CN104404624A - Controllable preparation method of three-dimensional nano plasmon polariton super crystals - Google Patents
Controllable preparation method of three-dimensional nano plasmon polariton super crystals Download PDFInfo
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- CN104404624A CN104404624A CN201410706175.4A CN201410706175A CN104404624A CN 104404624 A CN104404624 A CN 104404624A CN 201410706175 A CN201410706175 A CN 201410706175A CN 104404624 A CN104404624 A CN 104404624A
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Abstract
The invention discloses a controllable preparation method of three-dimensional nano plasmon polariton super crystals. The controllable preparation method of the three-dimensional nano plasmon polariton super crystals is characterized by comprising the following steps: adding a directional regulator into an optical anisotropic noble metal nano material solution, then dropwise adding the solution onto a substrate, controlling temperature and humidity of the environment in the lucifugal environment, naturally evaporating a solvent in the noble metal nano material for 15-30 hours, namely forming three-dimensional nano plasmon polariton super crystals with controllable direction and regular arrangement on the substrate. With combination of a nanocrystal plane chemical orientation anchoring method and an electrolyte ion activity physical adsorption method, the optical anisotropic three-dimensional nano plasmon polariton super crystals with the controllable direction and regular arrangement are formed on the substrate; the whole preparation process does not adopt complex instrument devices; the complex multi-step biological or chemical functionalization process is avoided; the preparation method of the three-dimensional nano plasmon polariton super crystals is simple and feasible to implement, and wide in universality.
Description
Technical field
The invention belongs to Meta Materials preparing technical field, be specifically related to the room temperature preparation method that a kind of optically anisotropic nanometer phasmon surpasses crystal.
Background technology
According to American Chemical Society's " chemistry comment " (Chemical Reviews, 2011, 111, the Review Study that the synthesis about noble metal nanometer material 3736-3827) forms Meta Materials with assembling shows, technique means main at present comprises with organism (as DNA, peptide chain, protein, microorganism) or chemical molecular (as organic polymer, colloidal materials) as template, by nanocrystals in template, the Meta Materials being combined to form different structure or the nanostructure utilizing ordered arrangement make mask, by the complicated physical technique means that technical requirements is high, as electron beam lithography, nanometer Meta Materials needed for focused-ion-beam lithography technique obtains.For these technique means reported, all relate to complicated biochemical reaction process, high to the stability requirement of the nano material relating to assembling, and physics preparation process is complicated.
Summary of the invention
What the object of this invention is to provide a kind of versatility prepares the simple technique means that noble metal nano surpasses crystal, and to realize, direction is controlled, the optically anisotropic three-dimensional manometer phasmon of arranging rule surpasses crystal.
Three-dimensional manometer phasmon of the present invention surpasses the controllable method for preparing of crystal, its feature is: in optically anisotropic noble metal nanometer material solution, add orientation adjustment agent, then drip in substrate, in light protected environment, control environment temperature and humidity, make the solvent spontaneous evaporation between 15 ~ 30 hours in noble metal nanometer material solution, in substrate, namely form that direction is controlled, the three-dimensional manometer phasmon of arranging rule surpasses crystal.
Three-dimensional manometer phasmon of the present invention surpasses the controllable method for preparing of crystal, and its feature is also: described orientation adjustment agent is nanocrystalline planar orientation anchoring agent or electrolyte ion activity conditioning agent;
When described orientation adjustment agent is nanocrystalline planar orientation anchoring agent, gained three-dimensional manometer phasmon surpasses crystal and is parallel to substrate arrangement;
When described orientation adjustment agent is electrolyte ion activity conditioning agent, gained three-dimensional manometer phasmon surpasses crystal and arranges perpendicular to substrate.
Described nanocrystalline planar orientation anchoring agent is sulfydryl-polyoxyethylene glycol; Described electrolyte ion activity conditioning agent is selected from sodium-chlor, saltpetre, magnesium chloride or potassium perchlorate.
When orientation adjustment agent is nanocrystalline planar orientation anchoring agent (sulfydryl-polyoxyethylene glycol), by nanocrystalline surface chemistry orientation anchorage method, the direction that three-dimensional surpasses crystal is controlled, in this technology of preparing, used the reactive behavior as its end face of optically anisotropic noble metal nanometer material (for nanometer rod) or three arms of angle (for triangular nano sheet) to be better than the reactive behavior of side (for nanometer rod) or triangular facet (for triangular nano sheet), control the consumption of sulfydryl-polyoxyethylene glycol, use is pretended by golden mercapto key, replace noble metal nanometer material tensio-active agent, shutoff is carried out to end face or three arms of angle, the tensio-active agent only leaving side or triangular facet forms three-dimensional super crystal for the self-assembly of nanometer rod or nanometer triangular plate.
When orientation adjustment agent is electrolyte ion activity conditioning agent (as NaCl), by adjustment electrolyte ion activity physical adsorption process, the direction that three-dimensional surpasses crystal is controlled, in this technology of preparing, use electrolytical intervention, change the ion(ic)activity in solution, have adjusted the balance between the electrostatic repulsion forces of the tensio-active agent of the coated noble metal nanometer material of tensio-active agent and in-fighting magnetism, the self-assembly that result in noble metal nanometer material forms three-dimensional phasmon and surpasses crystal.
Described optically anisotropic noble metal nanometer material is gold nanorods, gold nano triangular plate, gold and silver core-shell nanometer rod, gold and silver core-shell nano triangular plate.
Described substrate is silicon chip, sheet glass or indium tin oxide conductive film sheet glass.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, present invention utilizes the optical anisotropy noble metal nanometer material of single dispersiveness, under controlling moisture and temperature condition, by nanocrystalline surface chemistry orientation anchorage method in conjunction with electrolyte ion activity physical adsorption process, in the mode of spontaneous evaporation, dry in substrate, to form that direction is controlled, the optically anisotropic three-dimensional manometer phasmon of arranging rule surpasses crystal, whole making processes is not by the plant and instrument of complexity.
2, preparation method of the present invention avoids the process that multi-step biological or chemical functionalization is loaded down with trivial details, and its technology of preparing is simple, has universality widely simultaneously.The direction regulation and control of controlled synthesis, the three-dimensional manometer phasmon of arranging rule surpass crystal, pollutent in the environment, and the fields such as drugs, explosive substance and the identification of organism sensing have wide practical use.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of optical anisotropy gold nanorods;
Fig. 2 is the ultraviolet-visible-near infrared spectrogram of optical anisotropy gold nanorods;
Fig. 3 is the scanning electron microscope (SEM) photograph of the super crystal of three-dimensional manometer rod of the parallel silicon chip substrate arrangement of optical anisotropy gold nanorods;
Fig. 4 is the scanning electron microscope (SEM) photograph of the super crystal of three-dimensional manometer rod of the vertical silicon chip substrate arrangement of optical anisotropy gold nanorods;
Fig. 5 is the scanning electron microscope (SEM) photograph of optical anisotropy gold nano triangular plate;
Fig. 6 is the ultraviolet-visible-near infrared spectrogram of optical anisotropy gold nano triangular plate;
Fig. 7 is the scanning electron microscope (SEM) photograph that the three-dimensional manometer sheet of the vertical silicon chip substrate arrangement of optical anisotropy gold nano triangular plate surpasses crystal;
Fig. 8 is the scanning electron microscope (SEM) photograph that the three-dimensional manometer sheet of the parallel silicon chip substrate arrangement of optical anisotropy gold nano triangular plate surpasses crystal.
Embodiment
Embodiment 1: the three-dimensional gold nanorods phasmon of direction regulation and control surpasses the preparation of crystal
In the present embodiment, the regulatable three-dimensional gold nanorods phasmon in direction surpasses the concrete steps of crystal preparation:
1st step: by the hydrochloro-auric acid (HAuCl of 20mL, 0.5mM
4) solution is mixed to form mixed solution with the cetyl trimethylammonium bromide (CTAB) of 20mL, 0.2M mutually under condition of ice bath.Subsequently, the sodium borohydride (NaBH of 1.2mL, 0.02M
4) join in above-mentioned mixed solution, under 1000rpm speed conditions, vigorous stirring 2 minutes, and 1 hour is left standstill at 25 DEG C, obtain the solution containing nanometer gold seed; By the Silver Nitrate (AgNO of CTAB and the 10mL of 200mL, 0.2M, 4mM
3) solution is mixed to form yellow growth liquid at ambient temperature; By the HAuCl of 200mL, 1mM
4solution adds above-mentioned growth liquid, and along with the adding of xitix of 2.8mL, 0.08M, yellow growth liquid becomes colourless mixed solution, shows that the gold of three valence states is reduced into the gold of a valence state.The solution containing nanometer gold seed of 480 μ L is added above-mentioned colourless mixed solution, and after 5-10 minute, the color of solution becomes cinnabar redness from colourless, shows that gold nanorods is formed.The gold nanorods growth liquid of fresh preparation, leaves standstill 24 hours, under 10000rpm speed conditions centrifugal 20 minutes, removes supernatant liquor, is again dissolved in 40mL ultrapure water, obtains gold nanorods solution for standby.
Fig. 1 gives the scanning electron microscope (SEM) photograph of the optical anisotropy gold nanorods within the scope of the big scale of above-mentioned preparation.Clearly can observe single dispersiveness from Fig. 1, highly purified gold nanorods is produced.Fig. 2 gives the ultraviolet-visible-near infrared spectrogram of optical anisotropy gold nanorods.Highly purified gold nanorods is produced as can be seen from Figure 2, two plasmon resonance bands of gold nanorods, is namely distributed in the transverse direction of 519nm wavelength and the radial plasmon resonance band of 701nm wavelength, can be observed.
2nd step: get 1mL gold nanorods solution prepared by above-mentioned steps, add the sulfydryl-polyoxyethylene glycol (molecular weight 6000MW) of 100 μ L 1mg/mL, under 25 DEG C of conditions, react 2 hours, under 10000rpm speed conditions, within centrifugal 10 minutes, remove supernatant liquor, be again dissolved in 200 μ L ultrapure waters, get 10 μ L and drop on the clean silicon chip of the vitriol oil/hydrogen peroxide (3:1) 80 DEG C of conditions process in lower 1 hour.Then, under being placed in the environment of room temperature 25 DEG C and 80% humidity lucifuge, treat that it slowly dries for 24 hours naturally.After the process of slow evaporation, can at the bottom of silicon wafer-based on form a coffee ring, the three-dimensional being distributed in the regularly arranged parallel silicon chip substrate of gold nanorods height of formation on coffee ring surpasses crystal.In this technology of preparing, used the reactive behavior as optically anisotropic its end face of gold nanorods to be better than the reactive behavior of side, control the consumption of sulfydryl-polyoxyethylene glycol, use is pretended by golden mercapto key, replace gold nanorods tensio-active agent, carry out shutoff to end face, the tensio-active agent only leaving gold nanorods side forms three-dimensional super crystal for the self-assembly of gold nanorods.
The three-dimensional manometer rod phasmon that Fig. 3 gives the parallel silicon chip substrate arrangement of optical anisotropy gold nanorods within the scope of big scale surpasses the scanning electron microscope (SEM) photograph of crystal.From Fig. 3 can clearly observe gold nanorods parallel at the bottom of silicon wafer-based, define the bar-shaped super crystal of three-dimensional of tight regular array.
3rd step: get 1mL gold nanorods solution prepared by the first step, under 10000rpm speed conditions, centrifugal 10 minutes, remove supernatant liquor, again be dissolved in 50 μ L, 0.01M NaCl solution, get 10 μ L and drop on the clean silicon chip of the vitriol oil/hydrogen peroxide (3:1) 80 DEG C of conditions process in lower 1 hour.Then, under being placed in the environment of room temperature 25 DEG C and 80% humidity lucifuge, treat that it slowly dries for 24 hours naturally.After the process of slow evaporation, can at the bottom of silicon wafer-based on form a coffee ring, the three-dimensional being distributed in the regularly arranged vertical silicon chip substrate of gold nanorods height of formation on coffee ring surpasses crystal.In this technology of preparing, use electrolytical intervention, change the ion(ic)activity in solution, have adjusted the balance between tensio-active agent positive polarity cetyl trimethylammonium bromide (CTAB) electrostatic repulsion forces of the coated gold nanorods of tensio-active agent and in-fighting magnetism, the self-assembly that result in gold nanorods forms three-dimensional phasmon and surpasses crystal.
Fig. 4 gives the scanning electron microscope (SEM) photograph of the super crystal of three-dimensional manometer rod of the vertical silicon chip substrate arrangement of the optical anisotropy gold nanorods within the scope of big scale.From Fig. 4 clearly can observe that gold nanorods is vertically at the bottom of silicon wafer-based, define the bar-shaped super crystal of three-dimensional of tight regular array.
In view of the difference of the phasmon field-effect that the noble metal nanometer material of different-shape and component causes, therefore, in the inventive method, the optical anisotropy nano particle of gold nanorods, gold nano triangular plate, gold and silver core-shell nanometer rod, gold and silver core-shell nano triangular plate can be selected from as the noble metal nanometer material constructing three-dimensional phasmon and surpass crystal.Owing to wherein can cause the power of solion activity as electrolytical kind difference, affect super crystal in suprabasil arrangement, therefore as ion(ic)activity conditioning agent, sodium-chlor, saltpetre, magnesium chloride, potassium perchlorate can be selected from.As the super crystal formation substrate of support, silicon chip, sheet glass, indium tin oxide conductive film sheet glass can be selected from.
Embodiment 2: the controlled three-dimensional gold nano triangular plate phasmon in direction surpasses the preparation of crystal
The three-dimensional gold nano triangular plate phasmon that in the present embodiment, direction is controlled surpasses the concrete steps of crystal preparation:
1st step: 1mL, 0.01M chlorauric acid solution and 1mL, 0.01M citric acid three sodium solution, be diluted with water to 40mL, mixed solution is mixed to get under condition of ice bath, add 1mL, 0.1M sodium borohydride again, under 1000rpm speed conditions, vigorous stirring 2 minutes, leaves standstill 2-4 hour, obtains the solution containing nanometer gold seed at 25 DEG C.Then, 225mL, 0.05MCTAB, 1mL, 0.1M KI, 1.25mL, 0.1M xitix, 1.25mL, 0.1M NaOH, 6.25mL, 0.01M chlorauric acid solution is mixed to form mixing growth liquid mutually.Subsequently, from the Erlenmeyer flask C filling 225mL mixing growth liquid, get 22.5mL in tap web bottle B, in tap web bottle B, get 2.25mL in Erlenmeyer flask A.Finally, in tap web bottle A, add the solution of the nanometer gold seed of the above-mentioned preparation of 225 μ L, pour solution in A bottle into B bottle rapidly, then B bottle solution is transferred to C bottle immediately.After 5-10 minute, the color of solution becomes red-purple from colourless, shows that gold nano triangular plate starts to be formed.The gold nano triangular plate growth liquid of fresh preparation, leaves standstill 24 hours, collects the green solution bottom tap web bottle, then under 6000rpm speed conditions centrifugal treating 20 minutes, be again dissolved in 20mL ultrapure water and obtain gold nano triangular plate solution for standby.
Fig. 5 gives the scanning electron microscope (SEM) photograph of the optical anisotropy gold nano triangular plate within the scope of big scale.Clearly can observe single dispersiveness from Fig. 5, highly purified gold nano triangular plate is produced.Fig. 6 gives the ultraviolet-visible-near infrared spectrogram of optical anisotropy gold nano triangular plate.Two plasmon resonance bands of gold nano triangular plate as can be seen from Figure 6, namely the near infrared plasmon resonance band of moment of dipole in plane interior the moment of dipole vibration of 761 nano wave lengths and the plane of 1101 nano wave lengths is distributed in, can be observed, be distributed in the disappearance of the phasmon band of the spherical nanoparticle of 525 nano wave lengths simultaneously, illustrate that highly purified gold nano triangular plate is produced.
2nd step: get 2mL gold nano triangular plate solution prepared by above-mentioned steps, under 10000rpm rotating speed, centrifugal 10 minutes, remove supernatant liquor, again be dissolved in 50 μ L, 0.02M NaCl solution, get 10 μ L and drop on the clean silicon chip of the vitriol oil/hydrogen peroxide (3:1) 80 DEG C of conditions process in lower 1 hour.Get 10 μ L to drop on the clean silicon chip of the vitriol oil/hydrogen peroxide (3:1) 80 DEG C of conditions process in lower 1 hour.Then, under being placed in the environment of room temperature 25 DEG C and 80% humidity lucifuge, treat that it slowly dries for 24 hours naturally.After the process of slow evaporation, understand at the bottom of silicon wafer-based and form a coffee ring, the three-dimensional phasmon that the gold nano triangular plate be distributed on coffee ring is formed with regularly arranged vertical silicon chip substrate surpasses crystal.
The three-dimensional phasmon that Fig. 7 gives the vertical silicon chip substrate arrangement of optical anisotropy gold nano triangular plate within the scope of big scale surpasses the scanning electron microscope (SEM) photograph of crystal.From Fig. 7 clearly can observe that gold nano triangular plate is vertically at the bottom of silicon wafer-based, the three-dimensional phasmon defining tight regular array surpasses crystal.
3rd step: get 1mL gold nano triangular plate prepared by the first step, add 50 μ L, 1mg/mL sulfydryl-polyoxyethylene glycol (molecular weight 6000MW), under 25 DEG C of conditions, react 2 hours, under 6000rpm speed conditions, within centrifugal 10 minutes, remove supernatant liquor, be again dissolved in 200uL ultrapure water, get 10 μ L and drop on the clean silicon chip of the vitriol oil/hydrogen peroxide (3:1) 80 DEG C of conditions process in lower 1 hour.Then, under being placed in the environment of room temperature 25 DEG C and 80% humidity lucifuge, treat that it slowly dries for 24 hours naturally.After the process of slow evaporation, can at the bottom of silicon wafer-based on form a coffee ring, the three-dimensional being distributed in the regularly arranged parallel silicon chip of gold nano triangular plate height of formation on coffee ring surpasses crystal.In this technology of preparing, used the reactive behavior as optically anisotropic its three arm of angle of gold nano triangular plate to be better than the reactive behavior of triangular facet, control the consumption of mercapto-polyglycol, use is pretended by golden mercapto key, replace gold-nano-piece tensio-active agent, carry out shutoff to three arms of angle, the tensio-active agent only leaving gold-nano-piece triangular facet forms super crystal for the self-assembly of gold-nano-piece.
The three-dimensional manometer sheet phasmon that Fig. 8 gives the parallel silicon chip substrate arrangement of optical anisotropy gold nano triangular plate within the scope of big scale surpasses the scanning electron microscope (SEM) photograph of crystal.From Fig. 8 can clearly observe gold nano triangular plate parallel at the bottom of silicon wafer-based, the three-dimensional sheet phasmon defining tight regular array surpasses crystal.
With the chemical-biological reported at present compared with physics technology of preparing, the invention has the advantages that, make use of the optical anisotropy noble metal nanometer material of single dispersiveness, under controlling moisture and temperature condition, selected by orientation adjustment agent, comprise nanocrystalline surface chemistry orientation anchorage method and adjustment electrolyte ion activity physical adsorption process, dry in the mode of spontaneous evaporation in substrate, constructed direction regulation and control, the optically anisotropic nanometer phasmon of arranging rule surpasses crystal.Relative to current existing various technique means, the technology of the present invention, not by the plant and instrument of complexity, does not adopt the process that multi-step biological or chemical functionalization is loaded down with trivial details, and its technology of preparing is simple and have versatility widely.
Claims (5)
1. a three-dimensional manometer phasmon surpasses the controllable method for preparing of crystal, it is characterized in that: in optically anisotropic noble metal nanometer material solution, add orientation adjustment agent, then drip in substrate, in light protected environment, control environment temperature and humidity, make the solvent spontaneous evaporation between 15 ~ 30 hours in noble metal nanometer material solution, in substrate, namely form that direction is controlled, the three-dimensional manometer phasmon of arranging rule surpasses crystal.
2. method according to claim 1, is characterized in that: described orientation adjustment agent is nanocrystalline planar orientation anchoring agent or electrolyte ion activity conditioning agent;
When described orientation adjustment agent is nanocrystalline planar orientation anchoring agent, gained three-dimensional manometer phasmon surpasses crystal and is parallel to substrate arrangement;
When described orientation adjustment agent is electrolyte ion activity conditioning agent, gained three-dimensional manometer phasmon surpasses crystal and arranges perpendicular to substrate.
3. method according to claim 2, is characterized in that: described nanocrystalline planar orientation anchoring agent is sulfydryl-polyoxyethylene glycol;
Described electrolyte ion activity conditioning agent is sodium-chlor, saltpetre, magnesium chloride or potassium perchlorate.
4. method according to claim 1 and 2, is characterized in that: described optically anisotropic noble metal nanometer material is gold nanorods, gold nano triangular plate, gold and silver core-shell nanometer rod, gold and silver core-shell nano triangular plate.
5. method according to claim 1 and 2, is characterized in that: described substrate is silicon chip, sheet glass or indium tin oxide conductive film sheet glass.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2019165714A1 (en) * | 2018-03-01 | 2019-09-06 | 东南大学 | Large-scale controllable preparation method for surface plasmon nanonail structure |
| CN112719491A (en) * | 2021-01-20 | 2021-04-30 | 河南理工大学 | Method for electrolytically machining micro texture by using microbial mask |
| CN114016139A (en) * | 2021-11-09 | 2022-02-08 | 嘉兴学院 | Preparation method of nanocrystalline superlattice material |
| CN114226743A (en) * | 2021-10-08 | 2022-03-25 | 西安邮电大学 | Preparation method of island film-shaped nano cubic array structure |
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| CN104163453A (en) * | 2014-07-21 | 2014-11-26 | 复旦大学 | Preparation method of highly-ordered nano particle superlattice material |
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| CN104163453A (en) * | 2014-07-21 | 2014-11-26 | 复旦大学 | Preparation method of highly-ordered nano particle superlattice material |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019165714A1 (en) * | 2018-03-01 | 2019-09-06 | 东南大学 | Large-scale controllable preparation method for surface plasmon nanonail structure |
| US11077499B2 (en) | 2018-03-01 | 2021-08-03 | Southeast University | Large-scale controllable preparation method for plasmonic nanonail structure |
| CN112719491A (en) * | 2021-01-20 | 2021-04-30 | 河南理工大学 | Method for electrolytically machining micro texture by using microbial mask |
| CN112719491B (en) * | 2021-01-20 | 2022-03-15 | 河南理工大学 | Method for electrolytically machining micro texture by using microbial mask |
| CN114226743A (en) * | 2021-10-08 | 2022-03-25 | 西安邮电大学 | Preparation method of island film-shaped nano cubic array structure |
| CN114226743B (en) * | 2021-10-08 | 2023-11-21 | 西安邮电大学 | Preparation method of island film-shaped nano cubic array structure |
| CN114016139A (en) * | 2021-11-09 | 2022-02-08 | 嘉兴学院 | Preparation method of nanocrystalline superlattice material |
| CN114016139B (en) * | 2021-11-09 | 2022-07-29 | 嘉兴学院 | Preparation method of nanocrystalline material |
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