CN108489644A - High sensitive sensor based on MXene/rGO complex three-dimensional structures - Google Patents
High sensitive sensor based on MXene/rGO complex three-dimensional structures Download PDFInfo
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- CN108489644A CN108489644A CN201810143600.1A CN201810143600A CN108489644A CN 108489644 A CN108489644 A CN 108489644A CN 201810143600 A CN201810143600 A CN 201810143600A CN 108489644 A CN108489644 A CN 108489644A
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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
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
Abstract
The invention discloses a kind of high sensitive sensors based on MXene/rGO complex three-dimensional structures, which is characterized in that the sensing active component of the sensor is MXene/rGO complex three-dimensional structures；In the MXene/rGO complex three-dimensional structures, MXene is dispersed in redox graphene (rGO).The present invention is by being improved the composition of sensing active component, structure in sensor piezoresistive pressure sensor, introduce the MXene/rGO composite materials (especially MXene/rGO composite aerogels) of three-dimensional structure, the smaller MXene nanometer sheets of size are scattered in graphene oxide GO nanometer sheet colloidal solution, and ultimately form MXene be dispersed in redox graphene rGO and the MXene/rGO complex three-dimensional structures that constitute, the sensing sensitivity of piezoresistance sensor can be greatly improved.
Description
Technical field
The invention belongs to field of nanometer material technology, more particularly, to a kind of height based on MXene/rGO complex three-dimensional structures
Fast-response probe, the sensor utilize MXene/rGO (i.e. MXene/ redox graphenes, referred to as MX/rGO) aerogel pores
Diameter, the very big adjustable characteristic of Kong Yukong distances carry out the electrical contact of macro adjustments and controls device, to be sensed (such as pressure sensing
Deng).
Background technology
In past 10 years, two-dimensional material because of its unique electricity, mechanics, optical property and answering in various fields extensively
With arousing widespread concern.The two-dimensional material synthesized at present has dilute graphite, molybdenum sulfide, boron carbide, black phosphorus, antimony
Tin etc., Yury Gogotsi in 2011 are prepared for a kind of novel transition metal carbide-MXene by chemical etching method.
It is obtained by etching fertile material MAX, and wherein M is magnesium-yttrium-transition metal, and A is mainly III or IV race's element, and X is C or N
Element.Compared with the typical two-dimensional material such as graphene, molybdenum sulfide, MXene not only have large specific surface area, active site mostly with
And the characteristics such as atomic layer level thickness, also possess good hydrophily, metallic conductivity, the advantages such as chemical composition is adjustable, in super electricity
The fields such as container, lithium ion battery, electromagnetic-field-shielded, sea water desalination are demonstrated by good application.The sensing capabilities of MXenes with
And its but rarely has and refer in the correlative study of sensor field.
It is good with the graphene oxide yield height of Hummer methods preparation, quality, its colloidal solution can be freezed, in ice crystal
Growth course makes the orientation rule arrangement of GO lamellas, then is freeze-dried to obtain graphene oxide three-dimensional structure, finally heat treatment reduction
Obtain graphene aerogel.Graphene is widely used in design, prepares pressure drag type pressure sensing by its ultralight and superlastic characteristic
Device.Such as Zhang Zhong et al.[1]It is prepared for graphene/carbon pipe composite aerogel with ice template and vacuum high-temperature annealing method, sensitivity is
0.02-0.19kPa-1；The refined seminars of Li Yi[2]A kind of graphene/polyimides three-dimensional aeroge has been synthesized with similar method,
Its sensitivity is 0.023-0.18kPa-1。
Graphene has ultralight, superlastic characteristic, is readily applicable to be used for art of pressure sensors, however simple graphene compared with
Low sensitivity but limits its application in this field.
Bibliography：
[1]Kuang J,Dai Z,Liu L,et al.Synergistic effects from graphene and
carbon nanotubes endow ordered hierarchical structure foams with a
combination of compressibility,super-elasticity and stability and potential
application 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 sensor
application.ACS nano,2015,9(9):8933-8941.
Invention content
For the disadvantages described above or Improvement requirement of the prior art, the purpose of the present invention is to provide one kind being based on MXene/
The high sensitive sensor of rGO complex three-dimensional structures, wherein by sensing activity in sensor (such as piezoresistive pressure sensor)
Composition, structure of component etc. are improved, and introducing the MXene/rGO composite materials of three-dimensional structure, (especially MXene/rGO is compound
Aeroge), the smaller MXene nanometer sheets of size are scattered in graphene oxide GO nanometer sheet colloidal solution, and ultimately forms
MXene is dispersed in redox graphene rGO and the MXene/rGO complex three-dimensional structures of composition, can greatly improve sensing and live
The sensing sensitivity (especially pressure sensing sensitivity) of property component；Also, the present invention is also by MXene/rGO composite materials
The mass ratio (20 of MXene and rGO：1-5:1, preferably 10:1) and employed in its preparation process vacuum freeze-drying (as-
60 DEG C) and annealing (such as 200 DEG C) handle the treatment temperatures of the two techniques and optimize, can be derived that and responded with excellent pressure
MXene/rGO complex three-dimensional structures.
To achieve the above object, according to one aspect of the present invention, it provides a kind of based on MXene/rGO complex three-dimensional knots
The high sensitive sensor of structure, which is characterized in that the sensing active component of the sensor includes MXene/rGO complex three-dimensional structures；
In the MXene/rGO complex three-dimensional structures, MXene is dispersed in redox graphene rGO.
As present invention further optimization, the MXene/rGO complex three-dimensional structures are the compound airsettings of MXene/rGO
Glue；Preferably through MXene solution is added into graphene oxide (GO) nanometer sheet colloidal solution, after mixing, then should
Mixed solution carries out what vacuum freeze-drying was prepared with annealing.
As present invention further optimization, the dispersate MXene in the MXene solution, is by hydrochloric acid and fluorination
Lithium selective etch presoma MAX phases obtain；In the presoma MAX phases, M is magnesium-yttrium-transition metal, and A is mainly III race member
Element or IV race's element, X are C element or N element；The dispersate MXene is preferably Ti3C2Lamella, size 500-800nm.
As present invention further optimization, graphene oxide (GO) nanometer sheet is prepared into using Hummer methods
It arrives, the size of the stannic oxide/graphene nano piece is 1-5 μm.
As present invention further optimization, the corresponding resistance value of the sensing active component can be residing for sensor
Variation is generated when pressure condition changes；Preferably, under the effect of external force, the MXene/rGO complex three-dimensional structures
Aperture, Kong Yukong distances can change.
As present invention further optimization, the high sensitive sensor based on MXene/rGO complex three-dimensional structures is
Flexible sensor further includes flexible polyimide interdigital electrode；Preferably, which be prepared into using following steps
It arrives：By conductive metal on the good electrode magnetron sputtering of inkjet printing, then it is cleaned by ultrasonic and gets rid of because ink exists and substrate
The metal of poor contact forms flexible interdigital electrode and then MXene/rGO composite aerogels is fixed in the interdigital electrode,
It is finally encapsulated and is fixed with polyethylene film, and copper wire draws electrode, to obtain flexible sensor.
It is another aspect of this invention to provide that the present invention provides a kind of MXene/rGO complex three-dimensionals material, feature exists
In the MXene/rGO complex three-dimensionals material, which is dispersed in by MXene in redox graphene rGO, to be obtained.
As present invention further optimization, in the MXene/rGO complex three-dimensionals material, the MXene is gone back with described
The mass ratio of both former graphene oxide rGO is 20:1-5:1.
Another aspect according to the invention, the present invention provides the preparation method of above-mentioned MXene/rGO complex three-dimensionals material,
It is characterized in that, this method is by the way that MXene solution is added into graphene oxide (GO) nanometer sheet colloidal solution, is uniformly mixed
Afterwards, then by the mixed solution carry out what vacuum freeze-drying was prepared with annealing；
Preferably, the treatment temperature of the vacuum freeze-drying is (- 70)~(- 20) DEG C, the treatment temperature of the annealing
It is 100~450 DEG C.
It is another aspect of this invention to provide that the present invention provides above-mentioned MXene/rGO complex three-dimensionals materials to prepare sensing
Application in device；Preferably, the sensor is pressure sensor, more preferably piezoresistive pressure sensor.
The highly sensitive flexible biography based on MXene/ redox graphenes (MX/rGO) complex three-dimensional structures in the present invention
Sensor, sensing active component therein include MXene/rGO complex three-dimensional structures, and MX/rGO is porous aerogel structure, can be with
It is that three-dimensional structure is being prepared by desivac and vacuum annealing with simple, low cost ice template.In addition, the present invention is further preferably
Using flexible polyimide interdigital electrode, can be formed based on MXene/ redox graphenes (MX/rGO) complex three-dimensional structures
Highly sensitive flexible sensor.
The present invention provides a kind of new materials can get highly sensitive piezoresistive transducer (that is, MXene/rGO is compound
Three-dimensional material), by the way that New Two Dimensional material MXene and graphene are formed three dimensional composite structure, it can get highly sensitive sensing
Device (such as piezoresistive transducer is based especially on the pressure sensor of MX/rGO aeroges).When by ambient pressure, MX/rGO gas
Gel internal orifice dimension, hole and pitch-row defection reduce, and promote nanometer sheet contact close, form a large amount of conductive path, electric current is sharp
Increase；And after removing external force, MX/rGO aeroges internal orifice dimension, hole and pitch-row defection are restored to original state, and conductive path subtracts
Small, electric current reduces, therefore can obtain higher sensitivity；Pure graphene aerogel without adding MXene, in outer masterpiece
Under, although aperture, hole and pitch-row defection can reduce, the amplitude of variation of electric current is less (that is, compared to pure graphene gas
Gel, MX/rGO composite aerogels are big by the resistance variations amplitude of outer force effect).Under the effect of external force, MX/rGO aeroges
Aperture, hole and pitch-row defection significant change occurs.In order to confirm this conclusion, by in-situ scanning electron microscope to gas
Gel sample carries out implementation observation.It was found that with the increase of external force, aperture, hole and pitch-row defection are gradually reduced, when external force removes
Later, aperture, hole and pitch-row defection restore shape；And research finds that MX/rGO aeroges sample carrys out back pressure by up to ten thousand time
Contracting, still can restore initial configuration state.
The advantages that composite aerogel is sensitive with ultralight, high resiliency, high intensity and to the response of electricity, is readily applicable to pressure
Sensor, and there is low manufacture cost, feature simple for process.MX/rGO porous aerogels structure can be synthesized by solwution method
MXene and the mixing of graphene oxide (GO) nanometer sheet colloid simple physical after, be still uniform solution, it is rear to carry out vacuum jelly
Prepared by dry and annealing forms ultralight, super-elasticity three-dimensional structure.
MXene is a kind of two-dimentional carbide of atomic scale thickness, has abundant physicochemical properties, but it is easy to aoxidize
Characteristic hinder applications of the MXene in many fields.The present invention prepares ground MXene and GO by chemical solution method, carries out letter
After single physical mixed, it can be prepared into uniform solution, after vacuum freeze-drying and annealing, it is multiple to obtain classifying porous three-dimensional
Close aeroge.Such composite aerogel has good mechanical performance, and can show than simple graphene aerogel more
The synergistic effect of high sensitivity, MXene and graphene so that the composite material can improve the property of entire sensor systems
Energy.MXene has smaller size on the one hand can be to avoid graphene during forming aeroge with respect to graphene
Self is stacked；On the other hand, it can be embedded in graphene aerogel, stop the combination of itself and air to prevent the oxidation of MXene.
In addition, the present invention is also by being 20 by the mass ratio control of MXene and rGO in MXene/rGO composite materials:1-5:1 (preferably
10:1), and preferably in the preparation process of MXene/rGO composite materials, by the control of the treatment temperature of vacuum freeze-drying be (- 70)~
(- 20) DEG C (such as -60 DEG C), the treatment temperature control of annealing is 100~450 DEG C (such as 200 DEG C), can obtain having good
The MXene/rGO complex three-dimensional structures of pressure response.
As it can be seen that being based on the highly sensitive flexibility of MXene/ redox graphenes (MX/rGO) complex three-dimensional structures in the present invention
Sensor, can effectively prevent cumbersome and toxic technique makes sensing material have three-dimensional graded porous structure, and this hair
It is bright also to obtain highly sensitive flexible sensor by means of flexible interdigital electrode to draw electrode.
Description of the drawings
Fig. 1 is device assembling schematic diagram, wherein figure (a) is MX/rGO composite aerogel preparation flow schematic diagrames；Scheming (b) is
Preparation process based on MX/rGO composite aerogel pressure sensors；Scheme the work of (c) MX/rGO composite aerogel pressure sensors
Make principle..
The grain size distribution of (a) MXene nanometer sheets is schemed in Fig. 2；Scheme the grain size distribution of (b) GO nanometer sheets.
The pictorial diagram and Tyndall effect of (a) MXene colloidal solution are schemed in Fig. 3；Scheme (b) GO colloidal solution pictorial diagram and
Tyndall effect；Scheme the pictorial diagram and Tyndall effect of (c) MXene and GO mixed solutions.
Scanning electron microscope (SEM) figure of (a) redox graphene aerogel is schemed in Fig. 4；It is compound to scheme (b) MX/rGO
The SEM of aeroge schemes, and the mass ratio of GO and MXene is 20 during preparation:1；Scheme (c) MX/rGO composite aerogels
SEM schemes, and the mass ratio of GO and MXene is 10 during preparation:1；The SEM figures for scheming (d) MX/rGO composite aerogels, are making
The mass ratio of GO and MXene is 5 in standby process:1.
The mechanical performance figure of (a) MX/rGO composite aerogels and rGO aeroges is schemed in Fig. 5；It is compound based on MX/rGO to scheme (b)
The electroresponse figure of aeroge and rGO aeroges pressure sensor to different pressures.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
It does not constitute a conflict with each other and can be combined with each other.
The present invention uses MX/rGO composite aerogels for the active material of sensor, preferably polyimide metal interdigital electrode
For device electrode, a series of response of the electrical signal to ambient pressures is carried out.
In the present invention MXene can (presoma MAX be one with the A layers in HCl and LiF selective etch presomas MAX
The ternary layered compound of class), while being hydrated lithium ion and carrying out intercalation, then single layer is obtained by the method for ultrasound stripping, centrifugation
MXene nanometer sheets.And then ultrasonic mixing can be carried out with GO solution, after vacuum freeze-drying and annealing, obtains compound airsetting
Glue.It is preferred that the pliable pressure sensor based on MX/rGO aeroges can be prepared for by means of flexible polyimide interdigital electrode.
When by ambient pressure, MX/rGO aeroges internal orifice dimension, hole and pitch-row defection reduce, and promote nanometer sheet contact close, are formed a large amount of
Conductive path, electric current sharp increases, and obtains higher sensitivity.Pure graphene aerogel without adding MXene,
Under outer force effect, although aperture, hole and pitch-row defection can reduce, the amplitude of variation of electric current is little.
To reduce sensor manufacturing cost, the MXene and GO of solwution method synthesis are equably mixed by simple physical ultrasound
It closes, then carries out vacuum freeze-drying and annealing, as shown in Figure 1.This method is easy scale, and does not have secondary pollution.MXene
Specific synthesis step can be：0.5g MAX powder is taken to be slowly added to the hydrochloric acid and 0.5g LiF mixed solutions of 10ml 9M
In, it is reacted for 24 hours under magnetic agitation at 35 DEG C.Research finds to work as LiF:MAX=7.5:1 (molar ratio), when concentration of hydrochloric acid is 9M,
Obtained MXene nanometer sheets better quality (defect is few), yield higher.Then above-mentioned mixed liquor is subjected to eccentric cleaning 5-6
Secondary to reach neutrality to pH, last time centrifuged supernatant should be blackish green, indicate the successful synthesis of MXene.By above-mentioned conjunction
At MXene be distributed in a certain amount of deionized water, while being passed through inert gas, carry out ultrasonic mechanical stripping 1h.Note
During being intended to entire ultrasound, temperature is no more than 25 DEG C.MXene solution after ultrasound stripping centrifuges 1h at 3500rpm,
The supernatant of collection is MXene nanometer sheet colloidal solution.In our current research, required MXene nanometer sheets colloidal solution
A concentration of 2-8mg/ml, concentration can be with ultrasonic time (30-60min), centrifugation time (30-60min) and rotating speed (3500-
4500rpm) it is incremented by and increases.
MXene has good hydrophily, metallic conductivity, however it is easy to the characteristic of oxidation and hinders it in many fields
Application.And graphene synthetic technology is ripe, commercial application will also be realized, the GO synthesized with Hummer solwution methods is
Micron-scale, as shown in Fig. 2 (b).The MXene synthesized with solwution method is typically all nano-scale, as shown in Fig. 2 (a).MXene
Opposite graphene has smaller size, on the one hand can self stacking to avoid graphene during forming aeroge；
On the other hand, it can be embedded in graphene aerogel, stop the combination of itself and air to prevent the oxidation of MXene.
It is still uniform solution as shown in figure 3, after the mixing of MXene and GO colloidal solution, is not in reunite.Fig. 4 exhibitions
MX/rGO composite aerogels SEM figures are shown, it can be seen that composite aerogel possesses porous structure, aperture is from microcosmic to mesoporous
Distribution.And with the increase of MXene contents in aeroge, three-dimensional structure is more and more closely knit, and classification phenomenon is more and more obvious.
For the mechanical performance of pure graphene and MX/rGO composite aerogels, the mechanical strength of composite aerogel bigger is found, favorably
With the stability for improving entire sensor.Fig. 5 (a) illustrates pure graphene and MX/rGO composite aerogels (GO:MX=10:1)
Press force-strain curve, it is evident that MX/rGO composite aerogel mechanical performances are dilute better than pure graphite.Piezoresistive pressure sensor
The mathematic(al) representation of sensitivity is：In Fig. 5 (b), MX/rGO composite aerogels (GO:MX=10:1) one
When the response of Series Pressure, it is demonstrated by higher sensitivity, to confirm that MX/rGO composite aerogels have better electroresponse
Signal, as shown in Fig. 5 (b).
Used raw material MXene in the present invention is preferably Ti3C2Lamella, size be 500-800nm (such as
584.5nm)；Graphene oxide GO nanometer sheets are preferably to be prepared using Hummer methods, size be 1-5 μm (such as
1276.1nm)。
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all within the spirits and principles of the present invention made by all any modification, equivalent and improvement etc., should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of high sensitive sensor based on MXene/rGO complex three-dimensional structures, which is characterized in that the sensing of the sensor is lived
Property component includes MXene/rGO complex three-dimensional structures；In the MXene/rGO complex three-dimensional structures, MXene is dispersed in reduction-oxidation
In graphene rGO.
2. the high sensitive sensor as described in claim 1 based on MXene/rGO complex three-dimensional structures, which is characterized in that described
MXene/rGO complex three-dimensional structures are MXene/rGO composite aerogels；Preferably through to graphene oxide (GO) nanometer sheet glue
MXene solution is added in liquid solution, after mixing, then the mixed solution is subjected to vacuum freeze-drying and annealing and is prepared
's.
3. the high sensitive sensor as claimed in claim 2 based on MXene/rGO complex three-dimensional structures, which is characterized in that described
Dispersate MXene in MXene solution is obtained by hydrochloric acid with lithium fluoride selective etch presoma MAX phases；It is described
In presoma MAX phases, M is magnesium-yttrium-transition metal, and A is mainly III race's element or IV race's element, and X is C element or N element；Described point
It is preferably Ti to dissipate matter MXene3C2Lamella, size 500-800nm.
4. the high sensitive sensor as claimed in claim 2 based on MXene/rGO complex three-dimensional structures, which is characterized in that described
Graphene oxide (GO) nanometer sheet is prepared using Hummer methods, and the size of the stannic oxide/graphene nano piece is 1-5 μ
m。
5. the high sensitive sensor as described in claim 1 based on MXene/rGO complex three-dimensional structures, which is characterized in that described
The corresponding resistance value of sensing active component can generate variation when the pressure condition residing for sensor changes；Preferably,
Under the effect of external force, the aperture of the MXene/rGO complex three-dimensional structures, Kong Yukong distances can change.
6. the high sensitive sensor as described in claim 1 based on MXene/rGO complex three-dimensional structures, which is characterized in that described
High sensitive sensor based on MXene/rGO complex three-dimensional structures is flexible sensor, further includes the interdigital electricity of flexible polyimide
Pole；Preferably, which is prepared using following steps：It will be led on the good electrode magnetron sputtering of inkjet printing
Then electric metal is cleaned by ultrasonic and gets rid of because ink has the metal with substrate poor contact, form flexible interdigital electrode, connect
It, MXene/rGO composite aerogels is fixed in the interdigital electrode, finally encapsulated and fixed with polyethylene film, and copper wire draws electricity
Pole, to obtain flexible sensor.
7. a kind of MXene/rGO complex three-dimensionals material, which is characterized in that the MXene/rGO complex three-dimensional materials are by MXene points
It is dispersed in and obtains in redox graphene rGO.
8. MXene/rGO complex three-dimensionals material as claimed in claim 7, which is characterized in that the MXene/rGO complex three-dimensionals material
In material, the mass ratio of both the MXene and described redox graphene rGO are 20:1-5:1.
9. the preparation method of MXene/rGO complex three-dimensionals material as described in claim 7 or 8, which is characterized in that this method is logical
Addition MXene solution is crossed into graphene oxide (GO) nanometer sheet colloidal solution, after mixing, then the mixed solution is carried out
What vacuum freeze-drying and annealing were prepared；
Preferably, the treatment temperature of the vacuum freeze-drying is (- 70)~(- 20) DEG C, and the treatment temperature of the annealing is 100
~450 DEG C.
10. application of the MXene/rGO complex three-dimensionals material in preparing sensor as described in claim 7 or 8；Preferably, institute
It is pressure sensor, more preferably piezoresistive pressure sensor to state sensor.
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