CN101597786B - Device and method for preparing colloidal crystal simple layer film - Google Patents
Device and method for preparing colloidal crystal simple layer film Download PDFInfo
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- CN101597786B CN101597786B CN2009100880886A CN200910088088A CN101597786B CN 101597786 B CN101597786 B CN 101597786B CN 2009100880886 A CN2009100880886 A CN 2009100880886A CN 200910088088 A CN200910088088 A CN 200910088088A CN 101597786 B CN101597786 B CN 101597786B
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Abstract
The invention provides a device and a method for preparing colloidal crystal simple layer film, and the method comprises the following steps: 1) setting temperature of a constant temperature device; 2) adding colloidal turbid liquid to a growth tube and facilitating the liquid level of the colloidal turbid liquid to be higher than the liquid level a first valve by at least 10cm; 3) fixing a substrate on the growth tube and open the first valve so as to facilitate the proportion of the height drop of the colloidal turbid liquid to account for 1/10:4 at most of height difference between the original liquid level of the colloidal turbid liquid and the first valve; closing the first valve after completion of growth. The method of the invention for preparing colloidal crystal simple layer film features high efficiency, easy control, simple operation and good repeatability, can be used to grow high quality and large area of colloidal crystal simple layer film in a very short time, in addition, the method is applicable to self-assembly of colloidal particles of varying particle sizes and types.
Description
Technical field
The invention belongs to field of nano material preparation, relate in particular to the device and method that a kind of self-assembly prepares colloidal crystal simple layer film.
Background technology
The unitary film that utilizes the colloid bead to constitute big area and perfect structure is one of the most attracting target in the nano material preparation always.It can be nano impression, and nano material growth, even the growth of common colloidal crystal provides a substrate that well has periodic structure is for the preparation of material provides a kind of good control measures.Therefore, the research of its preparation method has received extensive concern for a long time.The traditional preparation process method of colloidal crystal simple layer film mainly contains drip method, spin-coating method, crystal pulling method; But; It is tens of to micron dimensions up to a hundred that the sample monocrystalline area of these methods preparation only can reach, and macroscopic defects (being blanking bar, different structure zonal arrangement) and microdefect (point defect, dislocation, multilayered structure) are more on the sample.
The vertical self-assembly method of colloidal crystal is by people's broad research in recent years; The Continuous Convective Assembling of Fine Particles intoTwo-Dimensional Arrays on Solid Surfaces that delivers referring to K.Nagayama etc.; Langmuir, volume was 1303 pages in 1996 the 12nd.This method is under certain temperature and humidity condition; Substrate is vertically inserted in the suspension liquid of single dispersion colloid particle; Utilize that liquid meniscus place solvent evaporation inductive liquid convection is transported to substrate with colloidal solid on the substrate; And utilize the Interglobular side direction capillary force of colloid that it is arranged in orderly close-packed structure, thereby form the film that colloid micro ball is formed.The speed that adopts the step motor control substrate upwards to lift in the literary composition makes it consistent with the colloidal crystal speed of growth, thereby obtains colloidal crystal simple layer film.The shortcoming of this method is the control section more complicated, and cost is higher, and the stepper-motor rate of pulling is not continuously adjustable, can not realize the purpose of high quality, big area colloidal crystal simple layer film.
On this basis, people such as X.S.Zhao are (referring to the Flow-ControlledVertical Deposition Method for the Fabrication of Photonic Crystals that X.S.Zhao etc. delivers, Langmuir; Volume was 1524 pages in 2004 the 20th) adopt peristaltic pump to come the colloid bead suspension liquid in the extraction system; Liquid level is descended, control the fall off rate of suspension liquid liquid level, but caused mechanical vibration meeting has influence on the quality and the area of the prepared single crystal film that goes out during peristaltic pump work through the extraction speed of regulating peristaltic pump; In addition; This method is colloid suspension liquid large usage quantity when the growth sample, and cost is high, is inappropriate for scale operation.
Summary of the invention
The objective of the invention is to overcome the defective that exists in the above-mentioned prior art, provide that a kind of to be used for growing high-quality, big area and preparation technology simple to operate, the device and method of the colloidal crystal simple layer film that cost is low.
The objective of the invention is to realize through following technical scheme:
According to an aspect of the present invention, a kind of device that is used to prepare colloidal crystal simple layer film is provided, comprises substrate, comprise the growth tube and the thermostat of colloid suspension liquid; Wherein, Said growth tube is provided with first valve, is used for controlling said growth tube liquid level fall off rate, and the liquid level of said colloid suspension liquid is higher than said first valve at least about 10cm; Preferably, the liquid level of said colloid suspension liquid is higher than said first valve at least about 20cm.
In technique scheme, said growth tube also comprise do not dissolve each other with said colloid suspension liquid and than the big liquid of said colloid suspension liquid density, be said colloid suspension liquid, lower floor layered structure in order in growth tube, to form the upper strata for this liquid.Preferably, the length of the colloid suspension liquid on said upper strata equals substrate length.
In technique scheme, also comprise the characteristic infrared lamp that is arranged on said colloid suspension liquid top.
According to another aspect of the present invention, a kind of method for preparing colloidal crystal simple layer film that adopts one of said apparatus is provided, may further comprise the steps:
1) temperature of the said thermostat of setting;
2) add the colloid suspension liquid in said growth tube, and make the liquid level of said colloid suspension liquid be higher than said first valve at least about 10cm;
3) fixing said substrate is opened said first valve, so that the height drop-out value of said colloid suspension liquid accounts for the former liquid level of colloid suspension liquid and the ratio of the difference of altitude between first valve is at most 1/10 in said growth tube;
4) treat that growth finishes, and closes first valve.
In technique scheme, said step 2) liquid level of colloid suspension liquid is higher than said first valve at least about 20cm described in.
In technique scheme, said step 2) also comprise: add do not dissolve each other with said colloid suspension liquid and than in big liquid to the said growth tube of said colloid suspension liquid density.Further; Also comprise step 5): add and saidly not dissolve each other with the colloid suspension liquid; And in the big liquid of colloid suspension liquid density to said growth tube, so that the liquid level of colloid suspension liquid is raised to the height when not opening said first valve, repeating step 1 then) to step 3).
In technique scheme, said step 3) also comprises: the opening characteristics infrared light.
Compared with prior art, the invention has the advantages that:
1. additional vibrations have been avoided with the machinery extraction;
2. the consumption of colloid suspension liquid is considerably less when preparing, and cost is reduced, and helps scale operation;
3. prepared colloidal crystal quality is high, area is big, and has shortened growth cycle.
Description of drawings
Below in conjunction with accompanying drawing the present invention is done further explain, wherein:
Fig. 1 is the device synoptic diagram that is used to prepare colloidal crystal simple layer film according to preferred embodiment of the present invention;
Fig. 2 a and Fig. 2 b are that prepared according to one embodiment of present invention particle diameter is a 596nm polystyrene colloid crystal simple layer film SEM vertical view;
Fig. 3 a and Fig. 3 b are respectively that prepared according to another embodiment of the present invention particle diameter is 1 μ m polystyrene colloid crystal simple layer film SEM vertical view and sectional view;
Fig. 4 a is that prepared according to one embodiment of present invention particle diameter is a 596nm polystyrene colloid crystal simple layer film microphotograph;
Fig. 4 b is that prepared according to another embodiment of the invention particle diameter is 1 μ m polystyrene colloid crystal simple layer film microphotograph.
Embodiment
[embodiment 1]: the preparation particle diameter is the polystyrene colloid crystal simple layer film of 596nm
Fig. 1 is the device that is used to prepare colloidal crystal simple layer film according to preferred embodiment of the present invention; This device comprises: the growth tube 1 that comprises colloid suspension liquid (being polystyrene colloid bead suspension liquid) 7; Be fixed in the substrate 2 in the growth tube 1, be positioned at the constant temperature water bath apparatus 3 of growth tube 1 outside, it is used to control the body phase temperature of said colloid suspension liquid 7; And being arranged on first valve 5 on the growth tube 1 such as needle-valve, it is used for the liquid level fall off rate of control growing pipe 1; Wherein, the liquid level of said colloid suspension liquid 7 is higher than first valve, 5 about 10cm.
Preferably, growth tube 1 stretches out a part from the bottom of thermostat 3, and first valve 5 is arranged on the end (as shown in the figure) of growth tube 1 extension.Be appreciated that in other embodiments of the invention first valve 5 can also be set in place the growth tube 1 lateral arbitrary position under liquid level; If thermostat 3 can be made enough highly in the reality; Growth tube 1 also can be arranged in the thermostat 3; But in this case, should be from first valve, 5 effusive liquid through the outside of catheter guidance to thermostat 3, promptly flowing liquid can not enter into thermostat 3.Of the present invention this with other embodiment in; The liquid level of colloid suspension liquid 7 is higher than first valve 5 at least about 10cm; Preferably at least about 20cm, guaranteeing when the preparation colloidal crystal simple layer film, the ratio of original liquid level and the difference of altitude between first valve 5 that the height change value of colloid suspension liquid 7 accounts for colloid suspension liquid 7 is very little; Account for 1/10 at most, the fluid column in the growth tube 1 utilizes the stable and almost decline evenly of self gravitation in the preparation process under the very little situation of Level Change thereby make.The length that is appreciated that growth tube 1 is decided according to the liquid level of testing the colloid suspension liquid 7 that is adopted.
Preferably, growth tube 1 also comprises carbon tetrachloride solution 8 (CCl
4), because tetracol phenixin does not dissolve each other with said polystyrene colloid suspension liquid 7 and be bigger than its density, therefore in growth tube 1, forming the upper strata is that polystyrene colloid suspension liquid 7, lower floor are CCl
4Layered structure; In addition; Preferably, substrate 2 is identical with the length of colloid suspension liquid 7, so that whole substrate 2 just all is immersed in the colloid suspension liquid 7; And when the falling head of preparation colloid suspension liquid 7 during colloidal crystal simple layer film is the height of substrate, the consumption of colloid suspension liquid 7 when reducing preparation to greatest extent like this.
Preferably, the device that is used to prepare colloidal crystal simple layer film of the present invention also comprises side pipe 9, and it is arranged on the bottom of growth tube 1, with the CCl of lower floor
4Be connected, wherein be equipped with in this side pipe 9 with growth tube 1 in the liquid of lower floor, CCl for example
4, be used for carrying out the forward direction of colloidal crystal self-assembly next time growth tube 1 additional CCl
4Thereby the liquid level build-up that makes colloid suspension liquid 7 is to former height; Side pipe 9 has second valve 6 such as needle-valve, is used to control the CCl that flows into growth tube 1
4Flow.
Preferably, the device that is used to prepare colloidal crystal simple layer film of the present invention also comprises characteristic infrared lamp 4, and its luminous spectrum peak is between 2.7～3.3 μ m; And be arranged on 5～50cm place, top of colloid bead suspension liquid, make illumination be mapped to colloid bead suspension liquid surface, thereby accelerate the vaporator rate at colloid suspension liquid 7 growth front places; Change growth front place Flow Field Distribution, thereby form the single-layer membrane structure of high-sequential, in addition; Infrared luminous energy suppresses the generation of various defectives such as room, dislocation effectively; The colloidal crystal quality is improved, and shortened the growth cycle of unitary film, the unitary film of growth 1cm length is generally between 5-15 minute.
In technique scheme, the pipe that growth tube 1 and side pipe 9 can be processed for conventional materials such as glass or quartz; Substrate 2 can be slide glass, quartz glass plate, conductive glass sheet or silicon chip; CCl
4Can more greatly and not replace, like chloroform and partial ion liquid (like pyrrolidines) etc. by color density with the liquid that the colloid suspension liquid dissolves each other yet; Constant temperature water bath apparatus 3 can be replaced by other temperature-control devices; But first valve 5 and second valve 6 can also use the valve of the minute adjustment of other types to substitute, like micrometering valve, motorized valve, piezo electric valve etc.; Side pipe 9 can also use other fluid Supplying apparatus to substitute.
According to the device that preferably is used to prepare colloidal crystal simple layer film of the invention described above, it is the method for the polystyrene colloid crystal simple layer film of 596nm that the preparation particle diameter is provided, and this method may further comprise the steps:
1) open constant temperature water bath apparatus 3, design temperature is 45 ℃, after about 1 hour in the constant temperature water bath apparatus temperature uniform and stable, using deionized water to be mixed with volume(tric)fraction monodispersed polystyrene sphere is 2% colloid suspension liquid 7, ultra-sonic dispersion 20 minutes;
2) in growth tube 1, add CCl
4, liquid-column height is about 10cm, then the polystyrene colloid suspension liquid 7 that step 1) disposed is added in the growth tube 1 the about 1cm of its liquid-column height;
3) with the about 1mm of thickness, the slide glass 2 of the about 1cm of length is used deionized water and absolute ethyl alcohol ultrasonic cleaning respectively, is vertically fixed on the central authorities of growth tube 1, and it just is immersed in the polystyrene colloid suspension liquid 7; Open ir lamp, and appropriateness opens first valve 5, make CCl
4Slowly low, make the about 1cm of liquid level decline; Along with solvent evaporation and liquid level descend, polystyrene sphere carries out self-assembled growth on slide glass 2 surfaces;
4) treat that slide glass 2 all exposes from colloid bead suspension liquid 7, after about 13 minutes, close first valve 5, take out the slide glass 2 of growth polystyrene colloid crystal simple layer film.
Fig. 2 a and Fig. 2 b are that wherein Fig. 2 a is the middle section SEM of this film according to the prepared polystyrene colloid crystal simple layer film SEM vertical view of embodiments of the invention, and Fig. 2 b is the SEM of fringe region.Can find out that from Fig. 2 a and Fig. 2 b prepared particle diameter is that the polystyrene colloid crystal simple layer film of 596nm is higher in order, defect concentration is lower; Can find out that from the microphotograph of Fig. 4 a the area of this colloidal crystal simple layer film is greater than 0.16mm
2
Of the present invention this with other embodiment in, said step 2) in the liquid level of colloid suspension liquid 7 should be higher than first valve 5 at least about 10cm, preferably at least about 20cm; In the said step 3) height change value of colloid suspension liquid 7 account at most colloid suspension liquid 7 original liquid level and the difference of altitude between first valve 5 1/10, then can realize the object of the invention.Yet should be appreciated that to those skilled in the art be worth under the constant situation in height change, the liquid level of colloid suspension liquid 7 is high more, the effect that the present invention obtained is good more.Therefore the liquid level height peak that is higher than first valve can be confirmed according to equipment in the actually operating and processing condition.In addition, in said step 2) in the length of colloid suspension liquid 7 can make the two equal in length only make the consumption of colloid suspension liquid 7 littler in the technique scheme greater than substrate 2 length; Similarly, in said step 2) in can not add such as CCl
4Do not dissolve each other and, can realize the object of the invention equally than the big liquid of colloid suspension liquid 7 density with colloid suspension liquid 7.The step of opening characteristics ir lamp is merely preferably in said step 3), also can not open ir lamp, can realize the object of the invention equally.
As another embodiment of the invention, aforesaid method also comprises step 5): open second valve 6 of side pipe 9, in growth tube 1, add The addition of C Cl
4, so that make the liquid level of colloid suspension liquid 7 get back to original height, promptly do not open the liquid level of first valve, 5 preceding colloid suspension liquids 7, repeating step 1 then) to step 3), up to the film that obtains the required number of plies.
Except that the volume(tric)fraction of in technique scheme, mentioning that is dissolved in the deionized water is 2% polystyrene sphere, in other embodiments of the invention, can also use the colloid suspension liquid of other different contents and composition.For example, polystyrene sphere can be in the scope of 0.03～5.0wt% in colloidal solution; Polystyrene sphere can be substituted by be used to the grow bead of polystyrene sphere, silicon-dioxide bead and other nucleocapsid structure of polynary colloidal crystal of particle diameter by 140～1500nm; Said solvent can also be water and alcoholic acid mixing solutions or ethanol.
In the present invention, because CCl
4Do not dissolve each other and bigger than colloid suspension liquid 7 density with colloid suspension liquid 7; Work to hold colloid suspension liquid 7; Significantly reduced the consumption of the colloid suspension liquid 7 of growing required on the one hand; And because the consumption of each self-assembly bead is all considerably less, the volume(tric)fraction of bead is almost constant in each secondary growth process, for the homogeneity of colloidal crystal film provides favourable condition; On the other hand; Liquid-column height in the preparation process in the growth tube 1 changes very little; The height that colloid suspension liquid 7 descends when promptly preparing is the about 1/10 of difference of altitude between liquid level and first valve 5 of colloid suspension liquid 7 before the preparation, and utilizes can critically control such as first valve 5 of needle-valve and flow out CCl
4Flow velocity very slow, like this, make liquid level can be stably, almost descend evenly, thereby effectively control the motion of osculatory, optimize the macroscopic view and the microscopic property of colloidal crystal film.Therefore, method and apparatus of the present invention is particularly suitable for preparing high-quality colloidal crystal simple layer film.In addition, through precision control, the present invention also is fit to the high quality of the required number of plies of growth, big area colloidal crystal.
[embodiment 2]: the preparation particle diameter is the polystyrene colloid crystal simple layer film of 1 μ m
It is 1 μ m polystyrene colloid crystal simple layer film that embodiment 2 employings prepare particle diameter with embodiment 1 similar apparatus and method; The liquid level of colloid suspension liquid 7 was higher than first valve, 5 about 20cm before difference was to prepare, and prepared the required growth time of 1 μ m polystyrene colloid crystal simple layer film about 6 minutes.
Fig. 3 a and Fig. 3 b show SEM figure and the cross-sectional view that prepared particle diameter is the polystyrene colloid crystal simple layer film of 1 μ m respectively.Find out colloid bead marshalling among the figure significantly, the degree of order is higher, and the macroscopic view and the microdefect of unitary film are less, can find out also that from Fig. 4 b its area is greater than 2500 μ m
2
Although the present invention is made specific descriptions with reference to the above embodiments; But for the person of ordinary skill of the art; Should be appreciated that and to make amendment based on content disclosed by the invention within spirit of the present invention and the scope or improve not breaking away from, these modifications and improving all within spirit of the present invention and scope.
Claims (10)
1. device that is used to prepare colloidal crystal simple layer film comprises substrate, comprises the growth tube and the thermostat of colloid suspension liquid, it is characterized in that,
Said growth tube is provided with first valve, is used for controlling said growth tube liquid level fall off rate; The liquid level of said colloid suspension liquid is higher than said first valve 10cm at least, and the height drop-out value of said colloid suspension liquid accounts for the liquid level of former colloid suspension liquid and the ratio of the difference of altitude between first valve is at most 1/10.
2. the device that is used to prepare colloidal crystal simple layer film according to claim 1 is characterized in that, the liquid level of said colloid suspension liquid is higher than said first valve 20cm at least.
3. the device that is used to prepare colloidal crystal simple layer film according to claim 1; It is characterized in that; Said growth tube also comprise do not dissolve each other with said colloid suspension liquid and than the big liquid of said colloid suspension liquid density, be said colloid suspension liquid, lower floor layered structure in order in growth tube, to form the upper strata for this liquid.
4. the device that is used to prepare colloidal crystal simple layer film according to claim 3 is characterized in that, also comprises fluid Supplying apparatus, and it is connected with lower floor's liquid in the said growth tube, is used to provide the liquid of this lower floor.
5. the device that is used to prepare colloidal crystal simple layer film according to claim 1 is characterized in that, also comprises the characteristic infrared lamp that is arranged on said colloid suspension liquid top.
6. method that adopts the said device of one of claim 1 to 5 to prepare colloidal crystal simple layer film may further comprise the steps:
1) temperature of the said thermostat of setting;
2) add the colloid suspension liquid in said growth tube, and make the liquid level of said colloid suspension liquid be higher than said first valve 10cm at least;
3) fixing said substrate is opened said first valve, so that the height drop-out value of said colloid suspension liquid accounts for the liquid level of former colloid suspension liquid and the ratio of the difference of altitude between first valve is at most 1/10 in said growth tube;
4) treat that growth finishes, and closes first valve.
7. the method that is used to prepare colloidal crystal simple layer film according to claim 6 is characterized in that, said step 2) in the liquid level of said colloid suspension liquid be higher than said first valve 20cm at least.
8. the method that is used to prepare colloidal crystal simple layer film according to claim 6 is characterized in that, said step 2) also comprise: add do not dissolve each other with said colloid suspension liquid and than in big liquid to the said growth tube of said colloid suspension liquid density.
9. the method that is used to prepare colloidal crystal simple layer film according to claim 6 is characterized in that, said step 3) also comprises: the opening characteristics infrared light.
10. method that adopts the said device of one of claim 1 to 5 to prepare the colloidal crystal multilayer film may further comprise the steps:
1) temperature of the said thermostat of setting;
2) add the colloid suspension liquid in said growth tube, and make the liquid level of said colloid suspension liquid be higher than said first valve 10cm at least; Add do not dissolve each other with said colloid suspension liquid and than in big liquid to the said growth tube of said colloid suspension liquid density;
3) fixing said substrate is opened said first valve, so that the height drop-out value of said colloid suspension liquid accounts for the liquid level of former colloid suspension liquid and the ratio of the difference of altitude between first valve is at most 1/10 in said growth tube;
4) treat that growth finishes, and closes first valve;
5) add and saidly not dissolve each other with the colloid suspension liquid, and than in big liquid to the said growth tube of colloid suspension liquid density, so that the liquid level of colloid suspension liquid is raised to the height when not opening said first valve, repeating step 1 then) to step 3).
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| CN103623748A (en) * | 2013-12-20 | 2014-03-12 | 复旦大学 | Colloid sphere vertical self assembly method based on piezoelectric ceramic vibrational excitation |
| CN103952768A (en) * | 2014-05-09 | 2014-07-30 | 中国科学院宁波材料技术与工程研究所 | Monocrystal silicon inverted pyramid array structure suede, and preparation method and application thereof |
Citations (2)
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| CN1470319A (en) * | 2003-06-25 | 2004-01-28 | �Ϻ���ͨ��ѧ | Capillary attration colloidal microball self-organization and two-dimensional, three-dimensional colloidal crystal preparing method |
| CN1936074A (en) * | 2005-09-21 | 2007-03-28 | 中国科学院物理研究所 | Method and apparatus for growing three-dimensional photon crystal film by pressure-reducing self-assembling |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1470319A (en) * | 2003-06-25 | 2004-01-28 | �Ϻ���ͨ��ѧ | Capillary attration colloidal microball self-organization and two-dimensional, three-dimensional colloidal crystal preparing method |
| CN1936074A (en) * | 2005-09-21 | 2007-03-28 | 中国科学院物理研究所 | Method and apparatus for growing three-dimensional photon crystal film by pressure-reducing self-assembling |
Non-Patent Citations (3)
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| Antony S.Dimitrov et al..Continuous Convective Assembling of Fine Particles into Two-Dimensional Arrays on Solid Surfaces.《Langmuir》.1996,第12卷(第5期),1303-1311. * |
| Zhongyu Zheng et al..Pressure controlled self-assembly of high quality three-dimensional colloidal photonic crystals.《Applied Physics Letters》.2007,第90卷051910-1到051910-3. * |
| Zuocheng Zhou et al..Flow Controlled Vertical Deposition Method for the Fabrication of Photonic crystals.《Langmuir》.2003,第20卷(第4期),1524-1526. * |
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