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 PDFInfo
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- 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
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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
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.
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Cited By (5)
| 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 |
| US12011736B2 (en) | 2020-12-22 | 2024-06-18 | The Board Of Trustees Of The University Of Illinois | Methods and systems for large area and low defect monolayer ordering of microspheres and nanospheres |
Citations (1)
| 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 |
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2016
- 2016-07-15 CN CN201610565422.2A patent/CN106220237A/en active Pending
Patent Citations (1)
| 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 (6)
| 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 |
| US12011736B2 (en) | 2020-12-22 | 2024-06-18 | The Board Of Trustees Of The University Of Illinois | Methods and systems for large area and low defect monolayer ordering of microspheres and nanospheres |
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Application publication date: 20161214 |