CN111665284A - Application of doped graphene as sensing material - Google Patents
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- CN111665284A CN111665284A CN201910175243.1A CN201910175243A CN111665284A CN 111665284 A CN111665284 A CN 111665284A CN 201910175243 A CN201910175243 A CN 201910175243A CN 111665284 A CN111665284 A CN 111665284A
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- electrode
- graphene
- glucose
- buffer solution
- phosphate buffer
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 48
- 239000011540 sensing material Substances 0.000 title claims abstract description 13
- 239000008055 phosphate buffer solution Substances 0.000 claims abstract description 27
- 239000004366 Glucose oxidase Substances 0.000 claims abstract description 24
- 108010015776 Glucose oxidase Proteins 0.000 claims abstract description 24
- 229940116332 glucose oxidase Drugs 0.000 claims abstract description 24
- 235000019420 glucose oxidase Nutrition 0.000 claims abstract description 24
- 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 claims abstract description 22
- 239000008103 glucose Substances 0.000 claims abstract description 22
- 239000007789 gas Substances 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910021397 glassy carbon Inorganic materials 0.000 claims abstract description 11
- 239000010453 quartz Substances 0.000 claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000002484 cyclic voltammetry Methods 0.000 claims abstract description 6
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000007772 electrode material Substances 0.000 claims abstract description 6
- 239000003792 electrolyte Substances 0.000 claims abstract description 6
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 229910052786 argon Inorganic materials 0.000 claims description 10
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 2
- 239000005977 Ethylene Substances 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 7
- 238000001514 detection method Methods 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 4
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 229960003638 dopamine Drugs 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000004557 single molecule detection Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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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
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
-
- 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
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3271—Amperometric enzyme electrodes for analytes in body fluids, e.g. glucose in blood
-
- 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
- G01N27/416—Systems
-
- 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
- G01N27/416—Systems
- G01N27/4166—Systems measuring a particular property of an electrolyte
- G01N27/4168—Oxidation-reduction potential, e.g. for chlorination of water
Abstract
The invention belongs to the field of sensors, and particularly relates to application of doped graphene as a sensing material. The method comprises the following steps of 1) modifying an electrode material by graphene, placing a glassy carbon electrode in a quartz tube, and introducing a carbon source gas and hydrogen; 2) preparing a sensing electrode, namely dropwise adding glucose oxidase phosphate buffer solution to the graphene modified electrode obtained in the step 1); 3) and (3) forming a three-electrode system by the sensing electrode prepared in the step 2), the saturated calomel electrode and the platinum sheet electrode to serve as a sensor, adding glucose into a phosphate buffer solution to form electrolyte, performing cyclic voltammetry scanning, and enabling the redox peak current on the CV curve to be changed regularly along with the concentration of the glucose, so that the glucose concentration is tested. The graphene and graphene oxide composite material and glucose oxidase composite modified electrode has good glucose detection performance, and has the characteristics of high sensitivity, wide detection range, good anti-interference property and the like.
Description
Technical Field
The invention belongs to the field of sensors, and particularly relates to application of doped graphene as a sensing material.
Background
Graphene is a polymer made of carbon atoms in sp2The hybrid tracks form a hexagonal honeycomb lattice two-dimensional carbon nanomaterial. The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future. Common graphene powderThe production method is a mechanical stripping method, an oxidation-reduction method and a SiC epitaxial growth method, and the film production method is a Chemical Vapor Deposition (CVD) method.
The sensitivity of graphene chemical probes is comparable to the limit of single molecule detection. The unique two-dimensional structure of graphene makes it very sensitive to the surrounding environment. Graphene is an ideal material for an electrochemical biosensor, and a sensor made of graphene has good sensitivity in medical detection of dopamine, glucose and the like.
Disclosure of Invention
The invention aims to provide application of doped graphene as a sensing material.
In order to achieve the purpose, the invention adopts the following technical scheme:
the application of doped graphene as a sensing material comprises the following steps:
1) modifying an electrode material by graphene, placing a glassy carbon electrode in a quartz tube, heating the quartz tube to 600-1200 ℃ under the protection of argon, and preserving heat for 20 min; introducing carbon source gas and hydrogen gas in the heat preservation process, and after the reaction is finished, introducing argon gas and cooling to room temperature to obtain a graphene modified electrode;
2) preparing a sensing electrode, namely dropwise adding glucose oxidase phosphate buffer solution to the graphene modified electrode obtained in the step 1); soaking the glassy carbon electrode dried at room temperature in a phosphate buffer solution to remove glucose oxidase which is not firmly combined with graphene oxide, taking out and drying at room temperature to obtain a sensing electrode;
3) and (3) forming a three-electrode system by the sensing electrode prepared in the step 2), a saturated calomel electrode and a platinum sheet electrode as a sensor, adding glucose into 0.05-0.5 mol/L phosphate buffer solution to form electrolyte, performing cyclic voltammetry scanning on an electrochemical workstation within a voltage range of 0.6-0.6V, and enabling the redox peak current on a CV curve to be changed regularly along with the concentration of glucose, thereby realizing the test of the concentration of the glucose.
The ratio of the carbon source gas to the hydrogen gas in the step 1) is 1: 10.
The carbon source gas in the step 1) is one or a mixture of more than one of acetylene, methane and ethylene.
In the step 2), the concentration of the glucose oxidase in the phosphate buffer solution is 5-30 mg/ml, and the dosage of the phosphate buffer solution of the glucose oxidase is 1-20 mul.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the modified electrode provided by the invention is simple, the graphene has excellent conductivity and good biocompatibility, and the graphene oxide is beneficial to fixing of glucose oxidase. The graphene and graphene oxide composite material and glucose oxidase composite modified electrode has the advantages of being good in glucose detection performance, high in sensitivity, wide in detection range, good in anti-interference property and the like, and can be used for preparing a novel glucose sensor. The preparation method is simple and feasible, and is easy to realize large-scale production.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the following preferred embodiments.
Example 1: the application of doped graphene as a sensing material comprises the following steps:
1) modifying an electrode material by graphene, placing a glassy carbon electrode in a quartz tube, heating the quartz tube to 800 ℃ under the protection of argon, and preserving heat for 20 min; introducing carbon source gas acetylene and hydrogen in the heat preservation process, wherein the ratio of the carbon source gas to the hydrogen is 1: 10; after the reaction is finished, introducing argon gas, and cooling to room temperature to obtain a graphene modified electrode;
2) preparing a sensing electrode, namely dropwise adding glucose oxidase phosphate buffer solution to the graphene modified electrode obtained in the step 1); soaking the glassy carbon electrode dried at room temperature in a phosphate buffer solution to remove glucose oxidase which is not firmly combined with graphene oxide, taking out and drying at room temperature to obtain a sensing electrode; in the step 2), the concentration of the glucose oxidase in the phosphate buffer solution is 20mg/ml, and the dosage of the phosphate buffer solution of the glucose oxidase is 10 mul.
3) And (3) forming a three-electrode system by the sensing electrode prepared in the step 2), a saturated calomel electrode and a platinum sheet electrode as a sensor, adding glucose into 0.05-0.5 mol/L phosphate buffer solution to form electrolyte, performing cyclic voltammetry scanning on an electrochemical workstation within a voltage range of 0.6-0.6V, and enabling the redox peak current on a CV curve to be changed regularly along with the concentration of glucose, thereby realizing the test of the concentration of the glucose.
Example 2: the application of doped graphene as a sensing material comprises the following steps:
1) modifying an electrode material by graphene, placing a glassy carbon electrode in a quartz tube, heating the quartz tube to 600 ℃ under the protection of argon, and preserving heat for 20 min; introducing carbon source gas acetylene and hydrogen in the heat preservation process, wherein the ratio of the carbon source gas to the hydrogen is 1: 10; after the reaction is finished, introducing argon gas, and cooling to room temperature to obtain a graphene modified electrode;
2) preparing a sensing electrode, namely dropwise adding glucose oxidase phosphate buffer solution to the graphene modified electrode obtained in the step 1); soaking the glassy carbon electrode dried at room temperature in a phosphate buffer solution to remove glucose oxidase which is not firmly combined with graphene oxide, taking out and drying at room temperature to obtain a sensing electrode; the concentration of the glucose oxidase in the phosphate buffer solution is 5mg/ml, and the dosage of the phosphate buffer solution of the glucose oxidase is 20 mul.
3) And (3) forming a three-electrode system by the sensing electrode prepared in the step 2), a saturated calomel electrode and a platinum sheet electrode as a sensor, adding glucose into 0.05-0.5 mol/L phosphate buffer solution to form electrolyte, performing cyclic voltammetry scanning on an electrochemical workstation within a voltage range of 0.6-0.6V, and enabling the redox peak current on a CV curve to be changed regularly along with the concentration of glucose, thereby realizing the test of the concentration of the glucose.
Example 3: the application of doped graphene as a sensing material comprises the following steps:
1) modifying an electrode material by graphene, placing a glassy carbon electrode in a quartz tube, heating the quartz tube to 1200 ℃ under the protection of argon, and preserving heat for 20 min; introducing carbon source gas acetylene and hydrogen in the heat preservation process, wherein the ratio of the carbon source gas to the hydrogen is 1: 10; after the reaction is finished, introducing argon gas, and cooling to room temperature to obtain a graphene modified electrode;
2) preparing a sensing electrode, namely dropwise adding glucose oxidase phosphate buffer solution to the graphene modified electrode obtained in the step 1); soaking the glassy carbon electrode dried at room temperature in a phosphate buffer solution to remove glucose oxidase which is not firmly combined with graphene oxide, taking out and drying at room temperature to obtain a sensing electrode; the concentration of glucose oxidase in phosphate buffer solution was 30mg/ml, and the amount of glucose oxidase phosphate buffer solution was 1. mu.l.
3) And (3) forming a three-electrode system by the sensing electrode prepared in the step 2), a saturated calomel electrode and a platinum sheet electrode as a sensor, adding glucose into 0.05-0.5 mol/L phosphate buffer solution to form electrolyte, performing cyclic voltammetry scanning on an electrochemical workstation within a voltage range of 0.6-0.6V, and enabling the redox peak current on a CV curve to be changed regularly along with the concentration of glucose, thereby realizing the test of the concentration of the glucose.
The above description is only a preferred embodiment of the present invention, and for those skilled in the art, the present invention should not be limited by the description of the present invention, which should be interpreted as a limitation.
Claims (4)
1. The application of doped graphene as a sensing material is characterized by comprising the following steps:
1) modifying an electrode material by graphene, placing a glassy carbon electrode in a quartz tube, heating the quartz tube to 600-1200 ℃ under the protection of argon, and preserving heat for 20 min; introducing carbon source gas and hydrogen gas in the heat preservation process, and after the reaction is finished, introducing argon gas and cooling to room temperature to obtain a graphene modified electrode;
2) preparing a sensing electrode, namely dropwise adding glucose oxidase phosphate buffer solution to the graphene modified electrode obtained in the step 1); soaking the glassy carbon electrode dried at room temperature in a phosphate buffer solution to remove glucose oxidase which is not firmly combined with graphene oxide, taking out and drying at room temperature to obtain a sensing electrode;
3) and (3) forming a three-electrode system by the sensing electrode prepared in the step 2), a saturated calomel electrode and a platinum sheet electrode as a sensor, adding glucose into 0.05-0.5 mol/L phosphate buffer solution to form electrolyte, performing cyclic voltammetry scanning on an electrochemical workstation within a voltage range of 0.6-0.6V, and enabling the redox peak current on a CV curve to be changed regularly along with the concentration of glucose, thereby realizing the test of the concentration of the glucose.
2. The application of the doped graphene as a sensing material according to claim 1, wherein the ratio of the carbon source gas to the hydrogen gas in the step 1) is 1: 10.
3. The application of the doped graphene as a sensing material according to claim 1, wherein the carbon source gas in step 1) is one or more of acetylene, methane and ethylene.
4. The application of the doped graphene as the sensing material according to claim 1, wherein the concentration of glucose oxidase in the phosphate buffer solution in the step 2) is 5-30 mg/ml, and the dosage of the phosphate buffer solution of glucose oxidase is 1-20 μ l.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910175243.1A CN111665284A (en) | 2019-03-08 | 2019-03-08 | Application of doped graphene as sensing material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910175243.1A CN111665284A (en) | 2019-03-08 | 2019-03-08 | Application of doped graphene as sensing material |
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| CN111665284A true CN111665284A (en) | 2020-09-15 |
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| CN201910175243.1A Pending CN111665284A (en) | 2019-03-08 | 2019-03-08 | Application of doped graphene as sensing material |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220566A (en) * | 2011-06-09 | 2011-10-19 | 无锡第六元素高科技发展有限公司 | Method for preparing single-layer or multi-layer graphene through chemical vapor deposition |
| CN102636540A (en) * | 2012-04-19 | 2012-08-15 | 湖南大学 | Glucose detection sensor, and preparation and application methods thereof |
| CN103529099A (en) * | 2013-09-23 | 2014-01-22 | 西南交通大学 | Method for preparing graphene chemically modified electrode through in-situ growth |
| US20150004329A1 (en) * | 2013-06-28 | 2015-01-01 | King Abdulaziz City For Science And Technology | Short-time growth of large-grain hexagonal graphene and methods of manufacture |
| CN107436316A (en) * | 2016-05-25 | 2017-12-05 | 中国科学院金属研究所 | The preparation of glucose sensor based on graphene and graphene oxide composite material |
| WO2019024396A1 (en) * | 2017-08-03 | 2019-02-07 | 中国科学院大连化学物理研究所 | Metallic single atom-embedded graphene material, and preparation method therefor and application thereof |
| WO2019031845A1 (en) * | 2017-08-08 | 2019-02-14 | 한국화학연구원 | Graphene electrode-based glucose sensor for in vitro diagnosis |
-
2019
- 2019-03-08 CN CN201910175243.1A patent/CN111665284A/en active Pending
Patent Citations (7)
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| CN102636540A (en) * | 2012-04-19 | 2012-08-15 | 湖南大学 | Glucose detection sensor, and preparation and application methods thereof |
| US20150004329A1 (en) * | 2013-06-28 | 2015-01-01 | King Abdulaziz City For Science And Technology | Short-time growth of large-grain hexagonal graphene and methods of manufacture |
| CN103529099A (en) * | 2013-09-23 | 2014-01-22 | 西南交通大学 | Method for preparing graphene chemically modified electrode through in-situ growth |
| CN107436316A (en) * | 2016-05-25 | 2017-12-05 | 中国科学院金属研究所 | The preparation of glucose sensor based on graphene and graphene oxide composite material |
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