CN101717994B - Method for preparing large-area single-domain two-dimensional colloidal crystal - Google Patents
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- CN101717994B CN101717994B CN2009102326048A CN200910232604A CN101717994B CN 101717994 B CN101717994 B CN 101717994B CN 2009102326048 A CN2009102326048 A CN 2009102326048A CN 200910232604 A CN200910232604 A CN 200910232604A CN 101717994 B CN101717994 B CN 101717994B
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- 239000013078 crystal Substances 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 49
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 9
- 230000000737 periodic effect Effects 0.000 claims abstract description 7
- 238000001704 evaporation Methods 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- 239000011806 microball Substances 0.000 claims description 14
- 235000012239 silicon dioxide Nutrition 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 4
- 229960001866 silicon dioxide Drugs 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 2
- 239000004005 microsphere Substances 0.000 abstract description 5
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000008204 material by function Substances 0.000 abstract 1
- 239000011664 nicotinic acid Substances 0.000 abstract 1
- 230000005693 optoelectronics Effects 0.000 abstract 1
- 239000000084 colloidal system Substances 0.000 description 27
- 239000004793 Polystyrene Substances 0.000 description 15
- 229920002223 polystyrene Polymers 0.000 description 15
- 238000001000 micrograph Methods 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 239000011324 bead Substances 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 240000007762 Ficus drupacea Species 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- 238000000151 deposition Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 230000005499 meniscus Effects 0.000 description 1
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- 238000004528 spin coating Methods 0.000 description 1
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a method for preparing a large-area single-domain two-dimensional colloidal crystal, which comprises the following steps of: firstly, placing and fixing two substrates at certain angle to form a wedge-shaped micro cavity; injecting a turbid liquid of monodisperse colloidal microspheres into the wedge-shaped micro cavity; standing the wedge-shaped micro cavity and evaporating the liquid in the wedge-shaped micro cavity, wherein the monodisperse colloidal microspheres are self organized on a contact line of a liquid dry interface and the substrates when driven by capillary force to form an ordered structure; and finally, obtaining the large-area single-domain two-dimensional colloidal crystal on the substrates after the liquid is completely dry. The preparation method is simple, low in cost and easy to manufacture; and the prepared colloidal crystal has the advantages of good single domain property, large area and the like. The method is favorable for preparing novel micro, nano periodic structures and novel optoelectronic devices and has important application value in the field of photoelectric functional materials, nano photonic materials, bionic materials, biochemistry sensing and the like.
Description
Technical field
The present invention relates to a kind of preparation method of Nano/micron fine structure material, be specifically related to a kind ofly can obtain large-area single-domain two-dimensional colloidal crystal and preparation method with low cost, maneuverable single-domain two-dimensional colloidal crystal.
Background technology
At present, fine structure material because its distinctive physical properties and aspect the photoelectric functional device application prospects, and get more and more people's extensive concerning.How preparing the big area fine structure material efficiently and effectively is the hot issue that people pay close attention to all the time.The method of preparation cycle property fine structure material can be divided into micro-processing method and self-organizing method substantially.Compare with micro-processing method, the method technology that the colloidal crystal that utilizes monodispersed colloid micro ball to organize themselves into obtains the two-dimensional and periodic microstructure is simple, with low cost.But up to now; The two-dimensional colloidal crystal of preparation large-area single-domain (the orderly area of single domain reaches centimeter scale) remains a technical difficult problem; Existing method can't prepare the colloidal crystal of large-area single-domain, this to a great extent limit the application of two-dimensional colloidal crystal.
The colloidal crystal preparation principle roughly is divided into the self-organization of colloid micro ball segregation drive, impressed field and drives self-organization, capillary force and drive convection current self-organization that self-organization, evaporation cause and the self-organization of pattern substrate inductive extension etc.Based on these principles, people have proposed the concrete preparation scheme of multiple colloidal crystal.These existing methods are very effective under some certain conditions, but also have certain limitation simultaneously.For example, pure rely on the gravity field effect (referring to K.E.Davis, W.B.Russel; W.J.Glantschnig, Science, 245; 507 (1989) .) often contain the more point or the polycrystalline of plane defect in the colloidal crystal for preparing; Crystalline thickness is restive, and preparation cycle is longer, is not suitable for the self-organization of those self gravitations greater than the colloid micro ball of the buoyancy in suspension-s; Realize that through extra electric field the method for colloidal spheres self-organization depends on the existence of electric field, after electric field was cancelled, the order of colloidal crystal also disappeared (referring to S.O.Lumsdon immediately; E.W.Kaler, J.P.Williams, O.D.Velev; Appl.Phys.Lett.82,949, (2003) .); Spin-coating method can prepare the big area colloidal crystal fast, but have no farmland that mechanism controls colloidal crystal to (referring to J.C.Hulteen, R.P.Van Duyne, J.Vac.Sci.Technol.A, 13,1553, (1995) .); The preparing method's vibrations condition to external world that lifts substrate or drag substrate based on machinery has very strict requirement; The problem of not basic simultaneously solution colloidal crystal large-area single-domain property (referring to B.G.Prevo, O.D.Velev, Langmuir; 20,2099 (2004) .); Utilize the meticulous technology of controlling; For example nano-machine hand (Nano-robotic manipulation) can be arranged in very perfectly structure with colloid micro ball; But poor efficiency and to the height of instrument and the requirement controlled be self-evident (referring to F.Garcia-Santamaria, et, al; Adv.Mater.14,1144 (2002) .).In the power-actuated self-organization mechanism of capillary attraction, colloid micro ball has formation close-packed direction to be parallel to the trend of the structure of liquid dried liquid level and substrate intersection., owing to can not control the shape of dry interface meniscus, the number of plies of the colloidal crystal that is grown alters a great deal based on this machine-processed vertical deposition method; And can't grow the single farmland of big area to colloidal crystal (referring to P.Jiang; J.F.Bertone, K.S.Hwang, V.L.Colvin; Chem.Mater.11,2132 (1999) .).Same reason, promptly the osculatory of liquid dried forward position and substrate is a camber line, the colloid monolayer crystal that the wet plate method under another kind of capillary force drives is prepared also has multiple farmland to (referring to N.D.Denkov; O.D.Velev, P.A.Kralchevsky, I.B.Ivanov; H.Yoshimura; K.Nagayama, Langmuir 8,3183 (1992) .).Based on the colloidal crystal preparation method (patent No. is 200410041939) of rectangular parallelepiped microcavity though can effectively prepare uniform two-dimensional colloidal crystal; But the formed osculatory of dry interface and substrate also is an arc line type in crystal growing process, also is difficult to grow the colloidal crystal of large-area single-domain.
Summary of the invention
Goal of the invention: in order to overcome the deficiency that exists in the prior art, the present invention provides a kind of can obtain large-area single-domain two-dimensional colloidal crystal and the preparation method with low cost, maneuverable large-area single-domain two-dimensional colloidal crystal that size breaks through centimeter scale.
Technical scheme: to achieve these goals, the preparation method of a kind of large-area single-domain two-dimensional colloidal crystal of the present invention may further comprise the steps:
(1) with first substrate and second substrates at certain angle placement and fixing, forms a wedge-shaped micro cavity;
(2) suspension liquid with single dispersoid microballoon injects in the wedge-shaped micro cavity;
(3) wedge-shaped micro cavity is left standstill, self-organization takes place in the liquid evaporation in the wedge-shaped micro cavity, the single dispersoid microballoon osculatory place at liquid dried interface and first substrate and second substrate under the driving of capillary force effect, forms ordered structure;
(4) after liquid evaporates fully, device is taken apart, on substrate, obtained large-area single-domain two-dimensional colloidal crystal.
Angle in the said step (1) is greater than 0 ° of angle less than 5 °.
Said first substrate and second substrate are smooth substrate or the pattern substrate for having periodic relief.
The material of said single dispersoid microballoon is polymkeric substance or silicon-dioxide or titanium oxide, and single dispersoid diameter of micro ball is between 200nm～10 μ m, and the monodispersity of the size of single dispersoid microballoon is less than 5%.
The osculatory of the said liquid dried interface and first substrate and second substrate is the straight line that is parallel to the intersection of two substrates.
The orderly area of said single-domain two-dimensional colloidal crystal single domain can be broken through centimeter scale, and the structural parameter of single-domain two-dimensional colloidal crystal are determined by the dry forward position of liquid and the structure of substrate jointly.
Beneficial effect: the preparation method of a kind of large-area single-domain two-dimensional colloidal crystal of the present invention; Because the introducing of wedge shape capillary microcavity; The osculatory of can controlled liq dry interface and substrate is parallel to the intersection of two substrates, thus the farmland of the colloidal crystal that control growing goes out to; Because use microcavity, the better evaporation of controlled liq grows even successive colloid monolayer crystal; Can realize the epitaxy of colloidal crystal through the substrate that use has a periodic patterns, obtain to have other symmetric two-dimensional colloidal crystals except that hexagonal solid matter symmetry; Present method is taked the drying mode that leaves standstill, do not use any lift or hold in the palm drag machinery, the process of self-organization of microballoon is not disturbed, can guarantee the high-sequential of colloidal crystal; Present method is not high to equipment, environment requirement, and is with low cost, easy handling.
Description of drawings
Fig. 1 is a wedge-shaped micro cavity structural representation of the present invention;
Fig. 2 is the optical photograph behind the injection colloid micro ball suspension liquid in the wedge-shaped micro cavity of the present invention;
Fig. 3 is the synoptic diagram of single dispersoid microballoon process of self-organization in wedge-shaped micro cavity among the present invention;
Fig. 4 is that prepared what go out is the monodisperse polystyrene colloid microballoon of 1.58 μ m is arranged the two-dimensional colloidal crystal that forms by the close heap dot matrix of hexagonal electron scanning micrograph by diameter in the present invention;
Fig. 5 is that prepared what go out is the monodisperse polystyrene colloid microballoon of 1.58 μ m is arranged the two-dimensional colloidal crystal that forms by the close heap dot matrix of hexagonal optical microscope photograph by diameter corresponding to the present invention of Fig. 4;
Fig. 6 is that prepared what go out is the monodisperse polystyrene colloid microballoon of 1.58 μ m is arranged the two-dimensional colloidal crystal that forms by the close heap dot matrix of hexagonal optical photograph by diameter corresponding to the present invention of Fig. 4;
Fig. 7 is that prepared what go out is the monodisperse polystyrene colloid microballoon of 1.58 μ m is arranged the two-dimensional colloidal crystal that forms by the hexagonal closed-paked lattice laser diffraction style by diameter corresponding to the present invention of Fig. 6;
Fig. 8 is that prepared what go out is the monodisperse silica colloid micro ball of 403nm is arranged the two-dimensional colloidal crystal that forms by the close heap dot matrix of hexagonal electron scanning micrograph by diameter in the present invention;
Fig. 9 be the present invention on the substrate with one dimension periodic undulations (cycle is 730nm), be the two-dimension square structure colloid crystalline electron scanning micrograph that the monodisperse polystyrene colloid microballoon of 1.02 μ m is prepared by diameter.
Embodiment
Below in conjunction with accompanying drawing the present invention is done explanation further.
Embodiment 1: as shown in Figure 1, and smooth quartz substrate 1 is fixed with 1 ° of angle with smooth quartz substrate 2, and support by upholder 3, form the device of a wedge-shaped micro cavity; The suspension liquid of single dispersoid microballoon is injected in the wedge-shaped micro cavity; Fig. 2 is the optical photograph of wedge-shaped micro cavity device of the present invention; White portion is the single dispersoid microballoon suspension liquid that injects in the wedge-shaped micro cavity; Single dispersoid microballoon is monodisperse polystyrene colloid microballoon (dispersiveness is 1%), and its diameter is 1.58 μ m; After single dispersoid microballoon suspension liquid injection wedge-shaped micro cavity; The wedge-shaped micro cavity device is left standstill; The room temperature normal pressure kept down after 5～8 hours, liquid complete drying, the two-dimentional large-area single-domain colloidal crystal with hexagonal solid matter structure that has the self-organization of polystyrene colloid microballoon to form on the substrate; Its cycle equals the polystyrene colloid diameter of micro ball, i.e. 1.58 μ m.Fig. 3 is the synoptic diagram of single dispersoid microballoon process of self-organization in wedge-shaped micro cavity among the present invention, and dotted line is illustrated the position at dry interface among the figure, and this dotted line is parallel to the intersection of two substrates, and arrow is illustrated dry interface direction of propulsion; The next organizational form of bead is illustrated at the interface of the colloid micro ball array that Dark grey bead signal has been organized, light grey bead.Fig. 4 is that prepared in the present embodiment what go out is the monodisperse polystyrene colloid microballoon of 1.58 μ m is arranged the two-dimensional colloidal crystal that forms by the hexagonal closed-paked lattice electron scanning micrograph by diameter.Fig. 5 be corresponding to Fig. 4 be that the monodisperse polystyrene colloid microballoon of 1.58 μ m is arranged the optical microscope photograph of the two-dimensional colloidal crystal form by the hexagonal closed-paked lattice by diameter, this photo has shown that the prepared colloidal crystal that goes out of the present invention has the characteristic of large-area single-domain.Fig. 6 is that the monodisperse polystyrene colloid microballoon of 1.58 μ m is arranged the optical photograph of the two-dimensional colloidal crystal that forms by the close heap dot matrix of hexagonal corresponding to Fig. 4's by diameter, and this photo demonstrates uniform color and luster.Fig. 7 is that spot diameter is the laser diffraction style that the laser of 1mm obtains during the scanning of path shown in the dotted line in Fig. 6; The spacing that the pairing laser facula of adjacent style is radiated at position on the colloidal crystal is 2.5mm, and diffraction pattern reflects the large-area single-domain property that sample is fabulous.
Embodiment 2: present embodiment and embodiment 1 are basic identical, but smooth quartz substrate 1 is 5 ° with smooth quartz substrate 2 angulations, and the cycle that still obtains is the two-dimensional colloidal crystal with hexagonal solid matter structure and large-area single-domain of 1.58 μ m.
Embodiment 3: present embodiment and embodiment 1 are basic identical; But single dispersoid micro-sphere material of selecting for use is a silicon-dioxide; Its diameter is 403nm, and obtaining by the cycle that the monodisperse silica colloid micro ball that is in contact with one another constitutes is the two-dimensional colloidal crystal with hexagonal solid matter structure and large-area single-domain of 403nm.Fig. 8 is to be the monodisperse silica colloid micro ball of 403nm is arranged the two-dimensional colloidal crystal form by the hexagonal closed-paked lattice electron scanning micrograph by diameter in the present embodiment
Embodiment 4: present embodiment and embodiment 1 are basic identical, but the monodisperse polystyrene colloid microsphere diameter of selecting for use is 200nm, and the cycle of obtaining is the two-dimensional colloidal crystal with hexagonal solid matter structure and large-area single-domain of 200nm.
Embodiment 5: present embodiment and embodiment 1 are basic identical, but the monodisperse polystyrene microsphere diameter of selecting for use is 10 μ m, and dispersiveness is 5%, and the cycle of obtaining is the two-dimensional colloidal crystal with hexagonal solid matter structure and large-area single-domain of 10 μ m.
Embodiment 6: present embodiment and embodiment 1 are basic identical; But what select for use is the substrate (cycle is 730nm) with one dimension periodic undulations; The monodisperse polystyrene colloid diameter of micro ball of selecting for use is 1.02 μ m, and the cycle of obtaining is the two-dimensional colloidal crystal with square structure and large-area single-domain of 1.02 μ m.Fig. 9 is the electron scanning micrograph that the monodisperse polystyrene colloid microballoon is arranged the two-dimension square colloidal crystal that forms in the present embodiment.
The above only is a preferred implementation of the present invention; Be noted that for those skilled in the art; Under the prerequisite that does not break away from the principle of the invention, can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (4)
1. the preparation method of a large-area single-domain two-dimensional colloidal crystal is characterized in that this preparation method may further comprise the steps:
(1) first substrate (1) and second substrate (2) are pressed certain angle placement and fixing, this angle is 1 °～5 °, forms a wedge-shaped micro cavity, and said first substrate (1) and second substrate (2) are quartz substrate;
(2) suspension liquid with single dispersoid microballoon injects in the wedge-shaped micro cavity; The material of said single dispersoid microballoon is silicon-dioxide or PS; Single dispersoid diameter of micro ball is between 200nm～10 μ m, and the monodispersity of the size of single dispersoid microballoon is less than 5%;
(3) wedge-shaped micro cavity is left standstill, self-organization takes place in the liquid evaporation in the wedge-shaped micro cavity, the single dispersoid microballoon osculatory place at liquid dried interface and substrate under the driving of capillary force effect, forms ordered structure;
(4) after liquid evaporates fully, device is taken apart, on first substrate (1) and second substrate (2), obtained large-area single-domain two-dimensional colloidal crystal.
2. the preparation method of a kind of large-area single-domain two-dimensional colloidal crystal according to claim 1 is characterized in that: said first substrate (1) and second substrate (2) are for smooth substrate or for having the pattern substrate of one dimension periodic undulations.
3. the preparation method of a kind of large-area single-domain two-dimensional colloidal crystal according to claim 1, it is characterized in that: the osculatory of said liquid dried interface and first substrate (1) and second substrate (2) is the straight line that is parallel to the intersection of two substrates.
4. the preparation method of a kind of large-area single-domain two-dimensional colloidal crystal according to claim 1; It is characterized in that: the orderly area of said single-domain two-dimensional colloidal crystal single domain can be broken through centimeter scale, and the structural parameter of single-domain two-dimensional colloidal crystal are determined by the dry forward position of liquid and the structure of substrate jointly.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1487108A (en) * | 2003-07-28 | 2004-04-07 | �Ϻ���ͨ��ѧ | Ordered 2D and 3D nano structure metal material comprising hollow metal spheres and its prepn process |
| CN1605386A (en) * | 2004-09-10 | 2005-04-13 | 南京大学 | Method for preparing two-dimensional or three dimensional colloid crystal |
| CN101143709A (en) * | 2007-10-24 | 2008-03-19 | 南京大学 | Method for preparing two-dimension square colloidal crystal |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1487108A (en) * | 2003-07-28 | 2004-04-07 | �Ϻ���ͨ��ѧ | Ordered 2D and 3D nano structure metal material comprising hollow metal spheres and its prepn process |
| CN1605386A (en) * | 2004-09-10 | 2005-04-13 | 南京大学 | Method for preparing two-dimensional or three dimensional colloid crystal |
| CN101143709A (en) * | 2007-10-24 | 2008-03-19 | 南京大学 | Method for preparing two-dimension square colloidal crystal |
Non-Patent Citations (2)
| Title |
|---|
| Jie Sun et al..《Fabrication and light-transmission properties of monolayer square symmetric colloidal crystals via controlled convective self-assembly on 1D grooves》.《Advanced Materials》.2008,第20卷(第1期), * |
| 王振林.《Preparation and optical properties of photonic and plasmonic crystals using colloidal crystals as templates》.《2008介观光学及其应用研讨会论文集》.2008, * |
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