CN104988475A - Copper-nickel alloy nanowire flexible electrode and preparation method thereof - Google Patents
Copper-nickel alloy nanowire flexible electrode and preparation method thereof Download PDFInfo
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- CN104988475A CN104988475A CN201510299607.9A CN201510299607A CN104988475A CN 104988475 A CN104988475 A CN 104988475A CN 201510299607 A CN201510299607 A CN 201510299607A CN 104988475 A CN104988475 A CN 104988475A
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Abstract
The invention discloses a copper-nickel alloy nanowire flexible electrode and a preparation method thereof. A certain quantity of copper-nickel alloy nanowires are scattered in a certain amount of a normal hexane solution; the copper-nickel alloy nanowires are used to form films on filtering films with an extraction filtration method; then the formed films are transferred to a prepared PDMS (polydimethylsiloxane) flexible substrate; the nanowires are embedded in the surface of the flexible substrate by certain pressure; and then under the condition of a reducing atmosphere, the flexible substrate is heated to a certain temperature for a certain period of time, so that the copper-nickel alloy nanowire flexible electrode of high quality is obtained. According to the copper-nickel alloy nanowire flexible electrode and the preparation method thereof, the operation process is simple, and the prepared flexible electrode has excellent electrical conductivity, stretchability, bendability and stability.
Description
Technical field
The present invention relates to flexible electrode technology of preparing, particularly relate to one and can be applicable to flexible screen, cupronickel nano wire flexible electrode of wearable electronic product and Organic Light Emitting Diode and preparation method thereof.
Background technology
Along with the development of modern display technology, flexible device more and more receives the concern of people.In the fields such as wearable electronic product and flexible screen, the electrode that flexible extensible bends has huge application potential undoubtedly.In traditional field of electronic devices, electrode in business is attached to rigid substrate often (as glass, silicon etc.) on, such as more modal circuit cards, electrode of solar battery etc., these rigid substrate electrode major advantages are technical maturities, and yield rate is high, can meet general device to electrode requirement.But along with people are on the increase the demand of various novel electron consuming product, these novel electron devices are often required to meet ergonomics, as the rise of wearable electronic product in recent years, as intelligent watch etc.This requires us to develop to have flexible electron device, as flexible PCB, and flexible screen etc.And flexible device will be realized, preparing flexible electrode substrate is an indispensable ring.
The flexible electrode material mainly used at present has Ag nano wire (Transferable self-welding silvernanowire network as high performance transparent flexible electrode.Nanotechnology, 2013,24 (33): 335202.), business-like ITO/PET electrode etc.To a certain extent, these flexible electrodes can meet the demand of current photoelectric device to flexible electrode substrate, and preparation technology is comparatively ripe.But the subject matter existed is that these electrodes material price used is more expensive, and as the indium in Ag, ITO, and ITO/PET electrode has larger fragility, should not be used for requiring, in higher flexible substrate, to which limits its range of application to bendability or stretchiness.
Ordinary copper nano wire (Transparent Cu nanowire mesh electrode on flexible substratesfabricated by transfer printing and its application in organic solar cells [J] .Solar EnergyMaterials and Solar Cells, 2010,94 (6): 1179-1184.) flexible electrical prepared is very easily oxidized, makes the resistivity of flexible electrode become large; And flexible electrode and flexible substrate in conjunction with bad, bending, stretch after conductive capability greatly reduce, performance is very unstable.
Summary of the invention
The object of this invention is to provide a kind of cupronickel nano wire flexible electrode and preparation method thereof.
The technical scheme realizing the object of the invention is: a kind of cupronickel nano wire flexible electrode and preparation method thereof, a certain amount of cupronickel nano wire is dispersed in appropriate hexane solution, cupronickel nano wire film forming on filter membrane is made by the method for suction filtration, again it is transferred in the PDMS flexible substrate of preparation, utilize certain pressure that nano wire is embedded in flexible substrate surface, then by being heated to certain temperature and keeping for some time under reducing atmosphere condition, thus high-quality cupronickel nano wire flexible extensible electrode is obtained.Concrete preparation process is as follows:
Step 1, with CuCl
2as the precursors of cupric ion, Ni (acac)
2as reductive agent, molar ratio computing, CuCl
2: Ni (acac)
2=2:1, oleyl amine is as solvent;
Step 2, at N
2under inert atmosphere, step 1 reagent is placed in container, insulated and stirred at being heated to 90-100 DEG C, precursor salt is fully mixed;
Step 3, continues to be warmed up to 175-185 DEG C, and after the reaction 3.5-4.5h time, cooling, centrifugal treating, obtain cupronickel nano wire after cleaning;
Step 4, is dispersed in normal hexane by cupronickel nano wire, by ultrasonic for this dispersion liquid rear suction filtration on filter membrane;
Step 5, takes off filter membrane and is attached to PDMS flexible substrate surface, apply 10 ~ 15N pressure, cupronickel nano wire is transferred to substrate surface;
Step 6, is heated to 200-210 DEG C by the flexible electrode substrate shifted and is incubated 2.5-3h, taking out after cool to room temperature under reducing atmosphere, obtains cupronickel nano wire flexible electrode.
In step 2, the described insulated and stirred time is 30-40min.
In step 4, the concentration of dispersion liquid is 0.02 ~ 0.08mg/ml; Ultrasonic time is 1 ~ 3 minute.
In step 6, reducing atmosphere is 5%H
2the hydrogen argon atmospher of+95%Ar.
The advantage that the present invention has is as follows: 1) preparation technology of the present invention is simply controlled, copper nano-wire is transferred to the convenient easily manipulation of flexible substrate; 2) the cupronickel nano wire used in the present invention is cheap, and nontoxicity, more environmental protection, the most important thing is that the flexible electrode product obtained is suitable with commercial product performance, meet the requirement of device to flexible electrode completely; 3) the present invention is by utilizing the method being embedded in PDMS surface, cupronickel nano wire is protected further, extends its work-ing life.
Accompanying drawing explanation
Fig. 1 is that the cupronickel nano wire shell structure TEM of example 1 of the present invention schemes.
Fig. 2 is the flexible electrode sample of example 1 gained of the present invention.
Fig. 3 is the flexible electrode square resistance change curve in time of example 1 gained of the present invention.
Fig. 4 is the flexible electrode sample of example 2 gained of the present invention.
Fig. 5 is the flexible electrode square resistance change curve in time of example 2 gained of the present invention.
Fig. 6 is the flexible electrode sample of invention example 3 gained.
Fig. 7 is the flexible electrode sample of example 3 gained of the present invention.
Specific implementation method
A kind of cupronickel nano wire of the present invention flexible electrode, that cupronickel nanowire dispersion is made its film forming on filter membrane by the method for suction filtration, again it is transferred in the PDMS flexible substrate of preparation, utilize certain pressure that nano wire is embedded in flexible substrate surface, then by being heated to certain temperature and keeping for some time under reducing atmosphere condition, thus high-quality cupronickel nano wire flexible extensible electrode is obtained.Specifically comprise the following steps:
Step 1: get certain proportion silicone resin solution and solidifying agent mix and blend, makes it be solidified into the PDMS substrate of diameter 40cm;
Step 2: get 3mL0.02 ~ 0.08mg/ml cupronickel nano wire and be dispersed in appropriate normal hexane, evenly ultrasonic;
Step 3: by the method for suction filtration by cupronickel nano wire equably suction filtration on filter membrane;
Step 4: undried filter membrane is taken off and is attached to PDMS flexible substrate surface, by the pressure of 10 ~ 15N, cupronickel nano wire is transferred to substrate surface;
Step 5: the flexible electrode substrate shifted is put into reducing atmosphere and to heat and cool to room temperature takes out after being incubated for some time, namely obtain cupronickel nano wire flexible extensible electrode.
In step 1, the preparation technology of PDMS flexible substrate is: get silicone resin solution and solidifying agent ratio 10:1, at room temperature through solidification in 18 ~ 20 hours after mixing and stirring, to obtain final product.
In step 2, the preparation technology of cupronickel nano wire is: CuCl
2with Ni (acac)
2routine 2:1 mixing, is dissolved in oleyl amine, at N in molar ratio
2under inert atmosphere, insulated and stirred 30-40min at being heated to 90-100 DEG C, makes it fully mix; Continue to be warmed up to 175-185 DEG C, reaction the 3.5-4.5h time after, cooling, centrifugal, namely obtain cupronickel nano wire after cleaning.Be dissolved in normal hexane, the cupronickel nano wire ink of preparation different concns.
Embodiment 1
A kind of cupronickel nano wire of the present invention flexible extensible electrode, concrete preparation process is as follows:
Step 1: get silicone resin solution and solidifying agent ratio 10:1, was at room temperature solidified into required PDMS substrate through 18 hours after mixing and stirring;
Step 2: configuration solubility is the cupronickel nanowire dispersion of 0.02mg/mL, makes it be uniformly dispersed in ultrasonic 1 minute for subsequent use;
Step 3: get 3mL cupronickel nanowire dispersion and be evenly distributed on vinyl acetate between to for plastic filter membrane surface by the method for vacuum filtration;
Step 4: undried filter membrane is taken off and is attached to PDMS flexible substrate surface, take filter membrane away after utilizing 10N pressure gently to press 10s, shift successfully;
Step 5: the flexible electrode substrate shifted is put into reducing atmosphere (5%H
2+ 95%Ar) vacuum oven in anneal, annealing temperature is 200 DEG C, through 2 hours insulation after take out naturally cooling, namely obtain cupronickel nano wire flexible extensible electrode.
Under air at room temperature environment, carry out performance characterization to obtained flexible electrode, as shown in Figure 1,2 and 3, result shows the processing parameter according to example 1, and obtained flexible electrode has good light transmission rate, conductivity and stability.
Embodiment 2
A kind of cupronickel nano wire of the present invention flexible extensible electrode, concrete preparation process is as follows:
Step 1: get silicone resin solution and solidifying agent ratio 10:1, was at room temperature solidified into required PDMS substrate through 19 hours after mixing and stirring;
Step 2: configuration solubility is the cupronickel nanowire dispersion of 0.04mg/mL, makes it be uniformly dispersed in ultrasonic 2 minutes for subsequent use;
Step 3: get 3mL cupronickel nanowire dispersion and be evenly distributed on vinyl acetate between to for plastic filter membrane surface by the method for vacuum filtration;
Step 4: with sharp tweezers undried filter membrane taken off and be attached to PDMS flexible substrate surface, take filter membrane away after utilizing 12N pressure to suppress 10s, shift successfully;
Step 5: the flexible electrode substrate shifted is put into reducing atmosphere (5%H
2+ 95%Ar) vacuum oven in anneal, annealing temperature is 200 DEG C, through 2 hours insulation after take out naturally cooling, namely obtain cupronickel nano wire flexible extensible electrode.
Under air at room temperature condition, carry out performance test chart to obtained flexible electrode to levy, as shown in Figure 4 and Figure 5, result shows the processing parameter according to example 2, and obtained flexible electrode has good light transmission rate, conductivity and stability.
Embodiment 3
A kind of cupronickel nano wire of the present invention flexible extensible electrode, concrete preparation process is as follows:
Step 1: get silicone resin solution and solidifying agent ratio 10:1, was at room temperature solidified into required PDMS substrate through 20 hours after mixing and stirring;
Step 2: configuration solubility is the cupronickel nanowire dispersion of 0.08mg/mL, makes it be uniformly dispersed in ultrasonic 3 minutes for subsequent use;
Step 3: get 3mL cupronickel nanowire dispersion and be evenly distributed on vinyl acetate between to for plastic filter membrane surface by the method for vacuum filtration;
Step 4: taken off by undried filter membrane and be attached to PDMS flexible substrate surface, takes filter membrane away after utilizing the weight pressure of 15N to suppress 10s, shifts successfully;
Step 5: the flexible electrode substrate shifted is put into reducing atmosphere (5%H
2+ 95%Ar) vacuum oven in anneal, annealing temperature is 200 DEG C, through 2 hours insulation after take out naturally cooling, namely obtain cupronickel nano wire flexible extensible electrode.
Under air at room temperature condition, carry out performance characterization to obtained flexible electrode, as shown in Figure 6 and Figure 7, result shows the processing parameter according to example 3, and obtained flexible electrode has good light transmission rate, conductivity and stability.
Claims (8)
1. a cupronickel nano wire flexible electrode, is characterized in that, described electrode is prepared by following steps:
Step 1, with CuCl
2as the precursors of cupric ion, Ni (acac)
2as reductive agent, molar ratio computing, CuCl
2: Ni (acac)
2=2:1, oleyl amine is as solvent;
Step 2, at N
2under inert atmosphere, step 1 reagent is placed in container, insulated and stirred at being heated to 90-100 DEG C, precursor salt is fully mixed;
Step 3, continues to be warmed up to 175-185 DEG C, and after the reaction 3.5-4.5h time, cooling, centrifugal treating, obtain cupronickel nano wire after cleaning;
Step 4, is dispersed in normal hexane by cupronickel nano wire, by ultrasonic for this dispersion liquid rear suction filtration on filter membrane;
Step 5, takes off filter membrane and is attached to PDMS flexible substrate surface, apply 10 ~ 15N pressure, cupronickel nano wire is transferred to substrate surface;
Step 6, is heated to 200-210 DEG C by the flexible electrode substrate shifted and is incubated 2.5-3h, taking out after cool to room temperature under reducing atmosphere, obtains cupronickel nano wire flexible electrode.
2. cupronickel nano wire flexible electrode as claimed in claim 1, it is characterized in that, in step 2, the described insulated and stirred time is 30-40min.
3. cupronickel nano wire flexible electrode as claimed in claim 1, it is characterized in that, in step 4, the concentration of dispersion liquid is 0.02 ~ 0.08mg/ml; Ultrasonic time is 1 ~ 3 minute.
4. cupronickel nano wire flexible electrode as claimed in claim 1, it is characterized in that, in step 6, reducing atmosphere is 5%H
2the hydrogen argon atmospher of+95%Ar.
5. a preparation method for cupronickel nano wire flexible electrode, is characterized in that, comprises the following steps:
Step 1, with CuCl
2as the precursors of cupric ion, Ni (acac)
2as reductive agent, molar ratio computing, CuCl
2: Ni (acac)
2=2:1, oleyl amine is as solvent;
Step 2, at N
2under inert atmosphere, step 1 reagent is placed in container, insulated and stirred at being heated to 90-100 DEG C, precursor salt is fully mixed;
Step 3, continues to be warmed up to 175-185 DEG C, and after the reaction 3.5-4.5h time, cooling, centrifugal treating, obtain cupronickel nano wire after cleaning;
Step 4, is dispersed in normal hexane by cupronickel nano wire, by ultrasonic for this dispersion liquid rear suction filtration on filter membrane;
Step 5, takes off filter membrane and is attached to PDMS flexible substrate surface, apply 10 ~ 15N pressure, cupronickel nano wire is transferred to substrate surface;
Step 6, is heated to 200-210 DEG C by the flexible electrode substrate shifted and is incubated 2.5-3h, taking out after cool to room temperature under reducing atmosphere, obtains cupronickel nano wire flexible electrode.
6. the preparation method of cupronickel nano wire flexible electrode as claimed in claim 5, it is characterized in that, in step 2, the described insulated and stirred time is 30-40min.
7. the preparation method of cupronickel nano wire flexible electrode as claimed in claim 5, it is characterized in that, in step 4, the concentration of dispersion liquid is 0.02 ~ 0.08mg/ml; Ultrasonic time is 1 ~ 3 minute.
8. the preparation method of cupronickel nano wire flexible electrode as claimed in claim 5, it is characterized in that, in step 6, reducing atmosphere is 5%H
2the hydrogen argon atmospher of+95%Ar.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105758909A (en) * | 2016-02-26 | 2016-07-13 | 武汉大学 | Gold nanotube based flexible stretchable electrode and preparation method and application thereof |
| CN106521551A (en) * | 2016-11-01 | 2017-03-22 | 电子科技大学 | Preparation method for NiAu nano catalyst used for ammonia borane hydrogen-production |
| CN108355661A (en) * | 2018-01-03 | 2018-08-03 | 东南大学 | A kind of threadiness Cu-Ni alloy nanometer crystals and its synthetic method |
| CN109727706A (en) * | 2019-03-08 | 2019-05-07 | 华南协同创新研究院 | A kind of flexible transparent conductive film and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105758909A (en) * | 2016-02-26 | 2016-07-13 | 武汉大学 | Gold nanotube based flexible stretchable electrode and preparation method and application thereof |
| CN105758909B (en) * | 2016-02-26 | 2018-06-19 | 武汉大学 | A kind of flexible extensible electrode based on gold nanotubes and preparation method and application |
| CN106521551A (en) * | 2016-11-01 | 2017-03-22 | 电子科技大学 | Preparation method for NiAu nano catalyst used for ammonia borane hydrogen-production |
| CN106521551B (en) * | 2016-11-01 | 2019-05-14 | 电子科技大学 | A kind of preparation method of the NiAu nanocatalyst for ammonia borane hydrogen manufacturing |
| CN108355661A (en) * | 2018-01-03 | 2018-08-03 | 东南大学 | A kind of threadiness Cu-Ni alloy nanometer crystals and its synthetic method |
| CN109727706A (en) * | 2019-03-08 | 2019-05-07 | 华南协同创新研究院 | A kind of flexible transparent conductive film and preparation method thereof |
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Application publication date: 20151021 |