CN109851832B - Method for constructing surface roughened PS ball array on flexible substrate - Google Patents
Method for constructing surface roughened PS ball array on flexible substrate Download PDFInfo
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- CN109851832B CN109851832B CN201811622327.7A CN201811622327A CN109851832B CN 109851832 B CN109851832 B CN 109851832B CN 201811622327 A CN201811622327 A CN 201811622327A CN 109851832 B CN109851832 B CN 109851832B
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Abstract
The invention discloses a method for constructing a surface roughened PS ball array on a flexible substrate, which comprises the following steps: obtaining an ultra-clean glass substrate; obtaining hexagonal close-packed single-layer PS balls on a flexible substrate; and (4) obtaining a surface roughened PS ball array. By utilizing a reactive ion etching method, the surface of the PS ball is directly roughened on the flexible substrate, so that a PS ball array with a micro-nano structure on the surface is obtained, and the surface of the array has the characteristics of the micro-nano structure. Compared with other preparation schemes, the scheme has the advantages of simpler manufacturing process, controllable surface appearance, controllable size of the PS balls and more uniform components, and in addition, the flexible substrate can be folded, is convenient to carry, has lower cost, can be prepared in a large scale and realizes batch production and manufacturing.
Description
Technical Field
The invention relates to a surface roughening method for PS (polystyrene) balls, in particular to a method for constructing a surface roughened PS ball array on a flexible substrate.
Background
As a high molecular polymer with controllable size and high sphericity, PS (polystyrene) spheres have been found by Vanderhoff, Brodford and the like, and are widely applied to biomedical materials, chemical materials, energy and technology materials and the like. Because the PS ball has better structural stability and chemical stability, the PS ball can resist high temperature to a certain degree and is difficult to degrade in natural environment and organisms, so the PS ball is used as a precursor for material synthesis and modification by extensive researchers. There are many methods for preparing and synthesizing PS spheres, and typically, emulsion polymerization and suspension polymerization are used. In addition, many researchers have conducted studies on the functionalization of PS beads, such as introduction of hydroxyl group (-OH), carboxyl group (-COOH), aldehyde group (-CHO), sulfonic acid group (-SO3), and the like, on the surface of PS beads.
But the prior proposal about roughening the surface of the PS sphere and showing micro-nano treatment is not common. In general, by adding other chemical materials and reacting with PS spheres in a harsher environment, the obtained surface appearance is difficult to control, and foreign impurities are introduced too much.
Disclosure of Invention
The invention aims to provide a method for constructing a surface roughened PS ball array on a flexible substrate.
The purpose of the invention is realized by the following technical scheme:
the invention discloses a method for constructing a surface roughened PS ball array on a flexible substrate, which comprises the following steps:
the method comprises the following steps: obtaining an ultra-clean glass substrate;
step two: obtaining hexagonal close-packed single-layer PS balls on a flexible substrate;
step three: and (4) obtaining a surface roughened PS ball array.
According to the technical scheme provided by the invention, the method for constructing the PS ball array with the roughened surface on the flexible substrate provided by the embodiment of the invention has the advantages of simpler manufacturing process, controllable surface appearance, controllable size of the PS balls and more uniform components, and in addition, the flexible substrate can be folded, is convenient to carry, has lower cost, can be prepared in a large scale and realizes batch production and manufacturing.
Drawings
Fig. 1 is a schematic diagram of a process for preparing a flexible substrate of a roughened PS spherical array surface micro-nano structure in an embodiment of the present invention.
FIG. 2 is an SEM photograph of different etching times under the conditions of vacuum degree of 12Pa, sulfur hexafluoride gas flow rate of 65sccm, and radio frequency power of 200w in the embodiment of the present invention. In the figure, (a), (b), (c), (d), (e) and (f) are SEM photographs obtained with etching times of 30s, 60s, 90s, 120s, 150s and 180s, respectively.
Detailed Description
The embodiments of the present invention will be described in further detail below. Details which are not described in detail in the embodiments of the invention belong to the prior art which is known to the person skilled in the art.
The invention discloses a method for constructing a surface roughened PS ball array on a flexible substrate, which comprises the following steps:
the method comprises the following steps:
the method comprises the following steps: obtaining an ultra-clean glass substrate;
step two: obtaining hexagonal close-packed single-layer PS balls on a flexible substrate;
step three: and (4) obtaining a surface roughened PS ball array.
The first step comprises the following steps:
putting a plurality of glass sheets into a beaker, adding an acetone solution until the glass sheets are immersed, and carrying out ultrasonic treatment by using an ultrasonic machine; pouring out the acetone solution, adding alcohol to immerse the glass sheet, and performing ultrasonic treatment by using an ultrasonic machine; pouring out alcohol, adding deionized water, and pouring out the deionized water after ultrasonic treatment, wherein the ultrasonic treatment time is not less than half an hour each time;
pouring hydrogen peroxide and concentrated sulfuric acid into a previous beaker in sequence according to the volume ratio of 1: 3 until a glass sheet is immersed, then carrying out ultrasonic treatment for 1h, standing for 12h, pouring waste liquid, fully washing the waste liquid with deionized water, then pouring the deionized water, ammonia water and hydrogen peroxide into the beaker in sequence according to the volume ratio of 3: 1 until the glass sheet is immersed, pouring the waste liquid after carrying out ultrasonic treatment for two hours, finally filling the glass sheet with deionized water, and carrying out ultrasonic treatment for 2h to obtain an ultra-clean glass sheet.
The second step comprises the following steps:
putting a plurality of required glass sheets into an oven, and adjusting a certain temperature to carry out drying treatment;
then, putting the glass sheet into an ozone cleaning machine for cleaning for a period of time, then directly adding a layer of deionized water film on the surface of the glass sheet, taking out a plurality of 500nm PS balls and high-purity alcohol by using a liquid transfer gun, mixing the two according to a certain proportion to obtain a mixed solution, putting the mixed solution into a 2ml test tube, and carrying out ultrasonic treatment by using an ultrasonic machine for standby application;
slowly injecting the mixed solution into a water film by using a liquid transfer gun to obtain one or more layers of PS ball films on the liquid surface, and drying the PS ball films;
and filling water into the beaker, adding a surfactant, transferring the PS ball film onto the water surface, and fishing up the PS ball film by using the PE film to obtain the single-layer PS ball array in hexagonal close packing on the flexible substrate.
The third step comprises:
putting the prepared PE film with the single-layer PS ball film into a reactive ion etching instrument, pumping the vacuum degree of the PE film to a lower level by using a mechanical pump, then pumping the vacuum degree to 0.3Pa by using a molecular pump, opening a sulfur hexafluoride gas valve after the vacuum degree is stable, controlling the flow rate to 65sccm, slowly adjusting the gas inlet valve until the vacuum degree is raised back to 12Pa, adjusting the radio frequency power to 200w after the flow rate of the sulfur hexafluoride gas flow is gradually stable, wherein the etching time changes from 30s to 180s every time, and the interval of each time is 30 s;
after the etching is finished, all air valves are closed, and N is introduced2And when the vacuum degree is recovered to normal atmospheric pressure, obtaining the flexible substrate of the PS ball array subjected to reactive ion etching roughening at different time, wherein the surface of the flexible substrate presents micro-nano structure characteristics.
The invention discloses a method for constructing a PS (polystyrene) ball array with a roughened surface on a flexible substrate, which directly roughens the surface of a PS ball on the flexible substrate by using a reactive ion etching method to obtain the PS ball array with the surface in a micro-nano structure, wherein the surface of the array has the characteristics of the micro-nano structure. Compared with other preparation schemes, the scheme has the advantages of simpler manufacturing process, controllable surface appearance, controllable size of the PS balls and more uniform components, and in addition, the flexible substrate can be folded, is convenient to carry, has lower cost, can be prepared in a large scale and realizes batch production and manufacturing.
The first problem solved by the invention is to prepare an array of PS balls with smooth surface and controllable size on a glass substrate.
The second problem solved by the invention is that the array of PS balls on the glass substrate is transferred to a PE film to obtain the array of PS balls on the flexible substrate, and the substrate can be folded and is convenient to carry, in addition, the cost is low, and the array of PS balls on the flexible substrate can be prepared in a large scale and can be produced in batches.
The third problem solved by the invention is that a roughened PS ball array is obtained by directly utilizing a reactive ion etching method, the surface of the array has micro-nano structural characteristics, and foreign impurities are basically not introduced, so that the components are relatively uniform.
The specific embodiment, as shown in fig. 1 and fig. 2, includes the steps of:
the method comprises the following steps: and obtaining an ultra-clean glass substrate. Putting a plurality of glass sheets into a beaker, adding an acetone solution until the glass sheets are immersed, and carrying out ultrasonic treatment by using an ultrasonic machine; pouring out the acetone solution, adding alcohol to immerse the glass sheet, and performing ultrasonic treatment by using an ultrasonic machine; pouring out alcohol, adding deionized water, and pouring out the deionized water after ultrasonic treatment. The ultrasonic treatment time should be no less than half an hour. Pouring hydrogen peroxide and concentrated sulfuric acid into a previous beaker in sequence according to the volume ratio of 1: 3 until the glass sheet is immersed, then carrying out ultrasonic treatment for 1h, standing for 12h, pouring waste liquid, fully washing the waste liquid with deionized water, then pouring the deionized water, ammonia water and hydrogen peroxide into the beaker in sequence according to the volume ratio of 3: 1 until the glass sheet is immersed, carrying out ultrasonic treatment for two hours, pouring the waste liquid, finally filling the glass sheet with deionized water for immersion, and carrying out ultrasonic treatment for 2h to obtain the ultra-clean glass sheet. Because of the long ultrasound time, several ice bags are typically placed while the ultrasound machine is running.
Step two: and obtaining the hexagonal close packed single layer PS balls on the flexible substrate. And (3) putting a plurality of required glass sheets into an oven, and adjusting a certain temperature to carry out drying treatment. Then, the glass sheet is put into an ozone cleaning machine for cleaning for a period of time, then a layer of deionized water membrane is directly added on the surface of the glass sheet, a liquid transfer gun is used for taking out a plurality of 500nm PS balls and high-purity alcohol, the two are mixed according to a certain proportion to obtain a mixed solution, the mixed solution is placed into a 2ml test tube, and the ultrasonic machine is used for standby application. The mixed solution is slowly injected into a water film by a liquid transfer gun to obtain a PS sphere film (generally a plurality of layers) on the liquid surface, and the PS sphere film is dried. And filling water into the beaker, adding a certain amount of surfactant, transferring the PS ball film to the water surface, and fishing up the PS ball film by using the PE film to obtain the single-layer PS ball array in hexagonal close packing on the flexible substrate.
Step three: surface roughened PSAnd (4) obtaining a ball array. The PE film with the single-layer PS ball film prepared previously is placed into a reactive ion etching instrument, the vacuum degree of the PE film is pumped to a lower level by a mechanical pump, then the vacuum degree is pumped to 0.3Pa by a molecular pump, after the vacuum degree is stabilized, a sulfur hexafluoride gas valve is opened, the flow rate is controlled to 65sccm, the gas inlet valve is slowly adjusted until the vacuum degree is raised to about 12Pa, after the flow rate of sulfur hexafluoride gas flow is gradually stabilized, the radio frequency power is adjusted to 200w, the etching time changes from 30s to 180s every time, and the interval of each time is 30 s. After the etching is finished, all air valves are closed, and N is introduced2And when the vacuum degree is recovered to normal atmospheric pressure, obtaining the flexible substrate of the PS ball array subjected to reactive ion etching roughening at different time, wherein the surface of the flexible substrate presents micro-nano structure characteristics.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (1)
1. A method of constructing a surface roughened array of PS spheres on a flexible substrate, comprising:
the method comprises the following steps: obtaining an ultra-clean glass substrate;
step two: obtaining hexagonal close-packed single-layer PS balls on a flexible substrate;
step three: obtaining a surface roughened PS ball array;
the first step comprises the following steps:
putting the glass sheet into a beaker, adding an acetone solution until the glass sheet is immersed, and carrying out ultrasonic treatment by using an ultrasonic machine; pouring out the acetone solution, adding alcohol to immerse the glass sheet, and performing ultrasonic treatment by using an ultrasonic machine; pouring out alcohol, adding deionized water, and pouring out the deionized water after ultrasonic treatment, wherein the ultrasonic treatment time is not less than half an hour each time;
pouring hydrogen peroxide and concentrated sulfuric acid into a previous beaker in sequence according to the volume ratio of 1: 3 until a glass sheet is immersed, then carrying out ultrasonic treatment for 1h, standing for 12h, pouring waste liquid, fully washing the waste liquid with deionized water, then pouring the deionized water, ammonia water and hydrogen peroxide into the beaker in sequence according to the volume ratio of 3: 1 until the glass sheet is immersed, pouring the waste liquid after carrying out ultrasonic treatment for two hours, finally filling the glass sheet with deionized water, and carrying out ultrasonic treatment for 2h to obtain an ultra-clean glass sheet, wherein in the process, the ultrasonic treatment time is longer, so that an ice bag is placed when an ultrasonic machine is operated;
the second step comprises the following steps:
putting the required glass sheet into an oven, and adjusting a certain temperature to carry out drying treatment;
then, putting the glass sheet into an ozone cleaning machine for cleaning for a period of time, then directly adding a layer of deionized water membrane on the surface of the glass sheet, taking out a 500nm PS ball and alcohol by using a liquid transfer gun, mixing the two according to a certain proportion to obtain a mixed solution, putting the mixed solution into a 2ml test tube, and carrying out ultrasonic treatment by using an ultrasonic machine for standby application;
slowly injecting the mixed solution into a water film by using a liquid transfer gun to obtain one or more layers of PS ball films on the liquid surface, and drying the PS ball films;
filling water into the beaker, adding a surfactant, transferring the PS ball film onto the water surface, and fishing up the PS ball film by using the PE film to obtain a single-layer PS ball array in hexagonal close packing on the flexible substrate;
the third step comprises:
putting the prepared PE film with the single-layer PS ball film into a reactive ion etching instrument, pumping the vacuum degree of the PE film to a lower level by using a mechanical pump, then pumping the vacuum degree to 0.3Pa by using a molecular pump, opening a sulfur hexafluoride gas valve after the vacuum degree is stable, controlling the flow rate to 65sccm, slowly adjusting the gas inlet valve until the vacuum degree is raised back to 12Pa, adjusting the radio frequency power to 200w after the flow rate of the sulfur hexafluoride gas flow is gradually stable, wherein the etching time changes from 30s to 180s every time, and the interval of each time is 30 s;
after the etching is finished, all air valves are closed, and N is introduced2And when the vacuum degree is recovered to normal atmospheric pressure, obtaining the flexible substrate of the PS ball array subjected to reactive ion etching roughening at different time, wherein the surface of the flexible substrate presents micro-nano structure characteristics.
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