CN105032354A - Silver nanowire/graphene composite elastic aerogel, and preparation method and application thereof - Google Patents
Silver nanowire/graphene composite elastic aerogel, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a silver nanowire/graphene composite elastic aerogel, and a preparation method and application thereof. The silver nanowire and graphene composite elastic aerogel adopts a three-dimensional network structure in which silver nanowires are distributed on the surface of graphene to be used as elastic supporting and conductivity enhancement units. The preparation method for the aerogel comprises the following steps: firstly, preparing silver nanowires and an oxidized graphene dispersion solution; secondly, mixing the silver nanowires and the graphene dispersion solution with a reducing agent for reduction reaction to obtain silver nanowire and graphene hydrogel; finally, drying the obtained silver nanowire and graphene hydrogel to obtain the silver nanowire and graphene composite elastic aerogel. The silver nanowire and graphene composite elastic aerogel has the characteristics of being high in specific surface area, compression resistance and resistance adjustability, and the like, and has a high application value in the field of organic pollutant adsorption, catalysis, pressure resistance switches and the like.
Description
Technical field
The present invention relates to a kind of graphene aerogel technology of preparing, particularly relate to a kind of nano silver wire/Graphene composite elastic aeroge and its preparation method and application.
Background technology
Graphene be a kind of by carbon atom with sp
2hybridized orbit composition hexangle type is the flat film of honeycomb lattice, only has the two-dimensional material of a carbon atom thickness.Graphene has the physical properties such as good conduction, heat conduction, mechanics, (Novoselov since being prepared by scientist first from 2004, K.S.etal.Science, 2004,306,666) just receive the extensive concern of scientists, have a wide range of applications in fields such as battery, ultracapacitor, electronic devices.
Aeroge is a kind of porous foam shape solid material, has extremely light density and very high specific area.Graphene aerogel has the characteristic of Graphene and aeroge concurrently, as much higher porosity, high specific area, ultralight density and high mechanical strength, thus receive multi-field concern in recent years, have a wide range of applications in fields such as absorption, Industrial Catalysis, environmental protection, the energy.
In graphene aerogel preparation process, easily there is the stacking phenomenon of graphene film, cause material specific surface area and electrical conductivity to decline.Therefore, develop suitable preparation method, electric conductivity and its application of expansion of improving graphene aerogel are further urgent problems.Graphene is adulterated or and other materials compound be effective solution route.As the graphene aerogel (Chen of filled high polymer, ZP, etal.Naturematerials, 2011,10,424-428), graphene aerogel (a kind of Graphene-carbon nano tube composite all-carbon ultra-light elastic aerogel, the application number: 201210123313.7 of filling carbon nano-pipe; A preparation method for graphene aerogel and Graphene-CNT aeroge, application number: 201410592608.8), graphene aerogel (nitrogen-doped graphene aeroge, the application number: 201310741365.5 of N doping; Nitrogen-doped graphene hydrogel or aeroge and preparation method, application number: 201210341778.X) etc.Nano silver wire has high specific area, excellent electric conductivity, thermal conductivity and flexible preferably, and has sterilizing function, silver nanoparticle and Graphene compound will be solved the problem, and current correlative study is not also carried out.
Summary of the invention
The object of this invention is to provide and a kind of there is high-specific surface area, high-compressibility, nano silver wire/Graphene composite elastic aeroge that resistance is adjustable and its preparation method and application.
The object of the invention is to be achieved through the following technical solutions:
Nano silver wire of the present invention/Graphene composite elastic aeroge take Graphene as the three-dimensional netted cross-linked structure that skeleton is built into, and nano silver wire is distributed in graphenic surface and makes resiliency supported and conduction enhancement unit, aeroge density 0.5 ~ 300mg/cm
3, compressible 20% ~ 85%, electrical conductivity 10
-2~ 10
3s/m.
The glue preparation method of nano silver wire of the present invention/Graphene composite elastic airsetting, comprises the following steps:
(1) graphene oxide is scattered in the deionized water of Different Weight part that to form concentration be 0.1 ~ 30mg/mL graphene oxide dispersion;
(2) nano silver wire is scattered in the deionized water of Different Weight part that to form concentration be 0.05 ~ 30mg/mL nano silver wire dispersion liquid;
(3) graphene oxide dispersion is mixed with nano silver wire dispersion liquid, obtain nano silver wire-graphene oxide mixed dispersion liquid through ultrasonic disperse or stirring;
(4) nano silver wire-graphene oxide dispersion that step (3) obtains is put into reaction vessel, add reducing agent and carry out chemical reduction method reduction, obtain nano silver wire/Graphene composite aquogel;
(5) nano silver wire/Graphene composite aquogel that step (4) obtains is put into deionized water or ammoniacal liquor, soak 1 ~ 10 day, remove reaction residual impurity;
(6) nano silver wire/Graphene hydrogel that step (5) obtains is carried out freeze drying or supercritical drying, obtain nano silver wire/Graphene composite elastic aeroge.
The application of nano silver wire of the present invention/Graphene composite elastic aeroge, for absorption, catalyze and degrade organic pollutants.
The application of nano silver wire of the present invention/Graphene composite elastic aeroge, in piezoresistive switch.
As seen from the above technical solution provided by the invention, the nano silver wire that the embodiment of the present invention provides/Graphene composite elastic aeroge and its preparation method and application, because this nano silver wire/graphene aerogel is the 3 D stereo network structure that nano silver wire is distributed in that graphenic surface makes resiliency supported and conduction enhancement unit; The preparation process of aeroge comprises step: first prepare nano silver wire, graphene oxide dispersion; Then nano silver wire and graphene dispersing solution are mixed with reducing agent and carry out reduction reaction, obtain nano silver wire/Graphene hydrogel, finally the nano silver wire obtained/Graphene hydrogel is carried out drying, obtain nano silver wire/Graphene composite aerogel.The characteristics such as this nano silver wire/Graphene composite aerogel has high-specific surface area, high-compressibility, resistance is adjustable, have extensive use and are worth in fields such as Adsorption of Organic, catalysis and piezoresistive switches.
Accompanying drawing explanation
The optics picture of Fig. 1 a nano silver wire prepared by the embodiment of the present invention 1/Graphene hydrogel, the optics picture of the nano silver wire/graphene aerogel of Fig. 1 b prepared by the embodiment of the present invention 1;
The XRD collection of illustrative plates of the nano silver wire/graphene aerogel of Fig. 2 prepared by the embodiment of the present invention 2;
The low power electron scanning micrograph (× 500 times) of the nano silver wire/graphene aerogel of Fig. 3 a prepared by the embodiment of the present invention 3;
The high power electron scanning micrograph (× 20000 times) of the nano silver wire/graphene aerogel of Fig. 3 b prepared by the embodiment of the present invention 3;
The low power electron scanning micrograph (× 500 times) of the nano silver wire/graphene aerogel of Fig. 4 a prepared by the embodiment of the present invention 4;
The high power electron scanning micrograph (× 20000 times) of the nano silver wire/graphene aerogel of Fig. 4 b prepared by the embodiment of the present invention 4;
The low power electron scanning micrograph (× 500 times) of the nano silver wire/graphene aerogel of Fig. 5 a prepared by the embodiment of the present invention 5;
The high power electron scanning micrograph (× 20000 times) of the nano silver wire/graphene aerogel of Fig. 5 b prepared by the embodiment of the present invention 5;
Fig. 6 is the effect relation curve in time of the degraded methyl orange of nano silver wire/graphene aerogel prepared by the embodiment of the present invention 3;
Fig. 7 is the electrical resistance compression ratio change curve of the nano silver wire/graphene aerogel prepared by the embodiment of the present invention 4.
Detailed description of the invention
To be described in further detail the embodiment of the present invention below.
Nano silver wire of the present invention/Graphene composite elastic aeroge, its preferably detailed description of the invention be:
Take Graphene as the three-dimensional netted cross-linked structure that skeleton is built into, nano silver wire is distributed in graphenic surface and makes resiliency supported and conduction enhancement unit, aeroge density 0.5 ~ 300mg/cm
3, compressible 20% ~ 85%, electrical conductivity 10
-2~ 10
3s/m.
The glue preparation method of nano silver wire of the present invention/Graphene composite elastic airsetting, its preferably detailed description of the invention be:
Comprise the following steps:
(1) graphene oxide is scattered in the deionized water of Different Weight part that to form concentration be 0.1 ~ 30mg/mL graphene oxide dispersion;
(2) nano silver wire is scattered in the deionized water of Different Weight part that to form concentration be 0.05 ~ 30mg/mL nano silver wire dispersion liquid;
(3) graphene oxide dispersion is mixed with nano silver wire dispersion liquid, obtain graphene oxide-nano silver wire mixed dispersion liquid through ultrasonic disperse or stirring;
(4) nano silver wire-graphene oxide dispersion that step (3) obtains is put into reaction vessel, add reducing agent and carry out chemical reduction method reduction, obtain nano silver wire/Graphene composite aquogel;
(5) nano silver wire/Graphene composite aquogel that step (4) obtains is put into deionized water or ammoniacal liquor, soak 1 ~ 10 day, remove reaction residual impurity;
(6) nano silver wire/Graphene hydrogel that step (5) obtains is carried out freeze drying or supercritical drying, obtain nano silver wire/Graphene composite elastic aeroge.
The appropriate method that step (1) described graphene oxide is known in the art, as standby in Hummers legal system.
Step (2) described nano silver wire diameter 2 ~ 300nm, length 5 ~ 200 μm.
Ultrasonic power 40 ~ the 1000W of step (3) described ultrasonic disperse, supersonic frequency 20 ~ 80KHz, described stirring is magnetic agitation or mechanical agitation, and rotating speed is 40 ~ 4000 revs/min.
The reducing agent that the described chemical reduction method of step (4) adopts is one or more in sodium hydrogensulfite, ascorbic acid, sodium ascorbate, hydrazine hydrate, glucose, sodium borohydride, hydroiodic acid, ethylenediamine etc.; Recovery time is 0.5 ~ 24h, and reduction temperature is 10 ~ 150 DEG C.
Step (5) described ammonia concn is 5 ~ 28%.
The described cryodesiccated condition of step (6) comprises: cryogenic temperature is-5 ~-65 DEG C, and baking temperature is-45 ~ 10 DEG C, vacuum 10 ~ 110Pa, and drying time is 12 ~ 96h; Described supercritical drying is that supercritical carbon dioxide is dry.
The application of nano silver wire of the present invention/Graphene composite elastic aeroge, its preferably detailed description of the invention be: for absorption, catalyze and degrade organic pollutants.
The application of nano silver wire of the present invention/Graphene composite elastic aeroge, its preferably detailed description of the invention be: in piezoresistive switch.
Raw material, reagent, instrument and equipment etc. involved in the present invention by the restriction of concrete model, process conditions, operating procedure etc., can not be the products of any business or non-commercial.
Nano silver wire of the present invention/Graphene composite elastic aeroge and its preparation method and application.This nano silver wire/graphene aerogel is the 3 D stereo network structure that nano silver wire is distributed in that graphenic surface makes resiliency supported and conduction enhancement unit.Preparation process and the step of the aeroge that the present invention relates to are as follows: first prepare nano silver wire, graphene oxide dispersion; Then nano silver wire and graphene dispersing solution are mixed with reducing agent and carry out reduction reaction, obtain nano silver wire/Graphene hydrogel, finally the nano silver wire obtained/Graphene hydrogel is carried out drying, obtain nano silver wire/Graphene composite aerogel.The characteristics such as this nano silver wire/Graphene composite aerogel has high-specific surface area, high-compressibility, resistance is adjustable, have extensive use and are worth in fields such as Adsorption of Organic, catalysis and piezoresistive switches.
The present invention is with low cost, preparation is simple, be easy to produce amplification, electric conductivity is good, in conduction, catalysis, absorption, ultracapacitor, resistance switch etc., have good application prospect.
The beneficial effect that the present invention compared with prior art has:
Employing graphene oxide, nano silver wire are that nano silver wire/Graphene composite elastic aeroge prepared by raw material, and raw material is easy to get;
Preparation process is simple and convenient;
Obtained nano silver wire/Graphene composite elastic aeroge take Graphene as the three-dimensional netted cross-linked structure that skeleton is built into, and nano silver wire makes resiliency supported and conduction enhancement unit is interspersed in graphene-structured;
The obtained electric conductivity that nano silver wire/Graphene composite elastic aeroge has good elasticity, extremely low density keeps excellence simultaneously, and can by the electric conductivity regulating nano silver wire content to control aeroge.
Specific embodiment:
Embodiment 1:
A preparation method for nano silver wire/Graphene composite elastic aeroge, concrete steps are as follows:
(1) graphene oxide is scattered in deionized water to form concentration be 2.0mg/mL graphene oxide dispersion;
(2) nano silver wire is scattered in deionized water to form concentration be 1.0mg/mL nano silver wire dispersion liquid;
(3) graphene oxide dispersion is mixed with nano silver wire dispersion liquid, mechanical agitation 0.5h, obtain nano silver wire-graphene oxide mixed dispersion liquid;
(4) nano silver wire-graphene oxide mixed dispersion liquid that step (3) obtains is added sodium hydrogensulfite (sodium hydrogensulfite and graphene oxide mass ratio are 1:30), put into water-bath, 95 DEG C of reduction 8h obtain nano silver wire/Graphene hydrogel;
(5) nano silver wire/Graphene composite aquogel that step (4) obtains is put into the ammoniacal liquor that concentration is 14%, soak 3 days, remove reaction residual impurity;
(6) nano silver wire/Graphene composite aquogel step (5) obtained is in-60 DEG C of freeze formings, and freeze drying 72h obtains shaping nano silver wire/Graphene composite aerogel.
The nano silver wire that this method obtains/Graphene composite elastic aeroge is that skeleton is built into three-dimensional netted cross-linked structure by Graphene, and nano silver wire is distributed in graphenic surface and makes resiliency supported and conduction enhancement unit, density 28mg/cm
3, compressible 74%, electrical conductivity 190S/m.
Embodiment 2:
(1) graphene oxide is scattered in deionized water to form concentration be 5.0mg/mL graphene oxide dispersion;
(2) nano silver wire is scattered in deionized water to form concentration be 1.0mg/mL nano silver wire dispersion liquid;
(3) graphene oxide dispersion is mixed with nano silver wire dispersion liquid, magnetic agitation 1.0h, obtain nano silver wire-graphene oxide mixed dispersion liquid;
(4) nano silver wire-graphene oxide mixed dispersion liquid that step (3) obtains is added ascorbic acid (ascorbic acid and graphene oxide mass ratio are 1:50), put into water-bath, 95 DEG C of reduction 3h obtain nano silver wire-Graphene hydrogel;
(5) nano silver wire/Graphene composite aquogel that step (4) obtains is put into the ammoniacal liquor that concentration is 10%, soak 5 days, remove reaction residual impurity;
(6) nano silver wire/Graphene composite aquogel step (5) obtained is in-60 DEG C of freeze formings, and freeze drying 48h obtains shaping nano silver wire/Graphene composite aerogel.
The nano silver wire that this method obtains/Graphene compound ultra-light elastic aeroge density 22mg/cm
3, compressible 70%, electrical conductivity 100S/m.
Embodiment 3:
(1) graphene oxide is scattered in deionized water to form concentration be 10.0mg/mL graphene oxide dispersion;
(2) nano silver wire is scattered in deionized water to form concentration be 8.0mg/mL nano silver wire dispersion liquid;
(3) graphene oxide dispersion is mixed with nano silver wire dispersion liquid, ultrasonic disperse 1.0h, obtain nano silver wire-graphene oxide mixed dispersion liquid;
(4) nano silver wire-graphene oxide mixed dispersion liquid that step (3) obtains is added hydroiodic acid (mass ratio of hydroiodic acid and graphene oxide is 1:35), put into water-bath, 90 DEG C of reduction 5h obtain nano silver wire/Graphene hydrogel;
(5) nano silver wire/Graphene composite aquogel that step (4) obtains is put into the ammoniacal liquor that concentration is 7%, soak 4 days, remove reaction residual impurity;
(6) nano silver wire/Graphene composite aquogel that step (5) obtains is carried out supercritical carbon dioxide drying and obtain shaping nano silver wire/Graphene composite aerogel.
The nano silver wire that this method obtains/Graphene composite elastic aeroge, density 35mg/cm
3, compressible 78%, electrical conductivity 350S/m.
Embodiment 4:
(1) graphene oxide is scattered in deionized water to form concentration be 6.0mg/mL graphene oxide dispersion;
(2) nano silver wire is scattered in deionized water to form concentration be 10.0mg/mL nano silver wire dispersion liquid;
(3) graphene oxide dispersion is mixed with nano silver wire dispersion liquid, ultrasonic disperse 0.5h, obtain nano silver wire-graphene oxide mixed dispersion liquid;
(4) nano silver wire-graphene oxide mixed dispersion liquid that step (3) obtains is added ethylenediamine (mass ratio of ethylenediamine and graphene oxide is 1:20), put into water-bath, 85 DEG C of reduction 8h obtain nano silver wire-Graphene hydrogel;
(5) nano silver wire/Graphene composite aquogel that step (4) obtains is put into the ammoniacal liquor that concentration is 10%, soak 6 days, remove reaction residual impurity;
(6) nano silver wire/Graphene composite aquogel that step (5) obtains is carried out supercritical carbon dioxide drying and obtain shaping nano silver wire-Graphene composite aerogel.
The nano silver wire that this method obtains/Graphene composite elastic aeroge, density 54mg/cm
3, compressible 80%, electrical conductivity 560S/m.
Embodiment 5:
(1) graphene oxide is scattered in deionized water to form concentration be 10.0mg/mL graphene oxide dispersion;
(2) nano silver wire is scattered in deionized water to form concentration be 12.0mg/mL nano silver wire dispersion liquid;
(3) graphene oxide dispersion is mixed with nano silver wire dispersion liquid, mechanical agitation 1.0h, obtain nano silver wire-graphene oxide mixed dispersion liquid;
(4) nano silver wire-graphene oxide mixed dispersion liquid that step (3) obtains is added sodium borohydride (mass ratio of sodium borohydride and graphene oxide is 1:11), put into water-bath, 90 DEG C of reduction 1h obtain nano silver wire/Graphene hydrogel;
(5) nano silver wire/Graphene composite aquogel that step (4) obtains is put into the ammoniacal liquor that concentration is 10%, soak 5 days, remove reaction residual impurity;
(6) nano silver wire/Graphene composite aquogel step (5) obtained is in-60 DEG C of freeze formings, and freeze drying 80h obtains shaping nano silver wire/Graphene composite aerogel.
The nano silver wire that this method obtains/Graphene composite elastic aeroge, density 42mg/cm
3, compressible 75%, electrical conductivity 420S/m.
Above-described embodiment is used for explaining and the present invention is described, instead of limits the invention, and in the protection domain of spirit of the present invention and claim, any amendment make the present invention and change, all fall into protection scope of the present invention.
The above; be only the present invention's preferably detailed description of the invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (10)
1. nano silver wire/Graphene composite elastic aeroge, it is characterized in that, be that skeleton is built into three-dimensional netted cross-linked structure with Graphene, nano silver wire is distributed in graphenic surface and makes resiliency supported and conduction enhancement unit, and this aeroge density is 0.5 ~ 300mg/cm
3, compressible is 20% ~ 85%, and electrical conductivity is 10
-2~ 10
3s/m.
2. nano silver wire according to claim 1/Graphene composite elastic aeroge preparation method, is characterized in that, comprise the following steps:
A, graphene oxide is scattered in Different Weight part deionized water in form concentration be 0.1 ~ 50mg/mL graphene oxide dispersion;
B, nano silver wire is scattered in Different Weight part deionized water in form concentration be 0.05 ~ 50mg/mL nano silver wire dispersion liquid;
C, graphene oxide dispersion to be mixed with nano silver wire dispersion liquid, obtain nano silver wire-graphene oxide mixed dispersion liquid through ultrasonic disperse or stirring;
D, the nano silver wire-graphene oxide mixed dispersion liquid obtained by step C put into reaction vessel, add reducing agent and carry out chemical reduction method reduction, obtain nano silver wire/Graphene composite aquogel;
E, the nano silver wire/Graphene composite aquogel obtained by step D put into deionized water or ammoniacal liquor, soak 1 ~ 10 day, remove reaction residual impurity;
F, nano silver wire/Graphene hydrogel step e obtained carry out freeze drying or supercritical drying, obtain nano silver wire-Graphene composite elastic aeroge.
3. nano silver wire/Graphene composite elastic aeroge preparation method according to claim 2, is characterized in that, the appropriate method that graphene oxide described in steps A is known in the art, as standby in Hummers legal system.
4. a kind of nano silver wire/Graphene composite elastic aeroge preparation method according to claim 2, is characterized in that, nano silver wire diameter 2 ~ 300nm described in step B, length 5 ~ 200 μm.
5. a kind of nano silver wire/Graphene composite elastic aeroge preparation method according to claim 2, it is characterized in that, the ultrasonic power 40 ~ 1000W of ultrasonic disperse described in step C, supersonic frequency 20 ~ 80KHz, described stirring is magnetic agitation or mechanical agitation, and rotating speed is 40 ~ 4000 revs/min.
6. a kind of nano silver wire/Graphene composite elastic aeroge preparation method according to claim 2, it is characterized in that, the reducing agent of chemical reduction method employing described in step D is one or more in sodium hydrogensulfite, ascorbic acid, sodium ascorbate, hydrazine hydrate, glucose, sodium borohydride, hydroiodic acid, ethylenediamine etc.; Recovery time is 0.5 ~ 24h, and reduction temperature is 10 ~ 160 DEG C.
7. a kind of nano silver wire/Graphene composite elastic aeroge preparation method according to claim 2, it is characterized in that, ammonia concn described in step e is 5 ~ 28%.
8. a kind of nano silver wire/Graphene composite elastic aeroge preparation method according to claim 2, it is characterized in that, described in step F, cryodesiccated condition comprises: cryogenic temperature is-5 ~-65 DEG C, and baking temperature is-45 ~ 10 DEG C, vacuum 10 ~ 110Pa, drying time is 12 ~ 96h; Described supercritical drying is that supercritical carbon dioxide is dry.
9. an application for nano silver wire described in claim 1/Graphene composite elastic aeroge, is characterized in that, for absorption, catalyze and degrade organic pollutants.
10. the application of a kind of nano silver wire-Graphene composite elastic aeroge according to claim 1, is characterized in that, in piezoresistive switch.
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