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A kind of method that utilizes wet film coating method to prepare silk protein thin film

A technology of silk protein and regenerated silk fibroin, which is applied in the field of preparation of silk protein films, can solve the problems of large film thickness, difficulty in effective control, and unsatisfactory mechanical properties, and achieve good mechanical properties, excellent mechanical properties, and excellent self-supporting sexual effect

Active Publication Date: 2021-11-30
ZHEJIANG LAB
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The thickness of the film prepared by the casting method is large and difficult to control effectively. The film obtained by casting the silk protein aqueous solution is brittle and has unsatisfactory mechanical properties.
Moreover, neither the pouring method nor the suction filtration method is suitable for large-scale production, and these characteristics affect the application prospects of silk protein films for flexible electronics.
[0005] In addition, it should be pointed out that the current wet film coating method is only used to make wet films and does not involve the peeling of the film. Therefore, how to peel off the substrate to obtain a self-supporting silk protein film is a blank
Although the suction filtration method can prepare ultra-thin silk protein films with a thickness of less than 9 μm, the process of separating the silk protein films is complicated
If wet film coating method is used to prepare self-supporting silk protein film, due to the difference of the substrate, the wet film coating method cannot adopt the same film separation method as the suction filtration method.
In fact, not only the preparation of silk fibroin films, but also how to separate the films so that the resulting films have good self-supporting properties when preparing other types of ultra-thin films with a thickness below 9 μm has always been a technical difficulty in the field of film preparation. , currently known methods for separating other types of thin films from substrates (such as sacrificial layer assisted etching) are more complicated

Method used

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  • A kind of method that utilizes wet film coating method to prepare silk protein thin film
  • A kind of method that utilizes wet film coating method to prepare silk protein thin film
  • A kind of method that utilizes wet film coating method to prepare silk protein thin film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Prepare a lithium chloride-formic acid solution with a concentration of 0.5wt%, take 0.4g of degummed silk and dissolve it in 7.8ml of the above solution, place it in an ultrasonic cleaner for oscillation for 1 hour, and filter the solution with a PTFE filter membrane with a pore size of 0.45 μm to obtain regeneration Silk fibroin solution.

[0038] Use a clean PET substrate with a water drop angle of 79.1°, set the scraper thickness of the scraper to 0.1 μm, and apply a layer of regenerated silk fibroin wet film by scraping; place the film on a hot stage at 60°C to dry for 5 minutes; The film was soaked in water for 0.5min, and then dried on a hot table at 60°C; by mechanical peeling, the dried regenerated silk fibroin film was peeled off from the substrate to obtain a self-supporting flexible silk protein film, which was finally formed into a film The thickness is about 0.05μm and the flatness is good.

Embodiment 2

[0040]Prepare a lithium bromide-formic acid solution with a concentration of 8.7wt%, take 2.5g of degummed silk and dissolve it in 5.7ml of the above solution, place it in an ultrasonic cleaner for oscillation for 1 hour, and filter the solution with a PTFE filter membrane with a pore size of 0.45 μm to obtain regenerated silk fibroin protein solution.

[0041] Using a clean polyimide PI substrate with a water drop angle of 82°, using a four-sided preparation device with a thickness of 200 μm, scrape and coat a layer of silk protein wet film; place the film on a hot table at 60°C to dry for 10 minutes; The film was soaked in water for 20 minutes, and then dried on a hot table at 60°C; by mechanical peeling, the dried silk protein film was peeled off from the substrate to obtain a self-supporting flexible silk protein film, and the final film thickness was about 25μm and good flatness.

Embodiment 3

[0043] Calcium chloride-formic acid solution with a concentration of 4.8wt% is prepared, 1.3g of degummed silk is dissolved in 6.8ml of the above solution, placed in an ultrasonic cleaner to vibrate for 1 hour, and the solution is filtered with a PTFE filter membrane with a pore size of 0.45 μm to obtain regeneration Silk fibroin solution.

[0044] Using a clean PET substrate with a water drop angle of 85°, use a four-sided preparation device with a thickness of 100 μm to scrape and coat a silk protein wet film; place the film on a hot table at 60°C for 10 minutes; rinse the dried film in water for 5 minutes, Then dry it on a hot table at 60°C; use mechanical peeling method to peel the dried silk protein film from the substrate to obtain an ultra-thin flexible silk protein film. The final film thickness is about 9 μm and the flatness is good.

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Abstract

The invention discloses a method for preparing a silk fibroin film by using a wet film coating method, which comprises the following steps: (1) scraping and coating a regenerated silk fibroin wet film on a substrate, and drying to obtain a regenerated silk fibroin film; (2) The regenerated silk fibroin film is placed in water so that the regenerated silk fibroin film can be peeled off from the substrate after drying; (3) the regenerated silk fibroin film is dried and peeled off from the substrate. The invention realizes for the first time the preparation of a silk protein film with excellent self-supporting properties by wet film coating method, and the film has the characteristics of ultra-thin, flexible, transparent, breathable, and excellent biocompatibility, and is suitable for flexible applications such as epidermal electronics. Electronic products, biomedicine and other fields. In addition, the method of the present invention is not only suitable for industrial mass production of silk protein films, but also can be matched with existing film processing techniques such as roll-to-roll and nanoimprinting, and is easy to prepare patterned functional films.

Description

technical field [0001] The invention relates to a preparation method of a self-supporting silk protein film, which belongs to the field of polymer materials. Background technique [0002] Flexible electronics has achieved rapid development in the past decade, but most of the research results have not been transformed into products. It is an obvious fact that the development of flexible electronics in industry lags behind the prosperity of academia. The adoption of new functional materials and manufacturing technologies is a prerequisite for the realization of flexible electronics products, and the research on industrial transformation will determine the commercial success of flexible electronics technology. At present, there are many kinds of materials for flexible electronic applications. Substrate materials are the supporting components of flexible electronic devices and the basis for determining the usability, comfort and manufacturability of flexible electronic products....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J5/18C08L89/00C08K5/09C08K3/16
CPCC08J5/18C08J2389/00C08K5/09C08K3/16C08K2003/162C08L89/00C09D189/00C08J3/07C08L2203/16
Inventor 刘海涛张磊
Owner ZHEJIANG LAB
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