CN106653159A - Preparation method and application for composite elastomer containing graphene coated copper nanowire - Google Patents
Preparation method and application for composite elastomer containing graphene coated copper nanowire Download PDFInfo
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- CN106653159A CN106653159A CN201611241454.3A CN201611241454A CN106653159A CN 106653159 A CN106653159 A CN 106653159A CN 201611241454 A CN201611241454 A CN 201611241454A CN 106653159 A CN106653159 A CN 106653159A
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- porous material
- water
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- slaine
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
-
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
- H01B1/026—Alloys based on copper
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
The invention relates to a composite elastomer containing a graphene coated copper nanowire. The composite elastomer comprises a porous material and a graphene coated metal nanowire. The graphene coated metal nanowire is grown on a skeleton of the porous material. The porous material is a rebounding porous material. The composite elastomer containing the graphene coated copper nanowire provided by the invention can rebound and recover to an original shape within 2 seconds after being pressed and released, after the composite elastomer is pressed and released for the first time, a resistance change rate is smaller than 2%, after the composite elastomer is pressed and released for 100 times, the composite elastomer can still rebound to the original shape, and the resistance change rate is smaller than 10%.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, and in particular to a kind of answering containing graphene coated copper nano-wire
Close method for producing elastomers and application.
Background technology
Excellent electric conductivity can be obtained using filler of the low-dimensional materials as conducing composite material.Metal nanometer line because
For its specific surface area greatly, the advantages of conducting electricity very well is widely used.Wherein the superior performance of gold, silver nano wire but its
Expensive price is the principal element for limiting its application, and copper nano-wire conducts electricity very well because its cheap, rich reserves
Advantage has obtained increasing concern, while it also has highly important application prospect in association area.But copper nanometer
The oxidizable problem of line limits its application in some aspects.Graphene effectively can grind preservation antioxidation material as a kind of
Study carefully and be increasingly becoming focus.When Graphene is covered to metal surface, its can improve in environment oxidation material from graphenic surface to
The activation energy of lower metal interface diffusion, forms a barrier, so as to improve the antioxygenic property of metal, but copper nano-wire is tied
Structure is unstable, easily caves in, bad mechanical strength, and the problem of compression resilience difference seems that effect is little, and material morphology and structure
Change can cause performance change, reliability decrease, service life to shorten.
CN105772741A by by Graphene/copper nano-wire composite and sodium alginate soln, poly-vinyl alcohol solution,
At least one mixing in chitosan solution, gelatin solution, using sodium alginate, polyvinyl alcohol, shitosan liquid, gelatin in water
The intramolecular or intermolecular hydrogen bonding of formation, for three-dimensional aerogel structure skeletal support is provided, and this preparation method needs first will be single
Solely synthesizing graphite alkene/copper nano-wire composite is simultaneously purified and dried process, complex steps to it, and Graphene in product/
Active force between copper nano-wire composite and skeleton is on the weak side, easy to fall off.
So seek a kind of oxidation that can effectively prevent copper nano-wire, and it is simple, can guarantee that material has again preferable
The preparation method of compression resilience be extremely necessary.
The content of the invention
In view of problems of the prior art, an object of the present invention is to provide a kind of containing graphene coated copper
The composite elastic body of nano wire, including porous material and graphene coated metal nanometer line；The graphene coated metal nano
Line is grown on the skeleton of the porous material；The porous material is the porous material of resiliency." resiliency " is referred to
Material volume after outer force compresses or stretcher strain changes can voluntarily restore to the original state after external force release.
Graphene coated metal nanometer line is grown on the skeleton of the porous material in the present invention, on the one hand, porous material
Material serves as the skeletal support of graphene coated metal nanometer line, prevents the irreversible decay of performance caused by structure collapses；It is another
Aspect porous material improves the mechanical strength and compression resilience of graphene coated metal nanometer line, and what is finally given is have three
The conductive good body of dimension cavernous structure.The elastomer containing graphene coated metal nanometer line that the present invention is prepared is depressed
Resilience and can return to the original form in 2 seconds with after release, its resistance change rate is less than 2%, 100 after pressing first and discharging
Remain to recoil to original shape after secondary pressing and release, resistance change rate resistance is less than 10%.
Metal of the present invention is selected from copper and silver；It is preferred that copper.
Porous material of the present invention includes any one in sponge, porous plastics and aeroge or at least two group
Close, preferred sponge.
The second object of the present invention is to provide a kind of preparation method of the composite elastic body as described in one of purpose, including
Following steps：
(1) slaine and graphene oxide are scattered in into deionized water, sequentially add covering and alkali, afterwards, under stirring
Reducing agent is added, mixed dispersion liquid is obtained；
(2) porous material is added in step (1) mixed dispersion liquid, it is ultrasonically treated, obtain reactant liquor；The porous
Material is the porous material of resiliency；
(3) step (2) gained reactant liquor is warming up to into 60～100 DEG C, 30～120min of isothermal reaction will be reacted more
Porous materials are washed, are dried, and obtain the composite elastic body containing graphene coated metal nanometer line.
For example, the reaction temperature in step (3) of the present invention be 60 DEG C, 61 DEG C, 63 DEG C, 65 DEG C, 67 DEG C, 69 DEG C, 70 DEG C, 71
℃、72℃、73℃、74℃、75℃、76℃、77℃、78℃、79℃、80℃、83℃、85℃、87℃、89℃、90℃、92
DEG C, 94 DEG C, 96 DEG C, 98 DEG C, 99 DEG C or 100 DEG C etc..For example, the isothermal reaction time in step (3) of the present invention be 30min,
32min、36min、39min、40min、41min、42min、43min、44min、45min、46min、47min、48min、
49min、50min、51min、52min、53min、54min、55min、56min、57min、58min、59min、60min、
65min, 70min, 80min, 90min, 100min, 105min, 110min, 118min or 120min etc..
The electrical conductivity of the elastomer containing graphene coated metal nanometer line that preparation method of the present invention is prepared up to 1.5 ×
10-2More than S/m, resilience and can return to the original form after depressed and release in 2 seconds, its electricity after pressing first and discharging
Resistive rate is less than 2%, remains to recoil to original shape after 100 pressings and release, and resistance change rate resistance is less than 10%.
And the preparation method mild condition, temperature is less than high temperature hydro-thermal method of the prior art, process is simple, and the porous of resiliency
Material source is extensively, cheap, compared with organic matters such as sodium alginate of the prior art, polyvinyl alcohol, shitosan liquid, gelatin
Post processing is simpler.
The cation of slaine described in step (1) is selected from Ag+And Cu2+, preferred Cu2+；In the slaine contend with from
Son is selected from NO3 -、SO4 2-、CH3COO-、Cl-And C6H5O7 3-In any one or at least two combination.For example, the metal
Salt is Cu (NO3)2、AgNO3、CuSO4、Cu(CH3COO)2、Cu3(C6H5O7)2Deng.
Preferably, slaine described in step (1) and the mass ratio of the graphene oxide are (1～120):1, such as 1:
1、1:10、1:20、1:30、1:40、1:50、1:53、1:58、1:61、1:65、1:68、1:70、1:72、1:74、1:76、1:79、
1:80、1:85、1:90、1:94、1:100、1:105、1:110、1:112、1:118 or 1:120 grades, preferred (20～50):1.
Covering described in step (1) of the present invention includes any one in ethylenediamine, cetylamine and octadecylamine, such as second
Diamines, cetylamine or octadecylamine, preferred ethylenediamine.
Preferably, the addition form of covering described in step (1) includes directly adding and/or being dissolved in add after water,
It is preferably dissolved in after water and adds.
Preferably, the slaine and the mass ratio of the covering are 1:(2～20), 1:2、1:3、1:4、1:5、1:
5.2、1:5.3、1:5.8、1:6、1:7、1:8、1:8.1、1:8.7、1:9、1:9.5、1:10、1:11、1:12、1:13、1:14、1:
15、1:16、1:17、1:18、1:19 or 1:20 etc., preferably 1:(5～15).
Covering can select any one in ethylenediamine, cetylamine and octadecylamine as bag with complexing of metal ion
Agent is covered, is conducive to the growth of metal nanometer line.Ethylenediamine is further selected, it is easy to washing and removes, and is conducive to improving compound bullet
The electric conductivity of gonosome.
Alkali described in step (1) of the present invention is including any one in barium hydroxide, NaOH and potassium hydroxide or extremely
Few two kinds combination, wherein, it is typical but non-limiting to be combined as：Barium hydroxide and NaOH, barium hydroxide and hydroxide
Potassium, NaOH and potassium hydroxide, preferred NaOH and/or potassium hydroxide.
Preferably, the addition form of alkali described in step (1) includes directly adding and/or being dissolved in add after water, preferably
It is dissolved in after water and adds.
Preferably, the slaine and the mass ratio of the alkali are 1:(200～800), such as 1:200、1:210、1:
220、1:230、1:240、1:250、1:280、1:300、1:320、1:350、1:370、1:400、1:410、1:430、1:450、
1:460、1:470、1:490、1:500、1:510、1:530、1:560、1:690、1:750 or 1:800 etc., preferably 1:(250～
500)。
Reducing agent described in step (1) of the present invention include hydrazine hydrate, catechin, ascorbic acid, sodium borohydride, citric acid and
In sodium hypophosphite any one or at least two combination, wherein typical but non-limiting be combined as：Hydrazine hydrate and catechu
Element, ascorbic acid and sodium borohydride, citric acid and sodium hypophosphite, hydrazine hydrate and sodium borohydride, citric acid and and catechin, preferably
Hydrazine hydrate and/or catechin.
Preferably, the addition form of reducing agent described in step (1) includes directly adding and/or being dissolved in add after water,
It is preferably dissolved in after water and adds.
Preferably, when the slaine and the mass ratio (1～10) of the reducing agent:1, such as 1:1、1.3:1、1.6:1、
1.9:1、2:1、2.2:1、2.3:1、2.4:1、2.5:1、2.6:1、2.7:1、2.8:1、2.9:1、3:1、3.3:1、3.5:1、
3.9:1、4:1、5:1、6:1、7:1、8:1、9:1、9.5:1 or 10:1 etc., preferably (1～4):1.
Metal complex ion reduction in reaction system can be grown to metal nanometer line, preferred hydrazine hydrate by reducing agent
And/or catechin helps to form gentle reducing environment, be conducive to reactant liquor compatible with sponge.
Metal salt concentrations are 0.05～0.5mol/L in mixed dispersion liquid described in step (1) of the present invention, for example
0.05mol/L、0.06mol/L、0.07mol/L、0.08mol/L、0.09mol/L、0.1mol/L、0.11mol/L、0.12mol/
L、0.13mol/L、0.14mol/L、0.15mol/L、0.16mol/L、0.17mol/L、0.18mol/L、0.19mol/L、
0.2mol/L、0.23mol/L、0.25mol/L、0.28mol/L、0.3mol/L、0.32mol/L、0.34mol/L、0.38mol/
L, 0.4mol/L, 0.41mol/L, 0.45mol/L, 0.49mol/L or 0.5mol/L etc., preferably 0.05～0.2mol/L.
Porous material described in step (2) of the present invention is including any one in sponge, porous plastics and aeroge or extremely
Few two kinds combination, wherein, it is typical but non-limiting to be combined as：Sponge and porous plastics, sponge and aeroge, porous plastics
And aeroge, preferred sponge.
Sponge is cheap and easy to get, and hole enriches, and compression resilience is good good with the compatibility of reactant liquor.Further increase compound producing
The compression resilience of thing and the uniformity of combination product.
Preferably, the porous material and the volume ratio of the mixed dispersion liquid are 1:(5～50), such as 1:5、1:6、1:
7、1:8、1:9、1:10、1:11、1:12、1:13、1:14、1:15、1:16、1:18、1:20、1:23、1:27、1:30、1:32、1:
36、1:39、1:40、1:42、1:47、1:49 or 1:50 etc., preferably 1:(8～15).
Preferably, ultrasound is described in step (2)：10～60min of ultrasound under 20kHz～100kHz, for example, the ultrasound
Frequency is 20kHz, 30kHz, 40kHz, 50kHz, 60kHz, 70kHz, 80kHz, 90kHz or 100kHz etc., and ultrasonic time is
10min, 15min, 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min or 60min etc., preferably
15～30min of ultrasound under 50kHz.
Heating up described in step (3) of the present invention includes warming-in-water.
Preferably, reaction temperature described in step (3) is 70～80 DEG C, and the reaction time is 40～60min.
Preferably, washing includes for the reacted porous material soaking 0.5 in deionized water described in step (3)
～5h, such as 0.5h, 0.8h, 1h, 1.2h, 1.5h, 1.8h, 2h, 2.4h, 2.9h, 3h, 3.5h, 4h, 4.5h or 5h etc..
Preferably, drying includes vacuum drying and/or freeze-drying described in step (3).
Preferably, the drying be included in vacuum oven process 1～5d, such as 1d, 1.5d, 2d, 2.5d, 3d,
3.5d, 4d, 4.5d or 5d etc..
The third object of the present invention is to provide as described in one of purpose composite elastic body in flexible electronic device, sensing
Application in device, ultracapacitor, water process.
Compared with prior art, the present invention at least has the advantages that：
Graphene coated metal nanometer line is grown on the skeleton of the porous material in the present invention, on the one hand, porous material
Material serves as the skeletal support of graphene coated metal nanometer line, prevents the irreversible decay of performance caused by structure collapses；It is another
Aspect porous material improves the mechanical strength and compression resilience of graphene coated metal nanometer line, and what is finally given is have three
The conductive good body of dimension cavernous structure.The electrical conductivity of the elastomer containing graphene coated metal nanometer line that the present invention is prepared exists
Resilience and can return to the original form in 2 seconds after depressed and release, its resistance change rate is little after pressing first and discharging
Remain to recoil to original shape in 2%, 100 pressing and after discharging, resistance change rate resistance is less than 10%.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the sponge in embodiment 1 after drying.
Fig. 2 is the surface sweeping electron microscope of the gained graphene coated copper nano-wire foam of embodiment 1.
Fig. 3 is the big multiple surface sweeping electron microscope of the gained graphene coated copper nano-wire foam of embodiment 1.
Wherein, described " foam " is the complex of graphene coated metal nanometer line and porous material, and retains porous material
The porous skeleton structure of material.
Fig. 4 is the resistance when gained graphene coated copper nano-wire foam of embodiment 1 is subject to discontinuity to press and discharge
Rate of change-time graph.Resistance change rate Δ R/R0Represent, wherein R0It is that graphene coated copper nano-wire foam is in standing
The resistance of state, Δ R is resistance compared to R0Value added.
Fig. 5 is the digital photograph of the gained graphene coated copper nano-wire foam of embodiment 1 and untreated sponge, wherein white
For untreated sponge, black gray expandable for graphene coated copper nano-wire foam.
Below the present invention is described in more detail.But following examples are only the simple example of the present invention, are not represented
Or the scope of the present invention is limited, protection scope of the present invention is defined by claims.
Specific embodiment
Further illustrate technical scheme below in conjunction with the accompanying drawings and by specific embodiment.
For the present invention is better described, technical scheme is readily appreciated, it is as follows that the present invention enumerates embodiment.Ability
Understanding is of the invention it will be clearly understood that the embodiment is only to aid in for field technique personnel, is not construed as the concrete restriction to the present invention.
Embodiment 1
By the Cu (NO that 10mL concentration is 0.1mol/L3)2Solution is mixed with the graphene oxide water solution of 5mL concentration 2mg/mL
Close uniform.Then the ethylenediamine solution of 2mL99% is added, after stirring 25min, the NaOH for adding the 10mol/L of 200mL is molten
Liquid simultaneously persistently stirs 50min, the hydrazine hydrate solution of 0.2mL35%, and ultrasound 15min is subsequently adding, subsequently by deionized water
It is cleaned by ultrasonic 10min and the sponge in 60 DEG C of drying is added in reactant liquor, and continue ultrasonically treated 20min, finally, will reacts
System reacts 80min under 70 DEG C of water bath condition, by the product for obtaining in vacuum drying oven drying at room temperature 24h, finally can obtain
To graphene coated copper nano-wire foam, electrical conductivity is up to 9 × 10-2S/m。
Fig. 1 is the scanning electron microscope (SEM) photograph of the sponge in embodiment 1 after drying.Sponge itself after drying as can be seen from Figure 1
With three-dimensional poroid skeleton structure, and surface free from admixture.
Fig. 2 is the surface sweeping electron microscope of the gained graphene coated copper nano-wire foam of embodiment 1.Sponge as can be seen from Figure 2
Three-dimensional poroid skeleton structure on cover a layer graphene cladding copper nano-wire, illustrate graphene coated copper nano-wire in sponge
Three-dimensional poroid skeleton structure on growth in situ, finally give graphene coated copper nano-wire foam.
Fig. 3 is the big multiple surface sweeping electron microscope of the gained graphene coated copper nano-wire foam of embodiment 1.Can see from Fig. 3
Observe graphene coated copper nano-wire non-directional to be dispersed on the three-dimensional poroid skeleton of sponge.
Fig. 4 is the resistance when gained graphene coated copper nano-wire foam of embodiment 1 is subject to discontinuity to press and discharge
Rate of change-time graph.As can be seen that after resulting graphene coated copper nano-wire foam is pressed by finger, its resistance subtracts
It is little, and the absolute value of resistance change rate increases with the increase of compression ratio；When resulting graphene coated copper nano-wire foam
It is discharged into after nature from pressed state, its resistance substantially returns to the resistance value in static condition again, illustrates with setting about
Refer to the release of pressing, the resistance of graphene coated copper nano-wire foam can just substantially return to the electricity under original nature in 1s
Resistance, the graphene coated copper nano-wire foam obtained by showing has preferable compression resilience.After 100 pressings and release still
Original shape can be recoiled to, the absolute value of resistance change rate is 5%.
Fig. 5 is the digital photograph of the gained graphene coated copper nano-wire foam of embodiment 1 and untreated sponge, wherein white
For untreated sponge.Black gray expandable for graphene coated copper nano-wire foam.Wherein graphene coated copper nano-wire foam
Color is uniform, illustrates on sponge equably growth in situ graphene coated copper nano-wire.
Comparative example 1-1
By the Cu (NO that 10mL concentration is 0.1mol/L3)2Solution is mixed with the graphene oxide water solution of 5mL concentration 2mg/mL
Close uniform.Then the ethylenediamine solution of 2mL99% is added, after stirring 25min, the NaOH for adding the 10mol/L of 200mL is molten
Liquid simultaneously persistently stirs 50min, the hydrazine hydrate solution of 0.2mL35%, and ultrasound 15min is subsequently adding, subsequently by deionized water
It is cleaned by ultrasonic 10min and the sponge in 60 DEG C of drying is added in reactant liquor, and continue ultrasonically treated 20min, finally, will reacts
System reacts 10h in the ptfe autoclave liner of 500mL is transferred at 150 DEG C, and the product for obtaining is dried in vacuum
Drying at room temperature 24h in case, is finally obtained graphene coated copper nano-wire foam.Its electrical conductivity is 1.8 × 10-2S/m, is pressed
Pressure and resilience and can return to the original form in 8 seconds after discharging, its resistance change rate is 4.6% after pressing first and discharging,
Remain to recoil to original shape after 100 pressings and release, resistance change rate is 18.7%.
Comparative example 1-2
By the Cu (NO that 10mL concentration is 0.1mol/L3)2Solution is mixed with the graphene oxide water solution of 5mL concentration 2mg/mL
Close uniform.Then the ethylenediamine solution of 2mL99% is added, after stirring 25min, the NaOH for adding the 10mol/L of 200mL is molten
Liquid simultaneously persistently stirs 50min, the hydrazine hydrate solution of 0.2mL35%, and ultrasound 15min is subsequently adding, by reaction system at 70 DEG C
Water bath condition under react 80min, the product for obtaining is washed three times in deionized water, then it is mixed with gelatin, Jing is cold
Freeze dried process 24h and obtain graphene coated copper nano-wire airsetting glue elastomer.Its electrical conductivity is 1 × 10-2S/m, it is depressed
Slow with resilience after release, returning to the original form needs 15 seconds, and its resistance change rate is 9%, 100 after pressing first and discharging
Remain to recoil to original shape substantially after secondary pressing and release, resistance change rate is 23.7%.
Embodiment 2
By the Cu (NO that 15mL concentration is 0.05mol/L3)2Solution is mixed with the graphene oxide water solution of 5mL concentration 1mg/mL
Close uniform.Then the ethylenediamine solution of 3mL80% is added, after stirring 20min, the NaOH for adding the 5mol/L of 250mL is molten
Liquid simultaneously persistently stirs 45min, the hydrazine hydrate solution of 0.3mL35%, and ultrasound 25min is subsequently adding, subsequently by deionized water
It is cleaned by ultrasonic 10min and the sponge in 60 DEG C of drying is added in reactant liquor, and continue ultrasonically treated 15min, finally, will reacts
System reacts 90min under 60 DEG C of water bath condition, by the product for obtaining in vacuum drying oven drying at room temperature 12h, finally can obtain
To graphene coated copper nano-wire foam.Its electrical conductivity is 5 × 10-2S/m, can the resilience in 1.5 seconds after depressed and release
And return to the original form, its resistance change rate is 1.2% after pressing first and discharging, and is remained to back after 100 pressings and release
To original shape, resistance change rate is 5.6% to bullet.
Embodiment 3
By the Cu (NO that 20mL concentration is 0.1mol/L3)2Solution and the graphene oxide water solution that 5mL concentration is 2mg/mL
It is well mixed.Then the ethylenediamine solution of 4mL60% is added, after stirring 30min, 400mL concentration is added for 15mol/L's
NaOH solution simultaneously persistently stirs 60min.Finally, the hydrazine hydrate solution of 0.4mL80%, and ultrasound 25min are added, subsequently will be spent
Ionized water is cleaned by ultrasonic 10min and the sponge in 60 DEG C of drying is added in reactant liquor, and continues ultrasonically treated 15min, finally,
Reaction system is reacted into 50min under 90 DEG C of water bath conditions, by the product for obtaining in vacuum drying oven drying at room temperature 20h, finally
Graphene coated copper nano-wire foam is obtained.
Its electrical conductivity is 7 × 10-2S/m, resilience and can return to the original form after depressed and release in 1.5 seconds,
Its resistance change rate is 1.3% after pressing first and discharging, and remains to recoil to original shape after 100 pressings and release, electricity
Resistive rate is 6.2%.
Embodiment 4
By the Cu (NO that 30mL concentration is 0.1mol/L3)2Solution and the graphene oxide water solution that 5mL concentration is 5mg/mL
It is well mixed.Then the ethylenediamine solution of 5mL99% is added, after stirring 30min, 600mL concentration is added for 15mol/L's
NaOH solution simultaneously persistently stirs 60min.Finally, the hydrazine hydrate solution of 0.5mL80%, and ultrasound 25min are added, subsequently will be spent
Ionized water is cleaned by ultrasonic 10min and the sponge in 60 DEG C of drying is added in reactant liquor, and continues ultrasonically treated 20min, finally,
Reaction system is reacted into 120min under 90 DEG C of water bath conditions, by the product for obtaining in vacuum drying oven drying at room temperature 24h, finally
Graphene coated copper nano-wire foam is obtained.
Its electrical conductivity is 6 × 10-2S/m, resilience and can return to the original form after depressed and release in 1.5 seconds,
Its resistance change rate is 1.1% after pressing first and discharging, and remains to recoil to original shape after 100 pressings and release, electricity
Resistive rate is 5.2%.
Embodiment 5
By the Cu (NO that 10mL concentration is 0.1mol/L3)2Solution is mixed with the graphene oxide water solution of 1mL concentration 2mg/mL
Close uniform.Then the ethylenediamine solution of 2mL99% is added, after stirring 25min, the NaOH for adding the 10mol/L of 200mL is molten
Liquid simultaneously persistently stirs 50min, the hydrazine hydrate solution of 0.2mL35%, and ultrasound 15min is subsequently adding, subsequently by deionized water
It is cleaned by ultrasonic 10min and the sponge in 60 DEG C of drying is added in reactant liquor, and continue ultrasonically treated 20min, finally, will reacts
System reacts 80min under 70 DEG C of water bath condition, by the product for obtaining in vacuum drying oven drying at room temperature 24h, finally can obtain
To graphene coated copper nano-wire foam.
Its electrical conductivity is 5 × 10-2S/m, resilience and can return to the original form after depressed and release in 2 seconds, first
Its resistance change rate is 1.6% after secondary pressing and release, remains to recoil to original shape, resistance after 100 pressings and release
Rate of change is 8.6%.
Embodiment 6
By the Cu (NO that 20mL concentration is 0.1mol/L3)2Solution and the graphene oxide water solution that 25mL concentration is 2mg/mL
It is well mixed.Then the ethylenediamine solution of 4mL60% is added, after stirring 30min, 400mL concentration is added for 15mol/L's
NaOH solution simultaneously persistently stirs 60min.Finally, the hydrazine hydrate solution of 0.4mL80%, and ultrasound 25min are added, subsequently will be spent
Ionized water is cleaned by ultrasonic 10min and the sponge in 60 DEG C of drying is added in reactant liquor, and continues ultrasonically treated 15min, finally,
Reaction system is reacted into 50min under 90 DEG C of water bath conditions, by the product for obtaining in vacuum drying oven drying at room temperature 20h, finally
Graphene coated copper nano-wire foam is obtained.
Its electrical conductivity is 3 × 10-2S/m, resilience and can return to the original form after depressed and release in 2 seconds, first
Its resistance change rate is 1.7% after secondary pressing and release, remains to recoil to original shape, resistance after 100 pressings and release
Rate of change is 7%.
Embodiment 7
By the Cu (NO that 20mL concentration is 0.1mol/L3)2Solution is water-soluble for the graphene oxide of 2mg/mL with 2.5mL concentration
Liquid is well mixed.Then the ethylenediamine solution of 4mL60% is added, after stirring 30min, 400mL concentration is added for 15mol/L
NaOH solution and persistently stir 60min.Finally, the hydrazine hydrate solution of 0.4mL80%, and ultrasound 25min are added, subsequently will be used
Deionized water is cleaned by ultrasonic 10min and the sponge in 60 DEG C of drying is added in reactant liquor, and continues ultrasonically treated 15min, most
Afterwards, reaction system is reacted into 50min under 90 DEG C of water bath conditions, by the product for obtaining in vacuum drying oven drying at room temperature 20h, most
Graphene coated copper nano-wire foam is obtained eventually.
Its electrical conductivity is 4 × 10-2S/m, resilience and can return to the original form after depressed and release in 2 seconds, first
Its resistance change rate is 1.62% after secondary pressing and release, remains to recoil to original shape, resistance after 100 pressings and release
Rate of change is 8.3%.
Embodiment 8
By the Cu (NO that 20mL concentration is 0.1mol/L3)2Solution and the graphene oxide water solution that 5mL concentration is 2mg/mL
It is well mixed.Then the ethylenediamine solution of 2mL60% is added, after stirring 30min, 400mL concentration is added for 15mol/L's
NaOH solution simultaneously persistently stirs 60min.Finally, the hydrazine hydrate solution of 0.4mL80%, and ultrasound 25min are added, subsequently will be spent
Ionized water is cleaned by ultrasonic 10min and the sponge in 60 DEG C of drying is added in reactant liquor, and continues ultrasonically treated 15min, finally,
Reaction system is reacted into 50min under 90 DEG C of water bath conditions, by the product for obtaining in vacuum drying oven drying at room temperature 20h, finally
Graphene coated copper nano-wire foam is obtained.
Its electrical conductivity is 2 × 10-2S/m, resilience and can return to the original form after depressed and release in 2 seconds, first
Its resistance change rate is 1.73% after secondary pressing and release, remains to recoil to original shape, resistance after 100 pressings and release
Rate of change is 9.6%.
Embodiment 9
Copper acetate solution of the 30mL concentration for 0.1mol/L is mixed with the graphene oxide water solution that 5mL concentration is 5mg/mL
Close uniform.Then the ethylenediamine solution of 15mL99% is added, after stirring 30min, 600mL concentration is added for 15mol/L's
NaOH solution simultaneously persistently stirs 60min.Finally, the hydrazine hydrate solution of 0.5mL80%, and ultrasound 25min are added, subsequently will be spent
Ionized water is cleaned by ultrasonic 10min and the sponge in 60 DEG C of drying is added in reactant liquor, and continues ultrasonically treated 20min, finally,
Reaction system is reacted into 120min under 90 DEG C of water bath conditions, by the product for obtaining in vacuum drying oven drying at room temperature 24h, finally
Graphene coated copper nano-wire foam is obtained.
Its electrical conductivity is 2.5 × 10-2S/m, resilience and can return to the original form after depressed and release in 2 seconds,
Its resistance change rate is 1.81% after pressing first and discharging, and remains to recoil to original shape after 100 pressings and release, electricity
Resistive rate is 8.7%.
Embodiment 10
By the copper citrate solution that 30mL concentration is 0.1mol/L and the graphene oxide water solution that 5mL concentration is 5mg/mL
It is well mixed.Then the ethylenediamine solution of 5mL99% is added, after stirring 30min, 240mL concentration is added for 15mol/L's
NaOH solution simultaneously persistently stirs 60min.Finally, the hydrazine hydrate solution of 0.5mL80%, and ultrasound 25min are added, subsequently will be spent
Ionized water is cleaned by ultrasonic 10min and the sponge in 60 DEG C of drying is added in reactant liquor, and continues ultrasonically treated 20min, finally,
Reaction system is reacted into 120min under 90 DEG C of water bath conditions, by the product for obtaining in vacuum drying oven drying at room temperature 24h, finally
Graphene coated copper nano-wire foam is obtained.
Its electrical conductivity is 1.8 × 10-2S/m, resilience and can return to the original form after depressed and release in 2 seconds,
Its resistance change rate is 1.85% after pressing first and discharging, and remains to recoil to original shape after 100 pressings and release, electricity
Resistive rate is 9.32%.
Embodiment 11
By the AgNO that 15mL concentration is 0.05mol/L3Solution mixes with the graphene oxide water solution of 5mL concentration 1mg/mL
Uniformly.Then the ethylenediamine solution of 3mL80% is added, after stirring 20min, the NaOH solution of the 5mol/L of 740mL is added
And 45min is persistently stirred, and the hydrazine hydrate solution of 0.3mL35%, and ultrasound 25min are subsequently adding, subsequently deionized water is surpassed
Sound cleans 10min and the sponge in 60 DEG C of drying is added in reactant liquor, and continues ultrasonically treated 15min, finally, by reactant
React 90min under the water bath condition for tying up to 60 DEG C, by the product for obtaining in vacuum drying oven drying at room temperature 12h, it is final available
Graphene coated nano silver wire foam.
Its electrical conductivity is 2.3 × 10-2S/m, resilience and can return to the original form after depressed and release in 2 seconds,
Its resistance change rate is 1.94% after pressing first and discharging, and remains to recoil to original shape after 100 pressings and release, electricity
Resistive rate is 7.6%.
Embodiment 12
By the Cu (NO that 10mL concentration is 0.1mol/L3)2Solution is mixed with the graphene oxide water solution of 5mL concentration 2mg/mL
Close uniform.Then the ethylenediamine solution of 2mL99% is added, after stirring 25min, the NaOH for adding the 10mol/L of 200mL is molten
Liquid simultaneously persistently stirs 50min, the hydrazine hydrate solution of 0.2mL10%, and ultrasound 15min is subsequently adding, subsequently by deionized water
It is cleaned by ultrasonic 10min and the sponge in 60 DEG C of drying is added in reactant liquor, and continue ultrasonically treated 20min, finally, will reacts
System reacts 80min under 70 DEG C of water bath condition, by the product for obtaining in vacuum drying oven drying at room temperature 24h, finally can obtain
To graphene coated copper nano-wire foam.
Its electrical conductivity is 4.2 × 10-2S/m, resilience and can return to the original form after depressed and release in 2 seconds,
Its resistance change rate is 1.73% after pressing first and discharging, and remains to recoil to original shape after 100 pressings and release, electricity
Resistive rate is 9.2%.
Embodiment 13
By the Cu (NO that 30mL concentration is 0.1mol/L3)2Solution and the graphene oxide water solution that 5mL concentration is 5mg/mL
It is well mixed.Then the ethylenediamine solution of 5mL99% is added, after stirring 30min, 600mL concentration is added for 15mol/L's
NaOH solution simultaneously persistently stirs 60min.Finally, the hydrazine hydrate solution of 0.5mL20%, and ultrasound 25min are added, subsequently will be spent
Ionized water is cleaned by ultrasonic 10min and the sponge in 60 DEG C of drying is added in reactant liquor, and continues ultrasonically treated 20min, finally,
Reaction system is reacted into 120min under 90 DEG C of water bath conditions, by the product for obtaining in vacuum drying oven drying at room temperature 24h, finally
Graphene coated copper nano-wire foam is obtained.
Its electrical conductivity is 3.9 × 10-2S/m, resilience and can return to the original form after depressed and release in 2 seconds,
Its resistance change rate is 1.84% after pressing first and discharging, and remains to recoil to original shape after 100 pressings and release, electricity
Resistive rate is 8.64%.
Embodiment 14
By the CuCl that 2mL concentration is 0.5mol/L2Solution mixes with the graphene oxide water solution of 5mL concentration 2mg/mL
It is even.Then the cetylamine solution of 2mL99% is added, after stirring 25min, the Ba (OH) of the 10mol/L of 200mL is added2It is molten
Liquid simultaneously persistently stirs 50min, the catechin solution of 0.2mL35%, and ultrasound 15min is subsequently adding, subsequently by deionized water
It is cleaned by ultrasonic 10min and the aeroge in 60 DEG C of drying is added in reactant liquor, and continues ultrasonically treated 20min, finally, will be anti-
Answer system to react 60min under 100 DEG C of water bath condition, by the product for obtaining in vacuum drying oven drying at room temperature 5d, finally may be used
Obtain graphene coated copper nano-wire foam.
Its electrical conductivity is 2 × 10-2S/m, resilience and can return to the original form after depressed and release in 2 seconds, first
Its resistance change rate is 1.93% after secondary pressing and release, remains to recoil to original shape, resistance after 100 pressings and release
Rate of change is 9.92%.
Embodiment 15
By the CuSO that 5mL concentration is 0.2mol/L4Solution mixes with the graphene oxide water solution of 5mL concentration 2mg/mL
It is even.Then the octadecylamine solution of 2mL99% is added, after stirring 25min, the KOH solution of 10mol/L of 200mL is added simultaneously
50min is persistently stirred, the ascorbic acid solution of 0.2mL35%, and ultrasound 15min is subsequently adding, is subsequently surpassed deionized water
Sound cleans 10min and the porous plastics in 60 DEG C of drying is added in reactant liquor, and continues ultrasonically treated 20min, finally, will be anti-
Answer system to react 40min under 70 DEG C of water bath condition, by the product for obtaining in vacuum drying oven drying at room temperature 1d, finally can obtain
To graphene coated copper nano-wire foam.
Its electrical conductivity is 1.7 × 10-2S/m, resilience and can return to the original form after depressed and release in 2 seconds,
Its resistance change rate is 1.79% after pressing first and discharging, and remains to recoil to original shape after 100 pressings and release, electricity
Resistive rate is 9.76%.
Applicant states that the present invention illustrates the detailed construction feature of the present invention by above-described embodiment, but the present invention is simultaneously
Above-mentioned detailed construction feature is not limited to, that is, does not mean that the present invention has to rely on above-mentioned detailed construction feature and could implement.Institute
Category those skilled in the art are it will be clearly understood that any improvement in the present invention, the equivalence replacement to part selected by the present invention
And increase, the selection of concrete mode of accessory etc., within the scope of all falling within protection scope of the present invention and disclosure.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment
Detail, the present invention range of the technology design in, various simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy is no longer separately illustrated.
Additionally, can also be combined between a variety of embodiments of the present invention, as long as it is without prejudice to this
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (10)
1. a kind of composite elastic body containing graphene coated metal nanometer line, it is characterised in that including porous material and graphite
Alkene coats metal nanometer line；The graphene coated metal nanometer line is grown on the skeleton of the porous material；The porous
Material is the porous material of resiliency.
2. composite elastic body as claimed in claim 1, it is characterised in that the metal is selected from copper and silver；It is preferred that copper.
3. composite elastic body as claimed in claim 1 or 2, it is characterised in that the porous material includes sponge, porous plastics
With any one in aeroge or at least two combination, preferred sponge.
4. the preparation method of the composite elastic body as described in any one of claims 1 to 3, it is characterised in that comprise the steps：
(1) slaine and graphene oxide are scattered in into deionized water, sequentially add covering and alkali, afterwards, stirring is lower to be added
Reducing agent, obtains mixed dispersion liquid；
(2) porous material is added in step (1) mixed dispersion liquid, it is ultrasonically treated, obtain reactant liquor；The porous material
For the porous material of resiliency；
(3) step (2) gained reactant liquor is warming up to into 60～100 DEG C, 30～120min of isothermal reaction, by reacted porous material
Material is washed, is dried, and obtains the composite elastic body containing graphene coated metal nanometer line.
5. preparation method as claimed in claim 4, it is characterised in that the cation of slaine described in step (1) is selected from Ag+
And Cu2+, preferred Cu2+；Counter ion counterionsl gegenions in the slaine are selected from NO3 -、SO4 2-、CH3COO-、Cl-And C6H5O7 3-In it is any
It is a kind of or at least two combination；
Preferably, slaine described in step (1) and the mass ratio of the graphene oxide are (1～120):1, preferably (20～
50):1。
6. the preparation method as described in claim 4 or 5, it is characterised in that covering described in step (1) include ethylenediamine,
Any one in cetylamine and octadecylamine, preferred ethylenediamine；
Preferably, the addition form of covering described in step (1) includes directly adding and/or being dissolved in add after water, preferably
It is dissolved in after water and adds；
Preferably, the slaine and the mass ratio of the covering are 1:(2～20), preferably 1:(5～15)；
Preferably, alkali described in step (1) includes any one in barium hydroxide, NaOH and potassium hydroxide or at least two
The combination planted, preferred NaOH and/or potassium hydroxide；
Preferably, the addition form of alkali described in step (1) includes directly adding and/or being dissolved in add after water, preferred dissolving
Add after water；
Preferably, the slaine and the mass ratio of the alkali are 1:(200～800), preferably 1:(250～500).
7. the preparation method as described in any one of claim 4～6, it is characterised in that reducing agent described in step (1) includes water
Close in hydrazine, catechin, ascorbic acid, sodium borohydride, citric acid and sodium hypophosphite any one or at least two combination, it is excellent
Select hydrazine hydrate and/or catechin；
Preferably, the addition form of reducing agent described in step (1) includes directly adding and/or being dissolved in add after water, preferably
It is dissolved in after water and adds；
Preferably, the mass ratio (1～10) of the slaine and the reducing agent:1, preferably (1～4):1；
Preferably, described in step (1) in mixed dispersion liquid metal salt concentrations be 0.05～0.5mol/L, preferably 0.05～
0.2mol/L。
8. the preparation method as described in any one of claim 4～7, it is characterised in that the porous material mixes point with described
The volume ratio of dispersion liquid is 1:(5～50), preferably 1:(8～15)；
Preferably, ultrasound is described in step (2)：10～60min of ultrasound under 20kHz～100kHz, ultrasound 15 under preferred 50kHz
～30min.
9. the preparation method as described in any one of claim 4～8, it is characterised in that heating up described in step (3) includes water-bath
Heat up；
Preferably, reaction temperature described in step (3) is 70～80 DEG C, and the reaction time is 40～60min；
Preferably, washing described in step (3) include for the reacted porous material soaking 0.5 in deionized water～
5h；
Preferably, drying includes vacuum drying and/or freeze-drying described in step (3)；
Preferably, the drying is included in vacuum oven and processes 1～5d.
10. as described in any one of claims 1 to 3 composite elastic body in flexible electronic device, sensor, ultracapacitor, water
Application in process.
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