CN107488267A - High resistive redox grapheme material being modified based on bead and preparation method thereof - Google Patents
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Abstract
The invention belongs to pliable pressure sensor field, there is provided a kind of high resistive redox grapheme material being modified based on bead and preparation method thereof；The material is formed by graphene oxide doped polyethylene nanometer bead, wherein, the size of the polyethylene nanometer bead is diameter 90nm~2000nm, and doping concentration is：Mass ratio, 1.56~12.5%.Polyethylene nanometer bead (PS beads) is doped into RGO films by the present invention, polyethylene nanometer bead introduces as insulator, so as to change the structure of RGO fragments stacking, under equal strained condition, the resistance variations of RGO after doping will become big, show good resistive characteristic；The sensor formed based on RGO films of the present invention also just possesses higher sensitivity (7~250), is far longer than conventional RGO sensors；The size of PS beads can also be adulterated by adjusting simultaneously and concentration realizes the regulation of strain detecting scope.
Description
Technical field
The invention belongs to pliable pressure sensor field, is related to the redox graphene material for pliable pressure sensor
Material, specially a kind of high resistive redox grapheme material being modified based on bead and preparation method thereof.
Background technology
With the development of information-intensive society, people are constantly lifted to the sampling depth of surrounding enviroment information with range, flexibility pressure
Force snesor obtains more and more extensive application, to the demand more and more higher of flexible material.Graphene, because its special nothing is hanged
Bond structure is hung, allows two-dimensional layer material to possess excellent power, Young's modulus is up to 1TPa, while its fracture strength also reaches
150GP a, it is a kind of good sensitive material.Redox graphene (abbreviation RGO) is a kind of for making piezoresistance sensor
Carbon-based material, it nontoxic, easily make, it is easy to operate the features such as cause it to can be very good to apply the particular portion in human body
Position.There are two kinds of mechanism of resistance change generally, for the strain transducer based on RGO.First, research shows necessarily to strain bar
The electrical and optical properties of graphene under part can change, and reason is that the lattice symmetry between two carbon atoms can quilt
Stress rupture, so that the band gap of graphene is opened, so that the resistance increase of graphene passage；Pass through calculating
The offset of the dirac point of graphene and the decrement of Fermi velocity understand answering for such graphene strain transducer
Become detection limit to be only capable of reaching 6%；It follows that the strain transducer for being based purely on RGO is not suitable for needing to small strain
Very sensitive wearable medical treatment ＆ health monitoring direction.Second, RGO fragments, which are stacked, can form a conductive network,
Connection between fragment can produce in the case of strain to be partially separated, so as to cause resistive；Importantly, this process can
To be reverse, when straining disappearance, resistance value can return to original value；Jieshan Qiu et al. will be prepared
RGO with yarn fabric is mixed in together is embedded into PDMS (flexible substrates), obtained film there is good ductility so that
Good tensile property must be had based on the sensor that this material prepares；Conduction in the conductive network formed due to RGO
Passage connectivity is fine, and prepared sensor out may be only available for very big strained condition and can not identify human body skin table
More complicated faint strain signal caused by face.
As can be seen here, the sensitivity of existing GRO strain transducers and detection range need further to be improved, and its core exists
In the modification of redox graphene material.
The content of the invention
It is an object of the invention to provide a kind of high resistive redox grapheme material being modified based on bead and its system
Preparation Method, for further improving the sensitivity of GRO strain transducers, effectively adjusting the detection range of GRO strain transducers；For
The purpose is realized, the technical solution adopted by the present invention is：
A kind of high resistive redox grapheme material being modified based on bead, it is characterised in that the material is by aoxidizing
Graphene doping polyethylene nanometer bead is formed, wherein, the size of the polyethylene nanometer bead is diameter 90nm~2000nm,
Doping concentration is：Mass ratio, 1.56~12.5%.
The preparation method of the above-mentioned high resistive redox grapheme material being modified based on bead, it is characterised in that including
Following steps：First, graphene oxide is ground to graphene oxide powder, poured into deionized water, obtain graphene oxide
The aqueous solution；Then, polyethylene nanometer bead solution is poured into graphene oxide water solution, magnetic agitation 30~40 minutes, obtained
The mixed dispersion liquid of graphene oxide doped polyethylene nanometer bead, it must can be changed with laser reduction based on bead after spin-coating film
The high resistive redox grapheme material of property.
The present invention operation principle be：Polyethylene nanometer bead (PS beads) is doped into RGO films, polyethylene by the present invention
Nanometer bead introduces as insulator, so as to change the structure of RGO fragments stacking, under equal strained condition, after doping
RGO resistance variations will become big；It is broken that PS nanometers bead (the being less than or equal to 400nm) doping of small size is mixed in the R GO being connected
The overlay region of piece, and large-sized PS nanometers bead (being more than 400nm) is then to be scattered in conductive interlayer, the doping of two types
Change RGO films structure so that RGO films under same strained condition, compared to undoped with R GO, fragment formed
Conductive channel is easier to be deteriorated, so as to show good resistive characteristic；Based on the modified RGO films of PS pill dopings
The sensor of formation also just possesses higher sensitivity (7~250), is far longer than conventional RGO sensors；Meanwhile pass through doping
The purpose that can also reach regulation and control strain induction range of PS nanometer beads, so that modified based on PS pill dopings
The sensor that RGO films are formed is applied to the strain monitoring of the privileged site of human body.
To sum up, the beneficial effects of the present invention are：
A kind of high resistive redox grapheme material being modified based on bead and preparation method thereof is provided, based on the oxidation
The coefficient of strain of strain transducer is 7~250 obtained by reduced graphene material is prepared, i.e. sensitivity is higher；Simultaneously can also
The enough size that PS beads are adulterated by adjusting and concentration realize the regulation of strain detecting scope.
Brief description of the drawings
Fig. 1 is the structural diagrams for the high resistive redox grapheme material being modified in the embodiment of the present invention 1 based on bead
It is intended to, wherein, (a) figure is schematic diagram, and (b) figure is measured drawing
Fig. 2 is that the SEM for the high resistive redox grapheme material being modified in the embodiment of the present invention 1 based on bead observes shape
Looks and resistive characteristic test curve.
Fig. 3 is that the SEM for the high resistive redox grapheme material being modified in the embodiment of the present invention 2 based on bead observes shape
Looks and resistive characteristic test curve.
Embodiment
The present invention is described in further details with reference to the accompanying drawings and examples.
Embodiment 1
The present embodiment provides the high resistive redox grapheme material being modified based on bead；Redox in the present embodiment
Grapheme material is shaped as by graphene oxide doped polyethylene nanometer pellet shapes, wherein, the size of polyethylene nanometer bead is
90nm or 2 50nm；Below by taking 90nm as an example, its specific preparation technology is as follows：
(1) preparation of mixed dispersion liquid
High-purity few layer graphene oxide 20mg prepared by the freeze-drying of Hummer methods is taken, grinding obtains graphite oxide in 5 minutes
Alkene powder, thickness 0.6-1nm, lamella size are 0.5-5um；Then, 9.9ml deionized water is taken to pour into plastic test tube,
Pour into graphene oxide powder, then with liquid-transfering gun take 100 μ l PS nanometer beads solution (insulating nano bead used is diameter
For 90nm, 2.5%w/v the polyethylene nanometer bead aqueous solution) add in test tube；Finally, a magnetic is put into mixed liquor to turn
Son, magnetic stirrer rotating speed are no more than 2000 revolutions per seconds, while use Ultrasound Instrument, and ultrasonic 37 points after 30 seconds, obtain nanometer bead and oxygen
The equally distributed mixed liquor of graphite alkene fragment；In mixed liquor, the volume ratio of graphene and bead is 100:1, graphene oxide
The percentage of dispersion liquid is 2mg/ml；The graphene oxide dispersion (2mg/ml) of corresponding proportion is added on the basis of mixed liquor
With mass ratio be respectively 1.56%, 2.50%, 6.25% mixed dispersion liquid；
(2) preparation of substrate and mixed liquor film forming
Epoxy resin structural adhesive (PDMS A glue) and acrylate structural adhesive (PDMS B glue) are pressed into volume fraction 10:1 enters
Row mixing, using agitator uniform stirring 5 minutes, until the mixed liquor of A glue and B glue is changed into diluting from sticky；
The polymer culture dish cleaned up is positioned on 60~80 DEG C of thermals source, after preheating, A glue B glue mixed liquors fallen
Enter in culture dish, by culture dish as on glue spreader, selected 30 seconds under 3000r/min revolutions, as on 50-60 DEG C of thermal source, 5
Hour can film forming；
PDMS films are torn from culture dish, are attached on CD, CD is put in vacuum chamber, filter 20min, are eliminated
Caused bubble during attaching；
On the PDMS film on dispersant liquid drop to optical disc surface that will be prepared into step (1), spin coating, air-dry at room temperature；
It can obtain graphene oxide/polyethylene nanometer glomerular membrane of uniform thickness；
(3) light carving redox graphene
The above-mentioned CD being prepared into is placed on light carving CD writer, selects respective graphical printing, duplicate printing is three times
Obtain the redox graphene/nanometer bead film for possessing complete pattern；
(4) test of test sample
Plastic plate common on the market is taken, is cut into 3cm × 1cm sizes；Then attached after the film on CD is torn
On plastic plate, the tensile properties and resistive effect of different nanometer bead sizes and different doping ratios are tested using displacement meter
Should；For its result as shown in figure 1, wherein, (a) figure is schematic diagram, (b) figure is measured drawing；
Adulterate the RGO films Steps of a diameter of 250nm PS beads as above (1), (2), (3), (4)；By in step (1)
90nm be changed to 250nm, other are constant, be made mixed with a diameter of 250nm PS beads RGO film samples；Test respectively not
Bead is adulterated, mixed with 90nmPS beads, mixed with resistive characteristic of the RGO films under certain strained condition of 250nmPS beads, is used
SEM observation patterns compare, as shown in Figure 2；(a) it is the film table with the SEM PS beads mixed with 90n m observed shown in
Face；(b) it is the film sections of the PS beads mixed with 90nm observed with SEM figures in；(c) it is the PS beads of doping small size
Resistance model for prediction afterwards；(d)~(f) is mixed with the film of the nanometer bead of various concentrations (6.25%, 2.50%, 1.56%)
Fragment stack schematic diagram；(g)~(i) represent respectively various concentrations (6.25%, 2.50%, 1.5 6%) under mixed with bead and
The resistive characteristic of the RGO films of bead is not mixed；As can be seen from the figure mixed with PS nanometer beads R GO films than undoped with
The resistive characteristic of RGO films will get well, and as the increase of concentration of small ball, resistive characteristic also significantly improve.
It is 6.25% in doping concentration, range of strain is for the RGO films for the nanometer bead for being doped with a diameter of 90nm
When 0% to 1.05%, the variable quantity of resistance increases 250% from 0%, and resistance change is contrasted with the RGO undoped with bead
It can only achieve 7%；Doping concentration is reduced to 2.50%, resistance change can only achieve 74%, but the linearity is fine；Continue to drop
Low doping concentration is to 1.56%, and under the conditions of maximum strain, resistance change can only achieve 15%, only small undoped with nanometer
Twice of the RGO films of ball.Similar measures, and is doped with the RGO of a diameter of 250nm nanometer bead, in doping concentration point
Not Wei 6.25%, 2.50%, under conditions of 1.56%, measure corresponding resistance change rate as 193%, 113% and 34%.These
Test result is indicated, and the PS nanometers bead of the doping small size of high concentration can be improved significantly based on R into RGO films
The sensitivity of the sensor of GO films, the concentration of bead is adulterated by changing can adjust the GF value scopes of prepared sensor
For 7~250.
Embodiment 2
Processing step is with step (1), (2), (3), (4) in embodiment 1 in the present embodiment, by the PS beads in step (1)
Change a diameter of 750nm, 1000nm, 2000nm PS nanometer beads into respectively, doping concentration is respectively 1.56%, 2.50%,
12.5%, by adulterate RGO films and undoped with RGO test resistive characteristic, its result is as shown in Figure 3；(a), (b) is respectively and mixed
The surface of RGO films of miscellaneous 1000nmPS nanometer beads and the SEM image in section；(c) figure is to be doped with large scale bead
The Resistance model for prediction of RGO Thin film conductives；(d)~(f) is respectively the stacking model of bead and RGO fragments under various concentrations；(g)~
(i) represent respectively under different doping concentration (being from left to right 12.5%, 2.50%, 1.56% respectively), it is various sizes of small
The resistive characteristic of ball and the RGO films undoped with bead.
From figure 3, it can be seen that different from the ball of small size, large-sized bead can be with separating piled fragment, broken
Piece interlayer forms conductive channel；When doping concentration very big (12.5%), the spacing between adjacent nanometer bead is too small, causes
Narrow passage is formd between nanometer bead, so as to which only a small amount of interlayer fragment conductive channel is formed, causes straining
Under the conditions of resistance change less (such as Fig. 3 (f))；When concentration is reduced to 2.5%, the spacing increase between nanometer bead, such as Fig. 3
(d) so that resistance change increase (170%), i.e. resistive characteristic improve under certain strained condition；Continue to reduce doping concentration
To 1. 56%, separate too remote between nanometer bead, RGO is stacked, so that only a small amount of interlayer conductive channel shape
Into under certain strained condition, resistance change is similar with highly doped situation, and such as Fig. 3 (h), resistance change about exists
50%.
When the size (400nm) of PS nanometer beads and the size of RGO fragments can compare, the addition of PS nanometer beads
The stacking situation in RGO is set to change to form complex pattern, it is very sensitive to the doping concentration of bead；Total comes
Say, for as above three kinds various sizes of PS beads, the GF values of prepared sensor are not as mixing small size nanometer bead
RG O sensors equally possess it is preferably linear, when bead size is 1000nm, doping concentration is 2.5%, strain transducer
The GF values for having maximum are 170.
The foregoing is only a specific embodiment of the invention, any feature disclosed in this specification, except non-specifically
Narration, can alternative features equivalent by other or with similar purpose replaced；Disclosed all features or all sides
Method or during the step of, in addition to mutually exclusive feature and/or step, can be combined in any way.
Claims (2)
1. the high resistive redox grapheme material being modified based on bead, it is characterised in that the material is by graphene oxide
Doping polyethylene nanometer bead is formed, wherein, the size of the polyethylene nanometer bead is diameter 90nm~2000nm, and doping is dense
Spend and be：Mass ratio, 1.56~12.5%.
2. the preparation method for the high resistive redox grapheme material being modified as described in claim 1 based on bead, its feature
It is, comprises the following steps：First, graphene oxide is ground to graphene oxide powder, poured into deionized water, obtain oxygen
Graphite aqueous solution；Then, polyethylene nanometer bead solution is poured into graphene oxide water solution, magnetic agitation 30~40
Minute, obtain the mixed dispersion liquid of graphene oxide doped polyethylene nanometer bead, base can be obtained with laser reduction after spin-coating film
In the high resistive redox grapheme material that bead is modified.
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| CN108548619A (en) * | 2018-03-30 | 2018-09-18 | 华中科技大学 | The method for promoting piezoresistive transducer sensitivity based on fragmentation structure |
| CN109827681A (en) * | 2019-02-19 | 2019-05-31 | 东南大学 | A kind of flexible strain transducer and preparation method thereof containing enlarged structure |
| CN110186599A (en) * | 2019-05-16 | 2019-08-30 | 电子科技大学 | A kind of preparation method of superlinearity resistive redox graphene strain gauge |
| CN112262188A (en) * | 2018-06-15 | 2021-01-22 | 安赛乐米塔尔公司 | Coated metal substrate |
| CN113834418A (en) * | 2021-09-06 | 2021-12-24 | 电子科技大学 | Flexible strain sensor with adjustable Poisson ratio |
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| CN112262188A (en) * | 2018-06-15 | 2021-01-22 | 安赛乐米塔尔公司 | Coated metal substrate |
| CN109827681A (en) * | 2019-02-19 | 2019-05-31 | 东南大学 | A kind of flexible strain transducer and preparation method thereof containing enlarged structure |
| CN110186599A (en) * | 2019-05-16 | 2019-08-30 | 电子科技大学 | A kind of preparation method of superlinearity resistive redox graphene strain gauge |
| CN113834418A (en) * | 2021-09-06 | 2021-12-24 | 电子科技大学 | Flexible strain sensor with adjustable Poisson ratio |
| CN113834418B (en) * | 2021-09-06 | 2023-04-18 | 电子科技大学 | Flexible strain sensor with adjustable Poisson ratio |
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