CN114767883A - Preparation method and application of nano composite material based on Au-PbS heterostructure - Google Patents
Preparation method and application of nano composite material based on Au-PbS heterostructure Download PDFInfo
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Abstract
The invention provides a preparation method and application of a nano composite material based on an Au-PbS heterostructure. The Au-PbS nano-particles synthesized by the method have uniform particle size, good monodispersity, good crystal structure, adjustable near-infrared II-region fluorescence emission performance and good fluorescence quantum yield. The Au-PbS nano-particles provided by the invention not only have the performances of nano-gold particles and lead sulfide quantum dots, but also have more excellent near infrared light absorption under the synergistic action of the two nano-particles, so that the Au-PbS nano-particles have good photo-thermal effect, can be used as a photo-thermal conversion agent, and can be used for tumor photo-thermal imaging and photo-thermal treatment. In addition, the Au-PbS nano-particles can be used as a Computed Tomography (CT) imaging contrast agent for CT imaging due to the large X-ray attenuation coefficient of the Au-PbS nano-particles.
Description
Technical Field
The invention relates to the technical field of analytical chemistry and nano-material preparation, in particular to a preparation method and application of a nano-composite material based on an Au-PbS heterostructure.
Background
The fluorescence emission wavelength of the PbS quantum dots in a second near infrared window (NIR-II, 1000-1700nm) is easy to regulate and control, the fluorescence intensity is high, and when the PbS quantum dots are used for in-vivo fluorescence imaging, the PbS quantum dots have lower self-fluorescence and deeper tissue penetrability, so the PbS quantum dots have important application value in the field of biomedicine. Meanwhile, the nano gold particles as a noble metal nano material play an important role in the aspects of catalysis, optics, biological diagnosis, treatment and the like. Therefore, two kinds of nanoparticles, namely PbS quantum dots and gold nanoparticles, are combined into one nano structure, and the PbS quantum dots and the gold nanoparticles are hopeful to be obtainedA novel hybrid material not only has the properties of the two nano materials at the same time, but also can enable the properties to be more excellent under the synergistic action, and develops new excellent properties. However, due to the large difference of crystal structures among different types of nanomaterials, which often results in lattice mismatch, synthesis of heterostructure nanoparticles with good crystal structures is very difficult. On the other hand, in some heterostructure nanoparticle Semiconductor-Metal nanostructures, the optical property from the Semiconductor, i.e., photoluminescence, is typically quenched by the presence of Metal nanoparticles, such as Janus Au-CdSe (Uri Banin, Selective Growth of Metal Tips on Semiconductor Quantum Rods and nanoparticles, Science 2004,304,1787-
Absorption Properties of Metal-Semiconductor hybrids, ACS Nano 2011,5, 4712-.
Disclosure of Invention
In order to overcome the problems and obtain a composite nano material with excellent performance, the first objective of the invention is to develop a novel method for preparing a heterostructure composite nano particle containing metal nano gold particles and semiconductor lead sulfide (PbS) quantum dots, so as to solve the problems of fluorescence quenching, imperfect crystal structure and low synthesis efficiency in the synthesis process of the 'Shuangshen' Au-PbS nano particle, and other excellent performances of the 'Shuangshen' Au-PbS nano particle.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a preparation method of a nano composite material based on an Au-PbS heterostructure comprises the following steps:
step 1, preparing nano gold particles, dispersing the nano gold particles in an organic solvent to prepare a solution A, and dissolving sublimed sulfur in oleylamine to prepare a solution B;
and 4, separating and purifying the nano-particles obtained in the step 3 by using a non-polar organic solvent and absolute ethyl alcohol to obtain the Au-PbS nano-particles with the heterostructure.
Preferably, in the step 1, the specific steps of preparing the gold nanoparticles are as follows: adding chloroauric acid into a room-temperature organic solvent 1, 2, 3, 4-tetrahydronaphthalene, then adding 1-3mMol reducing agent borane-tert-butylamine or ascorbic acid, and stirring at room temperature for 30-60min to prepare the nano gold particles.
Preferably, the diameter of the gold nanoparticles is 1-10 nm.
Preferably, in the step 1, the organic solvent is one of n-hexane or chloroform, and the concentration of the gold nanoparticles in the organic solvent is 1-20 mg/mL. The normal hexane and the chloroform are volatile organic solvents and are easy to remove.
Preferably, in the step 1, the concentration of the sublimed sulfur in the oleylamine is 1 to 10M. Because oleylamine is not only used as a simple solvent in a high-temperature organic phase, but also has certain reducibility, the sulfur precursor prepared by the method has higher reaction activity, and is different from pure sulfur. In addition, the primary amine in the oleylamine can form a coordinate bond with the cation, so the oleylamine can also be used as a surface ligand of the nanoparticle.
Preferably, in the step 2, the lead precursor is lead chloride or lead oleate, the organic solution is a mixed solution of 1-octadecene and oleylamine, wherein 1-octadecene is used as an experimental reaction solvent, oleylamine is used not only as a reducing agent to mediate nucleation, but also as a surface ligand of the nanoparticle to stabilize the synthesized nanoparticle, and the volume ratio of the two is 4-6: 1, the concentration of the lead precursor in the organic solution is 10-50 mM.
Preferably, in the step 3, the temperature is raised to be within the range of 140-180 ℃, the stirring time of the solution A and the solution B is 5-60min, and the volume ratio of the solution A to the solution B is 5: 1-2. In a high-temperature organic solution, the spontaneous epitaxial nucleation and growth of the lead sulfide are mediated by the gold nanoparticles, so that the Au-PbS heterostructure nanoparticles are obtained.
Preferably, in the step 4, the nonpolar organic solvent is n-hexane, the centrifugal rotation speed during purification is 7500-10000r/min, the centrifugal time is 5-10min, and the centrifugation is repeated for 2-4 times.
Preferably, the absolute fluorescence quantum yield of the Au-PbS heterostructure nanoparticles is 2% -40% at an emission wavelength of 1300 nm.
The method provides a brand new lead precursor, namely lead chloride or lead oleate, a preparation method of an improved sulfur precursor (sublimed sulfur is dissolved in oleylamine), and synthesizes a series of Au-PbS heterostructure nano-particles with adjustable fluorescence emission wavelength and positioned in a near-infrared II region by changing the ratio of nano-gold particles prepared by adding the improved synthesis method and the lead precursor to the sulfur precursor. The fluorescence emission wavelength of the Au-PbS heterostructure nano-particles is positioned in a near-infrared II region, the wavelength is in the range of 1000-1700nm, and the quantum yield is high; in addition, research also finds that the Au-PbS heterostructure nano-particles synthesized by the method have uniform particle size, good monodispersity, good crystal structure and good fluorescence quantum yield.
The second purpose of the invention is to provide the application of the Au-PbS heterostructure-based nano composite material prepared by the preparation method in tumor photothermal imaging, photothermal therapy and CT imaging.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method is novel and simple, and the prepared Au-PbS heterostructure nano-particles have the near-infrared II region fluorescence property with adjustable emission wavelength and higher fluorescence quantum yield;
(2) the Au-PbS heterostructure nano-particles prepared by the invention have uniform particle size, good monodispersity and good crystal structure;
(3) the Au-PbS heterostructure nano-particles prepared by the invention can be used as a Computed Tomography (CT) imaging contrast agent for CT imaging due to larger X-ray attenuation coefficient;
(4) the Au-PbS heterostructure nano-particles synthesized by the method not only have the performances of nano-gold particles and lead sulfide quantum dots, but also have more excellent near-infrared light absorption under the synergistic action of the two nano-particles, so that the Au-PbS heterostructure nano-particles have good photothermal effect in a near-infrared region, can be used as a photothermal conversion agent and is used for tumor photothermal imaging and photothermal treatment.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic diagram of the synthesis of Au-PbS heterostructure nanoparticles;
FIG. 2 is an electron micrograph of the gold nanoparticles;
FIG. 3 is a representation of Au-PbS heterostructure nanoparticles, wherein a is a transmission electron micrograph of Au-PbS heterostructure nanoparticles according to an embodiment of the present invention; b is a high-resolution electron microscope image of the Au-PbS heterostructure nano-particles according to the embodiment of the invention; c is a Scanning Transmission Electron Microscope (STEM) image of the Au-PbS heterostructure nanoparticles according to the embodiment of the invention; d is the X-ray diffraction (XRD) result of the Au-PbS heterostructure nanoparticle polycrystal in the embodiment of the invention;
fig. 4 is a fluorescence property of Au-PbS heterostructure nanoparticles, in which a is a fluorescence spectrum of Au-PbS heterostructure nanoparticles according to an embodiment of the present invention; b is a bright field photo picture and a fluorescence picture under 808nm laser irradiation of the Au-PbS heterostructure nano-particles according to the embodiment of the invention;
FIG. 5 is the photothermal properties of Au-PbS heterostructure nanoparticles, where a is the absorption spectra of Au-PbS heterostructure nanoparticles (Au-PbS NPs) with pristine gold nanoparticles (Au NPs), lead sulfide quantum dots (PbS QDs), and physical mixtures of Au NPs and PbS QDs (Au NPs/PbS QDs) in accordance with the present invention; b is the temperature change of Au NPs, PbS QDs, physical mixture of Au NPs/PbS QDs and the suspension of Au-PbS heterostructure nanoparticles; c is an infrared thermograph of Au NPs, PbS QDs and physical mixtures thereof and Au-PbS heterostructure nanoparticle suspension;
FIG. 6 is the CT imaging results of Au-PbS heterostructure nanoparticles, where a is the in vitro CT images of Au-PbS heterostructure nanoparticles at different concentrations and the HU values of Au-PbS heterostructure nanoparticles at different concentrations are linearly fitted; b is in vivo CT images of 4T1 tumor-bearing mice before and after the injection of Au-PbS heterostructure nanoparticles with different concentrations, and red circles represent tumor sites.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The experimental reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The invention will now be described in more detail with reference to the following examples, without however limiting the invention thereto.
Firstly, the source of raw materials
The reagents used in the examples of the invention were as follows:
lead chloride: 98%, Shanghai Aladdin Biotechnology, Inc.;
sublimed sulfur: AR, Shanghai Aladdin Biotechnology, Inc.;
chloroform: AR grade, jervine industrialisation industrial trade ltd, tianjin;
borane-t-butylamine: 98%, Tianjin Xiansi Oppon Kochia Co., Ltd;
1, 2, 3, 4-tetrahydronaphthalene: grade AR, tianjin xinshi opropposcid ltd;
chloroauric acid: 48-50% of Au, Tianjin Mayda Biotech limited;
oleylamine 80-90%, Shanghai Aladdin Biotechnology Co., Ltd;
1-octadecene: 90%, Shanghai Aladdin Biotechnology, Inc.
Second, example
Example 1: preparation method of Au-PbS heterostructure nanoparticles
(1) Dissolving 0.1g of chloroauric acid in 10mL of 1, 2, 3, 4-tetrahydronaphthalene at room temperature (25 +/-5 ℃), adding 1 mmol of borane-tert-butylamine, stirring at room temperature, and reacting for 45 minutes to obtain nano gold particles;
(2) dissolving 1 mmol of sublimed sulfur in 10ml of oleylamine to obtain a sulfur precursor B;
(3) dissolving 0.321g of lead chloride powder in 10mL of nonpolar organic solvent 1-octadecene and oleylamine (the volume ratio of 1-octadecene to oleylamine is 5: 1) at 120 ℃ to prepare a solution C, then preparing 10mg of nanogold seeds in organic solvent n-hexane to prepare a solution A (5mg/mL), and then preparing a mixed solution A according to the volume ratio of the solution C to the solution A of 5: 1, adding the solution A into the solution C, stirring, heating to 160 ℃, then immediately adding the solution B, immediately cooling to 120 ℃, preserving heat, reacting for 5 minutes, naturally cooling, and purifying, namely mixing n-hexane and absolute ethyl alcohol according to a volume ratio of 1: 3, centrifuging at the rotating speed of 8000r/min for 6min, repeating the centrifuging for 3 times, and removing the supernatant to obtain the Au-PbS heterostructure nanoparticles.
Third, result analysis
The structure and properties of the Au-PbS nanoparticles of the present invention are described in detail below with reference to the accompanying drawings.
Experimental example 1
FIG. 1 is a schematic diagram of the synthesis of Au-PbS heterostructure nanoparticles, from which the synthesis process of Au-PbS heterostructure nanoparticles can be known.
Experimental example 2
Fig. 2 is a transmission electron microscope representation of the gold nanoparticles described in embodiment 1 of the present invention, and the result shows that the Au nanoparticles have a uniform particle size and good monodispersity.
Experimental example 3
FIG. 3 is a characterization of Au-PbS heterostructure nanoparticles as described in example 1 of the present invention; fig. 3 a is a transmission electron microscope image of Au-PbS heterostructure nanoparticles according to an embodiment of the present invention, and the result shows that Au-PbS heterostructures are all heterostructures, and have uniform particle size and good monodispersity; b is a high-resolution electron microscope image of the Au-PbS heterostructure nanoparticles, the result shows that the components show different lattice spacing sizes, wherein the lattice plane spacing in the PbS nanoparticle domain is 0.22nm and corresponds to 220 crystal planes of the galena crystal phase, the lattice plane spacing in the Au nanoparticle domain is 0.24nm and corresponds to 111 crystal planes of the gold crystal phase, which indicates that the Au-PbS heterostructure nanoparticles have a good crystal structure; c is a Scanning Transmission Electron Microscope (STEM) image of the Au-PbS heterostructure nanoparticles, and different components on two sides clearly show the heterostructure of the Au-PbS heterostructure nanoparticles; d is the X-ray diffraction (XRD) result of the Au-PbS heterostructure nanoparticles of the embodiment of the present invention, all peaks of XRD are respectively assigned to the crystalline phases of PbS (JCPDS:05-0592) and Au (JCPDS:04-0784), indicating the successful preparation of Au-PbS heterostructure nanoparticles.
Experimental example 4
Fig. 4 shows the fluorescence property of the Au-PbS heterostructure nanoparticles of example 1 of the present invention, and a in fig. 4 shows the fluorescence spectrum of the Au-PbS heterostructure nanoparticles of example 1 of the present invention, and the results show that the fluorescence emission spectrum of the Au-PbS heterostructure nanoparticles prepared by the method is tunable, and the fluorescence emission spectrum ranges from 1000nm to 1700 nm; b is a bright field photograph and a fluorescence photograph of the Au-PbS heterostructure nanoparticles in example 1 of the present invention under 808nm laser irradiation, the concentration of the solution is 0.1mg/mL, the exposure time is 0.05s, and the results in the drawings show that the Au-PbS heterostructure nanoparticles have bright fluorescence properties.
Experimental example 5
Fig. 5 is an absorption spectrum of Au-PbS heterostructure nanoparticles according to example 1 of the present invention, and a in fig. 5 is an absorption spectrum of Au-PbS heterostructure nanoparticles (Au-PbS NPs) according to the present invention with primary gold nanoparticles (Au NPs), lead sulfide quantum dots (PbS QDs), and a physical mixture of Au NPs and PbS QDs (Au NPs/PbS QDs), and changes in the absorption spectra thereof are analyzed by comparing the absorption spectra of the four kinds of nanomaterials. The pristine Au NPs showed strong Local Surface Plasmon Resonance (LSPR) absorption at 521 nm. The original PbS quantum dots had no distinct absorption peaks. Compared with Au NPs, LSPR absorption of the physical mixture of Au NPs and PbS quantum dots at 521nm has no influence, but has broadening, which shows that the simple physical mixture of Au NPs and PbS quantum dots has little influence on LSPR absorption positions of Au NPs. However, of "Shuangmian" Au-PbS nanoparticlesThe LSPR absorbance at 553nm not only showed a broader and red shift than the original Au NPs, but also the absorption in the near infrared region was significantly enhanced, which indicates that the absorption spectrum of the Au-PbS heterostructure nanoparticles is not the sum of the absorption spectra of simple individual component homogeneous nanoparticles; in FIG. 5 b is a graph showing the power density of 1.2W/cm according to the present invention2The temperature of the Au NPs, PbS QDs, physical mixtures of Au NPs/PbS QDs, and the suspension of Au-PbS heterostructure nanoparticles varied 3 minutes after laser irradiation, and only the temperature of the Au-PbS heterostructure nanoparticle suspension varied most significantly under the same conditions in the figure, with little change in the other groups. In FIG. 5, c is the Au-PbS heterostructure nanoparticles according to example 1 of the present invention with a power density of 1.2W/cm2Under 808nm laser irradiation, the infrared thermography of Au NPs, PbS QDs and physical mixtures thereof and Au-PbS heterostructure nanoparticle suspension is obtained. These results show that the power density is 1.2W/cm2The control group temperature was slightly raised by 4.9 ℃ for 3min at 808nm laser irradiation, and the temperatures of Au NPs, PbS QDs and their physical mixtures were raised by 5.8 ℃, 4.1 ℃ and 10.5 ℃ respectively. However, under the same conditions, the Au-PbS heterostructure nanoparticles rose by 21.1 ℃, suggesting that the Au-PbS heterostructure nanoparticles play a key role in enhancing photothermal performance.
Experimental example 6
FIG. 6 is CT imaging of Au-PbS heterostructure nanoparticles according to an embodiment of the present invention, wherein a in FIG. 6 is in vitro CT images of Au-PbS heterostructure nanoparticles at different concentrations and HU values of Au-PbS heterostructure nanoparticles at different concentrations are linearly fitted; in fig. 6, b is an in vivo CT image of 4T1 tumor-bearing mice before and after the injection of Au-PbS heterostructure nanoparticles at different concentrations, and red circles indicate tumor sites. These results indicate that Au-PbS heterostructure nanoparticles may be potential clinical CT contrast agents.
The invention relates to a preparation method of a nano composite material based on an Au-PbS heterostructure, which comprises the steps of firstly, in a room-temperature organic phase, using borane-tert-butylamine or ascorbic acid as a reducing agent to reduce a chloroauric acid solution to prepare nano gold particles, then adding the purified nano gold particles dispersed in an organic solvent into a high-temperature organic solution containing lead chloride or lead oleate, heating to a certain temperature, and then adding an active sulfur precursor, thus preparing the nano particles, namely the Au-PbS heterostructure nano particles. Since the gold nanoparticles are added in advance during the preparation of the Au-PbS heterostructure nanoparticles, PbS quantum dots are always formed on the gold nanoparticles, which indicates that the gold nanoparticles mediate the nucleation and growth of lead sulfide on the gold nanoparticles. Moreover, when using smaller amounts of gold nanoparticles will result in a mixture of free PbS quantum dots and "dihedral". Thus, it was demonstrated that PbS quantum dots nucleate preferentially on the gold nanoparticles, rather than homogeneously. The final morphology depends on whether the gold surface allows only one nucleation point or multiple nucleation points. On the other hand, when we changed the preparation method of the sulfur precursor, i.e. dissolving sublimed sulfur in oleic acid or using simple sulfur in the experimental process, the experimental result found that the Au-PbS heterostructure nanoparticles could not be formed, which indicates that the activity of the sulfur precursor has a key role in the formation process of the Au-PbS heterostructure nanoparticles. This is related to the reducibility of oleylamine.
In addition, the Au-PbS heterostructure nano-particles not only have the performances of nano-gold particles and lead sulfide quantum dots, but also have more excellent near-infrared light absorption under the synergistic action of the two nano-particles, so that the Au-PbS heterostructure nano-particles have good photothermal effect in a near-infrared region, can be used as a photothermal conversion agent and is used for tumor photothermal imaging and photothermal treatment. The Au-PbS heterostructure nano-particles have bright near-infrared II-region fluorescence emission, so that the background can be ignored, the penetration depth is high, and the defect of the photothermal treatment penetration depth is overcome. The Au-PbS heterostructure nanoparticles are successfully used for near-infrared II-region fluorescence imaging/photothermal imaging/CT imaging multi-modal guided photothermal therapy (PTT), and good experimental results are obtained.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A preparation method of a nano composite material based on an Au-PbS heterostructure is characterized by comprising the following steps: the method comprises the following steps:
step 1, preparing nano gold particles, dispersing the nano gold particles in an organic solvent to prepare a solution A, and dissolving sublimed sulfur in oleylamine to prepare a solution B;
step 2, dissolving a lead precursor in an organic solution to prepare a solution C;
step 3, adding the solution A into the solution C, heating, raising the temperature, and adding the solution B to obtain nano particles;
and 4, separating and purifying the nano-particles obtained in the step 3 by using a non-polar organic solvent and absolute ethyl alcohol to obtain the Au-PbS nano-particles with the heterostructure.
2. The method for preparing the Au-PbS heterostructure-based nanocomposite material as recited in claim 1, wherein the method comprises the steps of: in the step 1, the specific steps for preparing the nano gold particles are as follows: adding chloroauric acid into a room-temperature organic solvent 1, 2, 3, 4-tetrahydronaphthalene, then adding a 1-3mMol reducing agent borane-tert-butylamine or ascorbic acid, and stirring at room temperature for 30-60min to prepare the nano-gold particles.
3. The method for preparing a nanocomposite material based on an Au-PbS heterostructure according to claim 1 or 2, wherein: the diameter of the nano gold particles is 1-10 nm.
4. The method for preparing the Au-PbS heterostructure-based nanocomposite material according to claim 1, wherein the Au-PbS heterostructure-based nanocomposite material comprises: in the step 1, the organic solvent is one of n-hexane or chloroform, and the concentration of the gold nanoparticles in the organic solvent is 1-20 mg/mL.
5. The method for preparing the Au-PbS heterostructure-based nanocomposite material as recited in claim 1, wherein the method comprises the steps of: in the step 1, the concentration of the sublimed sulfur in the oleylamine is 1-10M.
6. The method for preparing the Au-PbS heterostructure-based nanocomposite material according to claim 1, wherein the Au-PbS heterostructure-based nanocomposite material comprises: in the step 2, the lead precursor is lead chloride or lead oleate, the organic solution is a mixed solution of 1-octadecene and oleylamine, and the volume ratio of the lead precursor to the mixed solution is 4-6: 1, the concentration of the lead precursor in the organic solution is 10-50 mM.
7. The method for preparing the Au-PbS heterostructure-based nanocomposite material according to claim 1, wherein the Au-PbS heterostructure-based nanocomposite material comprises: in the step 3, the temperature is raised to a range of 140-180 ℃, the stirring time of the solution A and the solution B is 5-60min, and the volume ratio of the solution A to the solution B is 5: 1-2.
8. The method for preparing the Au-PbS heterostructure-based nanocomposite material according to claim 1, wherein the Au-PbS heterostructure-based nanocomposite material comprises: in the step 4, the nonpolar organic solvent is normal hexane, the centrifugal rotation speed during purification is 7500-10000r/min, the centrifugal time is 5-10min, and the centrifugation is repeated for 2-4 times.
9. The application of the Au-PbS heterostructure-based nanocomposite material prepared by the preparation method of any one of claims 1-8 in tumor photothermal imaging, photothermal therapy and CT imaging.
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