CN103233208A - Device and method for preparing micro nano-structure film by using ion beam sputtering method - Google Patents

Device and method for preparing micro nano-structure film by using ion beam sputtering method Download PDF

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CN103233208A
CN103233208A CN2013101462982A CN201310146298A CN103233208A CN 103233208 A CN103233208 A CN 103233208A CN 2013101462982 A CN2013101462982 A CN 2013101462982A CN 201310146298 A CN201310146298 A CN 201310146298A CN 103233208 A CN103233208 A CN 103233208A
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ion beam
beam sputtering
annulus
micro nano
structure film
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CN103233208B (en
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陶海华
张双喜
乔延琦
蒋为桥
陈险峰
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Shanghai Jiaotong University
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Shanghai Jiaotong University
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Abstract

The invention provides a device and method for preparing a micro nano-structure film by using an ion beam sputtering method. The device comprises an ion beam sputtering device and a collimating filter, wherein the collimating filter is connected with a sample frame of the ion beam sputtering device, and comprises a disc, a plurality of filter screens and a plurality of rings; the lower surface of the disc is connected with the sample frame; the rings are sequentially overlapped on the upper surface of the disc; and the filter screens are arranged among the rings. By adopting the device and the method, the quality of the micro nano-structure film can be effectively improved; and the device and the method have an important application value in the filed of nano integrated circuits.

Description

Utilize ion beam sputtering to prepare the device and method of micro nano structure film
Technical field
The present invention relates to the micro nano structure film preparing technology, particularly, relate to a kind of device and method that utilizes ion beam sputtering to prepare the micro nano structure film.
Background technology
Recently the more than ten years, along with developing rapidly of micro-nano processing technology, its minimum process yardstick strides forward to tens nanometers, and working accuracy also more and more higher (can reach several nanometers), and this film deposition techniques to micro nano structure is had higher requirement.Such as, in front line science researchs such as emerging nanophotonics, nanoelectronics, we often need prepare the metallic film with certain micro nano structure.In the fundamental research in this field, evaporation coating technique (as hot evaporation, electron beam evaporation plating) is because the energy of particles such as the atom that produces, elementide is lower, and its damage to the photoresist material mask is less, is easy to demoulding, thereby obtains at present using comparatively widely.But, adopt this deposition techniques film to have certain problem, such as problem such as the relative relatively poor and utilization rate of raw materials with the bonding force of substrate of film is low, this will become people's inevitable problem in the industrialization process of following nanometer integrated circuit.
Sputter coating is a kind of important thin film deposition processes, and it constitutes two kinds of important technologies of physical vapor deposition with evaporation, and it is bringing into play very important effect in present suitability for industrialized production.Large area film depositing operation or MEMS (micro electro mechanical system) (Micro-Electro-Mechanical Systems, be called for short MEMS) in the graphic structure used generally more than several microns, physical vapor sputtered film deposition technique is owing to save starting material, film and be combined advantages such as firm and compactness is good with substrate and play an important role in the scientific research in this field and suitability for industrialized production.Although the physical sputtering coating technique has the incomparable advantage of above-mentioned evaporation coating technique, in the fundamental research of the more and more littler nano structured unit of preparation size, this technology is but adopted by people hardly.As everyone knows, for evaporate process, particle energys such as the atom in the sputter coating process, elementide approximately are its tens times.When the dimension of picture of preparation more and more hour, also corresponding attenuation of the thickness of its photoresist material mask (specifically, the thickness of photoresist material mask is no more than three times of dimension of picture).Therefore, high energy particle in the physical sputtering coating process will produce the considerable damage effect to this very thin relatively photoresist material mask, particularly to the edge section of micro nano structure, it causes difficulty also for demoulding technology simultaneously, thereby causes the quality of micro nano structure film to reduce rapidly.
High-octane particle just can be used for this sputter coating process the preparation process of micro nano structure film to the destruction of photoresist material mask in the sputtering technology if can reduce.Particularly, mainly need to solve the problem of following two aspects: at first, reduce the energy of sputtering particle when deposit film; Secondly, further strengthen the directivity of sputtering particle, reduce the considerable damage that the oblique incidence particle produces the photoresist material edge.Among the present invention, be example with the ion beam sputtering deposition technology, by the one cover collimation filtration unit of addition in this complete equipment, can obviously improve the quality of micro nano structure film.This technology is simple and feasible, not only can improve the quality of micro nano structure film, and can utilize the physical sputtering equipment of present industrialization further to promote the process of industrialization of nanometer integrated circuit.
Summary of the invention
At defective of the prior art, the purpose of this invention is to provide a kind of device and method that utilizes ion beam sputtering to prepare the micro nano structure film.
According to an aspect of the present invention, a kind of device that utilizes ion beam sputtering to prepare the micro nano structure film is provided, comprise ion beam sputtering device and collimation filtration unit, the collimation filtration unit is connected with the specimen holder of ion beam sputtering device, the collimation filtration unit comprises: disk, some filtering nets and a plurality of annulus, the lower surface of disk is connected with specimen holder, and each annulus overlaps successively at disk upper surface, and filtering net is arranged between each annulus.
Preferably, be provided with perforate on disk and the annulus, disk and annulus are solidly connected to specimen holder by perforate by screw.
Preferably, the quantity of filtering net is one, and the quantity of annulus is two; Or the quantity of filtering net is two, and the quantity of annulus is three.
Preferably, the diameter of disk is 4 inches, and thickness is 3mm.
Preferably, filtering net is square, and its center mesh partly is circular, and mesh is hexagonal structure.
Preferably, the thickness of filtering net is 50 μ m, and the length of side is 50mm, and central network bore portion diameter is 42mm, and mesh aperture is 100 μ m, and rib width is 40~50 μ m.
Preferably, the annulus external diameter is 4 inches, and internal diameter is 45mm, and thickness is 3mm.
Preferably, disk, filtering net and annulus all adopt stainless material to make.
According to another aspect of the present invention, provide a kind of method of utilizing ion beam sputtering to prepare the micro nano structure film, may further comprise the steps:
Step 1: preparation has the sample of photoresist material polymethylmethacrylate mask;
Step 2: open the primary source of ion beam sputtering equipment, charge into nitrogen, open vacuum chamber;
Step 3: the sample of step 1 preparation is fixed on the disk of collimation filtration unit, filtering net is clamped between the annulus, and will collimates the specimen holder that filtration unit is fixed in the ion beam sputtering device;
Step 4: open water-cooling system and the mechanical pump power supply of vacuum chamber sample table successively, after vacuum tightness is higher than 1Pa, open molecular pump; When vacuum chamber base vacuum degree reaches 2*10 -4Behind the Pa, open ion beam sputter depositing equipment;
Step 5: after sputter was finished, closure molecule pump and mechanical pump charged into nitrogen successively, take out sample, place acetone reagent to soak about 5 hours in sample, remove the PMMA electron beam resist, and use acetone, ethanol and washed with de-ionized water successively, dry up with nitrogen at last.
Preferably, in the step 4, the processing parameter of ion beam sputtering is:
Ion energy: 850eV; Ion beam current: 70mA; In and electric current: 91mA;
Working gas and pressure: O 21.9*10 -2Pa;
Depositing time: Cr is 20sec, and Ag is 80sec;
Sputter is at interval: 5min intermittently behind every sputter 60sec.
Compared with prior art, the present invention has following beneficial effect: the present invention collimates filtration unit by design and is arranged on the specimen holder of ion beam sputtering equipment, not only can effectively stop large-angle inclined projectile in suprabasil deposition, reduce the destruction that it produces photoresist material mask (particularly its boundary member), and can stop the large size elementide that produces behind the ion beam bombardment target etc. in suprabasil deposition, thereby effectively improve the micro nano structure film quality of preparation.The present invention is that the application of coating process in micro nano structure element and following micro-nano integrated circuit of core is significant for expanding with the physical vapor sputtering technology.
Description of drawings
By reading the detailed description of non-limiting example being done with reference to the following drawings, it is more obvious that other features, objects and advantages of the present invention will become:
Fig. 1 prepares the structural representation of the device of micro nano structure film for the present invention utilizes ion beam sputtering;
Fig. 2 is the STRUCTURE DECOMPOSITION figure of the collimation filtration unit of the embodiment of the invention;
Fig. 3 is the filter screen structure synoptic diagram of the embodiment of the invention;
Fig. 4 compares for scanning electronic microscope (SEM) shape appearance figure that adopts the micro nano structure figure of the forward and backward preparation of collimation filtration unit among the present invention: (a) for not adopting the collimation filtration unit; (b) for adopting single layer filter net collimation filtration unit; (c) for adopting double-layer filtering net collimation filtration unit;
Fig. 5 is the optical morphology figure that utilizes the micro nano structure array that adopts double-layer filtering net collimation filtration unit deposition among the present invention.
Among the figure: 1 is specimen holder, and 2 are the collimation filtration unit, and 3 is disk, and 4 is filtering net, and 5 is annulus.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment.Following examples will help those skilled in the art further to understand the present invention, but not limit the present invention in any form.Should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make some distortion and improvement.These all belong to protection scope of the present invention.
A kind of device that utilizes ion beam sputtering to prepare the micro nano structure film, comprise ion beam sputtering device and collimation filtration unit 2, collimation filtration unit 2 is connected with the specimen holder 1 of ion beam sputtering device, collimation filtration unit 2 comprises: disk 3, two filtering nets 4 and three annulus 5, the lower surface of disk 3 is connected with specimen holder 1, each annulus 5 overlaps the upper surface at disk 3 successively, and filtering net 4 is arranged between each annulus 3.
The lower surface of disk 3 is connected with specimen holder 1, and upper surface is used for placing and fixed sample, and the diameter of disk 3 is 4 inches, and thickness is 3mm.
As shown in Figure 3, it is the structural representation of filtering net.The size of filtering net 4 is slightly larger than the internal diameter size of annulus 5, and the profile of filtering net 4 is the square of length of side 50mm, and the center is the filtering net of diameter 42mm, thickness is about 50 μ m, mesh is hexagonal structure, and mesh aperture is about 100 μ m, and rib width is about 40 μ m~50 μ m.
Annulus 5 not only can be fixed on the specimen holder 1 of ion beam sputtering device with disk 3, and tight clamping filtering net 4 between each annulus 5.The external diameter of annulus 5 is 4 inches, and internal diameter is 45mm, and thickness is 3mm.
Further, annulus 5 and disk 3 have the perforate that three diameters are 3.5mm respectively, and three perforates are evenly distinguished on circumference, can annulus 5 and disk 3 be fixed on the specimen holder 1 with the M3 screw.
More specifically, disk 3, filtering net 4 and annulus 5 all adopt stainless material to make.
In this example, adopt double-layer filtering net collimation filtration unit 2, comprised two filtering nets 4 and three annulus 5.But, need to prove that the present invention does not limit the quantity of concrete filtering net 4 and annulus 5.In actual applications, select the structure of concrete collimation filtration unit 2 according to actual needs, can be double-layer filtering net, can also be single layer filter net even bed filtration net, correspondingly, the quantity of filtering net 4 and annulus 5 can be a filtering net 4 and two annulus 5, or is a plurality of.Therefore, more than adopt just embodiment of double-layer filtering net collimation filtration unit 2, and be not used in restriction the present invention.
The present invention also provides a kind of method of utilizing ion beam sputtering to prepare the micro nano structure film, may further comprise the steps:
Step 1: preparation has the sample of photoresist material polymethylmethacrylate (Poly (methyl methacrylate) is called for short PMMA) mask.
Step 2: open the primary source of ion beam sputtering equipment, charge into nitrogen, open vacuum chamber.
Step 3: the sample of step 1 preparation is fixed on the disk of collimation filtration unit, filtering net is clamped between the annulus, and will collimates the specimen holder that filtration unit is fixed in the ion beam sputtering device.
Step 4: open water-cooling system and the mechanical pump power supply of vacuum chamber sample table successively, after vacuum tightness is higher than 1Pa, open molecular pump; When vacuum chamber base vacuum degree reaches 2*10 -4Behind the Pa, open ion beam sputter depositing equipment.
Particularly, the processing parameter of ion beam sputtering is:
Ion energy: 850eV; Ion beam current: 70mA; In and electric current: 91mA;
Working gas and pressure: O 21.9*10 -2Pa;
Depositing time: Cr is 20sec, and Ag is 80sec;
Sputter is at interval: 5min intermittently behind every sputter 60sec.
Under above sputtering parameter, when not adopting the collimation filtration unit, depositing of thin film speed is 4nm/sec; After adding single layer filter net collimation filtration unit, depositing of thin film speed is 2.6nm/sec; After adding double-layer filtering net collimation filtration unit, depositing of thin film speed is 1.8nm/sec.Thereby, adopt collimation filtration unit of the present invention, be the film of sediment-filled phase stack pile, need calculate the ion beam sputtering required time in advance.
Step 5: after sputter was finished, closure molecule pump and mechanical pump charged into nitrogen successively, take out sample, place acetone reagent to soak about 5 hours in sample, remove the PMMA electron beam resist, and with using acetone, ethanol and washed with de-ionized water successively, dry up with nitrogen at last.
For the above-mentioned technology of utilizing ion beam sputtering device deposition micro nano structure film, be example with the indicia patterns in everybody the graphene nano electrode production process paid close attention to widely below, specify how at SiO 2Deposit thickness is about the micro nano structure Cr/Ag film of 40nm in (290nm thickness)/Si substrate:
(1) is about the SiO of 10mm in the length of side 2The electron beam resist of spin coating PMMA495 and 950 two types successively in/the Si substrate, its thickness is respectively 290nm and 230nm, and photoresist material mask total thickness is 520nm.
(2) utilize Zeiss Ultra55 scanning electronic microscope and supporting electron beam diaphragm and graphicalphanumeric generator to be of a size of the indicia patterns of 500-1000nm in this substrate exposure with (1) described photoresist material mask, its exposure dose is 600.
(3) in the developing solution of the mix reagent of Virahol (IPA) and 4-methyl-2 pentanone (MIBK) preparation and IPA stop bath, developed successively 40 seconds and photographic fixing 60 seconds, dry up with nitrogen then.The volume ratio of IPA and MIBK is 3:1.After development, the photographic fixing, indicia patterns is transferred on the PMMA photoresist material mask.
(4) open the primary source of ion beam sputtering equipment, charge into nitrogen, open vacuum chamber.This ion beam sputtering equipment is the double ion beam sputtered depositing system of LDJ-2A-F100-100 series that Beijing Ai Dewansi ion beam technology institute produces.
(5) sample with photoresist material mask for preparing in the step of above-mentioned (1) to (3) is fixed on the disk of collimation filtration unit, then single filtering net is held between two annulus of near-neighbor sample and (namely adopts single-filtering net collimation filtration unit), perhaps two filtering nets are held on successively between three annulus and (namely adopt two filtering net collimation filtration units), at last this cover collimation filtration unit is fixed on the specimen holder of ion beam sputtering device.
(6) open water-cooling system and the mechanical pump power supply of vacuum chamber sample table successively.After vacuum tightness is higher than 1Pa, open molecular pump; When vacuum chamber base vacuum degree reaches 2*10 -4Behind the Pa, open ion beam sputter depositing equipment.
Significant parameter in the ion beam sputtering process is as follows:
Ion energy: 850eV; Ion beam current: 70mA; In and electric current: 91mA;
Working gas and pressure: 1.9*10 -2The O of Pa 2
Depositing time: Cr is 20sec, and Ag is 80sec;
Sputter is at interval: 5min intermittently behind every sputter 60sec.
(7) calculate sputtering time, after sputter procedure was finished, closure molecule pump and mechanical pump charged into nitrogen successively, took out sample.
(8) sample is placed acetone reagent soaked about 5 hours, remove the PMMA electron beam resist, and with using acetone, ethanol and washed with de-ionized water successively, dry up with nitrogen at last.
Utilize SEM to observe the metallic film shape appearance figure of above-mentioned ion beam sputtering equipment preparation, relatively employing collimates the morphology change of the micro nano structure figure of the forward and backward preparation of filtration unit, as shown in Figure 4.Can see that collimation filtration unit of the present invention can obviously improve the quality of the micro nano structure film that utilizes the ion beam sputtering equipment deposition.Utilize the optical morphology of ion beam sputtering equipment and the micro nano structure indicia patterns array that adopts the preparation of double-layer filtering net collimation filtration unit as shown in Figure 5, can reach application requiring.
The present invention is by the one cover collimation filtration unit of addition on the specimen holder of ion beam sputtering equipment, the large size elementides that produce in the time of can effectively stoping the oblique incidence particle to the destruction of mask (particularly boundary member) generation and stop the ion beam bombardment target etc. are in suprabasil deposition, thereby improve the quality of micro nano structure film, have important use in nanometer integrated circuit field and be worth.
More than specific embodiments of the invention are described.It will be appreciated that the present invention is not limited to above-mentioned specific implementations, those skilled in the art can make various distortion or modification within the scope of the claims, and this does not influence flesh and blood of the present invention.

Claims (10)

1. device that utilizes ion beam sputtering to prepare the micro nano structure film, it is characterized in that, comprise ion beam sputtering device and collimation filtration unit, described collimation filtration unit is connected with the specimen holder of described ion beam sputtering device, described collimation filtration unit comprises: disk, some filtering nets and a plurality of annulus, the lower surface of described disk is connected with described specimen holder, and described each annulus overlaps successively at described disk upper surface, and described filtering net is arranged between described each annulus.
2. the device that utilizes ion beam sputtering to prepare the micro nano structure film according to claim 1 is characterized in that, is provided with perforate on described disk and the annulus, and described disk and annulus are solidly connected to described specimen holder by described perforate by screw.
3. the device that utilizes ion beam sputtering to prepare the micro nano structure film according to claim 1 is characterized in that, the quantity of described filtering net is one, and the quantity of described annulus is two; Or the quantity of described filtering net is two, and the quantity of described annulus is three.
4. the device that utilizes ion beam sputtering to prepare the micro nano structure film according to claim 1 is characterized in that, the diameter of described disk is 4 inches, and thickness is 3mm.
5. the device that utilizes ion beam sputtering to prepare the micro nano structure film according to claim 1 is characterized in that, described filtering net is square, and the mesh of described filtering net is hexagonal structure.
6. the device that utilizes ion beam sputtering to prepare the micro nano structure film according to claim 5 is characterized in that, the thickness of described filtering net is 50 μ m, the length of side is 50mm, central network bore portion diameter is 42mm, and mesh aperture is 100 μ m, and rib width is 40~50 μ m.
7. the device that utilizes ion beam sputtering to prepare the micro nano structure film according to claim 1 is characterized in that, described annulus external diameter is 4 inches, and internal diameter is 45mm, and thickness is 3mm.
8. according to each described device that utilizes ion beam sputtering to prepare the micro nano structure film of claim 1 to 7, it is characterized in that described disk, filtering net and annulus all adopt stainless material to make.
9. a method of utilizing ion beam sputtering to prepare the micro nano structure film is characterized in that, may further comprise the steps:
Step 1: preparation has the sample of photoresist material polymethylmethacrylate mask;
Step 2: open the primary source of ion beam sputtering equipment, charge into nitrogen, open vacuum chamber;
Step 3: the sample of step 1 preparation is fixed on the disk of collimation filtration unit, filtering net is clamped between the annulus, and will collimates the specimen holder that filtration unit is fixed in the ion beam sputtering device;
Step 4: open water-cooling system and the mechanical pump power supply of vacuum chamber sample table successively, after vacuum tightness is higher than 1Pa, open molecular pump; When vacuum chamber base vacuum degree reaches 2*10 -4Behind the Pa, open ion beam sputter depositing equipment;
Step 5: after sputter was finished, closure molecule pump and mechanical pump charged into nitrogen successively, take out sample, place acetone reagent to soak about 5 hours in sample, remove the PMMA electron beam resist, and use acetone, ethanol and washed with de-ionized water successively, dry up with nitrogen at last.
10. the method for utilizing ion beam sputtering to prepare the micro nano structure film according to claim 9 is characterized in that, in the step 4, the processing parameter of ion beam sputtering is:
Ion energy: 850eV; Ion beam current: 70mA; In and electric current: 91mA;
Working gas and pressure: O 21.9*10 -2Pa;
Depositing time: Cr is 20sec, and Ag is 80sec;
Sputter is at interval: 5min intermittently behind every sputter 60sec.
CN201310146298.2A 2013-04-24 2013-04-24 Ion beam sputtering is utilized to prepare the method for micro nano structure film Expired - Fee Related CN103233208B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106282955A (en) * 2016-08-31 2017-01-04 北京埃德万斯离子束技术研究所股份有限公司 A kind of method preparing functional graphic films on flexible substrates thin film
CN112475293A (en) * 2020-12-08 2021-03-12 中北大学 Preparation method of micro-nano lattice hole ultrathin stainless steel filter plate

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5330628A (en) * 1990-01-29 1994-07-19 Varian Associates, Inc. Collimated deposition apparatus and method
CN101307430A (en) * 2008-07-04 2008-11-19 郑州大学 Energy filtrated magnetron sputtering plating method and apparatus for applying the method
CN203295598U (en) * 2013-04-24 2013-11-20 上海交通大学 Device for preparing micro-nano structure thin film by utilizing ion beam sputtering method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5330628A (en) * 1990-01-29 1994-07-19 Varian Associates, Inc. Collimated deposition apparatus and method
CN101307430A (en) * 2008-07-04 2008-11-19 郑州大学 Energy filtrated magnetron sputtering plating method and apparatus for applying the method
CN203295598U (en) * 2013-04-24 2013-11-20 上海交通大学 Device for preparing micro-nano structure thin film by utilizing ion beam sputtering method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106282955A (en) * 2016-08-31 2017-01-04 北京埃德万斯离子束技术研究所股份有限公司 A kind of method preparing functional graphic films on flexible substrates thin film
CN112475293A (en) * 2020-12-08 2021-03-12 中北大学 Preparation method of micro-nano lattice hole ultrathin stainless steel filter plate

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