CN108489644B - High-sensitivity sensor based on MXene/rGO composite three-dimensional structure - Google Patents
High-sensitivity sensor based on MXene/rGO composite three-dimensional structure Download PDFInfo
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- CN108489644B CN108489644B CN201810143600.1A CN201810143600A CN108489644B CN 108489644 B CN108489644 B CN 108489644B CN 201810143600 A CN201810143600 A CN 201810143600A CN 108489644 B CN108489644 B CN 108489644B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/18—Measuring force or stress, in general using properties of piezo-resistive materials, i.e. materials of which the ohmic resistance varies according to changes in magnitude or direction of force applied to the material
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a high-sensitivity sensor based on an MXene/rGO composite three-dimensional structure, which is characterized in that a sensing active component of the sensor is the MXene/rGO composite three-dimensional structure; in the MXene/rGO composite three-dimensional structure, MXene is dispersed in reduced graphene oxide (rGO). According to the invention, the composition and structure of a sensing active component in the piezoresistive pressure sensor are improved, an MXene/rGO composite material (especially MXene/rGO composite aerogel) with a three-dimensional structure is introduced, MXene nanosheets with small sizes are dispersed in a graphene oxide GO nanosheet colloidal solution, and an MXene/rGO composite three-dimensional structure formed by dispersing MXene in reduced graphene oxide rGO is finally formed, so that the sensing sensitivity of the piezoresistive pressure sensor can be greatly improved.
Description
Technical Field
The invention belongs to the field of nano materials, and particularly relates to a high-sensitivity sensor based on an MXene/rGO composite three-dimensional structure, which utilizes the characteristics of the MXene/rGO (namely MXene/reduced graphene oxide, referred to as MX/rGO for short) that the aperture and the hole-to-hole distance of an aerogel are greatly adjustable to macroscopically regulate and control the electrical contact of a device so as to carry out sensing (such as pressure sensing).
Background
Two-dimensional materials have attracted considerable attention over the past decade because of their unique electrical, mechanical, optical properties and wide application in many fields. Two-dimensional materials which are synthesized at present comprise graphene, molybdenum sulfide, boron carbide, black phosphorus, antimony tin and the like, and a novel transition metal carbide MXene is prepared from Yury Gogotsi in 2011 by a chemical etching method. It is obtained by etching a parent material MAX, wherein M is a transition metal, A is mainly a group III or IV element, and X is a C or N element. Compared with typical two-dimensional materials such as graphene and molybdenum sulfide, MXene not only has the characteristics of large specific surface area, more active sites, thickness of an atomic layer and the like, but also has the advantages of good hydrophilicity, metal conductivity, adjustable chemical composition and the like, and has good application in the fields of supercapacitors, lithium ion batteries, electromagnetic field shielding, seawater desalination and the like. The sensing performance of MXenes and its related research in the sensor field are not mentioned.
The graphene oxide prepared by the Hummer method has high yield and good quality, a colloidal solution of the graphene oxide can be frozen, GO sheets are regularly arranged in an oriented manner in the growth process of ice crystals, the graphene oxide is frozen and dried to obtain a graphene oxide three-dimensional structure, and finally the graphene oxide aerogel is obtained by thermal treatment and reduction. Graphene is widely used for designing and preparing piezoresistive pressure sensors by virtue of the characteristics of ultralight and superelasticity. Such as Zhang Zhong et al[1]The graphene/carbon tube composite aerogel is prepared by using an ice template and a vacuum high-temperature annealing method, and the sensitivity of the graphene/carbon tube composite aerogel is 0.02-0.19kPa-1(ii) a Li Yibin subject group[2]Synthesizing the graphene/polyimide three-dimensional aerogel by using a similar method, wherein the sensitivity of the graphene/polyimide three-dimensional aerogel is 0.023-0.18kPa-1。
Graphene has the characteristics of ultra-light and ultra-elasticity, and is very suitable for the field of pressure sensors, but the application of graphene in the field is limited due to the lower sensitivity of the graphene.
Reference documents:
[1]Kuang J,Dai Z,Liu L,et al.Synergistic effects from graphene and carbon nanotubes endow ordered hierarchical structure foams with acombination of compressibility,super-elasticity and stability and potentialapplication as pressure sensors.Nanoscale,2015,7(20):9252-9260.
[2]Qin Y,Peng Q,Ding Y,et al.Lightweight,superelastic,and mechanically flexible graphene/polyimide nanocomposite foam for strain sensorapplication.ACS nano,2015,9(9):8933-8941.
disclosure of Invention
Aiming at the defects or improvement requirements in the prior art, the invention aims to provide a high-sensitivity sensor based on an MXene/rGO composite three-dimensional structure, wherein a MXene/rGO composite material (especially an MXene/rGO composite aerogel) with a three-dimensional structure is introduced by improving the composition, structure and the like of a sensing active component in the sensor (such as a piezoresistive pressure sensor), MXene nanosheets with smaller sizes are dispersed in a graphene oxide GO nanosheet colloidal solution, and an MXene/rGO composite three-dimensional structure formed by dispersing MXene in reduced graphene oxide rGO is finally formed, so that the sensing sensitivity (especially the pressure sensing sensitivity) of the sensing active component can be greatly improved; in addition, the invention also optimizes the mass ratio of MXene to rGO (20: 1-5:1, preferably 10:1) in the MXene/rGO composite material and the treatment temperature of the two processes of vacuum freeze-drying (such as-60 ℃) and annealing (such as 200 ℃) adopted in the preparation process, so that the MXene/rGO composite three-dimensional structure with good pressure response can be obtained.
To achieve the above object, according to one aspect of the present invention, there is provided a highly sensitive sensor based on an MXene/rGO composite three-dimensional structure, wherein a sensing active component of the sensor comprises an MXene/rGO composite three-dimensional structure; in the MXene/rGO composite three-dimensional structure, MXene is dispersed in reduced graphene oxide rGO.
As a further preferable mode of the invention, the MXene/rGO composite three-dimensional structure is MXene/rGO composite aerogel; the graphene oxide nano-sheet is preferably prepared by adding MXene solution into Graphene Oxide (GO) nano-sheet colloidal solution, uniformly mixing, and then carrying out vacuum freeze-drying and annealing treatment on the mixed solution.
As a further preferred aspect of the present invention, the dispersoid MXene in the MXene solution is obtained by selectively etching a precursor MAX phase with hydrochloric acid and lithium fluoride; in the MAX phase of the precursor, M is transition metal, A is mainly III group element or IV group element, and X is C element or N element; the dispersoid MXene is preferably Ti3C2A sheet layer with a size of 500-800 nm.
As a further preferred aspect of the present invention, the Graphene Oxide (GO) nanosheets are prepared by a Hummer method, and the size of the graphene oxide nanosheets is 1-5 μm.
As a further preferred aspect of the present invention, the resistance value corresponding to the sensing active member is capable of changing when the pressure condition to which the sensor is exposed changes; preferably, under the action of an external force, the aperture and the distance between the apertures of the MXene/rGO composite three-dimensional structure are changed.
As a further preferable mode of the invention, the high-sensitivity sensor based on the MXene/rGO composite three-dimensional structure is a flexible sensor, and further comprises a flexible polyimide interdigital electrode; preferably, the flexible sensor is prepared by the following steps: conducting metal is formed on the electrode subjected to ink-jet printing through magnetron sputtering, then metal which is in poor contact with a substrate due to ink is removed through ultrasonic cleaning, a flexible interdigital electrode is formed, then MXene/rGO composite aerogel is fixed on the interdigital electrode, finally polyethylene film is used for packaging and fixing, and the copper wire is used for leading the electrode, so that the flexible sensor is obtained.
According to another aspect of the invention, the invention provides an MXene/rGO composite three-dimensional material, which is characterized in that the MXene/rGO composite three-dimensional material is obtained by dispersing MXene in reduced graphene oxide rGO.
In a further preferable aspect of the present invention, in the MXene/rGO composite three-dimensional material, a mass ratio of the MXene to the reduced graphene oxide rGO is 20:1 to 5: 1.
According to another aspect of the invention, the invention provides a preparation method of the MXene/rGO composite three-dimensional material, which is characterized in that the preparation method is obtained by adding MXene solution into Graphene Oxide (GO) nanosheet colloidal solution, uniformly mixing, and then carrying out vacuum freeze-drying and annealing treatment on the mixed solution;
preferably, the processing temperature of the vacuum freeze-drying is (-70) to (-20) DEG C, and the processing temperature of the annealing treatment is 100-450 ℃.
According to another aspect of the invention, the invention provides the application of the MXene/rGO composite three-dimensional material in preparing a sensor; preferably, the sensor is a pressure sensor, more preferably a piezoresistive pressure sensor.
The high-sensitivity flexible sensor based on the MXene/reduced graphene oxide (MX/rGO) composite three-dimensional structure comprises a sensing active component with the MXene/rGO composite three-dimensional structure, wherein the MX/rGO is a porous aerogel structure and can be prepared into the three-dimensional structure by a simple and low-cost ice template through a freeze-drying method and vacuum annealing. In addition, the invention also preferably uses a flexible polyimide interdigital electrode, and can form a high-sensitivity flexible sensor based on an MXene/reduced graphene oxide (MX/rGO) composite three-dimensional structure.
The invention provides a novel material (namely, MXene/rGO composite three-dimensional material) capable of obtaining a high-sensitivity piezoresistive sensor, and the novel two-dimensional material MXene and graphene form a three-dimensional composite structure, so that the high-sensitivity sensor (such as the piezoresistive sensor, especially a pressure sensor based on MX/rGO aerogel) can be obtained. When the MX/rGO aerogel is subjected to external pressure, the internal pore diameter and the pore-to-pore distance of the MX/rGO aerogel are reduced, so that the nanosheets are in close contact to form a large number of conductive paths, and the current is increased sharply; after the external force is removed, the internal pore diameter, the pore-to-pore distance and the like of the MX/rGO aerogel can be restored to the original state, the conductive path is reduced, and the current is reduced, so that higher sensitivity can be obtained; and the pure graphene aerogel without MXene is added, under the action of an external force, the pore diameter, the pore-to-pore distance of the pure graphene aerogel can be reduced, but the change amplitude of the current is not large (namely, compared with the pure graphene aerogel, the resistance change amplitude of the MX/rGO composite aerogel under the action of the external force is large). Under the action of external force, the pore diameter and the pore-to-pore distance of the MX/rGO aerogel can be obviously changed. To confirm this conclusion, the aerogel samples were observed by in situ scanning electron microscopy. The pore diameter, the pore-to-pore distance are gradually reduced along with the increase of the external force, and the pore diameter, the pore-to-pore distance are restored after the external force is removed; and researches find that the MX/rGO aerogel sample can still recover the original structural state after ten thousand times of back-and-forth compression.
The composite aerogel has the advantages of ultralight weight, high elasticity, high strength, sensitive response to electricity and the like, is very suitable for a pressure sensor, and has the characteristics of low manufacturing cost and simple process. The MX/rGO porous aerogel structure can be still a uniform solution after simple physical mixing of MXene and Graphene Oxide (GO) nanosheet colloids synthesized by a solution method, and then is subjected to vacuum freeze-drying and annealing to prepare an ultra-light and super-elastic three-dimensional structure.
MXene is a two-dimensional carbide with thick atomic scale and has abundant physicochemical properties, but the characteristic of easy oxidation of MXene prevents the application of MXene in many fields. MXene and GO prepared by a chemical solution method can be prepared into a uniform solution after simple physical mixing, and the hierarchical porous three-dimensional composite aerogel is obtained after vacuum freeze-drying and annealing. The composite aerogel has good mechanical properties and can show higher sensitivity than pure graphene aerogel, and the synergistic effect of MXene and graphene enables the composite material to improve the performance of the whole sensor system. MXene has a smaller size than graphene, so that self-stacking of graphene can be avoided in the process of forming aerogel; on the other hand, it can be embedded in graphene aerogel, blocking its combination with air to prevent the oxidation of MXene. In addition, the invention also controls the mass ratio of MXene to rGO in the MXene/rGO composite material to be 20:1-5:1 (preferably 10:1), and preferably controls the processing temperature of vacuum freeze-drying to be (-70) to (-20) DEG C (such as-60 ℃) in the preparation process of the MXene/rGO composite material, and controls the processing temperature of annealing treatment to be 100-450 ℃ (such as 200 ℃) so as to obtain the MXene/rGO composite three-dimensional structure with good pressure response.
Therefore, the high-sensitivity flexible sensor based on the MXene/reduced graphene oxide (MX/rGO) composite three-dimensional structure can effectively avoid the complicated and toxic process to enable the sensing material to have a three-dimensional hierarchical porous structure, and the high-sensitivity flexible sensor can be obtained by leading the electrodes by means of the flexible interdigital electrodes.
Drawings
FIG. 1 is a schematic view of device assembly, wherein FIG. (a) is a schematic view of MX/rGO composite aerogel preparation process; FIG. (b) is a process for preparing a MX/rGO-based composite aerogel pressure sensor; and (c) the working principle of the MX/rGO composite aerogel pressure sensor. .
The diagram (a) in fig. 2 shows the particle size distribution diagram of MXene nanosheets; panel (b) particle size distribution plot of GO nanoplates.
FIG. 3 is a graph (a) showing the physical diagram and the Tyndall effect of MXene colloidal solution; graph (b) physical representation and tyndall effect of GO colloidal solution; graph (c) physical representation and tyndall effect of mixed MXene and GO solutions.
Figure 4 is a Scanning Electron Microscope (SEM) image of a redox graphene aerogel of figure (a); FIG. (b) SEM image of MX/rGO composite aerogel, the mass ratio of GO to MXene in the preparation process is 20: 1; FIG. (c) SEM picture of MX/rGO composite aerogel, the mass ratio of GO to MXene in the preparation process is 10: 1; FIG. (d) SEM image of MX/rGO composite aerogel, the mass ratio of GO to MXene in the preparation process is 5: 1.
FIG. 5 is a graph of the mechanical properties of MX/rGO composite aerogels and rGO aerogels of FIG. (a); graph (b) is based on the electrical response plots of the MX/rGO composite aerogel and rGO aerogel pressure sensors to different pressures.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The MX/rGO composite aerogel is used as an active material of the sensor, and preferably, a polyimide metal interdigital electrode is used as a device electrode, so that response of an electrical signal to a series of external pressures is carried out.
The MXene in the invention can selectively etch the A layer in the precursor MAX by HCl and LiF (the precursor MAX is a type of ternary layered compound), and the hydrated lithium ions are intercalated, and then the single-layer MXene nanosheet is obtained by ultrasonic stripping and centrifuging. This can be followed by ultrasonic mixing with GO solution, after vacuum freeze-drying and annealing, resulting in a composite aerogel. Preferably, MX/rGO aerogel based flexible pressure sensors can be prepared by means of flexible polyimide interdigitated electrodes. When the MX/rGO aerogel is subjected to external pressure, the internal pore diameter, the pore-to-pore distance and the like of the MX/rGO aerogel are reduced, so that the nanosheets are closely contacted to form a large number of conductive paths, the current is sharply increased, and higher sensitivity is obtained. The pure graphene aerogel without MXene is reduced in pore diameter and pore-to-pore distance under the action of an external force, but the change range of the current is small.
To reduce the sensor manufacturing cost, MXene and GO synthesized by a solution method are uniformly mixed by simple physical ultrasound, and then vacuum freeze-drying and annealing are carried out, as shown in FIG. 1. The method is easy to scale up, and has no secondary pollution. The specific synthesis steps of MXene can be as follows: 0.5g of MAX powder was slowly added to a mixed solution of 10ml of 9M hydrochloric acid and 0.5g of LiF, and reacted at 35 ℃ for 24 hours with magnetic stirring. Research shows that when the molar ratio of LiF to MAX is 7.5 to 1 and the concentration of hydrochloric acid is 9M, the obtained MXene nanosheets have better quality (less defects) and higher yield. And then, carrying out centrifugal cleaning on the mixed solution for 5-6 times until the pH value reaches neutral, wherein the supernatant after the last centrifugation is black green, which marks the successful synthesis of MXene. And dispersing the synthesized MXene into a certain amount of deionized water, and performing ultrasonic mechanical stripping for 1h while introducing inert gas. Note that the temperature cannot exceed 25 ℃ throughout the sonication. Centrifuging the MXene solution subjected to ultrasonic stripping at 3500rpm for 1h, and collecting the supernatant to obtain the MXene nanosheet colloidal solution. In the research, the concentration of the MXene nanosheet colloidal solution is 2-8mg/ml, and the concentration can be increased along with the increment of the ultrasonic time (30-60min), the centrifugal time (30-60min) and the rotating speed (3500-.
MXene has good hydrophilicity and metal conductivity, but the characteristic of easy oxidation hinders the application of MXene in many fields. The graphene synthesis technology is mature, and the industrial application of the graphene synthesis technology is about to be realized, wherein GO synthesized by the Hummer solution method is micron-sized, as shown in fig. 2 (b). MXene synthesized by the solution method is generally nano-sized as shown in fig. 2 (a). MXene has a smaller size than graphene, so that self-stacking of graphene can be avoided in the process of forming aerogel; on the other hand, it can be embedded in graphene aerogel, blocking its combination with air to prevent the oxidation of MXene.
As shown in fig. 3, MXene and GO colloidal solutions, when mixed, remained as a homogeneous solution without agglomeration. Fig. 4 shows the SEM image of MX/rGO composite aerogel, from which it can be seen that the composite aerogel possesses a porous structure with pore size distribution from microscopic to mesoporous. And with the increase of the content of MXene in the aerogel, the three-dimensional structure is more and more compact, and the grading phenomenon is more and more obvious. For the mechanical properties of the pure graphene and MX/rGO composite aerogel, the composite aerogel is found to have higher mechanical strength, so that the stability of the whole sensor can be improved. Fig. 5(a) shows the pressure-strain curves of pure graphene and MX/rGO composite aerogel (GO: MX ═ 10:1), and it is clear that the MX/rGO composite aerogel mechanical properties are superior to those of pure graphene. The mathematical expression for the sensitivity of a piezoresistive pressure sensor is:
in fig. 5(b), MX/rGO composite aerogel (GO: MX ═ 10:1) shows higher sensitivity in response to a range of pressures, confirming better electrical response signals for MX/rGO composite aerogel, as shown in fig. 5 (b).
MXene as the raw material used in the present invention is preferably Ti3C2A sheet layer with a size of 500-800nm (such as 584.5 nm); graphene oxide GO nanosheets are preferably prepared by the Hummer method, and have a size of 1-5 μm (e.g., 1276.1 nm).
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. A high-sensitivity sensor based on an MXene/rGO composite three-dimensional structure is characterized in that a sensing active component of the sensor comprises the MXene/rGO composite three-dimensional structure; in the MXene/rGO composite three-dimensional structure, MXene is dispersed in reduced graphene oxide rGO; the resistance value corresponding to the sensing active component can change when the pressure condition of the sensor changes; under the action of external force, the aperture, the hole and the hole distance of the MXene/rGO composite three-dimensional structure can be changed.
2. The MXene/rGO composite three-dimensional structure-based highly sensitive sensor of claim 1, wherein the MXene/rGO composite three-dimensional structure is an MXene/rGO composite aerogel; the graphene oxide nano-sheet is prepared by adding MXene solution into Graphene Oxide (GO) nano-sheet colloidal solution, uniformly mixing, and then carrying out vacuum freeze-drying and annealing treatment on the mixed solution.
3. The MXene/rGO composite three-dimensional structure-based highly sensitive sensor of claim 2, wherein the dispersoid MXene in the MXene solution is obtained by selectively etching a precursor MAX phase with hydrochloric acid and lithium fluoride; in the MAX phase of the precursor, M is transition metal, A is mainly III group element or IV group element, and X is C element or N element; the dispersoid MXene is Ti3C2A sheet layer with a size of 500-800 nm.
4. The MXene/rGO composite three-dimensional structure-based highly sensitive sensor of claim 2, wherein the Graphene Oxide (GO) nanosheets are prepared by a Hummer method, and the graphene oxide nanosheets have a size of 1-5 μm.
5. The MXene/rGO composite three-dimensional structure-based high-sensitivity sensor of claim 1, wherein the MXene/rGO composite three-dimensional structure-based high-sensitivity sensor is a flexible sensor, further comprising a flexible polyimide interdigital electrode; the flexible sensor is prepared by the following steps: conducting metal is formed on the electrode subjected to ink-jet printing through magnetron sputtering, then metal which is in poor contact with a substrate due to ink is removed through ultrasonic cleaning, a flexible interdigital electrode is formed, then MXene/rGO composite aerogel is fixed on the interdigital electrode, finally polyethylene film is used for packaging and fixing, and the copper wire is used for leading the electrode, so that the flexible sensor is obtained.
6. An MXene/rGO composite three-dimensional material is characterized in that the MXene/rGO composite three-dimensional material is obtained by dispersing MXene in reduced graphene oxide rGO, and is specifically prepared by adding an MXene nanosheet colloidal solution obtained through ultrasonic stripping treatment into a Graphene Oxide (GO) nanosheet colloidal solution, uniformly mixing, and then carrying out vacuum freeze-drying and annealing treatment; under the action of external force, the aperture, the hole and the hole distance of the MXene/rGO composite three-dimensional material can be changed.
7. The MXene/rGO composite three-dimensional material according to claim 6, wherein the mass ratio of the MXene to the reduced graphene oxide rGO in the MXene/rGO composite three-dimensional material is 20:1-5: 1.
8. The method for preparing the MXene/rGO composite three-dimensional material according to claim 6, wherein the processing temperature of the vacuum freeze-drying is (-70) — (-20) ° C, and the processing temperature of the annealing treatment is 100-450 ℃.
9. Use of the MXene/rGO composite three-dimensional material of claim 6 or 7 in the preparation of a sensor; the sensor is a piezoresistive pressure sensor.
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