CN105084307A - Preparation method of metal nanostructure with adjustable resonance peak positions - Google Patents
Preparation method of metal nanostructure with adjustable resonance peak positions Download PDFInfo
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Abstract
Provided is a preparation method of a metal nanostructure with adjustable resonance peak positions. The method comprises following steps: firstly, uniformly dispersing a PS nanosphere solution for pre-assembly on a water surface in order to form PS nanosphere single-layer films; secondly, transferring the PS nanosphere single-layer films to the surface of a sample subjected to hydrophilic treatment; thirdly, depositing metal to the surface of the sample; and fourthly, removing PS nanospheres on the surface of the sample in order to obtain the metal nanostructure with adjustable resonance peak positions. The preparation method of the metal nanostructure with adjustable resonance peak positions has following beneficial effects: thickness of metal can be precisely controlled; the size of the metal nanostructure can be accurately controlled; concrete metal materials for disposition can be selected according to needs so that resonance peak positions of the metal nanostructure can be adjusted in order to be suitable for the requirement for different resonance peak positions in different applications; by adoption of the method, preparation temperature is low so as to avoid negative influence of high-temperature equipment on optoelectronic devices; the preparation process is simplified; solution pollution is reduced; and cleanliness of the surface of the sample is maintained so that performance of the optoelectronic devices is enhanced.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, be specifically related to the preparation method of the adjustable metal Nano structure of a kind of resonance peak.
Background technology
At present, because metal micro-nanostructure has good electrical and optical properties, it is made to have huge potential using value in fields such as optoelectronic areas (as solar cell, light emitting diode etc.), sensor (such as biology sensor etc.) and clinical medicine.Research shows, under the stimulation of additional light field, be in its being eager to excel at free space of fluorescence intensity ratio that the fluorophor near metal Nano structure gives off, this phenomenon is surface plasma bulk effect (LocalizedSurfacePlasmon, LSP), now one of noticeable research field has been become.
At present, the method for the preparation of metal micro-nanostructure has annealing, chemical synthesis etc.The metal being usually used in preparing micro-nano structure has nickel (Ni), silver (Ag), gold (Au) etc., the micro-nano structure annealing temperature of these preparation of metals is higher, if Ni is 800 DEG C ~ 900 DEG C (MaterialsScienceandEngineeringB113,125 – 129 (2004)), Ag and Au is 300 DEG C ~ 600 DEG C (JournalofCrystalGrowth310,234 – 239 (2008)).Higher annealing temperature brings negative impact can to the performance of photoelectric device and organic electro-optic device, such as high temperature can damage semiconductor light-emitting-diode (LightEmittingDiode, hereinafter referred to as LED) epitaxial structure, reduce its lattice quality, the annealing of more than 200 DEG C can improve organic conductive layers (PET film, ITO layer etc.) sheet resistance, and then reduce electricity and the optical property (CurrentAppliedPhysics14,1005 (2014)) of photoelectric device.So the low-temperature growth of metal micro-nanostructure has great importance for the optics and electric property improving photoelectric device and organic electro-optic device.
Also some metal Nano structures are had to be synthesized (Appl.Phys.Lett.100,013308 (2012)) by chemical solution.But the metal nanoparticle of synthesis like this needs heating, drying to remove solution, and this may bring pollution, and the metal nanoparticle arrangement of chemical synthesis is unordered, affects surface plasma bulk effect.
(as solar cell in the practical application of metal Nano structure, inorganic and Organic Light Emitting Diode etc.), need the resonance peak of metal Nano structure at a specific wave band, just can reach best surface plasma bulk effect, so in specific applications, need to regulate the resonance peak of corresponding metal Nano structure.Such as, Au nanostructured is applied to green glow Organic Light Emitting Diode (OrganicLED, OLED) time in, the resonance peak of Au nanostructured is needed to be adjusted within the scope of 500nm ~ 550nm, just can there is the LSP resonance enhancement that stronger, thus one is reached to raising OLED luminous efficiency strengthen effect (OpticsLetters37,2019 (2012)) preferably.But up to now, how low cost and the resonance peak of easy adjustment metal Nano structure is still a difficult problem.Adopt electron beam lithography and nanometer embossing can prepare the nanometer metal structure with different resonance peak, but still there is equipment price costliness in said method, the defects such as complicated operation.On the other hand, people attempt preparing nanometer metal structure (CN102212790A, 2011 with polystyrene (polystyrene, PS) nanosphere; CN104087899A, 2014), although preparation method's cost of report is low and easy and simple to handle, for some specific resonance crests, can only can not regulate resonant wavelength, there is certain limitation.
Document in the past and patent relate to mainly by annealing, the method such as nano impression, electron beam lithography and chemical synthesis prepares metal Nano structure, the resonance peak of the metal Nano structure prepared is fixed, not easily regulate, do not relate to the research of the metal Nano structure that low-temperature growth resonance peak is adjustable below 200 DEG C.
Summary of the invention
The preparation method of the metal Nano structure that the object of the present invention is to provide a kind of resonance peak adjustable, high annealing can be reduced to the negative effect prepared opto-electronic device and bring, and can preparation flow be simplified, reduce contaminated aqueous solution, keep the cleanliness factor of sample surfaces.
For reaching above object, the present invention takes following technical scheme to be achieved:
A preparation method for the metal Nano structure that resonance peak is adjustable, comprises the following steps:
A) hydrophily process is carried out to sample surfaces;
B) homodisperse PS nanosphere solution is prepared:
Be 1:(1 ~ 10 by volume by PS nanosphere dispersion liquid and absolute ethyl alcohol) mixing, ultrasonic disperse is even, obtains homodisperse PS nanosphere solution; Wherein the diameter of PS nanosphere is the mass fraction of PS nanosphere in 50nm ~ 1000nm, PS nanosphere dispersion liquid is 5% ~ 20%;
C) pre-assembled at the water surface of PS nanosphere:
Homodisperse PS nanosphere solution is added drop-wise on the Si sheet after hydrophily process, being stretched into the angle of inclination of 10 ~ 45 ° by this silicon chip fills in the container of deionized water again, PS nanosphere slips in deionized water, at the water surface pre-assembled formation PS nanosphere monofilm; The pass being wherein added drop-wise to the surface area S of deionized water in the volume V of the PS nanosphere solution on Si sheet and container is V/S=0.5 ~ 5 μ L/cm
2;
D) PS nanosphere monofilm is transferred to sample surfaces a) processed through step, obtains at sample surfaces the PS nanosphere structure that individual layer independently fills;
E) by the mode of electron beam evaporation, thermal evaporation or magnetron sputtering at the sample surfaces plated metal with the PS nanosphere structure that individual layer independently fills, the gross thickness of the metal of deposition is less than the radius of PS nanosphere in PS nanosphere structure;
F) the PS nanosphere structure of the sample surfaces after plated metal is removed, namely obtain the adjustable metal Nano structure of resonance peak at sample surfaces.
Concrete operations a) of described step are: sample is placed in ozone environment, with Ultraviolet radiation 1 ~ 30min; Or sample being placed in volume ratio is the concentrated sulfuric acid of 3:1 and the mixed solution of hydrogen peroxide, at 100 ~ 150 DEG C, soak 30 ~ 120min.
Described step a) in sample be Si sheet, sapphire, ITO layer, GaN layer or glass.
Described step c) in until PS nanosphere after water surface pre-assembled formation PS nanosphere monofilm, sodium dodecyl sulfate solution is injected at container edge, wherein the concentration of sodium dodecyl sulfate solution is 0.1 ~ 10g/L, the volume V of the sodium dodecyl sulfate solution of injection
1be V with the pass of the surface area S of deionized water in container
1/ S=0.01 ~ 0.1 μ L/cm
2.
Described steps d) concrete operations be: the sample that a) will process through step with the angle of inclination of 10 ~ 45 ° along step c) container edge insert in deionized water, when this sample immerses below PS nanosphere monofilm completely, upwards lift this sample, PS nanosphere monofilm is picked up, leave standstill sample until the moisture on PS nanosphere monofilm dries naturally, namely obtain at sample surfaces the PS nanosphere structure that individual layer independently fills.
Described step e) carry out before, first the size of the PS nanosphere in the PS nanosphere structure of sample surfaces is regulated and controled, namely the diameter of PS nanosphere is increased by the mode of heating using microwave or flat heater, or by the oxygen etching PS nanosphere of inductively coupled plasma etching machine, to reduce the diameter of PS nanosphere.
When increasing the diameter of PS nanosphere by the mode of flat heater, the heat time is 5 ~ 60s, and heating-up temperature is 80 ~ 150 DEG C;
When increasing the diameter of PS nanosphere by the mode of heating using microwave, the heat time is 5 ~ 200s, and heating-up temperature is 70 ~ 100 DEG C;
When reducing the diameter of PS nanosphere with inductively coupled plasma etching machine, etching power is 30 ~ 300W, and etch period is 0.5 ~ 10min, and pressure during etching is 0.5 ~ 5Pa.
When after the diameter increasing PS nanosphere, step e) in the gross thickness of metal of deposition be less than the original radius of PS nanosphere;
When after the diameter reducing PS nanosphere, step e) in the gross thickness of metal of deposition be less than the radius of the PS nanosphere after reduction.
Described step e) in deposition metal be simple metal, metallic compound and/or alloy, wherein simple metal is the mixture of one or more arbitrary proportions in aluminium, silver, gold, titanium, nickel, platinum, copper, and metallic compound is CdS, MgO, MgF
2in the mixture of one or more arbitrary proportions, alloy is Au/Sn alloy;
During plated metal, deposit various metals respectively, form multiple metal level, in each metal level, comprise one or more metals; Or deposit various metals simultaneously, form an overall metal mixed layer.
Described step f) in remove PS nanosphere structure concrete operations be: the sample after plated metal is soaked 1 ~ 10min in chloroform, and cleans with ultrasonic wave added, use acetone, ethanol or deionized water rinsing afterwards, finally with Ar gas or N
2air-blowing is done.
Relative to prior art, beneficial effect of the present invention is as follows:
The preparation method of the metal Nano structure that resonance peak provided by the invention is adjustable, at the water surface pre-assembled formation PS nanosphere monofilm after first making PS nanosphere Solution Dispersion evenly, then PS nanosphere monofilm is transferred to the sample surfaces through hydrophily process, the PS nanosphere structure that individual layer independently fills is obtained at sample surfaces, again at the sample surfaces plated metal with the PS nanosphere structure that individual layer independently fills, finally remove the PS nanosphere structure of sample surfaces, namely obtain the adjustable metal Nano structure of resonance peak at sample surfaces.The thickness of the metal that the present invention is deposited by the mode of electron beam evaporation, thermal evaporation, magnetron sputtering can accurately control, therefore, it is possible to accurately control the size of metal Nano structure, and the method can select the concrete metal material deposited as required, thus make the resonance peak of metal Nano structure adjustable, the requirement to different metal nanostructured resonance peak in different application can be adapted to.The preparation temperature of the method is lower, the preparation temperature of metal Nano structure can be reduced to less than 200 DEG C, not only reduce the requirement to equipment, and avoid high temperature and prepare the negative effect that opto-electronic device is brought, as reduced the damage to extension lattice quality, reduce the impact on conductive layer, and can preparation flow be simplified, reduce contaminated aqueous solution, in preparation process, do not introduce other impurity, the cleanliness factor of sample surfaces can be kept, thus the performance of opto-electronic device is promoted further.
Further, the mode etched by heating using microwave, flat heater or inductively coupled plasma etching machine (ICP) in the present invention can the size of accurate control PS nanosphere, by the amplitude that time and the temperature control PS nanosphere diameter of heating increase, the amplitude that the parameter control PS nanosphere diameters such as the power etched by ICP, time, pressure are reduced, make the lateral dimension of the metal Nano structure obtained for mask with this PS ball can be precisely controlled, thus reach the object regulating metal Nano structure resonance peak.And in the process of plated metal, by difference deposit multilayer not same metal, and the resonance peak that various metals regulates metal Nano structure can be deposited, to adapt to the requirement to different metal nanostructured resonance peak in different application simultaneously.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the PS nanosphere structure that independently fills of individual layer prepared by the embodiment of the present invention 1, and wherein (a) be the SEM figure not have the PS nanosphere heated, and (b) is that the SEM of PS nanosphere after heating schemes.
Fig. 2 is the abosrption spectrogram of metal Nano structure prepared by the embodiment of the present invention 1.
Fig. 3 is the abosrption spectrogram of metal Nano structure prepared by the embodiment of the present invention 2.
Fig. 4 is the abosrption spectrogram of metal Nano structure prepared by the embodiment of the present invention 3.
Fig. 5 is that the current efficiency with the OLED of different metal nanostructured prepared of the embodiment of the present invention 4 and efficiency attenuation coefficient are relative to the distribution map of electric current.
Fig. 6 is the simple and easy schematic diagram with the thin-film solar cells of metal Nano structure prepared by the embodiment of the present invention 5, and wherein 1 is back electrode, and 2 is silicon thin film, and 3 is ITO layer, and 4 is metal Nano structure.
Fig. 7 is the SEM figure of the PS nanosphere structure that the individual layer of the embodiment of the present invention 6 preparation independently fills, and wherein (a) is the SEM figure of the PS nanosphere do not etched, and (b) is the SEM figure of the PS nanosphere after ICP etching.
Detailed description of the invention
Below in conjunction with accompanying drawing, by specific embodiment, the present invention is further described.
The preparation method of the metal Nano structure that resonance peak provided by the invention is adjustable, its major advantage is: the size of (1) metal Nano structure can accurately control, accurately controlled the longitudinal size (thickness) of metal Nano structure by modes such as electron beam evaporation, thermal evaporation, magnetron sputterings, the mode simultaneously etched by heating or ICP accurately controls the lateral dimension of metal Nano structure; (2) resonance peak of metal Nano structure is adjustable, the method can by controlling the size of nanometer metal structure, also can alternating deposit multilayer not same metal, and deposit different metal simultaneously, make alloying metal layer, thus make this preparation method have very strong adaptability and practicality, the opto-electronic device of variety classes, different wave length can be applied to.In actual applications, regulate metal Nano structure resonance peak that surface plasmon resonance effect can be made to reach optimum efficiency flexibly.(3) preparation temperature of the present invention is low, not only reduces the requirement to equipment, and avoids the negative effect that high temperature brings opto-electronic device performance.(4) the method preparation process is simple, does not introduce other impurity, can keep the cleanliness factor of sample, be conducive to the electricity and the optical property that improve opto-electronic device further in preparation process.
Embodiment 1:
A) the hydrophily process of sample surfaces.Glass sample is placed in ozone environment, and uses Ultraviolet radiation 5min.
B) homodisperse PS nanosphere solution is prepared.Measure PS nanosphere dispersion liquid (mass fraction is the diameter of 10%, PS nanosphere is 200nm) with micropipettor and ethanol solution is placed in small beaker, the volume ratio of the two is 1:2.Ultrasonic for this solution 10min is uniformly dispersed, obtains homodisperse PS nanosphere solution.
C) pre-assembled at water surface of PS nanosphere.Prepare the culture dish (surface area of water is S) that fills with deionized water, measure with micropipettor homodisperse PS nanosphere solution (the V/S=1 μ L/cm that volume is V
2), be distributed on the Si sheet after hydrophily process, then this Si sheet is stretched in deionized water with the inclination angle of 20 °, PS nanosphere can be observed and slip into water surface, form one deck glossiness PS nanosphere monofilm at water surface gradually.Be V at culture dish edge injected slurry volume
1sodium dodecyl sulfate solution (concentration is 1g/L, V
1/ S=0.05 μ L/cm
2), PS nanosphere monofilm is arranged and more compacts with complete.
D) PS nanosphere monofilm is transferred to sample surfaces.Get the glass sample that a slice a) processes through step, insert gently in deionized water along culture dish edge with the angle of inclination of 20 °, when this sample immerses below PS nanosphere monofilm completely, slowly lift this sample, PS nanosphere monofilm is picked up, leave standstill sample until moisture dries naturally, the PS nanosphere structure (as Suo Shi Fig. 1 (a)) that individual layer independently fills can be obtained on glass sample surface.
E) size of PS nanosphere controls.Adopting the mode of flat heater, by flat heater to 130 DEG C, then by steps d) glass sample that obtains is placed on flat board and heats 10s, obtains the PS nanosphere structure (as Suo Shi Fig. 1 (b)) increased.
F) deposition of metal.By the mode (chamber pressure: 1 × 10 of thermal evaporation
-3pa, speed: 0.05nm/s) respectively in steps d) and step e) deposit thickness is the metal A g of 15nm on the glass sample that obtains.
G) PS nanosphere is removed.Glass sample after two kinds of plated metals is soaked 3min in chloroform, and cleans 5min with ultrasonic wave added, then clean by deionized water, and use N
2air-blowing is done, and namely obtains two kinds of metal Nano structures on two kinds of glass sample surfaces.
Fig. 1 is the SEM figure of the PS nanosphere structure that independently fills of individual layer prepared by the embodiment of the present invention 1, and wherein (a) be the SEM figure not have the PS nanosphere heated, and (b) is that the SEM of PS nanosphere after heating schemes.As can be seen from Figure 1 the PS nanosphere structure that individual layer independently fills is formed by some PS nanosphere close-packed arrays of uniform size, its compound with regular structure, densification, and the space after heating between PS nanosphere obviously diminishes.
The two kind metal Nano structures obtained to embodiment 1 carry out absorption spectra measurement, scanning wavelength is 300 ~ 800nm, the results are shown in Figure 2, wherein sample A is in steps d in embodiment 1) metal Nano structure that obtains after plated metal removes PS nanosphere again on the glass sample that obtains, sample B is in step e in embodiment 1) absorption spectrum of metal Nano structure that obtains after plated metal removes PS nanosphere again on the glass sample that obtains.As seen from Figure 2, through step e) the absorption resonance peak position of metal Nano structure that obtains after heating had obvious movement.
Embodiment 2:
A) the hydrophily process of sample surfaces.Glass sample is placed in ozone environment, and uses Ultraviolet radiation 5min.
B) homodisperse PS nanosphere solution is prepared.Measure PS nanosphere (diameter 200nm) dispersion liquid (mass fraction 10%) with micropipettor and ethanol solution is placed in small beaker, the volume ratio of the two is 1:1.By ultrasonic for this solution 5min, obtain homodisperse PS nanosphere solution.
C) pre-assembled at water surface of PS nanosphere.Prepare the culture dish (surface area of water is S) that fills with deionized water, measure with micropipettor homodisperse PS nanosphere solution (the V/S=2 μ L/cm that volume is V
2), be distributed on the Si sheet after hydrophily process, this Si sheet is stretched in deionized water with the inclination angle of 30 °, PS nanosphere can be observed and slip into water surface, form one deck glossiness PS nanosphere monofilm at water surface gradually.Be V at culture dish edge injected slurry volume
1sodium dodecyl sulfate solution (concentration is 2g/L, V
1/ S=0.01 μ L/cm
2), PS nanosphere monofilm is arranged and more compacts with complete.
D) PS nanosphere monofilm is transferred to sample surfaces.Get the glass sample of a slice through hydrophily process, insert gently in deionized water along culture dish edge with the angle of inclination of 10 °, when this sample immerses below PS nanosphere monofilm completely, slowly lift this sample, PS nanosphere monofilm is picked up, leave standstill sample until moisture dries naturally, the PS nanosphere structure that individual layer independently fills can be obtained on glass sample surface.
E) deposition of metal.First glass sample adopts the mode deposit thickness of thermal evaporation to be the metal A g of 15nm, second glass sample adopts the mode deposit thickness of electron beam evaporation to be the metal A u of 15nm, 3rd the first deposit thickness of glass sample is the metal A g of 7.5nm, deposit thickness is the metal A u of 7.5nm again, 4th glass sample evaporation metal Ag and metal A u simultaneously, thickness is 15nm (being designated as " 15nmAu/Ag "), and two kinds of metals evaporation rate is separately suitable.
F) PS nanosphere is removed.Four samples are soaked 3min in chloroform respectively, and cleans 5min with ultrasonic wave added, then clean by deionized water, and use N
2air-blowing is done, and namely obtains four kinds of metal Nano structures on four kinds of glass sample surfaces.
The four kind metal Nano structures obtained to embodiment 2 carry out absorption spectra measurement, scanning wavelength is 300 ~ 700nm, the results are shown in Figure 3, wherein sample C, D, E, F is respectively the metal Nano structure that plated metal obtains after removing PS nanosphere again on first, second, third and fourth glass sample.As seen from Figure 3, the absorption spectrum of different metal nanostructured is different.
Embodiment 3:
A) the hydrophily process of sample surfaces.Glass sample is placed in ozone environment, and uses Ultraviolet radiation 10min.
B) homodisperse PS nanosphere solution is prepared.Measure PS nanosphere (diameter 200nm) dispersion liquid (mass fraction 10%) with micropipettor and ethanol solution is placed in small beaker, the volume ratio of the two is 1:3.By ultrasonic for this solution 15min, obtain homodisperse PS nanosphere solution.
C) pre-assembled at water surface of PS nanosphere.Prepare the culture dish (surface area of water is S) that fills with deionized water, measure with micropipettor homodisperse PS nanosphere solution (the V/S=3 μ L/cm that volume is V
2), be distributed on the Si sheet after hydrophily process, this Si sheet is stretched in deionized water with the inclination angle of 30 °, PS nanosphere can be observed and slip into water surface, form one deck glossiness PS nanosphere monofilm at water surface gradually.Be V at culture dish edge injected slurry volume
1sodium dodecyl sulfate solution (concentration is 1g/L, V
1/ S=0.1 μ L/cm
2), PS nanosphere monofilm is arranged and more compacts with complete.
D) PS nanosphere monofilm is transferred to sample surfaces.Get the glass sample of a slice through hydrophily process, insert gently in deionized water along culture dish edge with the angle of inclination of 30 °, when this sample immerses below PS nanosphere monofilm completely, slowly lift this sample, PS nanosphere monofilm is picked up, leave standstill sample until moisture dries naturally, the PS nanosphere structure that individual layer independently fills can be obtained on glass sample surface.
E) deposition of metal.First glass sample adopts the mode (chamber pressure: 1 × 10 of electron beam evaporation
-4pa, speed: 0.03nm/s) deposit the metal A u of 15nm, second glass sample adopts the mode (chamber pressure: 1 × 10 of thermal evaporation
-4pa, speed: 0.08nm/s) deposit the metal A u/Sn alloy of 15nm.
F) PS nanosphere is removed.Two kinds of samples are soaked 3min in chloroform respectively, and cleans 5min with ultrasonic wave added, then clean by deionized water, and use N
2air-blowing is done, and namely obtains two kinds of metal Nano structures on two kinds of glass sample surfaces.
The two kind metal Nano structures obtained to embodiment 3 carry out absorption spectra measurement, and scanning wavelength is 300 ~ 700nm, the results are shown in Figure 4.As seen from Figure 4, the absorption spectrum of different metal nanostructured is different.
Embodiment 4: different metal nanostructured is applied to Organic Light Emitting Diode (OLED), produces surface phasmon effect (Surfaceplasma, SP), improves device optical performance.
A) the hydrophily process of sample surfaces.Be that the glass sample of ITO layer is placed in ozone environment by surface, and use Ultraviolet radiation 5min.
B) homodisperse PS nanosphere solution is prepared.Measure PS nanosphere (diameter 200nm) dispersion liquid (mass fraction 10%) with micropipettor and ethanol solution is placed in small beaker, the volume ratio of the two is 1:2.By ultrasonic for this solution 10min, obtain homodisperse PS nanosphere solution.
C) pre-assembled at water surface of PS nanosphere.Prepare the culture dish (surface area of water is S) that fills with deionized water, measure with micropipettor homodisperse PS nanosphere solution (the V/S=1 μ L/cm that volume is V
2), be distributed on the Si sheet after hydrophily process, this Si sheet is stretched in deionized water with the inclination angle of 20 °, PS nanosphere can be observed and slip into water surface, form one deck glossiness PS nanosphere monofilm at water surface gradually.Be V at culture dish edge injected slurry volume
1sodium dodecyl sulfate solution (concentration is 3g/L, V
1/ S=0.05 μ L/cm
2), PS nanosphere monofilm is arranged and more compacts with complete.
D) PS nanosphere monofilm is transferred to sample surfaces.Get the glass sample that a slice is ITO layer through the surface of step a) hydrophily process, insert gently in deionized water along culture dish edge with the angle of inclination of 20 °, when this sample immerses below PS nanosphere monofilm completely, slowly lift this sample, PS nanosphere monofilm is picked up, leave standstill sample until moisture evaporate to dryness, can obtain at sample surfaces the PS nanosphere structure that individual layer independently fills.
E) size of PS nanosphere controls.Adopting the mode of flat heater, by flat heater to 150 DEG C, and by steps d) glass sample (being labeled as " sample 4 ") that obtains is placed on hot plate and heats 5s, obtains the PS nanosphere structure increased.
F) deposition of metal.A steps d) not plated metal on the glass sample that obtains, a steps d) glass sample that obtains deposits the Au of 15nm, a steps d) glass sample that obtains deposits the Au/Sn alloy of 15nm, at a step e) glass sample that obtains deposits the Au/Sn alloy of 15nm.
G) PS nanosphere is removed.Four kinds of samples are soaked 3min in chloroform respectively, and cleans 5min with ultrasonic wave added, then clean by deionized water, and use N
2air-blowing is done, and namely obtains three kinds of metal Nano structures (not having metal Nano structure on non-plated metal sample) on four kinds of glass sample surfaces.
H) preparation of OLED.Four samples are completed under same technique the preparation of OLED, that luminescent material is chosen is Alq
3, the distance of the bottom of the distance luminous zone, top of metal Nano structure is 15nm.
Four obtained OLED are carried out to the measurement of current efficiency, the results are shown in Figure 5, wherein sample 1 is in steps d) the sample that do not obtain after directly removing PS nanosphere of plated metal is obtained on the glass sample that obtains OLED, sample 2 is in steps d) glass sample that obtains deposits the Au of 15nm after remove PS nanosphere again after the obtained OLED of the sample that obtains, sample 3 is in steps d) glass sample that obtains deposits the Au/Sn alloy of 15nm after remove PS nanosphere again after the obtained OLED of the sample that obtains, sample 4 is in step e) glass sample that obtains deposits the Au/Sn alloy of 15nm after remove PS nanosphere again after the obtained OLED of the sample that obtains.As can be seen from Fig. 5, there is OLED (>800mA/cm under big current of different metal nanostructured
2), current efficiency has raising in various degree, and its efficiency attenuation coefficient also has reduction in various degree.
Embodiment 5: different metal nanostructured is applied to thin-film solar cells, improves its photoelectric transformation efficiency.
A) prepare thin-film solar cells silicon film sample used, adulterated formation p-n junction, and prepare back electrode.
B) at N-shaped silicon side upper surface deposit (using physical vapor deposition technology) ITO as surface transparent electrode, its thickness is 5-100nm.
C) the hydrophily process of sample surfaces.The glass sample on ITO surface is placed in ozone environment, and uses Ultraviolet radiation 30min.
D) homodisperse PS nanosphere solution is prepared.Measure PS nanosphere (diameter 500nm) dispersion liquid (mass fraction 20%) with micropipettor and ethanol solution is placed in small beaker, the volume ratio of the two is 1:10.By ultrasonic for this solution 30min, obtain homodisperse PS nanosphere solution.
E) pre-assembled at water surface of PS nanosphere.Prepare the culture dish (surface area of water is S) that fills with deionized water, measure with micropipettor homodisperse PS nanosphere solution (the V/S=5 μ L/cm that volume is V
2), be distributed on the Si sheet after hydrophily process, this Si sheet is stretched in deionized water with the inclination angle of 45 °, PS nanosphere can be observed and slip into water surface, form one deck glossiness PS nanosphere monofilm at water surface gradually.
F) PS nanosphere monofilm is transferred to sample surfaces.Get a slice through step c) surface that processes is the glass sample of ITO conductive layer, insert gently in deionized water along culture dish edge with the angle of inclination of 45 °, when this sample immerses below PS nanosphere monofilm completely, slowly lift this sample, PS nanosphere monofilm is picked up, leave standstill sample until moisture evaporate to dryness, can obtain at sample surfaces the PS nanosphere structure that individual layer independently fills.
G) deposition of metal.Adopt mode (radio-frequency power 300W, the base vacuum 1 × 10 of magnetron sputtering
-5pa, reaction pressure 0.5Pa) first deposit the Ag of one deck 3nm, then deposit the Al of one deck 3nm, then deposit the Au of one deck 3nm.
H) PS nanosphere is removed.Sample is soaked 10min in chloroform, and clean 10min with ultrasonic wave added, then clean by deionized water, and use N
2air-blowing is done.
I) preparation technology of follow-up solar cell device is completed.The obtained schematic diagram with the thin-film solar cells of metal Nano structure as shown in Figure 6.
Embodiment 6:
A) the hydrophily process of sample surfaces.GaN sample is placed in ozone environment, and uses Ultraviolet radiation 5min.
B) homodisperse PS nanosphere solution is prepared.Measure PS nanosphere dispersion liquid (mass fraction is the diameter of 10%, PS nanosphere is 200nm) with micropipettor and ethanol solution is placed in small beaker, the volume ratio of the two is 1:2.Ultrasonic for this solution 10min is uniformly dispersed, obtains homodisperse PS nanosphere solution.
C) pre-assembled at water surface of PS nanosphere.Prepare the culture dish (surface area of water is S) that fills with deionized water, measure with micropipettor homodisperse PS nanosphere solution (the V/S=1 μ L/cm that volume is V
2), be distributed on the Si sheet after hydrophily process, then this Si sheet is stretched in deionized water with the inclination angle of 20 °, PS nanosphere can be observed and slip into water surface, form one deck glossiness PS nanosphere monofilm at water surface gradually.Be V at culture dish edge injected slurry volume
1sodium dodecyl sulfate solution (concentration is 1g/L, V
1/ S=0.05 μ L/cm
2), PS nanosphere monofilm is arranged and more compacts with complete.
D) PS nanosphere monofilm is transferred to sample surfaces.Get the sample that a slice a) processes through step, insert gently in deionized water along culture dish edge with the angle of inclination of 20 °, when this sample immerses below PS nanosphere monofilm completely, slowly lift this sample, PS nanosphere monofilm is picked up, leave standstill sample until moisture dries naturally, can obtain at sample surfaces the PS nanosphere structure (as Suo Shi Fig. 7 (a)) that individual layer independently fills.
E) size of PS nanosphere controls.Adopt inductively coupled plasma etching machine (ICP), at radio-frequency power 300W, base vacuum 1 × 10
-4under the etching condition of Pa, reaction pressure 0.5Pa, logical oxygen (O
2) etching 30s, thus reduce the diameter (as Suo Shi Fig. 7 (b)) of PS nanosphere.
F) deposition of metal.By the mode (chamber pressure: 1 × 10 of thermal evaporation
-3pa, speed: 0.05nm/s) respectively in steps d) and step e) deposit thickness is the metal A g of 15nm on the sample that obtains.
G) PS nanosphere is removed.GaN sample after two kinds of plated metals is soaked 3min in chloroform, and cleans 5min with ultrasonic wave added, then clean by deionized water, and use N
2air-blowing is done, and namely obtains two kinds of metal Nano structures at two kinds of sample surfaces.
Fig. 7 is the SEM figure of the PS nanosphere structure that independently fills of individual layer prepared by the embodiment of the present invention 6, and wherein (a) be the SEM figure not have the PS nanosphere etched, and (b) is that the SEM of PS nanosphere after etching schemes.As can be seen from Figure 7 the PS nanosphere structure that individual layer independently fills is formed by some PS nanosphere close-packed arrays of uniform size, and its compound with regular structure, densification, the space after etching processing between PS nanosphere obviously becomes large.
Embodiment 7:
A) the hydrophily process of sample surfaces.Si sheet is placed in dense H
2sO
4with H
2o
2volume ratio be in the mixed solution of 3:1, at 150 DEG C, soak 30min.
B) homodisperse PS nanosphere solution is prepared.Measure PS nanosphere dispersion liquid (mass fraction is the diameter of 10%, PS nanosphere is 50nm) with micropipettor and ethanol solution is placed in small beaker, the volume ratio of the two is 1:2.Ultrasonic for this solution 10min is uniformly dispersed, obtains homodisperse PS nanosphere solution.
C) pre-assembled at water surface of PS nanosphere.Prepare the culture dish (surface area of water is S) that fills with deionized water, measure with micropipettor homodisperse PS nanosphere solution (the V/S=5 μ L/cm that volume is V
2), be distributed on the Si sheet after hydrophily process, this Si sheet is stretched in deionized water with the inclination angle of 10 °, PS nanosphere can be observed and slip into water surface, form one deck glossiness PS nanosphere monofilm at water surface gradually.Be V at culture dish edge injected slurry volume
1sodium dodecyl sulfate solution (concentration is 10g/L, V
1/ S=0.05 μ L/cm
2), PS nanosphere monofilm is arranged and more compacts with complete.
D) PS nanosphere monofilm is transferred to sample surfaces.Separately get the Si sheet that a slice a) processes through step, insert gently in deionized water along culture dish edge with the angle of inclination of 10 °, when this sample immerses below PS nanosphere monofilm completely, slowly lift this sample, PS nanosphere monofilm is picked up, leave standstill sample until moisture dries naturally, can obtain at sample surfaces the PS nanosphere structure that individual layer independently fills.
E) size of PS nanosphere controls.Increase the diameter of PS nanosphere by the mode of heating using microwave, the heat time is 5s, and heating-up temperature is 100 DEG C, obtains the PS nanosphere structure increased;
F) deposition of metal.Adopt mode (radio-frequency power 400W, the base vacuum 1 × 10 of magnetron sputtering
-5pa, reaction pressure 0.5Pa) in step e) sample that obtains deposits CdS, MgO and MgF successively
2, every layer thickness is 5nm.
G) PS nanosphere is removed.Sample is soaked 1min in chloroform, and clean 5min with ultrasonic wave added, then clean with ethanol, and do with Ar air-blowing, namely obtain metal Nano structure at sample surfaces.
Embodiment 8:
A) the hydrophily process of sample surfaces.Be that the sample of GaN layer is placed in dense H by upper surface
2sO
4with H
2o
2volume ratio be in the mixed solution of 3:1, at 100 DEG C, soak 120min.
B) homodisperse PS nanosphere solution is prepared.Measure PS nanosphere dispersion liquid (mass fraction is the diameter of 10%, PS nanosphere is 600nm) with micropipettor and ethanol solution is placed in small beaker, the volume ratio of the two is 1:2.Ultrasonic for this solution 10min is uniformly dispersed, obtains homodisperse PS nanosphere solution.
C) pre-assembled at water surface of PS nanosphere.Prepare the culture dish (surface area of water is S) that fills with deionized water, measure with micropipettor homodisperse PS nanosphere solution (the V/S=4 μ L/cm that volume is V
2), be distributed on the Si sheet after hydrophily process, this Si sheet is stretched in deionized water with the inclination angle of 25 °, PS nanosphere can be observed and slip into water surface, form one deck glossiness PS nanosphere monofilm at water surface gradually.Be V at culture dish edge injected slurry volume
1sodium dodecyl sulfate solution (concentration is 5g/L, V
1/ S=0.08 μ L/cm
2).
D) PS nanosphere monofilm is transferred to sample surfaces.Get the sample that a slice a) processes through step, insert gently in deionized water along culture dish edge with the angle of inclination of 25 °, when this sample immerses below PS nanosphere monofilm completely, slowly lift this sample, PS nanosphere monofilm is picked up, leave standstill sample until moisture dries naturally, can obtain at sample surfaces the PS nanosphere structure that individual layer independently fills.
E) size of PS nanosphere controls.Increase the diameter of PS nanosphere by the mode of heating using microwave, the heat time is 200s, and heated solution temperature is 70 DEG C, obtains the PS nanosphere structure increased;
F) deposition of metal.Adopt mode (radio-frequency power 500W, the base vacuum 1 × 10 of magnetron sputtering
-5pa, reaction pressure 2Pa) in step e) sample surfaces that obtains depositing Ti and MgO simultaneously, form the hybrid metal layer that thickness is 20nm.
G) PS nanosphere is removed.Sample is soaked 5min in chloroform, and clean 10min with ultrasonic wave added, then clean with acetone, and do with Ar air-blowing, namely obtain metal Nano structure at sample surfaces.
Embodiment 9:
A) the hydrophily process of sample surfaces.Sapphire samples is placed in ozone environment, and uses Ultraviolet radiation 1min.
B) homodisperse PS nanosphere solution is prepared.Measure PS nanosphere dispersion liquid (mass fraction is the diameter of 5%, PS nanosphere is 1000nm) with micropipettor and ethanol solution is placed in small beaker, the volume ratio of the two is 1:5.Ultrasonic for this solution 10min is uniformly dispersed, obtains homodisperse PS nanosphere solution.
C) pre-assembled at water surface of PS nanosphere.Prepare the culture dish (surface area of water is S) that fills with deionized water, measure with micropipettor homodisperse PS nanosphere solution (the V/S=0.5 μ L/cm that volume is V
2), be distributed on the Si sheet after hydrophily process, then this Si sheet is stretched in deionized water with the inclination angle of 35 °, PS nanosphere can be observed and slip into water surface, form one deck glossiness PS nanosphere monofilm at water surface gradually.Be V at culture dish edge injected slurry volume
1sodium dodecyl sulfate solution (concentration is 0.1g/L, V
1/ S=0.03 μ L/cm
2), PS nanosphere monofilm is arranged and more compacts with complete.
D) PS nanosphere monofilm is transferred to sample surfaces.Get the sapphire samples that a slice a) processes through step, insert gently in deionized water along culture dish edge with the angle of inclination of 35 °, when this sample immerses below PS nanosphere monofilm completely, slowly lift this sample, PS nanosphere monofilm is picked up, leave standstill sample until moisture dries naturally, the PS nanosphere structure that individual layer independently fills can be obtained on sapphire samples surface.
E) size of PS nanosphere controls.Adopting the mode of flat heater, by flat heater to 80 DEG C, then by steps d) sapphire samples that obtains is placed on flat board and heats 60s, obtains the PS nanosphere structure increased.
F) deposition of metal.By the mode (chamber pressure: 1 × 10 of electron beam evaporation
-4pa, speed: 0.05nm/s) successively in step e) deposit thickness is the Cu of Pt and 5nm of Ni, 5nm of 5nm in the sapphire samples that obtains.
G) PS nanosphere is removed.Sapphire samples after plated metal is soaked 8min in chloroform, and cleans 5min with ultrasonic wave added, then clean by deionized water, and use N
2air-blowing is done, and namely obtains metal Nano structure on sapphire samples surface.
Embodiment 10:
A) the hydrophily process of sample surfaces.Si sheet is placed in dense H
2sO
4with H
2o
2volume ratio be in the mixed solution of 3:1, at 120 DEG C, soak 80min.
B) homodisperse PS nanosphere solution is prepared.Measure PS nanosphere dispersion liquid (mass fraction is the diameter of 15%, PS nanosphere is 100nm) with micropipettor and ethanol solution is placed in small beaker, the volume ratio of the two is 1:7.Ultrasonic for this solution 10min is uniformly dispersed, obtains homodisperse PS nanosphere solution.
C) pre-assembled at water surface of PS nanosphere.Prepare the culture dish (surface area of water is S) that fills with deionized water, measure with micropipettor homodisperse PS nanosphere solution (the V/S=1.5 μ L/cm that volume is V
2), be distributed on the Si sheet after hydrophily process, then this Si sheet is stretched in deionized water with the inclination angle of 15 °, PS nanosphere can be observed and slip into water surface, form one deck glossiness PS nanosphere monofilm at water surface gradually.Be V at culture dish edge injected slurry volume
1sodium dodecyl sulfate solution (concentration is 0.5g/L, V
1/ S=0.02 μ L/cm
2), PS nanosphere monofilm is arranged and more compacts with complete.
D) PS nanosphere monofilm is transferred to sample surfaces.Separately get the Si sheet that a slice a) processes through step, insert gently in deionized water along culture dish edge with the angle of inclination of 15 °, when this sample immerses below PS nanosphere monofilm completely, slowly lift this sample, PS nanosphere monofilm is picked up, leave standstill sample until moisture dries naturally, can obtain at sample surfaces the PS nanosphere structure that individual layer independently fills.
E) size of PS nanosphere controls.Adopt inductively coupled plasma etching machine (ICP), at radio-frequency power 30W, base vacuum 1 × 10
-4under the etching condition of Pa, reaction pressure 5Pa, logical oxygen (O
2) etching 10min, thus reduce the diameter of PS nanosphere.
F) deposition of metal.By the mode (chamber pressure: 1 × 10 of thermal evaporation
-3pa, speed: 0.05nm/s) respectively in steps d) and step e) deposit thickness is the metal A g of 15nm on the sample that obtains.
G) PS nanosphere is removed.Sample after two kinds of plated metals is soaked 3min in chloroform, and cleans 5min with ultrasonic wave added, then clean by deionized water, and use N
2air-blowing is done, and namely obtains two kinds of metal Nano structures at two kinds of sample surfaces.
Other technological processes related in the present invention and condition are common process, belong to this area the category be familiar with, do not repeat them here.
Above-described embodiment just schematically, not forms limiting the scope of the invention.Belonging to the researcher in field prepare in the present invention on the basis of metal micro-nanostructure scheme, do not need to pay creative work and the various amendment made or distortion still in protection scope of the present invention.
Claims (10)
1. a preparation method for the metal Nano structure that resonance peak is adjustable, is characterized in that, comprises the following steps:
A) hydrophily process is carried out to sample surfaces;
B) homodisperse PS nanosphere solution is prepared:
Be 1:(1 ~ 10 by volume by PS nanosphere dispersion liquid and absolute ethyl alcohol) mixing, ultrasonic disperse is even, obtains homodisperse PS nanosphere solution; Wherein the diameter of PS nanosphere is the mass fraction of PS nanosphere in 50nm ~ 1000nm, PS nanosphere dispersion liquid is 5% ~ 20%;
C) pre-assembled at the water surface of PS nanosphere:
Homodisperse PS nanosphere solution is added drop-wise on the Si sheet after hydrophily process, being stretched into the angle of inclination of 10 ~ 45 ° by this silicon chip fills in the container of deionized water again, PS nanosphere slips in deionized water, at the water surface pre-assembled formation PS nanosphere monofilm; The pass being wherein added drop-wise to the surface area S of deionized water in the volume V of the PS nanosphere solution on Si sheet and container is V/S=0.5 ~ 5 μ L/cm
2;
D) PS nanosphere monofilm is transferred to sample surfaces a) processed through step, obtains at sample surfaces the PS nanosphere structure that individual layer independently fills;
E) by the mode of electron beam evaporation, thermal evaporation or magnetron sputtering at the sample surfaces plated metal with the PS nanosphere structure that individual layer independently fills, the gross thickness of the metal of deposition is less than the radius of PS nanosphere in PS nanosphere structure;
F) the PS nanosphere structure of the sample surfaces after plated metal is removed, namely obtain the adjustable metal Nano structure of resonance peak at sample surfaces.
2. the preparation method of the metal Nano structure that resonance peak according to claim 1 is adjustable, is characterized in that: concrete operations a) of described step are: sample is placed in ozone environment, with Ultraviolet radiation 1 ~ 30min; Or sample being placed in volume ratio is the concentrated sulfuric acid of 3:1 and the mixed solution of hydrogen peroxide, at 100 ~ 150 DEG C, soak 30 ~ 120min.
3. the preparation method of the metal Nano structure that resonance peak according to claim 1 is adjustable, is characterized in that: described step a) in sample be Si sheet, sapphire, ITO layer, GaN layer or glass.
4. the preparation method of the metal Nano structure that resonance peak according to claim 1 is adjustable, it is characterized in that: described step c) in until PS nanosphere after water surface pre-assembled formation PS nanosphere monofilm, sodium dodecyl sulfate solution is injected at container edge, wherein the concentration of sodium dodecyl sulfate solution is 0.1 ~ 10g/L, the volume V of the sodium dodecyl sulfate solution of injection
1be V with the pass of the surface area S of deionized water in container
1/ S=0.01 ~ 0.1 μ L/cm
2.
5. the preparation method of the metal Nano structure that resonance peak according to claim 1 is adjustable, it is characterized in that: described steps d) concrete operations be: the sample that a) will process through step with the angle of inclination of 10 ~ 45 ° along step c) container edge insert in deionized water, when this sample immerses below PS nanosphere monofilm completely, upwards lift this sample, PS nanosphere monofilm is picked up, leave standstill sample until the moisture on PS nanosphere monofilm dries naturally, namely obtain at sample surfaces the PS nanosphere structure that individual layer independently fills.
6. the preparation method of the metal Nano structure that resonance peak according to claim 1 is adjustable, it is characterized in that: described step e) carry out before, first the size of the PS nanosphere in the PS nanosphere structure of sample surfaces is regulated and controled, namely the diameter of PS nanosphere is increased by the mode of heating using microwave or flat heater, or by the oxygen etching PS nanosphere of inductively coupled plasma etching machine, to reduce the diameter of PS nanosphere.
7. the preparation method of the metal Nano structure that resonance peak according to claim 6 is adjustable, is characterized in that: when increasing the diameter of PS nanosphere by the mode of flat heater, and the heat time is 5 ~ 60s, and heating-up temperature is 80 ~ 150 DEG C;
When increasing the diameter of PS nanosphere by the mode of heating using microwave, the heat time is 5 ~ 200s, and heating-up temperature is 70 ~ 100 DEG C;
When reducing the diameter of PS nanosphere with inductively coupled plasma etching machine, etching power is 30 ~ 300W, and etch period is 0.5 ~ 10min, and pressure during etching is 0.5 ~ 5Pa.
8. the preparation method of the metal Nano structure that resonance peak according to claim 6 is adjustable, is characterized in that: when after the diameter increasing PS nanosphere, step e) in the gross thickness of metal of deposition be less than the original radius of PS nanosphere;
When after the diameter reducing PS nanosphere, step e) in the gross thickness of metal of deposition be less than the radius of the PS nanosphere after reduction.
9. the preparation method of the metal Nano structure that resonance peak according to claim 1 is adjustable, it is characterized in that: described step e) in deposition metal be simple metal, metallic compound and/or alloy, wherein simple metal is the mixture of one or more arbitrary proportions in aluminium, silver, gold, titanium, nickel, platinum, copper, and metallic compound is CdS, MgO, MgF
2in the mixture of one or more arbitrary proportions, alloy is Au/Sn alloy;
During plated metal, deposit various metals respectively, form multiple metal level, in each metal level, comprise one or more metals; Or deposit various metals simultaneously, form an overall metal mixed layer.
10. the preparation method of the metal Nano structure that resonance peak according to claim 1 is adjustable, it is characterized in that: described step f) in remove PS nanosphere structure concrete operations be: the sample after plated metal is soaked 1 ~ 10min in chloroform, and clean with ultrasonic wave added, use acetone, ethanol or deionized water rinsing afterwards, finally with Ar gas or N
2air-blowing is done.
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