CN104744712A - Method for quickly preparing binary colloid crystals - Google Patents
Method for quickly preparing binary colloid crystals Download PDFInfo
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- CN104744712A CN104744712A CN201410797911.1A CN201410797911A CN104744712A CN 104744712 A CN104744712 A CN 104744712A CN 201410797911 A CN201410797911 A CN 201410797911A CN 104744712 A CN104744712 A CN 104744712A
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Abstract
The invention aims to provide a method for quickly preparing binary colloid crystals by horizontal self-assembly. The method comprises the following steps: (1) two colloid microsphere emulsions with different particle sizes are mixed ultrasonically; (2) a substrate, which is subjected to hydrophilic treatment, is horizontally placed at room temperature or in an oven, and then the mixture of the colloid microsphere emulsions is dropped onto the surface of the substrate and is spread to cover the whole surface of the substrate; (3) with volatilizing of a solvent, binary colloid crystals start growing and extend inwards along the substrate, and the binary colloid crystals are formed after the solvent volatilizes completely; and (4) reverse-phase binary colloid crystals can be obtained by filling with other materials and removing colloid microspheres.
Description
Technical field
The present invention relates to a kind of fast preparation method of binary colloidal crystal, propose a kind of colloid micro ball by two kinds of different-grain diameters and carry out the technology that Rapid self assembly prepares colloidal crystal film.
Background technology
Colloidal crystal is the crystal of two dimension or the ordered 3 D structure produced by colloid micro ball self-assembly, is widely used in the fields such as the preparation of photonic crystal, sensor, catalysis at present.The colloid micro ball that binary colloidal crystal adopts two kinds of size different carries out self-assembly and is formed.The existence of the microballoon that two kinds of particle diameters are different, is convenient to the control of colloidal crystal reflection peak position and the regulation and control to its pore structure.But due to the mutual interference of two kinds of particulates, the control overflow of its self assembling process is higher than the self-assembly of unitary colloidal crystal.
Current binary colloidal crystal self-assembly mainly adopts the method such as vertical deposition method, spin-coating method, liquid-gas interface self-assembly.Substrate generally inserts among emulsion by vertical self-assembly, and along with the volatilization of solvent, binary colloidal crystal grows on substrate, but the method generally needs ten hours or the longer time.Although spin-coating method is fast, generally, the colloidal crystal that in the colloidal crystal structure prepared by spin coating, defect obtains more than vertical self-assembly.Patent application CN101787139A proposes a kind of method preparing binary colloidal crystal in water surface self-assembly, but can only two-dimensional colloidal crystal be formed at the water surface in the method, if prepare three-dimensional colloidal crystal, need repeatedly to prepare two-dimensional colloidal crystal windrow of going forward side by side to fold, stacking process inevitably produces defect and crackle.
Summary of the invention
The object of the invention is to propose a kind of method being prepared binary colloidal crystal by horizontal self-assembly fast, can complete preparation process in 3 hours, the method includes the steps of:
(1) size two kinds of colloid micro ball emulsions are carried out ultrasonic mixing;
(2) substrate level through hydrophilic treatment is positioned in room temperature or baking oven, subsequently by colloid mixture microballoon emulsion droplets at substrate surface, and emulsion is spread out and covers whole substrate surface;
(3) along with the volatilization of solvent, binary colloidal crystal grows and extends internally along substrate from substrate edge, until form binary colloidal crystal after finish-drying;
(4) by using other materials fill and remove colloid micro ball, anti-phase binary colloidal crystal can be obtained.
In step 1, the colloid micro ball particle diameter ratio varied in size generally between 10:1-10:3, preferably between 10:1.5-10:2.2.Large microballoon is polymer microballoon in addition, preferred self-polystyrene microballoon, crosslinked polystyrene microsphere, poly (methyl methacrylate) micro-sphere, polyethyl methacrylate microballoon.The disperse phase of mixed emulsion is aqueous phase or the aqueous phase being mixed with micro-alcohols.Minimicrosphere can select polymer microballoon or inorganic microspheres.
In step 2, generally select the substrate of glass, quartz or silicon materials, and substrate is soaked in Piranha solution (98% vitriol oil and mass percentage concentration be 30% aqueous hydrogen peroxide solution be by volume 3:1 preparation mixing solutions, this solution has extremely strong oxidisability, meet organic solvent may be explosion caused, therefore use in and liquid waste disposal time answer rigorous concentration safety) in, in 90 DEG C of heat treated 30min, then use washed with de-ionized water, and dry up with nitrogen.
In step 3, substrate can be positioned in room temperature or baking oven, if be put in baking oven, temperature should control below 40 degree, to prevent solvent evaporates excessive velocities.
Accompanying drawing explanation
The digital photograph of the binary colloidal crystal that Fig. 1 obtains for embodiment 1.
The scanning electron microscope (SEM) photograph of the binary colloidal crystal film that Fig. 2 obtains for embodiment 1.
The scanning electron microscope (SEM) photograph of the binary colloidal crystal film that Fig. 3 obtains for embodiment 2.
Embodiment
The experimental technique used in the following stated embodiment if no special instructions, is ordinary method.
The raw material used in the following stated embodiment, reagent etc., if no special instructions, be and can buy from commercial channels.
The preparation of the binary colloidal crystal of embodiment 1,790nm and 150nm polystyrene colloid microballoon.
From buying two kinds of polystyrene microsphere emulsions (disperse phase is water) that particle diameter is 790nm and 150nm on the market, get two kinds of appropriate emulsions to mix, and add adjustment concentration by water, making the volume percent of 790nm microballoon in emulsion be the volume percent of 8%, 150nm microballoon is 0.14%.With ultrasonic disperse, mixed emulsion is uniformly dispersed, stand-by.
The sheet glass of 18mm × 18mm is placed in Piranha solution, and 90 DEG C of heat treated 30min, then use washed with de-ionized water, and dry up with nitrogen, and it be placed horizontally on desktop.
Get 30 μ L mixed emulsions with liquid-transfering gun, drip on the glass sheet, with liquid-transfering gun suction nozzle, emulsion is laid on whole sheet glass.As a child solvent evaporates is complete to leave standstill three, can obtain binary colloidal crystal.Its digital photograph and scanning electron microscope (SEM) photograph are shown in accompanying drawing 1 and accompanying drawing 2 respectively.
The preparation of the binary colloidal crystal of embodiment 2,1000nm and 150nm polystyrene colloid microballoon
First prepare by the method for letex polymerization the polystyrene colloid microballoon that particle diameter is 1000nm: successively 500ml deionized water and 25ml vinylbenzene are added and be equipped with in the 1L there-necked flask of mechanical stirrer and reflux condensing tube, there-necked flask is placed in the water-bath of 60 DEG C to carry out heating and lead to nitrogen and stirs, mechanical stirring speed is 300r/min, after 60 minutes, 0.13g Potassium Persulphate is added as letex polymerization initiator in there-necked flask, after reaction 25h, obtain the emulsion that particle diameter is 1000nm polystyrene colloid microballoon, the standard deviation of this polystyrene colloid microspherulite diameter is less than 3%.
From buying the polystyrene microsphere emulsion (disperse phase is water) that particle diameter is 150nm on the market, get appropriate two kinds of colloid micro ball emulsions to mix, and add adjustment concentration by water, making the volume percent of 1000nm microballoon in emulsion be the volume percent of 15%, 150nm microballoon is 0.24%.With ultrasonic disperse, mixed emulsion is uniformly dispersed, stand-by.
The silicon chip of 20mm × 20mm is placed in Piranha solution, and 90 DEG C of heat treated 30min, then use washed with de-ionized water, and dry up with nitrogen, and it be placed horizontally on desktop.
Get 40 μ L mixed emulsions with liquid-transfering gun, drip on the glass sheet, and with liquid-transfering gun suction nozzle, emulsion is laid on whole sheet glass.As a child solvent evaporates is complete to leave standstill three, can obtain binary colloidal crystal.Its scanning electron microscope (SEM) photograph is shown in accompanying drawing 3.
The preparation of the binary colloidal crystal that embodiment 3,790nm polystyrene colloid microballoon and 140nm silicon dioxide microsphere are formed.
From buying the silicon dioxide microsphere emulsion that polystyrene microsphere emulsion that particle diameter is 790nm and particle diameter are 140nm on the market, get appropriate two kinds of colloid micro ball emulsions to mix, configuration mixed emulsion, and add adjustment concentration by water, make the volume percent of polystyrene microsphere in emulsion be 6%, the volume percent of silicon dioxide microsphere is 0.09%.With ultrasonic disperse, mixed emulsion is uniformly dispersed, stand-by.
The sheet glass of 18mm × 18mm is placed in Piranha solution, and 90 DEG C of heat treated 30min, then use washed with de-ionized water, and dry up with nitrogen, and it be placed horizontally on desktop.
Get 30 μ L mixed emulsions with liquid-transfering gun, drip on the glass sheet, and with liquid-transfering gun suction nozzle, emulsion is laid on whole sheet glass.As a child solvent evaporates is complete to leave standstill three, can obtain binary colloidal crystal.
Claims (4)
1. prepare a method for binary colloidal crystal fast, the method includes the steps of:
Size two kinds of colloid micro ball emulsions are carried out ultrasonic mixing, the mixed emulsion microballoon concentration of configuration between 1-25%, preferred 2-15%;
Substrate level through hydrophilic treatment is positioned in room temperature or baking oven, subsequently by colloid mixture microballoon emulsion droplets at substrate surface, and emulsion is spread out and covers whole substrate surface;
Along with the volatilization of solvent, binary colloidal crystal grows and extends internally along substrate from substrate edge, until form binary colloidal crystal after finish-drying.
2. in claim 1, the colloid micro ball particle diameter ratio varied in size between 10:1-10:3, preferably between 10:1.5-10:2.2.
3. microballoon according to claim 1, large microballoon is polymer microballoon, preferred self-polystyrene microballoon, crosslinked polystyrene microsphere, poly (methyl methacrylate) micro-sphere, polyethyl methacrylate microballoon.The disperse phase of mixed emulsion is aqueous phase or the aqueous phase being mixed with micro-alcohols.Minimicrosphere can select polymer microballoon or inorganic microspheres.
4. the substrate hydrophilic treatment described in claim 1, selects glass, quartz or silicon chip, and is soaked in Piranha solution by substrate, makes it surface oxidation and reaches hydrophilic effect.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410797911.1A CN104744712A (en) | 2014-12-19 | 2014-12-19 | Method for quickly preparing binary colloid crystals |
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| CN201410797911.1A CN104744712A (en) | 2014-12-19 | 2014-12-19 | Method for quickly preparing binary colloid crystals |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107442045A (en) * | 2017-09-06 | 2017-12-08 | 蚌埠玻璃工业设计研究院 | A kind of method that micro-nano particle emulsion droplets add standby layer-controllable colloidal crystal |
| CN107604442A (en) * | 2017-09-06 | 2018-01-19 | 蚌埠玻璃工业设计研究院 | A kind of method that emulsion suspension prepares colloidal crystal |
| CN109504654A (en) * | 2019-01-08 | 2019-03-22 | 南京艾尔普再生医学科技有限公司 | Cardiac muscle cell's preparation method |
| CN109932760A (en) * | 2019-04-02 | 2019-06-25 | 上海第二工业大学 | A kind of preparation method of transparent colloid crystal film with photon |
| CN111593411A (en) * | 2020-05-20 | 2020-08-28 | 暨南大学 | Large-area ordered PS microsphere single-layer colloidal crystal and preparation method thereof |
| WO2020215307A1 (en) * | 2019-04-26 | 2020-10-29 | 深圳先进技术研究院 | Method for modifying surface of material, material modified thereby and use thereof, and medical product |
-
2014
- 2014-12-19 CN CN201410797911.1A patent/CN104744712A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| LIKUI WANG.ETAL: "Binary Colloidal Crystals Fabricated with a Horizontal Deposition Method", 《LANGMUIR》 * |
| QINGFENG YAN ETAL: "Inward-Growing Self-Assembly of Colloidal Crystal Films", 《LANGMUIR》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107442045A (en) * | 2017-09-06 | 2017-12-08 | 蚌埠玻璃工业设计研究院 | A kind of method that micro-nano particle emulsion droplets add standby layer-controllable colloidal crystal |
| CN107604442A (en) * | 2017-09-06 | 2018-01-19 | 蚌埠玻璃工业设计研究院 | A kind of method that emulsion suspension prepares colloidal crystal |
| CN109504654A (en) * | 2019-01-08 | 2019-03-22 | 南京艾尔普再生医学科技有限公司 | Cardiac muscle cell's preparation method |
| CN109504654B (en) * | 2019-01-08 | 2021-08-03 | 南京艾尔普再生医学科技有限公司 | Preparation method of myocardial cells |
| CN109932760A (en) * | 2019-04-02 | 2019-06-25 | 上海第二工业大学 | A kind of preparation method of transparent colloid crystal film with photon |
| CN109932760B (en) * | 2019-04-02 | 2021-05-25 | 上海第二工业大学 | Preparation method of transparent colloid photonic crystal film |
| WO2020215307A1 (en) * | 2019-04-26 | 2020-10-29 | 深圳先进技术研究院 | Method for modifying surface of material, material modified thereby and use thereof, and medical product |
| CN111593411A (en) * | 2020-05-20 | 2020-08-28 | 暨南大学 | Large-area ordered PS microsphere single-layer colloidal crystal and preparation method thereof |
| CN111593411B (en) * | 2020-05-20 | 2021-07-27 | 暨南大学 | Large-area ordered PS microsphere single-layer colloidal crystal and preparation method thereof |
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