CN113943439B - Method for preparing GO/rGO micro-wrinkle humidity-sensitive film by using biodegradable shape memory material - Google Patents
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Abstract
The invention discloses a manufacturing method of a GO/rGO micro-wrinkle humidity-sensitive film which is highly sensitive to a humidity environment, soft, wearable and biodegradable and is based on a degradable shape memory material. The method comprises the following steps: the surface of the pre-stretched shape memory polylactic acid film is treated by plasma to improve the hydrophilicity. A coating method is adopted to coat GO solution with a certain concentration on a shape memory polylactic acid film layer by layer, thermal shrinkage recovery is carried out at a certain temperature, a laser writing machine is utilized to carry out writing of interdigital electrodes on the surface of the GO film to obtain a GO/rGO micro-wrinkle film, the prepared GO/rGO micro-wrinkle film can be used for high-precision humidity detection, and the response and the sensitivity of a humidity-sensitive sensor are improved.
Description
Technical Field
The invention designs a preparation method for preparing GO/rGO micro-wrinkle humidity-sensitive film by using biodegradable shape memory material, and researches the humidity-sensitive characteristics of the GO/rGO micro-wrinkle humidity-sensitive film. Relates to the field of biodegradable shape memory film processing and humidity sensors.
Background
Humidity sensors are closely related to the fields of atmospheric monitoring, industrial production, biomedical science and the like. Graphene with high specific surface area, high light transmittance, high thermal conductivity, high electrical conductivity and high mechanical strength is one of ideal materials for manufacturing nano gas-sensitive and humidity-sensitive thin film sensors. The gas-sensitive and humidity-sensitive sensor prepared based on the graphene and the derivatives thereof has the characteristics of quick on-site response, high sensitivity, high stability, miniaturization, low energy consumption and low cost, and can realize detection at normal temperature. However, most of the traditional humidity-sensitive sensors are made of metal electrode materials, most of the graphene oxide and the derivatives thereof are only used as humidity-sensitive films for humidity detection, and few reports have been made that the sensor is prepared by using micro-folds as the humidity-sensitive films. In recent years, surface micro-corrugated materials are gradually applied to the fields of electronic sensors, electronic skins and wearable flexible electronic devices. Whether fibers or films, it is desirable to intelligently control the surface micro-wrinkle morphology. The graphene oxide is poor in film adhesion after thermal reduction and is easy to fall off from a substrate. The invention aims to improve the bonding strength of the thermal reduction graphene oxide. Grafting graphene oxide and a silane coupling agent on the surface, adding melamine to obtain surface-modified Graphene Oxide (GO), and preparing the prepared GO into a thin film material on the surface of degradable shape memory PLA with a pre-stretched shape fixed. The biodegradable shape memory film is restored to be prepared into an oriented micro-corrugated structure, the GO film is reduced by using a laser reduction technology, the GO/rGO micro-corrugated humidity-sensitive film is used for humidity detection, and finally humidity response and sensitivity are improved.
Problems to be solved by the invention
Humidity sensing is important for atmospheric detection and medical article detection. Traditional humidity sensors generally use metal electrodes for conduction, GO and GO derivatives as humidity sensitive membranes, but they are not sensitive to low humidity environments. The invention provides a method for preparing a GO/rGO micro-wrinkle humidity-sensitive film by utilizing a biodegradable shape memory material, and a sensing film highly sensitive to a humidity environment is obtained.
Disclosure of Invention
1. The preparation method of the modified graphene oxide comprises the following steps:
adding the graphene oxide aqueous solution and a silane coupling agent into a reaction kettle according to the mass ratio of 100: 0.1-5, controlling the temperature to be 40-80 ℃, and stirring for reaction for 4-10 hours to obtain the silane coupling agent grafted graphene oxide. The temperature was raised to 90 ℃ and melamine was added. The ratio of the graphene oxide aqueous solution to the melamine is 100: 1-5. And (4) carrying out ultrasonic dispersion after cooling, and taking the modified graphene oxide solution (GO) dispersed on the upper layer. The silane coupling agent comprises gamma-glycidoxypropyltrimethoxysilane KH550, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane KH560 and gamma-methacryloxypropyltrimethoxysilane KH570.
2. The preparation method of the micro-folded GO/rGO humidity-sensitive film adopts the following technical scheme:
cutting the pre-stretched 10-500% biodegradable shape memory film into certain size and plasma treating the pre-stretched surface for 1-5 min. The biodegradable shape memory film comprises: shape memory polylactic acid (SMPLA), shape Memory Polycaprolactone (SMPCL), shape memory polypropylene carbonate (SMPPC) and PLA blends with good biocompatibility. Including blends with polyethylene glycol (PLA/PEG), blends with polyacetic acid (PLA/PGA), blends with polycaprolactone (PLA/PCL), blends with polypropylene carbonate (PLA/PPC), etc. A certain concentration of modified graphene oxide solution GO with the concentration of O.1-5% is coated on the biodegradable shape memory film layer by adopting a coating method. The modified graphene oxide contains a silane coupling agent and melamine, so that the adhesion of the graphene oxide is improved through strong pi-pi action, hydrogen bond action and electrostatic attraction. The thermal contraction recovery is carried out at any temperature between 40 and 70 ℃. And (3) writing the interdigital electrode on the surface of the GO film by laser lithography to obtain the GO/rGO micro-corrugated film. The laser writing power is 5-20 mW, the writing depth is 0.01-1 mm, and the wavelength is 450-600 nm. And (3) leading out the interdigital electrode by silver paste to obtain two leads, thus preparing the GO/rGO humidity-sensitive sensing film. The humidity test is carried out in a humidity environment (11-90% RH) set up by different saturated salt solutions at room temperature by using a digital bridge, and the response and the sensitivity of the micro-wrinkle humidity sensitive film are greatly improved. According to the invention, graphene oxide is coated on a biodegradable shape memory film, an oriented micro-corrugated structure is prepared by thermal shrinkage recovery, the graphene oxide is reduced by laser to form an interdigital electrode, and the interdigital electrode is switched in different humidity environments to carry out humidity test. Because the specific surface area is increased by the micro-wrinkle structure, hydrogen bonding between oxygen-containing functional groups of GO and water molecules is easier to realize, and the purpose of improving the response and sensitivity of humidity-sensitive sensing is achieved by the hydrogen bonding between a small amount of oxygen-containing functional groups on rGO and the water molecules and the van der Waals force between rGO and the water molecules.
The invention has the advantages of
The GO/rGO micro-wrinkled humidity sensitive film is innovatively prepared, and response and sensitivity improvement of the GO-based humidity sensing film are realized.
Drawings
FIG. 1 shows the moisture sensitive properties of GO/rGO micropleated films.
FIG. 1 (a) is a continuous dynamic response recovery plot of GO/rGO micro-pleated membrane humidity;
FIG. 1 (b) is the repeatability of GO/rGO micro-pleated membrane humidity sensing at a certain humidity;
FIG. 1 (c) is a graph of the long term stability of GO/rGO micro-pleated membranes in different humidity environments.
Detailed Description
The present invention will be further described with reference to specific examples.
The preparation method of the modified graphene oxide comprises the following steps:
example 1:
the preparation method of the modified graphene oxide comprises the following steps: 100ml of graphene oxide aqueous solution and 1g of gamma-glycidyl ether oxypropyltrimethoxysilane are added into a 200ml reaction kettle, the temperature is controlled at 60 ℃, and the mixture is stirred and reacted for 6 hours to obtain the graphene oxide grafted by the silane coupling agent. The temperature is raised to 90 ℃ and 5g of melamine are added and the reaction is stirred for 2h. And (3) cooling, performing ultrasonic dispersion for 1h, and taking 50ml of upper-layer dispersion liquid as a modified graphene oxide solution (GO).
The preparation method of the GO/rGO film comprises the following steps:
example 2:
the steps of preparing an integrated GO/rGO film using GO are as follows: the shape memory PLA/PPC film is pre-stretched 50% in one direction at 50 ℃, cut into 2cm multiplied by 2cm, and coated with 2mg/mL GO solution layer by layer on the polymer film by adopting a coating method. And after the GO/rGO micro-corrugated film is dried, the shape memory PLA film is subjected to thermal shrinkage recovery at 60 ℃, the interdigital electrode is etched on the surface of the GO film with the laser wavelength of 450nm, the power of 10mW and the etching depth of 0.1mm, so that the complete GO/rGO micro-corrugated film can be obtained.
And (3) performance test results:
1. moisture sensitive characteristics:
continuous dynamic response reply: continuous dynamic response recovery curves can be obtained by placing GO/rGO micropleated film humidity films in different humidity environments (11-90% RH) at room temperature and switching back to P2O5 (0% RH) (the environment where the P2O5 powder is dry is the absolute humidity environment). From the continuous dynamic response recovery curve, the response, response time and recovery time of the GO/rGO micro-corrugated film to different humidity environments at room temperature can be obtained.
2. Repeatability:
the GO/rGO micro-corrugated film is repeatedly switched between a certain humidity environment and an absolute humidity environment for 5 times, so that a humidity-sensitive repeatability curve of the GO/rGO micro-corrugated film can be obtained.
3. Long-term stability:
the integrated GO/rGO film is measured once every 3 days in a humidity environment with the RH being 11-90 percent, and the long-term stability of the humidity sensitivity of the GO/rGO micro-corrugated film can be obtained by continuously measuring for 5 times.
The final moisture sensitive properties we measured for GO/rGO micro-pleated films can be seen in figure 1.
Claims (10)
1. A method for preparing GO/rGO micro-wrinkle humidity-sensitive film by using biodegradable shape memory material is characterized by comprising the following steps: taking a pre-stretched shape memory PLA film as a substrate material; the GO solution is used as a coating layer and is coated on the pre-stretched PLA film by a layer-by-layer coating method; after the GO solution is naturally dried, the PLA film is subjected to thermal shrinkage at a certain temperature; carrying out the etching of interdigital electrodes on the surface of the GO film by using a laser etching method to obtain an integrated GO/rGO film which can be used for humidity detection; adding a graphene oxide aqueous solution and a silane coupling agent into a reaction kettle according to the mass ratio of 100: 0.1-5, controlling the temperature to be 40-80 ℃, and stirring for reaction for 4-10 hours to obtain graphene oxide grafted by the silane coupling agent; the temperature is raised to 90 ℃ and melamine is added; the ratio of the graphene oxide aqueous solution to the melamine is 100: 1-5; and cooling, performing ultrasonic dispersion, and taking the modified graphene oxide solution dispersed on the upper layer.
2. The biodegradable shape memory material prepared GO/rGO micro-pleated humidity sensitive membrane according to claim 1, wherein: the shape memory PLA film comprises PLA copolymer and blend with good biocompatibility; wherein the blend comprises polyethylene glycol (PEG), polylactic acid (PLA) and Polycaprolactone (PCL).
3. The biodegradable shape memory material prepared GO/rGO micro-pleated humidity sensitive membrane according to claim 1, wherein: the GO solution concentration is 2mg/mL.
4. The biodegradable biological shape memory material prepared GO/rGO micro-pleated humidity sensitive membrane according to claim 1, wherein: the coating layer thickness was 20 μm.
5. The biodegradable shape memory material prepared GO/rGO micro-pleated humidity sensitive membrane according to claim 1, wherein: the thermal shrinkage recovery temperature is 50-90 ℃.
6. The biodegradable shape memory material prepared GO/rGO micro-corrugated humidity sensitive membrane as claimed in claim 1, wherein: the wavelength in the laser writing is 450-800 nm; the laser power is 0.5-20 mW; the laser writing depth is 0.01-2 mm.
7. The biodegradable shape memory material prepared GO/rGO micro-corrugated humidity sensitive membrane as claimed in claim 1, wherein: the interdigital electrode is required to be a rectangular interdigital electrode in shape.
8. The biodegradable shape memory material prepared GO/rGO micro-corrugated humidity sensitive membrane according to claim 1 or 2, wherein: the pre-stretching temperature is 40-80 ℃; the pre-stretching ratio is 10-500%.
9. The biodegradable shape memory material prepared GO/rGO micro-pleated humidity sensitive membrane according to claim 1 or 2, characterized in that: the additives required to be added into the PLA film are as follows: 25% melamine.
10. The biodegradable shape memory material prepared GO/rGO micro-corrugated humidity sensitive membrane according to claim 1 or 2, wherein: the PLA film has a film piece size of 40mm multiplied by 20mm and a thickness of 1mm.
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CN109810295A (en) * | 2018-12-29 | 2019-05-28 | 青岛科技大学 | A kind of preparation method of moisture-sensitive sensing membrane |
CN112097967A (en) * | 2020-09-15 | 2020-12-18 | 闽江学院 | Self-energy-supply-based flexible extensible mechanical sensing system and preparation method thereof |
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