CN111571880A - PDMS film substrate, film and preparation method thereof - Google Patents

PDMS film substrate, film and preparation method thereof Download PDF

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Publication number
CN111571880A
CN111571880A CN202010305251.6A CN202010305251A CN111571880A CN 111571880 A CN111571880 A CN 111571880A CN 202010305251 A CN202010305251 A CN 202010305251A CN 111571880 A CN111571880 A CN 111571880A
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China
Prior art keywords
pdms
pdms film
film
substrate
colloid
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CN202010305251.6A
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Chinese (zh)
Inventor
吴天昊
徐弘毅
谢辰同
臧振宇
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Beijing Institute of Electronic System Engineering
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Beijing Institute of Electronic System Engineering
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Priority to CN202010305251.6A priority Critical patent/CN111571880A/en
Publication of CN111571880A publication Critical patent/CN111571880A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C33/00Moulds or cores; Details thereof or accessories therefor
    • B29C33/38Moulds or cores; Details thereof or accessories therefor characterised by the material or the manufacturing process
    • B29C33/3842Manufacturing moulds, e.g. shaping the mould surface by machining
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C41/00Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
    • B29C41/02Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of definite length, i.e. discrete articles
    • B29C41/08Coating a former, core or other substrate by spraying or fluidisation, e.g. spraying powder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C41/00Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
    • B29C41/34Component parts, details or accessories; Auxiliary operations
    • B29C41/38Moulds, cores or other substrates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29LINDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2007/00Flat articles, e.g. films or sheets

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

The invention discloses a PDMS film base, a film and a preparation method thereof, wherein the preparation method of the PDMS film base comprises the steps of cleaning the surface of a glass substrate by adopting acetone and ethanol, hydroxylating the cleaned glass substrate, and silanizing the hydroxylated glass substrate to obtain the PDMS film base.

Description

PDMS film substrate, film and preparation method thereof
Technical Field
The invention relates to the technical field of PDMS film manufacturing. And more particularly, to a PDMS film substrate, a film, and a method for preparing the same.
Background
Polydimethylsiloxane (PDMS) is a polymeric organosilicon compound, commonly referred to as silicone. The polymer material has a micro-nano scale molecular chain structure, simple and controllable synthesis reaction and excellent physicochemical properties, so that the polymer material can be widely applied to microstructures. Among many polymer materials, PDMS has many uses in the microelectronics industry as an organosilicon material, and more importantly, PDMS has a unique application prospect in micro-nano manufacturing. On a micro-nano scale, PDMS is not only used as a component and a substrate material, but also often used as an elastomer mold or a stamp for preparing a microstructure.
Chinese patent application No. 201210555203.8 proposes a method for fabricating a PDMS film integrated with microstructures, which uses a PDMS transfer molding process to copy a target microstructure from a master mold fabricated based on a micromachining process to the surface of a hot-melt or water-soluble material, thereby forming a sacrificial layer mold with meltability or solubility characteristics. Then spin-coating a thin layer of PDMS on the surface of the sacrificial layer mold. The method can prepare the PDMS film, but the PDMS has strong adhesiveness to the substrate, so the film can be damaged during stripping, and the operation is difficult to achieve.
Disclosure of Invention
The invention aims to provide a preparation method of a PDMS film substrate, which solves the problem of common stripping difficulty in the PDMS manufacturing process, so that the manufacturing method is simple and easy to implement, the success rate of the prepared PDMS film is high, and a good PDMS film with high flexibility can be obtained. The invention also aims to provide a preparation method of the PDMS flexible sensor film. It is still another object of the present invention to provide a PDMS film substrate. It is yet another object of the present invention to provide a PDMS flexible sensor film.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention discloses a method for preparing a PDMS film substrate,
cleaning the surface of the glass substrate by adopting acetone and ethanol;
carrying out hydroxylation treatment on the cleaned glass substrate;
and performing silanization treatment on the hydroxylated glass substrate to obtain the PDMS film substrate.
Preferably, the hydroxylating treatment of the cleaned glass substrate specifically includes:
sequentially putting the cleaned glass substrate into flowing sulfuric acid and hydrogen peroxide for soaking and respectively ultrasonically cleaning;
taking out the glass sheet and cleaning the glass sheet by using deionized water;
n is adopted for the glass sheet cleaned by the deionized water2And (5) drying.
Preferably, the silanization treatment of the hydroxylated glass substrate to obtain the PDMS film substrate specifically includes:
immersing the glass substrate subjected to hydroxylation treatment into a trimethylchlorosilane solution;
heating for a preset time under the condition of a preset temperature, and taking out.
The invention also discloses a PDMS film substrate which is prepared by the preparation method of the DMS flexible sensor substrate.
The invention also discloses a preparation method of the PDMS flexible sensor film, which comprises the following steps:
preparing PDMS colloid;
forming a PDMS film on the PDMS film substrate of claim 4 by spin coating;
and peeling the PDMS film from the PDMS film substrate.
Preferably, the preparing of the PDMS colloid specifically includes:
putting a main reagent and a hardening agent of the PDMS bi-component reagent into a plastic beaker according to a preset mass ratio, mixing and fully stirring until a colloid with bubbles on the surface under a preset quantity condition is formed;
fixing the colloid in a vacuum cavity, degassing until bubbles on the surface of the colloid disappear to a preset condition;
and standing the colloid until bubbles on the surface of the colloid completely disappear to obtain the PDMS colloid.
Preferably, the step of forming the PDMS film on the PDMS film substrate according to claim 4 by spin coating includes:
placing the PDMS film substrate of claim 4 on a spin coater, and fixing the PDMS film substrate by turning on a vacuum pump;
dropwise adding PDMS colloid on the PDMS film substrate, and opening a spin coating machine to carry out spin coating until PDMS on the glass substrate is uniformly spin-coated to obtain a PDMS film;
and placing the PDMS film substrate with the formed PDMS film into an oven for baking.
Preferably, the peeling the PDMS film from the PDMS film substrate specifically includes:
taking the PDMS film substrate out of the oven, and standing for a preset cooling time;
peeling off a corner of the PDMS film from one end through a peeling tool so as to peel off the PDMS film from the PDMS film substrate;
and placing the peeled PDMS film on a glass template to obtain the PDMS film used as the substrate of the flexible pressure sensor.
The invention also discloses a PDMS flexible sensor film, which is prepared by the preparation method of the PDMS flexible sensor film.
The PDMS film is difficult to peel off because the PDMS is very easy to adhere to the glass substrate. The silanization treatment is carried out on the glass substrate, so that the adhesion of the PDMS film to the glass substrate is weaker and the PDMS film is easier to peel. The damage to the PDMS film when the PDMS film is stripped from the glass substrate is avoided, and the operation difficulty of stripping the PDMS film is reduced.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 shows a flow chart of one embodiment of the method for preparing a PDMS film substrate according to the present invention;
FIG. 2 shows a flow chart of a specific embodiment S120 of the preparation method of the PDMS film substrate according to the present invention;
FIG. 3 shows a flow chart of a method for preparing a PDMS film substrate according to an embodiment of the present invention S130;
FIG. 4 is a flow chart illustrating a method for preparing a PDMS flexible sensor film according to an embodiment of the present invention;
FIG. 5 shows a flowchart of a specific embodiment S210 of the preparation method of the PDMS flexible sensor film according to the invention;
FIG. 6 shows a flowchart of a specific embodiment S220 of the preparation method of the PDMS flexible sensor film according to the invention;
FIG. 7 is a flowchart illustrating a method for preparing a PDMS flexible sensor film according to an embodiment of the present invention S230;
FIG. 8 shows a scanning electron microscope image of one embodiment of the PDMS flexible sensor film of the present invention.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below with reference to preferred embodiments and the accompanying drawings. Similar parts in the figures are denoted by the same reference numerals. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
According to an aspect of the present invention, the present embodiment discloses a method for preparing a PDMS film substrate. As shown in fig. 1, in this embodiment, the method includes:
s110: the surface of the glass substrate was cleaned with acetone and ethanol. The glass substrate surface is cleaned by adopting acetone and ethanol, wherein the acetone is used for removing organic stains on the glass substrate surface, and the ethanol is used for removing water-soluble stains on the glass substrate surface.
S120: and carrying out hydroxylation treatment on the cleaned glass substrate. Wherein, at least one of concentrated sulfuric acid, hydrogen peroxide and other reagents can be used for introducing hydroxyl groups on the surface of the glass, so that the surface of the glass after hydroxylation treatment can be easily silanized.
S130: and performing silanization treatment on the hydroxylated glass substrate to obtain the PDMS film substrate. Wherein the hydroxylated glass surface is silanized with a silanization reagent to introduce hydrophobic groups. Therefore, when the silanized glass substrate is used as a base of the PDMS film, the PDMS film is easier to be peeled off.
The PDMS film is difficult to peel off because the PDMS is very easy to adhere to the glass substrate. The silanization treatment is carried out on the glass substrate, so that the adhesion of the PDMS film to the glass substrate is weaker and the PDMS film is easier to peel. The damage to the PDMS film when the PDMS film is stripped from the glass substrate is avoided, and the operation difficulty of stripping the PDMS film is reduced.
In a preferred embodiment, as shown in fig. 2, the S120 may specifically include:
s121: and (3) sequentially putting the cleaned glass substrate into flowing sulfuric acid and hydrogen peroxide for soaking and respectively carrying out ultrasonic cleaning.
S122: the glass sheet was removed and rinsed with deionized water.
S123: n is adopted for the glass sheet cleaned by the deionized water2And (5) drying.
In one specific example, the silanization treatment of the glass substrate can be achieved by: firstly, a glass substrate is sequentially placed into concentrated sulfuric acid and hydrogen peroxide for soaking to introduce-OH, so that the hydrophilicity of the glass substrate is obviously strong, and the glass substrate is respectively cleaned by ultrasonic for 15 min-30 min. The glass substrate was then removed, rinsed once with deionized water, and the surface was air-dried using N2.
In a preferred embodiment, as shown in fig. 3, the S130 may specifically include:
s131: and immersing the glass substrate subjected to hydroxylation treatment into a trimethylchlorosilane solution.
S132: heating for a preset time under the condition of a preset temperature, and taking out.
Wherein the preset temperature is preferably any value of 60-70 ℃, and the preset time is preferably any value of 30-60 min. In a specific example, the cleaned glass substrate is immersed in a TMCS (trimethylchlorosilane) solution, heated for 30min to 60min under a water bath condition of 60 ℃ to 70 ℃ to obtain a PDMS film base from the silanized glass substrate with stronger hydrophobicity, and the silanized glass substrate is taken out for standby. It should be noted that, in other embodiments, the preset temperature and the preset time may also be other values according to actual situations, and the silylation reagent for the silylation process may also be other chemical reagents, which are not limited to the trimethylchlorosilane solution, and may achieve the corresponding effect, which is not limited by the present invention.
Based on the same principle, the embodiment also discloses a preparation method of the PDMS flexible sensor film. As shown in fig. 4, in this embodiment, the method includes:
s210: PDMS colloids were prepared.
S220: the PDMS colloid is spin-coated to form a PDMS film on the PDMS film substrate according to this embodiment.
S230: and peeling the PDMS film from the PDMS film substrate.
The glass substrate of the PDMS film prepared by the invention is silanized, so that the adhesion of the PDMS film to the glass substrate is reduced, the problem of common difficulty in stripping in the process of manufacturing the PDMS film is solved, the manufacturing method is simple and easy to implement, the success rate of the prepared PDMS film is high, and the good PDMS film with high flexibility can be obtained.
In a preferred embodiment, as shown in fig. 5, the S210 may specifically include:
s211: putting a main reagent and a hardening agent of the PDMS bi-component reagent into a plastic beaker according to a preset mass ratio, mixing and fully stirring until a colloid with bubbles on the surface under a preset quantity condition is formed.
S212: and fixing the colloid in a vacuum cavity, and degassing until bubbles on the surface of the colloid disappear to a preset condition.
S213: and standing the colloid until bubbles on the surface of the colloid completely disappear to obtain the PDMS colloid.
In one specific example, the PDMS two-component reagents (primary reagent and hardener) may be first mixed in a plastic beaker at a predetermined mass ratio and stirred well until a predetermined amount of bubbles appear on the surface of the gel. The preset number of bubbles can be determined by man-made experience or other identification modes, and a large number of bubbles generated by the colloid are determined. The preset mass ratio of the main agent to the hardening agent is preferably 10: 1. the stirring time is preferably any of 20min to 30 min.
And then fixing the PDMS colloid in a vacuum chamber, degassing until bubbles on the surface of the colloid disappear to a preset condition, preferably degassing for 20min to 30min under the air pressure of-0.5 Pa to 0Pa until the bubbles on the surface of the colloid disappear to the preset condition. The preset conditions can be determined by man-made experience and other identification modes, and the bubbles of the colloid are determined to be basically disappeared. And finally, standing the colloid until bubbles on the surface of the colloid completely disappear to obtain the PDMS colloid. Preferably, the PDMS colloid can be kept still for 5-6 h until bubbles on the surface of the colloid completely disappear.
In a preferred embodiment, as shown in fig. 6, the S220 may specifically include:
s221: the PDMS film substrate is placed on a spin coater, and a vacuum pump is turned on to fix the PDMS film substrate.
S222: and dropwise adding PDMS colloid on the PDMS film substrate, and opening a spin coating machine to carry out spin coating until the PDMS on the glass substrate is uniformly spin-coated to obtain the PDMS film.
S223: and placing the PDMS film substrate with the formed PDMS film into an oven for baking.
Spin coating is also called spin coating because the fluid used has a high viscosity and is colloidal. High speed spinning and drying in spin coating is a key step in controlling properties such as film thickness, structure, etc. As one of the preparation methods of a plurality of films, the spin-coating method has the advantages of accurate and controllable film thickness, high cost performance, energy conservation, low pollution and the like. Therefore, in a specific example, when a PDMS thin film is formed on a glass substrate by a spin coating method, the silanized glass substrate may be placed on a spin coater and fixed by turning on a vacuum pump, thereby preventing the glass substrate from flying out during spin coating. The spin coater rotation speed is preferably set to any value of 400rpm to 500 rpm. And then dropwise adding a proper amount of PDMS colloidal solution on the glass substrate, opening a spin coater for spin coating until PDMS on the glass substrate is uniformly spin-coated to obtain a PDMS film, and obtaining the flat PDMS film. Among them, the preferable spin coating time is any value of 1 to 2 min. And finally, placing the glass substrate into an oven for baking, wherein in order to obtain a good PDMS film, the baking temperature of the oven can be set to be any value between 60 ℃ and 70 ℃, and the baking time of the oven can be set to be any value between 30min and 40 min.
In a preferred embodiment, as shown in fig. 7, the S230 may specifically include:
s231: and taking the PDMS film substrate out of the oven, and standing for a preset cooling time.
S232: peeling the PDMS film from one end of the PDMS film by a peeling tool to peel the PDMS film from the PDMS film substrate.
S233: and placing the peeled PDMS film on a glass template to obtain the PDMS film used as the substrate of the flexible pressure sensor.
In one embodiment, the PDMS film substrate is removed from the oven and allowed to stand for a predetermined cooling time, preferably 10min, until the surface of the PDMS film is hard and the temperature drops. Then, the PDMS film was peeled off from one end of the glass template with tweezers, and then the PDMS film was gradually peeled off from the glass template. During this process, the PDMS was noted to be self-adhering and the film was damaged by the tweezers. Finally, the peeled PDMS film is placed on a new glass template, so that the PDMS film which can be used as the substrate of the flexible pressure sensor is obtained, and the Scanning Electron Microscope (SEM) image and the size of the PDMS film are shown in FIG. 8. In other embodiments, the PDMS film may be peeled off in other manners, which is not limited in the present invention.
It should be noted that the parameter values in the embodiment are only preferred values, and are not necessary for the implementation of the present invention, and other technical solutions and parameter value selections based on the same inventive concept should also be within the protection scope of the present invention.
Because the principle of solving the problems by the method is similar to that of the method, the implementation of the method can be referred to the implementation of the method, and details are not repeated herein.
Based on the same principle, the embodiment also discloses a PDMS film substrate. The PDMS film substrate is prepared by the preparation method of the DMS flexible sensor substrate described in this embodiment.
Since the principle of the PDMS film substrate to solve the problems is similar to the above method, the implementation of the PDMS film substrate can be referred to the implementation of the method, and is not described herein again.
Based on the same principle, the embodiment also discloses a PDMS flexible sensor film. The PDMS flexible sensor film is prepared by the method for preparing the PDMS flexible sensor film described in this embodiment.
Because the principle of the PDMS flexible sensor film for solving the problems is similar to the method described above, the implementation of the PDMS flexible sensor film can be referred to the implementation of the method, and is not described herein again.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, for the system embodiment, since it is substantially similar to the method embodiment, the description is simple, and for the relevant points, reference may be made to the partial description of the method embodiment.
The above description is only an example of the present application and is not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.

Claims (9)

1. A preparation method of PDMS film substrate is characterized in that,
cleaning the surface of the glass substrate by adopting acetone and ethanol;
carrying out hydroxylation treatment on the cleaned glass substrate;
and performing silanization treatment on the hydroxylated glass substrate to obtain the PDMS film substrate.
2. The method for preparing a PDMS film base according to claim 1, wherein the hydroxylating the cleaned glass substrate specifically comprises:
sequentially putting the cleaned glass substrate into flowing sulfuric acid and hydrogen peroxide for soaking and respectively ultrasonically cleaning;
taking out the glass sheet and cleaning the glass sheet by using deionized water;
for separationThe glass sheet after being washed by the seed water adopts N2And (5) drying.
3. The method for preparing a PDMS film base according to claim 1, wherein the silanization of the hydroxylated glass substrate to obtain the PDMS film base specifically comprises:
immersing the glass substrate subjected to hydroxylation treatment into a trimethylchlorosilane solution;
heating for a preset time under the condition of a preset temperature, and taking out.
4. A PDMS film substrate prepared by the method of preparing a DMS flexible sensor substrate according to any one of claims 1 to 3.
5. A preparation method of a PDMS flexible sensor film is characterized by comprising the following steps:
preparing PDMS colloid;
forming a PDMS film on the PDMS film substrate of claim 4 by spin coating;
and peeling the PDMS film from the PDMS film substrate.
6. The method for preparing a PDMS flexible sensor film according to claim 5, wherein the preparing of the PDMS colloid specifically comprises:
putting a main reagent and a hardening agent of the PDMS bi-component reagent into a plastic beaker according to a preset mass ratio, mixing and fully stirring until a colloid with bubbles on the surface under a preset quantity condition is formed;
fixing the colloid in a vacuum cavity, degassing until bubbles on the surface of the colloid disappear to a preset condition;
and standing the colloid until bubbles on the surface of the colloid completely disappear to obtain the PDMS colloid.
7. The method for preparing a PDMS flexible sensor film according to claim 5, wherein the forming the PDMS film on the PDMS film substrate according to claim 4 by spin coating of the PDMS colloid specifically comprises:
placing the PDMS film substrate of claim 4 on a spin coater, and fixing the PDMS film substrate by turning on a vacuum pump;
dropwise adding PDMS colloid on the PDMS film substrate, and opening a spin coating machine to carry out spin coating until PDMS on the glass substrate is uniformly spin-coated to obtain a PDMS film;
and placing the PDMS film substrate with the formed PDMS film into an oven for baking.
8. The method for preparing a PDMS flexible sensor film according to claim 7, wherein the peeling the PDMS film from the PDMS film substrate specifically comprises:
taking the PDMS film substrate out of the oven, and standing for a preset cooling time;
peeling off a corner of the PDMS film from one end through a peeling tool so as to peel off the PDMS film from the PDMS film substrate;
and placing the peeled PDMS film on a glass template to obtain the PDMS film used as the substrate of the flexible pressure sensor.
9. A PDMS flexible sensor film, prepared by the method of any one of claims 5 to 8.
CN202010305251.6A 2020-04-17 2020-04-17 PDMS film substrate, film and preparation method thereof Pending CN111571880A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103280527A (en) * 2013-06-04 2013-09-04 东北师范大学 Preparation method for electrode embedded into plane
CN107644806A (en) * 2017-08-30 2018-01-30 中山大学 The graphical preparation method of the orderly self assembly of metal oxide and metal-oxide film
CN110364283A (en) * 2019-04-10 2019-10-22 中国科学院深圳先进技术研究院 A kind of flexible conductive film and preparation method thereof based on silver powder and PDMS

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103280527A (en) * 2013-06-04 2013-09-04 东北师范大学 Preparation method for electrode embedded into plane
CN107644806A (en) * 2017-08-30 2018-01-30 中山大学 The graphical preparation method of the orderly self assembly of metal oxide and metal-oxide film
CN110364283A (en) * 2019-04-10 2019-10-22 中国科学院深圳先进技术研究院 A kind of flexible conductive film and preparation method thereof based on silver powder and PDMS

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Application publication date: 20200825