain the silver-copper-sulfur fluorescent quantum dot.
Referring to fig. 1, a transmission electron micrograph of the near-infrared silver copper sulfide fluorescence quantum dot in this embodiment is shown, and it can be seen from fig. 1 that the near-infrared silver copper sulfide fluorescence quantum dot product obtained in this embodiment has a uniform morphology and a uniform size, the size is about 18nm, and the fluorescence wavelength is 1100nm.
Example 2
Uniformly dispersing 0.1mmol of silver nitrate and 20000mmol of dodecanethiol by ultrasonic, slowly heating to 100 ℃ to obtain a clear and transparent silver precursor solution, adding 0.1mmol of copper acetate, and reacting at 180 ℃ for 600min to obtain the silver-copper-sulfur fluorescent quantum dot.
Please refer to fig. 2, which shows a fluorescence emission spectrum of the near-infrared silver-copper-sulfur fluorescent quantum dot in this embodiment.
Example 3
Mixing 0.04mmol of silver diethyldithiocarbamate, 0.04mmol of dodecanethiol and 20mL of octadecylamine, ultrasonically dispersing uniformly, slowly heating to 110 ℃ to obtain a clear and transparent silver precursor solution, adding 0.05mmol of copper nitrate, and reacting at 195 ℃ for 200min to obtain the silver-copper-sulfur fluorescent quantum dot.
Example 4
Mixing 0.1mmol of silver trifluoroacetate, 100000mmol of octadecanethiol and 20mL of oleic acid, ultrasonically dispersing uniformly, then slowly heating to 120 ℃ to obtain a clear and transparent silver precursor solution, then adding 0.08mmol of copper sulfate, and reacting at 255 ℃ for 2min to obtain the silver-copper-sulfur fluorescent quantum dot.
Comparative example 1
The comparative example is different from example 1 in that: no copper source was added. The test result shows that: the size of the quantum dot is 8.2nm, and the fluorescence wavelength is 1200nm.
Comparative example 2
The comparative example is different from example 1 in that: no silver source was added. The test result shows that: the quantum dot size is 12nm, and the fluorescent property is avoided.
In addition, the inventor also carries out corresponding experiments by using other raw materials and other process conditions listed above to replace various raw materials and corresponding process conditions in the examples 1 to 4, and the obtained near-infrared silver-copper-sulfur fluorescent quantum dots have ideal shapes, performances and the like and are basically similar to the products of the examples 1 to 4.
In conclusion, the silver-copper-sulfur quantum dots are prepared by a simple high-temperature solvothermal method, the synthesis process is simple and controllable, the yield is high, the large-scale preparation can be realized, the obtained product is uniform in size, the fluorescence emission is near infrared, the high quantum efficiency and the excellent light stability are realized, and the silver-copper-sulfur quantum dots have wide application prospects in the fields of biological imaging, near infrared devices and the like.
The aspects, embodiments, features and examples of the present invention should be considered as illustrative in all respects and not intended to be limiting of the invention, the scope of which is defined only by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed invention.
The use of headings and chapters in this disclosure is not meant to limit the disclosure; each section may apply to any aspect, embodiment, or feature of the invention.
Throughout this specification, where compositions are described as having, containing, or comprising specific components, or where processes are described as having, containing, or comprising specific process steps, it is contemplated that compositions taught by the present invention also consist essentially of, or consist of, the recited components, and that processes taught by the present invention also consist essentially of, or consist of, the recited process steps.
Unless specifically stated otherwise, use of the terms "comprising", "including", "having" or "having" is generally to be understood as open-ended and not limiting.
It should be understood that the order of steps or the order in which particular actions are performed is not critical, so long as the teachings of the invention remain operable. Further, two or more steps or actions may be performed simultaneously.
While the invention has been described with reference to illustrative embodiments, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims. Moreover, unless specifically stated any use of the terms first, second, etc. do not denote any order or importance, but rather the terms first, second, etc. are used to distinguish one element from another.
Claims (6)
1. A preparation method of near-infrared silver copper sulfur quantum dots is characterized by comprising the following steps:
uniformly mixing a silver source, mercaptan and a weak polar solvent to form a first mixed reaction system, and then heating to 80-120 ℃ in a closed environment to react for less than 1h to prepare a precursor solution of silver; the molar ratio of the silver source to the mercaptan is 1-1000000, and the weak polar solvent is selected from any one or a combination of more than two of oleylamine, oleic acid, octadecene, octadecylamine, dodecylamine and tetradecylamine;
adding a copper source into a silver precursor solution at the temperature of 80-120 ℃ under continuous stirring to form a second mixed reaction system, then heating to 180-255 ℃ to perform solvothermal reaction for 2-600 min to obtain a near-infrared silver-copper-sulfur quantum dot, wherein the molar ratio of the silver source to the copper source is 0.8; the diameter of the near-infrared silver copper sulfur quantum dot is 2 to 25nm, the size distribution is uniform, and the wavelength of a fluorescence emission peak is 800 to 1160nm.
2. The method of claim 1, wherein: the silver source is selected from any one or combination of more than two of silver nitrate, silver acetate, silver trifluoroacetate and silver diethyldithiocarbamate.
3. The method of claim 1, wherein: the mercaptan is selected from one or the combination of more than two of dodecyl mercaptan, octyl mercaptan and octadecyl mercaptan.
4. The production method according to claim 1, characterized in that: the copper source is selected from any one or combination of more than two of copper nitrate, copper chloride, copper sulfate, copper acetate and copper diethyldithiocarbamate.
5. The application of the near-infrared silver copper sulfur quantum dots prepared by the preparation method of any one of claims 1 to 4 in the field of biological imaging or near-infrared devices.
6. Use according to claim 5, characterized in that: the near-infrared device is a near-infrared light-emitting diode.
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