CN101497067A - Preparation method for assembling large-area ordered microsphere template by liquid level swirl method - Google Patents
Preparation method for assembling large-area ordered microsphere template by liquid level swirl method Download PDFInfo
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Abstract
The invention relates to technology for preparing large-area ordered microsphere template assembled by a liquid surface eddy method, which prepares monodisperse polystyrene microspheres from monodisperse polystyrene microsphere emulsion through dispersion polymerization. Firstly, a certain amount of ultrapure water is filled in an open container, and a clean hollow Teflon plastic ring is placed on the water surface, and a stable eddy is generated through the stirring of a magneton or by a small-sized air blowing device; secondly, the monodisperse polystyrene microsphere emulsion is dropwise added onto the eddy water surface by a microinjector till a compact microsphere layer is formed in the hollow Teflon plastic ring, the eddy liquid surface is reduced to horizontal plane and the turbid liquid under the liquid surface is discharged out and the ultrapure water is filled into the contained; and finally, a substrate is immersed under the liquid surface and then pulled out by a lifting and pulling device to be dried at 80 DEG C, and thus the ordered microsphere template is obtained. A dried primary array membrane-plated sample is immersed under the liquid surface again for secondary array membrane plating to obtain a double-layer array structure, and the operation is carried out repeatedly to obtain a multilayer microsphere array.
Description
Technical field
The present invention relates to a kind of preparation method of sequential 2 D microsphere template, be specifically related to a kind of preparation method of assembling large-area ordered microsphere template by liquid level swirl method.
Background technology
The sequential 2 D template is owing to its its specific structure has very high using value, be widely applied to fields such as catalysis, opto-electronic information technology, present mould plate technique mainly comprises AAO template, photoetching technique, electron beam lithography technology and microsphere template technology etc.The microsphere template technology is a kind of relatively economical, convenience and the practical masterplate technology that grows up over past ten years, and the live width of template is only relevant with the particle diameter of institute use microballoon, can reach nanoscale.The preparation method that report is used for obtaining the sequential 2 D polymer template mainly comprises methods such as settling methods, vertical deposition method, physical constraints method and interface film forming.
(1) settling methods: deposition under the gravitational field effect realizes that it is microsphere template preparation method the most simply and easily that colloid micro ball is arranged.It is from having comprised the process of the precipitation under the gravitational field, diffusion motion (Brownian movement) and crystallization relative complex such as (nucleation and nucleus growth processes) in essence.Its crucial governing factor is size, density and the sedimentation rate etc. of regulating colloid micro ball.In the ordinary course of things, as long as colloid micro ball size and density enough just can be arranged in colloidal crystal greatly under the gravity effect.Because it is enough slow that the deposition process under the gravitational field effect is wanted, microballoon just can deposit out and finish from changing mutually of disorder to order and form final oldered array.Thereby this method to prepare time of colloidal crystal generally longer, need several weeks and even several months the colloidal particles of submicron order could be precipitated fully usually and form orderly colloidal crystal.And when colloid micro ball size less (less than 0.5 μ m) or density and dispersant near the time system equilibrium state that disperses with deposition is arranged, it is more difficult or the time is longer to cause forming colloidal crystal.
(2) vertical deposition method: this method utilizes solvent evaporates and capillarity (or surface tension) to make colloid micro ball form orderly colloidal crystal, and the colloidal crystal thickness of preparation can and can form speed (or pull rate) by microballoon concentration and film from one deck to the tens layers and control.(111) crystal face of the colloidal crystal of this method preparation is parallel with substrate, and single-crystal region can extend to centimetre, so vertical deposition method is a kind of preparation high-quality, the common method of uniform large tracts of land colloidal crystal.Yet because microspherulite diameter is when bigger, the infall process of colloidal particle is faster than the volatilization process of solvent, and therefore this method is considered to only be applicable to the light and particle diameter microballoon less than 400nm.Moreover, this method is very responsive to such environmental effects, and environment temperature and humidity all will directly influence the evaporation rate (being the formation speed of film) of solvent, so this method is not a kind of stable and controllable microballoon aligning method easily.
(3) physical constraints method: people such as Xia utilize the physical restriction method to prepare high-quality colloidal crystal, the liquid phase dispersion of colloidal particles is injected in the liquid sample pond under ultrasound condition, and this pond is by two substrate of glass and makes template framework with photoresist constitute in a substrate.One side of framework has the passage of photoetching that solvent can be flowed out and limits the microballoon outflow.Because the diameter of ball is greater than the height of groove, microballoon is left in the pond and at N
2Order about formation (111) face under stream effect and the ultrasonication and be parallel to glass matrix surface FCC type cubic closest packing structure.The advantage of this method is that process is very fast relatively, and sample is regular, fine and close, order is good; The crystal self assembly number of plies can freely be controlled; The particle diameter magnitude range wide (10nm～10 μ m) that is suitable for; No matter the chemistry of colloidal particle constitutes and surface nature how, various colloidal particles all are suitable for, but that this method has related to is expensive, the photoetching technique of degree of precision requirement.
(4) interface becomes embrane method: when surface tension between the research and utilization microballoon makes microballoon form two-dimensional colloidal crystal on plane, Goldenberg etc. have obtained colloidal particle dexterously and have arranged monofilm in order on the interface of water/alkane, and have realized the transfer to the surface of solids.This liquid surface assemble method makes things convenient for and is not subjected to the restriction of colloidal particle particle size.Only according to people's such as Goldenberg research, drip film and move the very difficult ordered microsphere array that obtains large-area than densification of film at aqueous solution liquid level, particularly for the bigger microsphere particle of particle diameter, when its emulsion droplets is on the water surface, the inhomogeneities that the slow flowability of bulky grain will cause the liquid level particle to be arranged, and simple film transfer technology is easy to cause breaking of liquid level rete.
The preparation method of the orderly template of existing two-dimensional, the process complexity, preparation time is longer, and difficulty is big, conveniently, controllably prepares the sequential 2 D microsphere template of ad hoc structure, still has difficulty up to now.
Summary of the invention
Technology of the present invention is dealt with problems: overcome the deficiencies in the prior art, a kind of preparation method of assembling large-area ordered microsphere template by liquid level swirl method is provided.
Technical solution of the present invention is: a kind of technology of preparing of assembling large-area ordered microsphere template by liquid level swirl method may further comprise the steps:
(1) in an open-top receptacle, injects a certain amount of ultra-pure water, and on the water surface, place the hollow teflon plastic hoop of a cleaning.Whole device places on the magnetic stirring apparatus, and the stirring of magneton makes and produces a stable whirlpool on the water surface; Or the additional small-sized blowning installation of whole device, adopt mechanical pump that Compressed Gas is provided, the angle of regulating gas blow pipe blows to the water surface and produces a stable whirlpool.
(2) utilize micro syringe to be added drop-wise on the vortex water surface ultrasonic finely dispersed monodisperse polystyrene microsphere emulsion, when polystyrene microsphere is covered with hollow teflon plastic hoop, and stop to drip emulsion when forming the individual particle layer of one deck densification, and slowly reduce the magneton rotating speed until stopping.
(3) when the infundibulate liquid level of vortex is reduced into horizontal plane, water pipe is discharged subsurface troubled liquor and is injected ultra-pure water, at last with behind the substrate immersed in liquid level, utilizes the equipment that lifts that substrate is pulled out, and 80 ℃ are drying to obtain the individual layer ordered microsphere template.
(4) once more below the immersed in liquid level, adopt step (1) and (2) to carry out the array plated film second time in the sample of the dried array plated film of step (3), obtain double-deck array structure; So can obtain the micro-sphere array of multilayer repeatedly.
Wherein, described monodisperse polystyrene microsphere emulsion, the preparation of employing dispersion copolymerization method: with styrene is monomer, azodiisobutyronitrile (AIBN) is an initator, PVP (PVP) is a dispersant, the mixture of absolute ethyl alcohol and water is a decentralized medium, the preparation monodisperse polystyrene microsphere.Synthetic basic step is: PVP is dissolved in the decentralized medium, and puts into the 250ml there-necked flask and stir.Logical nitrogen protection; then the styrene that stirs and the mixed solution of AIBN are joined polymerisation in the there-necked flask; react 24h down at 70 ℃; suspension is centrifugal; remove supernatant liquor, add the ultrasonic dispersion of absolute ethyl alcohol then, centrifugal again; disperse, so triplicate obtains pure uniform ethanol dispersion polystyrene microsphere emulsion again.Wherein, the shared mass percent of above-mentioned each component is: decentralized medium 65%～90%, styrene 10%～35%, ethanol/water ratio 4%～50% in the decentralized medium; PVP2.0%～5.0% (with respect to amount of monomer), AIBN0.5%～4.0% (with respect to amount of monomer).
The particle size range of monodisperse polystyrene microsphere described in the said method is 600nm～7 μ m, by regulating the microballoon that proportioning and monomer introducing mode obtain different-grain diameter, wherein monomer introducing mode is divided into two kinds: disposablely topple over mode, promptly the mixed solution of styrene and AIBN is disposable pours in the there-necked flask; The drop rate regulative mode, promptly the mixed solution of styrene and AIBN is poured 20mL feed liquor control valve earlier into, utilizes the valve control to regulate drop rate.
The used equipment of lifting is self assembly equipment in the said method, is made up of speed governing pull end two parts of commercially available high-accuracy pulse wide range speed control device and repacking, and both are connected by electric wire.Wherein the modified segment of speed governing pull end 4 has added self-control square metal frame 1 for the metallic rod end, a metal beam 2 is installed in the metal frame indoor design, with copper wire 3 pull end rotating shaft 5 parts are linked to each other with metal beam one end, make metal beam in metal frame, slide up and down, a metal iron clamp is fixed in the outer end of metal beam, this metal iron clamp is used for fixing substrate, as shown in Figure 2.
Pull rate used in the said method is regulated and control by arrangements for speed regulation, and the range of speeds is 0～200rpm, and it is 0～0.12mm/s that correspondence lifts linear velocity.
The preparation method of a kind of assembling large-area ordered microsphere template by liquid level swirl method of the present invention, its advantage and effect are: the template preparation process is simple, easy operating, and its raw material source is extensive, this method stable and controllable, the new technique that is suitable as the high-quality microsphere template of preparation large tracts of land is promoted, and higher using value is arranged.
Description of drawings
Fig. 1 vortex liquid level construction from part prepares large tracts of land microballoon oldered array
Fig. 2 microsphere template preparation facilities schematic diagram
The surperficial SEM pattern and the cross section pattern of Fig. 3 microsphere template array.
Concrete label is as follows among the figure:
1, metal frame 2, metal beam 3, copper wire 4, speed governing pull end
5, rotating shaft 6, high-accuracy pulse wide range speed control device
The specific embodiment
The specific embodiment
The present invention is described in detail below in conjunction with the specific embodiment and accompanying drawing, sees also Fig. 1 and shown in Figure 3.
In the three-neck flask of 250ml, add 49.5ml ethanol and 4.88ml water and lgPVP mixed solution; water-bath is heated to 70 ℃; feed nitrogen protection; after stirring certain hour, adopts and disposablely topple over mode and add washing good styrene 5.5ml, initiator A IBN0.05g, the taking-up emulsion is centrifugal behind the reaction 24h; discard supernatant liquor; use the ethanol supersound washing, repeated multiple times, it is standby to collect final emulsion.Characterize through SEM, the microspherulite diameter of preparation is 1.33 μ m.In an open-top receptacle, inject a certain amount of ultra-pure water, and on the water surface, place the hollow teflon plastic hoop of a cleaning.Utilize the stirring of magneton to make stable whirlpool of generation on the water surface, to slowly drip in the surface of whirlpool shape deionized water with the PS microballoon emulsion that ethanol disperses, until the PS microballoon film that forms one deck densification on the surface of water, stop to stir, when the infundibulate liquid level of vortex is reduced into horizontal plane, water pipe is discharged subsurface troubled liquor and the injection ultra-pure water, at last with in the substrate immersed in liquid level, the utilization equipment that lifts adopts and to lift linear velocity and for 0.02mm/s substrate is pulled out, and 80 ℃ are drying to obtain ordered microsphere template.Shown in Fig. 3 (a) and (b).
In the three-neck flask of 250ml, add 91.14ml ethanol and 0.81g PVP mixed solution; water-bath is heated to 70 ℃; feed nitrogen protection; behind the stirring certain hour, adopt the rate of addition of 99.53 μ L/s to add washing good styrene 30.87ml, initiator A IBN 0.28g, the taking-up emulsion is centrifugal behind the reaction 24h; discard supernatant liquor; use the ethanol supersound washing, repeated multiple times, it is standby to collect final emulsion.Characterize through SEM, the microspherulite diameter of preparation is 5.21 μ m.In an open-top receptacle, inject a certain amount of ultra-pure water, and on the water surface, place the hollow teflon plastic hoop of a cleaning.Utilize the stirring of magneton to make stable whirlpool of generation on the water surface, to slowly drip in the surface of whirlpool shape deionized water with the PS microballoon emulsion that ethanol disperses, until the PS microballoon film that forms one deck densification on the surface of water, stop to stir, when the infundibulate liquid level of vortex is reduced into horizontal plane, water pipe is discharged subsurface troubled liquor and the injection ultra-pure water, at last with in the substrate immersed in liquid level, the utilization equipment that lifts adopts and to lift linear velocity and for 0.03mm/s substrate is pulled out, and 80 ℃ are drying to obtain ordered microsphere template.
In the three-neck flask of 250ml, add 86.08ml ethanol and 0.96g PVP mixed solution; water-bath is heated to 70 ℃; feed nitrogen protection; behind the stirring certain hour, the rate of addition of adopting 87 μ L/s adds washing good styrene 35.28ml, initiator A IBN0.32g, and the taking-up emulsion is centrifugal behind the reaction 24h; discard supernatant liquor; use the ethanol supersound washing, repeated multiple times, it is standby to collect final emulsion.Characterize through SEM, the microspherulite diameter of preparation is 7.09 μ m.In an open-top receptacle, inject a certain amount of ultra-pure water, and on the water surface, place the hollow teflon plastic hoop of a cleaning.Adopt the gas blow pipe adjusting angle to blow to the water surface and produce a stable whirlpool, to slowly drip in the surface of whirlpool shape deionized water with the PS microballoon emulsion that ethanol disperses, until the PS microballoon film that forms one deck densification on the surface of water, stop to stir, when the infundibulate liquid level of vortex is reduced into horizontal plane, water pipe is discharged subsurface troubled liquor and the injection ultra-pure water, at last with in the substrate immersed in liquid level, the utilization equipment that lifts adopts and to lift linear velocity and for 0.04mm/s substrate is pulled out, and 80 ℃ are drying to obtain ordered microsphere template.
Embodiment 4
In the three-neck flask of 250ml, add 49.5ml ethanol and 4.88ml water and 1g PVP mixed solution; water-bath is heated to 70 ℃; feed nitrogen protection; after stirring certain hour, adopts and disposablely topple over mode and add washing good styrene 5.5ml, initiator A IBN 0.05g, the taking-up emulsion is centrifugal behind the reaction 24h; discard supernatant liquor; use the ethanol supersound washing, repeated multiple times, it is standby to collect final emulsion.Characterize through SEM, the microspherulite diameter of preparation is 1.33 μ m.In an open-top receptacle, inject a certain amount of ultra-pure water, and on the water surface, place the hollow teflon plastic hoop of a cleaning.Adopt the gas blow pipe adjusting angle to blow to the water surface and produce a stable whirlpool, to slowly drip in the surface of whirlpool shape deionized water with the PS microballoon emulsion that ethanol disperses, until the PS microballoon film that forms one deck densification on the surface of water, stop to stir, when the infundibulate liquid level of vortex is reduced into horizontal plane, water pipe is discharged subsurface troubled liquor and the injection ultra-pure water, at last with in the substrate immersed in liquid level, the utilization equipment that lifts adopts and to lift linear velocity and for 0.04mm/s substrate is pulled out, and it is standby that 80 ℃ of dryings obtain adhering to the substrate of individual layer microsphere template.The open-top receptacle that cleans up is refilled ultra-pure water, adopt the gas blow pipe adjusting angle to blow to the water surface and produce a stable whirlpool, repeat the PS microballoon film that above-mentioned steps forms one deck densification, derive troubled liquor and inject ultra-pure water, in 80 ℃ of standby substrate immersed in liquid level in dry back, the utilization equipment that lifts adopts and to lift linear velocity and for 0.02mm/s substrate is pulled out, and 80 ℃ are drying to obtain double-deck ordered microsphere template.Shown in Fig. 3 (c), (d).
Claims (6)
1, a kind of preparation method of assembling large-area ordered microsphere template by liquid level swirl method is characterized in that: this method may further comprise the steps:
(1), in open-top receptacle, inject a certain amount of ultra-pure water, and on the water surface, place the hollow teflon plastic hoop of a cleaning, make and produce a stable whirlpool on the water surface;
(2), utilize micro syringe to be added drop-wise on the vortex water surface ultrasonic finely dispersed monodisperse polystyrene microsphere emulsion, when polystyrene microsphere is covered with hollow teflon plastic hoop, and stop to drip emulsion when forming the individual particle layer of one deck densification, and slowly reduce the magneton rotating speed until stopping;
(3), when the infundibulate liquid level of vortex is reduced into horizontal plane, water pipe is discharged subsurface troubled liquor and is injected ultra-pure water, at last with behind the substrate immersed in liquid level, utilizes the equipment that lifts that substrate is pulled out, 80 ℃ are drying to obtain the individual layer ordered microsphere template;
(4), once more below the immersed in liquid level, adopt step (1) and (2) to carry out the array plated film second time in the sample of the dried array plated film of step (3), obtain double-deck array structure; So can obtain the micro-sphere array of multilayer repeatedly.
2, preparation method according to claim 1, it is characterized in that: described monodisperse polystyrene microsphere emulsion adopts the dispersion copolymerization method preparation, concrete grammar is as follows: be monomer with styrene, azodiisobutyronitrile is an initator, PVP is a dispersant, and the mixture of absolute ethyl alcohol and water is a decentralized medium; PVP is dissolved in the mixed solution that the second alcohol and water is formed, and puts into there-necked flask and stir; Logical nitrogen protection, then the styrene that stirs and the mixed solution of azodiisobutyronitrile are joined polymerisation in the there-necked flask, react 24h down at 70 ℃, suspension is centrifugal, remove supernatant liquor, add the ultrasonic dispersion of absolute ethyl alcohol then, centrifugal again, disperse, so triplicate obtains pure uniform ethanol dispersion polystyrene microsphere emulsion again; Wherein, decentralized medium 65%～90%, styrene 10%～35%, ethanol/water ratio 4%～50% in the decentralized medium, PVP is 2.0%～5.0% with respect to amount of monomer, azodiisobutyronitrile is 0.5%～4.0% with respect to amount of monomer.
3, preparation method according to claim 2, it is characterized in that: described monodisperse polystyrene microsphere particle size range is 600nm～7 μ m, by regulating the microballoon that proportioning and monomer introducing mode obtain different-grain diameter, wherein monomer introducing mode is divided into two kinds: disposablely topple over mode, promptly the mixed solution of styrene and azodiisobutyronitrile is disposable pours in the there-necked flask; The drop rate regulative mode, promptly the mixed solution of styrene and azodiisobutyronitrile is poured 20mL feed liquor control valve earlier into, utilizes the valve control to regulate drop rate.
4, preparation method according to claim 1 is characterized in that: the described equipment that lifts is made up of speed governing pull end two parts of high-accuracy pulse wide range speed control device and repacking, and both are connected by electric wire; Wherein the modified segment of speed governing pull end is the terminal additional square metal frame of metallic rod, the inner metal beam of installing of metal frame, with copper wire pull end rotating shaft part is linked to each other with metal beam one end, make metal beam in metal frame, slide up and down, a metal iron clamp is fixed in the outer end of metal beam, and this metal iron clamp is used for fixing substrate.
5, preparation method according to claim 4 is characterized in that: described high accuracy pulsewidth speed arrangements for speed regulation, and the range of speeds is 0～200rpm, it is 0～0.12mm/s that correspondence lifts linear velocity.
6, preparation method according to claim 1 is characterized in that: described whirlpool is to produce by following two kinds of methods: one, whole device place on the magnetic stirring apparatus, and the stirring of magneton makes and produces a stable whirlpool on the water surface; Its two, at the additional small-sized blowning installation of whole device, adopt mechanical pump that Compressed Gas is provided, the angle of regulating gas blow pipe blows to the water surface and produces a stable whirlpool.
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