CN108588778A - A method of Low-temperature electro-deposition prepares orderly ZnO nanorod in flexible plastic substrates - Google Patents
A method of Low-temperature electro-deposition prepares orderly ZnO nanorod in flexible plastic substrates Download PDFInfo
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- CN108588778A CN108588778A CN201810578307.8A CN201810578307A CN108588778A CN 108588778 A CN108588778 A CN 108588778A CN 201810578307 A CN201810578307 A CN 201810578307A CN 108588778 A CN108588778 A CN 108588778A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
- C25D5/56—Electroplating of non-metallic surfaces of plastics
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Abstract
The purpose of the present invention provides a kind of using simple, low temperature, direct electro-deposition means, the method that one-dimensional orderly ZnO nano-rod array is prepared in the flexible plastic substrate that load has ITO conductive films.Include the following steps：Use flexible PET/ITO substrates for working electrode, Pt electrodes are to electrode, and saturated calomel electrode is reference electrode, build three-electrode system；Three-electrode system is placed in electrolysis cup, the Zn (CH of a concentration of 0.0001mol/L~0.001mol/L are filled in electrolysis cup3COO)2Aqueous solution, and add the KCl enhancing solution conductivities of 0.1M；Electrolysis cup is put in 50~80 DEG C of thermostat water bath, and is passed through the O that flow is 10~20mL/min in advance into it2To ensure electrolyte oxygen content saturation until reaction terminates, deposition process uses constant potential cathodic deposition, and electrode both ends, which apply 0.9~1.2V and react 30min~60min, can be obtained uniform ZnO nano-rod array film.Low temperature controllable preparation ZnO nano-rod array film can be obtained in flexible PET/ITO substrates using the present invention, as flexible optoelectronic part material.
Description
Technical field
The present invention relates to the preparation fields of nano material, and simple, low temperature, direct electro-deposition are utilized more particularly to a kind of
Means, the method that one-dimensional orderly ZnO nano-rod array is prepared in the flexible plastic substrate that load has ITO conductive films.
Background technology
Flexible conductive substrates are before the numerous areas such as nano electron device and opto-electronic device all show wide application
Scape.Currently, common flexible conductive substrates are mostly the plastic supporting base that area load has ito thin film, there is transparent, shatter-proof, matter
Measure the features such as light.But largely there is high temperature resistant (100 DEG C or more start to be deformed, be denaturalized or melt) and acidproof in such substrate
The disadvantage of alkaline (surface conductance film is easy to fall off under acid-base environment) difference, limits thin in its area load semiconductor nano
The technology of preparing of membrane material.Meanwhile One-Dimensional ZnO nanostructure due to its special property in material, physics, chemical field quilt
It is widely used in the devices such as piezoelectricity, Flied emission, sensor and solar cell.Although a large amount of research work still tends to
The preparation of unordered One-Dimensional ZnO nanostructure, but more and more scholars recognize to be orientated consistent nano-structure array for each
The promotion of class device respective performances is most important.Therefore, in flexible plastic substrate (PET/ITO) directly, it is simple, easily make
It is the project of a great challenge for the One-Dimensional ZnO nanometer stick array of ordered orientation, structural integrity is gone out.
Currently, frequently with technological approaches there are mainly two types of：(1) ZnO nanorod film is prepared using conventional method
It then strips down and is transferred in flexible substrate on other temporary carriers；(2) directly by ZnO nano film magnetron sputtering or
Blade coating is supported on flexible substrate surface.The former semiconductive thin film be easy to cause structure destruction in stripping process, next shifts it
Caking property between back substrate and film is poor, influences the electron-transport of photoelectric device；The latter although realize ZnO film with it is soft
Binding directly between property plastic supporting base, but magnetron sputtering method manufacturing cost height is unfavorable for large-scale industrial production, knife coating
The disadvantage of film cohesiveness difference is equally existed, and two methods are suitable for preparing ZnO nanoparticle film, and cannot achieve one-dimensional
The preparation of ordered nano stick array.In addition, being limited by the disadvantage of flexible plastic substrate high temperature resistant, resistance to acid and alkali difference, other are rigid
The conventional method that ZnO nano-rod array is prepared in property conductive substrates, such as hydro-thermal method, template, vapour deposition process, gas-liquid-solid phase
Growth method etc. cannot be used directly in flexible substrate.It opens bright Zhe et al. to be combined with circulator bath using TEC, Zn (NO3)2Solution
Kept for -2 DEG C, thermoelectric cooler both ends form ice-nucleus by converting the voltage of application+3V and -3V, and last electro-deposition obtains ZnO and receives
Rice piece film, but operating process is complicated, it is difficult to realize the growth of ZnO nanorod.Though other scholars have also carried out electro-deposition preparation
It is related attempt, but be only by electro-deposition in hard substrate prepare the parameter simply transplanting of ZnO film in PET/ITO substrates it
On, gained sample ito thin film can mostly fall off, and electric conductivity drastically declines, and ZnO film morphology controllable is poor, it is difficult to is orientated
Preferable nanometer stick array.
Invention content
The present invention in view of the above problems, overcome existing for background technology it is insufficient, provide it is a kind of using simple, low temperature, directly
Electro-deposition means, the side of one-dimensional orderly ZnO nano-rod array is prepared in the flexible plastic substrate that load has ITO conductive films
Method.
A kind of Low-temperature electro-deposition in flexible plastic substrate provided by the invention prepares the side of ZnO nano-rod array film
Method includes the following steps：
(1) use flexibility PET/ITO substrates for working electrode, Pt electrodes are to electrode, and saturated calomel electrode is reference
Electrode builds three-electrode system；
(2) three-electrode system is placed in electrolysis cup, a concentration of 0.0001mol/L~0.001mol/L is filled in electrolysis cup
Zn (CH3COO)2Aqueous solution, and add the KCl enhancing solution conductivities of 0.1M；
(3) electrolysis cup is put in 50~80 DEG C of thermostat water bath, and it is 10~20mL/ to be passed through flow in advance into it
The O of min2To ensure electrolyte oxygen content saturation until reaction terminates, deposition process uses constant potential cathodic deposition, electrode two
End, which applies -0.9~-1.2V and reacts 30min~60min, can be obtained uniform ZnO nano-rod array film.
More specifically steps are as follows by the present invention：
Flexibility PET/ITO substrates use traditional cleaning formulations first, clear respectively at ultrasound in acetone, ethyl alcohol, deionized water
10min is washed, with with washing (deionized water long soaking time, pet sheet face ITO conductive films will fall off).Then with flexibility
PET/ITO substrates are that (electrode area control is 1.5 × 2.5cm to working electrode2), Pt electrodes are to electrode, saturation calomel electricity
Extremely reference electrode, electrode spacing 8mm, structure three-electrode system are placed in 50ml electrolysis cups, are filled in electrolysis cup a concentration of
Zn (the CH of 0.0001mol/L~0.001mol/L3COO)2Aqueous solution 35ml, and add the KCl enhancing solution conductivities of 0.1M.
Electrolysis cup is put in 50~80 DEG C of thermostat water bath, and 10min is passed through the O that flow is 10~20mL/min in advance into it2
To ensure electrolyte oxygen content saturation until reaction terminates, deposition process uses constant potential cathodic deposition, electrode both ends application-
0.9~-1.2V simultaneously reacts 30min~60min and can be obtained uniform ZnO nano-rod array film.
In a kind of Low-temperature electro-deposition in flexible plastic substrates of the present invention prepares the method for orderly ZnO nanorod, choosing
The sources Zn are Zn (CH3COO)2Aqueous solution.
In a kind of Low-temperature electro-deposition in flexible plastic substrates of the present invention prepares the method for orderly ZnO nanorod, system
Standby film is One-Dimensional ZnO nanometer stick array.
In a kind of Low-temperature electro-deposition in flexible plastic substrates of the present invention prepares the method for orderly ZnO nanorod, institute
Zn (the CH stated3COO)2Concentration is preferably that (the excessive ZnO nanorod of concentration is easy to reunite 0.0005mol/L, and concentration is too small to be unfavorable for
The growth of ZnO nanorod).
In a kind of Low-temperature electro-deposition in flexible plastic substrates of the present invention prepares the method for orderly ZnO nanorod, water
Bath temperature is preferably 75 DEG C, and (80 DEG C of bath temperature or more, the ito thin film in pet sheet face starts shedding off, and electric conductivity is deteriorated；Temperature mistake
Low easy generation zinc oxyhydroxide, dehydration are incomplete).In one kind Low-temperature electro-deposition preparation in flexible plastic substrates of the present invention
In the method for orderly ZnO nanorod, oxygen flow is preferably that (the too small OH- of flow is insufficient, and ZnO growths are insufficient by 15mL/min；Stream
Measure excessive, electro-deposition system is unstable).
In a kind of Low-temperature electro-deposition in flexible plastic substrates of the present invention prepares the method for orderly ZnO nanorod,
Be characterized in that using cathode deposit, electrode both ends apply current potential be preferably -1.1V (ZnO is not easy to grow when current potential is relatively low, current potential compared with
ZnO film blackening when high).
In a kind of Low-temperature electro-deposition in flexible plastic substrates of the present invention prepares the method for orderly ZnO nanorod, ZnO
The growth time of nanometer rods is preferably that (the long ZnO nanorod surface defect of growth time increases 40min, time short ZnO nanorod life
Length is insufficient, and grain size is small, and length is short).
Low temperature controllable preparation ZnO nano-rod array film can be obtained in flexible PET/ITO substrates using the present invention, made
For flexible optoelectronic part material.
Description of the drawings
Fig. 1 is the SEM figures of ZnO nano-rod array prepared by the embodiment of the present invention 1；
Fig. 2 is the XRD diagram of ZnO nano-rod array prepared by embodiment 1；
Fig. 3 is that the SEM for the ZnO nano-rod array that embodiment 2 is prepared with embodiment 3 schemes；
Fig. 4 is the XRD diagram for the ZnO nano-rod array that embodiment 2 is prepared with embodiment 3.
Specific implementation mode
Embodiment 1
1) 91.735mg zinc acetates (Zn (CH are added in 1L deionized waters3COO)2) and 7.455g potassium chloride (KCl), system
At uniform precursor liquid, and 35ml is taken to be placed in electrolysis cup, a concentration of 0.0005mol/L of zinc acetate, potassium chloride concentration is
0.1mol/L。
2) electrolysis cup is put in thermostat water bath, keep temperature be 75 DEG C it is constant terminate to reaction, O is passed through in precursor liquid2,
Flow is 15mL/min.
3) three-electrode system built using the present invention, constant potential cathode deposition, 40min is deposited at -1.1V.
4) sample is taken out after depositing, deionized water cleaning is used in combination, dries.
5) the SEM characterizations of the preparation-obtained ZnO nano-rod array film of the present embodiment are as shown in Figure 1, can be with from figure
Find out that sample thin film is to be orientated unanimously, perpendicular to the nanorod structure of substrate grown.
6) XRD characterization of the preparation-obtained ZnO nano-rod array film of the present embodiment is as shown in Fig. 2, can be with from figure
Find out in addition to the diffraction maximum of substrate PET/ITO, other diffraction maximums of sample with the standard card (JPCD of ZnO：01-079-
0207) consistent, illustrate that sample is the ZnO crystal of hexagonal wurtzite；(002) crystallographic plane diffraction peak is significantly stronger than other crystal face diffraction
Peak also illustrates ZnO nanorod perpendicular to substrate grown.
Embodiment 2
1) 18.347mg zinc acetates (Zn (CH are added in 1L deionized waters3COO)2) and 7.455g potassium chloride (KCl), system
At uniform precursor liquid, and 35ml is taken to be placed in electrolysis cup, a concentration of 0.0001mol/L of zinc acetate, potassium chloride concentration is
0.1mol/L。
2) electrolysis cup is put in thermostat water bath, keep temperature be 60 DEG C it is constant terminate to reaction, O is passed through in precursor liquid2,
Flow is 10mL/min.
3) three-electrode system built using the present invention, constant potential cathode deposition, deposits 60min at-1.0v.
4) sample uses processing mode in the same manner as in Example 1 after depositing.
Embodiment 3
1) 183.47mg zinc acetates (Zn (CH are added in 1L deionized waters3COO)2) and 7.455g potassium chloride (KCl), system
At uniform precursor liquid, and 35ml is taken to be placed in electrolysis cup, a concentration of 0.001mol/L of zinc acetate, potassium chloride concentration is
0.1mol/L。
2) electrolysis cup is put in thermostat water bath, keep temperature be 80 DEG C it is constant terminate to reaction, O is passed through in precursor liquid2,
Flow is 20mL/min.
3) using the three-electrode system built using the present invention, constant potential cathode deposition deposits 30min at -1.2V.
4) sample uses processing mode in the same manner as in Example 1 after depositing.
5) embodiment 2 and the SEM of 3 preparation-obtained ZnO nano-rod array film of example are characterized as shown in figure 3, from figure
In it can be seen that preparation condition is different, obtained ZnO nano-rod array pattern, grain size, crystallinity are significantly different.
6) embodiment 2 and the XRD characterization of 3 preparation-obtained ZnO nano-rod array film of example are as shown in figure 4, from figure
It can be seen that although two kinds of conditions have obtained the ZnO nano film of hexagonal wurtzite in, thin film diffraction peak intensity relative to
Substrate diffraction maximum is obviously reduced compared with Example 1, illustrates that film thickness is relatively thin.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (9)
1. a kind of method that the Low-temperature electro-deposition in flexible plastic substrate prepares ZnO nano-rod array film,
Characterized by the following steps：
(1) use flexibility PET/ITO substrates for working electrode, Pt electrodes are to electrode, and saturated calomel electrode is reference electrode,
Build three-electrode system；
(2) three-electrode system is placed in electrolysis cup, the Zn of a concentration of 0.0001mol/L~0.001mol/L is filled in electrolysis cup
(CH3COO)2Aqueous solution, and add the KCl enhancing solution conductivities of 0.1M；
(3) electrolysis cup is put in 50~80 DEG C of thermostat water bath, and it is 10~20mL/min to be passed through flow in advance into it
O2To ensure electrolyte oxygen content saturation until reaction terminates, deposition process uses constant potential cathodic deposition, electrode both ends
Apply -0.9~-1.2V and react 30min~60min and can be obtained uniform ZnO nano-rod array film.
2. preparation method according to claim 1, it is characterised in that the flexibility PET/ITO substrates are cleaned using usual manner
, respectively at being cleaned by ultrasonic 10min in acetone, ethyl alcohol, deionized water, with with washing.
3. preparation method according to claim 1, it is characterised in that the working electrode area control is 1.5 × 2.5cm2, electricity
Interpolar is away from for 8mm.
4. preparation method according to claim 1, it is characterised in that the film of preparation is One-Dimensional ZnO nanometer stick array.
5. preparation method according to claim 1, it is characterised in that the Zn (CH3COO)2A concentration of 0.0005mol/L.
6. preparation method according to claim 1, it is characterised in that the bath temperature is 75 DEG C.
7. preparation method according to claim 1, it is characterised in that the oxygen flow is 15mL/min.
8. preparation method according to claim 1, it is characterised in that using cathode deposit, electrode both ends apply current potential be-
1.1V。
9. preparation method according to claim 1, it is characterised in that reaction time 40min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109609960A (en) * | 2019-01-21 | 2019-04-12 | 河海大学 | Optical anode material Bi with optical electro-chemistry cathodic protection effect2S3The preparation method of/ZnO |
| CN110512225A (en) * | 2019-09-26 | 2019-11-29 | 广东先导稀材股份有限公司 | Preparation method of zinc oxide powder |
| CN114558592A (en) * | 2022-03-09 | 2022-05-31 | 北方民族大学 | ZnO/ZnS nanorod core-shell structure photocatalyst and preparation method thereof |
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| CN101348931A (en) * | 2008-09-11 | 2009-01-21 | 北京科技大学 | Method for preparing uniform transparent zinc oxide nanorod array film by pulse electrodeposition |
| CN102220615A (en) * | 2011-05-13 | 2011-10-19 | 中国科学院理化技术研究所 | Method for preparing CdS/ZnO nanotube array photoelectrode |
| CN102732927A (en) * | 2012-07-17 | 2012-10-17 | 西北工业大学 | Preparation method of zinc oxide/ cuprous oxide heterojunction |
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| CN101348931A (en) * | 2008-09-11 | 2009-01-21 | 北京科技大学 | Method for preparing uniform transparent zinc oxide nanorod array film by pulse electrodeposition |
| CN102220615A (en) * | 2011-05-13 | 2011-10-19 | 中国科学院理化技术研究所 | Method for preparing CdS/ZnO nanotube array photoelectrode |
| CN102732927A (en) * | 2012-07-17 | 2012-10-17 | 西北工业大学 | Preparation method of zinc oxide/ cuprous oxide heterojunction |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109609960A (en) * | 2019-01-21 | 2019-04-12 | 河海大学 | Optical anode material Bi with optical electro-chemistry cathodic protection effect2S3The preparation method of/ZnO |
| CN110512225A (en) * | 2019-09-26 | 2019-11-29 | 广东先导稀材股份有限公司 | Preparation method of zinc oxide powder |
| CN110512225B (en) * | 2019-09-26 | 2021-12-17 | 广东先导稀材股份有限公司 | Preparation method of zinc oxide powder |
| CN114558592A (en) * | 2022-03-09 | 2022-05-31 | 北方民族大学 | ZnO/ZnS nanorod core-shell structure photocatalyst and preparation method thereof |
| CN114558592B (en) * | 2022-03-09 | 2023-11-14 | 北方民族大学 | ZnO/ZnS nano-rod core-shell structure photocatalyst and preparation method thereof |
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Application publication date: 20180928 |