CN106220237A - A kind of preparation method of monolayer ordered silica nanosphere array - Google Patents

A kind of preparation method of monolayer ordered silica nanosphere array Download PDF

Info

Publication number
CN106220237A
CN106220237A CN201610565422.2A CN201610565422A CN106220237A CN 106220237 A CN106220237 A CN 106220237A CN 201610565422 A CN201610565422 A CN 201610565422A CN 106220237 A CN106220237 A CN 106220237A
Authority
CN
China
Prior art keywords
sio
monolayer
nanosphere
array
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610565422.2A
Other languages
Chinese (zh)
Inventor
梁继然
李景朋
宋晓龙
周立伟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tianjin University
Original Assignee
Tianjin University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tianjin University filed Critical Tianjin University
Priority to CN201610565422.2A priority Critical patent/CN106220237A/en
Publication of CN106220237A publication Critical patent/CN106220237A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5072Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with oxides or hydroxides not covered by C04B41/5025
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/60After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
    • C04B41/61Coating or impregnation
    • C04B41/65Coating or impregnation with inorganic materials

Abstract

The invention discloses the preparation method of a kind of monolayer ordered silica nanosphere array, have steps of: the cleaning of sapphire substrates;The cleaning of drainage piece;Monolayer SiO2The preparation of nanosphere: taking out drainage piece, oblique cutting enters in a certain amount of deionized water, the SiO that will again prepare2Ethanol solution is added drop-wise on drainage piece, forms monolayer SiO2Array, thus be configured to lift liquid;Standing is after liquid level stabilizing, with plated film pulling machine by Al2O3Substrate lifts, and stands and treats Al2O3Substrate is dried, at Al2O3Substrate is the formation of monolayer SiO2Nanosphere array.The present invention uses drain dispersion czochralski method at room temperature to prepare monolayer ordered silica nanosphere array, prepared SiO2Nanosphere array monolayer and dense arrangement, can carry out subsequent technique as mask plate and prepare large area cycle ordered nano array of particles, carry out preparation and the research of biochip, optics and nano-device, and the required cycle is short, low cost.

Description

A kind of preparation method of monolayer ordered silica nanosphere array
Technical field
The present invention relates to nanostructured prepare, particularly relate to a kind of system based on monolayer ordered silica nanosphere array Preparation Method.
Background technology
Along with the development of science and technology, to requirements such as the complexities of function, reliability and the structure of ultra-precision device It is more and more higher, so that electronic device trends towards miniaturization.Along with the demand of device miniaturization, particularly to nano-device, The requirement of the nanorize of the aspects such as optics, biochip and high sensor is increasingly stronger, micro-nano processing Method causes the concern of people more and more, and the core of nanometer technique is micro-nano process technology.Micro-nano process technology As causing the science and technology of a new Industrial Revolution, enjoy and catch people's attention.In order to the performance of systematic research device And put into commercial production, nano fabrication technique must be low cost, can change nano-particle shape flexibly, size and Interval and large-scale production.Up to the present, applying most common nano fabrication technique is exactly photoetching technique, but the spreading out of λ/2 Emitter-base bandgap grading limits photoetching technique application in prepared by nanometer.Wherein, beamwriter lithography is serial process pattern and precision height Can be good at controlling nano-particle geomery, but this technical costs is high and volume of production is low.X-ray lithography technology has also But row process pattern and have high volume of production cost the highest.By precision and the X-ray lithography technology of electron beam lithography Parallel processing capability combine, be developed the nanoimprinting technology of PSTM, but its parallel processing Ability still deficiency.Therefore, the nanometer etching technology that parallel processing capability is strong and cheap is one of research emphasis of nano science. Nanosphere lithography technique (Nanosphere lithography, NSL) is a kind of parallel self assembly side preparing nano-dot matrix Method, the instrument and equipment that the maximum feature of this method is exactly required is the cheapest, and technological operation is simple.Have only to change the straight of nanosphere Footpath just can obtain various sizes of large area cyclic array on various substrates.One committed step of this technology is received exactly The regularity of rice ball mask layer arrangement, owing to being affected by environment and various preparation condition, nanosphere mask layer neat Property there is great uncertainty, find appropriate preparation flow and preparation condition be solve nanosphere mask layer arrangement the most whole Neat key.
Summary of the invention
In order to solve the problems of the prior art, the present invention provides the system of a kind of monolayer ordered silica nanosphere array Preparation Method, solves the problem that in prior art, in Nanosphere lithography technique, nanosphere mask layer arranges non-regularity.
The technical scheme is that the preparation method of a kind of monolayer ordered silica nanosphere array, have following Step:
(1) cleaning of sapphire substrates;
(2) cleaning of drainage piece;
(3) monolayer SiO2The preparation of nanosphere:
The SiO bought2Nanosphere is immersed in dehydrated alcohol and deposits;The SiO that will buy during use2Nanosphere dehydrated alcohol Original solution and dehydrated alcohol carry out dosing again, then take out drainage piece with tweezers, and oblique cutting enters in a certain amount of deionized water, so The SiO that rear use liquid-transfering gun will prepare again2-ethanol solution is added drop-wise on drainage piece, and makes it slowly flow to the water surface On, uniform spreading launches to come, and forms high density, large-area monolayer SiO2Array, thus be configured to lift liquid;Standing treats that liquid level is steady After Ding, with plated film pulling machine lentamente by Al2O3Substrate is immersed in lifting liquid, and vertically and lentamente lifts out liquid level, lifting Speed is chosen between 10-180 μm/min according to experiment demand, waits the Al of submergence2O3Substrate is gone out by lifting completely, and standing is treated Al2O3Substrate is dried, at Al2O3Substrate is the formation of monolayer SiO2Nanosphere array.
The cleaning of described step (1) sapphire substrates refers to: sapphire sheet is sequentially placed into deionized water, acetone and nothing Ultrasonic cleaning respectively in water-ethanol, removes the organic impurities on surface;It is washed with deionized water clean again, finally sapphire substrate is put into In dehydrated alcohol standby.
The cleaning of described step (2) drainage piece refers to: drainage piece used is common microscope slide;Microscope slide is put successively Enter ultrasonic cleaning respectively in deionized water, acetone and dehydrated alcohol, remove the organic impurities on surface;It is washed with deionized water again Only, finally microscope slide is put in dehydrated alcohol standby.
Described step (3) SiO2A diameter of 300nm-600nm of nanosphere.
Described step (3) SiO2Nanosphere dehydrated alcohol original solution and dehydrated alcohol dosing ratio are 1:3-1:8.
The lifting filming equipment of described step (3) is ZR-4200 type plated film pulling machine.
The invention has the beneficial effects as follows: monolayer ordered arrangement SiO prepared by (1)2The method of nanosphere is relatively simple, is controlled The process conditions of system are few and easily controllable.
(2) a kind of monolayer ordered arrangement SiO is provided2The preparation method of nanosphere, repeatable high, it is suitable for high-volume raw Produce.
The present invention uses drain dispersion czochralski method at room temperature to prepare monolayer ordered silica nanosphere array, prepared SiO2Nanosphere array monolayer and dense arrangement, can carry out subsequent technique as mask plate and prepare the large area cycle and receive in order Rice grain array, carries out preparation and the research of biochip, optics and nano-device, and the required cycle is short, cost Low.
Accompanying drawing explanation
Fig. 1 (a)-(d) is the operational flowchart of drain dispersion czochralski method;
Fig. 2 (a)-(c) be a diameter of 600nm pull rate be the SiO prepared by 100 μm/min2Nanosphere array SEM Figure;
Fig. 3 be a diameter of 600nm pull rate be the SiO prepared by 130 μm/min2Nanosphere array SEM schemes;
Fig. 4 be a diameter of 300nm pull rate be the SiO prepared by 30 μm/min2Nanosphere array SEM schemes;
Fig. 5 be a diameter of 300nm pull rate be the SiO prepared by 20 μm/min2Nanosphere array SEM schemes.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail.
The present invention is raw materials used all uses commercially available chemically pure reagent.
Embodiment 1
(1) sapphire cleans
Sapphire used is the sapphire of double polishings of (0001) crystal face commercially bought, and thickness is 0.45mm, chi Very little 1cm*1cm.Sapphire sheet is once put into difference ultrasonic cleaning 20 minutes in deionized water, acetone and dehydrated alcohol, goes out Remove the organic impurities on surface;It is washed with deionized water clean again, finally sapphire substrate is put in dehydrated alcohol standby.
(2) cleaning of drainage piece
Drainage piece used is common microscope slide.Microscope slide is sequentially placed into deionized water, acetone and dehydrated alcohol Middle ultrasonic cleaning 20 minutes respectively, remove the organic impurities on surface;It is washed with deionized water clean again, finally microscope slide is put into anhydrous In ethanol standby.
(3) monolayer SiO2The preparation of nanosphere
The SiO of the diameter 600nm bought2Nanosphere is immersed in dehydrated alcohol and deposits, and density is 0.17g/ml.During use The SiO that will buy2Nanosphere dehydrated alcohol original solution and dehydrated alcohol, with the ratio dosing again of 1:6, then take out with tweezers Drainage piece, oblique cutting enters in a certain amount of deionized water, then uses the SiO that liquid-transfering gun will prepare again2-ethanol solution Being added drop-wise on drainage piece, and make it slowly flow on the water surface, uniform spreading launches to come, and forms high density, large-area monolayer SiO2 Array, thus be configured to lift liquid.Standing is after liquid level stabilizing, with plated film pulling machine lentamente by Al2O3Substrate is immersed in lifting In liquid, and vertically and lentamente lift out liquid level, pull rate 100 μm/min, wait the Al of submergence2O3Substrate is lifted completely Going out, standing a few minutes treat Al2O3Substrate is dried, at Al2O3Substrate is the formation of monolayer SiO2Nanosphere array, preparation orderly SiO2Nanosphere array is as shown in Figure 2.
A diameter of 600nm of the nanosphere that embodiment 1 prepares, arrangement that nanosphere is dense, above ground floor nanosphere There is second layer nanosphere in occasional, and this can ignore from the point of view of preparing nanostructured utilizing monolayer nanosphere.
Embodiment 2
The present embodiment is similar to Example 1, and difference is: in step (3), pull rate is 130 μm/min.Made The SiO obtained2The loose arrangement of nanosphere array.
Embodiment 3
The present embodiment is similar to Example 1, and difference is: SiO in step (3)2Nanosphere dehydrated alcohol original solution With dehydrated alcohol with the ratio dosing again of 1:3.Use the SiO that liquid-transfering gun will prepare again2-ethanol solution is added drop-wise to On drainage piece, and it is made slowly to flow on the water surface, SiO in the lifting liquid being configured to2Nanosphere is condensed into bulk, sprawls inequality Even, with plated film pulling machine lentamente by Al2O3Substrate is immersed in lifting liquid, and vertically and lentamente lifts out liquid level, has lifted At Al after Biing2O3On be easily formed multilamellar SiO2Nanosphere.
Embodiment 4
The present embodiment is similar to Example 1, and difference is: SiO in step (3)2Nanosphere dehydrated alcohol original solution With dehydrated alcohol with the ratio dosing again of 1:8.Use the SiO that liquid-transfering gun will prepare again2-ethanol solution is added drop-wise to On drainage piece, and it is made slowly to flow on the water surface, SiO in the lifting liquid being configured to2Nanosphere is difficult to condense film forming, uses plated film Pulling machine is lentamente by Al2O3Substrate is immersed in lifting liquid, and vertically and lentamente lifts out liquid level, lift complete after exist Al2O3Upper SiO without monolayer2Nanosphere array is formed.
Embodiment 5
The present embodiment and example 1 difference are the SiO of a diameter of 300nm of nanosphere used2Nanosphere, lifting speed Spend 30 μm/min.Obtained nanosphere array arrangement closely and almost monolayer nanosphere.
Embodiment 6
The present embodiment is similar to Example 5, and difference is that pull rate is 20 μm/min.Obtained nanometer spherical array Row fractional monolayer and dense, area has double-layer nanometer ball array.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For Yuan, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (6)

1. the preparation method of a monolayer ordered silica nanosphere array, it is characterised in that have steps of:
(1) cleaning of sapphire substrates;
(2) cleaning of drainage piece;
(3) monolayer SiO2The preparation of nanosphere:
The SiO bought2Nanosphere is immersed in dehydrated alcohol and deposits;The SiO that will buy during use2Nanosphere dehydrated alcohol is former molten Liquid and dehydrated alcohol carry out dosing again, then take out drainage piece with tweezers, and oblique cutting enters in a certain amount of deionized water, then makes The SiO that will again prepare with liquid-transfering gun2-ethanol solution is added drop-wise on drainage piece, and makes it slowly flow on the water surface, all Even sprawling is come, and forms high density, large-area monolayer SiO2Array, thus be configured to lift liquid;Standing after liquid level stabilizing, With plated film pulling machine lentamente by Al2O3Substrate is immersed in lifting liquid, and vertically and lentamente lifts out liquid level, pull rate Choose between 10-180 μm/min according to experiment demand, wait the Al of submergence2O3Substrate is gone out by lifting completely, stands and treats Al2O3 Substrate is dried, at Al2O3Substrate is the formation of monolayer SiO2Nanosphere array.
The preparation method of monolayer ordered silica nanosphere array the most according to claim 1, it is characterised in that described step Suddenly the cleaning of (1) sapphire substrates refers to: sapphire sheet is sequentially placed in deionized water, acetone and dehydrated alcohol and surpasses respectively Sound cleans, and removes the organic impurities on surface;It is washed with deionized water clean again, finally sapphire substrate is put in dehydrated alcohol standby With.
The preparation method of monolayer ordered silica nanosphere array the most according to claim 1, it is characterised in that described step Suddenly the cleaning of (2) drainage piece refers to: drainage piece used is common microscope slide;Microscope slide is sequentially placed into deionized water, third Ultrasonic cleaning respectively in ketone and dehydrated alcohol, removes the organic impurities on surface;It is washed with deionized water clean, finally by microscope slide again Put in dehydrated alcohol standby.
The preparation method of monolayer ordered silica nanosphere array the most according to claim 1, it is characterised in that described step Suddenly (3) SiO2A diameter of 300-600nm of nanosphere.
The preparation method of monolayer ordered silica nanosphere array the most according to claim 1, it is characterised in that described step Suddenly (3) SiO2Nanosphere dehydrated alcohol original solution and dehydrated alcohol dosing ratio are 1:3-1:8.
The preparation method of monolayer ordered silica nanosphere array the most according to claim 1, it is characterised in that described step Suddenly the lifting filming equipment of (3) is ZR-4200 type plated film pulling machine.
CN201610565422.2A 2016-07-15 2016-07-15 A kind of preparation method of monolayer ordered silica nanosphere array Pending CN106220237A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610565422.2A CN106220237A (en) 2016-07-15 2016-07-15 A kind of preparation method of monolayer ordered silica nanosphere array

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610565422.2A CN106220237A (en) 2016-07-15 2016-07-15 A kind of preparation method of monolayer ordered silica nanosphere array

Publications (1)

Publication Number Publication Date
CN106220237A true CN106220237A (en) 2016-12-14

Family

ID=57530930

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610565422.2A Pending CN106220237A (en) 2016-07-15 2016-07-15 A kind of preparation method of monolayer ordered silica nanosphere array

Country Status (1)

Country Link
CN (1) CN106220237A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106756813A (en) * 2016-12-18 2017-05-31 江苏师范大学 A kind of micro-nano motor and preparation method thereof
CN107604433A (en) * 2017-07-28 2018-01-19 华南师范大学 The preparation method of individual layer lattice
CN109013232A (en) * 2018-07-19 2018-12-18 燕山大学 The preparation method of automatically cleaning single layer Titanium dioxide spherical array wideband anti-reflection film
CN110434035A (en) * 2019-07-12 2019-11-12 天津大学 A kind of hydrophilic silicon oxides microballoon single layer period arrangement array and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103981488A (en) * 2014-05-23 2014-08-13 天津大学 Method for preparing vanadium oxide nanoparticle array by rapid heat treatment

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103981488A (en) * 2014-05-23 2014-08-13 天津大学 Method for preparing vanadium oxide nanoparticle array by rapid heat treatment

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106756813A (en) * 2016-12-18 2017-05-31 江苏师范大学 A kind of micro-nano motor and preparation method thereof
CN106756813B (en) * 2016-12-18 2018-12-14 江苏师范大学 A kind of micro-nano motor and preparation method thereof
CN107604433A (en) * 2017-07-28 2018-01-19 华南师范大学 The preparation method of individual layer lattice
CN109013232A (en) * 2018-07-19 2018-12-18 燕山大学 The preparation method of automatically cleaning single layer Titanium dioxide spherical array wideband anti-reflection film
CN110434035A (en) * 2019-07-12 2019-11-12 天津大学 A kind of hydrophilic silicon oxides microballoon single layer period arrangement array and preparation method thereof

Similar Documents

Publication Publication Date Title
Liang et al. Self‐assembly of colloidal spheres toward fabrication of hierarchical and periodic nanostructures for technological applications
CN102173376B (en) Preparation method for small silicon-based nano hollow array with orderly heights
CN102556952B (en) Metal cup-cylinder composite nano structure array and preparation method thereof
Qi et al. Simple approach to wafer-scale self-cleaning antireflective silicon surfaces
US9816176B2 (en) Preparation method for multi-layer metal oxide porous film nano gas-sensitive material
CN106220237A (en) A kind of preparation method of monolayer ordered silica nanosphere array
CN102530846B (en) Method for preparing metal nanobelt array with tip
CN102530845B (en) Method for preparing triangular metal nano-pore array
CN102923647A (en) Method for preparing ordered array of metal nano-particles with adjustable space and appearance
US8372752B1 (en) Method for fabricating ultra-fine nanowire
CN103933902B (en) A kind of binary ordered colloidal crystal, metal nano array and preparation method thereof
Tseng et al. Design and fabrication of vertically aligned single-crystalline Si nanotube arrays and their enhanced broadband absorption properties
CN104310304A (en) Preparation method of nano column array with controllable size and surface structure
CN102856434B (en) Preparation method for square silicon nano-porous array
CN106185792A (en) A kind of population parameter controllable method for preparing of super-hydrophobic micro-nano compound structure
CN103489753A (en) Method for manufacturing large-area small-size core-shell structure silicon nanowire array
CN116741896A (en) Submicron-order patterned sapphire substrate and preparation method thereof
CN104003354B (en) Aluminum nanometer particle size regulation method and application of aluminum nanometer particle size regulation method
Wu et al. The effects of Ag particle morphology on the antireflective properties of silicon textured using Ag-assisted chemical etching
CN111017869B (en) Silicon-based network structure and preparation method thereof
CN110540372B (en) Non-close-packed silicon dioxide ring nano array and preparation method thereof
CN108373136A (en) A kind of preparation method of the orderly polystyrene nanospheres template of non-solid matter
Li et al. Pattern transfer of hexagonal packed structure via ultrathin metal nanomesh masks for formation of Si nanopore arrays
Asoh et al. Pt–Pd-embedded silicon microwell arrays
Visser et al. Investigations of sol-gel ZnO films nanostructured by reactive ion beam etching for broadband anti-reflection

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20161214