CN104528629A - Janus microsphere array of excellent uniformity and preparation method thereof - Google Patents
Janus microsphere array of excellent uniformity and preparation method thereof Download PDFInfo
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- CN104528629A CN104528629A CN201410789253.1A CN201410789253A CN104528629A CN 104528629 A CN104528629 A CN 104528629A CN 201410789253 A CN201410789253 A CN 201410789253A CN 104528629 A CN104528629 A CN 104528629A
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Abstract
The invention discloses a Janus microsphere array of the excellent uniformity. Each whole Janus microsphere is in a disc shape. The upper surface of each Janus microsphere is provided with a regular strip pattern. A preparation method comprises the steps that self-assembly single-layer colloidal particle crystals and physical hot stamping are combined, PSt-MCC of 36.74 micrometers is prepared through the dripping coating method to be used as a stamping substrate, and the mechanical stretching method is utilized for preparing a PDMS wrinkle template which is used as seal. Microspheres are heated at 100 DEG C for 15 min, then the microspheres are covered with the wrinkle template and a certain load, and heating at temperature larger than PStTg is kept for a period of time; the template is removed after cooling, and the Janus microsphere array with the regular strip patterns on the upper surfaces are obtained. Janus microspheres of different deformation degrees are obtained through controlling annealing temperature and the load. By means of the simple operating way, patterns are built on the surfaces of PSt microspheres, meanwhile, the Janus microsphere array with the excellent uniformity are prepared, and the defects that the preparation process is complex, the uniformity is poor and the shape is not easy to control when most synthesis methods are used for preparing Janus microspheres are avoided.
Description
Technical field
The present invention relates to the micro-structural process technology of polymer microballoon, be specifically related to a kind of process utilizing PDMS wrinkle template to impress polystyrene microsphere.
Background technology
Compared with spherical symmetric particle, anisotropic particles declines due to its symmetry, imparts distinct physics or chemical property to single particle.As Janus (anisotropy) particle of a large class in anisotropic particles, have structural form and/or different two demifacets of chemical composition, have potential application prospect in various fields such as emulsion-stabilizing, mass transfer, biological medicine, optics, electronics.Mostly also there is the deficiency that repeatability controllability that is poor, shape is low, preparation process is loaded down with trivial details and yield poorly in existing Janus microballoon synthetic method.Particularly need to be studied further in preparation shape and uniform monodisperse polymer micro-sphere.And utilization carries out later stage modification to prepare " from top to bottom " formula strategy of Janus particle to existing symmetrical particle, because the features such as it is applied widely, gained particle homogeneity is good are more and more subject to the attention of academia.
Summary of the invention
For above-mentioned prior art, the invention provides one " from bottom to top " formula self-assembled monolayer colloidal crystals and " from top to bottom " formula physical thermal impression combines, the Janus microballoon of preparation homogeneity excellence and the method for array thereof.The present invention selects 36.74 μm of polystyrene microsphere individual layer colloidal crystals to be substrate, with the PDMS wrinkle of the standby periodic sinusoidal shape candy strip of mechanical stretching legal system for impression block, utilize simple physical thermal to impress and achieve the olive shape Janus microballoon of drum surface with regular streaks pattern and the preparation of array thereof.And accomplished, by changing moulding process parameter, to realize the regulation and control to Janus microballoon pattern.This process avoids the use of expensive instrument and the operating procedure of very complicated.
In order to solve the problems of the technologies described above, the Janus micro-sphere array of a kind of homogeneity excellence that the present invention proposes, the entirety of each Janus microballoon in this Janus micro-sphere array is patty, and the upper surface of described Janus microballoon is with regular streaks pattern.
The preparation method of the Janus micro-sphere array of a kind of homogeneity excellence that the present invention proposes, impresses self-assembled monolayer colloidal crystals with physical thermal and combines, and comprise the following steps:
Step one, utilize drop-coating to prepare polystyrene microsphere individual layer colloidal crystals that particle diameter is 36.74 μm, this polystyrene microsphere individual layer colloidal crystals is as imprinting substrates;
Step 2, utilize the standby dimethyl silicone polymer wrinkle template with bar shaped wrinkle of mechanical stretching legal system, this dimethyl silicone polymer wrinkle template is as seal;
Step 3, imprinting substrates obtained for step one is preheated 15min at 100 DEG C, the seal that then capping step two is obtained on this imprinting substrates, additional 10-40g load, heats 1h in annealing temperature under higher than polystyrene glass transition temperature; Cool to room temperature with the furnace, take off seal and unload, obtain the Janus micro-sphere array of homogeneity excellence.
Further, in described step one, get with liquid-transfering gun the 36.74 μm of polystyrene microsphere aqueous solution 15 μ l that volume fraction is 1%, drip on clean cover glass, naturally dry under room temperature environment, the polystyrene microsphere individual layer colloidal crystals obtained is imprinting substrates.
The particular content of step 2 comprises:
First, by polydimethylsiloxane prepolymer body and crosslinking agent in mass ratio for after 10:1 mixing, pour in culture dish, fully stir with glass bar and form uniform prepolymer;
Above-mentioned prepolymer after degassed 0.5-1.5 hour, is heated 3-6h and is cured in the multiplex vavuum pump of circulating water type at 60-80 DEG C; Obtain polydimethylsiloxaneelastomer elastomer;
Above-mentioned polydimethylsiloxaneelastomer elastomer is cut into the rectangle of 6cm × 2cm, oxygen plasma treatment 30min is used under the state of prestretched 10%, retraction speed in processing procedure is 0.1-0.5mm/min, obtains the dimethyl silicone polymer wrinkle template with bar shaped wrinkle after retraction.
In described step 3, annealing temperature is 110 DEG C or 120 DEG C.
In preparation method of the present invention, regulated and controled the deformation extent of microballoon by applied load and annealing temperature process parameter.
Compared with prior art, the invention has the beneficial effects as follows:
Method of the present invention has fast, simply, and reproducible feature.One-step method can prepare the Janus micro-sphere array of homogeneity excellence.Avoid the shortcoming that the repeatability that existing Janus microballoon synthetic method exists mostly is poor, particle homogeneity is poor, controllability that is shape is low, preparation process is loaded down with trivial details and yield poorly.
Accompanying drawing explanation
Fig. 1 is the optical microscope picture of the PDMS wrinkle pattern that the standby PDMS wrinkle template of the embodiment of the present invention 1 mechanical stretching legal system obtains;
Fig. 2 is the optical microscope picture that the embodiment of the present invention 1 obtains the olive shape Janus micro-sphere array of the olive shape Janus micro-sphere array prepared when imprint parameters is 110 DEG C of-1h-10g;
Fig. 3 is the optical microscope picture that the embodiment of the present invention 2 obtains the olive shape Janus micro-sphere array of the olive shape Janus micro-sphere array prepared when imprint parameters is 120 DEG C of-1h-10g;
Fig. 4 is the optical microscope picture that the embodiment of the present invention 3 obtains the olive shape Janus micro-sphere array of the olive shape Janus micro-sphere array prepared when imprint parameters is 120 DEG C of-1h-40g.
Detailed description of the invention
Below in conjunction with specific embodiment, the inventive method is described further.Thering is provided embodiment to be convenience in order to understand, is never restriction the present invention.
Embodiment 1: the Janus micro-sphere array of preparation homogeneity excellence, comprises the following steps:
Step one, utilize drop-coating to prepare polystyrene microsphere individual layer colloidal crystals that particle diameter is 36.74 μm, this polystyrene microsphere individual layer colloidal crystals is as imprinting substrates; Particular content is: get with liquid-transfering gun the 36.74 μm of PSt microballoon aqueous solution 15 μ l that volume fraction is 1%, drips on clean cover glass, naturally dries and obtain PSt-MCC imprinting substrates under room temperature environment.
Step 2, utilize the standby dimethyl silicone polymer wrinkle template with bar shaped wrinkle of mechanical stretching legal system, this dimethyl silicone polymer wrinkle template is as seal; Particular content is: first, by dimethyl silicone polymer (PDMS) performed polymer and crosslinking agent
184 (purchased from American Dow Corning Corporations) for after 10:1 mixing, pour in culture dish in mass ratio, fully stir form uniform prepolymer with glass bar; Then, above-mentioned prepolymer after degassed 1 hour, is heated 4h and is cured in the multiplex vavuum pump of circulating water type at 70 DEG C; Obtain PDMS elastomer; Finally, above-mentioned PDMS elastomeric shear is become the rectangle of 6cm × 2cm, oxygen plasma treatment 30min is used under the state of prestretched 10%, retraction speed in processing procedure is 0.1mm/min, obtain the PDMS wrinkle template with bar shaped wrinkle after retraction, the PDMS wrinkle pattern of this wrinkle template as shown in Figure 1.
Step 3, imprinting substrates obtained for step one is preheated 15min at 100 DEG C, the PDMS wrinkle template with bar shaped wrinkle that then capping step two is obtained on this imprinting substrates, additional 10g load, keep annealing temperature to be 110 DEG C of heating 1h in an oven; Cool to room temperature with the furnace take off PDMS wrinkle template and unload, obtain the Janus micro-sphere array of homogeneity excellence.
By optical microphotograph Microscopic observation, the entirety of each Janus microballoon in this Janus micro-sphere array is that (namely the reduction of vertical direction (highly) size occurs when being subject to External Force Acting vertically downward protocorm shape microballoon patty, lateral dimension increases, and microballoon upper and lower surface is plane), the upper surface of described Janus microballoon is with regular streaks pattern.The present embodiment 1 gained Janus micro-sphere array is as shown in the light microscopic figure of Fig. 2.
Embodiment 2: the Janus micro-sphere array of preparation homogeneity excellence, its step is substantially the same manner as Example 1, is differently only that the annealing temperature in wherein step 3 is 120 DEG C.The patty Janus micro-sphere array obtained is as shown in the light microscopic figure of Fig. 3.
Embodiment 3: the Janus micro-sphere array of preparation homogeneity excellence, its step is substantially the same manner as Example 1, is differently only that the loading load in wherein step 3 is 40g, and annealing temperature is 120 DEG C.The patty Janus micro-sphere array obtained is as shown in the light microscopic figure of Fig. 4.
To sum up, the inventive method mainly utilizes PDMS wrinkle template to carry out physical thermal impression to PSt-MCC microsphere substrate, prepares the olive shape Janus micro-sphere array of homogeneity excellence.By imprint parameters such as regulation and control annealing temperature, applied load etc., the Janus microballoon that deformation extent in Janus micro-sphere array is controlled can be obtained.When before inventive process avoids, most of synthetic method prepares Janus microballoon, homogeneity is poor, preparation process is complicated, the uppity shortcoming of pattern.
Although invention has been described for composition graphs above; but the present invention is not limited to above-mentioned specific embodiments; above-mentioned detailed description of the invention is only schematic; instead of it is restrictive; those of ordinary skill in the art is under enlightenment of the present invention; when not departing from present inventive concept, can also make a lot of distortion, these all belong within protection of the present invention.
Claims (5)
1. a Janus micro-sphere array for homogeneity excellence, is characterized in that, the entirety of each Janus microballoon in Janus micro-sphere array is patty, and the upper surface of described Janus microballoon is with regular streaks pattern.
2. the preparation method of the Janus micro-sphere array of homogeneity excellence according to claim 1, is characterized in that, impressed by self-assembled monolayer colloidal crystals and combine, and comprise the following steps with physical thermal:
Step one, utilize drop-coating to prepare polystyrene microsphere individual layer colloidal crystals that particle diameter is 36.74 μm, this polystyrene microsphere individual layer colloidal crystals is as imprinting substrates;
Step 2, utilize the standby dimethyl silicone polymer wrinkle template with bar shaped wrinkle of mechanical stretching legal system, this dimethyl silicone polymer wrinkle template is as seal;
Step 3, imprinting substrates obtained for step one is preheated 15min at 100 DEG C, the seal that then capping step two is obtained on this imprinting substrates, additional 10-40g load, heats 1h in annealing temperature under higher than polystyrene glass transition temperature; Cool to room temperature with the furnace, take off seal and unload, obtain the Janus micro-sphere array of homogeneity excellence.
3. the preparation method of the Janus micro-sphere array of homogeneity excellence according to claim 2, it is characterized in that, in described step one, the 36.74 μm of polystyrene microsphere aqueous solution 15 μ l that volume fraction is 1% are got with liquid-transfering gun, drip on clean cover glass, naturally dry under room temperature environment, the polystyrene microsphere individual layer colloidal crystals obtained is imprinting substrates.
4. the preparation method of the Janus micro-sphere array of homogeneity excellence according to claim 2, it is characterized in that, described step 2 comprises:
First, by polydimethylsiloxane prepolymer body and crosslinking agent in mass ratio for after 10:1 mixing, pour in culture dish, fully stir with glass bar and form uniform prepolymer;
Above-mentioned prepolymer after degassed 0.5-1.5 hour, is heated 3-6h and is cured in the multiplex vavuum pump of circulating water type at 60-80 DEG C; Obtain polydimethylsiloxaneelastomer elastomer;
Above-mentioned polydimethylsiloxaneelastomer elastomer is cut into the rectangle of 6cm × 2cm, oxygen plasma treatment 30min is used under the state of prestretched 10%, retraction speed in processing procedure is 0.1-0.5mm/min, obtains the dimethyl silicone polymer wrinkle template with bar shaped wrinkle after retraction.
5. the preparation method of the Janus micro-sphere array of homogeneity excellence according to claim 2, it is characterized in that, in described step 3, annealing temperature is 110 DEG C or 120 DEG C.
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Cited By (1)
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CN106188582A (en) * | 2016-08-12 | 2016-12-07 | 四川大学 | Surface has the preparation method of the polydimethylsiloxane microsphere of pleated structure |
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CN104034658A (en) * | 2013-03-05 | 2014-09-10 | 精工爱普生株式会社 | Analysis device, analysis method, optical element, method of designing optical element, and electronic apparatus |
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CN1132570A (en) * | 1993-09-30 | 1996-10-02 | 美国3M公司 | Patterned array of uniform metal microbeads |
US20030168639A1 (en) * | 2001-12-29 | 2003-09-11 | Cheon Jin Woo | Metallic nanoparticle cluster ink and method for forming metal pattern using the same |
US20090109569A1 (en) * | 2007-10-31 | 2009-04-30 | Hitachi Global Storage Technologies Netherlands B.V. | Apparatus, system, and method for guided growth of patterned media using monodisperse nanospheres |
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CN106188582A (en) * | 2016-08-12 | 2016-12-07 | 四川大学 | Surface has the preparation method of the polydimethylsiloxane microsphere of pleated structure |
CN106188582B (en) * | 2016-08-12 | 2018-07-10 | 四川大学 | Surface has the preparation method of the dimethyl silicone polymer microballoon of pleated structure |
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