CN103575780B - A kind of preparation method of zinc oxide nano film, electrochemical sensor electrodes and electrochemical sensor - Google Patents
A kind of preparation method of zinc oxide nano film, electrochemical sensor electrodes and electrochemical sensor Download PDFInfo
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- CN103575780B CN103575780B CN201310485760.1A CN201310485760A CN103575780B CN 103575780 B CN103575780 B CN 103575780B CN 201310485760 A CN201310485760 A CN 201310485760A CN 103575780 B CN103575780 B CN 103575780B
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- zinc oxide
- oxide nano
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- nano film
- metal sheet
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 61
- 239000002120 nanofilm Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000011701 zinc Substances 0.000 claims abstract description 45
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 45
- 229910052751 metal Inorganic materials 0.000 claims abstract description 42
- 239000002184 metal Substances 0.000 claims abstract description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 48
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 235000019441 ethanol Nutrition 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 229960001296 zinc oxide Drugs 0.000 description 51
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 13
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 13
- 239000000243 solution Substances 0.000 description 9
- 238000002484 cyclic voltammetry Methods 0.000 description 7
- 238000004502 linear sweep voltammetry Methods 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 238000000835 electrochemical detection Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical compound [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000001659 ion-beam spectroscopy Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000010897 surface acoustic wave method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The present invention relates to a kind of preparation method of zinc oxide nano film, electrochemical sensor electrodes and electrochemical sensor, utilize the ultra-thin zinc oxide nano film of hydro-thermal method controlled synthesis, the ultra-thin zinc oxide nano film of preparation is owing to being attached to zinc metal sheet surface, directly as electrode, material can be directly used in as sensor and detect.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of preparation method of zinc oxide nano film, electrochemical sensor electrodes and electrochemical sensor.
Background technology
ZnO(zinc paste) be II-VI race's broad stopband direct band gap compound semiconductor, it is hexagonal pricker zinc ore structure, and at room temperature its energy gap is about 3.37eV.ZnO film lattice, photoelectricity, piezoelectricity, air-sensitive, pressure-sensitive etc. many in there is excellent performance, thermal stability is high, obtain in surface acoustic wave device, solar cell, air-sensitive and pressure-sensitive device etc. are a lot of and apply comparatively widely, also have huge potentiality to be exploited at numerous areas such as ultraviolet detectors.And many manufacture crafts of ZnO film are compatible with integrated circuit technology, can realize integrated with multiple semiconductor devices such as silicon, thus enjoy people to pay attention to, there is vast potential for future development.
At present, the preparation method of zinc-oxide film is varied, mainly contain: radio frequency sputtering method, Dual ion beam sputtering deposition method, chemical vapour deposition technique, molecular beam hydatogenesis, pulsed laser deposition, spray heating decomposition and sol-gel method etc., but, above method is all more loaded down with trivial details, and preparation process is comparatively complicated.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of preparation method of zinc oxide nano film, electrochemical sensor electrodes and electrochemical sensor, utilize the ultra-thin zinc oxide nano film of hydro-thermal method controlled synthesis, the ultra-thin zinc oxide nano film of preparation is owing to being attached to zinc metal sheet surface, directly as electrode, material can be directly used in as sensor and detect.
The technical solution used in the present invention is:
A preparation method for zinc oxide nano film, comprises the following steps:
A, zinc metal sheet to be cleaned up; Cleaning method for zinc metal sheet is put into ethanol successively, water carries out ultrasonic cleaning, the ultrasonic cleaning time is respectively 10-20min, can reach activation zinc metal sheet surface, object at zinc metal sheet Surface Creation zinc-oxide nano seed;
B, absolute ethyl alcohol and concentrated hydrochloric acid are mixed after add in reactor, the zinc metal sheet that processed is immersed in mixed liquor, reactor is airtight, at 40 DEG C-80 DEG C, react 2-4 hour, be cooled to room temperature, cleaning, drying at room temperature, be i.e. obtained zinc oxide nano film; The volume ratio of described absolute ethyl alcohol and concentrated hydrochloric acid is 20-200:1; Described concentrated hydrochloric acid concentration >=8mol/L.
A kind of electrochemical sensor electrodes, uses the zinc metal sheet preparation comprising zinc oxide nano film.
A kind of electrochemical sensor, uses the electrode preparation comprising the zinc metal sheet of zinc oxide nano film.
The preparation method of zinc oxide nano film of the present invention is in airtight high-temperature high-pressure reaction kettle, adopts ethanol to do reaction dissolvent, by heating reaction system, produces a hyperbaric environment and carries out a kind of effective ways prepared by material.The present invention selects grow ultra-thin zinc oxide nano film on zinc metal sheet, and be based on zinc metal sheet in acid condition, hyperbaric heating, can in the ultra-thin zinc oxide nano film structure of Surface Creation one deck.Preparation method's product purity of the present invention is high, good dispersion, good crystalline and can control, and production cost is low, favorable reproducibility.Prepared ultra-thin zinc oxide nano film has larger specific surface area, fully can contact, make electrocatalytic reaction fully efficient as sensor material with determinand.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph (SEM) of zinc oxide nano film prepared by embodiment 1;
Fig. 2 is that zinc oxide nano film prepared by embodiment 1 carries out the cyclic voltammogram (CV) of Electrochemical Detection to hydrazine hydrate;
In figure:
1 zinc oxide nano film prepared for embodiment 1 does not add the cyclic voltammetry curve of hydrazine hydrate in the sodium hydroxide solution of pH=13; 2 zinc oxide nano films prepared for embodiment 1 have added the cyclic voltammetry curve of 0.05mM hydrazine hydrate in the sodium hydroxide solution of pH=13; 3 zinc oxide nano films prepared for embodiment 1 have added the cyclic voltammetry curve of 0.1mM hydrazine hydrate in the sodium hydroxide solution of pH=13;
Fig. 3 is that naked zinc carries out the linear sweep voltammetry figure (LSV) of Electrochemical Detection to hydrazine;
In figure:
1 zinc metal sheet that is clean non-developing zinc oxide does not add the linear sweep voltammetry figure of hydrazine hydrate in the sodium hydroxide solution of pH=13; 2 zinc metal sheets that are clean non-developing zinc oxide have added the linear sweep voltammetry figure of 0.05mM hydrazine hydrate in the sodium hydroxide solution of pH=13; 3 zinc metal sheets that are clean non-developing zinc oxide have added the linear sweep voltammetry figure of 0.1mM hydrazine hydrate in the sodium hydroxide solution of pH=13;
Fig. 4 is the time current curve (I-T figure) of zinc paste;
Fig. 5 is the electron scanning micrograph (SEM) of zinc oxide nano film prepared by embodiment 2;
Fig. 6 is the electron scanning micrograph (SEM) of zinc oxide nano film prepared by embodiment 3;
Fig. 7 is the electron scanning micrograph (SEM) of zinc oxide nano film prepared by embodiment 4;
Fig. 8 is the electron scanning micrograph (SEM) of zinc oxide nano film prepared by embodiment 5.
Embodiment
Embodiment 1
A preparation method for zinc oxide nano film, comprises the following steps:
A, zinc metal sheet is put into ethanol, water successively carry out ultrasonic cleaning 15min respectively;
B, the concentrated hydrochloric acid of 20mL absolute ethyl alcohol and 0.1mL12mol/L is mixed after add in 60mL reactor, the zinc metal sheet processed is immersed in mixed liquor, tighten kettle cover, react 2 hours at 80 DEG C, take out reactor and naturally cool to room temperature, rinse well with ethanol, redistilled water successively, drying at room temperature, i.e. obtained zinc oxide nano film.
A kind of electrochemical sensor electrodes, use the zinc metal sheet preparation comprising zinc oxide nano film, the mass area ratio of zinc-oxide film and zinc electrode is 0.0165g/cm
2.
A kind of electrochemical sensor, uses the electrode preparation comprising the zinc metal sheet of zinc oxide nano film.
The zinc metal sheet of coating zinc oxide nano thin-film embodiment 1 prepared, is directly used as electrode, does electrochemical properties test.Using NaOH solution as electrolyte, hydrazine hydrate is detected.
Get 10mL0.1MNaOH solution and put into electrolytic tank as electrolyte solution, using the electrode of preparation in embodiment 1 as working electrode, set correlation parameter, cyclic voltammetry curve (in Fig. 2 curve 1) is surveyed when not adding hydrazine, then the hydrazine injection electrolytic tank of 50 μ L0.01M is got with microsyringe, measure to obtain curve 2 in Fig. 2, in electrolytic tank, the concentration of hydrazine is 0.05mM.Comparison curves 1 and 2 can find, at electromotive force 0.6V, corresponding larger current is had to change, illustrate that this electrode pair hydrazine has electrochemical response, continue the hydrazine adding 50 μ L0.01M again, the cyclic voltammetry curve 3 recorded has stronger current-responsive at electromotive force 0.6V, and the concentration of hydrazine now in electrolytic tank is 0.1mM.From Fig. 2, we can see, curve 3 and curve 1 current peak difference are 2 times of curve 2 and curve 1 current peak difference.And 2 times of concentration (0.05mM) of hydrazine hydrate in electrolytic tank when the concentration (0.1mM) of hydrazine hydrate is curve 2 in electrolytic tank during curve 3, illustrate response current and hydrazine concentration linear.
In order to verificating current response is caused but not the direct effect of zinc metal sheet by ultra-thin zinc oxide nano film, the invention provides contrast experiment.Be about to the zinc metal sheet of clean non-developing zinc oxide, and the identical zinc metal sheet of specification detects hydrazine as working electrode, found that having added 50 μ L concentration be 0.01M hydrazine hydrate (in Fig. 3 curve 2) and to have added 100 μ L concentration be 0.01M hydrazine hydrate (in Fig. 3 curve 3), at electromotive force 0.6V place, current-responsive is less, goes curve almost to overlap with the cyclic voltammetric not adding hydrazine (in Fig. 3 curve 1).This sufficient proof electrode pair hydrazine hydrate provided by the invention has electrochemical response.
For studying electrochemical properties of the present invention further, be also the time current curve figure (Fig. 4) of electrode.Namely every 50 seconds, add the hydrazine of identical or different concentration, often add a capital and produce a step, until no longer produce step.The electrode pair hydrazine response time recording the embodiment of the present invention 1 preparation is on average less than 3 seconds, and detect and be limited to 0.1 μM, the range of linearity is 0.05-1050mM, shows that this electrode can as the electrochemical sensor of hydrazine.
Embodiment 2
A preparation method for zinc oxide nano film, comprises the following steps:
A, zinc metal sheet is put into ethanol, water successively carry out ultrasonic cleaning 20min respectively;
B, the concentrated hydrochloric acid of 20mL absolute ethyl alcohol and 0.4mL12mol/L is mixed after add in 60mL reactor, the zinc metal sheet processed is immersed in mixed liquor, tighten kettle cover, react 4 hours at 40 DEG C, take out reactor and naturally cool to room temperature, rinse well with ethanol, redistilled water successively, drying at room temperature, i.e. obtained zinc oxide nano film.
A kind of electrochemical sensor electrodes, uses the zinc metal sheet preparation comprising zinc oxide nano film.
A kind of electrochemical sensor, uses the electrode preparation comprising the zinc metal sheet of zinc oxide nano film.
Embodiment 3
A preparation method for zinc oxide nano film, comprises the following steps:
A, zinc metal sheet is put into ethanol, water successively carry out ultrasonic cleaning 15min respectively;
B, the concentrated hydrochloric acid of 20mL absolute ethyl alcohol and 0.8mL12mol/L is mixed after add in 60mL reactor, the zinc metal sheet processed is immersed in mixed liquor, tighten kettle cover, react 2 hours at 40 DEG C, take out reactor and naturally cool to room temperature, rinse well with ethanol, redistilled water successively, drying at room temperature, i.e. obtained zinc oxide nano film.
A kind of electrochemical sensor electrodes, uses the zinc metal sheet preparation comprising zinc oxide nano film.
A kind of electrochemical sensor, uses the electrode preparation comprising the zinc metal sheet of zinc oxide nano film.
Embodiment 4
A preparation method for zinc oxide nano film, comprises the following steps:
A, zinc metal sheet is put into ethanol, water successively carry out ultrasonic cleaning 10min respectively;
B, the concentrated hydrochloric acid of 20mL absolute ethyl alcohol and 0.2mL8mol/L is mixed after add in 60mL reactor, the zinc metal sheet processed is immersed in mixed liquor, tighten kettle cover, react 3 hours at 60 DEG C, take out reactor and naturally cool to room temperature, rinse well with ethanol, redistilled water successively, drying at room temperature, i.e. obtained zinc oxide nano film.
A kind of electrochemical sensor electrodes, uses the zinc metal sheet preparation comprising zinc oxide nano film.
A kind of electrochemical sensor, uses the electrode preparation comprising the zinc metal sheet of zinc oxide nano film.
Embodiment 5
A preparation method for zinc oxide nano film, comprises the following steps:
A, zinc metal sheet is put into ethanol, water successively carry out ultrasonic cleaning 15min respectively;
B, the concentrated hydrochloric acid of 20mL absolute ethyl alcohol and 0.2mL11mol/L is mixed after add in 60mL reactor, the zinc metal sheet processed is immersed in mixed liquor, tighten kettle cover, react 3 hours at 50 DEG C, take out reactor and naturally cool to room temperature, rinse well with ethanol, redistilled water successively, drying at room temperature, i.e. obtained zinc oxide nano film.
A kind of electrochemical sensor electrodes, uses the zinc metal sheet preparation comprising zinc oxide nano film.
A kind of electrochemical sensor, uses the electrode preparation comprising the zinc metal sheet of zinc oxide nano film.
Claims (4)
1. a preparation method for zinc oxide nano film, comprises the following steps:
A, zinc metal sheet to be cleaned up;
B, absolute ethyl alcohol and concentrated hydrochloric acid are mixed after add in reactor, the zinc metal sheet that processed is immersed in mixed liquor, reactor is airtight, at 40 DEG C-80 DEG C, react 2-4 hour, be cooled to room temperature, cleaning, drying at room temperature, be i.e. obtained zinc oxide nano film;
In described step b, the volume ratio of absolute ethyl alcohol and concentrated hydrochloric acid is 20-200:1, concentrated hydrochloric acid concentration >=8mol/L.
2. preparation method as claimed in claim 1, is characterized in that: in described step a cleaning method for zinc metal sheet is put into ethanol successively, water carries out ultrasonic cleaning, the ultrasonic cleaning time is respectively 10-20min.
3. an electrochemical sensor electrodes, uses the zinc metal sheet preparation comprising zinc oxide nano film prepared by claim 1 or 2 preparation method.
4. an electrochemical sensor, comprises electrode according to claim 3.
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| CN103575780B true CN103575780B (en) | 2015-12-02 |
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| CN105271361B (en) * | 2015-10-28 | 2017-03-08 | 中国科学院上海微系统与信息技术研究所 | A kind of preparation method of dendroid zinc oxide nano-wire array |
| CN113834862B (en) * | 2021-09-17 | 2023-05-30 | 电子科技大学 | Method for regulating/enhancing sensitivity of self-driven flexible gas sensor by interface stress |
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| CN102423755B (en) * | 2011-10-20 | 2013-12-11 | 西北师范大学 | Method for constructing nanotube-like super-hydrophobic structure on surface of zinc sheet |
| CN102691029B (en) * | 2011-12-22 | 2014-04-23 | 河南科技大学 | Method for preparing nano zinc oxide thin film |
| CN102692430A (en) * | 2012-06-07 | 2012-09-26 | 青岛大学 | Preparation method of carbon monoxide gas sensitive sensor operating in room temperature environment |
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