CN104034790B - Perfluorinated sulfonic acid resin modified SnO 2-coated ZnO nanotube array electrode for detecting dopamine and application - Google Patents
Perfluorinated sulfonic acid resin modified SnO 2-coated ZnO nanotube array electrode for detecting dopamine and application Download PDFInfo
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- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229960003638 dopamine Drugs 0.000 title claims abstract description 41
- 239000002071 nanotube Substances 0.000 title claims abstract description 40
- 239000011347 resin Substances 0.000 title claims abstract description 19
- 229920005989 resin Polymers 0.000 title claims abstract description 19
- 229910006404 SnO 2 Inorganic materials 0.000 title claims description 21
- 150000003460 sulfonic acids Chemical class 0.000 title abstract 2
- 239000013078 crystal Substances 0.000 claims abstract description 30
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000002484 cyclic voltammetry Methods 0.000 claims abstract description 19
- 238000001903 differential pulse voltammetry Methods 0.000 claims abstract description 19
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 13
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 10
- 239000002105 nanoparticle Substances 0.000 claims abstract description 4
- 239000011521 glass Substances 0.000 claims description 20
- 230000004044 response Effects 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 3
- 238000012986 modification Methods 0.000 claims description 3
- 229920000557 Nafion® Polymers 0.000 abstract description 25
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical class O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 abstract description 8
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 239000002073 nanorod Substances 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 241000725303 Human immunodeficiency virus Species 0.000 description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- NQTSTBMCCAVWOS-UHFFFAOYSA-N 1-dimethoxyphosphoryl-3-phenoxypropan-2-one Chemical compound COP(=O)(OC)CC(=O)COC1=CC=CC=C1 NQTSTBMCCAVWOS-UHFFFAOYSA-N 0.000 description 1
- 208000024827 Alzheimer disease Diseases 0.000 description 1
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- 208000018737 Parkinson disease Diseases 0.000 description 1
- 206010039966 Senile dementia Diseases 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 210000000748 cardiovascular system Anatomy 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000003907 kidney function Effects 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000036403 neuro physiology Effects 0.000 description 1
- 239000002858 neurotransmitter agent Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 201000000980 schizophrenia Diseases 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 238000000101 transmission high energy electron diffraction Methods 0.000 description 1
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- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
The invention belongs to the technical field of nano material application, and particularly relates to perfluorinated sulfonic acid resin (Nafion) modified SnO for detecting dopamine2A ZnO coated nanotube array electrode and application. The nanotube array electrode is a polycrystalline SnO (stannic oxide) modified by a conductive substrate and Nafion vertically grown on the conductive substrate2The nano-particle film is coated with the array of the single crystal ZnO nano-tube. The Nafion modified SnO for detecting dopamine2The ZnO-coated nanotube array electrode can detect dopamine in an aqueous solution, and can generate a very strong electrochemical signal when the dopamine in the aqueous solution is detected by Cyclic Voltammetry (CV) or Differential Pulse Voltammetry (DPV) by taking the nanotube array electrode as a working electrode, a platinum sheet electrode as a counter electrode and a saturated calomel electrode as a reference electrode.
Description
Technical field
The invention belongs to technical field of nano material application, particularly relate to a kind of perfluorinated sulfonic resin (Nafion) for detecting dopamine and modify SnO
2the nanometer pipe array electrode of clading ZnO and application.
Background technology
Dopamine (DA) is a kind of important neurotransmitter, plays an important role to central nervous system, Hormone system, cardiovascular system renal function of unifying.In human body, the concentration of DA can change, as schizophrenia, Parkinson's disease, senile dementia, HIV (human immunodeficiency virus) infection etc. with some major diseases.Therefore, in human body, the detection of DA concentration has great significance for the control of neuro-physiology research, medical diagnosis on disease and related drugs.
Electrochemical sensor is a kind of important means that dopamine detects.In electrochemical sensor, most important element is the electrode that can produce response to dopamine.Because the dopamine concentration in biosome is extremely low, the strong interference coming from ascorbic acid can be subject to simultaneously in dopamine testing process, therefore need to develop the dopamine electrochemical sensor electrodes with high sensitivity and high selectivity.The lifting developing into dopamine performance of electrochemical sensors of nanosecond science and technology provides good opportunity.The specific surface area huge due to it and special physical/chemical, nano material has been used to constructing of dopamine electrochemical sensor electrodes.Wherein, monodimension nanometer material is as particularly noticeable in nanometer rods, nano wire, nanobelt, nanotube etc.This is because these monodimension nanometer materials are except having huge specific surface area, the electronics participating in electrochemical reaction as " express passway " of transferring charge, can also be transported to external circuit by its special one-dimentional structure fast, thus improves the performance of sensor.At present, as most typical monodimension nanometer material, carbon nano-tube by a large amount of for dopamine electrochemical sensor electrodes (Electroanalysis, 2005,17,417; Analyst, 2007,132,876; Sensors, 2009,9,376; BiosensorsandBioelectronics, 2011,26,2917; SensorsandActuatorsB:Chemical, 2012,171,1132; ElectrochimicaActa, 2013,91,261; ChineseJournalofCatalysis, 2014,35,201.).But at these electrodes, carbon nano-tube is normally distributed in electrode surface in a jumble disorderly, its effect as charge transport " express passway " fails to be not fully exerted.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, providing a kind of and modifying SnO for what detect dopamine based on perfluorinated sulfonic resin (Nafion)
2the dopamine electrochemical sensor electrodes of the nano-tube array of clading ZnO.
An also object of the present invention is to provide modifies SnO for what detect dopamine based on perfluorinated sulfonic resin (Nafion)
2the application of the dopamine electrochemical sensor electrodes of the nano-tube array of clading ZnO.
Perfluorinated sulfonic resin (Nafion) for detecting dopamine of the present invention modifies SnO
2clading ZnO (SnO
2znO) nanometer pipe array electrode is the polycrystalline SnO that the perfluorinated sulfonic resin (Nafion) in this conductive substrates is modified by conductive substrates and vertical growth
2the array of the coated single crystal ZnO nanotube of nano-particular film is formed.
Described conductive substrates can be ito glass or FTO glass.
Described polycrystalline SnO
2the coated single crystal ZnO nanotube of nano-particular film is by polycrystalline SnO
2the film that nano particle is formed evenly is coated on the inner and outer wall of single crystal ZnO nanotube.
It is by by polycrystalline SnO that described perfluorinated sulfonic resin (Nafion) is modified
2the array of the coated single crystal ZnO nanotube of nano-particular film is carry out soaking (the general time of soaking is 8 ~ 15 minutes) in the Nafion solution of 5% to realize in mass concentration.
Perfluorinated sulfonic resin (Nafion) for detecting dopamine of the present invention modifies SnO
2clading ZnO (SnO
2the preparation method of nanometer pipe array electrode ZnO) is: first, with electrochemical deposition method at the upper making ZnO nanometer stick array of conductive substrates (ito glass or FTO glass), prepared ZnO nano-rod array is carried out in inorganic alkaline aqueous solution etching and obtain single crystal ZnO nano-tube array; Then, there is the conductive substrates of single crystal ZnO nano-tube array for substrate to grow, utilize thermal evaporation to prepare one deck polycrystalline SnO at the surfaces externally and internally of single crystal ZnO nanotube
2nano-particular film; By polycrystalline SnO
2the array of the coated single crystal ZnO nanotube of nano-particular film is carry out in the Nafion solution of 5% soaking (the general time of soaking is 8 ~ 15 minutes) in mass concentration.
Perfluorinated sulfonic resin (Nafion) for detecting dopamine of the present invention modifies SnO
2clading ZnO (SnO
2znO) nanometer pipe array electrode can detect the dopamine in aqueous solution, using nanometer pipe array electrode of the present invention as working electrode, using platinum plate electrode as to electrode, using saturated calomel electrode as contrast electrode, when detecting the dopamine in aqueous solution with cyclic voltammetry (CV) or differential pulse voltammetry (DPV), nanometer pipe array electrode of the present invention can produce extremely strong electrochemical signals.
Described use cyclic voltammetry (CV) or differential pulse voltammetry (DPV) detect the dopamine in aqueous solution, the linear response range of cyclic voltammetry (CV) is 0.1 ~ 500 μM, and the linear response range of differential pulse voltammetry (DPV) is 0.1 ~ 2 μM.
The concentration of the dopamine in described aqueous solution is 0.1 μM to 500 μMs.
In dopamine electrochemical sensor electrodes of the present invention, the SnO that Nafion modifies
2clading ZnO (SnO
2znO) nanotube is that vertically growth forms oldered array in conductive substrates, the electronics that electrochemical reaction occurs can along the nanotube fast transport described in person to external circuit, give full play to the potential of monodimension nanometer material as transferring charge " express delivery passage ", effectively improve the performance of dopamine electrochemical sensor.
Accompanying drawing explanation
Fig. 1. the polycrystalline SnO of the Nafion modification of the embodiment of the present invention 1
2the SEM image of the array of the coated single crystal ZnO nanotube of nano-particular film.
Fig. 2. single polycrystalline SnO prepared by the embodiment of the present invention 1
2the HRTEM (a) of the coated single crystal ZnO nanotube of nano-particular film and SAED (b) image.
Fig. 3. the CV (a) of the embodiment of the present invention 2 and DPV (b) figure.
Fig. 4. the CV (a) of the embodiment of the present invention 3 and DPV (b) figure.
Fig. 5. the CV (a) of the embodiment of the present invention 4 and DPV (b) figure.
Fig. 6. the CV (a) of the embodiment of the present invention 5 and DPV (b) figure.
Fig. 7. the CV (a) of the embodiment of the present invention 6 and DPV (b) figure.
Fig. 8. CV figure (a) of the embodiment of the present invention 7 and CV calibration curve (b) and DPV figure (c) and DPV calibration curve (d).
Embodiment
Embodiment 1.
In three-electrode system, using platinized platinum and saturated calomel electrode as to electrode and contrast electrode, with ito glass or FTO glass for working electrode.Electrolytic solution is the aqueous solution containing 5mM zinc nitrate and 5mM ammonium acetate.By water-bath electrolyte temperature risen to 85 DEG C and maintain 85 DEG C.Utilize electrochemical workstation (CHI660C, Shanghai Chen Hua Instrument Ltd.) to apply the current potential of-1V to working electrode, continue 3 hours, namely obtain growing the ZnO nano-rod array on ito glass or FTO glass; By this ZnO nano-rod array in concentration be 0.2M, temperature be 85 DEG C of sodium hydrate aqueous solutions in soak 1.5 hours, namely obtain single crystal ZnO nano-tube array.There are the ito glass of single crystal ZnO nano-tube array or FTO glass to be placed in porcelain boat growth, are placed on the low temperature center district of two temperature-area tubular furnace, place the porcelain boat that 2 grams of SnO powder are housed in the high temperature center district of tubular furnace.With mechanical pump, system is vacuumized, in system, pass into Ar/H
2combination gas (wherein H
2volume content be 5%), flow is 50sccm.By diamond heating, heating rate is 20 DEG C/min, makes the temperature of high temperature center and low temperature center reach 850 DEG C and 600 DEG C respectively, maintains this temperature after 1 hour, stops heating; Treat that temperature is down to room temperature, take out sample, namely obtain polycrystalline SnO
2the array of the coated single crystal ZnO nanotube of nano-particular film, and by polycrystalline SnO
2the film that nano particle is formed evenly is coated on the inner and outer wall of single crystal ZnO nanotube.By this polycrystalline SnO
2the array of the coated single crystal ZnO nanotube of nano-particular film is soak in the Nafion solution of 5% after 10 minutes to take out in mass concentration, naturally dries, namely obtains vertically growing the polycrystalline SnO having Nafion to modify on ito glass or FTO glass
2the array of the coated single crystal ZnO nanotube of nano-particular film.The polycrystalline SnO that prepared Nafion modifies
2the pattern of the array of nano-particular film coated single crystal ZnO nanotube and single polycrystalline SnO
2the structural characterization of the coated single crystal ZnO nanotube of nano-particular film respectively as depicted in figs. 1 and 2.The polycrystalline SnO that this Nafion modifies
2the array of the coated single crystal ZnO nanotube of nano-particular film can be used for detecting the dopamine in aqueous solution.
Embodiment 2.
The polycrystalline SnO that the vertical growth obtained with embodiment 1 is modified at the suprabasil Nafion of ito glass
2the array of the coated single crystal ZnO nanotube of nano-particular film is working electrode, using platinum plate electrode as to electrode, using saturated calomel electrode as contrast electrode, and composition three-electrode electro Chemical system.Detected object is the PBS solution (pH=7.4) of 0.1 μM of dopamine containing concentration.By electrochemical workstation, utilize cyclic voltammetry (CV) and differential pulse execution (DPV) to test the electrochemical response of detected object, result as shown in Figure 3.
Embodiment 3.
The polycrystalline SnO that the vertical growth obtained with embodiment 1 is modified at the suprabasil Nafion of ito glass
2the array of the coated single crystal ZnO nanotube of nano-particular film is working electrode, using platinum plate electrode as to electrode, using saturated calomel electrode as contrast electrode, and composition three-electrode electro Chemical system.Detected object is the PBS solution (pH=7.4) of 2 μMs of dopamines containing concentration.By electrochemical workstation, utilize cyclic voltammetry (CV) and differential pulse execution (DPV) to test the electrochemical response of detected object, result as shown in Figure 4.
Embodiment 4.
The polycrystalline SnO that the vertical growth obtained with embodiment 1 is modified at the suprabasil Nafion of ito glass
2the array of the coated single crystal ZnO nanotube of nano-particular film is working electrode, using platinum plate electrode as to electrode, using saturated calomel electrode as contrast electrode, and composition three-electrode electro Chemical system.Detected object is the PBS solution (pH=7.4) of 10 μMs of dopamines containing concentration.By electrochemical workstation, utilize cyclic voltammetry (CV) and differential pulse execution (DPV) to test the electrochemical response of detected object, result as shown in Figure 5.
Embodiment 5.
The polycrystalline SnO that the Nafion of the vertical growth obtained with embodiment 1 in FTO substrate of glass modifies
2the array of the coated single crystal ZnO nanotube of nano-particular film is working electrode, using platinum plate electrode as to electrode, using saturated calomel electrode as contrast electrode, and composition three-electrode electro Chemical system.Detected object is the PBS solution (pH=7.4) of 100 μMs of dopamines containing concentration.By electrochemical workstation, utilize cyclic voltammetry (CV) and differential pulse execution (DPV) to test the electrochemical response of detected object, result as shown in Figure 6.
Embodiment 6.
The polycrystalline SnO that the vertical growth obtained with embodiment 1 is modified at the suprabasil Nafion of ito glass
2the array of the coated single crystal ZnO nanotube of nano-particular film is working electrode, using platinum plate electrode as to electrode, using saturated calomel electrode as contrast electrode, and composition three-electrode electro Chemical system.Detected object is the PBS solution (pH=7.4) of 500 μMs of dopamines containing concentration.By electrochemical workstation, utilize cyclic voltammetry (CV) and differential pulse execution (DPV) to test the electrochemical response of detected object, result as shown in Figure 7.
Embodiment 7.
The polycrystalline SnO that the vertical growth obtained with embodiment 1 is modified at the suprabasil Nafion of ito glass
2the array of the coated single crystal ZnO nanotube of nano-particular film is working electrode, using platinum plate electrode as to electrode, using saturated calomel electrode as contrast electrode, and composition three-electrode electro Chemical system.Detected object is the PBS solution (pH=7.4) of 0.1 ~ 500 μM of dopamine containing concentration.By electrochemical workstation, utilize cyclic voltammetry (CV) and differential pulse execution (DPV) to test the electrochemical response of detected object, result as shown in Figure 8.
Claims (6)
1. modify SnO for the perfluorinated sulfonic resin detecting dopamine for one kind
2the nanometer pipe array electrode of clading ZnO, is characterized in that: described nanometer pipe array electrode is the polycrystalline SnO by conductive substrates and the vertically perfluorinated sulfonic resin modification of growth in this conductive substrates
2the array of the coated single crystal ZnO nanotube of nano-particular film is formed.
2. the perfluorinated sulfonic resin for detecting dopamine according to claim 1 modifies SnO
2the nanometer pipe array electrode of clading ZnO, is characterized in that: described conductive substrates is ito glass or FTO glass.
3. the perfluorinated sulfonic resin for detecting dopamine according to claim 1 modifies SnO
2the nanometer pipe array electrode of clading ZnO, is characterized in that: described polycrystalline SnO
2the coated single crystal ZnO nanotube of nano-particular film is by polycrystalline SnO
2the film that nano particle is formed evenly is coated on the inner and outer wall of single crystal ZnO nanotube.
4. the perfluorinated sulfonic resin for detecting dopamine according to claim 1 modifies SnO
2the nanometer pipe array electrode of clading ZnO, is characterized in that: it is by by polycrystalline SnO that described perfluorinated sulfonic resin is modified
2the array of the coated single crystal ZnO nanotube of nano-particular film is carry out soaking realizing in the perfluor sulfoacid resin solution of 5% in mass concentration.
5. the perfluorinated sulfonic resin modification SnO for detecting dopamine described in a Claims 1 to 4 any one
2the application of the nanometer pipe array electrode of clading ZnO, it is characterized in that: described nanometer pipe array electrode is used for detecting the dopamine in aqueous solution, using described nanometer pipe array electrode as working electrode, using platinum plate electrode as to electrode, using saturated calomel electrode as contrast electrode, when detecting the dopamine in aqueous solution with cyclic voltammetry or differential pulse voltammetry, described nanometer pipe array electrode produces extremely strong electrochemical signals;
The linear response range of cyclic voltammetry is 0.1 ~ 500 μM, and the linear response range of differential pulse voltammetry is 0.1 ~ 2 μM.
6. application according to claim 5, is characterized in that: the concentration of the dopamine in described aqueous solution is 0.1 μM to 500 μMs.
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| CN105671654B (en) * | 2016-01-21 | 2018-06-26 | 合肥工业大学 | A kind of ion induction type artificial skin array structure and preparation method thereof |
| CN108254426A (en) * | 2017-12-15 | 2018-07-06 | 新乡医学院 | It is prepared for dopamine concentration detection miniature electrochemical in animal brain |
| CN108288695B (en) * | 2018-01-11 | 2020-09-01 | 中南大学 | Zinc-based secondary battery negative electrode material and preparation method thereof |
| CN108717075B (en) * | 2018-05-21 | 2019-05-10 | 大连理工大学 | Utilize the method for the film modified electrode slice detection uric acid of electro-deposition perfluorinated sulfonic acid |
| CN111244399B (en) * | 2018-11-28 | 2021-11-26 | 中南大学 | Metal oxide modified zinc oxide tube composite negative electrode material for zinc secondary battery and preparation method thereof |
| CN111678963B (en) * | 2020-06-22 | 2021-11-12 | 南京大学 | Ultra-high-sensitivity dopamine biosensor and preparation method thereof |
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| CN102507683A (en) * | 2011-10-27 | 2012-06-20 | 西北师范大学 | Modified electrode based on functionalized multi-walled carbon nanotube, electrochemical system and application thereof |
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