CN101392407B - Method for preparing cylinder hollow macroporous ordered colloidal crystal - Google Patents
Method for preparing cylinder hollow macroporous ordered colloidal crystal Download PDFInfo
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- CN101392407B CN101392407B CN200810156587XA CN200810156587A CN101392407B CN 101392407 B CN101392407 B CN 101392407B CN 200810156587X A CN200810156587X A CN 200810156587XA CN 200810156587 A CN200810156587 A CN 200810156587A CN 101392407 B CN101392407 B CN 101392407B
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Abstract
The invention discloses a preparation method of a cylindrical hollow macroporous ordered colloidal crystal, which comprises the steps as follows: a glass capillary is cleaned in an ultrasonic cleaner with hydrochloric acid, acetone and deionized water; the glass capillary after being cleaned is vertically inserted into a glass bottle holding colloidal microsphere water solution; the upper end of the glass capillary is fixed on a metal filament and placed stilly for 10 minutes to 20 minutes; the vertical movement of the metal filament is controlled by a stepping motor; an electric field is externally added in the vertical direction of the bottle and the strength of the electric field is 50 V/m to 100 V/m; the whole device is placed at a constant temperature of 40 DEG C to 80 DEG C; the colloidal crystal grows in the inner wall of the glass capillary in a self-assembly manner. The method utilizes the externally added electric field to balance weight, slow down the deposition speed of colloidal microspheres and prolong the crystallization process of the colloidal crystal and adopts a stretching method to overcome the defect that the layer quantity of the colloidal crystal is uncontrollable; the colloidal crystal prepared has photonic bandgaps, and hollow structure of the colloidal crystal is adopted as a good linear defect, thus needing no introduction of any defect to the colloidal crystal.
Description
Technical field
The present invention relates to a kind of Technology, adopt extra electric field and drawing process to combine, the orderly colloidal crystal of preparation cylinder hollow type macropore in hollow glass capillary at hollow glass capillary inwall growth colloidal crystal.
Background technology
Colloidal crystal is meant single dispersoid microballoon spontaneous formation three-dimensional order periodic structure under appropriate condition of submicron order.The self-assembly of colloid micro ball is considered near infrared, optics and effective, the most promising preparation method of short-wave band three-D photon crystal more.Colloidal photon crystal does not have complete band gap, but it not only can be used to make spectral filter and photoswitch, high-density magnetic data memory device, chemistry and biosensor, and provides desirable template for utilizing mould plate technique to prepare the orderly pore structure with complete band gap.
The preparation method of colloidal crystal comprises: natural sedimentation, physical constraints unscrambled method, vertical sedimentation, colloid epitaxial method, centrifugal settling method etc.In above-mentioned method, adopting diameter is that the following colloidal solid of 400nm prepares colloidal crystal and can prepare the good period structure basically.But, at macrobead colloid micro ball (about 700nm),, can cause the colloidal solid deposition rate to be accelerated, thereby be difficult to form colloidal crystal with good periodic structure because the gravity of colloidal solid strengthens.Moreover, introduce defective at colloidal crystal, just can better form optical device, as introduce point defect in colloidal crystal, its behavior is just as a micro-resonant cavity; Introduce a L﹠S line defect, its behavior is similar to optical waveguides; The lead-in surface defective then can obtain the ideal plane of reflection; These character all have important application.But the technology of introducing defective in colloidal crystal is also among research.The multi-photon polymerization technique that has occurred recently is combined with this technology and colloidal crystal self-assembling technique may solve at colloidal crystal and introduces difficult this problem of defective.But cost is higher.
Summary of the invention
The present invention is based on promptly that this present situation carries out, a kind of preparation method of cylindrical hollow macroporous ordered colloidal crystal is provided, purpose is to make a kind of convenience, cheapness, use value height, photon band gap is in communication band (C+L wave band), has the orderly colloidal crystal of cylinder hollow type macropore of L﹠S line defect.Can be used as novel optical waveguides carrier, control the propagation of the light wave of a fixed frequency.
The preparation method of the colloidal crystal of a kind of cylinder hollow type of the present invention, its basic ideas are: as substrate, prepare cylinder hollow type macropore orderly colloidal crystal in glass capillary inside by glass capillary.
The preparation method of a kind of cylindrical hollow macroporous ordered colloidal crystal of the present invention, its step of preparation process is as follows:
(a) with hydrochloric acid (HCl), acetone, deionized water cleans glass capillary repeatedly in ultrasonic cleaner;
(b) the configuration colloid micro ball aqueous solution.The described colloid micro ball aqueous solution, microsphere diameter are 700nm, (diameter deviation/mean diameter) * %＜0.2%, and concentration (mass percent) is 2%～8%;
(c) the vertical insertion of cleaned glass capillary filled in the vial of the colloid micro ball aqueous solution, the upper end of glass capillary is fixed on the one metal wire, leaves standstill 10～20 minutes;
(d) wire is by step motor control vertical movement up and down under, and speed is 1～30 little meter per second;
(e) vertical direction at bottle adds an electric field, and strength of electric field is 50～100 volts/meter (V/m);
(f) whole device is placed under the constant temperature, temperature is 40 ℃～80 ℃; At glass capillary inwall self-assembled growth colloidal crystal.
The preparation method of the colloidal crystal of cylinder hollow type of the present invention, before on the preparation method, having overcome in the preparation colloidal crystal microballoon deposition fast, the uncontrollable shortcoming of the number of plies:
1. use the extra electric field balancing gravity, slowed down the sedimentary speed of colloid micro ball, prolonged the crystallisation process of colloidal crystal;
2. adopt the tensile method, overcome the uncontrollable shortcoming of the number of plies of colloidal crystal, by changing rate of extension, the number of plies of colloidal crystal and the speed relation of being inversely proportional to;
The orderly colloidal crystal of symmetrical cylinder hollow type macropore of the present invention's preparation, has photon band gap, and hollowly can be used as a good L﹠S line defect, do not need expensive multi-photon polymerization technique in colloidal crystal, to introduce defective again, for laying the foundation as new photonic device and optical waveguides later.
Description of drawings
Fig. 1 is a cylindrical hollow macroporous ordered colloidal crystal preparation facilities synoptic diagram; (1: glass capillary, the 2 colloid micro ball aqueous solution, 3: vial, 4: water, 5: water bath with thermostatic control well heater, 6: battery lead plate; 7: wire, 8: stepper-motor);
Fig. 2 is the synoptic diagram of crystallisation process in the preparation process; (9: colloid micro ball, 10: colloid micro ball aqueous solution planum semilunatum, 11: colloid micro ball gravity, 12: electrical forces, 13: microballoon cohesion, 14: hydrodynamic shear);
Fig. 3 is the colloidal crystal structural representation of cylinder hollow type; (Fig. 3 a: the colloidal crystal end face of cylinder hollow type, Fig. 3 b: the colloidal crystal section of cylinder hollow type, 15 is hollow)
Fig. 4 is the transmitted light spectrogram of symmetrical cylindrical hollow macroporous ordered colloidal crystal.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail.
Embodiment 1, prepare the orderly colloidal crystal of symmetrical cylinder hollow type macropore with the inventive method, its step of preparation process is as follows:
A, usefulness hydrochloric acid (HCl), acetone, deionized water cleans glass capillary repeatedly in ultrasonic cleaner;
B, the configuration colloid micro ball aqueous solution.The described colloid micro ball aqueous solution, microsphere diameter are 700nm, (diameter deviation/mean diameter) * %＜0.2%, and concentration (mass percent) is 2%;
C, the vertical insertion of cleaned glass capillary filled in the vial of the colloid micro ball aqueous solution, the upper end of glass capillary is fixed on the one metal wire, leaves standstill 20 minutes;
D, described wire are by step motor control vertical movement up and down, and speed is 1 little meter per second; Thereby glass capillary is done vertical movement up and down, is called drawing process.
E, add an electric field in the vertical direction of bottle, strength of electric field is 100 volts/meter (V/m) (as shown in Figure 3);
F, the described device of C～E is placed under the constant temperature, temperature is set to any temperature value of 40 ℃～80 ℃ and all can; At glass capillary inwall self-assembled growth colloidal crystal;
A, usefulness hydrochloric acid (HCl), acetone, deionized water cleans glass capillary repeatedly in ultrasonic cleaner;
B, the configuration colloid micro ball aqueous solution.The described colloid micro ball aqueous solution, microsphere diameter are 700nm, (diameter deviation/mean diameter) * %＜0.2%, and concentration (mass percent) is 8%;
C, the vertical insertion of cleaned glass capillary filled in the vial of the colloid micro ball aqueous solution, the upper end of glass capillary is fixed on the one metal wire, leaves standstill 10 minutes;
D, described wire are by step motor control vertical movement up and down, and speed is 30 little meter per seconds; Thereby glass capillary is done vertical movement up and down, is called drawing process.
E, add an electric field in the vertical direction of bottle, strength of electric field is 50 volts/meter (V/m) (as shown in Figure 3);
F, the described device of C～E is placed under the constant temperature, temperature is set to any temperature value of 40 ℃～80 ℃ and all can; At glass capillary inwall self-assembled growth colloidal crystal;
A, usefulness hydrochloric acid (HCl), acetone, deionized water cleans glass capillary repeatedly in ultrasonic cleaner;
B, the configuration colloid micro ball aqueous solution.The described colloid micro ball aqueous solution, microsphere diameter are 700nm, (diameter deviation/mean diameter) * %＜0.2%, and concentration (mass percent) is 5%;
C, the vertical insertion of cleaned glass capillary filled in the vial of the colloid micro ball aqueous solution, the upper end of glass capillary is fixed on the one metal wire, leaves standstill 15 minutes;
D, described wire are by step motor control vertical movement up and down, and speed is 15 little meter per seconds; Thereby glass capillary is done vertical movement up and down, is called drawing process.
E, add an electric field in the vertical direction of bottle, strength of electric field is 70 volts/meter (V/m) (as shown in Figure 3);
F, the described device of C～E is placed under the constant temperature, temperature is set to any temperature value of 40 ℃～80 ℃ and all can; At glass capillary inwall self-assembled growth colloidal crystal.
Claims (1)
1. the preparation method of a cylindrical hollow macroporous ordered colloidal crystal, its step is as follows:
A, glass capillary is cleaned in ultrasonic cleaner with hydrochloric acid, acetone, deionized water;
B, the configuration colloid micro ball aqueous solution; The described colloid micro ball aqueous solution, microsphere diameter are 700nm, and microsphere diameter deviation/mean diameter * %＜0.2%, mass percent concentration are 2%～8%;
C, the vertical insertion of cleaned glass capillary filled in the vial of the colloid micro ball aqueous solution, the upper end of glass capillary is fixed on the one metal wire, leaves standstill 10～20 minutes;
D, affiliated wire are by step motor control vertical movement up and down, and speed is 1～30 little meter per second;
E, add an electric field in the vertical direction of vial, strength of electric field is 50～100 volts/meter;
F, whole device is placed under the constant temperature, temperature is 40 ℃～80 ℃; At glass capillary inwall self-assembled growth colloidal crystal.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200810156587XA CN101392407B (en) | 2008-10-07 | 2008-10-07 | Method for preparing cylinder hollow macroporous ordered colloidal crystal |
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| CN200810156587XA CN101392407B (en) | 2008-10-07 | 2008-10-07 | Method for preparing cylinder hollow macroporous ordered colloidal crystal |
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| CN101392407A CN101392407A (en) | 2009-03-25 |
| CN101392407B true CN101392407B (en) | 2011-07-20 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101788697A (en) * | 2010-02-23 | 2010-07-28 | 南京师范大学 | Cladding type colloid crystalloid micro-structured fiber and preparation method thereof |
| CN102605416B (en) * | 2012-02-17 | 2015-04-29 | 北京交通大学 | Preparation method of controllable linear defects in colloidal photonic crystals |
| CN103623748A (en) * | 2013-12-20 | 2014-03-12 | 复旦大学 | Colloid sphere vertical self assembly method based on piezoelectric ceramic vibrational excitation |
| CN108796604B (en) * | 2017-05-03 | 2019-11-12 | 中国科学院化学研究所 | A kind of colloidal photon crystal and preparation method thereof with curved-surface structure |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5098675A (en) * | 1986-12-26 | 1992-03-24 | Toshiba Ceramics Co., Ltd. | Silicon single crystal pull-up apparatus |
| CN1358882A (en) * | 2001-11-27 | 2002-07-17 | 南京大学 | Preparation for external electric field controlled colloid particle self-composing and three-D photon crystal |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5098675A (en) * | 1986-12-26 | 1992-03-24 | Toshiba Ceramics Co., Ltd. | Silicon single crystal pull-up apparatus |
| CN1358882A (en) * | 2001-11-27 | 2002-07-17 | 南京大学 | Preparation for external electric field controlled colloid particle self-composing and three-D photon crystal |
Non-Patent Citations (1)
| Title |
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| JP特开2005-279633A 2005.10.13 |
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