CN111378205A - Preparation method of PDMS sponge-based strain sensor material - Google Patents
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Abstract
The invention belongs to the field of flexible electronic materials, and particularly relates to a preparation method of a PDMS sponge-based strain sensor material, which comprises the following steps: firstly, preparing a sugar cube by taking common white granulated sugar and soft white sugar in life as raw materials, then preparing PDMS sponge by taking the sugar cube as a sacrificial template, sequentially dipping and coating the PDMS sponge in a chitosan solution and a graphene oxide dispersion liquid, then reducing by using a reducing agent ascorbic acid to prepare RGO/PDMS sponge, finally coating a layer of silver nanowires (AgNWs) on the RGO/PDMS sponge by a dripping coating method, and drying to prepare the AgNWs/RGO/PDMS sponge strain sensor material. The strain sensor material disclosed by the invention has good conductivity, the resistance can be obviously changed in compressive strain, the stability of the compression cycle is excellent, the preparation process is simple, the operation is easy, and the strain sensor material is a novel material with very high development potential in the field of intelligent flexible strain sensors.
Description
Technical Field
The invention belongs to the field of flexible electronic materials, relates to preparation of a strain sensor material, and more particularly relates to a preparation method of a PDMS sponge-based strain sensor material.
Background
With the accelerated development of wearable intelligent equipment, the strain sensor shows good application prospects in the fields of human motion detection, human health monitoring, artificial muscles, human-computer interfaces and the like. However, the conventional strain sensor is generally made of metal or inorganic semiconductor, and the detection range thereof is limited (5%), which cannot meet the urgent requirement of the high strain sensor. In addition, the preparation process is complex, and the application and development of the preparation are restricted due to high manufacturing cost. Therefore, there is an urgent need to develop new flexible intelligent strain sensors. The flexible polymer material and the nanometer conductive material are assembled into the conductive composite material with the sponge structure, the deformation range is wide, and the flexible composite material is expected to be applied to the flexible strain sensor.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a novel method for preparing a strain sensor material with a sponge structure. Firstly, the different granularities of common white granulated sugar and soft white sugar in life are utilized to prepare the square sugar with two particle structures, and then the PDMS sponge with a developed pore structure is prepared by taking the square sugar as a sacrificial template. Due to the high hydrophobicity and inertia of PDMS, a layer of chitosan with positive charges is firstly attached to the surface of PDMS sponge, so that graphene oxide can be effectively attached to the PDMS sponge. And finally, covering a layer of silver nanowires on the surface of the RGO/PDMS by adopting a drop coating method, so that the PDMS sponge has stronger conductivity and the strain sensing performance is improved.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a PDMS sponge-based strain sensor material comprises the following steps:
(1) preparing the square sugar by taking white granulated sugar and soft white sugar as raw materials;
(2) preparing PDMS sponge by taking cubic sugar as a sacrificial template;
(3) graphene oxide is attached to the surface of PDMS sponge and reduced to prepare RGO/PDMS sponge;
(4) and (3) dropwise coating the silver nanowires on the surface of the RGO/PDMS sponge to obtain the AgNWs/RGO/PDMS sponge strain sensor material.
In the step (1), the preparation method of the cubic sugar comprises the following steps: weighing 5g of white granulated sugar and soft white sugar respectively, placing into a beaker, stirring uniformly, adding 1ml of deionized water, continuing stirring, placing the stirred sugar into a cubic mold with the edge length of 1-2cm, and placing into an oven to dry for 5h to obtain the cube sugar.
In the step (2), the mass ratio of 10: 1, weighing a proper amount of PDMS (polydimethylsiloxane) gum and a curing agent, placing the PDMS gum and the curing agent in a beaker, stirring for 5min violently, removing bubbles generated by stirring by using ultrasonic waves, immersing the cubic sugar prepared in the step (1) in the PDMS gum, placing the PDMS gum in a vacuum drying oven, vacuumizing and standing for 2h, taking out the PDMS gum and placing the PDMS gum in an oven for curing at the temperature of 100 ℃ and 120 ℃ for 1h, finally placing the cured cubic sugar in deionized water, and drying the PDMS sponge after the cubic sugar is fully dissolved.
In the step (3), firstly, the PDMS sponge prepared in the step (2) is immersed into 0.2-0.4mg/ml acidic chitosan solution with pH of 4-6 to be extruded for 5 times, and then the PDMS sponge is put into an oven to be dried, and then the PDMS sponge is immersed into 1-2mg/ml graphene oxide dispersion liquid to be extruded for 5 times, and the GO/PDMS sponge is prepared through drying in the oven, which is a GO attaching process in the PDMS sponge. This process was cycled three times, then GO/PDMS sponge was placed in 5mg/ml ascorbic acid solution and reduced in an oven at 95 ℃ for 12h to make RGO/PDMS sponge.
In the step (4), 3-5ml of the RGO/PDMS sponge surface prepared in the step (3) is coated with 1mg/ml of silver nanowire ethanol dispersion liquid drop by a drop coating method, and the AgNWs/RGO/PDMS sponge strain sensor material is obtained after natural drying.
Compared with the prior art, the invention has the following advantages:
(1) the invention utilizes different granularities of common white granulated sugar and soft white sugar in life to prepare the square sugar with two particle structures, and further prepares the PDMS sponge with a developed pore structure by taking the square sugar as a sacrificial template.
(2) Due to the high hydrophobicity and inertia of the PDMS, a layer of chitosan with positive charges is firstly attached to the surface of the PDMS sponge, so that the graphene oxide is effectively attached to the PDMS sponge.
(3) The method adopts a dripping method to drip and coat the silver nanowires on the RGO/PDMS sponge, and the prepared AgNWs/RGO/PDMS sponge has stronger conductivity and improves the strain sensing performance.
The PDMS sponge-based strain sensor material disclosed by the invention has good conductivity, the resistance can be obviously changed in compressive strain, and the PDMS sponge-based strain sensor material has excellent compressive cycle stability, is simple in preparation process and easy to operate, and is a new material with very high development potential in the field of intelligent flexible strain sensors.
Drawings
FIG. 1 is a photograph of the AgNWs/RGO/PDMS sponge prepared in example 1 after compression and recovery;
FIG. 2 is a graph of the change in resistance of the AgNWs/RGO/PDMS sponge made in example 1 at 0% to 70% cyclic compressive strain;
FIG. 3 is a graph of the change in resistance of the RGO/PDMS sponge prepared in comparative example 1 at 0% to 70% cyclic compressive strain.
Detailed Description
In order to make the present invention easier to understand, the following examples will further illustrate the present invention, but the scope of the present invention is not limited to these examples.
The invention simultaneously measures the resistance variation performance of the conductive composite material along with the compressive strain through a data acquisition system and a universal tester, sets the compression displacement speed of the universal tester to be 5mm/min and the displacement to be 0.7cm, then resets at a constant speed and cycles for 8 times, and sets the acquisition frequency of the data acquisition system to be 2 times per second.
Example 1
Weighing 5g of white granulated sugar and soft white sugar respectively, putting the white granulated sugar and the soft white sugar into a beaker, uniformly stirring, adding 1ml of deionized water, continuously stirring, putting the stirred sugar into a cube mold with the edge length of 1cm, and putting the cube mold into an oven to dry for 5 hours to obtain the cube sugar.
Step (2), according to 10: 1, weighing a proper amount of PDMS (polydimethylsiloxane) gum and a curing agent, placing the PDMS gum and the curing agent in a beaker, stirring for 5min vigorously, removing bubbles generated by stirring with ultrasound, immersing the cube sugar prepared in the step (1) in the mixture, placing the cube sugar in a vacuum drying oven for vacuumizing and standing for 2h, taking out the cube sugar, placing the cube sugar in an oven for curing at 100 ℃ for 1h, finally placing the cured cube sugar in deionized water, and drying the cube sugar after the cube sugar is fully dissolved to obtain the PDMS sponge.
And (3) firstly soaking the PDMS sponge prepared in the step (2) into an acidic chitosan solution of 0.2mg/ml for extrusion for 5 times, putting the PDMS sponge into an oven for drying, then soaking the PDMS sponge into a graphene oxide dispersion of 1mg/ml for extrusion for 5 times, and drying the PDMS sponge in the oven to obtain the GO/PDMS sponge, which is the process of attaching GO to the PDMS sponge once. This process was cycled three times, then GO/PDMS sponge was placed in 5mg/ml ascorbic acid solution and reduced in an oven at 95 ℃ for 12h to make RGO/PDMS sponge.
And (4) dripping 5ml of the silver nanowire ethanol dispersion liquid of 1mg/ml on the surface of the RGO/PDMS sponge prepared in the step (3) by using a dripping method, and naturally drying to obtain the AgNWs/RGO/PDMS sponge strain sensor material.
FIG. 1 is a photograph of the PDMS sponge based strain sensor material that can be compressed rapidly by finger-pressure and then recovered rapidly after relaxation. FIG. 2 shows that the PDMS sponge-based strain sensor material has a resistance of 2.68k Ω under an unstressed condition, and a resistance reduction of 18.2 Ω under 70% compressive strain (70 kPa), and has a good strain sensing range; in the 70% compression-release process, the sponge has high resistance change response speed and high sensitivity; and the resistance change trend keeps good stability and repeatability in 8 compression-release cycles. The results show that the PDMS sponge-based strain sensor material has good conductivity, the resistance can be obviously changed in compressive strain, and simultaneously, the PDMS sponge-based strain sensor material has excellent compressive cycle stability and can be used for manufacturing intelligent flexible strain sensors.
Comparative example 1
The procedure was exactly the same as in example 1 except that step (4) of example 1 was not performed, i.e., the silver nanowires were not drop-coated, i.e., RGO/PDMS sponge was prepared.
FIG. 3 shows that the RGO/PDMS sponge has a resistance of 3.9 k.OMEGA.under unstressed condition, and a resistance decrease of 2.7 k.OMEGA.under 70% compressive strain (70 kPa), and the strain sensing range is narrower than that of example 1; in the 70% compression-release process, the response speed of the resistance change of the RGO/PDMS sponge is slower than that of example 1, and the sensitivity is relatively low; also, the resistance change was less reproducible than in example 1 in 8 compression-release cycles. Therefore, in the AgNWs/RGO/PDMS sponge, AgNWs are very important for improving the conductivity and the strain sensing performance of the sponge.
Comparative example 2
Exactly the same procedure as in comparative example 1 was conducted except that the prepared PDMS sponge was extruded 5 times by immersing it in an acidic chitosan solution of 0.2mg/ml in step (3) of comparative example 1, i.e., RGO/PDMS sponge to which chitosan was not attached was prepared.
By comparing the resistances of the RGO/PDMS sponge in comparative example 1 and comparative example 2, the resistance of the RGO/PDMS sponge in comparative example 2 reaches 200 k.OMEGA.in the uncompressed state, whereas the resistance of the RGO/PDMS sponge in comparative example 2 is only 3.9 k.OMEGA.in the uncompressed state. The result shows that a layer of chitosan with positive charges is attached to the surface of the PDMS sponge, so that the graphene oxide can be effectively attached to the PDMS sponge, and the prepared RGO/PDMS has lower resistance. Therefore, chitosan plays a crucial role in the present invention.
Example 2
Weighing 5g of white granulated sugar and soft white sugar respectively, putting the white granulated sugar and the soft white sugar into a beaker, uniformly stirring, adding 1ml of deionized water, continuously stirring, putting the stirred sugar into a cube mold with the edge length of 1cm, and putting the cube mold into an oven to dry for 5 hours to obtain the cube sugar.
Step (2), according to 10: 1, weighing a proper amount of PDMS (polydimethylsiloxane) gum and a curing agent, placing the PDMS gum and the curing agent in a beaker, stirring for 5min vigorously, removing bubbles generated by stirring with ultrasound, immersing the cube sugar prepared in the step (1) in the mixture, placing the cube sugar in a vacuum drying oven for vacuumizing and standing for 2h, taking out the cube sugar, placing the cube sugar in an oven for curing at 100 ℃ for 1h, finally placing the cured cube sugar in deionized water, and drying the cube sugar after the cube sugar is fully dissolved to obtain the PDMS sponge.
And (3) firstly soaking the PDMS sponge prepared in the step (2) into an acidic chitosan solution of 0.2mg/ml for extrusion for 5 times, putting the PDMS sponge into an oven for drying, then soaking the PDMS sponge into a graphene oxide dispersion of 2mg/ml for extrusion for 5 times, and drying the PDMS sponge in the oven to obtain the GO/PDMS sponge, which is the process of attaching GO to the PDMS sponge once. This process was cycled three times, then GO/PDMS sponge was placed in 5mg/ml ascorbic acid solution and reduced in an oven at 95 ℃ for 12h to make RGO/PDMS sponge.
And (4) dripping 5ml of the silver nanowire ethanol dispersion liquid of 1mg/ml on the surface of the RGO/PDMS sponge prepared in the step (3) by using a dripping method, and naturally drying to obtain the AgNWs/RGO/PDMS sponge strain sensor material.
Example 3
Weighing 5g of white granulated sugar and soft white sugar respectively, putting the white granulated sugar and the soft white sugar into a beaker, uniformly stirring, adding 1ml of deionized water, continuously stirring, putting the stirred sugar into a cube mold with the edge length of 1cm, and putting the cube mold into an oven to dry for 5 hours to obtain the cube sugar.
Step (2), according to 10: 1, weighing a proper amount of PDMS (polydimethylsiloxane) gum and a curing agent, placing the PDMS gum and the curing agent in a beaker, stirring for 5min vigorously, removing bubbles generated by stirring with ultrasound, immersing the cube sugar prepared in the step (1) in the mixture, placing the cube sugar in a vacuum drying oven for vacuumizing and standing for 2h, taking out the cube sugar, placing the cube sugar in an oven for curing at 120 ℃ for 1h, placing the cured cube sugar in deionized water, and drying the cube sugar after the cube sugar is fully dissolved to obtain the PDMS sponge.
And (3) firstly soaking the PDMS sponge prepared in the step (2) into an acidic chitosan solution of 0.4mg/ml for extrusion for 5 times, putting the PDMS sponge into an oven for drying, then soaking the PDMS sponge into a graphene oxide dispersion of 1mg/ml for extrusion for 5 times, and drying the PDMS sponge in the oven to obtain the GO/PDMS sponge, which is a GO attaching process in the PDMS sponge. This process was cycled three times, then GO/PDMS sponge was placed in 5mg/ml ascorbic acid solution and reduced in an oven at 95 ℃ for 12h to make RGO/PDMS sponge.
And (4) dripping 5ml of the silver nanowire ethanol dispersion liquid of 1mg/ml on the surface of the RGO/PDMS sponge prepared in the step (3) by using a dripping method, and naturally drying to obtain the AgNWs/RGO/PDMS sponge strain sensor material.
Example 4
Weighing 5g of white granulated sugar and soft white sugar respectively, putting the white granulated sugar and the soft white sugar into a beaker, uniformly stirring, adding 1ml of deionized water, continuously stirring, putting the stirred sugar into a cube mold with the edge length of 1cm, and putting the cube mold into an oven to dry for 5 hours to obtain the cube sugar.
Step (2), according to 10: 1, weighing a proper amount of PDMS (polydimethylsiloxane) gum and a curing agent, placing the PDMS gum and the curing agent in a beaker, stirring for 5min vigorously, removing bubbles generated by stirring with ultrasound, immersing the cube sugar prepared in the step (1) in the mixture, placing the cube sugar in a vacuum drying oven for vacuumizing and standing for 2h, taking out the cube sugar, placing the cube sugar in an oven for curing at 100 ℃ for 1h, finally placing the cured cube sugar in deionized water, and drying the cube sugar after the cube sugar is fully dissolved to obtain the PDMS sponge.
And (3) firstly soaking the PDMS sponge prepared in the step (2) into an acidic chitosan solution of 0.2mg/ml for extrusion for 5 times, putting the PDMS sponge into an oven for drying, then soaking the PDMS sponge into a graphene oxide dispersion of 1mg/ml for extrusion for 5 times, and drying the PDMS sponge in the oven to obtain the GO/PDMS sponge, which is the process of attaching GO to the PDMS sponge once. This process was cycled three times, then GO/PDMS sponge was placed in 5mg/ml ascorbic acid solution and reduced in an oven at 95 ℃ for 12h to make RGO/PDMS sponge.
And (4) dripping 3ml of the silver nanowire ethanol dispersion liquid with the concentration of 1mg/ml on the surface of the RGO/PDMS sponge prepared in the step (3) by using a dripping method, and naturally drying to obtain the AgNWs/RGO/PDMS sponge strain sensor material.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (10)
1. A preparation method of a PDMS sponge-based strain sensor material is characterized by comprising the following steps: which comprises the following steps:
(1) preparing the square sugar by taking white granulated sugar and soft white sugar as raw materials;
(2) preparing PDMS sponge by taking cubic sugar as a sacrificial template;
(3) graphene oxide is attached to the surface of PDMS sponge and reduced to prepare RGO/PDMS sponge;
(4) and (3) dropwise coating the silver nanowires on the surface of the RGO/PDMS sponge to obtain the AgNWs/RGO/PDMS sponge strain sensor material.
2. The method of claim 1, wherein the method comprises the following steps: in the step (1), the preparation method of the cubic sugar comprises the following steps: weighing 5g of white granulated sugar and soft white sugar respectively, putting into a beaker, uniformly stirring, adding 1ml of deionized water, continuously stirring, putting the stirred sugar into a cube mold with the edge length of 1cm, and putting into an oven to dry for 5 hours to obtain the cube sugar.
3. The method of claim 1, wherein the method comprises the following steps: in the step (2), a proper amount of PDMS virgin rubber and a curing agent are weighed, placed in a beaker and stirred vigorously for 5min, bubbles generated by stirring are removed by ultrasonic, then the cube sugar prepared in the step (1) is immersed in the PDMS virgin rubber and the curing agent, placed in a vacuum drying oven for vacuumizing and standing for 2h, taken out and placed in an oven for curing, finally the cured cube sugar is placed in deionized water, and dried after the cube sugar is fully dissolved, so that the PDMS sponge is obtained.
4. The method of claim 3, wherein the method comprises the following steps: the PDMS virgin rubber and the curing agent are mixed according to the mass ratio of 10: 1, and mixing.
5. The method of claim 3, wherein the method comprises the following steps: the curing specifically comprises the following steps: curing at 100-120 ℃ for 1 h.
6. The method of claim 1, wherein the method comprises the following steps: in the step (3), firstly, soaking the PDMS sponge prepared in the step (2) into an acidic chitosan solution with the pH value of 4-6 of 0.2-0.4mg/ml, extruding for 5 times, drying in an oven, soaking in the graphene oxide dispersion liquid for treatment, and drying in the oven to obtain the GO/PDMS sponge, which is a GO attaching process in the PDMS sponge; the process is cycled for three times, and then the GO/PDMS sponge is reduced to prepare the RGO/PDMS sponge.
7. The method of claim 6, wherein the method comprises the following steps: the graphene oxide dispersion liquid is treated, specifically, 1-2mg/ml of graphene oxide dispersion liquid is extruded for 5 times.
8. The method of claim 6, wherein the method comprises the following steps: the reduction is specifically that GO/PDMS sponge is put into an ascorbic acid solution of 5mg/ml and reduced in an oven at 95 ℃ for 12 h.
9. The method of claim 1, wherein the method comprises the following steps: in the step (4), 3-5ml of the RGO/PDMS sponge surface prepared in the step (3) is coated with 1mg/ml of silver nanowire ethanol dispersion liquid drop by a drop coating method, and the AgNWs/RGO/PDMS sponge is obtained after natural drying.
10. PDMS sponge based strain sensor material obtainable by a method of preparation according to any one of claims 1 to 5.
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| CN113150371A (en) * | 2021-04-09 | 2021-07-23 | 华东师范大学 | PDMS sponge-based strain sensor and preparation method thereof |
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| CN114702826A (en) * | 2022-04-15 | 2022-07-05 | 电子科技大学 | Super-hydrophobic spongy three-dimensional conductive composite material and preparation method and application thereof |
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