CN104630772A - Multilayer stacked metal nanosphere array and preparation method thereof - Google Patents
Multilayer stacked metal nanosphere array and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of a multilayer stacked metal nanosphere array. The method comprises the following steps: 1, growing a first metal film with the thickness of 2-10nm on a clean substrate through using a film plating technology; 2, carrying out primary annealing on the substrate obtained in step 1; 3, growing alumina with the thickness of 1-10nm on the substrate obtained in step 2 through using an atom deposition technology; 4, growing a second metal film with the thickness of 2-10nm on the substrate obtained in step 3 through using the film plating technology; and 5, carrying out secondary annealing on the substrate obtained in step 4. The method can realize the preparation of a large area of double-layer stacked metal nanosphere arrays, and has good repeatability and consistency.
Description
Technical field
The present invention relates to metal nano ball array preparation method, be specifically related to long-pending metal nano ball array of multilayer buttress and preparation method thereof
Background technology
Precious metal (such as gold and silver, platinum or palladium) nanometer ball array structure is the important feature paid special attention in the popular research field such as nanocomposite optical and surface phasmon, this is because the nano gap of adjacent noble metal nano ball can produce very strong electromagnetic focusing effect, cause enhancing and the local surface phasmon coupled resonance of local fields, thus cause significant optical enhancement effect, therefore in nanocomposite optical antenna, Raman enhancing, Fluorescence Increasing and biological detection and high resolution biosensing device etc., there is very important application prospect.
Chinese patent Authorization Notice No. CN100465345C, CN101698961B and CN101551330B disclose the preparation method of surface plasmon crystal, in these patents, mainly adopt template, namely on substrate, first form the template of colloidal crystal, depositing metallic nanoparticles in template, finally removes colloidal crystal template afterwards.
The long-pending metal nano ball array of theoretical report multilayer buttress has more excellent performance and application prospect, but based on above-mentioned preparation method, can not prepare the long-pending metal nano ball array structure of multilayer buttress at present.
Summary of the invention
For above-mentioned prior art, An embodiment provides the preparation method of the long-pending metal nano ball array of a kind of multilayer buttress, comprise the following steps:
(1) on the substrate of cleaning, utilize coating process to grow first metallic membrane of 2nm-10nm;
(2) substrate that step (1) obtains is carried out first time annealing;
(3) aluminum oxide that the substrate obtained in step (2) utilizes atomic deposition technique growth thickness to be 1nm-10nm;
(4) substrate obtained in step (3) utilize coating process grow second metallic membrane of 2nm-10nm;
(5) substrate that step (4) obtains is carried out second time annealing.
Preferably, in described step (3), the temperature of described atomic deposition technique is 80 DEG C-150 DEG C.
Preferably, in described step (3), growth thickness is the aluminum oxide of 3nm-5nm.
Preferably, the temperature of described first time annealing is 400 DEG C-500 DEG C, and the temperature of described second time annealing is 400 DEG C-500 DEG C.
Preferably, described first time annealing time be 2.5 minutes-3.5 minutes, described second time annealing time is 2.5 minutes-3.5 minutes.
Preferably, described coating process comprises thermal evaporation, electron beam evaporation or magnetron sputtering.
Preferably, the first metal is gold and silver, platinum or palladium, and described second metal is gold and silver, platinum or palladium.
Preferably, also comprise the steps: after described step (5)
(6) substrate obtained in step (5) utilizes the atomic deposition technique aluminum oxide that growth thickness is 3nm-5nm at 80 DEG C-150 DEG C;
(7) substrate obtained in step (6) utilizes the 3rd metallic membrane of thermal evaporation, electron beam evaporation or Grown by Magnetron Sputtering 2nm-10nm, described 3rd metal is gold and silver, platinum or palladium;
(8) substrate that step (7) obtains is annealed 2.5 minutes-3.5 minutes at 400 DEG C-500 DEG C.
Present invention also offers the multilayer formed by the preparation method of the long-pending metal nano ball array of above-mentioned multilayer buttress and pile up neatly long-pending metal nano ball array.
Present invention achieves the preparation of big area and the long-pending metal nano ball array of highdensity multilayer buttress, and the gap controllable precise of every one deck metal nano ball array.High-sensitivity biological Molecular Detection is carried out in the ideal structure substrate that the long-pending metal nano ball array of multilayer buttress of the present invention can be used for surface Raman enhancement.
Accompanying drawing explanation
Referring to accompanying drawing, embodiments of the present invention is further illustrated, wherein:
Fig. 1 to Fig. 5 is the schematic diagram of the preparation method of the long-pending metal nano ball array of multilayer buttress of present pre-ferred embodiments.
Fig. 6 is the SEM image of the metallic film that example one according to the present invention is prepared on substrate.
Fig. 7 is the SEM image of the metal nano ball array that example one according to the present invention is prepared on substrate.
Fig. 8 is the SEM image that the multilayer buttress prepared according to example one of the present invention amasss metal nano ball array.
Fig. 9 is the SEM image that the multilayer buttress prepared according to example two of the present invention amasss metal nano ball array.
Figure 10 is the SEM image that the multilayer buttress prepared according to example three of the present invention amasss metal nano ball array.
Figure 11 is the SEM image of the long-pending metal nano ball array of multilayer buttress prepared by embodiment according to the present invention four.
Figure 12 is the SEM image of the long-pending metal nano ball array of multilayer buttress prepared by embodiment according to the present invention five.
Embodiment
In order to make object of the present invention, technical scheme and advantage are clearly understood, below in conjunction with accompanying drawing, by specific embodiment, the present invention is described in more detail.
Fig. 1 to Fig. 5 is the schematic diagram of the preparation method of the long-pending metal nano ball array of multilayer buttress of present pre-ferred embodiments.As shown in Figure 1, choose the substrate base 1 of a clean surface, substrate base 1 is grown on the substrate base 1 of cleaning by filming equipments such as thermal evaporation, electron beam evaporation or magnetron sputterings the metallic membrane 2 of 2nm-10nm, the material of this metallic membrane 2 can be gold and silver, platinum or palladium, and wherein formed metallic membrane 2 is irregular island particle.As shown in Figure 2, the substrate base 1 of metal-plated membrane 2 is annealed in quick anneal oven, wherein annealing temperature is 400 DEG C-500 DEG C, annealing time 2.5 minutes-3.5 minutes, and the metallic membrane 1 of irregular island particle is become the metal nano ball 21 of uniformity by annealed technique.As shown in Figure 3, utilize atomic deposition technique at the aluminum oxide (Al of Surface coating one deck 1nm-10nm of metal nano ball 21 subsequently
2o
3) film 3, wherein depositing temperature is 80 DEG C-150 DEG C.As shown in Figure 4, then on aluminum oxide film 3, utilize the metallic membrane 4 of the filming equipment growth 2nm-10nm such as thermal evaporation, electron beam evaporation or magnetron sputtering, same metallic membrane 4 is irregular island particle, the material of this metallic membrane 4 can be gold and silver, platinum or palladium, wherein metallic membrane 2 can be different metal materials with metallic membrane 4, and preferable alloy film 2 and metallic membrane 4 have identical material and be any one in gold and silver, platinum or palladium.As shown in Figure 5, finally anneal in quick anneal oven, wherein annealing temperature is 400 DEG C-500 DEG C, annealing time 2.5 minutes-3.5 minutes, the metallic membrane 4 of irregular island particle is become the metal nano ball 41 of uniformity by annealed technique, wherein Metal Ball 41 is positioned at the top of Metal Ball 21, forms the long-pending structure of double-deck buttress.
In an embodiment of the present invention; the thickness of preferential oxidation aluminium film 3 is 3nm-5nm; at the Surface coating layer of metal nano ball 21 and the aluminum oxide film 3 of densification; for avoiding second time annealing to impact the shape and structure of metal nano ball 21, provide protection is served to metal nano ball 21.Embodiments of the invention by the thickness of atomic deposition technique accurate controlled oxidization aluminium film 3, thus can accurately can control the adjacent gap of adjacent layers metal nano ball array.In addition, by controlling the thickness of metallic film, thus after short annealing, the controlled nanometer ball of diameter is obtained.Embodiments of the invention can adopt arbitrary coating process on substrate or first layer metal nanometer ball array, grow the metallic film of 2nm-10nm.Wherein substrate base 1 can be silicon chip, can also be oxidized silicon chip, can be smooth substrate base, also can be have patterned substrate base.
Be illustrated to the preparation method of the long-pending metal nano ball array of multilayer buttress of the present invention below.
Example one
Choose one piece of smooth silicon chip, successively through acetone, alcohol and washed with de-ionized water 5 minutes, dry up by nitrogen gun, on the hot plate of 180 DEG C, baking obtains clean silicon chip for 5 minutes afterwards, cleaning silicon chip with thermal evaporation growth 5nm gold thin film, as shown in Figure 6, gold thin film is the island structure of non-compactness.Anneal in quick anneal oven afterwards, wherein annealing temperature is 450 DEG C, and annealing time is 3 minutes, obtain metal nano ball array structure as shown in Figure 7, as can be seen from Figure 7, gold thin film becomes nano level spherical particle after annealing, and the diameter of the nm gold particles of formation is approximately 30nm.Under 80 DEG C of conditions, adopt atomic deposition technique at the thick amorphous alumina thin film of the surface growth 3nm of gold grain afterwards, then adopt thermal evaporation on aluminum oxide film, grow the gold thin film of 5nm, finally anneal in quick anneal oven, wherein annealing temperature is 450 DEG C, annealing time is 3 minutes, thus the long-pending metal nano ball array of bilayer buttress obtained as shown in Figure 8, as shown in Figure 8, the inclined brilliant white of color be the gold nanosphere on upper strata, the gold nanosphere of what color was partially dark is lower floor, the diameter of every one deck gold nanosphere is approximately 30nm, and the thickness of aluminum oxide defines the gap of the first layer gold nanosphere and second layer gold nanosphere, be 3nm.Wherein nanometer ball density reaches 1.1 × 1011/square centimeter.
Example two
Prepare bilayer according to the technique substantially identical with example one and pile up neatly long-pending metal nano ball array, difference is, at the silverskin of the grown above silicon 7nm of cleaning, utilize atomic deposition technique to grow the amorphous alumina thin film of 4nm after first time annealing, on the thick aluminum oxide film of 4nm, grow the silverskin of 7nm afterwards.Fig. 9 is the SEM image of the long-pending metal nano ball array of bilayer buttress that example two according to the present invention prepares.The diameter of the nano-Ag particles of every one deck is approximately 40nm as can see from Figure 9, and the adjacent gap of the first layer nanometer ball array and second layer nanometer ball array is determined by the thickness of aluminum oxide, is 4nm.
Example three
Prepare three stacks according to the technique substantially identical with example one and amass metal nano ball array, difference is, the bilayer buttress formed in example one amasss on the basis of metal nano ball array, on second layer gold nanosphere array, utilize atomic deposition technique to grow the amorphous alumina of 3nm, wherein the temperature of atomic deposition is 80 DEG C, the golden film of the growth of thermal evaporation afterwards 5nm, last short annealing 3 minutes at 450 DEG C, thus three stacks obtained as shown in Figure 10 amass metal nano ball array.Those skilled in the art is known, amasss on metal nano ball array basis at three stacks of example three of the present invention, can also be grown more multi-layered buttress amass metal nano ball array by identical technique.
Example four
Prepare bilayer according to the technique substantially identical with example one and pile up neatly long-pending metal nano ball array, difference is, chooses the silicon chip with pyramid silicon cone array structure, and the cycle of pyramid silicon cone is 9 microns, and the length of side is 5 microns.Figure 11 is the SEM image of the long-pending metal nano ball array of bilayer buttress that example four according to the present invention prepares, and Figure 11 shows 6 pyramid silicon cones wherein, pyramid silicon cone above and the small point of surrounding be metal nano ball array.The preparation method of the long-pending metal nano ball array of multilayer buttress of the present invention can also prepare the long-pending metal nano ball array of multilayer buttress on various patterned substrate.Therefore, it is possible to well this multilayer of expansion buttress amasss the Application Areas of metal nano ball array.
Example five
Prepare bilayer according to the technique substantially identical with example one and pile up neatly long-pending metal nano ball array, difference is, chooses the silicon chip with high-aspect ratio silicon cone array structure, and the cycle of silicon cone is 300 nanometers, cone length 1.5 microns.At the golden film of this grown above silicon 2nm, after first time annealing, utilize atomic deposition technique to grow the amorphous alumina thin film of 5nm, on the thick amorphous alumina thin film of 5nm, grow the golden film of 2nm afterwards.Figure 12 demonstrates the SEM figure in silicon cone array cross section, and clearly can see that poppet surface and top part are uniformly distributed metal nano ball array, the micro bright point namely in Figure 12, wherein gold grain is of a size of 20 nanometers.The preparation method of the long-pending metal nano ball array of multilayer buttress of the present invention can also be attached on the nano graph array of structures of other long-width ratio.
In other embodiments of the invention, can by the size regulating the thickness of metallic membrane to change Metal Ball, the thickness of the metallic membrane in the present invention can be the arbitrary value between 2nm-10nm.In other embodiments of the invention, can be identical with the thickness of the second metallic membrane grown on aluminum oxide film at the thickness of the first metallic membrane of Grown, also can be different, in addition, first metal and the second metal can be identical metals, also can be different metals.
In the above embodiment of the present invention, the temperature of atomic deposition technique can be the arbitrary value between 80 DEG C-150 DEG C.Embodiments of the invention, except the preparation of the long-pending metal nano ball array of multilayer buttress that can realize gold and silver, can also realize the preparation of the long-pending metal nano ball array of multilayer buttress of the precious metal such as platinum and palladium.
Present invention achieves the preparation of the long-pending metal nano ball array of large-area bilayer buttress, and repeatable and consistence is good.The long-pending metal nano ball array of multilayer of the present invention buttress is significant to the applied research based on fields such as the molecular detection of surface enhanced Raman scattering, guided transmission and surface phasmons, especially can carry out high-sensitivity biological Molecular Detection as the desired result substrate of surface Raman enhancement.
Although the present invention is described by preferred embodiment, but the present invention is not limited to embodiment as described herein, also comprises done various change and change without departing from the present invention.
Claims (9)
1. a preparation method for the long-pending metal nano ball array of multilayer buttress, is characterized in that, comprise the following steps:
(1) on the substrate of cleaning, utilize coating process to grow first metallic membrane of 2nm-10nm;
(2) substrate that step (1) obtains is carried out first time annealing;
(3) aluminum oxide that the substrate obtained in step (2) utilizes atomic deposition technique growth thickness to be 1nm-10nm;
(4) substrate obtained in step (3) utilize coating process grow second metallic membrane of 2nm-10nm;
(5) substrate that step (4) obtains is carried out second time annealing.
2. the preparation method of the long-pending metal nano ball array of multilayer buttress according to claim 1, it is characterized in that, in described step (3), the temperature of described atomic deposition technique is 80 DEG C-150 DEG C.
3. the preparation method of the long-pending metal nano ball array of multilayer buttress according to claim 1 and 2, it is characterized in that, in described step (3), growth thickness is the aluminum oxide of 3nm-5nm.
4. the preparation method of the long-pending metal nano ball array of multilayer buttress according to claim 1, is characterized in that, the temperature of described first time annealing is 400 DEG C-500 DEG C, and the temperature of described second time annealing is 400 DEG C-500 DEG C.
5. the preparation method of the long-pending metal nano ball array of multilayer according to claim 4 buttress, is characterized in that, described first time annealing time be 2.5 minutes-3.5 minutes, described second time annealing time is 2.5 minutes-3.5 minutes.
6. the preparation method of the long-pending metal nano ball array of multilayer buttress according to claim 1, it is characterized in that, described coating process comprises thermal evaporation, electron beam evaporation or magnetron sputtering.
7. the preparation method of the long-pending metal nano ball array of multilayer buttress according to claim 1, it is characterized in that, the first metal is gold and silver, platinum or palladium, and described second metal is gold and silver, platinum or palladium.
8. the preparation method of the long-pending metal nano ball array of multilayer buttress according to claim 1, is characterized in that, also comprise the steps: after described step (5)
(6) substrate obtained in step (5) utilizes the atomic deposition technique aluminum oxide that growth thickness is 3nm-5nm at 80 DEG C-150 DEG C;
(7) substrate obtained in step (6) utilizes the 3rd metallic membrane of thermal evaporation, electron beam evaporation or Grown by Magnetron Sputtering 2nm-10nm, described 3rd metal is gold and silver, platinum or palladium;
(8) substrate that step (7) obtains is annealed 2.5 minutes-3.5 minutes at 400 DEG C-500 DEG C.
9. the multilayer formed by the preparation method of the long-pending metal nano ball array of multilayer buttress described in any one of claim 1 to 8 piles up neatly long-pending metal nano ball array.
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Application publication date: 20150520 |