CN110668395A - Preparation method of highly-ordered and axisymmetric nano periodic structure - Google Patents

Preparation method of highly-ordered and axisymmetric nano periodic structure Download PDF

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CN110668395A
CN110668395A CN201910870299.9A CN201910870299A CN110668395A CN 110668395 A CN110668395 A CN 110668395A CN 201910870299 A CN201910870299 A CN 201910870299A CN 110668395 A CN110668395 A CN 110668395A
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polystyrene
array
silicon wafer
sputtering
preparing
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张小龙
张永军
王雅新
陈雷
赵晓宇
朱琪
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Jilin Normal University
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Jilin Normal University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
    • B81C1/00023—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
    • B81C1/00119—Arrangement of basic structures like cavities or channels, e.g. suitable for microfluidic systems
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
    • B81C1/00023—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
    • B81C1/00031—Regular or irregular arrays of nanoscale structures, e.g. etch mask layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
    • B81C1/00523—Etching material
    • B81C1/00531—Dry etching
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
    • B81C1/00523—Etching material
    • B81C1/00539—Wet etching
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00841—Cleaning during or after manufacture
    • B81C1/00849—Cleaning during or after manufacture during manufacture
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/20—Metallic material, boron or silicon on organic substrates
    • C23C14/205—Metallic material, boron or silicon on organic substrates by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering

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Abstract

The invention discloses a preparation method of a highly ordered and axisymmetric nano periodic structure, which belongs to the technical field of nano structure conversion and composite material synthesis. The method is different from the traditional physical method and chemical corrosion method, is a brand-new method for preparing the nano periodic structure, and is expected to be applied to the preparation of more interesting periodic structures.

Description

Preparation method of highly-ordered and axisymmetric nano periodic structure
Technical Field
The invention belongs to the technical field of nano-structure conversion and composite material synthesis, and particularly relates to a method for designing and preparing a highly ordered and axisymmetric nano periodic structure.
Technical Field
The surface plasma regulation and control chemical reaction has wide application prospect in the research of plasma chemistry. The unique physical effects of surface plasmons, which are based on changes in the physical structure of nanomaterials. Magnetron sputtering is one of the means to modify existing structures. The optical performance of the nanometer material is enhanced by adjusting the sputtering condition to change the geometric parameters of the nanometer material structure. Meanwhile, the electric field intensity is regulated and controlled by adopting plasma-assisted chemistry, so that the nano particles grow at a specific position, and the optical performance is further improved. Because the distribution area of the local surface plasmon is very concentrated and the energy is high, the method is particularly suitable for controlling the chemical reaction at the nanometer scale. The distribution of localized surface-based plasmons is very sensitive to their structure, so researchers have been working on achieving microstructure tuning by changing the structure.
Disclosure of Invention
The invention takes the Au nanometer bowl as a basic structure, regulates and controls the hot spot distribution of the Au nanometer bowl through incident light, realizes the control of the growth position and the size of the silver nanometer particles, and prepares a nanometer annular periodic structure consisting of highly ordered and regionally grown silver nanometer particles.
The preparation method comprises the following specific steps:
1) preparing a highly ordered polystyrene bead array by a self-assembly method;
1a) and cleaning the silicon wafer. And putting the silicon wafer into a beaker, and adding a mixed solution of ammonia water, hydrogen peroxide and deionized water in a volume ratio of 1:2:6 into the beaker respectively. And (3) placing the beaker on a scorching table, heating to boil, keeping for 5-10 min, cooling, pouring out the liquid, and repeatedly performing ultrasonic treatment for 15min by using deionized water and absolute ethyl alcohol in sequence.
1b) An array of hexagonal close-packed polystyrene spheres was prepared. Mixing polystyrene pellets with the diameter of 500nm and absolute ethyl alcohol according to the volume ratio of 1:1, then uniformly dispersing the polystyrene pellets through ultrasonic treatment, dripping the dispersed polystyrene pellets on a large silicon wafer by using a liquid transfer gun to uniformly distribute dispersion liquid on the silicon wafer, slowly and obliquely sliding the large silicon wafer into a vessel with a stable liquid surface to form a closely-arranged polystyrene pellet array on the water surface, finally slowly fishing up the pellet array floating on the water surface by using the cleaned silicon wafer, and absorbing water and drying for later use.
2) Etching the highly ordered polystyrene bead array for 1min by using a plasma etcher with volume ratio of etching gas of O2Reducing the diameter of the etched polystyrene spheres from 500nm to 460nm by mixed gas with Ar being 4:1, then carrying out colloid particle separation, and separating the etched polystyrene sphere array;
3) and forming a spherical coated array structure on the surface of the polystyrene bead array by vertically sputtering a metal material with the thickness of 320nm on the surface of the polystyrene bead array by magnetron sputtering. In this example, Au is used as an example, and the sputtering power is 25W, and the degree of vacuum is 2X 10-4The flow of argon gas is introduced to be 20sccm under the high vacuum condition, the sputtering is performed perpendicular to the etched polystyrene bead array for 8min, and the Au obtained in the embodiment can be replaced by Ag or other metal materials, but the corresponding sputtering condition is changed in the future.
4) Transferring the sputtered sample to the surface of an adhesive tape by using the adhesive tape, enabling the small holes to face upwards and exposing partial polystyrene spheres;
5) putting the adhesive tape sample obtained by sticking into a tetrahydrofuran solution, and dissolving and removing the polystyrene spheres to obtain a nanometer bowl sample adhered on the adhesive tape;
6) the size of the particles is 2 x 2cm2Putting the nanometer bowl sample into silver nitrate 1 multiplied by 10 in an inverted way-2mol/L and 3.5X 10 sodium citrate-3In the mixed solution of mol/L, and performing illumination. The light source is a white LED lamp, the power is 3W, the distance from the sample is 5cm, and the illumination reaction time is 5And min, finally obtaining a highly ordered and axisymmetric nano periodic structure.
The invention has the beneficial effects that:
the preparation of the periodic structure is different from the traditional physical method and chemical corrosion method, is a brand-new preparation method of the nano periodic structure, and innovatively applies the local surface plasma to the structure preparation through the combination of etching and sputtering. The preparation method is expected to be applied to preparation of more interesting periodic structures.
Drawings
Figure 1 nano etched jar structure
FIG. 2 shows a six-axis symmetrical structure generated at the neck of a gold nano-jar
Detailed Description
The preparation method of the structure comprises the following specific steps:
1) preparing a highly ordered polystyrene bead array by a self-assembly method;
1a) and cleaning the silicon wafer. And putting the silicon wafer into a beaker, and adding a mixed solution of ammonia water, hydrogen peroxide and deionized water in a volume ratio of 1:2:6 into the beaker respectively. And (3) placing the beaker on a scorching table, heating to boil, keeping for 5-10 min, cooling, pouring out the liquid, and repeatedly performing ultrasonic treatment for 15min by using deionized water and absolute ethyl alcohol in sequence.
1b) An array of hexagonal close-packed polystyrene spheres was prepared. Mixing polystyrene pellets with the diameter of 500nm and absolute ethyl alcohol according to the volume ratio of 1:1, then uniformly dispersing the polystyrene pellets through ultrasonic treatment, dripping the dispersed polystyrene pellets on a large silicon wafer by using a liquid transfer gun to uniformly distribute dispersion liquid on the silicon wafer, slowly and obliquely sliding the large silicon wafer into a vessel with a stable liquid surface to form a closely-arranged polystyrene pellet array on the water surface, finally slowly fishing up the pellet array floating on the water surface by using the cleaned silicon wafer, and absorbing water and drying for later use.
2) Etching the highly ordered polystyrene bead array for 1min by using a plasma etcher with volume ratio of etching gas of O2Ar is mixed gas of 4:1, the diameter of the etched polystyrene spheres is 500Reducing the nm to 460nm, then carrying out colloid particle separation, and separating the etched polystyrene bead array;
3) and forming a spherical coated array structure on the surface of the polystyrene bead array by vertically sputtering a metal material with the thickness of 320nm on the surface of the polystyrene bead array by magnetron sputtering. In this example, Au is used as an example, and the sputtering power is 25W, and the degree of vacuum is 2X 10-4The sputtering time is 8min, the Au obtained in the embodiment can also be replaced by Ag or other metal materials, but the corresponding sputtering conditions are changed in the future.
4) Transferring the sputtered sample to the surface of the adhesive tape by using the adhesive tape, enabling the small holes to face upwards and exposing partial polystyrene spheres
5) Putting the adhesive tape sample obtained by sticking into a tetrahydrofuran solution, and dissolving and removing the polystyrene spheres; obtaining a nanometer bowl sample adhered on the adhesive tape (as shown in figure 1);
6) the size of the particles is 2 x 2cm2Putting the nanometer bowl sample into silver nitrate 1 multiplied by 10 in an inverted way-2mol/L and 3.5X 10 sodium citrate-3In the mixed solution of mol/L, and performing illumination. The light source is a white LED lamp, the power is 3W, the distance from the sample is 5cm, the illumination reaction time is 5min, and finally, a highly-ordered and axisymmetric nano periodic structure is obtained (as shown in figure 2).

Claims (4)

1. A method for preparing a highly ordered and axisymmetric nano periodic structure comprises the following specific steps:
1) preparing a highly ordered polystyrene bead array by a self-assembly method;
2) etching the highly ordered polystyrene bead array for 1min by using a plasma etcher with volume ratio of etching gas of O2Reducing the diameter of the etched polystyrene spheres from 500nm to 460nm by mixed gas with Ar being 4:1, then carrying out colloid particle separation, and separating the etched polystyrene sphere array;
3) and forming a spherical coated array structure on the surface of the polystyrene bead array by vertically sputtering a metal material with the thickness of 320nm on the surface of the polystyrene bead array by magnetron sputtering.
4) Transferring the sputtered sample to the surface of the adhesive tape by using the adhesive tape, enabling the small holes to face upwards and exposing partial polystyrene spheres
5) Putting the adhesive tape sample obtained by sticking into a tetrahydrofuran solution, and dissolving and removing the polystyrene spheres to obtain a nanometer bowl sample adhered on the adhesive tape;
6) the size of the particles is 2 x 2cm2Putting the nanometer bowl sample into silver nitrate 1 multiplied by 10 in an inverted way-2mol/L and 3.5X 10 sodium citrate- 3In the mixed solution of mol/L, and illuminating; the light source is a white LED lamp, the power is 3W, the distance from the light source to the sample is 5cm, the illumination reaction time is 5min, and finally the highly-ordered and axisymmetric nano periodic structure is obtained.
2. The method for preparing highly ordered and axisymmetric nano-periodic structure according to claim 1, wherein the step 1) comprises the following steps:
1a) and cleaning the silicon wafer. And putting the silicon wafer into a beaker, and adding a mixed solution of ammonia water, hydrogen peroxide and deionized water in a volume ratio of 1:2:6 into the beaker respectively. And (3) placing the beaker on a scorching table, heating to boil, keeping for 5-10 min, cooling, pouring out the liquid, and repeatedly performing ultrasonic treatment for 15min by using deionized water and absolute ethyl alcohol in sequence.
1b) An array of hexagonal close-packed polystyrene spheres was prepared. Mixing polystyrene pellets with the diameter of 500nm and absolute ethyl alcohol according to the volume ratio of 1:1, then uniformly dispersing the polystyrene pellets through ultrasonic treatment, dripping the dispersed polystyrene pellets on a large silicon wafer by using a liquid transfer gun to uniformly distribute dispersion liquid on the silicon wafer, slowly and obliquely sliding the large silicon wafer into a vessel with a stable liquid surface to form a closely-arranged polystyrene pellet array on the water surface, finally slowly fishing up the pellet array floating on the water surface by using the cleaned silicon wafer, and absorbing water and drying for later use.
3. The method for preparing the periodic wavy nanopore structure array according to claim 1, wherein the sputtering material in step 3) and step 5) is Au.
4. The method for preparing the periodic wavy nanopore structure array according to claim 3, wherein the sputtering power in step 3) is 25W, and the vacuum degree is 2 x 10-4Introducing argon gas with the flow rate of 20sccm under the high vacuum condition of Pa, sputtering perpendicularly to the etched polystyrene small ball array for 8min, wherein the sputtering thickness is 320 nm.
CN201910870299.9A 2019-09-16 2019-09-16 Preparation method of highly-ordered and axisymmetric nano periodic structure Pending CN110668395A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113652689A (en) * 2021-08-03 2021-11-16 杭州电子科技大学 Construction method of curved honeycomb array and application of curved honeycomb array
CN116285989A (en) * 2022-12-15 2023-06-23 浙江大学杭州国际科创中心 Rare earth doped nanocomposite and preparation method and application thereof

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CN103626119A (en) * 2013-12-08 2014-03-12 中国科学院光电技术研究所 Preparation method of nano metal ball bowl array structure
CN105973867A (en) * 2016-05-06 2016-09-28 厦门大学 Metalloid-metal composite hollow cavity array structure and preparation method thereof
CN106770165A (en) * 2016-12-22 2017-05-31 吉林大学 Surface enhanced Raman substrate prepared based on the reaction of surface plasma body resonant vibration induced chemical and preparation method thereof
CN109440072A (en) * 2018-11-23 2019-03-08 杭州电子科技大学 A kind of novelty nanometer periodic array and preparation method thereof
CN109592635A (en) * 2019-01-22 2019-04-09 杭州电子科技大学 A kind of method of controllable preparation composite nano figure line array
US20190178801A1 (en) * 2016-04-19 2019-06-13 University Of Florida Research Foundation, Inc. Surface plasmon-mediated chemical deposition and plasmonic structures

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050224779A1 (en) * 2003-12-11 2005-10-13 Wang Zhong L Large scale patterned growth of aligned one-dimensional nanostructures
CN103626119A (en) * 2013-12-08 2014-03-12 中国科学院光电技术研究所 Preparation method of nano metal ball bowl array structure
US20190178801A1 (en) * 2016-04-19 2019-06-13 University Of Florida Research Foundation, Inc. Surface plasmon-mediated chemical deposition and plasmonic structures
CN105973867A (en) * 2016-05-06 2016-09-28 厦门大学 Metalloid-metal composite hollow cavity array structure and preparation method thereof
CN106770165A (en) * 2016-12-22 2017-05-31 吉林大学 Surface enhanced Raman substrate prepared based on the reaction of surface plasma body resonant vibration induced chemical and preparation method thereof
CN109440072A (en) * 2018-11-23 2019-03-08 杭州电子科技大学 A kind of novelty nanometer periodic array and preparation method thereof
CN109592635A (en) * 2019-01-22 2019-04-09 杭州电子科技大学 A kind of method of controllable preparation composite nano figure line array

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113652689A (en) * 2021-08-03 2021-11-16 杭州电子科技大学 Construction method of curved honeycomb array and application of curved honeycomb array
CN116285989A (en) * 2022-12-15 2023-06-23 浙江大学杭州国际科创中心 Rare earth doped nanocomposite and preparation method and application thereof

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