CN104965015A - Method for preparing cadmium telluride electrodes and application thereof - Google Patents
Method for preparing cadmium telluride electrodes and application thereof Download PDFInfo
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- CN104965015A CN104965015A CN201510339181.5A CN201510339181A CN104965015A CN 104965015 A CN104965015 A CN 104965015A CN 201510339181 A CN201510339181 A CN 201510339181A CN 104965015 A CN104965015 A CN 104965015A
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Abstract
The invention discloses a method for manufacturing cadmium telluride electrodes and application thereof. The method includes depositing and modifying ITO (indium tin oxide) conductive glass by the aid of CdTe (cadmium telluride) under a constant-potential condition; sequentially ultrasonically cleaning the ITO in acetone, ethanol and pure water for a few minutes and drying the ITO in nitrogen flow; adhering and controlling the dried ITO in an appropriate working area by the aid of insulating tapes to obtain ITO electrodes; dissolving cadmium salt and TeO2 in acid solution according to a certain molar ratio, and stirring the cadmium salt and the TeO2 until the cadmium salt and the TeO2 are completely dissolved, to obtain electrolyte; carrying out depositing under the constant-potential condition for a few minutes by the aid of the ITO electrodes, platinum wire electrodes and Ag/AgCl electrodes to obtain the cadmium telluride electrodes CdTe/ITO. The ITO electrodes are used as working electrodes during depositing, the platinum wire electrodes are used as counter electrodes during depositing, and the Ag/AgCl electrodes are used as reference electrodes during depositing. The method for preparing the cadmium telluride electrodes and the application thereof have the advantages that the method can be implemented at the room temperature, and environmental pollution can be prevented; the cadmium telluride electrodes can be used in the field of environment monitoring and are low in cost, easy and convenient to operate, high in response speed and sensitivity and low in detection limit, and the like.
Description
Technical field
The present invention relates to preparation method and the application of a kind of cadmium telluride electrode CdTe/ITO, the application especially in Electrochemical Detection, belongs to environmental monitoring field.
Background technology
Cadmium telluride (CdTe) is a kind of novel semiconductor material, has unique optics and electrology characteristic.At present, CdTe material is widely used in spectral analysis, solar cell, infrared modulator, infrared window electroluminescent device, photoelectric cell, infrared acquisition, X X-ray detection X, nuclear activity detector, sensor.
CdTe thin film preparation method is various, common are radio frequency sputtering method, close spaced sublimation method, vacuum vapor deposition method, silk screen print method, element vapour phase chemical combination method and spray pyrolysis method etc.Although these methods are widely used, they all require to operate under the high temperature conditions and preparation process is complicated, length consuming time.In addition due to high-temperature operation, also there is certain danger in building-up process, and to human body and bad environmental, industrialization cost compare is high.Therefore, need to develop a kind of quick, easy, new method that normal temperature prepares CdTe thin film.
Summary of the invention
Object: in order to overcome the deficiencies in the prior art, the invention provides a kind of preparation method and application of cadmium telluride electrode, CdTe can be made to synthesize and at room temperature carry out, and reaction is fast and to operating personnel and environmental friendliness.
Technical scheme: for solving the problems of the technologies described above, the technical solution used in the present invention is:
A preparation method for cadmium telluride electrode, is characterized in that, comprises the following steps:
Step (1) electro-conductive glass ITO successively at acetone, ethanol, in pure water ultrasonic several minutes, and dry under nitrogen flowing; Dried ITO insulating tape is pasted and is controlled, at proper operation area, to obtain ITO electrode;
Step (2) prepares electrolytic solution: by cadmium salt and TeO
2be dissolved in acid solution according to certain mol ratio, be stirred to and dissolve completely;
Step (3) potentiostatic electrodeposition: make working electrode with the ITO electrode that step (1) is obtained, platinum electrode is done electrode, and Ag/AgCl electrode makes contrast electrode, does electrolytic solution with mixed solution prepared by step (2), precipitation number minute under constant potential, obtains cadmium telluride electrode CdTe/ITO.
Preferably, the preparation method of described cadmium telluride electrode, is characterized in that: described step (1), and the ultrasonic cleaning time is 1 ~ 10 min, and the working area of ITO electrode controls to be 1 cm
2.
Preferably, the preparation method of described cadmium telluride electrode, is characterized in that: in described step (2), and cadmium salt is cadmium sulfate, caddy or cadmium nitrate.
Preferably, the preparation method of described cadmium telluride electrode, is characterized in that: in described step (2), and acid solution is dilute sulfuric acid, watery hydrochloric acid or dust technology, and acid solution pH value is 1 ~ 3.
Preferably, the preparation method of described cadmium telluride electrode, is characterized in that: in described step (2), cadmium salt and TeO
2mol ratio be 1:(0.01 ~ 0.0001); Wherein cadmium ion volumetric molar concentration is 0.2 M.
Preferably, the preparation method of described cadmium telluride electrode, is characterized in that: in described step (3), the controling parameters of potentiostatic electrodeposition is as follows: the current potential of deposition is-0.8 ~-0.4 V, and sedimentation time is 30 ~ 600 s.
The present invention also provides a kind of cadmium telluride electrode, adopts the preparation method of above-mentioned cadmium telluride electrode to be prepared from.
Described cadmium telluride electrode carries out the application of Electrochemical Detection.
Described cadmium telluride electrode is measuring the application in phenol.
Beneficial effect: the preparation method of a kind of cadmium telluride electrode provided by the invention and application, cadmium telluride CdTe is deposited to electro-conductive glass ITO surface by the present invention's potentiostatic electrodeposition method, and the modified electrode obtained is applied to the quick detection of phenol.This electrode has that cost is low, easy and simple to handle, quick, sensitive, good selective.(1) cadmium telluride electrode provided by the invention, preparation technology is simple, with low cost, ambient operation; (2) cadmium telluride electrode provided by the invention can detect phenol effectively fast; (3) cadmium telluride electrode sensitivity provided by the invention is high, and detectability is low; (4) cadmium telluride electrode provided by the invention can be applicable to environmental monitoring field.
Accompanying drawing explanation
Fig. 1 is ITO electrode schematic diagram;
Fig. 2 is the principles of electro-deposition key diagram of CdTe;
Fig. 3 is 30000 times of scanning electron microscope diagram sheets of CdTe/ITO in embodiment 1;
Fig. 4 is the X-ray diffraction spectrogram of CdTe/ITO in embodiment 1;
Fig. 5 is the contrast cyclic voltammogram that in embodiment 2, Different electrodes detects phenol;
Fig. 6 is the differential pulse voltammetry figure (illustration is the matched curve of peak flow valuve and phenol concentration) that in embodiment 3, CdTe/ITO detects variable concentrations phenol;
Fig. 7 is 30000 times of scanning electron microscope diagram sheets of CdTe/ITO in embodiment 4;
Fig. 8 is that in embodiment 5, electric current and phenol concentration change linear relationship chart;
Fig. 9 is 30000 times of scanning electron microscope diagram sheets of CdTe/ITO in embodiment 6;
Figure 10 is that in embodiment 7, electric current and phenol concentration change linear relationship chart.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described.Described starting material all can obtain from open commercial sources if no special instructions.
embodiment 1, CdTe/ITO(electro-conductive glass) preparation of electrode
The pre-service of ITO: ITO successively at acetone, ethanol, ultrasonic 3 min in pure water, and dry under nitrogen flowing; It is 1 cm that dried ITO insulating tape controls its working area
2.
Deposit fluid is prepared: by 5.1304g CdSO
48/3H
2o and 0.798g TeO
2add in the dilution heat of sulfuric acid (pH=1.5) of 100mL, magnetic agitation is to dissolving completely;
Potentiostatic electrodeposition: with the CdSO obtained
4-TeO
2mixed liquor is cooked electrolytic solution, and ITO makes working electrode, and platinum electrode is done electrode, and Ag/AgCl electrode makes contrast electrode, deposits 300 s under-0.6V current potential.
Fig. 1 is the schematic diagram of pretreated ITO electrode.
Fig. 2 is the principle key diagram of potentiostatic electrodeposition CdTe.
The scanning electron microscope (SEM) photograph of gained CdTe/ITO and X-ray diffraction spectrogram are respectively as shown in Figure 3 and Figure 4.As seen from the figure, in order to upper method, successfully at ITO Surface Creation CdTe.
embodiment 2, CdTe/ITO electrode electrochemical property test
Different electrodes detects phenol contrast:
Phenol is joined in 0.1 M phosphate buffered solution (pH=7.0), prepare the phenol solution of 20 μMs.The CdTe/ITO electrode of gained is prepared for working electrode respectively with ITO and embodiment 1, platinum electrode is done electrode, Ag/AgCl electrode makes contrast electrode, carries out cyclic voltammetry scan phenol solution, record stable cyclic voltammogram in-0.6 ~ 0.6 V potential range.
Be illustrated in figure 5 the cyclic voltammetric comparison diagram that Different electrodes detects phenol, there is no obvious electrochemical response on the ITO electrode surface of unmodified as seen, and have obvious reduction peak to occur in the ITO electrode of CdTe modification.Contrast show that CdTe/ITO Pyrogentisinic Acid's has good electrochemical response.
embodiment 3, phenol quantitative detection
Prepare the phenol solution of 8,10,20,30,40,50,60,70,80,90,100 μMs respectively.The CdTe/ITO electrode preparing gained by embodiment 1 makes working electrode, and platinum electrode is done electrode, and Ag/AgCl electrode makes contrast electrode, adopts differential pulse cyclic voltammetry to scan the phenol solution of these 11 variable concentrations, and scanning potential range is-0.4 ~ 0.4 V.Peak flow valuve and the phenol concentration of getting phenol under each concentration do matched curve.
Fig. 6 is the differential pulse voltammetry figure that CdTe/ITO detects variable concentrations phenol, illustration be peak flow valuve and phenol concentration matched curve (
i(phenol)=-0.1163
c(phenol)-3.2196).Obtained by map analysis, the range of linearity of CdTe/ITO to detection phenol is 8-100 μM, and sensitivity is 0.1163 μ A μM
-1, detect and be limited to 2.67 μMs.
embodiment 4, CdTe/ITO electrode preparation
The pre-service of ITO: ITO successively at acetone, ethanol, ultrasonic 1 min in pure water, and dry under nitrogen flowing.It is 1 cm that dried ITO insulating tape controls its working area
2.
Deposit fluid is prepared: by 6.1696g Cd (NO
3)
24H
2o and 0.0003g TeO
2add in the dilute nitric acid solution (pH=1.0) of 100mL, magnetic agitation is to dissolving completely.
Potentiostatic electrodeposition: with the Cd (NO obtained
3)
2-TeO
2mixed liquor is cooked electrolytic solution, and ITO makes working electrode, and platinum electrode is done electrode, and Ag/AgCl electrode makes contrast electrode, deposits 30 s under-0.4V current potential.
Fig. 7 is the scanning electron microscope (SEM) photograph of gained CdTe/ITO.As shown in Figure 7, in order to upper method, successfully at ITO Surface Creation CdTe.
embodiment 5, phenol quantitative detection
Prepare the phenol solution of 8,10,20,30,40,50,60,70,80,90,100 μMs respectively.The CdTe/ITO electrode preparing gained by embodiment 4 makes working electrode, and platinum electrode is done electrode, and Ag/AgCl electrode makes contrast electrode, adopts differential pulse cyclic voltammetry to scan the phenol solution of these 11 variable concentrations, and scanning potential range is-0.4 ~ 0.4 V.Peak flow valuve and the phenol concentration of getting phenol under each concentration do matched curve.
Fig. 8 be current value and phenol concentration matched curve (
i(phenol)=-0.1142
c(phenol)-3.1241).Obtained by map analysis, the range of linearity of CdTe/ITO to detection phenol is 8-100 μM, and sensitivity is 0.1142 μ A μM
-1, detect and be limited to 2.78 μMs.
embodiment 6, CdTe/ITO electrode preparation
The pre-service of ITO: ITO successively at acetone, ethanol, ultrasonic 10 min in pure water, and dry under nitrogen flowing.It is 1 cm that dried ITO insulating tape controls its working area
2.
Deposit fluid is prepared: by 3.6664g CdCl
2with 0.0319g TeO
2add in the dilute hydrochloric acid solution (pH=3.0) of 100mL, magnetic agitation is to dissolving completely.
Potentiostatic electrodeposition: with the CdCl obtained
2-TeO
2mixed liquor is cooked electrolytic solution, and ITO makes working electrode, and platinum electrode is done electrode, and Ag/AgCl electrode makes contrast electrode, deposits 600 s under-0.8V current potential.
Fig. 9 is the scanning electron microscope (SEM) photograph of gained CdTe/ITO.As shown in Figure 9, in order to upper method, successfully at ITO Surface Creation CdTe.
embodiment 7, phenol quantitative detection
Prepare the phenol solution of 8,10,20,30,40,50,60,70,80,90,100 μMs respectively.The CdTe/ITO electrode preparing gained by embodiment 6 makes working electrode, and platinum electrode is done electrode, and Ag/AgCl electrode makes contrast electrode, adopts differential pulse cyclic voltammetry to scan the phenol solution of these 11 variable concentrations, and scanning potential range is-0.4 ~ 0.4 V.Peak flow valuve and the phenol concentration of getting phenol under each concentration do matched curve.
Figure 10 be current value and phenol concentration matched curve (
i(phenol)=-0.1130
c(phenol)-3.2183).Obtained by map analysis, the range of linearity of CdTe/ITO to detection phenol is 8-100 μM, and sensitivity is 0.1130 μ A μM
-1, detect and be limited to 2.82 μMs.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (9)
1. a preparation method for cadmium telluride electrode, is characterized in that, comprises the following steps:
Step (1) electro-conductive glass ITO successively at acetone, ethanol, in pure water ultrasonic several minutes, and dry under nitrogen flowing; Dried ITO insulating tape is pasted and is controlled, at proper operation area, to obtain ITO electrode;
Step (2) prepares electrolytic solution: by cadmium salt and TeO
2be dissolved in acid solution according to certain mol ratio, be stirred to and dissolve completely;
Step (3) potentiostatic electrodeposition: make working electrode with the ITO electrode that step (1) is obtained, platinum electrode is done electrode, and Ag/AgCl electrode makes contrast electrode, does electrolytic solution with mixed solution prepared by step (2), precipitation number minute under constant potential, obtains cadmium telluride electrode CdTe/ITO.
2. the preparation method of cadmium telluride electrode according to claim 1, is characterized in that: described step (1), and the ultrasonic cleaning time is 1 ~ 10 min, and the working area of ITO electrode controls to be 1 cm
2.
3. the preparation method of cadmium telluride electrode according to claim 1, is characterized in that: in described step (2), and cadmium salt is cadmium sulfate, caddy or cadmium nitrate.
4. the preparation method of cadmium telluride electrode according to claim 1, is characterized in that: in described step (2), and acid solution is dilute sulfuric acid, watery hydrochloric acid or dust technology, and acid solution pH value is 1 ~ 3.
5. the preparation method of cadmium telluride electrode according to claim 1, is characterized in that: in described step (2), cadmium salt and TeO
2mol ratio be 1:(0.01 ~ 0.0001); Wherein cadmium ion volumetric molar concentration is 0.2 M.
6. the preparation method of cadmium telluride electrode according to claim 1, is characterized in that: in described step (3), the controling parameters of potentiostatic electrodeposition is as follows: the current potential of deposition is-0.8 ~-0.4 V, and sedimentation time is 30 ~ 600 s.
7. a cadmium telluride electrode, adopts the preparation method of the cadmium telluride electrode described in any one of claim 1-6 to be prepared from.
8. cadmium telluride electrode as claimed in claim 7 carries out the application of Electrochemical Detection.
9. cadmium telluride electrode as claimed in claim 7 is measuring the application in phenol.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108682651A (en) * | 2018-05-23 | 2018-10-19 | 大连大学 | A kind of flexible electrode and preparation method thereof based on dendritic nano-silver structure |
| CN109030605A (en) * | 2018-08-30 | 2018-12-18 | 武汉钢铁有限公司 | The determination method of chrome plating surface metal chromium content height |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108682651A (en) * | 2018-05-23 | 2018-10-19 | 大连大学 | A kind of flexible electrode and preparation method thereof based on dendritic nano-silver structure |
| CN109030605A (en) * | 2018-08-30 | 2018-12-18 | 武汉钢铁有限公司 | The determination method of chrome plating surface metal chromium content height |
| CN109030605B (en) * | 2018-08-30 | 2020-08-04 | 武汉钢铁有限公司 | Method for judging metal chromium content on surface of chromium plated plate |
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