CN109851832A - The method of the PS ball array of surface roughening is constructed on flexible substrates - Google Patents

The method of the PS ball array of surface roughening is constructed on flexible substrates Download PDF

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Publication number
CN109851832A
CN109851832A CN201811622327.7A CN201811622327A CN109851832A CN 109851832 A CN109851832 A CN 109851832A CN 201811622327 A CN201811622327 A CN 201811622327A CN 109851832 A CN109851832 A CN 109851832A
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ball
sheet glass
ball array
ultrasonic
flexible substrates
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CN201811622327.7A
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CN109851832B (en
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刘广强
张鹏
蔡伟平
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Hefei Institutes of Physical Science of CAS
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Hefei Institutes of Physical Science of CAS
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Abstract

The invention discloses the methods that one kind constructs the PS ball array of surface roughening on flexible substrates, comprising steps of the acquisition of ultra-clean substrate of glass;The acquisition of six side's solid matter single layer PS balls in flexible substrate;The acquisition of the PS ball array of surface roughening.Using the method for reactive ion etching, it is directly roughened PS ball surface on flexible substrates, has obtained a kind of PS ball array of surface presentation micro nano structure, the surface of the array has the feature of micro nano structure.Compare with other preparation methods, program production process is more simple, and surface topography is controllable, PS ball size is controllable, and ingredient is more uniform, and furthermore the flexible substrate can fold, it is easy to carry, cost it is more cheap and can large scale preparation, realize batch production manufacture.

Description

The method of the PS ball array of surface roughening is constructed on flexible substrates
Technical field
The present invention relates to a kind of PS ball surface roughening methods, more particularly to one kind to construct rough surface on flexible substrates The method of the PS ball array of change.
Background technique
The high molecular polymer that PS (polystyrene) ball is controllable as a kind of size, sphericity is high, since quilt After Vanderhoff and Brodford et al. synthesis discovery, just it is widely used in biomedical material, chemical material, energy Source tech materials etc..Since PS ball itself has preferable structural stability and chemical stability, thus it can be with resistance to one Determine the high temperature of degree, and more difficult to degrade in natural environment and organism, so materials synthesis is used as by vast researcher With modified presoma.At present about the method there are many synthesizing for preparing of PS ball, typically there are emulsion polymerization and suspension polymerisation Etc. schemes.In addition, the function dough about PS ball is also studied there are many researcher, such as hydroxyl is introduced in PS ball surface Base (- OH), carboxyl (- COOH), aldehyde radical (- CHO), sulfonic group (- SO3) etc..
But it is roughened at present about PS ball surface, and the scheme that micro-nano processing is presented is actually rare.Under normal circumstances, By adding other chemical materials and reacting under more harsh environment with PS ball, obtained surface topography is difficult to control, And it is excessive to introduce exogenous impurity.
Summary of the invention
The object of the present invention is to provide the methods that one kind constructs the PS ball array of surface roughening on flexible substrates.
The purpose of the present invention is what is be achieved through the following technical solutions:
The method of the PS ball array for constructing surface roughening on flexible substrates of the invention, comprising:
Step 1: the acquisition of ultra-clean substrate of glass;
Step 2: the acquisition of six side's solid matter single layer PS balls in flexible substrate;
Step 3: the acquisition of the PS ball array of surface roughening.
As seen from the above technical solution provided by the invention, provided in an embodiment of the present invention to construct on flexible substrates The method of the PS ball array of surface roughening, production process is more simple, and surface topography is controllable, and PS ball size is controllable, and Ingredient is more uniform, and furthermore the flexible substrate can fold, easy to carry, cost it is more cheap and can large scale preparation, it is real Now batch production manufacture.
Detailed description of the invention
Fig. 1 is the flexible substrate preparation flow signal that PS ball array surface micro-nano structure is roughened in the embodiment of the present invention Figure.
It in vacuum degree is 12Pa, sulfur hexafluoride gas flow velocity 65sccm, radio-frequency power 200w that Fig. 2, which is in the embodiment of the present invention, Under conditions of, the SEM photograph of different etching time.(a), (b), (c), (d), (e), (f) are that etch period is respectively in figure The SEM photograph that 30s, 60s, 90s, 120s, 150s, 180s are obtained.
Specific embodiment
The embodiment of the present invention will be described in further detail below.What is be not described in detail in the embodiment of the present invention is interior Appearance belongs to the prior art well known to professional and technical personnel in the field.
The method of the PS ball array for constructing surface roughening on flexible substrates of the invention, preferable specific embodiment party Formula is:
Include:
Step 1: the acquisition of ultra-clean substrate of glass;
Step 2: the acquisition of six side's solid matter single layer PS balls in flexible substrate;
Step 3: the acquisition of the PS ball array of surface roughening.
The step 1 includes:
Several sheet glass are put into beaker, acetone soln is added until submergence sheet glass, ultrasonic with ultrasonic machine;Pour out third Ketone solution is added alcohol and submerges sheet glass, with ultrasonic machine ultrasound;Alcohol is poured out, deionized water is added, pours out deionization after ultrasound Water, each ultrasonic time should be no less than half an hour;
Until submerging sheet glass, later in beaker before hydrogen peroxide and the concentrated sulfuric acid are successively poured into according to volume ratio 1: 3 Ultrasonic 1h pours out waste liquid after standing 12h, after sufficiently washing away waste liquid with deionized water, then by deionized water, ammonium hydroxide, dioxygen Water successively pours into beaker according to volume ratio 3: 1: 1, until submergence sheet glass, ultrasound are poured out waste liquid after two hours, finally filled Deionized water submerges sheet glass, and ultrasonic 2h obtains ultra-clean sheet glass, since ultrasonic time is longer during being somebody's turn to do, usually in ultrasound Machine is put into several ice bags when operating.
The step 2 includes:
Required several sheet glass are put into baking oven, certain temperature is adjusted and carries out drying and processing;
Then, sheet glass is put into ozone clean machine and carries out cleaning a period of time, directly added in glass sheet surface later Enter one layer of deionization moisture film, take out 500nm PS ball with liquid-transfering gun and high-purity alcohol is several, and by the above two according to certain ratio Example is mixed to get mixed liquor and is placed in 2ml test tube, with stand-by after ultrasonic machine ultrasound;
It mixed liquor with liquid-transfering gun is slowly injected into moisture film can be obtained and obtain one or more layers PS ball film on liquid level, to It is dried;
Water will be filled in beaker, and surfactant is added, PS ball film is transferred on the water surface later, is fished out with PE film It rises, six side's solid matters can be obtained on flexible substrates and obtain single layer PS ball array.
The step 3 includes:
Will prepare before with single layer PS ball film PE film merging reactive ion etching instrument in, first with mechanical pump by its Vacuum degree is extracted into lower level, and vacuum degree is extracted into 0.3Pa with molecular pump again later, after vacustat, opens hexafluoro Change sulphur air valve, by flow control to 65sccm, and slowly adjust intake valve, until vacuum degree goes back up to 12Pa, to sulfur hexafluoride After air-flow velocity is gradually stable, adjusts radio-frequency power and arrive 200w, each etch period changes by 30s to 180s, every minor tick 30s;
After the completion of etching, all air valves are closed, N is passed through2It is restored to normal atmosphere (An) to vacuum degree, when can be obtained different Between the lower roughened PS ball array of reactive ion etching flexible substrate, micro nano structure feature is presented in surface.
The method of the PS ball array for constructing surface roughening on flexible substrates of the invention, utilizes reactive ion etching Method is directly roughened PS ball surface on flexible substrates, has obtained a kind of PS ball array of surface presentation micro nano structure, should The surface of array has the feature of micro nano structure.Compare with other preparation methods, program production process is more simple, table Face morphology controllable, PS ball size is controllable, and ingredient is more uniform, and furthermore the flexible substrate can fold, easy to carry, at This it is more cheap and can large scale preparation, realize batch production manufacture.
The first problem that the present invention solves is to be prepared for that a kind of surface is smooth, size is controllable on a glass substrate PS ball array.
The Second Problem that the present invention solves is that the array of the PS ball in glass substrate is transferred to on PE film, is obtained A kind of PS ball array in flexible substrate, and the substrate can fold, easy to carry, furthermore cost is more cheap, can advise greatly Mould preparation, batch production.
The third problem that the present invention solves is the method for directly utilizing reactive ion etching method, obtains roughened PS ball The surface of array, the array has micro nano structure feature, will not substantially introduce exogenous impurity, thus ingredient is more uniform.
Specific embodiment, as shown in Figure 1 and Figure 2, comprising steps of
Step 1: the acquisition of ultra-clean substrate of glass.Several sheet glass are put into beaker, acetone soln is added until leaching No sheet glass, with ultrasonic machine ultrasound;Acetone soln is poured out, alcohol is added and submerges sheet glass, with ultrasonic machine ultrasound;Alcohol is poured out, Deionized water is added, pours out deionized water after ultrasound.Each ultrasonic time should be no less than half an hour.Hydrogen peroxide and the concentrated sulfuric acid are pressed Until submergence sheet glass, ultrasound 1h, pours out waste liquid after standing 12h later in beaker before successively being poured into according to volume ratio 1: 3, use After deionized water sufficiently washes away waste liquid, deionized water, ammonium hydroxide, hydrogen peroxide are successively then poured into burning according to volume ratio 3: 1: 1 In cup, until submergence sheet glass, ultrasound poured out waste liquid after two hours, deionized water submergence sheet glass is finally filled, ultrasonic 2h is obtained To ultra-clean sheet glass.Since ultrasonic time is longer, several ice bags usually are put into when ultrasonic machine operates.
Step 2: the acquisition of six side's solid matter single layer PS balls in flexible substrate.Required several sheet glass are put into baking oven In, it adjusts certain temperature and carries out drying and processing.Then, sheet glass is put into ozone clean machine and carries out cleaning a period of time, It is directly added into one layer of deionization moisture film in glass sheet surface later, if taking out 500nm PS ball and high-purity alcohol with liquid-transfering gun It is dry, and the above two are mixed to get mixed liquor according to a certain percentage and is placed in 2ml test tube, with stand-by after ultrasonic machine ultrasound.It will mix It closes liquid and slowly injects moisture film with liquid-transfering gun and can be obtained and obtain PS ball film (general multilayer) on liquid level, to its drying.It will burn Water is filled in cup, a certain amount of surfactant is added, PS ball film is transferred on the water surface later, is picked up with PE film, Six side's solid matters can be obtained on flexible substrates obtains single layer PS ball array.
Step 3: the acquisition of the PS ball array of surface roughening.The PE film with single layer PS ball film will be prepared before It is placed in reactive ion etching instrument, its vacuum degree is first extracted into lower level with mechanical pump, later again with molecular pump by vacuum Degree is extracted into 0.3Pa, after vacustat, opens sulfur hexafluoride air valve, by flow control to 65sccm, and slowly adjusts air inlet Valve, until vacuum degree goes back up to 12Pa or so, after sulfur hexafluoride air-flow velocity is gradually stable, adjusting radio-frequency power to 200w, Each etch period variation is by 30s to 180s, every minor tick 30s.After the completion of etching, all air valves are closed, N is passed through2To vacuum Degree is restored to normal atmosphere (An), and the flexible substrate of the roughened PS ball array of reactive ion etching under different time can be obtained, Micro nano structure feature is presented in surface.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, Within the technical scope of the present disclosure, any changes or substitutions that can be easily thought of by anyone skilled in the art, It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims Subject to enclosing.

Claims (4)

1. the method that one kind constructs the PS ball array of surface roughening on flexible substrates characterized by comprising
Step 1: the acquisition of ultra-clean substrate of glass;
Step 2: the acquisition of six side's solid matter single layer PS balls in flexible substrate;
Step 3: the acquisition of the PS ball array of surface roughening.
2. the method for the PS ball array according to claim 1 for constructing surface roughening on flexible substrates, feature exist In the step 1 includes:
Several sheet glass are put into beaker, acetone soln is added until submergence sheet glass, ultrasonic with ultrasonic machine;It is molten to pour out acetone Liquid is added alcohol and submerges sheet glass, with ultrasonic machine ultrasound;Alcohol is poured out, deionized water is added, pours out deionized water after ultrasound, Each ultrasonic time should be no less than half an hour;
Until submergence sheet glass, ultrasonic later in beaker before hydrogen peroxide and the concentrated sulfuric acid are successively poured into according to volume ratio 1: 3 1h pours out waste liquid after standing 12h, after sufficiently washing away waste liquid with deionized water, then presses deionized water, ammonium hydroxide, hydrogen peroxide Successively poured into beaker according to volume ratio 3: 1: 1, until submergence sheet glass, ultrasound two hours after pour out waste liquid, finally fill from Sub- water immersion sheet glass, ultrasonic 2h obtain ultra-clean sheet glass, since ultrasonic time is longer during being somebody's turn to do, usually transport in ultrasonic machine Several ice bags are put into when turning.
3. the method for the PS ball array according to claim 2 for constructing surface roughening on flexible substrates, feature exist In the step 2 includes:
Required several sheet glass are put into baking oven, certain temperature is adjusted and carries out drying and processing;
Then, sheet glass is put into ozone clean machine and carries out cleaning a period of time, be directly added into one in glass sheet surface later Layer deionization moisture film takes out 500nm PS ball with liquid-transfering gun and high-purity alcohol is several, and the above two are mixed according to a certain percentage Conjunction obtains mixed liquor and is placed in 2ml test tube, with stand-by after ultrasonic machine ultrasound;
It mixed liquor with liquid-transfering gun is slowly injected into moisture film can be obtained and obtain one or more layers PS ball film on liquid level, it is dry to it It is dry;
Water will be filled in beaker, and surfactant is added, PS ball film is transferred on the water surface later, is picked up with PE film, Six side's solid matters can be obtained on flexible substrates obtains single layer PS ball array.
4. the method for the PS ball array according to claim 3 for constructing surface roughening on flexible substrates, feature exist In the step 3 includes:
It will prepare before in the PE film merging reactive ion etching instrument with single layer PS ball film, first with mechanical pump by its vacuum Degree is extracted into lower level, and vacuum degree is extracted into 0.3Pa with molecular pump again later, after vacustat, opens sulfur hexafluoride Air valve by flow control to 65sccm, and slowly adjusts intake valve, until vacuum degree goes back up to 12Pa, to sulfur hexafluoride air-flow After flow velocity is gradually stable, adjusts radio-frequency power and arrive 200w, each etch period changes by 30s to 180s, every minor tick 30s;
After the completion of etching, all air valves are closed, N is passed through2It is restored to normal atmosphere (An) to vacuum degree, can be obtained under different time Micro nano structure feature is presented in the flexible substrate of the roughened PS ball array of reactive ion etching, surface.
CN201811622327.7A 2018-12-28 2018-12-28 Method for constructing surface roughened PS ball array on flexible substrate Active CN109851832B (en)

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DE102011112696A1 (en) * 2011-08-31 2013-02-28 Martin-Luther-Universität Halle-Wittenberg Film for back contact of solar cell utilized for power production, has conductive diffractive optical structure comprising photonic crystal, where structure is arranged on flexible conductive substrate, which comprises metallization part
CN103515484A (en) * 2013-09-13 2014-01-15 南开大学 Textured transparent conductive thin film with periodic structure and preparation method thereof
CN105206175A (en) * 2015-10-23 2015-12-30 浙江大学 Anti-counterfeit label based on patterned metal nanocomposite and production method of anti-counterfeit label
CN106277822A (en) * 2016-07-28 2017-01-04 李志刚 Silicon nanometer column array material and preparation method thereof
CN107101988A (en) * 2017-03-16 2017-08-29 中国科学院合肥物质科学研究院 A kind of high density nanometer pinpoint array of golden film covering and its application
CN108046211A (en) * 2017-11-23 2018-05-18 中国科学院合肥物质科学研究院 A kind of preparation method and applications of silicon substrate thorniness shape nanocone oldered array
CN108417650A (en) * 2018-04-03 2018-08-17 芜湖孺子牛节能环保技术研发有限公司 A kind of amorphous silicon membrane improving solar cell photoelectric transformation efficiency
CN108594288A (en) * 2018-04-25 2018-09-28 西北核技术研究所 A kind of surface has the plastic scintillant and preparation method thereof of microlens array
CN108754418A (en) * 2018-06-28 2018-11-06 吉林大学 Self-supporting chiral nano hollow cone array film with chiral optical rotation property and preparation method thereof

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101497429A (en) * 2009-03-06 2009-08-05 吉林大学 Method for preparing silicon hollow nano-cone array
DE102011112696A1 (en) * 2011-08-31 2013-02-28 Martin-Luther-Universität Halle-Wittenberg Film for back contact of solar cell utilized for power production, has conductive diffractive optical structure comprising photonic crystal, where structure is arranged on flexible conductive substrate, which comprises metallization part
CN103515484A (en) * 2013-09-13 2014-01-15 南开大学 Textured transparent conductive thin film with periodic structure and preparation method thereof
CN105206175A (en) * 2015-10-23 2015-12-30 浙江大学 Anti-counterfeit label based on patterned metal nanocomposite and production method of anti-counterfeit label
CN106277822A (en) * 2016-07-28 2017-01-04 李志刚 Silicon nanometer column array material and preparation method thereof
CN107101988A (en) * 2017-03-16 2017-08-29 中国科学院合肥物质科学研究院 A kind of high density nanometer pinpoint array of golden film covering and its application
CN108046211A (en) * 2017-11-23 2018-05-18 中国科学院合肥物质科学研究院 A kind of preparation method and applications of silicon substrate thorniness shape nanocone oldered array
CN108417650A (en) * 2018-04-03 2018-08-17 芜湖孺子牛节能环保技术研发有限公司 A kind of amorphous silicon membrane improving solar cell photoelectric transformation efficiency
CN108594288A (en) * 2018-04-25 2018-09-28 西北核技术研究所 A kind of surface has the plastic scintillant and preparation method thereof of microlens array
CN108754418A (en) * 2018-06-28 2018-11-06 吉林大学 Self-supporting chiral nano hollow cone array film with chiral optical rotation property and preparation method thereof

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