CN109721026B - Method for preparing composite metal nanoparticle array with assistance of laser pulse - Google Patents
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Abstract
A method for preparing a composite metal nanoparticle array by laser pulse assistance. The invention provides a method for preparing a noble metal nanoparticle array with adjustable size, shape and material type. And bombarding the back of the noble metal nanoparticle array substrate by using a laser beam with high energy density as a heat source, melting and falling off the noble metal nanoparticle array from the surface of the substrate, and compounding the noble metal nanoparticle array with the surface of another group of noble metal nanoparticle arrays right below the substrate to form two-layer or multi-layer three-dimensional noble metal nanoparticle arrays. The method can obtain composite alloy nanoparticle arrays with different shapes by changing the shapes and materials of the upper and lower layers of precious metal nanoparticle arrays and adjusting parameters such as laser energy and frequency. The ordered alloy nanoparticle array has wide application prospects in the aspects of chemical and biological sensors, ultra-high density data storage media, photoelectric devices, chemical catalysts and the like.
Description
Technical Field
The invention relates to a preparation method of a noble metal nanoparticle array, in particular to a preparation method of a noble metal nanoparticle array with adjustable size, shape and material type.
Background
The noble metal nanoparticles have a strong absorption peak in the visible light range, because the vibration frequency of a large number of conduction electrons in the particles is equal to the frequency of incident light waves, and a surface plasmon resonance effect is generated, so that the strong absorption peak is generated. The peak position of the surface plasmon resonance spectrum is very sensitive to the shape, size, distribution and change of the external medium environment of the nano particles. With the development of modern nanotechnology, the preparation of noble metal nanoparticles with different morphologies and the research on their corresponding optical properties have attracted a great deal of interest. Two-dimensional and three-dimensional ordered composite nanoparticle arrays are increasingly receiving attention among precious metal nanostructures of different morphologies.
The two-dimensional and three-dimensional ordered nanoparticle array refers to a structure in which nanoparticles are orderly arranged according to a certain rule in two-dimensional and three-dimensional directions, and people can control the characteristics of the nanoparticles in a large range through the size, the distance and even the components of the nanoparticles. The nanoparticle array has potential application prospects in the fields of biosensing, medicine, photoelectricity, catalysis, detection and the like. Based on this, a large number of processes for preparing structures with dimensions of nanometers or less than micrometers, such as photolithography, electron beam lithography, X-ray lithography, etc., have been developed and derived. However, these etching techniques are complicated, expensive, inefficient, and difficult to fabricate large-scale nanoparticle array systems.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method capable of preparing a nanoparticle array with adjustable size, shape and material type, and the method has the advantages of simple equipment, convenient and flexible experimental means and high efficiency.
The technical scheme of the invention can be realized by the following technical measures:
a method for preparing a composite metal nanoparticle array by laser pulse assistance comprises the following steps:
(1) preparing a two-dimensional metal nanoparticle array on a substrate;
(2) covering a two-dimensional semiconductor film on the surface of the two-dimensional metal nanoparticle array in the step (1);
(3) and (2) bombarding the back of the substrate, which is attached with the two-dimensional metal nanoparticle array and is obtained in the step (1), by using laser pulses as a heat source, so that the two-dimensional metal nanoparticle array is melted and falls off from the surface of the substrate, falls on the surface of another group of two-dimensional metal nanoparticle arrays or two-dimensional semiconductor films right below, and is compounded with the two-dimensional metal nanoparticle arrays or the two-dimensional semiconductor films to obtain two layers of three-dimensional compound metal nanoparticle arrays or metal/semiconductor/metal sandwich nano structures.
Preferably, the method in step (3) is adopted, and the assembly is continued on the surface of the obtained three-dimensional composite metal nanoparticle array or noble metal/semiconductor/metal sandwich nanostructure to obtain three or more layers of three-dimensional composite metal nanoparticle arrays or metal/semiconductor composite nanostructures.
Preferably, the shape of the two-dimensional metal nanoparticle array includes a triangular shape, a bowl shape, a ring shape, and a mesh shape.
Preferably, the metal nanoparticles comprise silver nanoparticles, gold nanoparticles.
Preferably, the two-dimensional semiconductor thin film material includes: graphene, molybdenum disulfide and black phosphorus.
Preferably, the substrate for laser bombardment is a transparent good thermal conductor comprising: al (Al)2O3Quartz glass, ITO glass.
A three-dimensional composite metal nanoparticle array is prepared by the method.
The above technical solution may specifically include the following solutions:
in the first scheme, the first step is that,
(1) preparing a triangular two-dimensional single-layer noble metal nanoparticle array on the surface of a substrate by using a self-assembly means;
(2) and bombarding the back of the substrate of the triangular two-dimensional noble metal nanoparticle array by using laser pulses, and after the triangular noble metal nanoparticle array is stripped from the substrate at high temperature, falling on the surface of the other group of triangular two-dimensional noble metal nanoparticle arrays vertical to the right lower side for compounding to obtain two layers of three-dimensional composite noble metal nanoparticle arrays.
The substrate may be Al2O3Or quartz glass. This process corresponds to fig. 1.
In the second scheme, the first step is that,
(1) preparing a triangular two-dimensional single-layer triangular noble metal nanoparticle array on the surface of a substrate by using a self-assembly means;
(2) preparing a bowl-shaped two-dimensional single-layer noble metal nanoparticle array on the surface of the other substrate by using a self-assembly means;
(3) and bombarding the back of the substrate of the triangular two-dimensional noble metal nanoparticle array by using laser pulses, and after the triangular two-dimensional noble metal nanoparticle array is stripped from the substrate, falling on the surface of the bowl-shaped two-dimensional noble metal nanoparticle array vertical to the right lower part for compounding to obtain two layers of three-dimensional composite metal nanoparticle arrays.
The substrate may be Al2O3Or quartz glass. This process corresponds to fig. 2.
In the third scheme, the first step of the method,
(1) preparing a triangular two-dimensional single-layer triangular noble metal nanoparticle array on the surface of a substrate by using a self-assembly means;
(2) preparing a two-layer three-dimensional composite noble metal nanoparticle array by using the method of the second scheme;
(3) and continuously bombarding the back of the substrate of the triangular two-dimensional noble metal nanoparticle array by using laser pulses, and after the triangular noble metal nanoparticle array is stripped from the substrate, falling onto the surfaces of two layers of three-dimensional composite noble metal nanoparticle arrays vertical to the right lower part for compounding to obtain a three-layer three-dimensional composite noble metal nanoparticle array.
The substrate may be Al2O3GaN or quartz glass. This process corresponds to fig. 3.
In the fourth scheme, the first step is that,
(1) preparing a triangular two-dimensional single-layer noble metal nanoparticle array on the surface of a substrate by using a self-assembly means;
(2) covering a two-dimensional semiconductor single-layer film on the surface of the two-dimensional single-layer precious metal nanoparticle array obtained in the step (1);
(3) bombarding the back of the substrate of the two-dimensional single-layer precious metal nanoparticle array obtained in the step (1) by using laser pulses, and after the precious metal nanoparticle array is stripped from the substrate, dropping the precious metal nanoparticle array on the surface of the two-dimensional semiconductor single-layer film obtained in the step (2) vertical to the right lower side and compounding to obtain the precious metal/semiconductor/precious metal sandwich nanostructure array.
The substrate may be Al2O3GaN or quartz glass. This process corresponds to fig. 4.
Compared with the prior art, the invention can obtain composite alloy nanoparticle arrays with different shapes by changing the appearance and the material of the upper and lower layers of precious metal nano arrays and adjusting parameters such as laser energy, frequency and the like, thereby obtaining composite materials with different optical properties. The method has the advantages of simple equipment, convenient and flexible experimental means and high efficiency. The obtained three-dimensional ordered alloy nanoparticle array has wide application prospects in the aspects of chemical and biological sensors, ultra-high density data storage media, photoelectric devices, chemical catalysts and the like.
Drawings
The invention is further illustrated by means of the attached drawings, the examples of which are not to be construed as limiting the invention in any way.
FIG. 1 is a schematic diagram of a two-layer three-dimensional composite noble metal nanoparticle array prepared by the first embodiment of the invention;
FIG. 2 is a schematic diagram of a two-layer three-dimensional composite metal nanoparticle array prepared according to a second embodiment of the present invention;
FIG. 3 is a schematic diagram of a three-layer three-dimensional composite noble metal nanoparticle array prepared by the third embodiment of the invention;
FIG. 4 is a schematic representation of a noble metal/semiconductor/noble metal sandwich nanoparticle array prepared according to scheme four of the present invention.
Description of the drawings:
1, a heat source; 2, a convex lens; 3, a substrate; 4, triangular two-dimensional precious metal nano-arrays; 5, bowl-shaped two-dimensional noble metal nanoparticle arrays; 6, two-dimensional semiconductor single-layer film.
Detailed Description
In order that the invention may be more readily understood, specific embodiments thereof will be described further below.
Methods for preparing polystyrene colloid ball single-layer mask plates and preparing two-dimensional metal nanoparticle arrays in different shapes are disclosed in chinese patent CN 102747320A:
example 1
Using laser pulses (0.06J/cm)230fs) bombarding the back of the substrate with triangular silver nanoparticles, and placing a projection between the laser and the back of the substrateAnd (3) focusing by a mirror, stripping the silver nanoparticle array from the surface of the substrate by using a laser high-temperature melting principle, dropping the silver nanoparticle array on the surface of the lower triangular silver nanoparticle array by using a self-falling body motion rule, and compounding the silver nanoparticle array with the triangular silver nanoparticle array to obtain two layers of three-dimensional silver nanoparticle arrays. The experiment can adjust parameters such as the size, the distance and the like of the silver nanoparticles through the distance between the upper substrate and the lower substrate and laser energy, so that the optical property of the silver nanoparticles can be conveniently and quantitatively researched.
Example 2
Using laser pulses (0.05J/cm)230fs) striking the back of the substrate of the triangular silver nanoparticle array, placing a convex lens between laser and the back of the substrate for focusing, stripping the silver nanoparticle array from the surface of the substrate by using a laser high-temperature dissolution principle, dropping the silver nanoparticle array on the surface of the bowl-shaped silver nanoparticle array below by using an own falling motion rule, and compounding the silver nanoparticle array with the bowl-shaped silver nanoparticle array to obtain two layers of three-dimensional silver nanoparticle arrays. The experiment can adjust parameters such as the size, the distance and the like of the silver nanoparticles through the distance between the upper substrate and the lower substrate and laser energy, so that the optical property of the silver nanoparticles can be conveniently and quantitatively researched.
Example 3
Using laser pulses (0.05J/cm)230fs) striking the back of the triangular gold nanoparticle array substrate, placing a convex lens between laser and the back of the substrate for focusing, stripping the gold nanoparticle array from the surface of the substrate by using a laser high-temperature dissolution principle, falling on the surface of the bowl-shaped silver nanoparticle array below by using a falling body movement rule, and compounding with the bowl-shaped silver nanoparticle array to obtain a two-layer three-dimensional gold/silver nanoparticle array. The experiment can adjust parameters such as the size, the distance and the like of the silver nanoparticles through the distance between the upper substrate and the lower substrate and laser energy, so that the optical property of the silver nanoparticles can be conveniently and quantitatively researched.
Example 4
Using laser pulses (0.05J/cm)230fs) striking the back of the substrate of the triangular silver nanoparticle array, placing a convex lens between the laser and the back of the substrate for focusing, stripping the silver nanoparticle array from the surface of the substrate by using the laser high-temperature dissolution principle, and performing surface recombination on the two layers of three-dimensional gold/silver nanoparticle arrays obtained in the embodiment 4 by using the movement rule of the self-falling body to fall below to obtain three-dimensional gold/silver nanoparticle arraysAnd (3) forming a three-dimensional composite silver/gold/silver nanoparticle array. The experiment can adjust parameters such as the size, the distance and the like of the silver nanoparticles through the distance between the upper substrate and the lower substrate and laser energy, so that the optical property of the silver nanoparticles can be conveniently and quantitatively researched.
Example 5
Methane is used as a carbon source, and a chemical vapor deposition method is adopted to prepare high-quality single-layer graphene on a copper sheet with the thickness of 25 mu m. And spin-coating a layer of PMMA on the surface of the copper sheet covered with the graphene, and then baking the copper sheet at 120 ℃ for 30 minutes. Immersing the copper sheet in ferric chloride solution (0.4g/mL) containing a small amount of hydrochloric acid for more than 30 minutes to obtain the PMMA/graphene film. And then, transferring the PMMA/graphene film to the surface of the triangular silver metal nanoparticle array obtained in the step 1).
Then, a laser pulse (0.06J/cm) was applied230fs) strikes the back of another two-dimensional triangular silver nanoparticle array substrate, places a convex lens in the middle of laser and the substrate back for focusing, peels off silver nanoparticle array from the substrate surface through the laser high-temperature dissolution principle, utilizes the two-dimensional graphene film surface that the law of motion of falling from oneself drops in the below, and silver nanoparticle combines with two-dimensional graphene film to obtain silver nanoparticle array graphene composite structure. The experiment can adjust parameters such as the size, the distance and the like of the silver nanoparticles through the distance between the upper substrate and the lower substrate and laser energy, so that the optical property of the silver nanoparticles can be conveniently and quantitatively researched.
The optical permeability of biological tissues in the wavelength range of 800-1300 nm is found to be optimal, so that the material with the optical property can be utilized to assist in the treatment of cancers. The plasma absorption peak of the noble metal composite nano-particles can change along with the change of the structure and the component proportion of the composite material, and the optical property of the material at visible light and near infrared wavelength can meet the requirement of use through the metal proportion of the noble metal composite material, so that the application of the nano-material has wider prospect and more flexibility.
Meanwhile, the biosensing utilizes the phenomena of 'blue shift' and 'red shift' of the SPR absorption band of the metal nanoparticles, namely the influence of the refractive index of an environmental medium on the absorption band of the metal nanoparticles. The geometric structure parameter regulation and control capability of the noble metal composite nano-particles is stronger than that of the pure metal nano-particles.
Graphene is a single-layer sheet graphite, and has bright development prospects in the fields of optics and optoelectronics due to its special electrical, optical and structural characteristics. Graphene is also an ideal standard material for researching SERS. The noble metal composite nanoparticles and the graphene respectively have unique and incomparable advantages in SERS research and application, and the composite materials with different structures prepared by combining the noble metal composite nanoparticles and the graphene have very excellent SERS effect and are mainly reflected in that:
when the graphene/precious metal composite nanoparticle composite material is used as an SERS substrate for Raman detection, compared with a pure precious metal composite nanoparticle, the Raman signal of a detection molecule can be further improved, and meanwhile, the sensitivity and repeatability stability of detection are also greatly improved. The graphene plays an important role in passivation and protection of fluorescence quenching, so that the measured SERS signal is more pure.
Meanwhile, when graphene oxide is attached to the sandwich structure and further used as the interlayer to construct the sandwich structure, the SERS effect of the sandwich structure is greatly improved. Firstly, the existence of graphene can still play a role in passivation protection. Secondly, when a sandwich structure is formed, graphene oxide serves as an intermediate spacing zone, resonance coupling effect between particles in layers and resonance coupling effect between particles between layers exist between two layers, and the SERS effect of the substrate is enhanced greatly.
The composite structure shows unique SERS activity after the surface of the Ag nano array is covered with high-quality single-layer graphene. The single-layer graphene synthesized by the chemical vapor deposition method has high optical transparency in a visible light region and strong chemical stability. As a protective layer, the single-layer graphene effectively prevents sulfide in the air from vulcanizing the Ag bow-tie nano-antenna array and the Ag nano-grid array. After the graphene-covered Ag nanostructures were left in air for one month, the surface was still smooth and maintained its original structure. In addition, the graphene-covered Ag nanostructure exhibits higher raman signal enhancement and electromagnetic field enhancement than the graphene-uncovered Ag nanostructure. Therefore, the metal nanomaterial surface-coated single-layer graphene provides potential for application of novel surface plasmon materials. And the material can be applied to living organisms and has great potential for detecting cancer cells in the future.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (7)
1. A method for preparing a composite metal nanoparticle array by laser pulse assistance is characterized by comprising the following steps:
(1) preparing a two-dimensional metal nanoparticle array on a substrate;
(2) covering a two-dimensional semiconductor film on the surface of the two-dimensional metal nanoparticle array in the step (1);
(3) and (2) bombarding the back of the substrate, which is attached with the two-dimensional metal nanoparticle array and is obtained in the step (1), by using laser pulses as a heat source, so that the two-dimensional metal nanoparticle array is melted and falls off from the surface of the substrate, falls on the surface of another group of two-dimensional metal nanoparticle arrays or two-dimensional semiconductor films right below, and is compounded with the two-dimensional metal nanoparticle arrays or the two-dimensional semiconductor films to obtain two layers of three-dimensional compound metal nanoparticle arrays or metal/semiconductor/metal sandwich nano structures.
2. The method for laser pulse assisted preparation of a composite metal nanoparticle array according to claim 1, wherein the method of step (3) is adopted, and the assembly is continued on the surface of the obtained three-dimensional composite metal nanoparticle array or metal/semiconductor/metal sandwich nanostructure to obtain three-or more-layer three-dimensional composite metal nanoparticle array or metal/semiconductor composite nanostructure.
3. The method of claim 1, wherein the two-dimensional metal nanoparticle array comprises a triangular shape, a bowl shape, a ring shape, and a grid shape.
4. The method for laser pulse assisted preparation of composite metal nanoparticle arrays according to claim 1, wherein the metal nanoparticles comprise silver nanoparticles and gold nanoparticles.
5. The method for laser pulse assisted preparation of composite metal nanoparticle arrays according to claim 1, wherein the two-dimensional semiconductor thin film material comprises: graphene, molybdenum disulfide and black phosphorus.
6. The method of claim 1, wherein the substrate material for laser bombardment comprises: al (Al)2O3Quartz glass, ITO glass.
7. A three-dimensional composite metal nanoparticle array prepared by the method of any one of claims 1 to 6.
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| CN1926420A (en) * | 2004-03-05 | 2007-03-07 | 加利福尼亚大学董事会 | Glass-modified stress waves for separation of ultra thin films and nanoelectronics device fabrication |
| CN101566571A (en) * | 2009-06-03 | 2009-10-28 | 哈尔滨工业大学 | Surface enhanced raman spectroscopy substrate of continuous three dimensional structural nano silver and preparation method thereof |
| WO2012144728A3 (en) * | 2011-04-19 | 2013-01-17 | 한국과학기술원 | Method for manufacturing a nanoparticle array the size of which is adjustable, nanoparticle array manufactured thereby, and uses thereof |
| CN104630772A (en) * | 2013-11-12 | 2015-05-20 | 中国科学院物理研究所 | Multilayer stacked metal nanosphere array and preparation method thereof |
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| US7397558B2 (en) * | 2005-03-17 | 2008-07-08 | Hewlett-Packard Development Company, L.P. | Ordered array of nanoparticles for efficient nanoenhanced Raman scattering detection and methods of forming the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1926420A (en) * | 2004-03-05 | 2007-03-07 | 加利福尼亚大学董事会 | Glass-modified stress waves for separation of ultra thin films and nanoelectronics device fabrication |
| CN101566571A (en) * | 2009-06-03 | 2009-10-28 | 哈尔滨工业大学 | Surface enhanced raman spectroscopy substrate of continuous three dimensional structural nano silver and preparation method thereof |
| WO2012144728A3 (en) * | 2011-04-19 | 2013-01-17 | 한국과학기술원 | Method for manufacturing a nanoparticle array the size of which is adjustable, nanoparticle array manufactured thereby, and uses thereof |
| CN104630772A (en) * | 2013-11-12 | 2015-05-20 | 中国科学院物理研究所 | Multilayer stacked metal nanosphere array and preparation method thereof |
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