CN111928770A - Two-dimensional net-shaped graphene-based tensile strain sensor and preparation method thereof - Google Patents
Two-dimensional net-shaped graphene-based tensile strain sensor and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of a two-dimensional reticular graphene-based tensile strain sensor, which is characterized in that graphene with a two-dimensional reticular structure is formed in a flexible substrate applied with prestress, so that the self-repairing performance of the sensor is improved under the condition of ensuring the detection sensitivity and the strain resistance of the sensor. In the preparation process, N-isopropylacrylamide and vinyl pyrrolidone which are materials with temperature-sensitive characteristics are directly used for preparing the soft gel and are applied to the polydimethylsiloxane electrode template, so that the stretching deformation of the electrode template is realized, the operation is simple, the repeatability is good, the electrode template does not need to be stretched and deformed by additionally applying external force, and the uneven stretching deformation caused by the external force can be avoided. Graphene with a two-dimensional network structure is directly immersed into polydimethylsiloxane containing a temperature-sensitive material, extra modification treatment on the graphene is not needed, complex modification operation is omitted, and cost is reduced.
Description
Technical Field
The invention belongs to the field of sensor preparation, and particularly relates to a two-dimensional reticular graphene-based tensile strain sensor and a preparation method thereof.
Background
The sensor is a detection device, and can convert detected information into an easily-recognized electric signal, a digital signal and the like according to a certain rule. The indexes for determining the quality of the sensor mainly comprise the sensitivity of information receiving and the effectiveness of information conversion. The sensitivity of information reception is closely related to the material and structure of the sensor itself.
The strain sensor is based on the basic principle that a resistance strain effect is utilized, a resistance strain sensitive element is adhered to an elastic element, when the elastic element in the sensor is subjected to strain deformation under the action of the outside, the resistance of the strain sensitive element is correspondingly changed, and then a resistance signal is converted by a conversion circuit and then output. At present, the sensor with the most excellent performance is a graphene-based flexible sensor, which inherits the excellent mechanical property, conductivity, flexibility and stability of graphene and can detect various micro deformations.
After the strain sensor is used for multiple times, strain can be gradually accumulated, and meanwhile, the flexible material can also generate internal damage, so that the sensitivity of the sensor is reduced, namely the self-repairing performance of the sensor is insufficient. Therefore, the invention aims to solve the technical problem that the sensitivity of the tensile strain sensor gradually declines in the using process, and the stability of the sensitivity of the sensor is ensured and the service life is prolonged by improving the self-repairing performance of the sensor.
Disclosure of Invention
In order to solve the problems in the existing two-dimensional reticular graphene-based tensile strain sensor, the invention provides a preparation method of the two-dimensional reticular graphene-based tensile strain sensor.
The preparation method of the two-dimensional reticular graphene-based tensile strain sensor comprises the following steps:
(1) preparation of soft gel precursor:
dissolving 1-5g of urea and 5-10g of formaldehyde in 50ml of water to obtain a mixed solution A; respectively dissolving vinyl polydimethylsiloxane, N-isopropyl acrylamide and vinyl pyrrolidone in a solvent to obtain a solution B, C, D with the mass volume concentration of 5-10g/100ml, and mixing and reacting the solution A, B, C, D according to the volume ratio of 1:2:1:1 to obtain a reaction product M, namely a soft gel precursor.
(2) Preparing graphene with a two-dimensional network structure:
sequentially carrying out ultrasonic cleaning on a two-dimensional copper mesh by using alcohol, acetone and deionized water, drying by using nitrogen, taking the cleaned and dried two-dimensional copper mesh as a template for growing graphene with a two-dimensional network structure, transferring the cleaned and dried two-dimensional copper mesh into a chemical vapor deposition device, carrying out chemical vapor deposition by using raw materials of methane and hydrogen, growing the graphene on the template to obtain the graphene with the two-dimensional network structure, and then etching and removing the two-dimensional copper mesh template by using a chemical etching method to obtain the self-supporting graphene with the two-dimensional network structure;
(3) and (2) heating the soft gel precursor obtained in the step (1) into polydimethylsiloxane to obtain uncured soft gel, placing the uncured soft gel into a transparent glass mold, then soaking the self-supporting graphene with the two-dimensional network structure obtained in the step (2) into the middle position of the uncured soft gel, compacting the uncured soft gel in the mold by using a transparent glass cover plate, then drying and curing, and then cooling to room temperature.
In the step (1), the volume ratio of the soft gel precursor to the polydimethylsiloxane is 1 (2-4).
Wherein, in the step (2), the growth temperature of the graphene with the two-dimensional network structure is 1000-1100 ℃, the flow rate of methane is 30-50sccm, and the flow rate of hydrogen is 20-30 sccm.
Further, in the step (3), electrodes connected to both ends of the graphene of the two-dimensional network structure and wires connected to the electrodes are immersed into the middle of the uncured soft gel together, and then dried and cured.
The drying and curing temperature is 60-80 ℃, and the time is 1-2 h.
In the step (2), the chemical etching method is to chemically etch the two-dimensional copper mesh by using ferric chloride as an etching solution.
In the invention, N-isopropyl acrylamide and vinyl pyrrolidone are added in the process of preparing the soft gel precursor, so that the prepared soft gel has temperature-sensitive characteristics, particularly thermal expansion characteristics. The soft gel precursor with the temperature-sensitive characteristic is added into polydimethylsiloxane, then compaction and heating solidification are carried out in a glass mold, so that the PDMS electrode template obtained after solidification can show uniform expansion and tensile deformation, and after cooling to room temperature, the PDMS electrode template can show a uniformly distributed local compressive stress state. Particularly, the temperature-sensitive material is used for realizing the expansion and tensile deformation of the PDMS electrode template, the temperature-sensitive material is uniformly distributed in the polydimethylsiloxane, the uniform expansion and tensile deformation in the PDMS electrode template is ensured, the internal pressure stress is uniformly distributed after cooling, and the phenomenon of stress concentration is avoided.
Particularly, in the strain sensor, when the sensor is used for measuring the tensile strain of a material, the detection sensitivity of the sensor to the tensile strain can be higher due to the uniformly distributed compressive stress in the PDMS electrode template. Meanwhile, due to the existence of internal compressive stress, the loss of the tensile strain of the measured material to the sensor is reduced, the compressive stress is also beneficial to the self-recovery and self-repairing of the sensor to the tensile strain, the sensitivity of the sensor cannot be reduced due to long-term use, and therefore the service life of the sensor is prolonged.
In the preparation method, the soft gel made of the temperature-sensitive material is directly applied to the polydimethylsiloxane electrode template, so that the stretching deformation of the electrode template is realized, the operation is simple, the repeatability is good, the electrode template is not required to be subjected to stretching deformation by additionally applying external force, and the uneven stretching deformation caused by the external force can be avoided. Graphene with a two-dimensional network structure is directly immersed into polydimethylsiloxane containing a temperature-sensitive material, extra modification treatment on the graphene is not needed, complex modification operation is omitted, and cost is reduced.
Drawings
FIG. 1 is a graph of raw sensitivity of a two-dimensional reticulated graphene-based tensile strain sensor of the present invention at different tensile strains;
FIG. 2 is a graph of raw sensitivity of a sensor of a comparative example at different tensile strains;
FIG. 3 is a graph of the raw sensitivity of a two-dimensional reticulated graphene-based tensile strain sensor of the present invention at different tensile strains after 1000 tensile strain tests at 50%;
FIG. 4 is a graph of the raw sensitivity of the sensor of the comparative example at different tensile strains after 1000 tensile strain tests at 50%.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
A two-dimensional reticular graphene-based tensile strain sensor is prepared by the following steps:
(1) preparation of soft gel precursor:
dissolving 5g of urea and 8g of formaldehyde in 50ml of water to obtain a mixed solution A; dissolving vinyl polydimethylsiloxane, N-isopropylacrylamide and vinyl pyrrolidone in a solvent respectively to obtain a solution B, C, D with the mass volume concentration of 8g/100ml, and mixing and reacting the solution A, B, C, D according to the volume ratio of 1:2:1:1 to obtain a reaction product M, namely a soft gel precursor.
(2) Preparing graphene with a two-dimensional network structure:
sequentially carrying out ultrasonic cleaning on a two-dimensional copper mesh by using alcohol, acetone and deionized water, drying by using nitrogen, taking the cleaned and dried two-dimensional copper mesh as a template for growing graphene with a two-dimensional network structure, transferring the cleaned and dried two-dimensional copper mesh into a chemical vapor deposition device, carrying out chemical vapor deposition by using raw materials of methane and hydrogen, growing the graphene on the template to obtain the graphene with the two-dimensional network structure, and then etching and removing the two-dimensional copper mesh template by using a chemical etching method to obtain the self-supporting graphene with the two-dimensional network structure;
(3) and (2) heating the soft gel precursor obtained in the step (1) into polydimethylsiloxane to obtain uncured soft gel, placing the uncured soft gel into a transparent glass mold, then immersing the self-supporting graphene with the two-dimensional network structure obtained in the step (2), electrodes connected to two ends of the graphene with the two-dimensional network structure and a lead connected with the electrodes into the middle position of the uncured soft gel, drying and curing, and cooling to room temperature.
Wherein, in the step (1), the volume ratio of the soft gel precursor to the polydimethylsiloxane is 1: 3.
In the step (2), the growth temperature of the graphene with the two-dimensional network structure is 1050 ℃, the flow rate of methane is 35sccm, and the flow rate of hydrogen is 20 sccm.
In the step (3), the drying and curing temperature is 80 ℃ and the time is 1 h.
In the step (2), the chemical etching method is to perform chemical etching on the two-dimensional copper mesh by using ferric chloride as an etching solution.
Example 2
A two-dimensional reticular graphene-based tensile strain sensor is prepared by the following steps:
(1) preparation of soft gel precursor:
dissolving 3g of urea and 7g of formaldehyde in 50ml of water to obtain a mixed solution A; dissolving vinyl polydimethylsiloxane, N-isopropylacrylamide and vinyl pyrrolidone in a solvent respectively to obtain a solution B, C, D with the mass volume concentration of 6g/100ml, and mixing and reacting the solution A, B, C, D according to the volume ratio of 1:2:1:1 to obtain a reaction product M, namely a soft gel precursor.
(2) Preparing graphene with a two-dimensional network structure:
sequentially carrying out ultrasonic cleaning on a two-dimensional copper mesh by using alcohol, acetone and deionized water, drying by using nitrogen, taking the cleaned and dried two-dimensional copper mesh as a template for growing graphene with a two-dimensional network structure, transferring the cleaned and dried two-dimensional copper mesh into a chemical vapor deposition device, carrying out chemical vapor deposition by using raw materials of methane and hydrogen, growing the graphene on the template to obtain the graphene with the two-dimensional network structure, and then etching and removing the two-dimensional copper mesh template by using a chemical etching method to obtain the self-supporting graphene with the two-dimensional network structure;
(3) and (2) heating the soft gel precursor obtained in the step (1) into polydimethylsiloxane to obtain uncured soft gel, placing the uncured soft gel into a transparent glass mold, then immersing the self-supporting graphene with the two-dimensional network structure obtained in the step (2), electrodes connected to two ends of the graphene with the two-dimensional network structure and a lead connected with the electrodes into the middle position of the uncured soft gel, drying and curing, and cooling to room temperature.
Wherein, in the step (1), the volume ratio of the soft gel precursor to the polydimethylsiloxane is 1: 4.
In the step (2), the growth temperature of the graphene with the two-dimensional network structure is 1000 ℃, the flow rate of methane is 40sccm, and the flow rate of hydrogen is 30 sccm.
In the step (3), the drying and curing temperature is 70 ℃ and the time is 1 h.
In the step (2), the chemical etching method is to perform chemical etching on the two-dimensional copper mesh by using ferric chloride as an etching solution.
Example 3
A two-dimensional reticular graphene-based tensile strain sensor is prepared by the following steps:
(1) preparation of soft gel precursor:
dissolving 3g of urea and 10g of formaldehyde in 50ml of water to obtain a mixed solution A; dissolving vinyl polydimethylsiloxane, N-isopropylacrylamide and vinyl pyrrolidone in a solvent respectively to obtain a solution B, C, D with the mass volume concentration of 10g/100ml, and mixing and reacting the solution A, B, C, D according to the volume ratio of 1:2:1:1 to obtain a reaction product M, namely a soft gel precursor.
(2) Preparing graphene with a two-dimensional network structure:
sequentially carrying out ultrasonic cleaning on a two-dimensional copper mesh by using alcohol, acetone and deionized water, drying by using nitrogen, taking the cleaned and dried two-dimensional copper mesh as a template for growing graphene with a two-dimensional network structure, transferring the cleaned and dried two-dimensional copper mesh into a chemical vapor deposition device, carrying out chemical vapor deposition by using raw materials of methane and hydrogen, growing the graphene on the template to obtain the graphene with the two-dimensional network structure, and then etching and removing the two-dimensional copper mesh template by using a chemical etching method to obtain the self-supporting graphene with the two-dimensional network structure;
(3) and (2) heating the soft gel precursor obtained in the step (1) into polydimethylsiloxane to obtain uncured soft gel, placing the uncured soft gel into a transparent glass mold, then immersing the self-supporting graphene with the two-dimensional network structure obtained in the step (2), electrodes connected to two ends of the graphene with the two-dimensional network structure and a lead connected with the electrodes into the middle position of the uncured soft gel, drying and curing, and cooling to room temperature.
Wherein, in the step (1), the volume ratio of the soft gel precursor to the polydimethylsiloxane is 1: 2.
In the step (2), the growth temperature of the graphene with the two-dimensional network structure is 1100 ℃, the flow rate of methane is 50sccm, and the flow rate of hydrogen is 20 sccm.
In the step (3), the drying and curing temperature is 60 ℃ and the time is 2 h.
In the step (2), the chemical etching method is to perform chemical etching on the two-dimensional copper mesh by using ferric chloride as an etching solution.
Comparative example
By taking the example 1 as a comparison, the prepared graphene with the two-dimensional network structure is directly laid between two polydimethylsiloxane film layers to prepare the corresponding graphene-based sensor.
The sensitivity profiles of the sensors of example 1 and comparative example were tested at different tensile strains, respectively. At the same time, two sensors were subjected to 1000 tensile strain tests at 50% and then their sensitivity profiles at different tensile strains were measured again. The results are shown in FIGS. 1 to 4.
The good sensitivity of the sensor of the present invention is shown in fig. 1 compared to the sensitivity curve of the sensor of the comparative example shown in fig. 2. Compared with the sensitivity curve of the sensor of the comparative example shown in fig. 4, fig. 3 further shows that the sensor of the present invention has good sensitivity after 1000 uses, which proves that the sensor of the present invention has excellent self-repairing capability, the sensitivity of the sensor is not reduced due to long-term use, and the service life of the sensor is long. Taking the sensitivity of 50% tensile strain rate as an example, the original sensitivity of 50% tensile strain rate is 11.2, the sensitivity after 1000 uses is 11, and the recovery rate reaches 98%.
Claims (7)
1. A preparation method of a two-dimensional reticular graphene-based tensile strain sensor comprises the following steps:
(1) preparation of soft gel precursor:
dissolving 1-5g of urea and 5-10g of formaldehyde in 50ml of water to obtain a mixed solution A; respectively dissolving vinyl polydimethylsiloxane, N-isopropyl acrylamide and vinyl pyrrolidone in a solvent to obtain B, C, D solution with the mass volume concentration of 5-10g/100ml, and mixing and reacting A, B, C, D solution according to the volume ratio of 1:2:1:1 to obtain a reaction product M, namely a soft gel precursor;
(2) preparing graphene with a two-dimensional network structure:
sequentially carrying out ultrasonic cleaning on a two-dimensional copper mesh by using alcohol, acetone and deionized water, drying by using nitrogen, taking the cleaned and dried two-dimensional copper mesh as a template for growing graphene with a two-dimensional network structure, transferring the cleaned and dried two-dimensional copper mesh into a chemical vapor deposition device, carrying out chemical vapor deposition by using raw materials of methane and hydrogen, growing the graphene on the template to obtain the graphene with the two-dimensional network structure, and then etching and removing the two-dimensional copper mesh template by using a chemical etching method to obtain the self-supporting graphene with the two-dimensional network structure;
(3) and (2) simultaneously heating the soft gel precursor obtained in the step (1) into polydimethylsiloxane to obtain uncured soft gel, placing the uncured soft gel into a transparent glass mold, then soaking the self-supporting graphene with the two-dimensional network structure obtained in the step (2) into the middle position of the uncured soft gel, compacting the uncured soft gel in the mold by using a transparent glass cover plate, then drying and curing, and then cooling to room temperature.
2. The method of claim 1, wherein the method comprises the following steps: in the step (1), the volume ratio of the soft gel precursor to the polydimethylsiloxane is 1 (2-4).
3. The method of claim 2, wherein the method comprises the following steps: in the step (2), the growth temperature of the graphene with the two-dimensional network structure is 1000-1100 ℃, the flow rate of methane is 30-50sccm, and the flow rate of hydrogen is 20-30 sccm.
4. The method of claim 1, wherein the method comprises the following steps: in the step (3), electrodes connected to both ends of the graphene in the two-dimensional network structure and a lead connected with the electrodes are immersed into the middle of the uncured soft gel together, and then drying and curing are performed.
5. The method of claim 1, wherein the method comprises the following steps: the drying and curing temperature is 60-80 ℃, and the time is 1-2 h.
6. The method of claim 1, wherein the method comprises the following steps: in the step (2), the chemical etching method is to perform chemical etching on the two-dimensional copper mesh by using ferric chloride as an etching solution.
7. A two-dimensional netted graphene-based tensile strain sensor is characterized in that: the two-dimensional reticular graphene-based tensile strain sensor is prepared by the preparation method of any one of claims 1 to 6.
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