CN110108376B - Method for preparing patterned graphene temperature sensor by using laser - Google Patents
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- CN110108376B CN110108376B CN201910378266.2A CN201910378266A CN110108376B CN 110108376 B CN110108376 B CN 110108376B CN 201910378266 A CN201910378266 A CN 201910378266A CN 110108376 B CN110108376 B CN 110108376B
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Abstract
The invention provides a method for preparing patterned graphene temperature sensing by using laser, which comprises the following steps: step 1, placing a copper foil sample loaded with graphene into a corrosive solution to etch foil, transferring the graphene into deionized water to clean after copper in the sample is completely etched, and then transferring the graphene onto a transparent substrate; step 2, arranging geometric patterns in an array arrangement on a flexible substrate carrying graphene to obtain the flexible substrate with the geometric patterns, wherein the distance between two adjacent geometric patterns is 50-1000 microns; the side length of each pattern is 30-300 mu m; step 3, etching the geometric patterns on the flexible substrate with the geometric pictures in the step 2 by using pulse laser to obtain patterned graphene formed on the surface of the transparent substrate; step 4, assembling patterned graphene formed on the surface of the transparent substrate into a graphene temperature sensor; the preparation process is safe and pollution-free, and can be completed in an open environment at normal temperature and normal pressure; meanwhile, the invention fills the blank of the temperature sensor in the aspect of flexible transparent nano-sensors.
Description
Technical Field
The invention belongs to the field of nano sensors, and particularly relates to a method for preparing a patterned graphene temperature sensor by using laser.
Background
We are about to step into an era of wearable smart products, where the most critical one is the flexible transparent user interface. The appearance of graphene provides a better choice for next-generation wearable smart products. The graphene material has unique physicochemical properties, such as huge specific surface area, high intrinsic mobility, high Young modulus, high thermal conductivity, high optical transmittance and high electrical conductivity; compared with the carbon nano tube, the graphene has the characteristics of softness, biocompatibility, large surface area effect and easiness in chemical modification and functionalization, and lays a foundation for realizing sensitivity, intellectualization and convenience of the sensor. In many applications of graphene, a graphene flexible sensor has become a core component of a next-generation wearable smart product.
Through development for many years, the traditional temperature sensor has multiple advantages of high sensitivity, low cost and the like, but still has some inherent defects due to the self structure and the like, for example, the traditional sensor has lower resolution on a micro-nano scale and is difficult to be embedded into a structural material for testing. Graphene sensors based on nanomaterials and their synthetic components are therefore of increasing interest due to their unique sensing properties. According to the report, a Jumbo team of Qinghua university utilizes a copper mesh to prepare the reticular graphene, and the reticular graphene is assembled into a simple strain sensor, so that the ultrahigh sensitivity is measured, the sensing performance of the simple strain sensor is comparable to that of a traditional sensor, and the simple strain sensor has the characteristics of transparency, flexibility and the like. This work lays a foundation for graphene sensors.
However, the research on the graphene sensor is mainly focused on the strain sensor at present, and the temperature sensing is rarely reported. The important detection data in the electronic skin (E-skin) is the body temperature of a human body, so that the temperature sensing in the range of 36-42 ℃ is an important ring for the practical application of the electronic skin.
Disclosure of Invention
The invention aims to provide a method for preparing a patterned graphene temperature sensor by using laser, which solves the defects in the prior art.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a method for preparing a patterned graphene temperature sensor by using laser, which comprises the following steps:
step 1, placing a copper foil sample loaded with graphene into a corrosive solution to etch foil, transferring the graphene into deionized water to clean after copper in the sample is completely etched, and then transferring the graphene onto a transparent substrate;
step 2, arranging geometric patterns in an array arrangement on a flexible substrate carrying graphene to obtain the flexible substrate with the geometric patterns, wherein the distance between two adjacent geometric patterns is 50-1000 microns; the side length of each pattern is 30-300 mu m;
step 3, etching the geometric patterns on the flexible substrate with the geometric pictures in the step 2 by using pulse laser to obtain patterned graphene formed on the surface of the transparent substrate;
and 4, assembling the patterned graphene formed on the surface of the transparent substrate into the graphene temperature sensor.
Preferably, in step 1, the etching solution is a mixed solution of ferric chloride and hydrochloric acid, wherein the weight ratio of ferric chloride to hydrochloric acid is 1: 1, were mixed in a mass ratio of 1.
Preferably, in the step 1, the concentration of the etching solution is 0.5mol/L, wherein the concentration of ferric chloride in the etching solution is 0.25mol/L, and the concentration of hydrochloric acid is 0.25 mol/L.
Preferably, in step 2, the geometric pattern is a circle, a triangle, a square, an ellipse, a wave, a polygon, a zigzag or a spiral.
Preferably, in step 3, the pulsed laser is a nanosecond laser, a picosecond laser, or a femtosecond laser.
Preferably, the wavelength of the pulse laser is 256-1100 nm, and the laser power is 1-100W.
Preferably, in step 3, the parameters of the laser pulse: laser power density of 1.0X 105～100.0×105W/cm2(ii) a The energy distribution of the light spots is uniform distribution, Gaussian distribution or multi-mode distribution; the scanning speed is 10-500 mm/s; the laser frequency is 1-100 KHz.
Preferably, in step 1, the flexible transparent substrate is glass, polymethyl methacrylate, polydimethylsiloxane or polyethylene terephthalate.
Preferably, in the step 1, the graphene is prepared by a chemical vapor deposition method, wherein the number of graphene layers is 2-20.
Compared with the prior art, the invention has the beneficial effects that:
according to the method for preparing the patterned graphene temperature sensor by using the laser, provided by the invention, the pulse laser can be focused to an ultrafine space region, the influence on surrounding materials in the related space range cannot be caused in the processing process, and no energy transfer, conversion, heat existence and heat diffusion exist in the process; establishing a one-to-one correspondence relationship of graphene pattern-defect-temperature sensing performance by designing topological structures of different pattern types and densities; the preparation process is safe and pollution-free, and can be completed in an open environment at normal temperature and normal pressure; meanwhile, the invention fills the blank of the temperature sensor in the aspect of flexible transparent nano-sensors.
Further, the power density by the laser is 1.0 × 105～100.0×105W/cm2(ii) a The energy distribution of the light spots is uniform distribution, Gaussian distribution or multi-mode distribution; the scanning speed is 10-500 mm/s; the laser frequency is 1-100 KHz and other technological parameters, ultra-fine processing of each independent pattern can be realized, and the edges are neat in nanometer scale.
Drawings
FIG. 1 is a square array pattern;
FIG. 2 is a circular array pattern;
FIG. 3 is a triangular array pattern;
fig. 4 is a graph of resistance change values versus temperature.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
In order to solve the technical problems in the background art, the invention provides a preparation method of a patterned graphene gas sensor, which is to perform patterning processing on complete graphene by adopting ultrashort pulse laser to enable the complete graphene to have a specific topological structure, wherein each topological structure has a specific defect type and density, so that the purpose of controllable defect introduction is achieved, the heat conductivity of the graphene is reduced in a controllable manner, and large resistance change can be generated for small temperature change, and further sensing is performed.
The invention provides a method for preparing a patterned graphene temperature sensor by using laser, which comprises the following steps:
step 1, placing a copper foil sample carrying graphene into a corrosive solution to etch a copper foil, transferring the graphene into deionized water after copper in the sample is completely etched, soaking for 30min, repeating the process for 2-3 times, and then transferring the graphene onto a transparent substrate;
wherein, the corrosion solution is a mixed solution of ferric chloride and hydrochloric acid, wherein the ferric chloride solution and the hydrochloric acid solution are mixed according to the weight ratio of 1: 1, and the concentration of the etching solution is 0.5mol/L, wherein the concentration of ferric chloride in the etching solution is 0.25mol/L, and the concentration of hydrochloric acid is 0.25 mol/L.
Step 2, designing a graphene topological structure: the complete graphene has ultrahigh heat conduction performance, once the graphene is damaged, the heat transfer of carriers can be interrupted, the temperature sensing characteristic can be realized, the graphene topological structure is designed, namely the pattern array of the graphene film transferred to the flexible substrate in the step 1 is designed, and the inside of each independent pattern is an area to be irradiated by laser.
Step 3, irradiating the pattern array preset in the step 2 by using an ultrashort pulse laser beam to obtain patterned graphene formed on the surface of the transparent substrate;
and 4, assembling the patterned graphene in the step 3 into a graphene temperature sensor and testing the temperature sensing performance of the graphene temperature sensor.
In step 1, the flexible transparent substrate is glass, polymethyl methacrylate (PMMA), Polydimethylsiloxane (PDMS), or polyethylene terephthalate (PET plastic).
In the step 1, the graphene is prepared by a chemical vapor deposition method, wherein the number of graphene layers is 2-20.
In the step 2, the graphene pattern array is in a shape of a circle, a triangle, a square, an ellipse, a wave, a polygon, a sawtooth or a spiral line, the side length of each pattern is 30-300 μm, and the distance between the patterns is 50-1000 μm.
In the step 3, the laser beam is nanosecond laser, picosecond laser or femtosecond laser; the wavelength of the laser beam is 256-1100 nm, and the laser power is 1-100W.
In the process of patterning graphene, laser parameters have a large influence on the graphene pattern processing, and orthogonal experiments are required to optimize parameters such as the power density of laser, the energy distribution of light spots, the scanning speed, the laser frequency and the like, wherein the optimal power density of laser is 1.0 × 105～100.0×105W/cm2(ii) a The energy distribution of the light spots is uniform distribution, Gaussian distribution or multi-mode distribution; the scanning speed is 10-500 mm/s; the laser frequency is 1-100 KHz.
In the step 4, in the performance test, the test temperature range is 30-50 ℃.
Example 1
Performing square etching treatment on graphene on Polydimethylsiloxane (PDMS) by using picosecond laser, and detecting the temperature sensing performance of the patterned graphene.
The preparation steps are as follows:
(1) preparation of transparent substrate PDMS
Mixing the DC184 and the curing agent in a ratio of 10: 1, fully stirring to generate bubbles, putting the bubbles into an ultrasonic cleaning instrument for ultrasonic treatment until the bubbles disappear completely, pouring the bubbles into a mould (150mm x 10mm), and placing the mould in an oven at 80 ℃ for curing for 2 hours.
(2) Graphene transfer
FeCl with the concentration of 0.5mol/L is prepared3And the/HCl solution is used for etching copper, and graphene/copper foil with the area of 10mm x 10mm is cut and placed on the surface of the etching solution. And (3) after etching for 2-4 hours, transferring the graphene into deionized water by using filter paper, soaking for 30min, transferring into new deionized water, soaking for 30min, and transferring to the PDMS substrate in the step 1.
(3) Laser preparation of patterned graphene
And (3) irradiating the surface of the graphene/PDMS obtained in the step (2) by using a picosecond (ps) laser beam, wherein the diameter of a light spot is 30 micrometers, the power is 10W, the scanning speed is 10-200mm/s, and the repetition frequency is 10 KHz. A square array with a pattern area of 100 μm and a pattern density of 100 μm is designed in advance, and a high-energy laser beam ablates graphene in an irradiation area in cooperation with the movement of a galvanometer or a numerical control machine, so as to obtain the patterned graphene with the square array formed on the surface of the transparent substrate in the step 1, as shown in fig. 1.
(4) Patterned graphene temperature sensor assembly and testing
And 3, leading out silver wires at two ends of the square array patterned graphene as electrodes, and connecting the electrodes to a detection circuit to obtain the patterned graphene temperature sensor. The sensor is placed in a temperature control table, the temperature is increased from 30 ℃ to 50 ℃, the temperature increasing speed is 1 ℃/min, the graphene resistance is changed along with the temperature change, and the relation curve of the resistance change value and the time is obtained and is shown in figure 4. Under the condition, the sensitivity range of the square patterned graphene can reach 292 mV/g.
Example 2
And performing square etching treatment on graphene on Polydimethylsiloxane (PDMS) by using femtosecond laser, and detecting the temperature sensing performance of the patterned graphene sample.
The preparation steps are as follows:
(1) preparation of transparent substrate PDMS
Mixing the DC184 and the curing agent in a ratio of 10: 1, fully stirring to generate bubbles, putting the bubbles into an ultrasonic cleaning instrument for ultrasonic treatment until the bubbles disappear completely, pouring the bubbles into a mould (150mm x 10mm), and placing the mould in an oven at 80 ℃ for curing for 2 hours.
(2) Graphene transfer
FeCl with the concentration of 0.5mol/l is prepared3And the/HCl solution is used for etching copper, and graphene/copper foil with the area of 10mm x 10mm is cut and placed on the surface of the etching solution. And (3) after etching for 2-4 hours, transferring the graphene into deionized water by using filter paper, soaking for 30min, transferring into new deionized water, soaking for 30min, and transferring to the PDMS substrate in the step 1.
(3) Laser preparation of patterned graphene
And (3) irradiating the surface of the graphene/PDMS obtained in the step (2) by using a femtosecond (fs) laser beam, wherein the diameter of a light spot is 30 micrometers, the power is 1W, the scanning speed is 50mm/s, and the repetition frequency is 60 KHz. A circular square array with a pattern area of 100 μm and a pattern density of 100 μm is designed in advance, and a high-energy laser beam ablates graphene in an irradiation area by matching with the motion of a galvanometer or a numerical control machine tool, so as to obtain the patterned graphene with the circular array formed on the surface of the transparent substrate in the step 1, as shown in fig. 2.
(4) Patterned graphene temperature sensor assembly and testing
And 3, leading out silver wires at two ends of the square array patterned graphene as electrodes, and connecting the electrodes to a detection circuit to obtain the patterned graphene temperature sensor. And (3) placing the sensor in a temperature control table, so that the temperature is increased from 30 ℃ to 50 ℃, the temperature increase speed is 1 ℃/min, and the graphene resistance is changed along with the temperature change, so that a relation curve of the resistance change value and the time is obtained. Under the condition, the sensitivity range of the square patterned graphene can reach 468 mV/g.
Example 3
Triangular etching treatment is carried out on graphene on Polydimethylsiloxane (PDMS) by femtosecond laser, and the adsorption and desorption performances of a patterned graphene sample on formaldehyde are detected.
The preparation steps are as follows:
(1) preparation of transparent substrate PDMS
Mixing the DC184 and the curing agent in a ratio of 10: 1, fully stirring to generate bubbles, putting the bubbles into an ultrasonic cleaning instrument for ultrasonic treatment until the bubbles disappear completely, pouring the bubbles into a mould (150mm x 10mm), and placing the mould in an oven at 80 ℃ for curing for 2 hours.
(2) Graphene transfer
FeCl with the concentration of 0.5mol/l is prepared3And the/HCl solution is used for etching copper, and graphene/copper foil with the area of 10mm x 10mm is cut and placed on the surface of the etching solution. And (3) after etching for 2-4 hours, transferring the graphene into deionized water by using filter paper, soaking for 30min, transferring into new deionized water, soaking for 30min, and transferring to the PDMS substrate in the step 1.
(3) Laser preparation of patterned graphene
And (3) irradiating the surface of the graphene/PDMS obtained in the step (2) by using a femtosecond (fs) laser beam, wherein the diameter of a light spot is 30 micrometers, the power is 1W, the scanning speed is 50mm/s, and the repetition frequency is 60 KHz. Designing a triangular array with the side length of the pattern being 100 microns and the pattern density being 100 microns in advance, and matching with the motion of a galvanometer or a numerical control machine, the high-energy laser beam can ablate graphene in an irradiation area to obtain the patterned graphene with the triangular array formed on the surface of the transparent substrate in the step 1, as shown in fig. 3.
(4) Patterned graphene temperature sensor assembly and testing
And 3, leading out silver wires at two ends of the circular array patterned graphene as electrodes, and connecting the electrodes to a detection circuit to obtain the patterned graphene temperature sensor. The sensor is placed in a temperature control table, so that the temperature is increased from 30 ℃ to 50 ℃, the temperature increasing speed is 1 ℃/min, the graphene resistance is changed along with the temperature change, and a relation curve of the resistance change value and the temperature is obtained, as shown in the attached figure 2. Under the condition, the sensitivity range of the square patterned graphene can reach 833 mV/g.
Claims (7)
1. A method for preparing a patterned graphene temperature sensor by using laser is characterized by comprising the following steps:
step 1, placing a copper foil sample loaded with graphene into a corrosive solution to etch foil, transferring the graphene into deionized water to clean after copper in the sample is completely etched, and then transferring the graphene onto a transparent substrate;
step 2, arranging geometric patterns in an array arrangement on the transparent substrate carrying the graphene to obtain the transparent substrate with the geometric patterns, wherein the distance between two adjacent geometric patterns is 50-1000 microns; the side length of each pattern is 30-300 mu m; the geometric figure is a triangle;
step 3, etching the geometric patterns on the transparent substrate with the geometric pictures in the step 2 by using pulse laser to obtain patterned graphene formed on the surface of the transparent substrate;
step 4, assembling patterned graphene formed on the surface of the transparent substrate into a graphene temperature sensor;
in step 3, parameters of the pulse laser are as follows: laser power density of 1.0X 105～100.0×105W/cm2(ii) a The energy distribution of the light spots is uniform distribution, Gaussian distribution or multi-mode distribution; the scanning speed is 10-500 mm/s; the laser frequency is 1-100 KHz;
in step 4, the patterned graphene formed on the surface of the transparent substrate is assembled into the graphene temperature sensor, and the specific method comprises the following steps:
and (4) leading out silver wires as electrodes from two ends of the patterned graphene formed on the surface of the transparent substrate obtained in the step (3), connecting the electrodes into a detection circuit, and assembling to obtain the graphene temperature sensor.
2. The method for preparing the patterned graphene temperature sensor by using the laser as claimed in claim 1, wherein in the step 1, the etching solution is a mixed solution of ferric chloride and hydrochloric acid, wherein the ratio of ferric chloride to hydrochloric acid is 1: 1, were mixed in a mass ratio of 1.
3. The method for preparing the patterned graphene temperature sensor by using the laser according to claim 1 or 2, wherein in the step 1, the concentration of the etching solution is 0.5mol/L, wherein the concentration of ferric chloride in the etching solution is 0.25mol/L, and the concentration of hydrochloric acid is 0.25 mol/L.
4. The method for preparing the patterned graphene temperature sensor by using the laser as claimed in claim 1, wherein in the step 3, the pulse laser is a nanosecond laser, a picosecond laser or a femtosecond laser.
5. The method for preparing the patterned graphene temperature sensor by using the laser according to claim 1 or 4, wherein the wavelength of the pulse laser is 256-1100 nm, and the laser power is 1-100W.
6. The method for preparing the patterned graphene temperature sensor by using the laser according to claim 1, wherein in the step 1, the transparent substrate is glass, polymethyl methacrylate, polydimethylsiloxane or polyethylene terephthalate.
7. The method of claim 1, wherein in the step 1, the graphene is prepared by a chemical vapor deposition method, wherein the number of graphene layers is 2-20.
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| CN111748112B (en) * | 2020-06-19 | 2022-04-08 | 辽宁格莱菲尔健康科技有限公司 | Method for compounding and integrating graphene high-sensitivity sensing circuit and latex |
| CN112244766A (en) * | 2020-09-23 | 2021-01-22 | 浙江工业大学 | Wound microenvironment detection device |
| CN112758918A (en) * | 2021-02-22 | 2021-05-07 | 陕西科技大学 | Preparation method and application of purple phosphorus/graphene composite material |
| CN112964380A (en) * | 2021-03-22 | 2021-06-15 | 浙江大学 | Preparation method of flexible temperature sensor based on laser processing method |
| CN113091939A (en) * | 2021-03-29 | 2021-07-09 | 哈尔滨工业大学 | Preparation method of high-sensitivity temperature sensor based on graphene/barium strontium titanate heterojunction |
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