CN107699954B - Strong-coupling gold nano superlattice structure and self-assembly preparation method thereof - Google Patents
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Abstract
The invention discloses a strongly coupled gold nano superlattice structure and a self-assembly preparation method thereof, wherein the superlattice structure is formed by densely arranging a series of thirty-dihedral gold nano particles, the average distance of the particles is controlled to be dozens of nanometers to several nanometers, the whole superlattice is in a single-layer film form, and two characteristic plasma coupling resonance peaks exist in a visible-near infrared band range; the self-assembly preparation method combines the combined action of static electricity and capillary adsorption. The reagent and the instrument selected by the invention are simple and easily obtained, the self-assembly mode is flexible and efficient, and the actual area of the prepared strong coupling alloy nano superlattice structure reaches cm2And the repeatability is good. The invention lays an experimental foundation for constructing and designing functional novel optical materials and devices, and has important reference value for preparing large-area super crystals by self-assembling nano crystal structure units in other forms and application thereof.
Description
Technical Field
The invention relates to the field of synthesis and preparation of functional nano materials, in particular to a gold nano superlattice structure with a strong coupling effect and a self-assembly preparation method thereof.
Background
In recent years, the design of colloidal nanoparticle structures to form various large-scale block super junctions by using a chemical self-assembly technology is a main research mode for the effective preparation and the engineering application of functional nano composite materials. Noble metal nano superlattice structures with coupling effects, particularly two-dimensional or three-dimensional superlattice thin films, have attracted much attention in the whole chemical self-assembly research because of their ability to generate a variety of unusual physical properties under specific frequency electromagnetic waves, such as abnormal optical absorption or scattering, adjustable near fields and distributions, directional plasma polarization, and the like. Based on the existence of various singular physical characteristics, the coupled noble metal nano superlattice has potential research and application values in the fields of spectrum sensing, plasma metamaterials, surface enhanced Raman scattering, novel light absorption systems and the like.
Until now, some self-assembly research work on noble metal nanoparticles (including spherical, rod-shaped, cubic and octahedral) with simple morphology has been carried out, but due to the limitation of the preparation method, it is difficult to precisely control the distance between adjacent nanoparticles to reach the ideal size range, thereby generating possible surface plasmon coupling. Especially for single-layer noble metal superlattice thin film structures, the reported chemical self-assembly method cannot effectively regulate the aggregation and distribution states of nanoparticles, so that the characteristic coupling effect generally cannot occur in the structures. Attempts have been made to achieve superlattice structures and strong coupling by stacking nanoparticles repeatedly, but most fail due to complexity and instability in experimental operation. In addition, for noble metal nanoparticles with complex morphology, taking high-crystal-face super-polyhedron nanoparticles as an example, due to the existence of commonly exposed high surface energy and a very limited preparation process, few researches on the construction of a super-lattice structure and related properties of the super-polyhedron nanoparticles with chemical self-assembly high crystal faces are currently carried out. And we know that the hyper-polyhedral noble metal nanoparticles with high crystal planes have surface plasma resonance phenomena with different conventional forms, and the occurrence of the mutual coupling effect is also greatly different theoretically.
Therefore, in summary, the research of a novel chemical self-assembly method through experiments to construct a noble metal nano superlattice single-layer structure (especially a high crystal face super polyhedral nano particle unit containing a complex form) for realizing a specific coupling effect has pioneering research significance and practical engineering application value.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: taking into account the existing monolayerThe occurrence of coupling effect and the uniqueness of the appearance of the constituent structural units in the gold nano superlattice structure are difficult to exist, and a gold nano superlattice single layer structure with strong coupling is provided, wherein the gold nano superlattice single layer with strong coupling is formed by densely arranging a series of thirty-dihedral gold nanoparticles with uniform appearance, and the superlattice structure stably has two characteristic plasma coupling resonance peaks in a visible-near infrared wide band range. Meanwhile, the invention provides a simple, convenient and efficient chemical self-assembly method capable of realizing large-scale manufacturing, namely, the combined action of static electricity and capillary adsorption is combined, a substrate with negative charges on the surface is placed in a thirty-dihedral gold nanoparticle solution with positive charges on the lower surface at saturation concentration to carry out slow vertical pulling, and the strongly coupled alloy nano superlattice with different particle spacing distributions is finally obtained by controlling a plurality of experimental condition parameters in the self-assembly process. The reagent and the instrument selected by the invention are simple and easily obtained, the self-assembly mode is flexible and efficient, and the actual area of the prepared strong coupling alloy nano superlattice single-layer structure reaches cm2And the repeatability is good.
The technical scheme adopted by the invention is as follows:
the gold nano superlattice structure is formed by densely arranging a series of thirty-dihedral gold nanoparticles with uniform appearance, is a two-dimensional single-layer film in appearance, and has two characteristic plasma coupling resonance peaks in a visible-near infrared broadband range.
In the invention, the selected thirty-dihedral gold nanoparticles comprise 8 hexagonal planes and 24 pentagonal planes, and the particle size is less than 100 nm.
In the invention, the average distance between adjacent thirty-dihedral gold nanoparticles is controlled within the range of 1nm to 100nm, and the spatial orientation of each nanoparticle is in a disordered state.
In the invention, two plasma coupling resonance peaks appear in the wavelength range of 400 nm-1000 nm, and the first characteristic peak is positioned between 400 nm-580 nm, so that the peak shape is strong and sharp; the second characteristic peak is located between 600nm and 1000nm, and the peak shape is weak and broadened.
A self-assembly preparation method of a strongly coupled gold nano superlattice structure comprises the following steps:
the selected self-assembly mode combines the combined action of static electricity and capillary adsorption and mainly comprises two steps. Firstly, cleaning a solid substrate by using various solutions, and then placing the solid substrate in a goby boiling solution for a period of time to carry out surface negative electricity hydroxylation treatment. And secondly, soaking the dried substrate after the negative electricity treatment in a high-concentration positively charged thirty-dihedron gold nanoparticle solution, and then separating the substrate from the liquid surface at a slow speed, wherein the environmental temperature of the whole self-assembly process is maintained within a certain range. After the self-assembly process is finished, the single-layer gold nano superlattice thin film structure can be formed on one end of the substrate in a large scale.
In the invention, the solid substrate is a common glass sheet, a silicon wafer or a germanium sheet, and the shape of the solid substrate can be round or square. Preferably, the substrate is a common glass sheet or a silicon sheet, and the shape of the substrate is square.
In the invention, the cleaning solution of the substrate is a toluene solution, an anhydrous methanol solution, an anhydrous ethanol solution and deionized water in sequence, the grade of the solution is analytically pure, the cleaning mode of the substrate is ultrasonic cleaning, and the cleaning time is 5-15 min each time. Preferably, each washing time is 10 min.
In the invention, the surface negative electricity hydroxylation treatment time of the clean substrate in the goby boiling solution is at least more than 10 min.
In the invention, the high-concentration thirty-dihedral gold nanoparticle solution is an aqueous solution, an absolute ethyl alcohol solution or a toluene solution, and the solution is close to or reaches a saturated condition. Preferably, the high-concentration solution of the thirty-dihedral gold nanoparticles is an absolute ethanol solution, and the concentration of the solution is a saturated concentration.
In the invention, a layer of poly diallyl dimethyl ammonium chloride (PDDA) molecules is coated on the surface of the positively charged thirty-sided body nano particles.
In the invention, the drying substrate after the negative electricity treatment also needs to be in the vertical direction when being separated from the liquid surface, and the separation speed is controlled to be 0.1 mm/min-30 mm/min.
In the invention, the external environment temperature in the whole self-assembly process is 25-100 ℃. Preferably, the external temperature of the whole self-assembly process is 30-80 ℃.
Compared with the prior art, the invention has the following advantages: the invention discloses a gold nanometer superlattice single-layer film structure with strong coupling effect, the average distance of the constituent units of the dodecahedron nanometer particles can be well controlled between dozens of nanometers and several nanometers, the spatial orientation of all the particles does not need to be strictly unified, and the particles can be in a disordered state; the adopted superlattice structure self-assembly method is flexible, efficient and good in repeatability, all chemical reagents and instruments are simple and easy to obtain, and the actual area of the prepared strongly-coupled alloy nanometer superlattice single-layer structure reaches cm2And (4) stages. The invention lays an experimental foundation for constructing and designing functional novel optical materials and devices, and has important reference value for preparing large-area super crystals by self-assembling nano crystal structure units in other forms and application thereof.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) image and a visible-near infrared (Vis-NIR) extinction spectrum of a strongly coupled alloy nano superlattice structure provided in example 1 of the present invention, wherein fig. 1(a) is a low-power SEM image, and fig. 1(a) is an inset image of a high-power SEM image; FIG. 1(b) is a plot of Vis-NIR extinction spectra;
FIG. 2 is a Scanning Electron Microscope (SEM) image and a visible-near infrared (Vis-NIR) extinction spectrum of a self-assembled and large-size structural unit-based strongly-coupled alloy nano superlattice structure prepared in example 2 of the present invention, wherein FIG. 2(a) is the SEM image, and FIG. 2(b) is the Vis-NIR extinction spectrum;
FIG. 3 is a Scanning Electron Microscope (SEM) image and a visible-near infrared (Vis-NIR) extinction spectrum of a strongly coupled alloy nano superlattice structure based on small-sized structural units prepared by self-assembly in example 2, wherein FIG. 3(a) is the SEM image and FIG. 3(b) is the Vis-NIR extinction spectrum;
FIG. 4 is a Scanning Electron Microscope (SEM) image and a visible-near infrared (Vis-NIR) extinction spectrum of a strongly coupled alloy nano superlattice structure with a larger nano-particle spacing prepared by self-assembly in example 3 of the invention, wherein FIG. 4(a) is the SEM image and FIG. 4(b) is the Vis-NIR extinction spectrum;
FIG. 5 is a Scanning Electron Microscope (SEM) image and a visible-near infrared (Vis-NIR) extinction spectrum of a strongly coupled alloy nano superlattice structure with a small nano-particle spacing prepared by self-assembly in example 3 of the invention, wherein FIG. 5(a) is the SEM image and FIG. 5(b) is the Vis-NIR extinction spectrum;
FIG. 6 is a Scanning Electron Microscope (SEM) image and a visible-near infrared (Vis-NIR) extinction spectrum of a gold nano superlattice structure with octahedral structural units prepared by self-assembly in example 4 of the present invention, wherein FIG. 6(a) is the SEM image, and FIG. 6(b) is the Vis-NIR extinction spectrum;
FIG. 7 is a Scanning Electron Microscope (SEM) image and a visible-near infrared (Vis-NIR) extinction spectrum of a gold nano superlattice structure with random structural units prepared by self-assembly in example 5 of the invention, wherein FIG. 7(a) is the SEM image, and FIG. 7(b) is the Vis-NIR extinction spectrum;
fig. 8 is a Scanning Electron Microscope (SEM) image of the self-assembled gold nanoparticle superlattice structure prepared in example 6 at different external environmental temperatures, wherein fig. 8(a) is a SEM image of the self-assembled gold nanoparticle superlattice structure prepared at a temperature of 30 ℃, and fig. 8(b) is a SEM image of the self-assembled gold nanoparticle superlattice structure prepared at a temperature of 75 ℃.
Detailed Description
The present invention will be further described with reference to the following embodiments and the accompanying drawings, but the present invention is not limited to the following embodiments. Modifications and improvements of the present invention will occur to those skilled in the art, and are intended to be within the scope of the present invention as defined by the appended claims.
Embodiment 1, the self-assembly preparation process of a strongly coupled gold nano superlattice structure of the present invention comprises the following steps:
1. placing a square substrate (a common glass sheet or a silicon wafer) in a toluene solution, an anhydrous methanol solution, an anhydrous ethanol solution and a deionized water solution of analytical grade in sequence for ultrasonic cleaning, wherein the cleaning time is 10min each time. After the substrate is cleaned, drying the substrate by using high-purity nitrogen;
2. placing the substrate treated in the step 1 in a goby boiling solution for carrying out surface negative electricity hydroxylation treatment for 15min, taking out the substrate, and drying the substrate by using high-purity nitrogen again;
3. vertically soaking the substrate after the treatment in the step 2 in absolute ethanol solution of the thirty-dihedron gold nanoparticles (the particle size is about 85nm) with positive electricity under the saturated concentration, and vertically separating the substrate from the liquid level again at the speed of 4 mm/min; the ambient temperature for the whole self-assembly process was 40 ℃.
4. After the substrate is completely separated from the self-assembly solution and dried, one end of the substrate obtains a strongly coupled gold nano superlattice single-layer structure;
as shown in fig. 1, wherein fig. 1(a) and the insets are SEM images of the prepared strongly coupled alloy nano superlattice structure at low power and high power, and fig. 1(b) is a Vis-NIR extinction spectrum diagram of the strongly coupled alloy nano superlattice structure. It can be seen that the strongly coupled alloy nano superlattice structure in this embodiment is composed of a series of densely arranged thirty-dihedral gold nanoparticles, the average inter-particle spacing is 20nm, and the spatial orientation of each particle is different. Within a visible-near infrared band, two characteristic strong coupling plasma resonance peaks appear at 530nm and 795nm, the first characteristic peak is strong and sharp, and the second characteristic peak is weak and wide.
Example 2 self-assembly preparation of strongly coupled alloy nano-superlattice structures based on different sized structural units
Other conditions and procedures were as described in example 1. In the above embodiment, the thirty-dihedral gold nanoparticle unit of 85nm is replaced by 64nm and 98nm, respectively, so as to obtain the strongly coupled alloy nano superlattice structures with different sizes of structural units, as shown in fig. 2 and 3. Wherein, fig. 2(a) and fig. 2(b) are respectively a Scanning Electron Microscope (SEM) image and a visible-near infrared (Vis-NIR) extinction spectrum image of the strongly coupled alloy nano superlattice structure based on the large-size structural unit, and fig. 3(a) and fig. 3(b) are respectively a Scanning Electron Microscope (SEM) image and a visible-near infrared (Vis-NIR) extinction spectrum image of the strongly coupled alloy nano superlattice structure based on the small-size structural unit. It can be seen that no matter whether the large-size or small-size thirty-dihedral gold nanoparticle units are selected for self-assembly, the average distance between the nanoparticles in the obtained strongly-coupled alloy nano superlattice structure is between 10nm and 20nm, except that the large-size structural units cause red shift of two characteristic strongly-coupled plasma resonance peaks to 541nm and 802nm, and the small-size structural units cause blue shift of the coupling resonance peaks to 505nm and 654 nm.
Example 3 self-assembly preparation of strongly coupled alloy nano-superlattice structures with different nano-particle spacing
Other conditions and procedures were as described in example 1. In the above embodiments, the vertical separation speed of the substrate from the self-assembly solution is adjusted to 20mm/min and 0.8mm/min, respectively, so as to obtain the super-lattice structure of the strongly coupled alloy with different nanoparticle pitches, as shown in fig. 4 and 5, where fig. 4(a) and 4(b) respectively show the Scanning Electron Microscope (SEM) image and the visible-near infrared (Vis-NIR) extinction spectrum image of the super-lattice structure of the strongly coupled alloy with larger nanoparticle pitch, and fig. 5(a) and 5(b) respectively show the Scanning Electron Microscope (SEM) image and the visible-near infrared (Vis-NIR) extinction spectrum image of the super-lattice structure of the strongly coupled alloy with smaller nanoparticle pitch. From the SEM image, it can be seen that the separation speed of 20mm/min increases the average distance between the nanoparticles in the self-assembled super-lattice structure of the strongly coupled alloy nanoparticles to 90nm, and the separation speed of 0.8mm/min decreases the average distance between the nanoparticles to 7 nm. The resonance peaks of the characterized strong coupling plasmas all move and respectively appear at 518nm, 786nm, 532nm and 800 nm.
Example 4 self-assembly preparation of gold nano-superlattice structure with octahedral structural units
Other conditions and procedures were as described in example 1. In the above examples 85nm of thirty-dihedral gold nanoparticle units were replaced with octahedral gold nanoparticles with an average size of 70 nm. As shown in FIG. 6, by adopting the same self-assembly preparation method, the obtained gold nano superlattice structure still presents a single-layer close packing state, the average distance of octahedral nano particles also reaches 20nm, and the spatial orientation of the particles keeps disordered. The visible-near infrared extinction spectrum test result shows that the gold nano superlattice of the octahedral structural unit only has a characteristic plasma resonance peak at 582 nm. Wherein, FIG. 6(a) and FIG. 6(b) are SEM image and Vis-NIR extinction spectrum image of gold nano superlattice structure with octahedral structural unit, respectively.
Example 5 self-assembly preparation of gold nano-superlattice structure with random structural unit
Other conditions and procedures were as described in example 1. In the above embodiment, 85nm of thirty-dihedral gold nanoparticle units are changed into any morphology particles with a particle size of about 67nm, and a gold nano superlattice structure with random morphology structural units can be prepared by self-assembly, as shown in fig. 7, at this time, the nanoparticles still maintain dense arrangement, and the average distance between the particles is about 10 nm. And the visible-near infrared extinction spectrum test result shows that the gold nano superlattice of the random structural unit only has one characteristic plasma resonance peak at 564 nm. Wherein, FIG. 7(a) and FIG. 7(b) are SEM image and Vis-NIR extinction spectrum image of gold nano superlattice structure with other random structural units, respectively.
Example 6 self-assembly preparation of gold nano-superlattice structures at different ambient temperatures
Other conditions and procedures were as described in example 1. In the above embodiment, the self-assembly external environment temperature is adjusted to 30 ℃ and 75 ℃ respectively, and other derived gold nano superlattice structures can be prepared, as shown in fig. 8, it can be seen that with the decrease of the self-assembly external environment temperature, the aggregation arrangement manner of the nanoparticles in the gold nano superlattice structure is changed, the density is reduced, and the average distance between the nanoparticles is close to hundred nanometers; with the rise of the temperature of the self-assembly external environment, the density of particle units in the gold nano superlattice structure is increased, and the average distance between particles is dozens of nanometers. Wherein, FIG. 8(a) and FIG. 8(b) are SEM images of the gold nano superlattice structure prepared by self-assembly at 30 deg.C and 75 deg.C, respectively.
Claims (8)
1. A strongly coupled gold nano superlattice structure is characterized in that: the gold nano superlattice structure is formed by densely arranging a series of thirty-dihedral gold nanoparticles with uniform appearance, the appearance of the gold nano superlattice structure is a two-dimensional single-layer film, and two characteristic plasma coupling resonance peaks exist in a visible-near infrared broadband range;
the selected thirty-dihedral gold nanoparticles comprise 8 hexagonal surfaces and 24 pentagonal surfaces, and the particle size is less than 100 nm;
the average distance between adjacent arranged thirty-dihedral gold nanoparticles is controlled within the range of 1nm to 100nm, and the spatial orientation of each nanoparticle is in a disordered state.
2. The strongly coupled alloy nano-superlattice structure as recited in claim 1, wherein: the two plasma coupling resonance peaks appear in the wavelength range of 400 nm-1000 nm, the first characteristic peak is positioned between 400 nm-580 nm, and the peak shape is strong and sharp; the second characteristic peak is located between 600nm and 1000nm, and the peak shape is weak and broadened.
3. A self-assembly preparation method of a strongly coupled gold nano superlattice structure is characterized by comprising the following steps: the selected self-assembly mode combines the combined action of static electricity and capillary adsorption and comprises two steps:
firstly, cleaning a solid substrate by using various solutions, and then placing the solid substrate in a goby boiling solution for a period of time to carry out surface negative electricity hydroxylation treatment;
step two, vertically soaking the dried substrate after the negative electricity treatment in a high-concentration positively charged dodecahedron gold nanoparticle solution, wherein the high-concentration dodecahedron gold nanoparticle solution is an aqueous solution, an absolute ethanol solution or a toluene solution, and the solution is close to or reaches a saturated condition; then, the substrate is vertically separated from the liquid level at a slow speed, the environmental temperature in the whole self-assembly process is maintained within a certain range, and after the self-assembly process is finished, a single-layer gold nano-super-crystalline film structure can be formed on one end of the substrate in a large scale.
4. The self-assembly manufacturing method according to claim 3, characterized in that: the solid substrate is a common glass sheet, a silicon wafer or a germanium sheet, and the shape of the solid substrate is circular or square.
5. The self-assembly manufacturing method according to claim 3, characterized in that: the cleaning solution of the substrate is a toluene solution, an anhydrous methanol solution, an anhydrous ethanol solution and deionized water in sequence, the grade of the solution is analytically pure, the cleaning mode of the substrate is ultrasonic cleaning, and the cleaning time is 5-15 min each time.
6. The self-assembly manufacturing method according to claim 3, characterized in that: the surface negative electricity hydroxylation treatment time of the clean substrate in the goby boiling solution is at least more than 10 min.
7. The self-assembly manufacturing method according to claim 3, characterized in that: the high concentration solution of the thirty-dihedral gold nanoparticles is an aqueous solution, an absolute ethanol solution or a toluene solution, which is close to or reaches a saturated condition.
8. The self-assembly manufacturing method according to claim 3, characterized in that: the surface of the positively charged thirty-hedron nano particle is wrapped with a layer of poly diallyl dimethyl ammonium chloride (PDDA) molecules;
the dried substrate after the negative electricity treatment also needs to be in the vertical direction when being separated from the liquid surface, and the separation speed is controlled to be 0.1 mm/min-30 mm/min;
the external environment temperature in the whole self-assembly process is 25-100 ℃.
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