CN114163989A - Silver chalcogenide-iron carbide heterogeneous nano structure and preparation method and application thereof - Google Patents

Silver chalcogenide-iron carbide heterogeneous nano structure and preparation method and application thereof Download PDF

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CN114163989A
CN114163989A CN202010984900.XA CN202010984900A CN114163989A CN 114163989 A CN114163989 A CN 114163989A CN 202010984900 A CN202010984900 A CN 202010984900A CN 114163989 A CN114163989 A CN 114163989A
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iron carbide
silver
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侯仰龙
汪志义
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Peking University
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Abstract

The invention discloses a chemical liquid phase method based on seed crystal growth for controllable preparation of a core-shell structure silver sulfide-iron carbide heterogeneous nano structure. Dissolving silver sulfide quantum dots, a metal organic compound of iron and ammonium bromide salt in a high-boiling-point organic solvent, carrying out high-temperature carbonization reaction, and precipitating by using a polar organic liquid to obtain the core-shell structure silver sulfide-iron carbide heterogeneous nano structure. The material shows ferromagnetism, and the maximum magnetic saturation intensity is higher. Meanwhile, the heterogeneous nano-particles show excellent near-infrared two-region luminous performance. The invention prepares high-quality silver sulfide-iron carbide heterogeneous nanoparticles by using silver sulfide quantum dots, metal organic compounds of precursor iron and ammonium chloride salts. Carrying out water-soluble modification by distearoyl phosphatidyl ethanolamine-polyethylene glycol to obtain water-soluble silver sulfide-iron carbide heterogeneous nanoparticles. The preparation method has potential application in the fields of optics, biomedicine, environmental science, materials, catalysis, energy, magnetic storage and the like, is simple and easy to implement, and is suitable for industrial production.

Description

Silver chalcogenide-iron carbide heterogeneous nano structure and preparation method and application thereof
Technical Field
The invention belongs to the technical field of materials, relates to preparation of a silver chalcogenide-iron carbide heterogeneous nano structure, and particularly relates to an ammonium halide assisted chemical liquid phase synthesis method which has universality for preparation of the silver chalcogenide-iron carbide heterogeneous nano structure.
Background
The heterostructure nanostructure has wide application prospect in the fields of optics, biomedicine, environmental science, materials, catalysis, energy, magnetic storage and the like due to excellent performances such as multifunctionality, tunability, stability and the like.
Specifically, in all multi-component nanomaterials, the types of heterogeneous nanostructures include core-shell structures, dimers (dumbbells, biplanars), and multimers, among others. The advantages of the heterogeneous nano structure are mainly reflected in the following five aspects: (1) and (4) multiple functions. The heterogeneous nano structure consists of an inner core and an outer shell which are made of different materials, so that the combination of different properties of different materials results in some new characteristics of the heterogeneous materials, thereby expanding the application of the heterogeneous materials in the aspects of electronics, optics, magnetism and catalysis; (2) effectively reducing the cost. In general, hetero-nanostructures can reduce the specific gravity of noble or transition metals as compared to pure metal nanoparticles. For example, by coating a thin layer thereof on an inexpensive support, the use of precious metals can be significantly reduced; (3) controllability. By varying the size, shape, morphology and composition, as well as thickness, shape, of the hetero-nanostructure, the properties of the nanostructure can be easily and significantly tuned; (4) the stability and the dispersibility are improved. The influence of aggregation, sintering or other agents of the nano particles can be prevented; (5) biocompatibility is improved. From the practical biological application point of view, biocompatibility is an important issue, and the biocompatibility of the hetero-nanostructure can be improved by coating chemical components with high biocompatibility.
The silver chalcogenide quantum dots show excellent fluorescence emission performance in the near infrared region. In addition, the excellent magnetic and photo-thermal properties of ferromagnetic carbide nanostructures are receiving more and more attention. The preparation of the silver chalcogenide-iron carbide heterogeneous nano structure has potential application prospect. Currently, achieving precise control of heterostructures at the nanoscale remains a significant challenge. Therefore, the development of a method with simple synthesis and low cost for preparing the heterostructure nano-structure has important significance in science and engineering.
Disclosure of Invention
The invention aims to provide a method for preparing a silver chalcogenide-iron carbide heterogeneous nano structure. The prepared monodisperse silver sulfide-iron carbide heterogeneous nano-particles (the core is 5-15 nanometers, and the shell layer is 1-10 nanometers in thickness). In one aspect, the heterojunction nanoparticles exhibit intrinsic ferromagnetism. On the other hand, the heterojunction nano-particle also shows good near-infrared two-region fluorescence luminescence performance, the excitation wavelength is 808 nanometers, the emission wavelength is 1071 nanometers, and the fluorescence lifetime is 218.16 nanoseconds. Therefore, the heterojunction nano-particle has important potential application value in the construction of a nano-probe based on magnetic resonance imaging and near-infrared two-region fluorescence imaging.
The silver chalcogenide-iron carbide heterogeneous nano structure is formed by reacting silver chalcogenide quantum dots with a metal organic compound of iron in a high-boiling-point organic solvent, the halogen ions play a very important role in phase control of the iron carbide, and finally the high-quality silver chalcogenide-iron carbide heterogeneous nano structure is obtained by cleaning with the organic solvent.
The preparation method of the silver chalcogenide-iron carbide heterogeneous nano structure comprises the following steps:
1) preparing silver sulfide quantum dots;
2) growing an iron carbide nano-shell layer on the prepared silver sulfide quantum dots to obtain silver sulfide-iron carbide heterogeneous nanoparticles;
3) and (3) preparing water-soluble silver sulfide-iron carbide heterogeneous nanoparticles.
Step 1) selecting a precursor silver diethyldithiocarbamate or silver acetate of silver, such as silver diethyldithiocarbamate, and dissolving the precursor silver diethyldithiocarbamate or silver acetate in a high-boiling organic solvent 1-dodecanethiol or 1-hexadecanethiol, such as 1-dodecanethiol;
the dissolving process of step 1) is usually performed under a high temperature protective atmosphere, the temperature is 180-;
and 2) sequentially adding the prepared silver sulfide quantum dots and the metal organic compound of iron into a high-boiling point mixed organic solvent oleylamine/1-octadecene or 1-octadecylamine/1-octadecene, such as oleylamine/1-octadecene. Ammonium halide salts, including ammonium chloride, cetyltrimethylammonium chloride, ammonium bromide and cetyltrimethylammonium bromide, such as ammonium bromide, are then added;
step 2) the mixture is further stirred, again at predominantly room temperature, for example 25 ℃, for 10-30 minutes, for example 10 minutes. The reaction process is typically carried out under a high temperature protective atmosphere at a temperature of 280-360 degrees celsius, such as 300 degrees celsius, for a period of 1-3 hours, such as 1 hour, under a high purity argon or high purity nitrogen, such as high purity argon. The precipitation is usually carried out at room temperature, and the washing organic solvent is ethanol or acetone, such as ethanol.
And 3) synthesizing water-soluble silver sulfide-iron carbide heterogeneous nanoparticles by using distearoyl phosphatidyl ethanolamine-polyethylene glycol through an oil-in-water microemulsion method. Performing microemulsion method with ultrasonicator.
The invention further provides a magnetic test of the silver sulfide-iron carbide heterogeneous nano-particles. In addition, a fluorescence luminescence performance test of the silver sulfide-iron carbide heterogeneous nano-particles is provided, and the potential application of the silver sulfide-iron carbide heterogeneous nano-particles in the biomedical field is further clarified.
Drawings
Fig. 1 is a transmission electron microscope image of the silver sulfide quantum dots prepared in example 1.
Fig. 2 is a transmission electron microscope image of silver sulfide-iron carbide heterogeneous nanoparticles prepared in example 1.
Fig. 3 is an X-ray diffraction analysis diagram of the silver sulfide-iron carbide heterogeneous nanoparticles prepared in example 1.
Fig. 4 is a transmission electron microscope image of the water-soluble silver sulfide-iron carbide heterogeneous nanoparticles prepared in example 1.
Fig. 5 is a graph of magnetic susceptibility versus temperature for silver sulfide-iron carbide heterogeneous nanoparticles prepared in example 1.
Fig. 6 is a graph of magnetic susceptibility versus temperature for the water-soluble silver sulfide-iron carbide heterogeneous nanoparticles prepared in example 1.
Fig. 7 is a fluorescence spectrum of silver sulfide-iron carbide heterogeneous nanoparticles prepared in example 1.
Fig. 8 is a fluorescence spectrum of the water-soluble silver sulfide-iron carbide heterogeneous nanoparticles prepared in example 1.
Fig. 9 is a fluorescence lifetime analysis of the water-soluble silver sulfide-iron carbide heterogeneous nanoparticles prepared in example 1.
Fig. 10 is a transmission electron microscope image of silver sulfide-iron carbide heterogeneous nanoparticles prepared in example 2.
Fig. 11 is a transmission electron microscope image of silver sulfide-iron carbide heterogeneous nanoparticles prepared in example 3.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Preparing silver sulfide quantum dots;
25.6 mg of silver diethyldithiocarbamate was dissolved in 10 g of 1-dodecanethiol, and the system was heated to 210 ℃ under a high-purity argon atmosphere and maintained for 1 hour. After the system is cooled to the room temperature, 60 milliliters of absolute ethyl alcohol is added after the system is cooled to the room temperature, and the silver sulfide quantum dots are obtained by centrifugation at 8000 revolutions per minute for 3 minutes. The prepared silver sulfide quantum dots are dispersed in n-hexane for later use.
(2) Preparing silver sulfide-iron carbide heterogeneous nanoparticles;
adopts a simple seed crystal growth method to synthesize the silver sulfide-iron carbide heterogeneous nano-particles. 1 ml of silver sulfide quantum dots (10 mg/ml) and 9.8 mg of ammonium bromide were added to a mixed organic solvent system of 200. mu.l oleylamine and 20 ml of octadecene, and the system was heated to 120 ℃ under an argon atmosphere and kept warm for 30 minutes. The temperature was then increased to 80 ℃ and 0.4 ml of carbonyl iron was injected rapidly and incubated for 10 minutes. And (3) continuously heating the reaction system for 10 minutes, and preserving the temperature for 30 minutes when the temperature reaches 300 ℃. And then cooling the system to room temperature, adding 60 ml of absolute ethyl alcohol, and centrifuging at 8000 rpm for 3 minutes to obtain the monodisperse silver sulfide-iron carbide heterogeneous nanoparticles.
(3) And (3) preparing water-soluble silver sulfide-iron carbide heterogeneous nanoparticles.
250 mg of distearoylphosphatidylethanolamine-polyethylene glycol (molecular weight 4000) was dispersed in 12 ml of deionized water. Silver sulfide-iron carbide heterogeneous nanoparticles were dispersed in 3 ml of dichloromethane at a concentration of 10 mg/ml. The two solution systems were mixed uniformly and then treated with an ultrasonic disruptor for 10 minutes (ultrasonic mode: 5 minutes, 5 minutes off, ultrasonic power: 2000 watts/hour) to obtain an emulsion. And then treating for 2 hours at 25 ℃ by using a rotary evaporator to obtain the water-soluble silver sulfide-iron carbide heterogeneous nano particles. .
As shown in fig. 1, the transmission electron microscope pictures characterize the size and morphology of the silver sulfide quantum dots.
As shown in fig. 2, the transmission electron microscope pictures characterize the size and morphology of the silver sulfide-iron carbide heterogeneous nanoparticles.
As shown in fig. 3, X-ray diffraction analysis revealed that both the position and intensity of the diffraction peaks matched well to the standard cards of silver sulfide quantum dots (JCPDS 04-0072) and silver sulfide-iron carbide heterogeneous nanoparticles (JCPDS 36-1249), indicating that the material prepared by the above method was a homogeneous FeSe material.
As shown in fig. 4, transmission electron microscopy pictures demonstrate water-soluble silver sulfide-iron carbide heterogeneous nanoparticle size and morphology.
As shown in FIG. 5, the temperature was 298KThe magnetization curve proves the ferromagnetism of the silver sulfide-iron carbide heterogeneous nano-particles, and the maximum magnetic saturation intensity is 116.97emu g-1。
As shown in FIG. 6, the magnetization curve at room temperature (298K) proves the ferromagnetism of the water-soluble silver sulfide-iron carbide heterogeneous nanoparticles, and the maximum saturation intensity is 50.12emu g-1。
As shown in FIG. 7, the fluorescence spectrum at room temperature (298K) proves the luminescence property of the silver sulfide-iron carbide heterogeneous nanoparticles, the excitation wavelength is 808nm, and the emission wavelength is 1068 nm.
As shown in FIG. 8, the fluorescence spectrum at room temperature (298K) proves the luminescence property of the silver sulfide-iron carbide heterogeneous nanoparticles, the excitation wavelength is 808nm, and the emission wavelength is 1071 nm.
As shown in fig. 9, the fluorescence lifetime characterization demonstrates the luminescence property of the water-soluble silver sulfide-iron carbide heterogeneous nanoparticles, and the fluorescence lifetime is 218.16 ns.
Example 2
Adopts a simple seed crystal growth method to synthesize the silver sulfide-iron carbide heterogeneous nano-particles. 1 ml of silver sulfide quantum dots (10 mg/ml) and 36.5 mg of cetyltrimethylammonium bromide were added to a mixed organic solvent system of 200. mu.l oleylamine and 20 ml of octadecene, and the system was heated to 120 ℃ under an argon atmosphere and kept warm for 30 minutes. The temperature was then increased to 80 ℃ and 0.4 ml of carbonyl iron was injected rapidly and incubated for 10 minutes. And (3) continuously heating the reaction system for 10 minutes, and preserving the temperature for 30 minutes when the temperature reaches 300 ℃. And then cooling the system to room temperature, adding 60 ml of absolute ethyl alcohol, and centrifuging at 8000 rpm for 3 minutes to obtain the monodisperse silver sulfide-iron carbide heterogeneous nanoparticles.
As shown in fig. 10, the transmission electron microscope picture shows the size and morphology thereof.
Example 3
Adopts a simple seed crystal growth method to synthesize the silver sulfide-iron carbide heterogeneous nano-particles. 1 ml of silver sulfide quantum dots (10 mg/ml) and 9.8 mg of ammonium bromide were added to a mixed organic solvent system of 200. mu.l oleylamine and 20 ml of octadecene, and the system was heated to 120 ℃ under an argon atmosphere and kept warm for 30 minutes. The temperature was then increased to 80 ℃ and 1.412 grams of iron acetylacetonate were injected rapidly and incubated for 10 minutes. And (3) continuously heating the reaction system for 10 minutes, and preserving the temperature for 30 minutes when the temperature reaches 320 ℃. And then cooling the system to room temperature, adding 60 ml of absolute ethyl alcohol, and centrifuging at 8000 rpm for 3 minutes to obtain the monodisperse silver sulfide-iron carbide heterogeneous nanoparticles.
As shown in fig. 11, the transmission electron microscope picture shows the size and morphology thereof.
Example 4
Adopts a simple seed crystal growth method to synthesize the silver sulfide-iron carbide heterogeneous nano-particles. 1 ml of silver sulfide quantum dots (10 mg/ml) and 36.5 mg of cetyltrimethylammonium bromide were added to a mixed organic solvent system of 200. mu.l oleylamine and 20 ml of octadecene, and the system was heated to 120 ℃ under an argon atmosphere and kept warm for 30 minutes. The temperature was then increased to 80 ℃ and 0.4 ml of carbonyl iron was injected rapidly and incubated for 10 minutes. And (3) continuously heating the reaction system for 10 minutes, and preserving the temperature for 30 minutes when the temperature reaches 320 ℃. And then cooling the system to room temperature, adding 60 ml of absolute ethyl alcohol, and centrifuging at 8000 rpm for 3 minutes to obtain the monodisperse silver sulfide-iron carbide heterogeneous nanoparticles.

Claims (10)

1. A general synthetic method for preparing a silver chalcogenide-iron carbide heterogeneous nano structure based on a chemical liquid phase synthetic method and water-soluble modification thereof.
2. The silver chalcogenide-iron carbide heteronanostructure of claim 1, wherein the silver chalcogenide quantum dots comprise silver sulfide quantum dots, silver selenide quantum dots, and silver telluride quantum dots.
3. Silver chalcogenide-iron carbide heteronanostructures according to claim 1, wherein the structure and phase of the material can be precisely controlled, in particular the phase of low carbon iron carbides, including Fe3C，Fe5C2And Fe2C。
4. The silver chalcogenide-iron carbide heteronanostructure of claim 1 wherein the material has ferromagnetic and near infrared two-region fluorescent properties.
5. The silver chalcogenide-iron carbide heteronanostructure of claim 1, wherein the heteronanostructure comprises a core-shell structure, a dimer (dumbbell, biplane) and a multimer, etc., the size of the core is about 5-15 nm and the thickness of the shell layer is about 1-10 nm.
6. The general synthetic method according to claim 1, wherein the technical means used is chemical liquid phase synthesis.
7. The synthesis method according to claim 1, wherein in the preparation of silver sulfide-iron carbide heterogeneous nanoparticles, the selection of iron organometallic compounds is important, and the iron organometallic compounds include ferric acetylacetonate, ferric stearate, carbonyl iron, and the like.
8. The method of claim 1, wherein in the preparation of silver chalcogenide-iron carbide heterogeneous nanostructures, the presence of ammonium halide is important for phase control of iron carbide, and the ammonium halide includes ammonium fluoride, ammonium chloride, ammonium bromide, ammonium iodide, cetyltrimethylammonium chloride, cetyltrimethylammonium bromide, and the like.
9. The water-soluble modification of silver chalcogenide-iron carbide heterogeneous nanoparticles as claimed in claim 1, wherein the technical means adopted is to use distearoyl phosphatidyl ethanolamine-polyethylene glycol to carry out water transfer modification of silver sulfide-iron carbide heterogeneous nanoparticles by an oil-in-water emulsion method, and the molecular weight of distearoyl phosphatidyl ethanolamine-polyethylene glycol is between 2000 and 20000.
10. The method as claimed in claim 1, wherein the parameters include a reaction temperature of 180-220 ℃ for the synthesis of the silver sulfide quantum dots, and a carbonization temperature of 280-360 ℃ for the iron carbide coated silver sulfide quantum dots.
CN202010984900.XA 2020-09-11 2020-09-11 Silver chalcogenide-iron carbide heterogeneous nano structure and preparation method and application thereof Pending CN114163989A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140087409A1 (en) * 2011-05-30 2014-03-27 Suzhou Institute of Nano-Bionics, Shinese Academy of Sciences Near-infrared silver sulfide quantum dot, preparation method therefor and biological application thereof
CN106077699A (en) * 2016-06-30 2016-11-09 青岛科技大学 A kind of preparation method of silver ferrite composite nanometer particle
CN106925316A (en) * 2015-12-30 2017-07-07 北京大学 Gold/cementite C-base composte material and its preparation method and application
WO2019163808A1 (en) * 2018-02-20 2019-08-29 国立大学法人九州大学 Method for producing luminescent particles, luminescent particles, and bioimaging material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140087409A1 (en) * 2011-05-30 2014-03-27 Suzhou Institute of Nano-Bionics, Shinese Academy of Sciences Near-infrared silver sulfide quantum dot, preparation method therefor and biological application thereof
CN106925316A (en) * 2015-12-30 2017-07-07 北京大学 Gold/cementite C-base composte material and its preparation method and application
CN106077699A (en) * 2016-06-30 2016-11-09 青岛科技大学 A kind of preparation method of silver ferrite composite nanometer particle
WO2019163808A1 (en) * 2018-02-20 2019-08-29 国立大学法人九州大学 Method for producing luminescent particles, luminescent particles, and bioimaging material

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