CN105583408A - Preparation method and application of Cu nanowire-reduced graphene oxide three-dimensional porous film - Google Patents
Preparation method and application of Cu nanowire-reduced graphene oxide three-dimensional porous film Download PDFInfo
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- CN105583408A CN105583408A CN201510976766.8A CN201510976766A CN105583408A CN 105583408 A CN105583408 A CN 105583408A CN 201510976766 A CN201510976766 A CN 201510976766A CN 105583408 A CN105583408 A CN 105583408A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
- G01B7/18—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge using change in resistance
Abstract
The invention provides a preparation method of a Cu nanowire-reduced graphene oxide-PDMS composite strain sensor, and belongs to the field of reduced graphene oxide composite sensors. The preparation method comprises the steps that copper nanowires are added into graphene oxide containing ascorbic acid, Cu nanowire-reduced graphene oxide hydrogel is obtained after reducing, and a Cu nanowire-reduced graphene oxide film with the three-dimensional porous appearance is obtained through washing, stir-breaking and suction filtration film formation; and then liquid PDMS is poured, vacuum filtration is carried out to remove bubbles, the liquid PDMS is subjected to cross-linking and curing at the temperature of 70 DEG C, and finally the Cu nanowire-reduced graphene oxide-PDMS composite strain sensor is obtained. The composite film is large in specific surface area and excellent in electric conductivity and mechanical performance, and the preparation method of a Cu nanowire-reduced graphene oxide-PDMS composite is mild in condition, simple, practical, controllable in process parameter, low in cost and high in repeatability.
Description
Technical field
The invention belongs to redox graphene composite sensor field, relate in particular to a kind of Cu of use and receiveRice noodles, redox graphene and PDMS composite material and preparation method thereof, and prepare strain transducer with itMethod. Belong to technical field prepared by advanced graphene composite material sensor.
Background technology
Cu finds at first as the mankind and one of the metallic element that utilizes, and nature reserves are large, cheap,Its price is about 1/10th of one of golden percentage, silver. Cu nano wire is as monodimension nanometer material, not onlyRetain the general character of other nano material, also there is larger draw ratio and specific area, good conduction, urgeChange and mechanical performance. Therefore, Cu nano wire is widely used in electronic circuit, chemical catalysis and compliant conductive deviceThe fields such as part.
Graphene be a kind of by carbon atom with SP2Hybridized orbit composition hexagon is the two-dimension single layer of honeycomb latticeLaminated structure, has light transmittance is high, carrier mobility is high, good chemical stability and remarkable machine thereofThe advantages such as tool performance. Therefore, Graphene is widely used in the fields such as battery, ultracapacitor and catalyst carrierAnd also can be used as chemistry, biology sensor, for wearable device. But Graphene generally by loaded down with trivial details,Complicated and expensive chemical vapour deposition technique preparation, is unfavorable for large-scale promotion application. So, major partResearcher adopts simply, oxidation-reduction method is prepared the alternative Graphene of redox graphene efficiently, is protectingDemonstrate,prove on the basis of its fundamental characteristics, reduce production costs and technical difficulty.
PDMS is owing to having fabulous elasticity and biocompatibility, extensively as the flexibility of flexible electronic deviceLining body. In addition, PDMS also possesses high light transmittance, high sensitivity, and the advantage such as extremely short relaxation time,Set it as the flexible liner body of Graphene or redox graphene, make strain transducer or chemistry biographySensor, the premium properties that not only can give full play to Graphene and redox graphene can also improve devicePliability, makes the more realistic application of sensor.
In recent years, flexible wearable capacitor type and resistor-type strain transducer are subject to researcher's extensive concern.As carbon nano-tube film/PDMS microarray capacitor type strain transducer, three-dimensional grapheme/PDMS resistor-type are answeredBecome sensor and nano silver wire/PDMS resistor-type strain transducer etc. But capacitor type strain transducer can not holdBe subject to larger strain, the sensitivity of resistor-type strain transducer is lower and strain detecting scope is narrower, restricts that it is extensiveBe applied to wearable device. And we make full use of Cu nano wire, three-dimensional redox graphene and PDMSAdvantage, preparation Cu nano wire-redox graphene-PDMS composite is also applied to resistor-typeStrain transducer, has the advantages such as highly sensitive and strain detecting scope is wide. In addition this materials and devices system,Preparation Method mild condition, simple, technological parameter is controlled, with low cost, repeatable high. Therefore,This Cu nano wire-redox graphene-PDMS composite strain transducer has as wearable deviceHuge application prospect.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of Cu nano wire-oxygen reduction fossil is providedPreparation method and the application of the three-dimensional porous film of China ink alkene.
The object of the invention is to be achieved through the following technical solutions: a kind of Cu nano wire-reduction-oxidation graphiteThe preparation method of the three-dimensional porous film of alkene, step is as follows:
(1) in ethylene glycol, add Cu nano wire, ascorbic acid and graphene oxide, make Cu nano wireConcentration be 0.1mg/mL-0.4mg/mL, the concentration of ascorbic acid is 2.0mg/mL, graphene oxideConcentration is 1.0mg/mL; After mixing, move in hydrothermal reaction kettle, be placed on 120 DEG C of air dry ovensMiddle reaction 4h, then be cooled to room temperature, obtain Cu nano wire-redox graphene composite aquogel;
(2) Cu nano wire-redox graphene composite aquogel step 1 being prepared is placed in 0.5The 16h that dialyses in wt% hydrazine hydrate solution, then take out and pour deionized water for stirring into and be uniformly dispersed, obtain suspension,With core filter suction filtration dry, obtain the three-dimensional porous film of Cu nano wire-redox graphene again.
Further, in step 1, the mass ratio of graphene oxide and ascorbic acid is 1:2.
An application for the three-dimensional porous film of Cu nano wire-redox graphene, this is applied as: Cu is receivedThe three-dimensional porous film of rice noodles-redox graphene is for the preparation of strain transducer.
Further, this application is specially: Cu nano wire-oxidation graphene film is cut into 2cm × 0.5Cm's is rectangular, and two ends are connected as electrode with copper cash by elargol respectively, and reusable liquid PDMS enters filmRow cast, vacuum filtration bubble removing, and be placed in 70 DEG C of air dry oven 2h, make its crosslinking curing,To strain transducer.
The present invention has the following advantages: adding of Cu nano wire has more three-dimensional porous redox grapheneLarge specific area, more excellent electric conductivity and mechanical performance; Using PDMS as flexible liner body, make it respectivelyPlant distortion performance and keep stable. This Cu nano wire-redox graphene-PDMS composite preparation sideMethod mild condition, simple, technological parameter is controlled, with low cost, repeatable high. This Cu nano wire-redox graphene-PDMS composite strain transducer has highly sensitive and strain detecting scope is wideEtc. advantage, and can be used for wearable device.
Brief description of the drawings
Fig. 1 is that the three-dimensional porous film of redox graphene and Cu nano wire-redox graphene are three-dimensional porousFilm schematic diagram;
Fig. 2 is the XRD figure that the present invention prepares the three-dimensional porous film of a kind of Cu nano wire-redox graphene;
Fig. 3 is the SEM figure that the present invention prepares the three-dimensional porous film of a kind of Cu nano wire-redox graphene;
Fig. 4 is that the present invention prepares a kind of Cu nano wire-redox graphene-PDMS composite sensorBending schematic diagram.
Fig. 5 is that the present invention prepares a kind of Cu nano wire-redox graphene-PDMS composite sensorSurvey and bend elbow motion schematic diagram.
Fig. 6 is that the present invention prepares a kind of Cu nano wire-redox graphene-PDMS composite sensorSurvey pulse vibration schematic diagram.
Detailed description of the invention
The invention provides a kind of Cu nano wire-redox graphene-PDMS composite strain transducerPreparation method, comprises following content:
The preparation method of graphene oxide is: in ice-water bath slowly by the 270mL concentrated sulfuric acid/phosphoric acid mixing acid(H2SO4：H3PO3=9:1, V/V) drop to and be equipped with in 2g natural graphite powder beaker and keep stirring, withSlowly add afterwards 12g potassium permanganate, after mixing, beaker is transferred in 50 DEG C of water-baths and reacts 12h.After completion of the reaction, 300mL frozen water is added in beaker, be cooled to after room temperature, then it is two to drip 5mL30%Oxygen water, obtains glassy yellow product. Finally product is used respectively to hydrochloric acid, deionized water centrifuge washing, until pH=6,Rotating speed is 8000rpm/min, and last freeze drying obtains graphene oxide.
The preparation method of copper nano-wire is: preparation method is disclosed on Langmuir according to people such as Y.Chang(the Y.Chang that method is carried out; M.L.Lye; H.C.Zeng; Large-ScaleSynthesisofHigh-QualityUltralongCopperNanowires.Langmuir, 2005,21,3746-3748.). Be specially: configuration 15MNaOH solution, get that 20mL is added in single port flask and heating water bath to 60 DEG C, drip 1mL0.1MCu(NO3)2To in NaOH solution and vigorous stirring, then add successively 0.17mL anhydrous ethylenediamine, 29uLMass fraction is 35% N2H4The aqueous solution, stirs after 45s, leaves standstill reaction 90min. After completion of the reaction,Flask is placed in ice-water bath, is cooled to after 10 DEG C, the product of one deck rufous that suspends above solution,Sop up solution with dropper, retain the rufous product on upper strata, last water and alcohol mixed solution centrifuge washingRufous product, centrifugal rotational speed 6000rpm/min, centrifugation time 10min, repeated washing 5 times, vacuumAfter dry, obtain Cu nano wire powder.
Embodiment 1
Get a 50mL beaker, amount 22mL ethylene glycol solution, pours 5mg rufous Cu nano wire into,Stirring, ultrasonic, repeated multiple times, obtains red tan solution, adds 50mg ascorbic acid and 3.1mL8mg/mLGraphene oxide, then stir, ultrasonic, until graphene oxide is uniformly dispersed, then moved to waterIn thermal response still, reactor is placed in to 120 DEG C of air dry ovens and reacts 4h, finally cool the temperature to room temperature,Just obtain Cu nano wire-redox graphene composite aquogel.
Cu nano wire-redox graphene composite aquogel in hydrothermal reaction kettle is rinsed by deionized water4-5 time, then be poured in 100mL beaker and rinse 3-4 time, object is remove this gel surface organicSolvent. Then be placed on the 16h that dialyses in 500mL0.5wt% hydrazine hydrate solution, object is to remove that this is solidifyingOrganic solvent in glue. Finally be poured into again in 150mL beaker, rinse 3 times after by deionized water by itBreak up, be put on magnetic stirring apparatus and stir, and ultrasonic, until obtain short grained, particle diameter is uniformBlack suspension, carries out suction filtration with core filter, obtains Cu nano wire-oxidation graphene film,Carry out freeze drying processing.
Embodiment 2
Get a 50mL beaker, amount 22mL ethylene glycol solution, falls 10mg rufous Cu nano wireEnter, stirring, ultrasonic, repeated multiple times, obtains red tan solution, adds 50mg ascorbic acid and 3.1mL8Mg/mL graphene oxide, then stir, ultrasonic, until graphene oxide is uniformly dispersed, then by itMove in hydrothermal reaction kettle, reactor is placed in to 120 DEG C of air dry ovens and reacts 4h, finally temperature is fallenTo room temperature, just obtain Cu nano wire-redox graphene composite aquogel.
Cu nano wire-redox graphene composite aquogel in hydrothermal reaction kettle is rinsed by deionized water4-5 time, then be poured in 100mL beaker and rinse 3-4 time. Then be placed on 500mL0.5wt%The 16h that dialyses in hydrazine hydrate solution, is finally poured in 150mL beaker again, uses deionization after rinsing 3 timesWater is broken up, and be put on magnetic stirring apparatus and stir, and ultrasonic, until obtain short grained, particle diameterUniformly black suspension, carries out suction filtration with core filter, obtains Cu nano wire-reduction-oxidation graphiteAlkene film, carries out freeze drying processing.
Embodiment 3
Get a 50mL beaker, amount 22mL ethylene glycol solution, falls 2.5mg rufous Cu nano wireEnter, stirring, ultrasonic, repeated multiple times, obtains red tan solution, adds 50mg ascorbic acid and 3.1mL8Mg/mL graphene oxide, then stir, ultrasonic, until graphene oxide is uniformly dispersed, then by itMove in hydrothermal reaction kettle, reactor is placed in to 120 DEG C of air dry ovens and reacts 4h, finally temperature is fallenTo room temperature, just obtain Cu nano wire-redox graphene composite aquogel.
Cu nano wire-redox graphene composite aquogel in hydrothermal reaction kettle is rinsed by deionized water4-5 time, then be poured in 100mL beaker and rinse 3-4 time. Then be placed on 500mL0.5wt%The 16h that dialyses in hydrazine hydrate solution, is finally poured in 150mL beaker again, uses deionization after rinsing 3 timesWater is broken up, and be put on magnetic stirring apparatus and stir, and ultrasonic, until obtain short grained, particle diameterUniformly black suspension, carries out suction filtration with core filter, obtains Cu nano wire-reduction-oxidation graphiteAlkene film, carries out freeze drying processing.
Embodiment 4
Get a 50mL beaker, amount 22mL ethylene glycol solution, by 3.1mL8mg/mL graphene oxideAdd in beaker with 50mg ascorbic acid, then stir, ultrasonic, repeated multiple times, until graphite oxideAlkene is uniformly dispersed, and is then moved in hydrothermal reaction kettle, and reactor is placed in to 120 DEG C of air dry ovensReaction 4h, finally cools the temperature to room temperature, just obtains redox graphene hydrogel.
Redox graphene hydrogel in hydrothermal reaction kettle is rinsed 4-5 time by deionized water, then fallenEnter in 100mL beaker and rinse 3-4 time. Then be placed in 500mL0.5wt% hydrazine hydrate solution and dialyse16h, is finally poured in 150mL beaker again, is broken up after rinsing 3 times by deionized water, is put intoOn magnetic stirring apparatus, stir, and ultrasonic, until obtain short grained, the uniform black suspension of particle diameter,Carry out suction filtration with core filter, obtain oxidation graphene film, carry out freeze drying processing.
Show through lot of experiments research: when (1) does not add Cu nano wire, the redox graphene that suction filtration goes out is thinThere are a large amount of crackles (as Fig. 1) on film surface; While adding the amount of Cu nano wire to exceed 0.4mg/mL, although strainThe electric conductivity of sensor improves, but Cu nano wire can reunite in composite aquogel, skewness,Cause mechanical performance and the sensitivity of strain transducer. (2) quality of graphene oxide and ascorbic acidThan being less than at 0.5 o'clock, in hydro-thermal reaction, be difficult to form Cu nano wire-redox graphene composite aquogel;And the mass ratio of graphene oxide and ascorbic acid is greater than at 0.5 o'clock, the reduction of graphene oxide in hydro-thermal reactionDegree is too high, between redox graphene sheet and sheet pi-pi bond effect violent, Cu nano wire-reduction-oxidationGraphene composite aquogel porosity reduces, and cause to be difficult to suction filtration and to become high-quality thin film, and film surface occursA large amount of crackles.
Accompanying drawing 1 is the three-dimensional porous film of redox graphene and Cu nano wire-redox graphene three-dimensionalPorous membrane schematic diagram. Wherein, the three-dimensional porous film surface of redox graphene has a large amount of crackles, and CuThe three-dimensional porous film surface of nano wire-redox graphene is smooth.
By in embodiment 1 through the Cu of freeze drying processing nano wire-oxidation graphene film from filter membranePeel off, cut the rectangular of a 2cm × 0.5cm, be stained with copper cash as electrode at two ends with elargol respectively, thenEmbedded in the PDMS that spin coating is good, and covered one deck PDMS on upper strata, left standstill 10min, then by itVacuumize, object is to remove bubble and make PDMS infiltrate the porous knot of Cu nano wire-redox grapheneIn structure to improve the mechanical performance of strain transducer. Cu nano wire-the redox graphene of bubble will be removed-PDMS composite is put in the air dry oven of 70 DEG C and is incubated 2h, just obtains easy strain transducer.
Accompanying drawing 2-Fig. 6 is strain transducer prepared by embodiment 1.
Fig. 2 is the XRD figure that the present invention prepares the three-dimensional porous film of a kind of Cu nano wire-redox graphene.The peak of Cu and PDF card coincide, and do not occur other assorted peaks; What 24.5 ° of peaks of locating were redox grapheneDiffraction maximum, illustrates that graphene oxide has been reduced.
Fig. 3 is the SEM figure that the present invention prepares the three-dimensional porous film of a kind of Cu nano wire-redox graphene.Due to the existence of one dimension Cu nano wire, make three-dimensional porous redox graphene there is larger specific area,More excellent conduction and mechanical performance.
Fig. 4 is that the present invention prepares a kind of Cu nano wire-redox graphene-PDMS composite sensorBending schematic diagram. Utilize this strain transducer to measure the resistance variations situation under differently curved angle.
Fig. 5 and 6 passes for the present invention prepares a kind of Cu nano wire-redox graphene-PDMS compositeSensor is measured the schematic diagram of human motion. Fig. 5 is the situation of change of resistance while bending elbow motion, and Fig. 6 is human bodyThe situation of change of pulse when vibration resistance, a pulse vibration is divided into three phases, respectively corresponding P1, P2And P3, and as can be seen from the figure P3 stage of the male sex more obvious than women's the P3 stage. This strain transducerCan be used for wearable device field human body health.
Above-mentioned example is used for the present invention that explains, but and non-limiting the present invention. In spirit of the present invention andIn the protection domain of claim, any amendment and change that the present invention is made, all fall into guarantor of the present inventionProtect scope.
Claims (4)
1. a preparation method for the three-dimensional porous film of Cu nano wire-redox graphene, is characterized in that,Step is as follows:
(1) in ethylene glycol, add Cu nano wire, ascorbic acid and graphene oxide, make Cu nano wireConcentration be 0.1mg/mL-0.4mg/mL, the concentration of ascorbic acid is 2.0mg/mL, graphene oxideConcentration is 1.0mg/mL; After mixing, move in hydrothermal reaction kettle, be placed on 120 DEG C of air dry ovensMiddle reaction 4h, then be cooled to room temperature, obtain Cu nano wire-redox graphene composite aquogel;
(2) Cu nano wire-redox graphene composite aquogel step 1 being prepared is placed in 0.5The 16h that dialyses in wt% hydrazine hydrate solution, then take out and pour deionized water for stirring into and be uniformly dispersed, obtain suspension,Finally, with core filter suction filtration dry, obtain Cu nano wire-redox graphene three-dimensional porous thinFilm.
2. preparation method according to claim 1, is characterized in that, in step 1, graphene oxide is with anti-The mass ratio of bad hematic acid is 1:2.
3. Cu nano wire-redox graphene that prepared by a method claimed in claim 1 is three-dimensional porous thinThe application of film, is characterized in that, this is applied as: by three-dimensional porous Cu nano wire-redox graphene thinFilm is for the preparation of strain transducer.
4. application according to claim 3, is characterized in that, this application is specially: by Cu nano wire-Oxidation graphene film is cut into the rectangular of 2cm × 0.5cm, and two ends are connected respectively work with copper cash by elargolFor electrode, reusable liquid PDMS pours into a mould film, vacuum filtration bubble removing, and be placed in 70 DEG C of air blast2h in drying box, makes its crosslinking curing, obtains strain transducer.
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| CN110085687A (en) * | 2019-04-26 | 2019-08-02 | 潮州市亿加光电科技有限公司 | A kind of combination electrode and its preparation method and application |
| CN110127672A (en) * | 2019-06-10 | 2019-08-16 | 中国烟草总公司郑州烟草研究院 | A kind of preparation method of redox graphene film |
| WO2021040722A1 (en) * | 2019-08-29 | 2021-03-04 | Hewlett-Packard Development Company, L.P. | Flexible printed articles |
| CN111925776A (en) * | 2020-07-11 | 2020-11-13 | 西北工业大学 | Preparation method of polypyrrole nanowire interface modified three-dimensional graphene/PDMS composite photo-thermal material |
| CN111961903A (en) * | 2020-08-19 | 2020-11-20 | 西安理工大学 | Preparation method of nanoparticle-doped graphene oxide reinforced copper-based composite material |
| CN111961903B (en) * | 2020-08-19 | 2021-11-16 | 西安理工大学 | Preparation method of nanoparticle-doped graphene oxide reinforced copper-based composite material |
| CN114427174A (en) * | 2022-02-21 | 2022-05-03 | 浙江理工大学 | Preparation method of filter paper-based flexible sensor with antibacterial function |
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