CN111282785A - Silicon dioxide microsphere array for patterning planar substrate and preparation method thereof - Google Patents
Silicon dioxide microsphere array for patterning planar substrate and preparation method thereof Download PDFInfo
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- CN111282785A CN111282785A CN202010086318.1A CN202010086318A CN111282785A CN 111282785 A CN111282785 A CN 111282785A CN 202010086318 A CN202010086318 A CN 202010086318A CN 111282785 A CN111282785 A CN 111282785A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
- B05D1/20—Processes for applying liquids or other fluent materials performed by dipping substances to be applied floating on a fluid
- B05D1/202—Langmuir Blodgett films (LB films)
- B05D1/204—LB techniques
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating 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
- C04B41/5072—Coating 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
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Abstract
The invention discloses a silicon dioxide microsphere array for plane substrate imaging and a preparation method thereof, which utilizes n-butyl alcohol to wrap silicon dioxide microspheres, overcomes the defect that the density of silicon dioxide is higher than that of water solution, prevents the silicon dioxide microspheres from settling, enables the silicon dioxide microspheres to be distributed on the surface of a liquid, heats the liquid surface, and utilizes intermolecular force to closely arrange the microspheres into a uniform monolayer spherical membrane; the template can be transferred to the surface of a substrate to complete self-assembly at a proper pulling rate by using a pulling coating machine, so that the preparation of the planar substrate graphical technical template is realized. Compared with the surfactant-assisted method, the method saves the time for groping modification process parameters, and is suitable for silicon dioxide spheres with various micron sizes; the surface patterning technical template is realized by self-assembling the silicon dioxide microsphere array, compared with a photoetching method, the surface patterning technical template is simple in equipment and low in cost, and the problem that the completeness of the pattern is influenced by uneven photoresist coating at the edge is solved.
Description
Technical Field
The invention relates to a silicon dioxide microsphere array and a preparation method thereof, in particular to a silicon dioxide microsphere array for patterning a planar substrate and a preparation method thereof.
Background
The surface patterning is to construct a micro-pattern region with an ordered structure on the surface of a material by using a material processing technology, and can be used for researching or improving the physical and chemical properties of the micro-pattern region. The assembly and construction of the micro-nano particles can be realized by various technical means, such as optical tweezers technology, photoetching technology, self-assembly technology and the like. The optical tweezers technology indirectly controls single molecules through a medium small ball handle, and an ultra-stable system is required to be used as a guarantee for achieving high-precision measurement and positioning. The photolithography technique copies the target pattern on the mask on the substrate through the exposure and etching processes of the photoresist material, and although the precision is high and the repeatability is good, the cost is expensive. The self-assembly method is a method of spontaneously organizing or aggregating a plurality of individuals into a stable and regular structure under the interaction based on non-covalent bonds, and in order to realize the ordered arrangement of a large-range monolayer microsphere array, the problems of uniform arrangement and close adsorption of a spherical structure are required to be solved, and a surfactant-assisted method is generally adopted. The method aims to modify the nano-microspheres to graft hydrophilic groups and hydrophobic groups on the surfaces of the nano-microspheres to form double nano-microspheres, alcohol and the modified nano-microspheres are mixed and dripped to the water surface, and after the alcohol is evaporated, a regular single-layer nano-sphere film is formed on the water surface. However, the above microsphere modification method is only suitable for nanometer size, and the success rate of modification of micron-sized microspheres is low. Meanwhile, the microspheres have larger volume, are easy to settle on the liquid surface, and are difficult to realize uniform ball arrangement.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a silicon dioxide microsphere array for planar substrate patterning and a preparation method thereof, and solves the problems that in the prior art, the modification success rate of microspheres with micron sizes is low, the microspheres are large in size, and are easy to settle on the liquid surface, so that uniform ball arrangement is difficult to realize.
The technical scheme of the invention is as follows:
a preparation method of a silicon dioxide microsphere array for patterning a planar substrate comprises the following steps:
(1) cleaning of the sapphire substrate:
sequentially putting the sapphire substrate into deionized water, absolute ethyl alcohol and acetone, and respectively carrying out ultrasonic cleaning to remove organic impurities on the surface; cleaning with deionized water, and drying the sapphire substrate in a constant-temperature drying oven for later use;
(2) preparing a silicon dioxide microsphere solution:
adding the silicon dioxide microsphere powder into a centrifuge tube, pouring n-butanol into the centrifuge tube, and preparing a solution with the concentration of 0.33-0.5 mg/ml; ultrasonically treating the centrifugal tube until the suspension is uniformly dispersed and is milky;
(3) preparing a SiO2 microsphere liquid film:
adding deionized water into a weighing bottle for half, standing, and slowly dripping the solution prepared in the step (2) along the edge of the weighing bottle; meanwhile, heating the weighing bottle on a heating table to ensure that the n-butanol is quickly diffused on the liquid level, the solid spheres are coagulated into a lamella, and a uniform single-layer silicon dioxide microsphere film is formed on the liquid level;
(4) coating film of lifting coating machine
Transferring the single-layer silicon dioxide microspheres on the liquid surface obtained in the step (3) to a sapphire planar substrate by using a dip coating machine;
(5) heating and drying
And (4) placing the sapphire substrate coated with the silicon dioxide microspheres on the surface obtained in the step (4) on a heating table, drying and hardening, and evaporating redundant water and organic solution.
The solution prepared in the step (2) is dripped in the step (3), and the dripping amount is 1 ml; the heating stage temperature was 90 ℃.
The pulling speed in the step (4) is 0.03mm/min-0.06 mm/min.
The silicon dioxide microsphere array prepared by the method.
The invention has the beneficial effects that:
1) compared with the method assisted by the surfactant, the method saves the time for groping modification process parameters, and is suitable for silicon dioxide spheres with various micron sizes;
2) the surface patterning technical template is realized by self-assembling the silicon dioxide microsphere array, compared with a photoetching method, the surface patterning technical template is simple in equipment and low in cost, and the problem that the completeness of the pattern is influenced by uneven photoresist coating at the edge is solved.
The preparation process is simple and easy to control, overcomes the defect that the density of silicon dioxide is higher than that of an aqueous solution, prevents the silicon dioxide from settling, enables the silicon dioxide to be distributed on the surface of a liquid, heats the liquid surface, and utilizes intermolecular force to closely arrange microspheres into a uniform monolayer spherical membrane; the template can be transferred to the surface of a substrate to complete self-assembly at a proper pulling rate by using a pulling coating machine, so that the preparation of the planar substrate graphical technical template is realized. On the basis of no surface modification, the micro-spheres are controlled to be arranged into a uniform and compact single-layer spherical film on the liquid surface.
Drawings
FIG. 1 is a flow chart of the preparation of a silica microsphere array; wherein (a) n-butanol-silica sphere suspension is dripped; (b) spreading the suspension on the liquid surface of the weighing bottle; (c) heating and evaporating the deionized water and the n-butyl alcohol; (d) lifting and transferring the substrate to a substrate by a lifting coating machine;
FIG. 2 is a schematic view of a lift coater wherein ① cantilever ② clamp ③ weigh bottle ④ numerically controlled faceplate and base;
FIG. 3 is a comparison graph of the morphology of samples prepared from 5mg of silica microsphere powder and different doses of n-butanol; wherein (a) 5ml of n-butanol is added for the film-coating result by pulling; (b) adding 10ml of n-butyl alcohol to obtain a pulling coating result; (c) adding 15ml of n-butyl alcohol to obtain a pulling coating result;
FIG. 4 is a graph of the structural morphology formed by an array of silica microspheres at different pull rates; wherein (a) a ball array formed by pulling at a speed of 0.06mm/min (b) a ball array formed by pulling at a speed of 0.045mm/min (c) a ball array formed by pulling at a speed of 0.03 mm/min.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
The raw materials used in the invention are all commercially available materials and are not further purified.
A preparation method of a two-dimensional ordered silicon dioxide microsphere array for surface patterning comprises the following steps:
(1) cleaning of the sapphire substrate:
sequentially putting the sapphire substrate into deionized water, absolute ethyl alcohol and acetone, and respectively carrying out ultrasonic cleaning for 20 minutes to remove organic impurities on the surface; cleaning with deionized water, and drying the sapphire substrate in a constant-temperature drying oven for later use;
(2) preparing a silicon dioxide microsphere solution:
weighing 5mg of silicon dioxide microsphere powder by using an electronic balance, adding the silicon dioxide microsphere powder into a centrifugal tube 1, and pouring 5ml of n-butyl alcohol; as a control, 10ml and 15ml of n-butanol were added to centrifuge tubes 2, 3, respectively, while 5mg of silica powder was added; all three centrifugal tubes are subjected to ultrasonic treatment for 30min until the suspension is uniformly dispersed and is milky;
(3) preparation of SiO2 microsphere liquid film
And (3) adding deionized water into a weighing bottle for half, standing for 10min, and then slowly dripping the solution prepared in the step (2) along the edge of the weighing bottle, wherein the dripping amount is 1 ml. Meanwhile, heating the weighing bottle on a heating table at 90 ℃ to ensure that the n-butanol is quickly diffused on the liquid level, the solid spheres are condensed into a lamellar layer, and a uniform single-layer silicon dioxide microsphere film is formed on the liquid level; the results are shown in FIG. 3.
(4) Coating film of lifting coating machine
Transferring the single-layer silicon dioxide microspheres on the liquid surface obtained in the step 3) to a sapphire planar substrate by using a pulling coating machine, wherein the pulling speed is 0.03mm/min-0.06 mm/min; as shown in FIG. 4, the best pulling effect was observed at a speed of 0.045mm/min under a magnification of 1000 times by an optical microscope.
(5) Heating and drying
And 4) placing the sapphire substrate coated with the silicon dioxide microspheres on the surface obtained in the step 4) on a heating table, drying and hardening, and evaporating redundant water and organic solution.
The invention is not limited to the embodiments described above, many variations in detail are possible without departing from the scope and spirit of the invention.
Claims (4)
1. A preparation method of a silicon dioxide microsphere array for patterning a planar substrate is characterized by comprising the following steps:
(1) cleaning of the sapphire substrate:
sequentially putting the sapphire substrate into deionized water, absolute ethyl alcohol and acetone, and respectively carrying out ultrasonic cleaning to remove organic impurities on the surface; cleaning with deionized water, and drying the sapphire substrate in a constant-temperature drying oven for later use;
(2) preparing a silicon dioxide microsphere solution:
adding the silicon dioxide microsphere powder into a centrifuge tube, pouring n-butanol into the centrifuge tube, and preparing a solution with the concentration of 0.33-0.5 mg/ml; ultrasonically treating the centrifugal tube until the suspension is uniformly dispersed and is milky;
(3) preparing a SiO2 microsphere liquid film:
adding deionized water into a weighing bottle for half, standing, and slowly dripping the solution prepared in the step (2) along the edge of the weighing bottle; meanwhile, heating the weighing bottle on a heating table to ensure that the n-butanol is quickly diffused on the liquid level, the solid spheres are coagulated into a lamella, and a uniform single-layer silicon dioxide microsphere film is formed on the liquid level;
(4) coating film of lifting coating machine
Transferring the single-layer silicon dioxide microspheres on the liquid surface obtained in the step (3) to a sapphire planar substrate by using a dip coating machine;
(5) heating and drying
And (4) placing the sapphire substrate coated with the silicon dioxide microspheres on the surface obtained in the step (4) on a heating table, drying and hardening, and evaporating redundant water and organic solution.
2. The method for preparing a silica microsphere array used for patterning a planar substrate according to claim 1, wherein the solution prepared in the step (2) is dripped in the step (3) in an amount of 1 ml; the heating stage temperature was 90 ℃.
3. The method for preparing a silica microsphere array used for patterning a planar substrate according to claim 1, wherein the pulling speed in the step (4) is 0.03mm/min to 0.06 mm/min.
4. An array of silica microspheres produced by the method of any one of claims 1 to 3.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112723303A (en) * | 2020-12-14 | 2021-04-30 | 苏州拉索生物芯片科技有限公司 | Microbead chip and spin coating preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112723303A (en) * | 2020-12-14 | 2021-04-30 | 苏州拉索生物芯片科技有限公司 | Microbead chip and spin coating preparation method thereof |
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