CN110302792B - Carbon nanotube-loaded NiCoO in non-enzymatic electrochemical glucose sensingxPreparation method and application of composite material catalyst - Google Patents
Carbon nanotube-loaded NiCoO in non-enzymatic electrochemical glucose sensingxPreparation method and application of composite material catalyst Download PDFInfo
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- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 title claims abstract description 40
- 239000008103 glucose Substances 0.000 title claims abstract description 39
- 239000003054 catalyst Substances 0.000 title claims abstract description 37
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 30
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 19
- 230000002255 enzymatic effect Effects 0.000 title claims abstract description 17
- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 27
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 10
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 238000001291 vacuum drying Methods 0.000 claims abstract description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 238000001514 detection method Methods 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
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- 229910052759 nickel Inorganic materials 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 239000002114 nanocomposite Substances 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 102000004190 Enzymes Human genes 0.000 description 3
- 108090000790 Enzymes Proteins 0.000 description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 3
- 238000000970 chrono-amperometry Methods 0.000 description 3
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 238000000835 electrochemical detection Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 229910000314 transition metal oxide Inorganic materials 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
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 210000002966 serum Anatomy 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910016553 CuOx Inorganic materials 0.000 description 1
- ODKSFYDXXFIFQN-BYPYZUCNSA-N L-arginine Chemical compound OC(=O)[C@@H](N)CCCN=C(N)N ODKSFYDXXFIFQN-BYPYZUCNSA-N 0.000 description 1
- 229930064664 L-arginine Natural products 0.000 description 1
- 235000014852 L-arginine Nutrition 0.000 description 1
- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 description 1
- TVWHNULVHGKJHS-UHFFFAOYSA-N Uric acid Natural products N1C(=O)NC(=O)C2NC(=O)NC21 TVWHNULVHGKJHS-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229960003638 dopamine Drugs 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229960002163 hydrogen peroxide Drugs 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229960002668 sodium chloride Drugs 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
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- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229940116269 uric acid Drugs 0.000 description 1
- 229910003145 α-Fe2O3 Inorganic materials 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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- B01J35/23—
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- B01J35/33—
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- B01J35/393—
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- B01J35/399—
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
Abstract
The invention discloses a carbon nano tube loaded NiCoO in non-enzymatic electrochemical glucose sensingxA preparation method and application of a composite catalyst are disclosed, wherein the method comprises the following steps: 1) adding 10mg of acidified multi-walled carbon nano-tubes into a crucible filled with 5mL of absolute ethyl alcohol, performing ultrasonic treatment at normal temperature for 15 minutes, adding a 0.1M cerium nitrate and 0.1M nickel nitrate aqueous solution, controlling the atomic ratio of Ni to Ce in the added cerium nitrate and nickel nitrate solution to be Ni: Ce =1:0.33-3, continuing ultrasonic treatment to evaporate the liquid, and performing vacuum drying at 60 ℃; 2) putting the dried sample prepared in the step 1) into a tube furnace, and performing reaction in N2/H2In a mixed atmosphere of H2The volume percentage of the carbon nano tube is 10 percent, and the reaction is carried out for 0.5 to 7 hours at the temperature of between 100 and 500 ℃ to obtain the carbon nano tube loaded NiCoOxA composite catalyst. The method has the advantages of simple process, few operation steps, mild and controllable conditions, and excellent electrochemical performance of the prepared material, and has good application prospect.
Description
Technical Field
The invention relates to the field of electrocatalysis and electrochemical glucose sensing, in particular to a carbon nano tube loaded NiCoO in non-enzymatic electrochemical glucose sensingxA composite catalyst, a preparation method and application thereof.
Background
In the field of electrochemical sensing of glucose, an enzyme-based sensor has the advantages of high selectivity and quick response, but also has an obvious defect that the enzyme is easily inactivated by factors such as environment and the like, so that the detection of the glucose is influenced, and therefore, the development of a sensitive and efficient non-enzymatic glucose sensor is valued by people. At present, metal oxides, particularly transition metal oxides, are widely used in the construction of non-enzymatic glucose sensors, because the metal atom of the transition metal oxide is usually in an intermediate valence state, and is more prone to gain and lose electrons in an electrochemical environment to generate an oxidation-reduction reaction, thereby showing excellent electrocatalytic performance. However, different metal oxides vary in their crystal structure, morphology, electronic conductivity, and electrocatalytic properties, resulting in large differences in the performance of sensors constructed from these oxides.
Among a plurality of transition metal oxides, NiO has excellent electrocatalytic performance, high sensitivity and stability and is a good catalyst for glucose oxidation. In order to enhance the synergistic effect between different components of the catalyst and further improve the electrocatalytic performance of the catalyst, an attempt is made to add another transition metal on the basis of nickel oxide to obtain a nickel-based bimetallic oxide composite material. In recent years, few research literatures are reported on the synthesis of nickel-based bimetallic oxide composite materials and the application of the nickel-based bimetallic oxide composite materials in the aspect of glucose electrochemical sensing, and the research literatures mainly relate to the following several reports: (1)2019, Journal of Electroanalytical Chemistry reported Co3O4-synthesis of NiO nanoneedles and their use for electrochemical detection of glucose; (2)2019 Microchimica Acta reports CuOx/NiOySynthesis of hollow nanocomposites and their use for glucose and H2O2Non-enzymatic electrochemical detection of (1); (3)2018, Applied Catalysis, B: Environmental, reported p-NiO/n-alpha-Fe2O3Synthesis of heterostructures and for constructing high performance glucose sensors; (4) in 2017, Journal of Alloys and Compounds reports the synthesis of a three-dimensional macroporous carbon-supported ZnO-NiO nanosheet composite material and the application of the three-dimensional macroporous carbon-supported ZnO-NiO nanosheet composite material in the electrochemical detection of glucose; (5) flower-shaped NiO-SnO is reported in RSC Advances in 20172A non-enzymatic glucose sensing platform constructed by nano composite materials; (6)2016 International Journal of Electrochemical Science reports a reduced graphene oxide NiO/CuO-loaded nanocomposite and non-enzymatic electrochemical sensing performance of the nanocomposite on glucose. However, it relates to the preparation of carbon nanotube-supported NiCoO by hydrogen co-reductionxThe research on the composite material catalyst and the application of the composite material catalyst to the non-enzymatic electrochemical sensing of glucose is not reported in documents and patents.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a carbon nanotube-loaded NiCoO in non-enzymatic electrochemical glucose sensingxA composite catalyst, a preparation method and application thereof. The method has the advantages of simple process, few operation steps, mild and controllable conditions, and excellent electrochemical performance of the prepared material, and has good application prospect.
The technical scheme for realizing the purpose of the invention is as follows:
carbon nanotube-loaded NiCoO in non-enzymatic electrochemical glucose sensingxThe preparation method of the composite material catalyst is different from the prior art in that the preparation method comprises the following steps:
1) adding 10mg of acidified multi-walled carbon nano-tubes into a crucible filled with 5mL of absolute ethyl alcohol, performing ultrasonic treatment at normal temperature for 15 minutes, adding an aqueous solution of 0.1M cerium nitrate and 0.1M nickel nitrate, controlling the atomic ratio of Ni to Ce in the added cerium nitrate and nickel nitrate solution to be Ni: Ce to be 1:0.33-3, continuing to perform ultrasonic treatment to evaporate the liquid, and performing vacuum drying at 60 ℃ for later use;
2) putting the dried sample prepared in the step 1) into a tube furnace, and performing reaction in N2/H2In a mixed atmosphere of H2The volume percentage of the carbon nano tube is 10 percent, and the reaction is carried out for 0.5 to 7 hours at the temperature of between 100 and 500 ℃ to obtain the carbon nano tube loaded NiCoOxComposite material catalyst namely NiCoOx/MWCNTs。
The carbon nano tube loaded NiCoO prepared by the preparation methodxComposite material catalyst namely NiCoOx/MWCNTs。
The carbon nano tube loaded NiCoO prepared by the preparation methodxComposite material catalyst namely NiCoOxApplication of MWCNTs in non-enzymatic electrochemical glucose sensing.
Most of nickel-based bimetal oxide composite materials reported in the literature at present are prepared by a hydrothermal method, the process is complex and the time consumption is long, in the technical scheme, after mixed suspension of nickel nitrate, cerium nitrate and acidified carbon nanotubes is subjected to ultrasonic evaporation, the carbon nanotube-loaded NiCoO can be prepared by a hydrogen co-reduction methodxThe composite material catalyst has simple and easy-to-implement technological process, and obviously improves NiCoOxThe degree of dispersion of the nanoparticles and the electrocatalytic properties for glucose oxidation.
The technical scheme is that acidified carbon nano tubes are used as carriers, and NiCoO is deposited on the surfaces of the acidified carbon nano tubes by a hydrogen co-reduction methodxAnd (3) nanoparticles.
The technical scheme is that the carbon nano tube loaded NiCoO is prepared by taking the acidified carbon nano tube as a carrier through a hydrogen co-reduction methodxIn the composite material catalyst, bimetallic oxide nanoparticles of Ni and Ce are uniformly dispersed on the surface of the carbon nano tube, so that the electrocatalytic activity of the bimetallic oxide nanoparticles to glucose oxidation is obviously enhanced, and a non-enzymatic electrochemical glucose sensor constructed based on the composite material catalyst has the advantages of high sensitivity, wide linear range, low detection limit, good reproducibility, stability and anti-interference performance and the like.
The method has the advantages of simple process, few operation steps, mild and controllable conditions, and excellent electrochemical performance of the prepared material, and has good application prospect.
Drawings
FIG. 1 is a schematic diagram of the preparation of carbon nanotube-loaded NiCoO in the examplexA schematic flow diagram of the catalyst;
FIG. 2 is a schematic diagram of a carbon nanotube-supported NiCoO prepared in the examplexTEM images of the catalyst;
FIG. 3 shows NiCoO on carbon nanotube prepared in examplexA particle size histogram of the catalyst;
FIG. 4 is a NiCoO prepared in the examplexMWCNTs, NiO/MWCNTs and CeO2Cyclic voltammogram of the MWCNTs catalyst in a 0.1M NaOH solution containing 2mM glucose.
Detailed Description
The invention will be further elucidated with reference to the drawings and examples, without however being limited thereto.
Example (b):
referring to FIG. 1, a carbon nanotube loaded NiCoO in non-enzymatic electrochemical glucose sensingxThe preparation method of the composite material catalyst comprises the following steps:
1) adding 10mg of acidified multi-walled carbon nano-tubes into a crucible filled with 5mL of absolute ethyl alcohol, performing ultrasonic treatment at normal temperature for 15 minutes, adding an aqueous solution of 0.1M cerium nitrate and 0.1M nickel nitrate, controlling the atomic ratio of Ni to Ce in the added cerium nitrate and nickel nitrate solution to be Ni: Ce to be 1:0.33-3, continuing to perform ultrasonic treatment to evaporate the liquid, and performing vacuum drying at 60 ℃ for later use;
2) putting the dried sample prepared in the step 1) into a tube furnace, and performing reaction in N2/H2In a mixed atmosphere of H2The volume percentage of the carbon nano tube is 10 percent, and the reaction is carried out for 0.5 to 7 hours at the temperature of between 100 and 500 ℃ to obtain the carbon nano tube loaded NiCoOxComposite material catalyst namely NiCoOx/MWCNTs。
The carbon nano tube loaded NiCoO prepared by the preparation methodxComposite material catalyst namely NiCoOx/MWCNTs。
The carbon nano tube loaded NiCoO prepared by the preparation methodxComposite material catalyst namely NiCoOxApplication of MWCNTs in non-enzymatic electrochemical glucose sensing.
For comparison, CeO was also prepared under the same conditions in this example2MWCNTs and NiO/MWCNTs catalysts.
TEM analysis showed that NiCoO was present in the catalyst prepared according to the method of this examplexThe nanoparticles are uniformly distributed on the MWCNTs, the average particle size is 4.08nm, as shown in FIG. 2 and FIG. 3, and the NiCoO prepared in this example is shown in FIG. 2 and FIG. 3 respectivelyxTEM image and particle size statistical distribution diagram of/MWCNTs catalyst.
The NiCoO prepared in this example was compared by cyclic voltammetryxMWCNTs, NiO/MWCNTs and CeO2The electrocatalytic performance of the MWCNTs catalyst on glucose oxidation in a 0.1M NaOH solution containing 2mM of glucose shows that CeO2MWCNTs to grapeSugar oxidation is almost inactive, while NiCoOxThe MWCNTs showed the highest electrocatalytic activity for glucose oxidation, as shown in fig. 4, which fig. 4 gives the cyclic voltammogram of the different catalysts in a 0.1M NaOH solution containing 2mM glucose.
Based on NiCoO by continuous addition of glucose solutions of different concentrations in a 0.1M NaOH solution by chronoamperometryxThe result of an ampere response curve of a non-enzyme sensor constructed by the MWCNTs catalyst to glucose indicates that the sensor has high sensitivity to the detection of the glucose (315.64 mu A mM)-1cm-2) Wide linear range (3.21X 10)-22.12 mM) and low detection limit (9.5 mu M, S/N is 3), and the anti-interference performance of the prepared sensor is tested in 0.1M NaOH solution by a chronoamperometry method, and the result shows that common interference substances such as L-arginine, hydrogen peroxide, ascorbic acid, dopamine, sodium chloride and uric acid have no obvious influence on the detection of glucose.
The glucose concentration in the actual serum samples is detected by a chronoamperometry method, the glucose concentration test results of the three serum samples are similar to the actual values provided by hospitals, the relative standard deviations are 1.4%, 2.26% and 2.53%, respectively, and the recovery rates are 100.8%, 101.4% and 99.6%, respectively, indicating that the sample is based on NiCoOxThe sensor constructed by the MWCNTs catalyst has high detection reliability when being used for an actual sample, and the result is satisfactory.
Claims (3)
1. Carbon nanotube-loaded NiCoO in non-enzymatic electrochemical glucose sensingxThe preparation method of the composite material catalyst is characterized by comprising the following steps:
1) adding 10mg of acidified multi-walled carbon nano-tubes into a crucible filled with 5mL of absolute ethyl alcohol, performing ultrasonic treatment at normal temperature for 15 minutes, adding a 0.1M cerium nitrate and 0.1M nickel nitrate aqueous solution, controlling the atomic ratio of Ni to Ce in the added cerium nitrate and nickel nitrate solution to be Ni: Ce =1:0.33-3, continuing ultrasonic treatment to evaporate the liquid, and performing vacuum drying at 60 ℃ for later use;
2) putting the dried sample prepared in the step 1) into a tube furnace, and performing reaction in N2/H2In a mixed atmosphere of H2The volume percentage of the carbon nano tube is 10 percent, and the reaction is carried out for 0.5 to 7 hours at the temperature of between 100 and 500 ℃ to obtain the carbon nano tube loaded NiCoOxComposite material catalyst namely NiCoOx/MWCNTs。
2. The method of claim 1, wherein the carbon nanotubes of the NiCoO carrier are prepared by the same method as that of the above methodxComposite material catalyst namely NiCoOx/MWCNTs。
3. The preparation method of claim 2, wherein the carbon nanotube-supported NiCoO is prepared by the methodxComposite material catalyst namely NiCoOxApplication of MWCNTs in non-enzymatic electrochemical glucose sensing.
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| US7118668B1 (en) * | 2002-03-07 | 2006-10-10 | Bayer Healthcare Llc | Electrochemical test sensor |
| CN104614425A (en) * | 2015-01-21 | 2015-05-13 | 广西师范大学 | Preparation and application of Cu2O hexagram microcrystal composite material adopting functionalized carbon nano tubes as carrier |
| CN105424774A (en) * | 2015-10-23 | 2016-03-23 | 西北大学 | Enzyme-free glucose electrochemical sensor electrode and preparation method and application thereof |
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| Title |
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