CN108982632A - A kind of flexible electrode and preparation method thereof based on flower-like nanometer gold structure - Google Patents
A kind of flexible electrode and preparation method thereof based on flower-like nanometer gold structure Download PDFInfo
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- CN108982632A CN108982632A CN201810830539.8A CN201810830539A CN108982632A CN 108982632 A CN108982632 A CN 108982632A CN 201810830539 A CN201810830539 A CN 201810830539A CN 108982632 A CN108982632 A CN 108982632A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/36—Glass electrodes
Abstract
The present invention relates to a kind of flexible electrode and preparation method thereof based on flower-like nanometer gold structure, belongs to technical field of electronic materials.Main technical schemes are as follows: by ito glass LBL self-assembly, carrying out electrochemical deposition gold using chrono-amperometric method on assembled ito glass, after electrochemical deposition, one layer of golden yellow flower-like nanometer gold will be deposited on ito glass, be called ITO-Au.Electrolyte used is KAuCl4And H2SO4Mixed solution, reference electrode are Ag/AgCl electrode, are platinum filament to electrode, and working electrode is assembled ito glass；Ito glass is cleaned before assembly.Cleaning process is to clean ito glass with deionized water, acetone and EtOH Sonicate respectively.Flexible electrode prepared by the present invention has lower sheet resistance, and repeatedly and after stretching repeatedly still is able to maintain good electric conductivity in bending.
Description
Technical field
The present invention relates to technical field of electronic materials, and in particular to a kind of flexible electrode based on flower-like nanometer gold structure and
Preparation method.
Background technique
With the development of electronic information technology, electronic equipment and electronic device are towards integrated, lighting, micromation
Develop with directions such as flexibilities.In order to meet the growth requirement of electronic technology, prepare with flexible and stretchable function new
Type electrode is necessary.Traditionally the conduction of electronic component often is realized mutually by conductor of brazing metals such as tin-lead copper
Even, but with the demands such as electronic device lighting and flexibility and unleaded environmental requirement, brazing metal is due to processing temperature
The disadvantages of degree is high, hardness is big, lead contamination is difficult to meet the manufacture craft requirement of modern flexible electronic equipment.Therefore, flexible electrode
Research and development and application have become current research hotspot.Now, main problem existing for most of flexible electrodes is mechanical performance
(bending resistance, stretch-resistance) and electric conductivity are bad.The key for preparing flexible conducting material is conductive component and flexibility
Polymeric matrix be effectively combined, make finally obtained material in the case where multiple bending or multi-drawing, electric property
Be not in fatigue or be remarkably decreased.
In recent years, carbon nanotube, graphene, conductive polymer material and metal nano material are used as flexibility in succession and lead
The preparation of electric material, and be applied in a variety of electronic equipments flexible.Wherein, the nanogold nano material novel as one kind,
Excellent flexibility and have high conductivity, makes it that there is very wide application prospect in the preparation of flexible conducting material.
However also there is the problems such as bending resistance and poor stretch-resistance in the flexible conducting material based on nanogold, limit the extensive of them
Using.
Summary of the invention
In order to solve the above technical problems, the purpose of the present invention is to provide one kind have both superior electrical conductivity, stretch-resistance and
The flexible electrode and preparation method thereof based on flower-like nanometer gold structure of bending resistance.The method that this method passes through electrochemical deposition
Go out one layer of nanogold with floriform appearance structure in tin indium oxide (ITO) deposition on glass by modification, and this layer is received
The golden conductive layer of rice is solidificated in PDMS flexible substrates, prepares the novel flexible electrode with flower-like structure nanogold.It is such soft
Property electrode have lower sheet resistance, and bending repeatedly and stretch repeatedly after be still able to maintain good electric conductivity.
To achieve the above object, flexible electrode of the present invention is the nanometer of embedding attached one layer of flower-like structure in PDMS flexible substrates
Golden conductive layer.
The flexible electrode the preparation method is as follows:
(1) by ito glass LBL self-assembly, electrochemistry is carried out using chrono-amperometric method on assembled ito glass
Deposition gold, after electrochemical deposition, one golden layer flower-like nanometer gold will be deposited on ito glass, be called ITO-Au.It is used
Electrolyte is KAuCl4And H2SO4Mixed solution, reference electrode are Ag/AgCl electrode, are platinum filament to electrode, working electrode is group
The ito glass installed；
Ito glass is cleaned before assembly.Cleaning process is that ito glass is used to deionized water, acetone respectively
It is cleaned 20~40 minutes with EtOH Sonicate.It is put into after cleaning in ozone clean machine and carries out surface hydroxylation.Then again by ito glass
LBL self-assembly is carried out in PDDA (diallyl dimethyl ammoniumchloride) and PSS (kayexalate) solution.
(2) ITO-Au is immersed in the PDMS with curing agent (dimethyl silicone polymer) solution, is heating and curing, will solidifies
Good PDMS flexible substrates are taken off from ITO-Au, and golden yellow flower-like nanometer gold is attached in PDMS flexible substrates, is as based on
The flexible electrode PDMS-Au of flower-like nanometer gold structure.
Preferably, the self assembly number of plies is 6~10 layers in the step (1).
Since the deposition morphology of nanogold and the concentration of sedimentation potential, sedimentation time and electrolyte are closely related, it needs
Comprehensively consider these because usually control nanogold electrode floriform appearance.Preferably, in the step (1) when electrochemical deposition
Between be 400~1200s, the potential range that electrochemical deposition is set is (- 0.2)~(- 0.3) V.
It is finer and close that suitable concentration of electrolyte can be such that gold deposits, while also the nanogold peeled can be made more to add
It is whole, it is preferred that KAuCl in the step (1)4(0.01~0.05mol/L) and H2SO4(0.1~0.5mol/L).
Preferably, PDMS stoste and the volume ratio of curing agent are 10:1 in the step (2).
It is stronger that suitable solidification temperature and time can allow nanogold and PDMS to combine, it is preferred that the solidification temperature
Degree is 50~100 DEG C, and curing time is 2~10 hours.
Compared with prior art, the invention has the following advantages: that the present invention provides a kind of electric conductivities is excellent, anti-
Draftability and bending resistance be good, Portable durable flexible electrode.The technology for preparing electrode is simple, easily realization volume production.The present invention
Key point be the electrochemical deposition on ito glass have flower-like structure nanogold.Nanometer golden flower has clusters
Tendency, causes adjacent several cluster spacing smaller, is conducive to the transmission of electronics, and then reduce electrode resistance.Good electric conductivity
It can be the guarantee for preparing highly sensitive electrochemical sensor.And the electrochemical deposition for the preparation nanogold conductive layer that the present invention uses
Method, sharpest edges are simple and easy, reproducible, do not need to be synthetically prepared, and overcome in synthesis and separation nanogold
The difficulty encountered, while can solve nanogold electrode caducous problem of gold in Electrochemical Detection.
Detailed description of the invention
Fig. 1 is process flow chart of the invention；
Fig. 2 is the SEM image for the flexible electrode nano surface gold conductive layer that the present invention prepares；
Fig. 3 is flexible electrode resistance to bend(ing) experimental test result of the embodiment of the present invention；
Fig. 4 is flexible electrode stretch-resistance experimental test result of the embodiment of the present invention；
Fig. 5 is flexible circuit figure of the present invention using the flexible conducting material design prepared.
Specific embodiment
Further description of the technical solution of the present invention in the following with reference to the drawings and specific embodiments, but the present invention not with
Any form constrained is in embodiment content.Experimental method described in embodiment is conventional method unless otherwise specified；Such as without spy
Different explanation, the experiment reagent and material, commercially obtain.
Embodiment 1
(1) it is cleaned by ultrasonic ito glass with dehydrated alcohol, then is placed in UV ozone cleaning machine 30 minutes, it then will cleaning
The conduction of good ITO is placed up, is put into the PDDA solution of 5mg/mL and is impregnated 5min, a small amount of using distilled water after taking-up
It is repeatedly cleaned, then using being dried with nitrogen.
(2) same step is used, PSS assembling is carried out to the ito glass for being assembled with PDDA layers.After the completion, one can be made
Layer (PDDA/PSS) Iy self-assembled layer.Above-mentioned process 6 times are repeated, can prepare and have (PDDA/PSS)6Multilayer self-assembled film
Ito glass.Finally it is encapsulated in culture dish for use with nitrogen.
(3) flower-like nanometer gold will be deposited on assembled ito glass, used method is chronoamperometry, reference electricity
Extremely Ag/AgCl electrode is platinum filament to electrode, and working electrode is assembled ito glass, and electrolyte is by KAuCl4
(0.01mol/L) and H2SO4(0.5mol/L) mixed liquor.Using chronoamperometry, fixed deposition voltage is -0.3V, using 400s
Sedimentation time, carry out nanogold deposition.By electrochemical deposition, one layer of golden yellow nanometer is prepared on ito glass surface
Golden conductive layer, by scanning electron microscope it can be observed that its flower-shaped microscopic appearance structure.
By in the ito glass merging PDMS solution after deposition gold, it is put into baking oven and solidifies, solidification temperature is 60 DEG C, solidification
Time is 10 hours.The PDMS being cured is taken off from ito glass, flower-like nanometer gold thin film can be fixed on PDMS substrate
On, the flower-like structure of PDMS nano surface gold conductive layer can be observed by scanning mirror.It is obtained to have flower-like structure nanometer
The PDMS film of gold can be used as required based on flower-like structure nanogold flexible electrode.
Embodiment 2
(1) it is cleaned by ultrasonic ito glass with dehydrated alcohol, then is placed in UV ozone cleaning machine 30 minutes, it then will cleaning
The conduction of good ITO is placed up, is put into the PDDA solution of 5mg/mL and is impregnated 5min, a small amount of using distilled water after taking-up
It is repeatedly cleaned, then using being dried with nitrogen.
(2) same step is used, PSS assembling is carried out to the ito glass for being assembled with PDDA layers.After the completion, one can be made
Layer (PDDA/PSS) Iy self-assembled layer.Above-mentioned process 6 times are repeated, can prepare and have (PDDA/PSS)6Multilayer self-assembled film
Ito glass is finally encapsulated in culture dish for use with nitrogen.
Flower-like nanometer gold will be deposited on assembled ito glass, used method is chronoamperometry, and reference electrode is
Ag/AgCl electrode, is platinum filament to electrode, and working electrode is assembled ito glass, electrolyte KAuCl4(0.01mol/L)
And H2SO4(0.5mol/L) mixed solution, sets current potential as -0.3V, sedimentation time 800s.
By in the ito glass merging PDMS solution after deposition gold, it is put into baking oven and solidifies, solidification temperature is 60 DEG C, solidification
Time is 5 hours.The PDMS being cured is taken off from ito glass can be fixed in PDMS substrate from, flower-like nanometer gold thin film,
PDMS film obtained with flower-like structure nanogold is as based on flower-like structure nanogold flexible electrode.
Embodiment 3
(1) it is cleaned by ultrasonic ito glass with dehydrated alcohol, then is placed in UV ozone cleaning machine 30 minutes, it then will cleaning
The conduction of good ITO is placed up, is put into the PDDA solution of 5mg/mL and is impregnated 5min, a small amount of using distilled water after taking-up
It is repeatedly cleaned, then using being dried with nitrogen.
(2) same step is used, PSS assembling is carried out to the ito glass for being assembled with PDDA layers.After the completion, one can be made
Layer (PDDA/PSS) Iy self-assembled layer.Above-mentioned process 6 times are repeated, can prepare and have (PDDA/PSS)6Multilayer self-assembled film
Ito glass is finally encapsulated in culture dish for use with nitrogen.
Flower-like nanometer gold will be deposited on assembled ito glass, used method is chronoamperometry, and reference electrode is
Ag/AgCl electrode, is platinum filament to electrode, and working electrode is assembled ito glass, electrolyte KAuCl4(0.01mol/L)
And H2SO4(0.5mol/L) mixed solution, sets current potential as -0.3V, sedimentation time 1200s.
By in the ito glass merging PDMS solution after deposition gold, it is put into baking oven and solidifies, solidification temperature is 70 DEG C, solidification
Time is 8 hours.The PDMS being cured to be taken off from ito glass, flower-like nanometer gold thin film can be fixed in PDMS substrate,
PDMS film obtained with flower-like structure nanogold can be used as required based on flower-like structure nanogold flexible electrical
Pole.
Embodiment 4
(1) it is cleaned by ultrasonic ito glass with dehydrated alcohol, then is placed in UV ozone cleaning machine 30 minutes, it then will cleaning
The conduction of good ITO is placed up, is put into the PDDA solution of 10mg/mL and is impregnated 5min, a small amount of using distilled water after taking-up
It is repeatedly cleaned, then using being dried with nitrogen.
(2) same step is used, PSS assembling is carried out to the ito glass for being assembled with PDDA layers.After the completion, one can be made
Layer (PDDA/PSS) Iy self-assembled layer.Above-mentioned process 8 times are repeated, can prepare and have (PDDA/PSS)8Multilayer self-assembled film
Ito glass is finally encapsulated in culture dish for use with nitrogen.
Flower-like nanometer gold will be deposited on assembled ito glass, used method is chronoamperometry, and reference electrode is
Ag/AgCl electrode, is platinum filament to electrode, and working electrode is assembled ito glass, electrolyte KAuCl4(5mmol/L) and
H2SO4(0.2mol/L) mixed solution, sets current potential as -0.2V, sedimentation time 800s.
By in the ito glass merging PDMS solution after deposition gold, it is put into baking oven and solidifies, solidification temperature is 80 DEG C, solidification
Time is 8 hours.The PDMS being cured to be taken off from ito glass, flower-like nanometer gold thin film can be fixed in PDMS substrate,
PDMS film obtained with flower-like structure nanogold can be used as required based on flower-like structure nanogold flexible electrical
Pole.
Embodiment 5
(1) it is cleaned by ultrasonic ito glass with dehydrated alcohol, then is placed in UV ozone cleaning machine 30 minutes, it then will cleaning
The conduction of good ITO is placed up, is put into the PDDA solution of 10mg/mL and is impregnated 5min, a small amount of using distilled water after taking-up
It is repeatedly cleaned, then using being dried with nitrogen.
(2) same step is used, PSS assembling is carried out to the ito glass for being assembled with PDDA layers.After the completion, one can be made
Layer (PDDA/PSS) Iy self-assembled layer.Above-mentioned process 10 times are repeated, can prepare and have (PDDA/PSS)10Multilayer self-assembled film
Ito glass is finally encapsulated in culture dish for use with nitrogen.
Flower-like nanometer gold will be deposited on assembled ito glass, used method is chronoamperometry, and reference electrode is
Ag/AgCl electrode, is platinum filament to electrode, and working electrode is assembled ito glass, electrolyte KAuCl4(0.01mol/L)
And H2SO4(0.5mol/L) mixed solution, sets current potential as -0.3V, sedimentation time 800s.
By in the ito glass merging PDMS solution after deposition gold, it is put into baking oven and solidifies, solidification temperature is 50 DEG C, solidification
Time is 10 hours.The PDMS being cured is taken off from ito glass, flower-like nanometer gold thin film can be fixed on PDMS substrate
On, the PDMS film obtained with flower-like structure nanogold can be used as required flexible based on flower-like structure nanogold
Electrode.
The obtained sample of embodiment 1-5 is tested for the property, by test, the electric conductivity of embodiment 1-3 sample, bending
Parameter such as table 1, Fig. 3 and Fig. 4 of property and draftability.
Table 1: the electric conductivity of flexible electrode
| Sample | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Sheet resistance (ohm/sq) | 9.758 | 9.080 | 4.822 | 4.564 | 3.942 |
The data from table 1 are it is found that the square resistance of the flexible electrode reduces with the increase for depositing the golden time.Fig. 3 is
The variation of resistance after resistance to 300 bendings of flexible electrode, Fig. 4 are the variation of resistance after stretching for flexible electrode resistance to 200 times, from Fig. 3 and
Fig. 4 can be seen that the flexible electrode bending resistance and stretch-resistance are promoted also with the increase of sedimentation time.Fig. 5 is with system
The circuit diagram of standby flexible conducting material design out, as can be seen from the figure the conductive material is in the case where bending, electric conductivity
It is still good.
The above description is only an embodiment of the present invention, all equivalent changes done according to scope of the present invention patent with repair
Decorations, are all covered by the present invention.
Claims (7)
1. a kind of flexible electrode based on flower-like nanometer gold structure, which is characterized in that the flexible electrode includes flexible substrates PDMS
And its embedding attached nanogold conductive layer with flower-like structure in surface.
2. the preparation method of flexible electrode according to claim 1, which comprises the following steps:
(1) by ito glass LBL self-assembly, electrochemical deposition gold is carried out on assembled ito glass, obtains ITO-Au；Institute
It is KAuCl with electrolyte4And H2SO4Mixed solution, reference electrode are Ag/AgCl electrode, are platinum filament to electrode, working electrode is
Assembled ito glass；
(2) ITO-Au is immersed in the PDMS solution containing curing agent, is heating and curing, by the PDMS flexible substrates being cured from
It is taken off on ITO-Au, obtaining PDMS-Au is the flexible electrode based on flower-like nanometer gold structure.
3. preparation method according to claim 2, which is characterized in that the self assembly number of plies is 6~10 in the step (1)
Layer.
4. preparation method according to claim 2, which is characterized in that the electrochemical deposition time is 400 in the step (1)
~1200s, the potential range that electrochemical deposition is set is (- 0.2)~(- 0.3) V.
5. preparation method according to claim 2, which is characterized in that KAuCl in the step (1)4Concentration be 0.01~
0.05mol/L, H2SO4Concentration is 0.1~0.5mol/L.
6. preparation method according to claim 2, which is characterized in that PDMS stoste and curing agent in the step (2)
Volume ratio is 10:1.
7. preparation method according to claim 2, which is characterized in that solidification temperature described in the step (2) be 50~
100 DEG C, curing time is 2~10 hours.
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Cited By (6)
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| CN110600608A (en) * | 2019-09-18 | 2019-12-20 | 东北师范大学 | Flexible transparent electrode and preparation method and application thereof |
| CN112864404A (en) * | 2019-11-28 | 2021-05-28 | 大连大学 | Three-dimensional flower-shaped gold-nickel-platinum modified nano composite electrode |
| CN112979180A (en) * | 2019-12-16 | 2021-06-18 | 大连大学 | ITO glass processing method and application thereof |
| CN113036164A (en) * | 2019-12-24 | 2021-06-25 | 大连大学 | Preparation method and application of composite electrode based on mesoporous carbon foam |
| CN113130917A (en) * | 2019-12-31 | 2021-07-16 | 大连大学 | Construction method of electrocatalytic oxidation ethanol fuel cell |
| CN113417157A (en) * | 2021-06-18 | 2021-09-21 | 广东省科学院微生物研究所(广东省微生物分析检测中心) | Super-washable dual-function wearable electronic fabric and preparation method thereof |
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| CN113036164A (en) * | 2019-12-24 | 2021-06-25 | 大连大学 | Preparation method and application of composite electrode based on mesoporous carbon foam |
| CN113130917A (en) * | 2019-12-31 | 2021-07-16 | 大连大学 | Construction method of electrocatalytic oxidation ethanol fuel cell |
| CN113417157A (en) * | 2021-06-18 | 2021-09-21 | 广东省科学院微生物研究所(广东省微生物分析检测中心) | Super-washable dual-function wearable electronic fabric and preparation method thereof |
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