CN102796271A - Controllable self-assembly method for block polymer on elastic substrate - Google Patents
Controllable self-assembly method for block polymer on elastic substrate Download PDFInfo
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- CN102796271A CN102796271A CN2012102435935A CN201210243593A CN102796271A CN 102796271 A CN102796271 A CN 102796271A CN 2012102435935 A CN2012102435935 A CN 2012102435935A CN 201210243593 A CN201210243593 A CN 201210243593A CN 102796271 A CN102796271 A CN 102796271A
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Abstract
The invention provides a controllable self-assembly method for a block polymer on an elastic substrate. The method comprises the following steps of: slicing a cured polydimethylsiloxane (PDMS) elastomer, and then treating with oxygen plasma for 0.5 to 2 minutes; spinning a 0.5wt% methylbenzene/tetrahydrofuran mixed solution of polystyrene-b-polyvinyl pyrrolidone (PS-b-PVP) onto the treated PDMS to form a polymer film using the PDMS as a substrate; treating the film for 3 to 5 hours in methylbenzene/tetrahydrofuran mixed saturated steam, soaking into ethanol for 30 minutes, and performing vacuum drying; and finally forming a regular nano micro zone structure on the polymer film using the PDMS as the substrate, and thus realizing controllable self-assembly of the block polymer on the elastic substrate. The cheap and readily available PDMS is used as a substrate spinning block polymer to obtain the equivalently regular hole-like micro zone structure on the hard substrate.
Description
Technical field
The invention belongs to macromole self-assembly field, relate in particular to a kind of method that realizes the controlled self-assembly of block polymer on elastic substrates.
Background technology
In order macromolecule member material is because its characteristic dimension and constitutional features and to the response characteristic in outfield become the focus that polymer science is studied.The polymer template of patterning can be carried out further nanometer processing on the one hand, to make nano materials such as nanoelectronic, opto-electronic device; On the other hand, the polymer of patterning itself can be used as sorbent material, tissue engineering bracket of separatory membrane, high-specific surface area etc.
Utilize the microphase-separated of block polymer can construct ordered nano-structure.But block polymer substrate that film uses at present is the hard and expensive silicon base of matter.
Summary of the invention
To above-mentioned prior art, the present invention provides the method for the controlled self-assembly of a kind of block polymer on elastic substrates, be with elastomerics as substrate, utilize block polymer to construct the method for on nanoscale macromolecule membrane surface ordered micro structure.The inventive method is with the elastomerics YSR 3286 (PDMS) and polystyrene-poly vinyl pyrrolidone block polymer (PS-b-PVP) composite membrane-forming of oxygen plasma treatment; Utilize selective solvent to handle and induce the PS-b-PVP microphase-separated to form the microcell of nanoscale, thereby realized the controlled self-assembly of block polymer on elastomeric substrate.
In order to solve the problems of the technologies described above, the method for the controlled self-assembly of a kind of block polymer of the present invention on elastic substrates, step is following:
(1) solidified PDMS is cut into pieces, put into the oxygen plasma cleanser and carried out oxygen plasma treatment 0.5 ~ 2 minute;
(2) with toluene/THF mixing solutions of the PS-b-PVP of mass concentration 0.5%, be spin-coated on through on the PDMS of above-mentioned processing, formed the polymeric film as substrate with PDMS;
(3) the above-mentioned polymeric film for preparing is put into toluene/THF mixing saturation steam and handled vacuum-drying 2 hours 3 ~ 5 hours; Then, immersed in the ethanol vacuum-drying 30 minutes; Finally, forming well-regulated nano level domain structure on as the polymeric film of substrate, realized the controlled self-assembly of block polymer on elastic substrates with PDMS.
The vacuum tightness of the PDMS film being carried out oxygen plasma treatment is 300 millitorrs, and power is 9W.
The processing condition of spin coating are: temperature is 20 ℃, and humidity is 25RH%, and the spin coating rotating speed is 2000 ~ 3000rpm.
The nano level domain structure is the nano aperture structure.Domain structure characterizes: with using scanning electron microscopic observation behind AFM direct viewing film surface microstructure or the film metal spraying.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention utilizes elastomerics YSR 3286 (PDMS) cheap and easy to get as substrate spin coating block polymer; Through the parameters such as oxygen plasma treatment time, spin coating rotating speed and solvent-induced time of regulation and control PDMS, realized equal regular hole shape domain structure on block polymer and the hard substrate.
Description of drawings
Fig. 1-the 1st, the sem photograph of the hole shape domain structure that embodiment 1 obtains
Fig. 1-2 is the AFM figure of the correspondence of the hole shape domain structure that obtains of embodiment 1;
Fig. 2 is the sem photograph of the hole shape domain structure that obtains of embodiment 2;
The sem photograph of the hole shape domain structure that Fig. 3 embodiment 3 obtains;
The sem photograph of the hole shape domain structure that Fig. 4 embodiment 4 obtains.
Embodiment
Below tell about detailed process of the present invention through embodiment, it is the convenience in order to understand that embodiment is provided, never be the restriction the present invention.
Embodiment 1
(1) solidified PDMS is cut into pieces, put into the oxygen plasma cleanser and carry out oxygen plasma treatment, its vacuum tightness is 300 millitorrs, and middle-grade power is 9W, and the treatment time is 0.5 minute;
(2) with toluene/THF mixing solutions of the PS-b-PVP of mass concentration 0.5%, be 20 ℃ with temperature, humidity is 25RH%, and the spin coating rotating speed is that 2500rpm is spin-coated on PDMS through above-mentioned processing and goes up and form with the polymeric film of PDMS as substrate;
(3) the above-mentioned polymer thin film system for preparing is put into toluene/THF mixing saturation steam processing and be placed on vacuum in 3 hours dry 2 hours; Then, immersed in the ethanol vacuum-drying 30 minutes; Finally, forming well-regulated nano level domain structure on as the polymeric film of substrate, realized the controlled self-assembly of block polymer on elastic substrates with PDMS.With ESEM, atomic force microscope observation film surface microstructure, with shown in Fig. 1-2, hole shape microcell is six square gauges then to be arranged like Fig. 1-1, and pitch of holes is 26nm.
Embodiment 2
(1) solidified PDMS is cut into pieces, put into the oxygen plasma cleanser and carry out oxygen plasma treatment, its vacuum tightness is 300 millitorrs, and middle-grade power is 9W, and the treatment time is 0.5 minute;
(2) with toluene/THF mixing solutions of the PS-b-PVP of mass concentration 0.5%, be 20 ℃ with temperature, humidity is 25RH%, and the spin coating rotating speed is that 2500rpm is spin-coated on PDMS through above-mentioned processing and goes up and form with the polymeric film of PDMS as substrate;
(3) the above-mentioned polymer thin film system for preparing is put into toluene/THF mixing saturation steam processing and be placed on vacuum in 5 hours dry 2 hours; Then, immersed in the ethanol vacuum-drying 30 minutes; Finally, forming well-regulated nano level domain structure on as the polymeric film of substrate, realized the controlled self-assembly of block polymer on elastic substrates with PDMS.With scanning electron microscopic observation film surface microstructure, as shown in Figure 2, microcell is similar to and is six sides arrangement, and comparatively regular, pitch of holes is 30nm, and the hole degree of depth is compared dark slightly with embodiment 1.
Embodiment 3
(1) solidified PDMS is cut into pieces, put into the oxygen plasma cleanser and carry out oxygen plasma treatment, its vacuum tightness is 300 millitorrs, and middle-grade power is 9W, and the treatment time is 0.5 minute;
(2) with toluene/THF mixing solutions of the PS-b-PVP of mass concentration 0.5%, be 20 ℃ with temperature, humidity is 25RH%, and the spin coating rotating speed is that 2000rpm is spin-coated on PDMS through above-mentioned processing and goes up and form with the polymeric film of PDMS as substrate;
(3) the above-mentioned polymer thin film system for preparing is put into toluene/THF mixing saturation steam processing and be placed on vacuum in 3 hours dry 2 hours; Then, immersed in the ethanol vacuum-drying 30 minutes; Finally, forming well-regulated nano level domain structure on as the polymeric film of substrate, realized the controlled self-assembly of block polymer on elastic substrates with PDMS.With scanning electron microscopic observation film surface microstructure, as shown in Figure 3, microcell is similar to and is six sides arrangement, and comparatively regular, pitch of holes is 20nm.
Embodiment 4
(1) solidified PDMS is cut into pieces, put into the oxygen plasma cleanser and carry out oxygen plasma treatment, its vacuum tightness is 300 millitorrs, and middle-grade power is 9W, and the treatment time is 2 minutes;
(2) with toluene/THF mixing solutions of the PS-b-PVP of mass concentration 0.5%, be 20 ℃ with temperature, humidity is 25RH%, and the spin coating rotating speed is that 2500rpm is spin-coated on PDMS through above-mentioned processing and goes up and form with the polymeric film of PDMS as substrate;
(3) the above-mentioned polymer thin film system for preparing is put into toluene/THF mixing saturation steam processing and be placed on vacuum in 3 hours dry 2 hours; Then, immersed in the ethanol vacuum-drying 30 minutes; Finally, forming well-regulated nano level domain structure on as the polymeric film of substrate, realized the controlled self-assembly of block polymer on elastic substrates with PDMS.With scanning electron microscopic observation film surface microstructure, as shown in Figure 4, microcell is similar to and is six sides arrangement, and comparatively regular, pitch of holes is 27nm.
In a word, the present invention is through changing OP treatment time length, spin coating rotating speed, reaching the pitch of holes that the mixing steam induction time is regulated and control the micropore of self-assembly gained.
Although invention has been described for top combination figure; But the present invention is not limited to above-mentioned embodiment, and above-mentioned embodiment only is schematically, rather than restrictive; Those of ordinary skill in the art is under enlightenment of the present invention; Under the situation that does not break away from aim of the present invention, can also make a lot of distortion, these all belong within the protection of the present invention.
Claims (4)
1. the method for the controlled self-assembly of block polymer on elastic substrates, step is following:
(1) solidified elastomerics PDMS is cut into pieces, put into the oxygen plasma cleanser and carried out oxygen plasma treatment 0.5 ~ 2 minute;
(2) with toluene/THF mixing solutions of the PS-b-PVP of mass concentration 0.5%, be spin-coated on through on the PDMS of above-mentioned processing, formed the polymeric film as substrate with PDMS;
(3) the above-mentioned polymeric film for preparing is put into toluene/THF mixing saturation steam and handled vacuum-drying 2 hours 3 ~ 5 hours; Then, immersed in the ethanol vacuum-drying 30 minutes; Finally, forming well-regulated nano level domain structure on as the polymeric film of substrate, realized the controlled self-assembly of block polymer on elastic substrates with PDMS.
2. according to the method for the controlled self-assembly of the said block polymer of claim 1 on elastic substrates, it is characterized in that the vacuum tightness of PDMS being carried out oxygen plasma treatment is 300 millitorrs, power is 9W.
3. according to the method for the controlled self-assembly of the said block polymer of claim 1 on elastic substrates, it is characterized in that the processing condition of spin coating are: temperature is 20 ℃, and humidity is 25RH%, and the spin coating rotating speed is 2000 ~ 3000rpm.
4. according to the method for the controlled self-assembly of the said block polymer of claim 1 on elastic substrates, it is characterized in that the nano level domain structure is the nano aperture structure.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102831986A (en) * | 2012-09-10 | 2012-12-19 | 台州美新源环保设备科技有限公司 | Aluminum sheath crushing wire-stripping machine for aluminum sheath wire |
| CN104671198A (en) * | 2015-02-03 | 2015-06-03 | 天津大学 | Method for preparing stripe-shaped micro-nanometer wrinkle structure by using electron beam induction method |
| CN105384952A (en) * | 2015-09-15 | 2016-03-09 | 北京航空航天大学 | Method for adjusting and controlling block copolymer self-assembled orientation by using mechanical shearing force |
| CN105418960A (en) * | 2014-09-19 | 2016-03-23 | 天津工业大学 | Construction of temperature-sensitive ordered porous film |
-
2012
- 2012-07-13 CN CN2012102435935A patent/CN102796271A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| 《中国优秀硕士学位论文全文数据库工程科技I辑（月刊）B014-158》 20120315 葛文佳 "高级多孔微结构的聚合物膜的水滴模板法制备与应用研究" 第14～20页，第32～36页,第5页 1－4 , 第03期 * |
| 葛文佳: ""高级多孔微结构的聚合物膜的水滴模板法制备与应用研究"", 《中国优秀硕士学位论文全文数据库工程科技I辑（月刊）B014-158》 * |
| 陈刚等: ""通过NMP控制制备嵌段共聚物及自组装行为研究"", 《青岛大学学报（工程技术版）》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102831986A (en) * | 2012-09-10 | 2012-12-19 | 台州美新源环保设备科技有限公司 | Aluminum sheath crushing wire-stripping machine for aluminum sheath wire |
| CN105418960A (en) * | 2014-09-19 | 2016-03-23 | 天津工业大学 | Construction of temperature-sensitive ordered porous film |
| CN104671198A (en) * | 2015-02-03 | 2015-06-03 | 天津大学 | Method for preparing stripe-shaped micro-nanometer wrinkle structure by using electron beam induction method |
| CN105384952A (en) * | 2015-09-15 | 2016-03-09 | 北京航空航天大学 | Method for adjusting and controlling block copolymer self-assembled orientation by using mechanical shearing force |
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Application publication date: 20121128 |