CN102212790A - Preparation method of noble metal/submicron spherical shell arrays - Google Patents
Preparation method of noble metal/submicron spherical shell arrays Download PDFInfo
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Abstract
The invention discloses a preparation method of noble metal/submicron spherical shell arrays, which comprises the following steps: firstly, self-assembling submicron polystyrene microsphere arrays with different diameters on quartz and other substrates; then, depositing noble metal layers on the polystyrene microsphere arrays through direct current magnetron sputtering; and finally, carrying out heat treatment in a vacuum chamber to remove the polystyrene microsphere templates. In the method, the growing process is simple and controllable, and the prepared spherical shell arrays are uniform in dimension and are regularly arranged; and by regulating the thickness of the noble metal layers, the spherical shell arrays with different surface plasmon resonance peaks can be obtained and can be used in the fields such as biosensors, photonic crystals, surface-enhanced Raman spectra, luminescent spectra and the like.
Description
Technical field
The invention belongs to the photonic material preparation field, be specifically related to a kind of preparation method of precious metal submicron spherical shell array.
Background technology
Surface plasma resonance technology is a kind of biomolecule detection technology that grows up the nineties in 20th century, in medical diagnosis, and biological detection, fields such as medicine development and food safety all are widely used.Surface plasma is meant near the charge density oscillation of local metal nanoparticle.When incident electromagnetic field (light) and plasma frequency generation resonance excitation, can produce the enhancing of intensive delustring (absorbing and scattering) or localized electromagnetic field.Equaling nineteen eighty-three from Liedberg uses plasma resonance technology to carry out since antigen antibody interaction analyzes first, this biosensor technology has been widely used in proteomics, cell signaling, receptor/ligand, the antibody/antigen molecule is fished, immunity identification, life science such as cancer research and new medicament screen, be used for real-time and dynamic studies protein-protein, protein-nucleic acid, bio-molecular interaction processes such as new drug molecule-target protein, since particularly using from business-like surface phasmon of nineteen ninety (SPR), spr sensor has fundamentally changed the biomolecules cognitive science, becomes the tool master in life science and the pharmacy research.
Precious metal (as silver, gold etc.) micro-nano particle has very strong local surface plasma effect, its surface plasma resonance wavelength is positioned at the Visible-to-Near InfaRed district, and resonance delustring character changes with the variation of factors such as particulate size, shape, arrangement mode, dielectric environment.Up to the present, the surface plasma resonance effect of noble metal nano particles has obtained application more and more widely at aspects such as light transmission, local fields enhanced spectrum, bio-sensings.
Noble metal granule with spherical shell structure is a kind of very important photonic material with surface plasma resonance characteristic, this material can be regulated its surface etc. from resonant wavelength by the inside/outside diameter size of control metal spherical shell, its peak position can be adjusted to the near-infrared region from whole visible region, and has good scattering properties.After precious metal sub-micron ball hull shape became array, the local surface plasma resonance coupling in the structure made and forms the high local point of electromagnetic field in some zone, strengthens the intensity of electromagnetic field greatly, thereby improves the sensitivity that detects.This characteristic has stronger application prospect aspect biological detection, sensing and the enhanced spectrum.
Generally speaking, template is mainly adopted in the preparation of metal nano spherical shell structure, and for example forming core on silicon-dioxide or polystyrene microsphere adopts the chemical method growth in solution.This method exist the metal shell unlikely close, metallic particles is easily reunited, preparation method's complexity, shortcoming such as yield poorly, and has limited the application of precious metal spherical shell structure greatly.
Generally speaking, the existing preparation technology can not satisfy the requirement of the precious metal submicron spherical shell array photonic material of scale operation highly sensitive, high homogeneity.
Summary of the invention
The invention provides a kind of preparation method of precious metal submicron spherical shell array, the densification of can growing, the adjustable layer of precious metal of even, interior external diameter relative dimension.
A kind of preparation method of precious metal submicron spherical shell array comprises the steps:
(1) be that the polystyrene microsphere of 100-1000nm is scattered in the mixed solution of water and alcohol with diameter, the concentration that is mixed with polystyrene microsphere is the mixing solutions of 0.54-1.89mg/ml; Drip described mixing solutions at the bottom of quartzy, graphite or the silicon wafer-based and dry, obtain the substrate of polystyrene microsphere array;
(2) reaction chamber of direct current reaction magnetron sputtering device is put in the substrate that the polystyrene microsphere array is arranged that step (1) is obtained, and is target with the precious metal, in a vacuum by the magnetron sputtering deposition layer of precious metal;
(3) substrate behind the depositing noble metal layer that step (2) is obtained is heated to 200-300 ℃, is incubated 10-60 minute, to remove polystyrene microsphere template, obtains precious metal submicron spherical shell array on substrate.
In the optimized technical scheme, in the step (1), the volume ratio of described water and alcohol is 1: 5-1: 1.
In the optimized technical scheme, in the step (2), the vacuum tightness of the reaction chamber of described direct current reaction magnetron sputtering device is 5 * 10
-3Pa and following is that sputtering atmosphere feeds reaction chamber with the argon gas, and dominant discharge is 20-30sccm, and the reaction chamber internal gas pressure remains on 10～20Pa, and sputtering power is at 40-70W, and sputtering time is controlled at 20s-120s, and growth temperature is a room temperature.In the most preferred technical scheme, the flow of argon gas is 30sccm, and deposition pressure is 10Pa, and sputtering power is 58-62W, can prepare evenly neat array structure under this condition at low temperatures.
Described precious metal is preferably gold and silver, platinum, palladium etc., most preferably is gold or silver.
Described precious metal is selected high-purity precious metal usually for use, purity be 99% and more than.
Among the present invention, described polystyrene microsphere can be by commercially available acquisition, as lark prestige chemical company.
The present invention prepares precious metal submicron spherical shell array with magnetron sputtering method, what adopt is to be the preparation technology of the metal vacuum deposition of template with the polystyrene microsphere array, at first at the submicron polystyrene microsphere array of substrate self-assembly different diameters such as quartz, utilize magnetically controlled DC sputtering depositing noble metal layer on the polystyrene microsphere array again, remove polystyrene microsphere template by thermal treatment in vacuum chamber at last.With the polystyrene microsphere is template, and can simply remove by the method for heating; Adopt the method growth precious metal spherical shell of magnetically controlled DC sputtering, the metal spherical shell array good uniformity of growth, to be easy to repetition, output height and step simple, can control footpath relative dimension inside and outside the metal spherical shell by sputtering time, obtain having the spherical shell array from resonance characteristic such as different surfaces.
The process of growth simple controllable of the inventive method, the spherical shell array sizes homogeneous of preparation, marshalling, by regulating external diameter relative dimension in the precious metal spherical shell, can obtain the different spherical shell array of surface plasmon resonance peak position, can be used for fields such as bio-sensing, photonic crystal, surface enhanced Raman spectroscopy and luminescent spectrum.
Description of drawings
Fig. 1 is a field emission scanning electron microscope photo of removing the preceding array structure of template among the embodiment 1;
Fig. 2 is the field emission scanning electron microscope photo of the array structure after the removal template among the embodiment 1;
The transmission electron microscope photo of the metal spherical shell that Fig. 3 makes for embodiment 1;
The metal spherical shell selected area electron diffraction photo that Fig. 4 makes for embodiment 1;
Fig. 5 is the ultraviolet-visible delustring spectrum that sample is removed the template front and back among the embodiment 1;
The ultraviolet-visible delustring spectrum of the ping-pong ball shell array of the different thickness that Fig. 6 makes for embodiment 1,2,3;
Fig. 7 is the field emission scanning electron microscope photo of the gold goal shell array structure after the removal template among the embodiment 5.
Embodiment
Below, describe content of the present invention in detail by embodiment and accompanying drawing, but the present invention is not limited thereto.
Embodiment 1:
With diameter is that the polystyrene microsphere of 200nm is scattered in the mixed solution that volume ratio is 1: 1 water and alcohol, and the concentration that is mixed with polystyrene microsphere is the mixing solutions of 1.89g/ml; Get the above-mentioned mixing solutions of 20 μ l and drip on quartz substrate and at room temperature dry, obtain the quartz substrate of polystyrene microsphere array; The reaction chamber that will have the quartz substrate of polystyrene microsphere array to put into the direct current reaction magnetron sputtering device deposits silver layer, and reaction chamber vacuum tightness is evacuated to 5 * 10
-3Pa feeds argon gas as shielding gas, and argon flow amount is controlled at 30sccm, reaction chamber air pressure is adjusted into 10Pa, is that silver more than 99% is that target carries out sputtering sedimentation with purity, and sputtering current and power are controlled at 0.2A and 60W respectively, sputtering time is 60s, and growth temperature is a room temperature; After silver layer deposition was finished, the temperature to 200 of the sample table that reacting by heating is indoor ℃ kept about 30 minutes, with the removal polystyrene microsphere template, obtained ping-pong ball shell array on substrate.
The final product that embodiment 1 is obtained carries out transmission electron microscope and field emission scanning electron microscope test and analysis, and shown in Fig. 3 and 4, the field emission scanning electron microscope photo as shown in Figure 2 respectively for transmission electron microscope photo and selected area electron diffraction picture.
The spherical shell structure of marshalling as seen from Figure 2, the about 250 ± 10nm of spherical shell external diameter; About 40nm ± the 5nm of the thickness of spherical shell as seen from Figure 3; Analysis draws to Fig. 4, and shell is the crystallinity simple substance silver of face-centred cubic structure preferably.
In order to contrast, provided the field emission scanning electron microscope photo of removing the preceding silver-microballoon nucleocapsid array of polystyrene ball template among the embodiment 1, as shown in Figure 1, visible metal shell has wrapped up microsphere surface fully.
Further, give the delustring spectrum of removing sample before and after the polystyrene ball template, as shown in Figure 5, as seen: the surface of sample etc. from resonance peak from the 700nm blue shift to 600nm.This shows that also polystyrene moulding is removed, and change has taken place dielectric environment around the metal shell.
Embodiment 2
With diameter is that the polystyrene microsphere of 200nm is scattered in the mixed solution that volume ratio is 1: 1 water and alcohol, and the concentration that is mixed with polystyrene microsphere is the mixing solutions of 1.89g/ml; Get the above-mentioned mixing solutions of 20 μ l and drip on quartz substrate and at room temperature dry, obtain the quartz substrate of polystyrene microsphere array; The reaction chamber that will have the quartz substrate of polystyrene microsphere array to put into the direct current reaction magnetron sputtering device deposits silver layer, and reaction chamber vacuum tightness is evacuated to 5 * 10
-3Pa feeds argon gas as shielding gas, and argon flow amount is controlled at 30sccm, reaction chamber air pressure is adjusted into 10Pa, is that silver more than 99% is that target carries out sputtering sedimentation with purity, and sputtering current and power are controlled at 0.2A and 60W respectively, sputtering time is 45s, and growth temperature is a room temperature; After silver layer deposition was finished, the temperature to 200 of the sample table that reacting by heating is indoor ℃ kept about 30 minutes, with the removal polystyrene microsphere template, obtained ping-pong ball shell array on substrate.
The final product that embodiment 2 is obtained carries out transmission electron microscope and field emission scanning electron microscope test and analysis, observes as seen: the spherical shell structure of marshalling, the about 250 ± 10nm of spherical shell external diameter, the about 30 ± 5nm of the thickness of spherical shell; Further analyze, the spherical shell shell is the crystallinity simple substance silver of face-centred cubic structure preferably.
Embodiment 3
With diameter is that the polystyrene microsphere of 200nm is scattered in the mixed solution that volume ratio is 1: 1 water and alcohol, and the concentration that is mixed with polystyrene microsphere is the mixing solutions of 1.89g/ml; Get the above-mentioned mixing solutions of 20 μ l and drip on quartz substrate and at room temperature dry, obtain the quartz substrate of polystyrene microsphere array; The reaction chamber that will have the quartz substrate of polystyrene microsphere array to put into the direct current reaction magnetron sputtering device deposits silver layer, and reaction chamber vacuum tightness is evacuated to 5 * 10
-3Pa feeds argon gas as shielding gas, and argon flow amount is controlled at 30sccm, reaction chamber air pressure is adjusted into 10Pa, is that silver more than 99% is that target carries out sputtering sedimentation with purity, and sputtering current and power are controlled at 0.2A and 60W respectively, sputtering time is 20s, and growth temperature is a room temperature; After silver layer deposition was finished, the temperature to 200 of the sample table that reacting by heating is indoor ℃ kept about 30 minutes, with the removal polystyrene microsphere template, obtained ping-pong ball shell array on substrate.
The final product that embodiment 3 is obtained carries out transmission electron microscope and field emission scanning electron microscope test and analysis, observes as seen: the spherical shell structure of marshalling, the about 250 ± 10nm of spherical shell external diameter, the about 10 ± 5nm of the thickness of spherical shell; Further analyze, the spherical shell shell is the crystallinity simple substance silver of face-centred cubic structure preferably.
Fig. 6 has provided in embodiment 1,2 and 3, the delustring of ping-pong ball shell structure spectrum under the different preparation condition of sputtering time, and as can be seen, along with the increase of sputtering time, it is big that silver-colored shell thickness becomes, the generation red shift of delustring peak.
Embodiment 4
With diameter is that the polystyrene microsphere of 500nm is scattered in the mixed solution that volume ratio is 1: 1 water and alcohol, and the concentration that is mixed with polystyrene microsphere is the mixing solutions of 1.89g/ml; Get the above-mentioned mixing solutions of 20 μ l and drip on quartz substrate and at room temperature dry, obtain the quartz substrate of polystyrene microsphere array; The reaction chamber that will have the quartz substrate of polystyrene microsphere array to put into the direct current reaction magnetron sputtering device deposits silver layer, and reaction chamber vacuum tightness is evacuated to 5 * 10
-3Pa feeds argon gas as shielding gas, and argon flow amount is controlled at 30sccm, reaction chamber air pressure is adjusted into 10Pa, is that silver more than 99% is that target carries out sputtering sedimentation with purity, and sputtering current and power are controlled at 0.2A and 60W respectively, sputtering time is respectively 100s, and growth temperature is a room temperature; After silver layer deposition was finished, the temperature to 200 of the sample table that reacting by heating is indoor ℃ kept about 30 minutes, with the removal polystyrene microsphere template, obtained ping-pong ball shell array on substrate.
The final product that embodiment 4 is obtained carries out transmission electron microscope and field emission scanning electron microscope test and analysis, observes as seen: the spherical shell structure of marshalling, the about 550 ± 10nm of spherical shell external diameter, the about 50 ± 5nm of the thickness of spherical shell; Further analyze, the spherical shell shell is the crystallinity simple substance silver of face-centred cubic structure preferably.
Embodiment 5
With diameter is that the polystyrene microsphere of 200nm is scattered in the mixed solution that volume ratio is 1: 1 water and alcohol, and the concentration that is mixed with polystyrene microsphere is the mixing solutions of 1.89g/ml; Get the above-mentioned mixing solutions of 10 μ l and drip on quartz substrate and at room temperature dry, obtain the quartz substrate of polystyrene microsphere array; To have the quartz substrate of polystyrene microsphere array to put into the reaction chamber deposited gold layer of direct current reaction magnetron sputtering device, reaction chamber vacuum tightness is evacuated to 5 * 10
-3Pa feeds argon gas as shielding gas, and argon flow amount is controlled at 20sccm, reaction chamber air pressure is adjusted into 10Pa, is that gold more than 99% is that target carries out sputtering sedimentation with purity, and sputtering current and power are controlled at 0.2A and 60W respectively, sputtering time is respectively 45s, and growth temperature is a room temperature; After gold layer deposition finished, the temperature to 300 of the sample table that reacting by heating is indoor ℃ kept about 30 minutes, with the removal polystyrene microsphere template, obtained gold goal shell array on substrate.
The final product that embodiment 5 is obtained carries out field emission scanning electron microscope (Fig. 7) test and analysis, observe as seen: the spherical shell structure of marshalling, about 250 ± the 10nm of spherical shell external diameter further analyzes, and the spherical shell shell is the crystallinity simple substance gold of face-centred cubic structure preferably.
Claims (6)
1. the preparation method of a precious metal submicron spherical shell array is characterized in that, comprises the steps:
(1) be that the polystyrene microsphere of 100-1000nm is scattered in the mixed solution of water and alcohol with diameter, the concentration that is mixed with polystyrene microsphere is the mixing solutions of 0.54-1.89mg/ml; Drip described mixing solutions at the bottom of quartzy, graphite or the silicon wafer-based and dry, obtain the substrate of polystyrene microsphere array;
(2) reaction chamber of direct current reaction magnetron sputtering device is put in the substrate that the polystyrene microsphere array is arranged that step (1) is obtained, and is target with the precious metal, in a vacuum by the magnetron sputtering deposition layer of precious metal;
(3) substrate behind the depositing noble metal layer that step (2) is obtained is heated to 200-300 ℃, is incubated 10-60 minute, to remove polystyrene microsphere template, obtains precious metal submicron spherical shell array on substrate.
2. preparation method according to claim 1 is characterized in that: the volume ratio of water and alcohol is 1 in the described step (1): 5-1: 1.
3. preparation method according to claim 1 is characterized in that: the vacuum tightness of the reaction chamber of the direct current reaction magnetron sputtering device described in the described step (2) is 5 * 10
-3Pa and following is that sputtering atmosphere feeds reaction chamber with the argon gas, and dominant discharge is 20-30sccm, and the reaction chamber internal gas pressure remains on 10～20Pa, and sputtering power is at 40-70W, and sputtering time is controlled at 20s-120s, and growth temperature is a room temperature.
4. preparation method according to claim 3 is characterized in that: the flow of argon gas is 30sccm in the described step (2), and deposition pressure is 10Pa, and sputtering power is 58-62W.
5. method according to claim 1 is characterized in that: described precious metal is gold and silver, platinum or palladium.
6. method according to claim 1 is characterized in that: the purity of described precious metal be 99% and more than.
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| CN103058124A (en) * | 2011-10-21 | 2013-04-24 | 中国科学院合肥物质科学研究院 | Copper oxide grading array film and preparation method thereof |
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| CN104535532A (en) * | 2014-12-24 | 2015-04-22 | 宁波工程学院 | Metal micro-/nano-sensing device |
| CN105004698A (en) * | 2015-06-09 | 2015-10-28 | 安徽师范大学 | Novel surface plasmon resonance biosensor |
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| CN103833031B (en) * | 2014-02-28 | 2016-04-13 | 游学秋 | Three-dimensional communication bends Graphene and preparation method thereof, electrode, electric capacity and lithium cell |
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