CN102795592A - Selective etching reparation method and application of PDMS (polydimethylsiloxane) elastomer surface hard film layer - Google Patents
Selective etching reparation method and application of PDMS (polydimethylsiloxane) elastomer surface hard film layer Download PDFInfo
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Abstract
The invention discloses a selective etching preparation method and application of a PDMS (polydimethylsiloxane) elastomer surface hard film layer. The preparation method comprises the following steps: mixing a PDMS prepolymer and a crosslinking agent in a mass ratio of 10:1, and stirring for 30 to 60 minutes; degassing for 2 hours with a vacuum pump, and curing for 6 hours at 60 DEG C to obtain a PDMS film; performing selective plasma treatment for 10 minutes by using a copper wire mesh as a mask, taking off the copper wire mesh to finally form a PDMS double-layer composite film with PDMS as a bottom layer and SiOx hard layer as a surface layer; and immersing the sample in a hydrofluoric acid solution with concentration being 2-5mol/L for 5 to 40 minutes to form a selectively etched pattern with a microstructure on the surface of the PDMS double-layer composite film. According to the preparation method, accurate and controllable microstructure processing can be performed on the PDMS surface in a simple operation mode with low-price reagents, so that usage of instrument with high cost and complicated operation steps can be avoided.
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 PDMS elastomer constituency etching.
Background technology
The micro-structural of using the method for simple and fast, cheap raw material to obtain on the film surface micro/nano-scale has in recent years become one of research focus of material science and chemical field.Along with the develop rapidly of micro-processing technology and improving constantly of operating instrument precision; The micro-structural processing of carrying out on the micro/nano-scale on the thin polymer film surface has developed the processing mode that many maturations; These technology can be divided into two types: a kind of is method, i.e. methods such as photoetching technique, nanometer embossing, soft printing technology, scan-probe process technology from top to bottom; Another kind is a method from bottom to top, promptly prepares regular micro-structural based on architectural characteristics such as physics, chemistry, such as self-assembling technique.Though these methods have pluses and minuses separately aspect different, do not have new processing mode to be developed to occur making the process of carrying out carrying out on the micro/nano-scale micro-structural on the thin polymer film surface to remain a process complicacy, costliness and for a long time process consuming time suffering from.Present development trend is to seek a kind of not only simple and fast but also cheap mode is carried out the processing of the micro-structural on the micro/nano-scale of thin polymer film surface.
Dimethyl silicone polymer (PDMS) has a lot of purposes, is prone to processing, optical property is good and has unique flexible active material obtaining application widely like emerging fields such as biochip, organic electronic, micro-fluid chips as a kind of organosilicon material in microelectronic industry; And then, how carry out micro-structural processing on the micro/nano-scale and become the focus in the focus of research at PDMS system film surface.
Summary of the invention
To above-mentioned prior art; The present invention provides the preparation method of a kind of PDMS surface of elastomer ganoine thin film layer constituency etching; Select for use PDMS as substrate; Utilize the cheap reagent of shirtsleeve operation mode to realize carrying out the micro-structural processing on the micro/nano-scale on the PDMS surface, and accomplished the pattern of accurate regulation and control micro-structural, thereby avoided the use and the complex operating steps of the high instrument of cost.
In order to solve the problems of the technologies described above, the preparation method of PDMS surface of elastomer ganoine thin film layer of the present invention constituency etching may further comprise the steps:
(1) the PDMS performed polymer is mixed by 10:1 with crosslinking agent, pour in the container, at the uniform velocity stirred 0.5-1.5 hour, form prepolymer with glass bar;
(2), then many with the vavuum pump degassing 2 hours through the circulation ability of swimming if in the prepolymer that mixes minute bubbles are arranged;
(3) prepolymer after will outgasing is put into the constant temperature air dry oven, and solidifies 6 hours down at 60 degrees centigrade, promptly obtains the PDMS film;
(4) the PDMS film is cut to 1cm * 1cm sheet material; One copper mesh is placed on the surface of this PDMS film sheet, carried out plasma treatment 10 minutes, take off copper mesh with the plasma clean device; Forming PDMS thus is that substrate, SiOx hard layer are the PDMS double-layered compound film on top layer
(5) the PDMS double-layered compound film is soaked in the hydrofluoric acid solution that molar concentration is 2mol/L to 5mol/L handled 5-40 minute;
(6), and place air to dry with distilled water flushing PDMS double-layered compound film, thereby, be formed with the constituency etching pattern of micro-structural on the PDMS double-layered compound film surface.
Among the preparation method of PDMS surface of elastomer ganoine thin film layer of the present invention constituency etching, one deck copper mesh that is placed on PDMS film sheet surface can be a copper mesh, also can be by more than two and column distribution and the order number copper mesh different with shape of a mesh constitute.
The controllable size of the PDMS surface of elastomer ganoine thin film layer constituency etching pattern that the present invention obtains is built in micron or Nano grade.
The PDMS multilayer complex films that the surface that the present invention obtains has the constituency etching pattern of micro-structural has potential widely application at aspects such as elastomeric stamp, micrometastasis, cell cultivations.
Compared with prior art, the invention has the beneficial effects as follows:
As everyone knows, polymeric material makes it in microstructure, be able to extensive use with the molecular chain structure of its micro/nano-scale, synthetic reaction and remarkable these three advantages of physical and chemical performance of simple controllable.In numerous polymeric materials, dimethyl silicone polymer (PDMS) has a lot of purposes as a kind of organosilicon material in microelectronic industry, and what is more important PDMS has its unique and wide application prospect in minute manufacturing.On micro/nano-scale, PDMS prepares microstructure not only as components and parts and base material but also often be used as elastomer moulds or elastomeric stamp.
Be as substrate with the PDMS elastomer among the preparation method of constituency of the present invention etching; Covering through the different size copper mesh;, make to be become the SiOx hard layer by the place of plasma treatment to reach the selective plasma exposure on the PDMS surface, promptly obtain to constitute the soft or hard compound system by PDMS elastomer and macromolecule membrane on the PDMS surface; Then under the auxiliary etch of hydrofluoric acid; Reach the effect of constituency etching, thereby obtain surface roughness according to the difference of constituency patterning and different micro-structurals, avoided utilizing the consuming time long shortcoming of the loaded down with trivial details and self assembly of micrometastasis.
The preparation method of constituency of the present invention etching has fast, characteristic of simple, finely regulating the pattern of patterning micro-structural of PDMS surface of elastomer, avoided using expensive instrument, complicated process conditions and harsh shortcoming and defect such as experiment parameter.Adopt PDMS rough surface that the preparation method of constituency of the present invention etching makes at aspects such as elastomeric stamp, micrometastasis, cell cultivations potential widely application to be arranged as the micro-structural of patterning.
Method of the present invention has fast, easy characteristics, and have good repeatability, but large tracts of land realizes the preparation of PDMS surface micro-structure.The rough morphology of preparation has the controlled characteristics of patterning; Size can reach micron level even Nano grade, and the PDMS rough surface of method preparation of the present invention has potential widely application as the micro-structural of patterning at aspects such as elastomeric stamp, micrometastasis, cell cultivations.
Description of drawings
Fig. 1-1 is the light microscope picture of 100 order tetragonal PDMS constituency etchings for copper mesh in the embodiment of the invention 1;
Fig. 1-2 is the light microscope picture of 100 order hexagonal structure PDMS constituency etchings for copper mesh in the embodiment of the invention 1;
Fig. 2-1 is the light microscope picture of 100 order tetragonal PDMS constituency etchings for copper mesh in the embodiment of the invention 2;
Fig. 2-2 is the light microscope picture of 100 order hexagonal structure PDMS constituency etchings for copper mesh in the embodiment of the invention 2;
Fig. 3-1 is the light microscope picture of 300 order tetragonal PDMS constituency etchings for copper mesh in the embodiment of the invention 3;
Fig. 3-2 is the light microscope picture of 300 order hexagonal structure PDMS constituency etchings for copper mesh in the embodiment of the invention 3.
The specific 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) the PDMS performed polymer is mixed by 10:1 with crosslinking agent, pour in the container, at the uniform velocity stirred 40 minutes, form prepolymer with glass bar;
(2) in the prepolymer that mixes minute bubbles are arranged, many through the circulation ability of swimming with the vavuum pump degassing 2 hours;
(3) prepolymer after will outgasing is put into the constant temperature air dry oven, and solidifies 6 hours down at 60 degrees centigrade, promptly obtains the PDMS film;
(4) the PDMS film that is cured is cut to 1cm * 1cm sheet material; The copper mesh of the copper mesh of one 100 order hexagonal structures and one 100 order tetragonals is placed on side by side the surface of this PDMS film sheet; Carried out plasma treatment 10 minutes with the plasma clean device; Take off copper mesh, forming PDMS thus is that substrate, SiOx hard layer are the PDMS double-layered compound film on top layer
(5) the PDMS double-layered compound film is soaked in the hydrofluoric acid solution that molar concentration is 2.5mol/L handled 5 minutes;
(6), and place air to dry with this PDMS double-layered compound film of distilled water flushing, thereby, be formed with the constituency etching pattern of micro-structural on the PDMS double-layered compound film surface.Its pattern is seen Fig. 1-1 and Fig. 1-2, Fig. 1-the 1st wherein, and mask copper mesh specification is the pattern of the constituency etching pattern of 100 order tetragonal positions, Fig. 1-2 is that mask copper mesh specification is the pattern of the constituency etching pattern of 100 order hexagonal structure positions.
Embodiment 2:
(1) the PDMS performed polymer is mixed by 10:1 with crosslinking agent, pour in the container, at the uniform velocity stirred 1 hour, form prepolymer with glass bar;
(2) in the prepolymer that mixes minute bubbles are arranged, many through the circulation ability of swimming with the vavuum pump degassing 2 hours;
(3) prepolymer after will outgasing is put into the constant temperature air dry oven, and solidifies 6 hours down at 60 degrees centigrade, promptly obtains the PDMS film;
(4) the PDMS film that is cured is cut to 1cm * 1cm sheet material; The copper mesh of the copper mesh of one 100 order hexagonal structures and one 100 order tetragonals is placed on side by side the surface of this PDMS film sheet; Carried out plasma treatment 10 minutes with the plasma clean device; Take off copper mesh, forming PDMS thus is that substrate, SiOx hard layer are the PDMS double-layered compound film on top layer
(5) the PDMS double-layered compound film is soaked in the hydrofluoric acid solution that molar concentration is 4mol/L handled 20 minutes;
(6), and place air to dry with this PDMS double-layered compound film of distilled water flushing, thereby, be formed with the constituency etching pattern of micro-structural on the PDMS double-layered compound film surface.Its pattern is seen Fig. 2-1 and Fig. 2-2, Fig. 2-the 1st wherein, and mask copper mesh specification is the pattern of the constituency etching pattern of 100 order tetragonal positions, Fig. 2-the 2nd, mask copper mesh specification is the pattern of the constituency etching pattern of 100 order hexagonal structure positions.
Embodiment 3:
(1) the PDMS performed polymer is mixed by 10:1 with crosslinking agent, pour in the container, at the uniform velocity stirred 1.5 hours, form prepolymer with glass bar;
(2) in the prepolymer that mixes minute bubbles are arranged, many through the circulation ability of swimming with the vavuum pump degassing 2 hours;
(3) prepolymer after will outgasing is put into the constant temperature air dry oven, and solidifies 6 hours down at 60 degrees centigrade, promptly obtains the PDMS film;
(4) the PDMS film that is cured is cut to 1cm * 1cm sheet material; The copper mesh of the copper mesh of one 300 order hexagonal structures and one 300 order tetragonals is placed on side by side the surface of this PDMS film sheet; Carried out plasma treatment 10 minutes with the plasma clean device; Take off copper mesh, forming PDMS thus is that substrate, SiOx hard layer are the PDMS double-layered compound film on top layer
(5) the PDMS double-layered compound film is soaked in the hydrofluoric acid solution that molar concentration is 3mol/L handled 30 minutes;
(6), and place air to dry with this PDMS double-layered compound film of distilled water flushing, thereby, be formed with the constituency etching pattern of micro-structural on the PDMS double-layered compound film surface.Its pattern is seen Fig. 3-1 and Fig. 3-2, Fig. 3-the 1st wherein, and mask copper mesh specification is the pattern of the constituency etching pattern of 300 order tetragonal positions, Fig. 3-the 2nd, mask copper mesh specification is the pattern of the constituency etching pattern of 300 order hexagonal structure positions.
The copper mesh order number and the shape of a mesh that are adopted among the present invention have multiple choices; The order number of copper mesh can select a kind of in 50 orders, 100 orders, 300 orders and 1000 orders, the shape of copper mesh mesh can select a kind of in rectangle, square, regular hexagon and the circle.The order number of constituency etching pattern and selecting for use mask copper mesh and size are to consistent.
The PDMS double-layered compound film constituency etching structure by preparation method's acquisition of the present invention shown in Fig. 1-1, Fig. 1-2, Fig. 2-1, Fig. 2-2, Fig. 3-1 and Fig. 3-2, its size all can be controlled in micron order.
Although invention has been described for top combination figure; But the present invention is not limited to the above-mentioned specific embodiment, and the above-mentioned specific 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 (5)
1. the preparation method of a PDMS surface of elastomer ganoine thin film layer constituency etching may further comprise the steps:
(1) the PDMS performed polymer is mixed by 10:1 with crosslinking agent, pour in the container, at the uniform velocity stirred 0.5-1 hour, form prepolymer with glass bar;
(2), then many with the vavuum pump degassing 2 hours through the circulation ability of swimming if in the prepolymer that mixes minute bubbles are arranged;
(3) prepolymer after will outgasing is put into the constant temperature air dry oven, and solidifies 6 hours down at 60 degrees centigrade, promptly obtains the PDMS film;
(4) the PDMS film is cut to 1cm * 1cm sheet material; One deck copper mesh is placed on surface in this PDMS film sheet, carries out plasma treatment 10 minutes with the plasma clean device, takes off copper mesh; Forming PDMS thus is that substrate, SiOx hard layer are the PDMS double-layered compound film on top layer
(5) the PDMS double-layered compound film is soaked in the hydrofluoric acid solution that molar concentration is 2mol/L to 5mol/L handled 5-40 minute;
(6), and place air to dry with distilled water flushing PDMS double-layered compound film, thereby, be formed with the constituency etching pattern of micro-structural on the PDMS double-layered compound film surface.
2. according to the preparation method of the said PDMS surface of elastomer of claim 1 ganoine thin film layer constituency etching; It is characterized in that; The order number of copper mesh is selected a kind of in 50 orders, 100 orders, 300 orders and 1000 orders, and the shape of copper mesh mesh is selected a kind of in rectangle, square, regular hexagon and the circle.
3. according to the preparation method of the said PDMS surface of elastomer of claim 2 ganoine thin film layer constituency etching, it is characterized in that, one deck copper mesh that is placed on PDMS film sheet surface by more than two and column distribution and the order number copper mesh different with shape of a mesh constitute.
4. according to the preparation method of the said PDMS surface of elastomer of claim 1 ganoine thin film layer constituency etching, it is characterized in that etching pattern is of a size of micron or Nano grade.
5. a surface has the application of PDMS multilayer complex films aspect elastomeric stamp, micrometastasis, cell cultivation of the constituency etching pattern of micro-structural.
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CN104445052A (en) * | 2014-12-05 | 2015-03-25 | 天津大学 | Method of etching surface topography of polydimethylsiloxane (PDMS) by oxygen plasmas |
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 |
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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 |
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CN104445052A (en) * | 2014-12-05 | 2015-03-25 | 天津大学 | Method of etching surface topography of polydimethylsiloxane (PDMS) by oxygen plasmas |
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 |
CN105016294A (en) * | 2015-06-04 | 2015-11-04 | 天津大学 | Method for preparing high-level micro-structured poly-dopamine film |
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 |
CN106079845A (en) * | 2016-06-17 | 2016-11-09 | 无锡英普林纳米科技有限公司 | A kind of preparation technology of nanometer seal |
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CN106546362A (en) * | 2016-10-27 | 2017-03-29 | 中国科学院重庆绿色智能技术研究院 | A kind of capacitance pressure transducer, based on Graphene |
CN109021270A (en) * | 2017-06-11 | 2018-12-18 | 吴浪 | PDMS elastomer micro-nano processing method based on crosslinking control trans-printing |
CN108100989A (en) * | 2017-12-20 | 2018-06-01 | 武汉大学 | A kind of nick cheats array structure processing method |
CN111892303A (en) * | 2019-05-06 | 2020-11-06 | 苏州苏大维格科技集团股份有限公司 | Preparation method of micro-nano structure for glass anti-counterfeiting |
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