CN112553693B - Method for preparing large-area single-layer colloidal crystal based on water film - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000002356 single layer Substances 0.000 title claims abstract description 33
- 239000013078 crystal Substances 0.000 title claims description 20
- 239000000758 substrate Substances 0.000 claims abstract description 104
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000002245 particle Substances 0.000 claims abstract description 31
- 239000000084 colloidal system Substances 0.000 claims abstract description 30
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- 239000010410 layer Substances 0.000 claims abstract description 12
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 10
- 239000012498 ultrapure water Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 229910010272 inorganic material Inorganic materials 0.000 claims description 4
- 239000011147 inorganic material Substances 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims 7
- 238000001338 self-assembly Methods 0.000 abstract description 19
- 239000007788 liquid Substances 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000011160 research Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract 1
- 230000008569 process Effects 0.000 description 5
- 239000004005 microsphere Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 210000000170 cell membrane Anatomy 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000007702 DNA assembly Methods 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 238000000707 layer-by-layer assembly Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000005381 potential energy Methods 0.000 description 1
- 238000001243 protein synthesis Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 230000014616 translation Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/64—Flat crystals, e.g. plates, strips or discs
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/02—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent
- C30B7/04—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent using aqueous solvents
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- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention belongs to the field of colloid science, and particularly relates to a self-assembly method for particles by utilizing water film power. The invention can control the position and shape of the liquid drop on the surface of the substrate and the shape of the substrate, and the water film can promote the self-assembly of the particles, thereby achieving the purpose of rapidly preparing large-area single-layer silicon dioxide colloid; if a multilayer region exists in the sample, the other layers of substrates are attached to the multilayer region, so that the upper layer particles of the multilayer region which is difficult to use originally are separated from the original substrate and adhered to the other substrates to complete self-assembly. The invention has the advantages that: compared with the traditional method, the preparation time is shorter, and a multilayer area which cannot be used by the traditional preparation method can be utilized, so that research materials are saved.
Description
Technical Field
The invention belongs to the field of colloid science, and particularly relates to a preparation method of a single-layer colloid crystal.
Background
The glue system and the gas-liquid interface are generally existed in nature and are very close to production and scientific research. In recent years, since various experimental instruments based on the theory of colloid science are excellent in application to industrial production, colloid processing and application have received much attention and have shown great application potential in important fields such as optics, electromagnetism, biosensing, biomedicine, and the like. Therefore, it is very necessary to develop an effective colloid processing technique to realize large-area lattice-complete two-dimensional colloids with adjustable parameters and to reduce production costs. Many methods for preparing two-dimensional colloidal structures have been developed so far, however, these methods still have problems of small processing area, low efficiency, high cost, incomplete crystal lattice, and being limited by the substrate.
In studies in the biological and medical fields, two-dimensional colloids are an ideal physical model by which researchers have deeply analyzed various complex phenomena of biological macromolecules in cells such as DNA assembly, protein synthesis, and kinetic behavior on cell membranes. The two-dimensional colloid is a single-layer colloid formed by periodically arranging monodisperse colloid particles. In order to more accurately simulate the movement of various biomolecules on cell membranes, the most critical step is to prepare a monolayer colloidal crystal with large area and high quality. At present, many international research groups are concerned with the self-assembly process, mechanism and application of large-area and high-quality monolayer colloidal crystals. Through the development of many years, the scientists of many countries successively put forward advanced colloid particle self-assembly methods such as a spin coating self-assembly method, a vertical self-assembly method, an ultrasonic-assisted self-assembly method, a template-assisted self-assembly method, ink-jet printing, a laser-assisted self-assembly method and the like in the field, and the purpose is to obtain a large-area and high-quality colloid monolayer so as to prepare a high-performance surface plasma device. China scientists also put forward methods of preparing high-quality colloid monolayers by capillary self-assembly, electrostatic self-assembly, microfluid-assisted self-assembly and the like. However, the current colloid self-assembly technology still has the key technical problems of large agglomerate particle coverage rate, poor large-area micro-order, more crystal boundaries and the like in the aspect of preparing a large-area and high-quality colloid single layer, and the periodicity of surface potential energy is damaged by the structural defects. Therefore, there is a need for a self-assembly method that can effectively control the micro-order and grain boundary density of large area and can avoid the agglomeration, deposition and adhesion of colloidal particles during the self-assembly process, thereby providing a solid technical support for the wide commercial application of colloidal particles.
Disclosure of Invention
Technical problem to be solved
Aiming at the problems in the background art, the invention aims to provide a monolayer colloidal crystal self-assembly method based on interface water film driving, and the two-dimensional colloidal crystal monolayer prepared by the method has the remarkable advantages of few surface adhesive particles, good large-area microscopic orderliness, low grain boundary density and the like.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme:
step 1, respectively cleaning a substrate and a culture dish, and then carrying out super-hydrophilic treatment;
2, oscillating the silicon dioxide colloidal particle monodisperse solution in an ultrasonic instrument for 5 minutes;
step 4, dripping 50 microliters of ultrapure water in the center of the substrate in the step 3 to form a water film on the surface of the substrate;
step 5, placing the substrate in the step 4 under a microscope, slowly dripping 100 microliters of the silica colloid particle monodisperse solution in the step 2 to the center, and observing the density distribution of colloid balls under the microscope until the particles are arranged into a single layer, wherein the temperature of the sample is controlled to be about 25 ℃ and the humidity is controlled to be about 50%;
and 6, horizontally placing another substrate in the step 1 above the substrate in the step 5 for 5 mm, approaching the substrate in the step 5, waiting for about 5 seconds to enable the water film to be adhered to the upper substrate when the upper substrate is contacted with the water film but not contacted with the substrate, and keeping away from the substrate after the water film is adhered until the upper substrate is completely separated from the water film.
Step 7, placing the sample obtained in the step 6 into a thermostat, and standing for 10 minutes, wherein the temperature is controlled to be about 55 ℃, and the humidity is less than 50%;
and 8, placing the substrate under a microscope to observe whether the substrate is completely covered by a single-layer area or not, if a multi-layer area exists, dripping 50 microliters of ultrapure water in the center of the substrate, slowly attaching the substrate in the step 1 to completely attach the upper substrate and the lower substrate above the substrate, continuously applying pressure for 10 seconds, separating the upper substrate and the lower substrate, and horizontally standing the substrate until the water film on the surface of the substrate is completely evaporated.
And 9, observing the substrate under a microscope, and if a multi-layer region still exists, repeating the step 8 until all the substrates only have a single-layer region, so that the single-layer colloidal crystal can be obtained on the surface of the substrate.
Further, the substrate in step 1 is an inorganic material.
Further, the inorganic material in the step 1 is glass or quartz.
Further, the super-hydrophilic treatment in the step 1 is to soak in 75% ethanol solution for 5min and then place the ethanol solution in ultrapure water for ultrasonic cleaning for 5min, and repeat the above cleaning for 2-3 times.
Further, the alternating diameter of the silica in the silica colloidal particle monodisperse solution in the step 2 is in the range of 0.6 μm to 3.0. mu.m.
Further, the speed of the upper substrate approaching to and departing from the lower substrate in the step 6 is 0.1mm/s-0.3 mm/s.
Further, the monolayer region in step 8 is a region where the colloidal particles of the substrate are only arranged in a monolayer manner when observed under a microscope.
Further, the multi-layer region in step 8 is a region where the substrate is observed under a microscope to show that a large amount of colloid particles are piled up to form a shadow, which cannot be observed.
Further, the pressure applied to the substrate in step 8 is 1.00N to 1.50N.
The invention utilizes the water film dynamics self-diffusion of colloid particles to rapidly prepare two-dimensional colloid, and the working principle is as follows:
because the microspheres in the diluted silica microsphere suspension may have a small amount of clusters, the clusters can become condensation nuclei in the evaporation process to cause a large amount of silica microspheres to be aggregated to form overlapping, the microspheres can be dispersed in the ultrasonic oscillation process to reduce the number of the condensation nuclei and reduce the overlapping area, then when an upper substrate is moved, liquid drops are driven to deform through surface tension, particles at the edge liquid level are mainly subjected to Van der Waals force of the substrate to enable the particles to rapidly settle and self-assemble, finally, a small amount of multi-layer silica microspheres still in the cluster state can be soaked by ultrapure water and then are contacted with the upper substrate through pressure, because the attraction of the upper substrate to the silica microspheres is larger than the attraction among the clusters, and the multi-layer separation into a single layer and self-assembly are carried out to form a non-overlapping two-dimensional.
(III) advantageous effects
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. the method of the invention can also break away the silicon dioxide balls of the clusters when the ultrasonic wave is skillfully utilized to clean the substrate, and can effectively reduce the clusters of the colloid particles, thereby obtaining a large-area single-layer colloid.
2. The method of the invention can accelerate the continuous transition between air and liquid level and the self-assembly of particles by moving the upper substrate to deform the liquid drops, and can effectively avoid the clustering and adhesion of colloid particles in the self-assembly process, thereby obviously reducing the surface coverage rate of overlapped colloids.
3. The method utilizes the extremely strong capillary force of the water films on the surfaces of the two layers of super-hydrophilic substrates to drive the colloidal particles of the water-air interface in the glass container to be spontaneously assembled on the surfaces of the substrates, and can repair and recycle the overlapped area to a certain extent.
Drawings
FIG. 1 is a schematic diagram of the present invention; fig. 2, fig. 3 and fig. 4 are the work diagrams of the present invention.
Detailed Description
The invention is further illustrated by the following example embodiments and the accompanying drawings.
Step 1, respectively cleaning two 20 × 20mm silicon dioxide substrates and a culture dish, soaking in alcohol with the concentration higher than 75% for 5min, placing in ultrapure water, ultrasonically cleaning for 5min, and repeating the cleaning for 2-3 times to ensure that the front side and the back side of the culture dish both have super-hydrophilic characteristics;
2, oscillating the monodisperse solution of the silica colloidal particles with the radius of 1.01 mu m in an ultrasonic instrument for 5 minutes to disperse and reduce clusters as much as possible;
step 4, dripping 50 microliters of ultrapure water in the center of the substrate in the step 3 to form a water film on the surface of the substrate;
step 5, placing the substrate in the step 4 under a microscope, slowly dripping 100 microliters of the silica colloid particle monodisperse solution in the step 2 to the center, and observing the density distribution of colloid balls under the microscope at the same time until the particles are arranged into a single layer in a large area, wherein the temperature of the sample is controlled to be about 25 ℃ and the humidity is controlled to be about 50%;
and 6, horizontally placing another substrate in the step 1 above the substrate in the step 5 for 5 mm, approaching the substrate in the step 5 at a speed of 0.2mm/s, waiting for about 5 seconds to enable the water film to be adhered to the upper substrate when the upper substrate is in contact with the water film but not in contact with the substrate, and keeping away from the substrate after the water film is adhered until the upper substrate is completely separated from the water film.
Step 7, placing the sample obtained in the step 6 into a thermostat, and standing for 10 minutes, wherein the temperature is controlled to be about 55 ℃, and the humidity is less than 50%;
and 8, placing the substrate under a microscope to observe whether the substrate is completely covered by a single-layer area, if a multi-layer area appears, dripping 50 microliters of ultrapure water in the center of the substrate, slowly attaching the substrate in the step 1 to completely attach the upper substrate and the lower substrate, continuously applying 1.00N pressure for 10 seconds, separating the upper substrate and the lower substrate, placing the substrate into the thermostat again, controlling the temperature to be about 55 ℃, controlling the humidity to be less than 50%, and horizontally standing the substrate until the water film on the surface of the substrate is completely evaporated.
Claims (9)
1. A method for preparing large-area single-layer colloidal crystals based on a water film is characterized by comprising the following steps:
step 1, respectively cleaning a substrate and a culture dish, and then carrying out super-hydrophilic treatment;
2, oscillating the silicon dioxide colloidal particle monodisperse solution in an ultrasonic instrument for 5 minutes;
step 3, placing a culture dish on a horizontal test bed, and placing a substrate in the step 1 in the center of the culture dish;
step 4, dripping 50 microliters of ultrapure water in the center of the substrate in the step 3 to form a water film on the surface of the substrate;
step 5, placing the substrate in the step 4 under a microscope, slowly dripping 100 microliters of the silica colloid particle monodisperse solution in the step 2 to the center, observing the density distribution of colloid balls under the microscope at the same time until the particles are arranged into a single layer, and controlling the temperature of the sample to be 25 ℃ and the humidity to be 50%;
step 6, horizontally placing another substrate in the step 1 above the substrate in the step 5 for 5 mm, approaching the substrate in the step 5, waiting for 5 seconds to enable the water film to be adhered to the upper substrate when the upper substrate is in contact with the water film but not in contact with the substrate, and keeping away from the substrate after the water film is adhered until the upper substrate is completely separated from the water film;
step 7, placing the sample obtained in the step 6 into a thermostat, standing for 10 minutes, controlling the temperature to be 55 ℃, and controlling the humidity to be less than 50%;
step 8, placing the substrate under a microscope to observe whether the substrate is completely covered by a single-layer area, if a multi-layer area appears, dripping 50 microliters of ultrapure water in the center of the substrate, slowly attaching the substrate in the step 1 to completely attach the upper substrate and the lower substrate above the substrate, continuously applying pressure for 10 seconds, separating the upper substrate and the lower substrate, and horizontally standing the substrate until the water film on the surface of the substrate is completely evaporated;
and 9, observing the substrate under a microscope, and if a multi-layer region still exists, repeating the step 8 until all the substrates only have a single-layer region, so that the single-layer colloidal crystal can be obtained on the surface of the substrate.
2. The method for preparing large area single-layered colloidal crystals based on water membrane according to claim 1, wherein the substrate in step 1 is an inorganic material.
3. The method for preparing large area single-layered colloidal crystals based on water membrane according to claim 2, wherein the inorganic material is glass or quartz.
4. The method for preparing large area single-layered colloidal crystals based on water membrane of claim 1, wherein the ultra-hydrophilic treatment in step 1 is soaking in ethanol solution with concentration higher than 75% for 5min, and then ultrasonic cleaning in ultra-pure water for 5min, and repeating the above cleaning 2-3 times.
5. The method for preparing large area monolayer colloidal crystals based on water membrane according to claim 1, wherein the colloidal diameter of silica in the monodisperse solution of silica colloidal particles in step 2 is in the range of 0.6 μm to 3.0 μm.
6. The method for preparing large area monolayer colloidal crystals based on water membrane according to claim 1, wherein the speed of the upper substrate approaching and departing from the lower substrate in step 6 is 0.1mm/s to 0.3 mm/s.
7. The method for preparing large-area monolayer colloidal crystals based on the water membrane of claim 1, wherein the monolayer region in step 8 is a region where colloidal particles of the substrate are aligned only in a monolayer manner when observed under a microscope.
8. The method for preparing large-area single-layer colloidal crystals based on the water film according to claim 1, wherein the multi-layer region in step 8 is a region where the substrate is observed under a microscope to show that a large amount of colloidal particles are piled up to form a shadow, which cannot be observed.
9. The method for preparing large area monolayer colloidal crystals based on water membrane according to claim 1, wherein the pressure applied to the substrate in step 8 is 1.00N-1.50N.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106370534A (en) * | 2016-08-15 | 2017-02-01 | 常州大学 | Novel self-assembling method for colloidal crystals |
| CN108193278A (en) * | 2017-12-25 | 2018-06-22 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of method that two steps spin-coating method prepares colloid monolayer crystal |
| CN110685014A (en) * | 2019-10-29 | 2020-01-14 | 电子科技大学 | Self-assembly method of single-layer colloidal crystal based on interface water film driving |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106370534A (en) * | 2016-08-15 | 2017-02-01 | 常州大学 | Novel self-assembling method for colloidal crystals |
| CN108193278A (en) * | 2017-12-25 | 2018-06-22 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of method that two steps spin-coating method prepares colloid monolayer crystal |
| CN110685014A (en) * | 2019-10-29 | 2020-01-14 | 电子科技大学 | Self-assembly method of single-layer colloidal crystal based on interface water film driving |
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