CN102491254A - Method for wrinkling polydimethylsiloxane (PDMS) elastomer in selective area - Google Patents
Method for wrinkling polydimethylsiloxane (PDMS) elastomer in selective area Download PDFInfo
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- CN102491254A CN102491254A CN2011104158415A CN201110415841A CN102491254A CN 102491254 A CN102491254 A CN 102491254A CN 2011104158415 A CN2011104158415 A CN 2011104158415A CN 201110415841 A CN201110415841 A CN 201110415841A CN 102491254 A CN102491254 A CN 102491254A
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Abstract
The invention discloses a technological preparation method for wrinkling a hard thin film layer on the surface of a PDMS elastomer in a selective area. The method comprises the following steps of: taking the PDMS as a film material, covering by using copper nets in different specifications and performing selective plasma exposure, so that a PDMS surface treatment layer becomes a SiOx hard layer; and forming wrinkles in the selective area under outside stimulation. The method has the characteristics of rapidness and simpleness, expensive instruments, complex process conditions and extreme experimental parameters are avoided, and the microstructure morphology on the surface of the PDMS elastomer is finely regulated and controlled.
Description
Technical field
The present invention relates to the micro-structural process technology of polymer, be specifically related to the process of a kind of dimethyl silicone polymer (PDMS) elastomer constituency creped.
Background technology
In the research field of material science in recent years, utilizing the graphic structure of polymeric material controlledly synthesis micro-nano-scale is one of them.It is polymerized through chemical reaction by a lot of monomers; Performances such as the micro/nano-scale characteristic of its strand, synthetic reaction stable and control easily, shirtsleeve operation flow process make it more and more become requisite material in the field of micro-Na manufacture; Quake has delivered one piece of review article of using in fields such as microfluidic device and minute manufacturings about soft material on " science " in 2000; Wherein polymeric material is affirmed fully, this show polymeric material in the micro-nano field extensive application prospect.At present the micro-structural process technology based on polymer can classify as two kinds of approach with processing mode: a kind of is method from top to bottom; Promptly through photoetching technique, nanometer embossing, soft printing technology, scan-probe process technology etc.; The functional product microminiaturization of on characteristic size, the mankind being created; This method all adopts the manufacturing process or the equipment of macroscopic view to prepare the microstructure with specific function, like large scale integrated circuit; Another kind is a method from bottom to top; Be meant that with atom (group), molecule (group), strand etc. be elementary cell; Mentality of designing according to people is built into the product with specific function; This method normally prepares regular micro-structural based on architectural characteristics such as physics, chemistry, such as self-assembling technique.Present development trend is that both are effectively combined, thereby obtains all regular micro-structural of both macro and micro.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art; A kind of method is provided; This method has selected for use dimethyl silicone polymer (PDMS) for substrate, finely regulating the microstructure appearance of PDMS surface of elastomer, avoided using expensive instrument, complicated process conditions.
The present invention is achieved through following technical proposals:
The preparation method of a kind of polydimethylsiloxaneelastomer elastomer surface hard thin layer constituency creped is achieved according to following step:
(1) the dimethyl silicone polymer performed polymer is pressed (10-20) with crosslinking agent: 1 mass ratio mixes, and pours in the vessel, fully stirs with glass bar
(2) in the prepolymer that mixes minute bubbles are arranged, need to outgas with vavuum pump through the circulation ability of swimming is many, the preferred time is 2 hours
(3) after the degassing is accomplished, put it into the constant temperature air dry oven, the mixture that mixes is put into 60 degree-70 degree down, solidify and got final product in 2 hours-6 hours
(4) the dimethyl silicone polymer film that is cured is cut into 1cm * 5cm, with 100 orders, six side's copper mesh, 100 orders four directions copper mesh; 300 orders, six side's copper mesh, 300 orders four directions copper mesh is placed on PDMS film surface, gives film 10%-30% extensibility with drawing stand; Under vacuum 200 millitorrs, carried out plasma treatment 20 minutes-30 minutes, after handling; Copper mesh is taken down, then the PDMS that stretches was handled under identical vacuum 10 minutes-20 minutes, after handling again; The PDMS film is released into free state, obtains the senior wrinkle pattern in constituency.
In the technical scheme of the present invention, in the said step (4), when using plasma is handled; Prepared the very thin SiOx hard layer of one deck at the dimethyl silicone polymer surface layer; This soft or hard compound system that forms under above-mentioned experiment condition, has prepared constituency wrinkle structure.
Method of the present invention has fast, easy characteristics, and have good repeatability, but large tracts of land realizes the preparation of PDMS chill markization.The fold pattern of preparation has the constituency characteristics, and size can reach micron level.
Description of drawings
Fig. 1 is the light microscope picture of the PDMS constituency wrinkle structure of the embodiment of the invention 1 preparation.
Fig. 2 is the light microscope picture of the PDMS constituency wrinkle structure of the embodiment of the invention 2 preparations.
Fig. 3 is the light microscope picture of the PDMS constituency wrinkle structure of the embodiment of the invention 3 preparations.
Fig. 4 is the light microscope picture of the PDMS constituency wrinkle structure of the embodiment of the invention 4 preparations.
The specific embodiment
Further specify technical scheme of the present invention below in conjunction with specific embodiment.Select for use the Observer.A1 fluorescence microscope of German Zeiss Co., Ltd to observe; Selecting crosslinking agent for use is the crosslinking agent
184 of Dow corning company, and the plasma power of selecting for use is middle-grade 15w.
Embodiment 1:
1. the PDMS performed polymer was mixed than 20: 1 by certain mass with crosslinking agent, pour in the vessel, fully stir with glass bar.
2. in the prepolymer that mixes minute bubbles are arranged, need to outgas with vavuum pump through the circulation ability of swimming is many.Be set at 2 hours in the degassing this experiment of time.
3. after the degassing is accomplished, put it into the constant temperature air dry oven, the mixture that mixes is solidified under 60 degree, solidified 6 hours.
4. the PDMS film that is cured is cut into 1cm * 5cm, the copper mesh of 100 order hexagonal structures and the copper mesh of 100 order tetragonals are placed on PDMS film surface, give the extensibility of film 20% with drawing stand; Under vacuum 200 millitorrs; Carry out plasma treatment 30min with KQ-300E type ultrasonic cleaner, after handling, the PDMS film is released into free state; Obtain the constituency wrinkle, its pattern is seen Fig. 1.
Embodiment 2:
1. the PDMS performed polymer was mixed than 10: 1 by certain mass with crosslinking agent, pour in the vessel, fully stir with glass bar.
2. in the prepolymer that mixes minute bubbles are arranged, need to outgas with vavuum pump through the circulation ability of swimming is many.Be set at 2 hours in the degassing this experiment of time.
3. after the degassing is accomplished, put it into the constant temperature air dry oven, the mixture that mixes is solidified under 60 degree, solidified 6 hours.
4. the PDMS film that is cured is cut into 1cm * 5cm, the copper mesh of 300 order hexagonal structures and the copper mesh of 500 order hexagonal structures are placed on PDMS film surface, give the extensibility of film 10% with drawing stand; Under vacuum 200 millitorrs; Carry out plasma treatment 15min with KQ-300E type ultrasonic cleaner, after handling, the PDMS film is released into free state; Obtain the constituency wrinkle, its pattern is seen Fig. 2.
Embodiment 3:
1. the PDMS performed polymer was mixed than 10: 1 by certain mass with crosslinking agent, pour in the vessel, fully stir with glass bar.
2. in the prepolymer that mixes minute bubbles are arranged, need to outgas with vavuum pump through the circulation ability of swimming is many.Be set at 2 hours in the degassing this experiment of time.
3. after the degassing is accomplished, put it into the constant temperature air dry oven, the mixture that mixes is solidified under 60 degree, solidified 6 hours.
4. the PDMS film that is cured is cut into 1cm * 5cm, the copper mesh in 100 orders four directions and the copper mesh in 300 orders four directions are placed on PDMS film surface, give the extensibility of film 10% with drawing stand; Under vacuum 200 millitorrs, carry out plasma 25min with KQ-300E type ultrasonic cleaner, after handling; Copper mesh is taken down, then the PDMS that stretches is handled 5min again under identical vacuum, after handling; The PDMS film is released into free state, obtains the senior wrinkle pattern in constituency, its pattern is seen Fig. 3.
Embodiment 4:
1. the PDMS performed polymer was mixed than 10: 1 by certain mass with crosslinking agent, pour in the vessel, fully stir with glass bar.
2. in the prepolymer that mixes minute bubbles are arranged, need to outgas with vavuum pump through the circulation ability of swimming is many.Be set at 2 hours in the degassing this experiment of time.
3. after the degassing is accomplished, put it into the constant temperature air dry oven, the mixture that mixes is solidified under 70 degree, solidified 2 hours.
4. the PDMS film that is cured is cut into 1cm * 5cm, 300 orders, six sides' copper mesh is placed on PDMS film surface, give the extensibility of film 30% with drawing stand; Under vacuum 200 millitorrs, carry out plasma 20min with KQ-300E type ultrasonic cleaner, after handling; Copper mesh is taken down, then the PDMS that stretches is handled 10min again under identical vacuum, after handling; The PDMS film is released into free state, obtains the senior wrinkle pattern in constituency, its pattern is seen Fig. 4.
More than the present invention has been done exemplary description; Should be noted that; Under the situation that does not break away from core of the present invention, the replacement that is equal to that any simple distortion, modification or other those skilled in the art can not spend creative work all falls into protection scope of the present invention.
Claims (2)
1. the preparation method of a polydimethylsiloxaneelastomer elastomer surface hard thin layer constituency creped is characterized in that, carries out according to following step:
(1) the dimethyl silicone polymer performed polymer is pressed (10-20) with crosslinking agent: 1 mass ratio mixes, and pours in the vessel, fully stirs with glass bar
(2) in the prepolymer that mixes minute bubbles are arranged, need to outgas with vavuum pump through the circulation ability of swimming is many, the preferred time is 2 hours
(3) after the degassing is accomplished, put it into the constant temperature air dry oven, the mixture that mixes is put into 60 degree-70 degree down, solidify and got final product in 2 hours-6 hours
(4) the dimethyl silicone polymer film that is cured is cut into 1cm * 5cm, with 100 orders, six side's copper mesh, 100 orders four directions copper mesh; 300 orders, six side's copper mesh, 300 orders four directions copper mesh is placed on PDMS film surface, gives film 10%-30% extensibility with drawing stand; Under vacuum 200 millitorrs, carried out plasma treatment 20 minutes-30 minutes, after handling; Copper mesh is taken down, then the PDMS that stretches was handled under identical vacuum 10 minutes-20 minutes, after handling again; The PDMS film is released into free state, obtains the senior wrinkle pattern in constituency.
2. the preparation method of a kind of polydimethylsiloxaneelastomer elastomer surface hard thin layer according to claim 1 constituency creped; It is characterized in that, in the said step (4), when using plasma is handled; Prepared the very thin SiOx hard layer of one deck at the dimethyl silicone polymer surface layer; This soft or hard compound system that forms under above-mentioned experiment condition, has prepared constituency wrinkle structure.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102794904A (en) * | 2012-07-13 | 2012-11-28 | 天津大学 | Preparation method and application of PDMS (polydimethylsiloxane) surface double-layer selected area wrinkle |
| CN102795592A (en) * | 2012-07-13 | 2012-11-28 | 天津大学 | Selective etching reparation method and application of PDMS (polydimethylsiloxane) elastomer surface hard film layer |
| CN102795595A (en) * | 2012-07-13 | 2012-11-28 | 天津大学 | Preparation method of wrinkles by combining selected area ultraviolet ozonization and solvent swelling and application thereof |
| CN103466540A (en) * | 2013-07-05 | 2013-12-25 | 天津大学 | Method used for preparing wrinkles of multilayer composite silver film on PDMS elastomer substrate |
| CN104445052A (en) * | 2014-12-05 | 2015-03-25 | 天津大学 | Method of etching surface topography of polydimethylsiloxane (PDMS) by oxygen plasmas |
| CN104476895A (en) * | 2014-12-05 | 2015-04-01 | 天津大学 | Method for constructing multistage ordered microstructure by combination of template imprinting and surface wrinkling |
| CN105016294A (en) * | 2015-06-04 | 2015-11-04 | 天津大学 | Method for preparing high-level micro-structured poly-dopamine film |
| CN105085908A (en) * | 2015-07-31 | 2015-11-25 | 天津大学 | Method for preparing patterned polypyrrole film based on in-situ wrinkling |
| CN105181891A (en) * | 2015-07-31 | 2015-12-23 | 天津大学 | Method for construction of polypyrrole membrane with hierarchical morphology based on in-situ wrinkling and solvent swelling |
| CN105699703A (en) * | 2016-01-26 | 2016-06-22 | 天津大学 | A method for measuring light softening of an azobenzene thin film through utilization of surface wrinkling |
| CN105731365A (en) * | 2016-02-29 | 2016-07-06 | 天津大学 | PDMS elastomer micro-nano processing method based on crosslinking control control transfer printing |
| CN105731364A (en) * | 2016-02-29 | 2016-07-06 | 天津大学 | PDMS elastomer micro-nano processing method based on surface oxidation control transfer printing |
| CN107954392A (en) * | 2017-11-28 | 2018-04-24 | 上海理工大学 | The preparation method of PDMS variable period annular micro-fold structures |
| CN108519833A (en) * | 2018-04-03 | 2018-09-11 | 京东方科技集团股份有限公司 | The forming method and touch-control display master blank of touch-control display panel |
| CN109640513A (en) * | 2019-01-22 | 2019-04-16 | 广州安费诺诚信软性电路有限公司 | A kind of own elasticity axial stretching flexible circuit board and preparation method thereof |
| CN110243506A (en) * | 2018-03-08 | 2019-09-17 | 中国科学院深圳先进技术研究院 | A kind of piezoresistive pressure sensor and preparation method thereof |
| CN111071983A (en) * | 2019-12-23 | 2020-04-28 | 大连海洋大学 | Rapid preparation method of elastomer PDMS (polydimethylsiloxane) multistage wrinkled surface |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1668448A (en) * | 2002-06-17 | 2005-09-14 | 罗狄亚化学公司 | Method of treating the surface of an article comprising silicon which is cross-linked by polyaddition |
| US20070111353A1 (en) * | 2003-12-08 | 2007-05-17 | Protolife Sr.L | Hybrid microfluidic chip and method for manufacturing same |
| CN101126900A (en) * | 2007-08-31 | 2008-02-20 | 中国科学院光电技术研究所 | Photolithography method based on metal local effect |
| CN102145875A (en) * | 2011-03-08 | 2011-08-10 | 南京大学 | Preparation method of polydimethylsiloxane micro-nanofluidic chip |
-
2011
- 2011-12-14 CN CN201110415841.5A patent/CN102491254B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1668448A (en) * | 2002-06-17 | 2005-09-14 | 罗狄亚化学公司 | Method of treating the surface of an article comprising silicon which is cross-linked by polyaddition |
| US20070111353A1 (en) * | 2003-12-08 | 2007-05-17 | Protolife Sr.L | Hybrid microfluidic chip and method for manufacturing same |
| CN101126900A (en) * | 2007-08-31 | 2008-02-20 | 中国科学院光电技术研究所 | Photolithography method based on metal local effect |
| CN102145875A (en) * | 2011-03-08 | 2011-08-10 | 南京大学 | Preparation method of polydimethylsiloxane micro-nanofluidic chip |
Non-Patent Citations (1)
| Title |
|---|
| CONGHUA LU, ET AL.: "Large-Scale Regioselective Formation of Well-Defined Stable Wrinkles of Multilayered Films via Embossing", 《CHEMISTRY OF MATERIALS》, vol. 20, no. 22, 29 October 2008 (2008-10-29), pages 7052 - 7059 * |
Cited By (21)
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|---|---|---|---|---|
| CN102795592A (en) * | 2012-07-13 | 2012-11-28 | 天津大学 | Selective etching reparation method and application of PDMS (polydimethylsiloxane) elastomer surface hard film layer |
| CN102795595A (en) * | 2012-07-13 | 2012-11-28 | 天津大学 | Preparation method of wrinkles by combining selected area ultraviolet ozonization and solvent swelling and application thereof |
| CN102794904A (en) * | 2012-07-13 | 2012-11-28 | 天津大学 | Preparation method and application of PDMS (polydimethylsiloxane) surface double-layer selected area wrinkle |
| CN103466540A (en) * | 2013-07-05 | 2013-12-25 | 天津大学 | Method used for preparing wrinkles of multilayer composite silver film on PDMS elastomer substrate |
| CN104476895B (en) * | 2014-12-05 | 2016-08-24 | 天津大学 | The method constructing multilevel ordered micro structure that template imprints and surface wrinkling combines |
| CN104445052A (en) * | 2014-12-05 | 2015-03-25 | 天津大学 | Method of etching surface topography of polydimethylsiloxane (PDMS) by oxygen plasmas |
| CN104476895A (en) * | 2014-12-05 | 2015-04-01 | 天津大学 | Method for constructing multistage ordered microstructure by combination of template imprinting and surface wrinkling |
| CN105016294A (en) * | 2015-06-04 | 2015-11-04 | 天津大学 | Method for preparing high-level micro-structured poly-dopamine film |
| CN105085908A (en) * | 2015-07-31 | 2015-11-25 | 天津大学 | Method for preparing patterned polypyrrole film based on in-situ wrinkling |
| CN105181891A (en) * | 2015-07-31 | 2015-12-23 | 天津大学 | Method for construction of polypyrrole membrane with hierarchical morphology based on in-situ wrinkling and solvent swelling |
| CN105699703A (en) * | 2016-01-26 | 2016-06-22 | 天津大学 | A method for measuring light softening of an azobenzene thin film through utilization of surface wrinkling |
| CN105731365A (en) * | 2016-02-29 | 2016-07-06 | 天津大学 | PDMS elastomer micro-nano processing method based on crosslinking control control transfer printing |
| CN105731364A (en) * | 2016-02-29 | 2016-07-06 | 天津大学 | PDMS elastomer micro-nano processing method based on surface oxidation control transfer printing |
| CN107954392A (en) * | 2017-11-28 | 2018-04-24 | 上海理工大学 | The preparation method of PDMS variable period annular micro-fold structures |
| CN110243506A (en) * | 2018-03-08 | 2019-09-17 | 中国科学院深圳先进技术研究院 | A kind of piezoresistive pressure sensor and preparation method thereof |
| CN108519833A (en) * | 2018-04-03 | 2018-09-11 | 京东方科技集团股份有限公司 | The forming method and touch-control display master blank of touch-control display panel |
| WO2019192333A1 (en) * | 2018-04-03 | 2019-10-10 | 京东方科技集团股份有限公司 | Touch panel, forming method for touch display panel and touch display motherboard |
| CN108519833B (en) * | 2018-04-03 | 2024-03-15 | 京东方科技集团股份有限公司 | Touch display panel forming method and touch display motherboard |
| CN109640513A (en) * | 2019-01-22 | 2019-04-16 | 广州安费诺诚信软性电路有限公司 | A kind of own elasticity axial stretching flexible circuit board and preparation method thereof |
| CN109640513B (en) * | 2019-01-22 | 2024-04-02 | 广州安费诺诚信软性电路有限公司 | Self-elastic axial telescopic flexible circuit board and preparation method thereof |
| CN111071983A (en) * | 2019-12-23 | 2020-04-28 | 大连海洋大学 | Rapid preparation method of elastomer PDMS (polydimethylsiloxane) multistage wrinkled surface |
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