CN103696019A - Large-area defect-free two-dimensional colloidal monocrystal as well as preparation method and transfer method thereof - Google Patents
Large-area defect-free two-dimensional colloidal monocrystal as well as preparation method and transfer method thereof Download PDFInfo
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Abstract
The invention relates to a preparation method and a bumpless transfer method of a large-area defect-free two-dimensional colloidal monocrystal. The two-dimensional colloidal monocrystal is formed by self-assembling colloidal particles in a water/gas interface, is excellent in transferability, has the size capable of reaching several square centimeters, and is free from any defect. The invention further provides an improved bumpless transfer method of the two-dimensional colloidal monocrystal, by which the two-dimensional colloidal monocrystal can be transferred to different substrate surfaces under the circumstance that the two-dimensional colloidal monocrystal is not remarkably bumped. The preparation method is simple and efficient, the transfer method is non-selective for the hydrophobicity and hydrophilicity and the curvature of the substrate surfaces, and the application prospect is wide.
Description
Invention field
The present invention relates to a kind of big area zero defect two-dimensional colloidal monocrystalline, also relate to the preparation and the unperturbed transfer method thereof that comprise this colloid monocrystalline.
Background of invention
Two-dimensional colloidal crystalline substance, because of its unique cycle regularity, is used as the structure that template is widely used in various ordered structures.For the ordered structure that based on two-dimensional colloidal crystalline substance is template, build, the problem that first will solve is how to prepare the flawless two-dimensional colloidal crystalline substance of big area.So far, people have been developed various ways and have been prepared two-dimensional colloidal crystalline substance, and wherein the most frequently used is the self-assembling technique based on convection current sedimentation.Existing bibliographical information, by this technology, at the auxiliary lower flawless two-dimensional colloidal monocrystalline that can prepare centimetre-sized of special Wedge device.But this method quite expends time in (conventionally more than half an hour) and substrate surface hydrophilic and hydrophobic is had to requirement, once colloid monocrystalline forms and cannot shift to other substrates in smooth substrate in addition.
Than convection current sedimentation self-assembling technique, the two-dimensional colloidal crystalline substance forming in the self-assembly of water/gas interface based on capillary force, because of its transferability easily, is subject to people's favor gradually.When colloidal particle suspension is added dropwise to water surface, suspension can be sprawled at the water surface rapidly, drives colloidal particle to do corresponding motion at the water surface simultaneously.Under capillary force effect, colloidal particle attracts each other and is finally paved with whole water/gas interface.In preparing the brilliant process of colloid, the self-assembly behavior of colloidal particle is uncontrolled by this method, and the dislocation meeting between colloidal particle is introduced a large amount of internal stresss at colloid intracrystalline, finally tends to form polycrystalline structure.Generally, the area of individual domain between hundreds of to thousands of square microns.We find in experimentation, prepare in the brilliant process of two-dimensional colloidal, to introduce outfield (air-flow) and drive colloidal particle can effectively eliminate at water/gas Interface Motion the internal stress producing because of colloidal particle dislocation at water/gas interface.By introduce emulsifying agent in water, regulate the capillary force size between colloidal particle, and be aided with the release that air-flow promotes stress, finally at water/gas interface, can prepare big area (10cm
2left and right) do not have defective two-dimensional colloidal monocrystalline.
In principle, the two-dimensional colloidal crystalline substance of preparing at water/gas interface can be realized to the transfer on different base surface by crystal pulling method, but this transfer method can be introduced water membrane between substrate and two-dimensional colloidal crystalline substance, and the colloidal particle being submerged in water in the brilliant preparation process of two-dimensional colloidal also can be introduced.After water volatilization, these colloidal particles that are introduced into just can replace the position of original colloidal particle in two-dimensional colloidal crystalline substance, and the substituted colloidal particle in these positions is randomly distributed in the brilliant surface of two-dimensional colloidal.On stricti jurise, saying, is not now that two-dimensional colloidal is truly brilliant at substrate surface.In order to address this problem, we also improve the tranfer system of colloid crystalline substance.In the brilliant unperturbed tranfer system of our improved colloid, substrate is close to wall in the mode of near vertical.After large-area two-dimensional colloid single crystal preparation is good, by drip the aqueous solution along wall, are blocked other three are connected of colloid monocrystalline and wall, after water is siphoned off from container, colloid monocrystalline just spontaneously deposits to wall under capillary force, thereby realizes the transfer on basad surface.Because in transfer process, substrate near vertical is in the water surface, thus can effectively avoid the formation of moisture film, and then avoid the formation of the colloidal particle that two-dimensional colloidal single-crystal surface freely distributes.In addition, the brilliant tranfer system of improved colloid is a spontaneous process, and the disturbance of human factor to colloid monocrystalline in the time of effectively avoiding adopting crystal pulling method, makes this transfer method have reliable repeatability.
The two-dimensional colloidal monocrystalline size of preparing in the self-assembly of water/gas interface under said flow booster action can reach 10cm
2left and right and without any defect, preparation method is easy and simple to handle, and the colloidal particle of different grains is all suitable for; Improved unperturbed tranfer system can be realized in the situation that colloid monocrystalline not being produced to obvious disturbance the transfer to different base surface.
Summary of the invention
The object of the present invention is to provide its unperturbed transfer method of preparation of a kind of big area zero defect two-dimensional colloidal monocrystalline.Two-dimensional colloidal monocrystalline size of the present invention can reach 10cm
2, preparation method is simply efficient; Improved unperturbed tranfer system can be realized in the situation that colloid monocrystalline not being produced to obvious disturbance the transfer to different base surface.In order to realize the present invention, the invention provides following technical proposals:
The flawless two-dimensional colloidal monocrystalline of big area, is characterized in that, whole colloid crystal face is long-pending can reach several square centimeters.Preferably, two-dimensional colloidal monocrystalline size reaches 10cm
2.
According to the present invention, it is characterized in that, the raw material of preparing described two-dimensional colloidal monocrystalline comprises colloidal particle, alcohols dispersion medium, ionic emulsifying agent and pure water.
According to two-dimensional colloidal monocrystalline of the present invention, it is characterized in that, colloidal particle is the close heap close-packed arrays of six sides at water/gas interface, very convenient to required substrate surface transfer.
According to two-dimensional colloidal monocrystalline of the present invention, it is characterized in that, described colloidal particle is polymkeric substance or the inorganics spherocolloid particle of micron or submicron-scale.Preferably, take polymer spherical particle as model particle.The consumption of described alcohols dispersion medium of take is benchmark, and the concentration of colloidal particle is 5-50mg/mL.
According to two-dimensional colloidal monocrystalline of the present invention, it is characterized in that, two-dimensional colloidal monocrystalline is to form under the booster action at compressed air stream in water/gas interface.
According to the present invention, described alcohols dispersion medium particular methanol, the binary dispersion system that ethanol or propyl alcohol and butanols form; With described methyl alcohol, the consumption of ethanol or propyl alcohol is benchmark, and the 3-9 that the consumption of butanols is for the former doubly.
According to the present invention, the consumption of pure water of take is benchmark, and the consumption of ionic emulsifying agent is 17.8-72.6mg/L.
In the present invention, colloidal particle is for forming each element of two-dimensional colloidal crystalline substance.Alcohols dispersion medium is for dispersoid particle, and the abundant dispersion of colloidal particle is the key of preparing high quality two-dimensional colloidal monocrystalline, and in addition, the dispersion system that we select can also improve its floatability of colloidal particle effectively.If its floatability of colloidal particle is too low, waste material on the one hand, be unfavorable on the other hand follow-up film transfer process, for example can form the final particle of staying the brilliant surface of colloid as crystal pulling method.Ionic emulsifying agent is used for regulating the surface tension of water, thereby reaches the object of controlling capillary force between colloidal particle.And this point is also very important to preparing high-quality two-dimensional colloidal monocrystalline.
The preparation method who the invention provides a kind of big area zero defect two-dimensional colloidal monocrystalline, is characterized in that, comprises the following steps:
(1) monodispersed colloidal particle is scattered in to dibasic alcohol dispersion medium, forms stable suspension (excellent
Gating is crossed ultrasonic dispersion);
(2) by the hanging drop in step (1) to the water surface, simultaneously to the water surface, be aided with compressed air stream (airshed 3-6L/min) and drive colloidal particle to move at the water surface, until the whole water surface is paved with colloidal particle;
(3) increase airshed (being for example controlled at 8-12L/min), drive the colloidal film being formed by colloidal particle to travel forward and finally at the flawless two-dimensional colloidal monocrystalline of water/gas interface formation big area.
The method according to this invention, the transfer of described two-dimensional colloidal single crystal direction substrate surface is by the spontaneous deposition process implementation based on capillary force mediation.
According to the present invention, the consumption of described alcohols dispersion medium of take is benchmark, and the concentration of colloidal particle is 5-50mg/mL.
According to the present invention, the consumption of pure water of take is benchmark, and the consumption of ionic emulsifying agent is 17.8-72.6mg/L.
According to the present invention, described methyl alcohol, the consumption of ethanol or propyl alcohol is benchmark, the 3-9 that the consumption of butanols is for the former is doubly.
In the present invention, the degree of scatter of colloidal particle in dispersion system depends on methyl alcohol, ethanol or the propyl alcohol ratio in dibasic alcohol dispersion medium, and ratio is more high more easily disperses.We find, the fully ultrasonic dispersion that can promote colloidal particle.
In the present invention, described airshed is excessive, can directly two dimensional crystal film be dispelled, and cannot prepare perfect colloid monocrystalline.
The present invention also provides a kind of unperturbed transfer method of big area zero defect two-dimensional colloidal monocrystalline, it is characterized in that, comprises the following steps:
(1) before two-dimensional colloidal monocrystalline is prepared at water/gas interface, substrate is close to wall and is immersed in the water, according to aforementioned preparation method, at water/gas interface, prepare afterwards large-area two-dimensional colloid monocrystalline;
(2) along wall, drip pure water to break being connected between other three of brilliant and walls of two-dimensional colloidal;
(3) water siphon is gone out to container (for example flow control is at 5-30mL/min), two-dimensional colloidal monocrystalline deposits from being sent to the remaining wall face that is glued with substrate, thereby realizes two-dimensional colloidal monocrystalline from the based transfer in water/gas interface.
Unperturbed tranfer system in the present invention is spontaneous process, can effectively avoid human factor disturbance to colloid monocrystalline in transfer process.And described method is all suitable for having the substrate of different close and distant water surfaces and curvature, has wide range of applications.
The preparation of big area zero defect two-dimensional colloidal monocrystalline involved in the present invention and unperturbed thereof shift and have the following advantages:
1. this two-dimensional colloidal single crystal preparation desired raw material is simple, cheap and easy to get, and preparation method is simply efficient.
2. this two-dimensional colloidal monocrystalline size is large, can reach 10cm
2left and right, and zero defect, be suitable for the structure of extensive ordered structure.
3. this two-dimensional colloidal crystal formation, in water/gas interface, is suitable for the transfer to various substrate surfaces.And the monocrystalline of the centimetre-sized that existing method is prepared, preparation process quite expends time in, and cannot shift to other substrate.
4. improved unperturbed tranfer system is spontaneous process, can effectively avoid human factor disturbance to colloid monocrystalline in transfer process.
5. improved unperturbed transfer method is all suitable for having the substrate of different close and distant water surfaces and curvature, has wide range of applications.
Accompanying drawing explanation
Fig. 1 be take the two-dimensional colloidal monocrystalline that polystyrene particle that particle dia is 1.4 μ m makes as model particle in the embodiment 1 that obtains of scanning electronic microscope.
Fig. 2 be take the two-dimensional colloidal monocrystalline that polystyrene particle that particle dia is 1.4 μ m makes as model particle in the embodiment 2 that obtains of scanning electronic microscope.
Fig. 3 is for by example 2(Fig. 3 a-e) and 3(Fig. 3 f-j) the big area zero defect two-dimensional colloidal crystalline substance prepared transfers in substrate of glass the optical photograph of laser light diffraction pattern afterwards.
For the big area zero defect two-dimensional colloidal crystalline substance that obtains by example 2 is transferred to hydrophobic polyvinyl chloride through improved unperturbed transfer method, (Fig. 4 a) substrate and diameter is 1mm to Fig. 4, and surface coverage has the stereoscan photograph after copper cash (Fig. 4 b) substrate of polyvinyl chloride.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.But protection scope of the present invention is not limited only to following examples.According to content disclosed by the invention, those skilled in the art will recognize that in the situation that do not depart from the given technical characterictic of technical solution of the present invention and scope, the above embodiment is made many variations and revised all belong to protection scope of the present invention.
Embodiment 1:
It is the monodisperse spherical polystyrene particle of 1.4 μ m that raw material adopts diameter, sodium laurylsulfonate, ethanol, butanols, pure water.Wherein, take pure water consumption as benchmark, sodium laurylsulfonate concentration is 17.9mg/mL; In colloidal particle suspension system, the ratio of ethanol and butanols is 1:7(v:v), take dibasic alcohol consumption as benchmark, the concentration of colloidal particle is 30.0mg/mL.First colloidal particle is scattered in to dibasic alcohol dispersion medium, after ultrasonic being uniformly dispersed, dropwise drips to the pure water surface that is dissolved with sodium laurylsulfonate.When dropping is dispersed with colloidal particle suspension, by a flat nozzle, to the water surface, impose air-flow (flow 6.0L/min), after colloidal particle is paved with the whole water surface, colloidal particle is no longer with air motion.Increase air flow rate (10.0L/min), by container bottom, move left and right nozzle and drive colloidal film integral body to move forward, until obtain a colloidal film that is similar to minute surface, slowly move forward nozzle, make the above-mentioned colloidal film that is minute surface extend to whole water/gas interface.
The colloid monocrystalline of above-mentioned preparation is transferred in substrate of glass by improved unperturbed tranfer system and use the field emission scanning electron microscope of Japanese HITACHI company to observe.Fig. 1 is that in the embodiment 1 that obtains of scanning electronic microscope, to take the polystyrene particle that particle dia is 1.4 μ m be model particle, sodium laurylsulfonate concentration be the two-dimensional colloidal monocrystalline prepared in 17.9mg/mL situation photo, photo size is 120 * 80 μ m
2.
Embodiment 2:
It is the monodisperse spherical polystyrene particle of 1.4 μ m that raw material adopts diameter, sodium laurylsulfonate, ethanol, butanols, pure water.Wherein, take pure water consumption as benchmark, sodium laurylsulfonate concentration is 35.7mg/mL; In colloidal particle suspension system, the ratio of ethanol and butanols is 1:7(v:v), take dibasic alcohol consumption as benchmark, the concentration of colloidal particle is 30.0mg/mL.First colloidal particle is scattered in to dibasic alcohol dispersion medium, after ultrasonic being uniformly dispersed, dropwise drips to the pure water surface that is dissolved with sodium laurylsulfonate.When dropping is dispersed with colloidal particle suspension, by a flat nozzle, to the water surface, impose air-flow (flow 6.0L/min), after colloidal particle is paved with the whole water surface, colloidal particle is no longer with air motion.Increase air flow rate (10.0L/min), by container bottom, move left and right nozzle and drive colloidal film integral body to move forward, until obtain a colloidal film that is similar to minute surface, slowly move forward nozzle, make the above-mentioned colloidal film that is minute surface extend to whole water/gas interface.
The colloid monocrystalline of above-mentioned preparation transferred in substrate of glass by improved unperturbed tranfer system and use the laser beam vertical incidence that the field emission scanning electron microscope observation of Japanese HITACHI company the spot diameter of take are 3mm, adopting digital camera to record diffraction pattern.Fig. 2 is that in the embodiment 2 that obtains of scanning electronic microscope, to take the polystyrene particle that particle dia is 1.4 μ m be model particle, sodium laurylsulfonate concentration be the two-dimensional colloidal monocrystalline prepared in 35.7mg/mL situation photo, photo size is 120 * 80 μ m
2.For the big area zero defect two-dimensional colloidal crystalline substance that obtains by example 2 is transferred to hydrophobic polyvinyl chloride through improved unperturbed transfer method, (Fig. 4 a) substrate and diameter is 1mm to Fig. 4, and surface coverage has the stereoscan photograph after copper cash (Fig. 4 b) substrate of polyvinyl chloride.Photo size is 120 * 80 μ m
2.Clearly, by improved unperturbed tranfer system, can realize in the situation that colloid monocrystalline not being produced to obvious disturbance the transfer to different base surface.
Embodiment 3:
It is the monodisperse spherical polystyrene particle of 0.8 μ m that raw material adopts diameter, sodium laurylsulfonate, ethanol, butanols, pure water.Wherein, take pure water consumption as benchmark, sodium laurylsulfonate concentration is 35.7mg/mL; In colloidal particle suspension system, the ratio of ethanol and butanols is 1:7(v:v), take dibasic alcohol consumption as benchmark, the concentration of colloidal particle is 30.0mg/mL.First colloidal particle is scattered in to dibasic alcohol dispersion medium, after ultrasonic being uniformly dispersed, dropwise drips to the pure water surface that is dissolved with sodium laurylsulfonate.When dropping is dispersed with colloidal particle suspension, by a flat nozzle, to the water surface, impose air-flow (flow 6.0L/min), after colloidal particle is paved with the whole water surface, colloidal particle is no longer with air motion.Increase air flow rate (10.0L/min), by container bottom, move left and right nozzle and drive colloidal film integral body to move forward, until obtain a colloidal film that is similar to minute surface, slowly move forward nozzle, make the above-mentioned colloidal film that is minute surface extend to whole water/gas interface.
The colloid monocrystalline of above-mentioned preparation is transferred to and in substrate of glass, be take the laser beam vertical incidence that spot diameter is 3mm by improved unperturbed tranfer system, and record diffraction pattern with digital camera.Fig. 3 is for by example 2(Fig. 3 a-e) and 3(Fig. 3 f-j) the big area zero defect two-dimensional colloidal crystalline substance prepared transfers in substrate of glass the optical photograph of laser light diffraction pattern afterwards.Laser beam diameter used is 3mm.When laser beam vertical incidence, almost in whole substrate, can obtain regular hexagon diffraction pattern as shown in the figure, what show that method thus obtains is a monoblock colloid monocrystalline.
Claims (8)
1. the flawless two-dimensional colloidal monocrystalline of big area, is characterized in that, whole colloid crystal face is long-pending can reach several square centimeters and without any defect.Preferably, two-dimensional colloidal monocrystalline size reaches 10cm
2.
2. two-dimensional colloidal monocrystalline according to claim 1, is characterized in that, described two-dimensional colloidal monocrystalline consists of the monodisperse polymer or the inorganics spheroidal particle that are of a size of micron or submicron order.Preferably, take polymer spherical particle as model particle.
3. according to the two-dimensional colloidal monocrystalline described in claim 1-2 any one, its feature is, two-dimensional colloidal monocrystalline is to form under the booster action at compressed air stream in water/gas interface.Preferably, colloidal particle is the close heap close-packed arrays of six sides at water/gas interface.
4. according to the two-dimensional colloidal monocrystalline of claim 1-3 any one, it is characterized in that, the raw material of preparing described two-dimensional colloidal monocrystalline comprises colloidal particle, alcohols dispersion medium, ionic emulsifying agent and pure water.
Preferably, described colloidal particle is polymkeric substance or the inorganics spherocolloid particle of micron or submicron-scale.
Preferably, the consumption of described alcohols dispersion medium of take is benchmark, and the concentration of colloidal particle is 5-50mg/mL.
Preferably, described alcohols dispersion medium particular methanol, the binary dispersion system that ethanol or propyl alcohol and butanols form; With described methyl alcohol, the consumption of ethanol or propyl alcohol is benchmark, and the 3-9 that the consumption of butanols is for the former doubly.
Preferably, the consumption of pure water of take is benchmark, and the consumption of ionic emulsifying agent is 17.8-72.6mg/L.
5. according to the preparation method of the big area zero defect two-dimensional colloidal monocrystalline described in claim 1-4 any one, it is characterized in that, described method comprises the steps:
(1) monodispersed colloidal particle is scattered in to dibasic alcohol mixed system, forms stable suspension (preferably by ultrasonic dispersion);
(2) by the hanging drop in step (1) to the water surface, simultaneously to the water surface, be aided with compressed air stream (airshed 3-6L/min) and drive colloidal particle to move at the water surface, until the whole water surface is paved with colloidal particle;
；
(3) after the water surface is paved with colloidal particle, increase air flow rate (being for example controlled at 8-12L/min), drive the colloidal film being formed by colloidal particle to travel forward and finally at the flawless two-dimensional colloidal monocrystalline of water/gas interface formation big area.
6. preparation method according to claim 5, is characterized in that, the transfer of described two-dimensional colloidal single crystal direction substrate surface is by the spontaneous deposition process implementation based on capillary force mediation.
7. according to the unperturbed transfer method of the two-dimensional colloidal monocrystalline described in claim 1-4 any one, it is characterized in that, described method comprises the steps:
(1) before two-dimensional colloidal monocrystalline is prepared at water/gas interface, substrate is close to wall and is immersed in the water, by step described in claim 5 or 6, at water/gas interface, prepare afterwards large-area two-dimensional colloid monocrystalline;
(2) along wall, drip pure water to break being connected between other three of brilliant and walls of two-dimensional colloidal;
(3) water siphon is gone out to container (for example flow control is at 5-30mL/min), two-dimensional colloidal monocrystalline deposits from being sent to the remaining wall face that is glued with substrate, thereby realizes two-dimensional colloidal monocrystalline from the based transfer in water/gas interface.
8. according to the unperturbed transfer method of the two-dimensional colloidal monocrystalline of claim 7, it is characterized in that, described method does not produce obvious disturbance to two-dimensional colloidal monocrystalline and is applicable to have the substrate of different close and distant water surfaces and curvature.
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| CN1512179A (en) * | 2002-12-30 | 2004-07-14 | 中国科学院化学研究所 | Particle formwork and particle assembling and transferring method |
| CN101318618A (en) * | 2008-06-17 | 2008-12-10 | 东南大学 | Process for producing one-dimensional nano material film removing orientation by solution |
| CN101497067A (en) * | 2009-01-16 | 2009-08-05 | 北京航空航天大学 | Preparation method for assembling large-area ordered microsphere template by liquid level swirl method |
| CN102826505A (en) * | 2012-09-19 | 2012-12-19 | 电子科技大学 | Self-assembly preparation method of colloidal microsphere single-layer film |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1512179A (en) * | 2002-12-30 | 2004-07-14 | 中国科学院化学研究所 | Particle formwork and particle assembling and transferring method |
| CN101318618A (en) * | 2008-06-17 | 2008-12-10 | 东南大学 | Process for producing one-dimensional nano material film removing orientation by solution |
| CN101497067A (en) * | 2009-01-16 | 2009-08-05 | 北京航空航天大学 | Preparation method for assembling large-area ordered microsphere template by liquid level swirl method |
| CN102826505A (en) * | 2012-09-19 | 2012-12-19 | 电子科技大学 | Self-assembly preparation method of colloidal microsphere single-layer film |
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