CN102923647A - Method for preparing ordered array of metal nano-particles with adjustable space and appearance - Google Patents
Method for preparing ordered array of metal nano-particles with adjustable space and appearance Download PDFInfo
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Abstract
The invention discloses a method for preparing an ordered array of metal nano-particles with adjustable space and appearance. According to the method, a self-assembled compactly-arranged nano-sphere layer used as a template is etched by adopting an etching method to change the space, size and appearance of the nano-spheres, then a metal material is deposited on the nano-sphere layer used as the template by adopting a thermal vapor deposition method, and the nano-sphere layer is removed to obtain the ordered array of the metal nano-particles. The ordered array of the metal nano-particles is arranged orderly and periodically repeated, and the nano-particles are basically same in size. The method provided by the invention adopts reliable techniques and simple processes, has low cost and can be used for industrially producing the high-quality orderly-arranged nano-particles with adjustable space and appearance.
Description
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Technical field
The invention belongs to field of nanometer material technology, relate in particular to the preparation method of the regulatable metal nanoparticle oldered array of a kind of spacing and pattern.
Background technology
When scantling reaches nanometer scale, will have many peculiar physical propertys, show the character that not only is different from corresponding body material but also is different from individual molecule.But along with material particle size reduces, surface energy increases, and particle is easier reunion also, thereby can cover many good character.If measure-alike nano particle is arranged on the two dimensional surface regularly by certain way, form orderly nano particle two-dimensional array system, then the character of this class nano material just can show well.
Preparing in general this ordered nano particle two-dimensional array has two kinds of approach, i.e. self-organizing ranking method and the etching method of particle.The former can only form the regularly arranged of small scale, can't realize particle interval, isoparametric control of cycle; And etching method can realize the regularly arranged of large scale in principle, and can control grain spacing, but existing standard etch method such as photoengraving, owing to be subjected to the restriction of resolution of diffraction, is difficult to use in the manufacturing nanostructured; Utilize electron beam, X ray and STM(PSTM) etc. etching method, equipment is complicated, cost is expensive, efficient is low, prepares the nano-grain array system for large tracts of land and also has difficulties.
In recent years, a kind of new etching method occurs in the world and prepared the nano particle two-dimensional ordered array, it is the Nano microsphere etching method, the method is that the nano-array composite that forms take Nano microsphere is as mask, deposit required element thereon, just can obtain arranging orderly nano-grain array after removing mask.But, for the preparation of industrialization of spacing with the regulatable nano particle ordered array of pattern of arranging, not yet form the universal method of high efficiency, low cost.Therefore, but how the nano particle of the high-quality spacing of simple, low-cost suitability for industrialized production and the regulatable ordered arrangement of pattern of arranging is at present difficult point and the focus of research of this area.
Summary of the invention
Preparation method for existing spacing and the regulatable nano-grain array of pattern is unsuitable for industrial problem; the invention provides a kind of spacing of suitability for industrialized production and preparation method of the regulatable metal nanoparticle oldered array of pattern of being suitable for, the method is simple, efficient, with low cost and be easy to large-scale production.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
The preparation method of the regulatable metal nanoparticle oldered array of a kind of spacing and pattern comprises step:
Step 2 is by size, spacing and the pattern of nanosphere in the etching method regulation and control nanosphere layer template;
Step 3 adopts Vacuum Coating method plated metal nano-array on the nanosphere layer template after the etching;
Step 4 is removed nanosphere layer template, namely obtains the metal nanoparticle oldered array.
Nanosphere described in the step 1 is polystyrene nanospheres, and its diameter is 460 ~ 800nm; Described self assembly substrate is silicon chip.
At first adopt deionized water, plasma cleaning to process the self assembly substrate, the nanosphere layer template that then adopts the liquid level self-assembly method closely to arrange in self assembly substrate preparation; Described plasma cleaning adopts plasma cleaner to carry out, and cleaning is: scavenging period 30 min, and plasma cleaner cleans power 30 W, and atmosphere is oxygen, gas pressure intensity 10Pa.
Adopt size, the spacing of nanosphere in the plasma etching method regulation and control nanosphere layer template in the step 2, regulate and control size, spacing and the pattern of nanosphere by the control etch period, concrete etching technics is: utilize plasma etching machine to carry out etching, the etching gas atmosphere is oxygen, gas pressure intensity 10Pa, plasma cleaner etching power 30 W.
Metal nano array described in the step 3 is the cadmium gold-nano array, and the Vacuum Coating method that adopts is the thermal evaporation coating method.
The a kind of of step 3 is embodied as:
Utilize vacuum coating equipment 2 * 10
-3Under the vacuum of Pa, with 3 nmmin
-1Sedimentation rate, successively evaporation cadmium film, gold thin film on the nanosphere layer template surface after the etching obtain the cadmium gold-nano array.
Adopt chemical etching method corrosion nanosphere layer template in the step 4.When nanosphere layer template is polystyrene nanospheres layer template, adopt chloroform soln to dissolve nanosphere layer template.
The pattern of the metal nanoparticle oldered array that step 4 obtains is triangle or network structure.
The basic ideas of the inventive method are: the nanosphere layer that the self assembly after etching is closely arranged is template, adopt Vacuum Coating method at template preparation metal nanoparticle oldered array, regulate and control size and the spacing of nanosphere in the nanosphere layer template by nanosphere and two aspects of control etch period of selecting different-diameter, thereby reach the spacing of regulation and control nano particle ordered array and the purpose of the pattern of arranging.
Etching of the present invention is the plasma etching method that adopts, this process is to carry out in the oxygen atmosphere, excite lower oxygen to be ionized high-tension, produce oxygen plasma oxidation nanometer ball surface, chemical reaction occurs and is corroded gradually in the nanosphere surface, along with etch period prolongs, the nanosphere diameter diminish gradually and nanosphere between spacing become large, thereby reach the purpose of regulation and control nanosphere size, spacing and pattern.
What vacuum coating of the present invention was adopted is the thermal evaporation coating method, under vacuum environment, metal is deposited on the nanosphere layer template surface after the etching because high temperature evaporation becomes gaseous atom, metallic atom is filled in the space between the nanosphere, forms nano particle ordered array.
The present invention adopts the nano-array of the method preparation that nanosphere etching and vacuum coating combines to have following several unique advantage: (1) Nano microsphere lithographic technique and vacuum coating technology develop into and have leveled off to now maturation, being widely used in field of nano material preparation, is very reliable technology; (2) the Nano microsphere etching technics is very simple, only needs simple a few step operation, and required main equipment is plasma cleaner, so cost is also very cheap; (3) vacuum coating have low energy consumption, nontoxic, without waste liquid, the advantage such as pollution is little, cost is low, good decorating effect, metal sense are strong; (4) the large I of Nano microsphere of experiment usefulness is precisely controlled, and domestic Properties of Polystyrene Nano Particles is dispersed in the aqueous solution with mass fraction 1%, and its diameter error coefficient is no more than 3%.
Description of drawings
Fig. 1 is the scanning electron microscope diagram sheet of the cadmium gold-nano array of embodiment 1 preparation;
Fig. 2 is the scanning electron microscope diagram sheet of the cadmium gold-nano array of embodiment 2 preparations;
Fig. 3 is the scanning electron microscope diagram sheet of the cadmium gold-nano array of embodiment 3 preparations;
Fig. 4 is the scanning electron microscope diagram sheet of the cadmium gold-nano array of embodiment 4 preparations;
Fig. 5 is the scanning electron microscope diagram sheet of the cadmium gold-nano array of embodiment 5 preparations;
Fig. 6 is the scanning electron microscope diagram sheet of the cadmium gold-nano array of embodiment 6 preparations.
Among the figure, a among Fig. 1,2,4 and 5 is the length of side of nano particle, and d is the distance between the adjacent nano particle; A among Fig. 3 and 6 is among the figure in the circular hole 1/6 of girth, and the distance between the adjacent nano particle is 0.
The specific embodiment
A kind of implementation of the inventive method is as follows:
Uniform self assembly one deck of surface of silicon of the single-sided polishing of two group of 1 cm after processing through washed with de-ionized water, plasma cleaning * 1 cm is arranged closely polystyrene nanospheres layer, and described polystyrene nanospheres diameter is 460 ~ 800nm.
Adopt the gas ions cleaning machine to clean the organic matter on monocrystalline substrate surface in this step, scavenging period is 30 min, and power is 30 W, and the plasma gas atmosphere is oxygen, and gas pressure is 10 Pa.
Step 2 is regulated and control size, spacing and the pattern of nanosphere in the nanosphere layer that self assembly closely arranges by etching method.
This step preferably adopts plasma etching method p-poly-phenyl ethene nanosphere to carry out etching, and the etching gas atmosphere is oxygen, and gas pressure intensity is 10 pa, and etching power is 30 W, and etch period can be regulated and control in 1 ~ 7min.
Step 3, the nanosphere layer after the etching adopt Vacuum Coating method plated metal nano-array thereon as template.
Adopt the thermal evaporation coating method, 2 * 10
-3Under the vacuum of Pa, on the polystyrene nanospheres layer template after the etching, at first deposit one deck 10nm thickness every, then deposit the gold of one deck 30nm, sedimentation rate is 3 nmmin
-1, obtain at last the cadmium gold-nano array.
Step 4 is removed nanosphere layer template, namely obtains nano particle ordered array.
With chloroform soln dissolved polystyrene nanosphere self assembly layer, clean respectively with absolute ethyl alcohol and deionized water again, obtain the cadmium gold-nano array after drying up with nitrogen, the pattern of the nano particle ordered array that obtains is triangle or network structure.
The present invention is further illustrated below in conjunction with embodiment.
In the oxygen atmosphere of 10Pa, the plasma clean acc power is transferred to 30 W, clean monocrystalline substrate surface 30 min, take out substrate; Adopt the liquid level self-assembly method on silicon substrate equably the layer overlay diameter be the polystyrene nanospheres layer of 460nm.In the oxygen atmosphere of 10Pa, the plasma clean acc power is transferred to 30 W, with the plasma clean machine to being covered with silicon substrate etching 1 min of polystyrene nanospheres layer.
Polystyrene nanospheres layer after the etching utilizes vacuum coating equipment 2 * 10 as template
-3Under the Pa vacuum, deposit first the cadmium of 10 nm at polystyrene nanospheres layer template surface, then deposit the gold of 30 nm, sedimentation rate is 3 nmmin
-1, form the cadmium gold thin film.By chloroform soln dissolved polystyrene nanosphere self assembly layer, clean respectively with absolute ethyl alcohol and deionized water again, dry up through nitrogen and obtain the cadmium gold-nano array.
Fig. 1 is SEM (SEM) image of present embodiment gained cadmium gold-nano array, can see that by SEM large-area cadmium gold-nano array is neat and orderly, presenting periodically repetition and cycle is 460nm, illustrates that the nanosphere as template is evenly closely to be arranged on the silicon substrate.The pattern of metal nanoparticle all is to be similar to equilateral triangle, and spacing is almost identical, and the size that nanosphere is described is precisely consistent, embodies the height reliability of Nano microsphere etching technics.Because the etch period of nanosphere is only had 1 min, so the nanosphere surface only has small part oxidized, so the cadmium gold nano grain of deposition is less, the length of side is about 100nm, and the spacing of adjacent nano particle is about 150nm.
Embodiment 2
In the oxygen atmosphere of 10 Pa, the plasma clean acc power is transferred to 30 W, clean monocrystalline substrate surface 30 min, take out substrate; Adopt the liquid level self-assembly method on silicon substrate equably the layer overlay diameter be the polystyrene nanospheres layer of 460 nm.In the oxygen atmosphere of 10 Pa, the plasma clean acc power is transferred to 30 W, with the plasma clean machine to being covered with silicon substrate etching 2 min of polystyrene nanospheres layer.
Individual layer pipe/polyhenylethylene nano after the etching utilizes vacuum coating equipment 2 * 10 as template
-3Under the Pa vacuum, deposit first the cadmium of 10 nm at polystyrene nanospheres layer template surface, then deposit the gold of 30 nm, sedimentation rate is 3 nmmin
-1, form the cadmium gold thin film.By chloroform soln dissolved polystyrene nanosphere self assembly layer, clean respectively with absolute ethyl alcohol and deionized water again, dry up through nitrogen and obtain the cadmium gold-nano array.
Fig. 2 is present embodiment gained SEM image, can see that by SEM large-area cadmium gold-nano array is neat and orderly, and presenting periodically repetition and cycle is 460nm, illustrates that the nanosphere as template is evenly closely to be arranged on the silicon substrate.The pattern of most of metal nanoparticle all is to be similar to equilateral triangle, and the spacing of nano particle is almost identical, illustrates that the nanosphere size as template is precisely consistent, embodies the height reliability of Nano microsphere etching technics.Because the etch period to nanosphere is 2 min, therefore some is oxidized on the nanosphere surface, nanosphere after the etching obviously diminishes than embodiment 1, so, large than among the embodiment 1 of the cadmium gold nano grain of deposition, small part nano particle even couple together, particle length of side size is about 150 nm, and the spacing of adjacent nano particle is about 110nm.
Embodiment 3
In the oxygen atmosphere of 10Pa, the plasma clean acc power is transferred to 30 W, clean monocrystalline substrate surface 30 min, take out substrate; Adopt the liquid level self-assembly method on silicon substrate equably the layer overlay diameter be the polystyrene nanospheres layer of 460 nm.In the oxygen atmosphere of 10Pa, the plasma clean acc power is transferred to 30W, with the plasma clean machine to being covered with silicon substrate etching 5 min of polystyrene nanospheres.
Individual layer polystyrene nanospheres layer after the etching utilizes vacuum coating equipment 2 * 10 as template
-3Under the vacuum of Pa, deposit first the cadmium of 10 nm at polystyrene nanospheres layer template surface, then deposit the gold of 30 nm, sedimentation rate is 3 nmmin
-1, form the cadmium gold thin film.By chloroform soln dissolved polystyrene nanosphere self assembly layer, clean respectively with absolute ethyl alcohol and deionized water again, after drying up, nitrogen obtains the cadmium gold-nano array.
Fig. 3 is the SEM image of present embodiment, can see that by SEM large-area cadmium gold-nano array is neat and orderly, and nano particle all coupled together and present the network structure that periodically repeats, and namely distance is 0 between the nano particle, and the cycle is 460nm.The cavity size of removing behind the nanosphere is identical, illustrate that the nanosphere as template is evenly closely to be arranged on the silicon substrate, and the size of nanosphere is accurate consistent, embodies the height reliability of Nano microsphere etching technics.Because the time to the Nano microsphere etching is 5 min, so the surface of nanosphere is basically oxidized, the nanosphere after the etching obviously diminishes than embodiment 1 and 2, so the cadmium gold nano grain of deposition has been linked to be netted, from obviously different among the embodiment 1,2.Thus, comparative example 1,2,3, the time by control etching Nano microsphere of can finding out can reach the purpose of regulation and control nano particle size, spacing and pattern.
Embodiment 4
In the oxygen atmosphere of 10 Pa, the plasma clean acc power is transferred to 30 W, clean monocrystalline substrate surface 30 min, take out substrate; Adopt the liquid level self-assembly method on silicon substrate equably the layer overlay diameter be the polystyrene nanospheres layer of 800nm.In the oxygen atmosphere of 10 Pa, the plasma clean acc power is transferred to 30 W, with the plasma clean machine to being covered with silicon substrate etching 1 min of polystyrene nanospheres layer.
Individual layer polystyrene nanospheres layer after the etching utilizes vacuum coating equipment 2 * 10 as template
-3Deposit first the cadmium of 10 nm under the vacuum of Pa at polystyrene nanospheres layer template surface, then deposit the gold of 30 nm, sedimentation rate is 3 nmmin
-1, form the cadmium gold thin film.By chloroform soln dissolved polystyrene nanosphere self assembly layer, clean respectively with absolute ethyl alcohol and deionized water again, after drying up, nitrogen obtains the cadmium gold-nano array.
Fig. 4 is the SEM image of present embodiment, can see that by SEM large-area cadmium gold-nano array is neat and orderly, and presenting periodically repetition and cycle is 800nm, illustrates that the nanosphere as template is evenly closely to be arranged on the substrate.The pattern of each metal nanoparticle is to be similar to equilateral triangle, and spacing is almost identical, and the size that nanosphere is described is precisely consistent, embodies the height reliability of nanosphere etching technics.Because the time of Nano microsphere etching is only had 1 min, so the surface of nanosphere only has part seldom oxidized, so the cadmium gold nano grain of deposition is less, the length of side is about 220 nm, and is more much bigger than the nano particle among the embodiment 1.Comparative example 1 and embodiment 4 can find out, select different big or small Nano microspheres also can regulate and control spacing and the size of nano particle, and the spacing of adjacent nano particle is about 200nm.
Embodiment 5
In the oxygen atmosphere of 10 Pa, the plasma clean acc power is transferred to 30 W, clean monocrystalline substrate surface 30 min, take out substrate; Adopt the liquid level self-assembly method on silicon substrate equably the layer overlay diameter be the polystyrene nanospheres layer of 800nm, form nanosphere layer template.In the oxygen atmosphere of 10 Pa, the plasma clean acc power is transferred to 30 W, with the plasma clean machine to being covered with silicon substrate etching 3 min of polystyrene nanospheres.
Individual layer polystyrene nanospheres layer after the etching utilizes vacuum coating equipment 2 * 10 as template
-3Deposit first the cadmium of 10 nm under the vacuum of Pa at polystyrene nanospheres layer template surface, then deposit the gold of 30 nm, sedimentation rate is 3 nmmin
-1, form the cadmium gold thin film.By chloroform soln dissolved polystyrene nanosphere self assembly layer, clean respectively with absolute ethyl alcohol and deionized water again, obtain the cadmium gold-nano array after drying up with nitrogen.
Fig. 5 is the SEM image of present embodiment, can see that by SEM large-area cadmium gold-nano array is neat and orderly, and presenting periodically repetition and cycle is 800nm, illustrates that the nanosphere as template is evenly closely to be arranged on the substrate.The pattern of most of metal nanoparticle all is to be similar to equilateral triangle, and the spacing of nano particle is almost identical, illustrates that the nanosphere size as template is precisely consistent, embodies the reliability that the Nano microsphere etching technics has height.Because the time to the Nano microsphere etching is 3 min, therefore some is oxidized on the surface of Nano microsphere, Nano microsphere after the etching obviously diminishes than embodiment 4, so, large than among the embodiment 4 of the cadmium gold nano grain of deposition, small part nano particle even couple together, particle length of side size is about 350nm, and the spacing of adjacent nano particle is about 50nm.
Embodiment 6
In the oxygen atmosphere of 10 Pa, the plasma clean acc power is transferred to 30 W, clean monocrystalline substrate surface 30 min, take out substrate; Adopt the liquid level self-assembly method on silicon substrate equably the layer overlay diameter be the polystyrene nanospheres layer of 800 nm.In the oxygen atmosphere of 10Pa, the plasma clean acc power is transferred to 30 W, with the plasma clean machine to being covered with silicon substrate etching 7 min of polystyrene nanospheres layer.
Individual layer polystyrene nanospheres layer after the etching utilizes vacuum coating equipment 2 * 10 as template
-3Deposit first the cadmium of 10 nm under the Pa vacuum at polystyrene nanospheres layer template surface, then deposit the gold of 30 nm, sedimentation rate is 3 nmmin
-1, form the cadmium gold thin film.By chloroform soln dissolving nanosphere self assembly layer, clean respectively with absolute ethyl alcohol and deionized water again, after drying up, nitrogen obtains the cadmium gold-nano array.
Fig. 6 is the SEM image of present embodiment, can see that by SEM large-area cadmium gold-nano array is neat and orderly, and nano particle all coupled together and present the network structure that periodically repeats, and namely distance is 0 between the nano particle, and the cycle is 800nm.The cavity size of removing behind the nanosphere is identical, illustrate that the Nano microsphere as masterplate is evenly closely to be arranged on the substrate, and the size of Nano microsphere is accurate consistent, embodies the height reliability of Nano microsphere etching technics.Because the etch period to nanosphere is 7 min, so the surface of Nano microsphere is basically oxidized, the Nano microsphere after the etching obviously diminishes than embodiment 4 and 5, so the cadmium gold nano grain of deposition has been linked to be netted obviously different from embodiment 4,5.Thus, comparative example 4,5,6, we can reach regulation and control nano particle size and the purpose of spacing and the pattern of nano-array by the time of control etching Nano microsphere; Comparative example 1 and 4, embodiment 2 and 5, embodiment 3 and 6, we can regulate and control by the Nano microsphere of selecting different sizes size, spacing and the cycle of nano particle.
Claims (10)
1. the preparation method of a spacing and the regulatable metal nanoparticle oldered array of pattern is characterized in that, comprises step:
Step 1, the nanosphere layer template that adopts the liquid level self-assembly method closely to arrange in self assembly substrate preparation;
Step 2 is by size, spacing and the pattern of nanosphere in the etching method regulation and control nanosphere layer template;
Step 3 adopts Vacuum Coating method plated metal nano-array on the nanosphere layer template after the etching;
Step 4 is removed the nanosphere template, namely obtains the metal nanoparticle oldered array.
2. the preparation method of spacing as claimed in claim 1 and the regulatable nano particle ordered array of pattern is characterized in that:
Nanosphere described in the step 1 is polystyrene nanospheres, and its diameter is 460 ~ 800nm.
3. the preparation method of spacing as claimed in claim 1 and the regulatable nano particle ordered array of pattern is characterized in that:
Self assembly substrate described in the step 1 is silicon chip.
4. the preparation method of spacing as claimed in claim 1 and the regulatable nano particle ordered array of pattern is characterized in that:
Step 1 is specially:
At first adopt deionized water, plasma cleaning to process the self assembly substrate, the nanosphere layer template that then adopts the liquid level self-assembly method closely to arrange in self assembly substrate preparation; Described plasma cleaning adopts plasma cleaner to carry out, and cleaning is: scavenging period 30 min, and plasma cleaner cleans power 30 W, and atmosphere is oxygen, gas pressure intensity 10Pa.
5. the preparation method of spacing as claimed in claim 1 and the regulatable nano particle ordered array of pattern is characterized in that:
Size, spacing and the pattern of regulating and control nanosphere in the nanosphere layer template by the control etch period in the step 2.
6. the preparation method of spacing as claimed in claim 1 and the regulatable nano particle ordered array of pattern is characterized in that:
Etching method described in the step 2 is the plasma etching method.
7. the preparation method of spacing as claimed in claim 1 and the regulatable nano particle ordered array of pattern is characterized in that:
Metal nano array described in the step 3 is the cadmium gold-nano array, and concrete preparation method is:
Utilize vacuum coating equipment 2 * 10
-3Under the vacuum of Pa, successively evaporation cadmium film, gold thin film on the nanosphere layer template surface after the etching obtain the cadmium gold-nano array.
8. the preparation method of spacing as claimed in claim 1 and the regulatable nano particle ordered array of pattern is characterized in that:
The Vacuum Coating method that adopts in the step 3 is the thermal evaporation coating method.
9. the preparation method of spacing as claimed in claim 1 and the regulatable nano particle ordered array of pattern is characterized in that:
Adopt chemical etching method corrosion nanosphere layer template in the step 4.
10. the preparation method of spacing as claimed in claim 1 and the regulatable nano particle ordered array of pattern is characterized in that:
The pattern of the metal nanoparticle oldered array that step 4 obtains is triangle or network structure.
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| CN110668397A (en) * | 2019-09-16 | 2020-01-10 | 吉林师范大学 | Preparation method of highly ordered inclined nano-column |
| CN113156554A (en) * | 2020-01-03 | 2021-07-23 | 杭州柔谷科技有限公司 | Optical functional film, preparation method thereof and flexible optoelectronic device |
| CN111349892A (en) * | 2020-03-24 | 2020-06-30 | 扬州大学 | Silver-superposed triangular nanoparticle array and preparation method thereof |
| CN111349892B (en) * | 2020-03-24 | 2022-05-13 | 扬州大学 | Silver-superposed triangular nanoparticle array and preparation method thereof |
| CN112713202A (en) * | 2020-12-29 | 2021-04-27 | 贵州梅岭电源有限公司 | Plasma optical gain film for solar cell |
| CN114262866A (en) * | 2021-12-21 | 2022-04-01 | 武汉中维创发工业研究院有限公司 | Powder and preparation method thereof |
| CN114262866B (en) * | 2021-12-21 | 2023-11-28 | 维达力实业(深圳)有限公司 | Powder and preparation method thereof |
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