CN102621208A - Preparation method and application of three-dimensional graphene electrode for electrochemical biosensor - Google Patents
Preparation method and application of three-dimensional graphene electrode for electrochemical biosensor Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a three-dimensional graphene electrode for an electrochemical biosensor. The preparation method comprises the following steps of: fixing spongy graphene in which industrially produced foam nickel is taken as a substrate and which has a three-dimensional structure and is synthesized through chemical vapor deposition on a glass or quartz sheet; connecting the spongy graphene with the three-dimensional structure and a wire by using a silver conductive adhesive; and coating organic silica gel on a connection point of the metal wire and the graphene for insulation to obtain a spongy graphene electrochemical electrode with the three-dimensional structure. The three-dimensional spongy graphene electrode has the outstanding characteristics of high conductivity, high specific surface area, high electrochemical stability and the like, is easily subjected to surface functional modification, and has high detection sensitivity to dopamine and nicotinamide adenine dinucleotide; and a highly sensitive electrochemical biosensor for non-enzymatically and selectively detecting glucose can be obtained after the surface of the electrode is modified by Co3O4.
Description
Technical field
The present invention relates to a kind of preparation method of the three-dimensional spongy Graphene electrodes that is used for the electrochemica biological sensing and in the application of electrochemica biological sensory field.
Background technology
Electrochemica biological sensor plays crucial effects in current highly sensitive biomolecule detection, clinical medicine and genetic engineering research field.Wherein, The conductivity of electrochemical electrode, specific surface area and and with the compatibility of biomolecule be the key that influences electrochemica biological sensor detection sensitivity and detection limit, its performance to the application of expansion electrochemica biological sensor with guarantee that its stable operation is most important.Yet traditional glass-carbon electrode exists poorly conductive, surface to be difficult to shortcomings such as functional modification and specific surface area be low, makes that electrochemica biological sensor is low to the detection sensitivity of biomolecule, specific selectivity is poor.Graphene is a kind of novel carbon nanomaterial as Nobel prize for physics achievement in research appearance in 2010; It is the bi-dimensional cellular shape crystal structure by the monolayer carbon atomic building; Have the electron mobility of superelevation, big specific surface area and excellent physics, chemistry, optics and mechanical property; In field effect transistor, nanoelectronic bio-sensing, transparent conductive film, prepare composite boundless application prospect is arranged; Wherein the Graphene modified glassy carbon electrode has obtained extensive studies in the bio-sensing field, and the result who announces like patent of invention CN 201110112989 shows that the Graphene modified glassy carbon can detect rutin and Quercetin simultaneously; The result that patent of invention CN 200910084344.4 announces proves that the film modified glass-carbon electrode of Graphene/Nafion can realize the Sensitive Detection of dopamine; But these method of modifying based on graphene oxide make Graphene reunite easily, are difficult to effectively bring into play the characteristic of big specific surface area of Graphene and high conductivity.
The spongy Graphene of three-dimensional structure has Stability Analysis of Structures, good conductivity, specific surface area and realizes characteristics such as surface-functionalized modification greatly, easily, is the ideal electrode material of preparation high sensitive electrochemical biology sensor.Yet, study report that it is used at the electrochemica biological sensory field after finding as yet at present to utilize the spongy Graphene of three-dimensional structure directly to prepare electrochemical electrode and functionalization.
Summary of the invention
Technical matters:The purpose of this invention is to provide a kind of preparation method of the three-dimensional spongy Graphene electrodes that is used for the electrochemica biological sensing and in the application of electrochemica biological sensory field.
Technical scheme:A kind of method for preparing three-dimensional spongy Graphene electrochemical electrode provided by the present invention and in the application of electrochemica biological sensory field, the preparation method comprises following preparation process:
1) chemical vapor deposition is the synthetic spongy graphene film of three-dimensional structure is fixed on glass sheet or piezoid surface with organic silica gel;
2) with conductive silver glue glue the spongy Graphene of three-dimensional is connected with plain conductor;
3) tie point that organic silica gel is applied to plain conductor and Graphene insulate, and solidifies the back and forms the three-dimensional spongy Graphene electrodes of non-functionalized;
4) with CoCl
26H
2O, urea, H
2O adds in the agitated reactor, after stirring, puts into the glass sheet or the piezoid that are loaded with three-dimensional spongy graphene film, and 100-200 ℃ was reacted 5 ~ 20 hours.
5) the spongy graphene film that is loaded in glass sheet or piezoid surface after will reacting with distilled water flushing 3-6 time after, in baking oven after the oven dry, put into muffle furnace 300-500 ℃ roasting 1-5 hour, the spongy Graphene electrodes of formation functionalization three-dimensional.
The spongy graphene film of described three-dimensional is that diameter is that the disk or the length of side of 0.1 ~ 5cm is the square or rectangular of 0.1 ~ 5cm.
Described plain conductor material is copper or titanium or silver.
The three-dimensional spongy Graphene electrodes of described non-functionalized can be carried out the Electrochemical Detection of dopamine, NADH, uric acid.
The no enzyme that the three-dimensional spongy Graphene electrochemical electrode of described functionalization can carry out glucose detects.
The selectivity that the three-dimensional spongy Graphene electrochemical electrode of described functionalization can carry out glucose, uric acid and ascorbic acid in the blood plasma does not have enzyme and detects.
Beneficial effect:Compare with existing electrochemical electrode biosensor technique, the invention has the advantages that
1, the present invention discloses a kind of novel three-dimensional spongy Graphene electrochemical electrode preparation method first, and this technology for preparing electrode is simple, cheap, be easy to realize scale preparation;
2, the prepared three-dimensional spongy Graphene electrochemical electrode conductivity of the present invention is high, specific surface area is big, electrochemical stability good, detection sensitivity is high;
3, the prepared easy functional modification in three-dimensional spongy Graphene electrochemical electrode surface of the present invention is realized the highly sensitive and high specific selectivity of different biological molecules is detected.
Description of drawings
Fig. 1. be the optical photograph of the three-dimensional spongy Graphene electrochemical electrode of preparation among the embodiment 1.
Fig. 2. be the three-dimensional spongy Graphene electrochemical electrode of preparation among the embodiment 1 and the comparison of traditional glass-carbon electrode cyclic voltammetry curve and impedance.
Fig. 3. the three-dimensional spongy Graphene electrochemical electrode for preparing for the present invention among the embodiment 2 is 5.6 o'clock detection limits to dopamine in signal to noise ratio (S/N ratio).
Fig. 4. detect the cyclic voltammetry curve of dopamine and uric acid simultaneously for the spongy Graphene electrochemical electrode of three-dimensional structure of the present invention's preparation among the embodiment 3.
Fig. 5. be the Co of the present invention's preparation among the embodiment 5
3O
4The SEM photo of the three-dimensional Graphene electrochemical electrode of functionalization and to the no enzyme detection time-map of current of glucose.
Fig. 6. for the three-dimensional spongy Graphene electrochemical electrode of the present invention preparation among the embodiment 6 through Co
3O
4Modify time-map of current that the back is detected glucose, uric acid, ascorbic acid selectivity in the blood plasma.
Embodiment
Below in conjunction with accompanying drawing and instantiation the present invention is elaborated.
Embodiment 1:
The spongy graphene film of three-dimensional structure that chemical vapor deposition is synthetic uses 0.2mL concentration to be fixed on glass sheet surface as the organic silica gel of 48g/L;
Conductive silver glue glue 0.2mg is connected three-dimensional Graphene under 20 ℃ with plain conductor one end, tack time is 5 minutes;
The tie point that the organic silica gel of 20mg is applied to plain conductor and Graphene insulate, and be 5 hours set time, forms the three-dimensional spongy Graphene electrodes of non-functionalized;
Three-dimensional spongy graphene film is that the length of side is the square of 0.5cm.
The plain conductor material is a titanium.
Fig. 1 is the optical photograph of the three-dimensional spongy Graphene electrodes of method for preparing; Fig. 2 is the three-dimensional spongy Graphene electrodes of method for preparing and the comparison of traditional glass-carbon electrode cyclic voltammetry curve and impedance.
Embodiment 2:
The spongy graphene film of three-dimensional structure that chemical vapor deposition is synthetic uses 0.2mL concentration to be fixed on the piezoid surface as the organic silica gel of 48g/L;
Conductive silver glue glue 0.3mg is connected three-dimensional Graphene under 25 ℃ with plain conductor one end, tack time is 10 minutes;
The tie point that the organic silica gel of 35mg is applied to plain conductor and Graphene insulate, and be 12 hours set time, forms the three-dimensional spongy Graphene electrodes of non-functionalized.
The spongy graphene film of three-dimensional structure is the disk of diameter 2cm.
The plain conductor material is a copper.
Fig. 3 carries out time-map of current that dopamine detects for the three-dimensional spongy Graphene utmost point of above-mentioned non-functionalized.
Embodiment 3:
The spongy graphene film of three-dimensional structure that chemical vapor deposition is synthetic uses 0.2mL concentration to be fixed on the piezoid surface as the organic silica gel of 48g/L;
Conductive silver glue glue 0.3mg is connected three-dimensional Graphene under 25 ℃ with plain conductor one end, tack time is 10 minutes;
The tie point that the organic silica gel of 50mg is applied to plain conductor and Graphene insulate, and be 12 hours set time, forms the three-dimensional spongy Graphene electrodes of non-functionalized.
The spongy graphene film of three-dimensional structure is that the length of side is the square of 0.5cm.
The plain conductor material is a silver.
Fig. 4 carries out the galvanochemistry cyclic voltammetry curve that dopamine and uric acid detect simultaneously for the three-dimensional spongy Graphene utmost point of above-mentioned non-functionalized.
Embodiment 4:
The spongy graphene film of three-dimensional structure that chemical vapor deposition is synthetic uses 0.2mL concentration to be fixed on the piezoid surface as the organic silica gel of 48g/L;
Conductive silver glue glue 0.3mg is connected three-dimensional Graphene under 25 ℃ with plain conductor one end, tack time is 10 minutes;
The tie point that the organic silica gel of 50mg is applied to plain conductor and Graphene insulate, and be 12 hours set time, forms the three-dimensional spongy Graphene electrodes of non-functionalized.
The spongy graphene film of three-dimensional structure is that the length of side is the square of 1cm.
The plain conductor material is a titanium.
The three-dimensional spongy Graphene utmost point of above-mentioned non-functionalized can carry out the detection of NADH, and its detection limit reaches 50nM.
Embodiment 5:
The spongy graphene film of three-dimensional structure that chemical vapor deposition is synthetic uses 0.2mL concentration to be fixed on glass sheet surface as the organic silica gel of 48g/L;
Conductive silver glue glue 0.4mg is connected three-dimensional Graphene under 25 ℃ with plain conductor one end, tack time is 20 minutes;
The tie point that the organic silica gel of 100mg is applied to plain conductor and Graphene insulate, and be 24 hours set time, forms the three-dimensional spongy Graphene electrodes of non-functionalized;
With 0.3g CoCl
26H
2O, 0.04g urea, 24gH
2O adds in the agitated reactor of 0.05L, and glass bar stirred after 3 minutes, put into the glass sheet that is loaded with spongy graphene film, and 120 ℃ were reacted 10 hours.
With the reacted glass sheet that is loaded with spongy graphene film with distilled water flushing 5 times after, oven dry 5 hours in 40 ℃ is last in baking oven, puts into 400 ℃ of roastings of muffle furnace 2 hours, forms the three-dimensional spongy Graphene electrodes of functionalization.
The spongy graphene film of three-dimensional structure is the square of length of side 1cm.
The plain conductor material is a titanium.
Fig. 5 is the SEM picture and the time-map of current of carrying out the no enzyme detection of grape sugar of the three-dimensional spongy Graphene electrodes of above-mentioned non-functionalized.
Embodiment 6:
The spongy graphene film of three-dimensional structure that chemical vapor deposition is synthetic uses 0.4mL concentration to be fixed on glass sheet or piezoid surface as the organic silica gel of 48g/L;
Conductive silver glue glue 1mg is connected three-dimensional Graphene under 20 ℃ with plain conductor one end, tack time is 30 minutes;
The tie point that the organic silica gel of 120mg is applied to plain conductor and Graphene insulate, and be 24 hours set time, forms the three-dimensional spongy Graphene electrodes of non-functionalized;
With 0.24g CoCl
26H2O, 0.06g urea, 24gH
2O adds in the agitated reactor of 0.05L, and glass bar stirred after 5 minutes, put into the glass sheet that is loaded with spongy graphene film, and 120 ℃ were reacted 16 hours.
With the reacted glass sheet that is loaded with spongy graphene film or piezoid with distilled water flushing 5 times after, oven dry 4 hours in 50 ℃ is last in baking oven, puts into 450 ℃ of roastings of muffle furnace 2 hours, forms the three-dimensional spongy Graphene electrodes of functionalization.
The square that the spongy graphene film length of side of three-dimensional structure is 1cm.
The plain conductor material is a silver.
Fig. 6 does not have enzyme detection time-map of current for the selectivity that the three-dimensional spongy Graphene electrodes of above-mentioned functionsization is carried out glucose, uric acid and ascorbic acid in the blood plasma.
Claims (6)
1. the preparation method of the three-dimensional Graphene electrodes of an electrochemica biological sensing is characterized in that this method may further comprise the steps:
1). the spongy graphene film of three-dimensional structure that chemical vapor deposition is synthetic is fixed on glass sheet or piezoid surface with organic silica gel;
2). with conductive silver glue glue three-dimensional Graphene is connected with plain conductor one end;
3). the tie point that organic silica gel is applied to plain conductor and Graphene insulate, and solidifies the back and forms the three-dimensional spongy Graphene electrodes of non-functionalized;
4). with CoCl
26H
2O, urea and H
2O adds in the agitated reactor, puts into the glass sheet or the piezoid that are loaded with spongy graphene film after stirring, and 100-200 ℃ was reacted 5 ~ 20 hours;
5). be loaded in after will reacting glass sheet or piezoid the surface spongy graphene film with distilled water flushing 3-6 time after; In baking oven, put into muffle furnace after the oven dry; At 300-500 ℃ of following roasting 1-5 hour, form the three-dimensional spongy Graphene electrochemical electrode of functionalization.
2. the preparation method of the three-dimensional Graphene electrodes of electrochemica biological sensing according to claim 1 is characterized in that the spongy graphene film of described three-dimensional structure is that diameter is that the disk or the length of side of 0.1 ~ 5cm is the square or rectangular of 0.1 ~ 5cm.
3. the three-dimensional Graphene electrodes preparation method who is used for the electrochemica biological sensing according to claim 1 is characterized in that described plain conductor, and material is copper, titanium or silver.
4. application that is used for the three-dimensional Graphene electrodes of electrochemica biological sensing as claimed in claim 1 is characterized in that the three-dimensional spongy Graphene electrodes of described non-functionalized can carry out the Electrochemical Detection of dopamine, NADH and uric acid.
5. application that is used for the three-dimensional Graphene electrodes of electrochemica biological sensing as claimed in claim 1 is characterized in that the three-dimensional spongy Graphene electrochemical electrode of described functionalization can carry out the no enzyme detection of glucose.
6. the application that is used for the three-dimensional Graphene electrodes of electrochemica biological sensing according to claim 5 is characterized in that selectivity that the three-dimensional spongy Graphene electrochemical electrode of described functionalization can carry out glucose, uric acid and ascorbic acid in the blood plasma do not have enzyme and detect.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103076375A (en) * | 2012-12-21 | 2013-05-01 | 吉林大学 | Preparation method and application of coaxial entity/nano porous gold/Co3O4 compound electrode material |
| CN103257168A (en) * | 2013-01-31 | 2013-08-21 | 浙江工业大学 | Acetylcholine esterase electrode adopting foam nickel as carrier, and applications thereof |
| CN103424447A (en) * | 2013-08-22 | 2013-12-04 | 中国科学院上海微系统与信息技术研究所 | Nano-particle enhancement detection device based on non-modified monolayer graphene being used as working electrode and application thereof |
| CN104062339A (en) * | 2014-07-09 | 2014-09-24 | 华南师范大学 | [Ru(tatp)3]<2+> modified electrode and method for detecting glucose, uric acid and ascorbic acid in blood by adopting electrode |
| CN104807861A (en) * | 2015-04-09 | 2015-07-29 | 山东师范大学 | Preparation method of spongy graphene-based stretchable gas sensor |
| CN105936525A (en) * | 2016-05-24 | 2016-09-14 | 安徽普氏生态环境工程有限公司 | Production method of novel graphene electrode used for sewage treatment |
| CN106525915A (en) * | 2016-09-30 | 2017-03-22 | 山东师范大学 | Support vector machine based foamed graphene sensor sample detection method and system |
| CN104760949B (en) * | 2014-01-08 | 2017-04-05 | 奈创科技股份有限公司 | Graphene generating means |
| CN107462620A (en) * | 2017-08-23 | 2017-12-12 | 齐齐哈尔大学 | Glucose sensor electrode based on graphene/ZnO/ nickel foam nano composite materials |
| CN109239150A (en) * | 2018-08-07 | 2019-01-18 | 山东大学 | A kind of Co with high sensitivity3O4Porous nano-sheet non-enzymatic base glucose sensor and preparation method thereof |
| CN109975380A (en) * | 2019-03-28 | 2019-07-05 | 山东师范大学 | Magnetic control graphene field effect tube sensor and its production, measurement and detection method |
| CN110404544A (en) * | 2019-07-26 | 2019-11-05 | 华东理工大学 | A kind of bimetallic catalytic material and its preparation method and application method |
| CN110907502A (en) * | 2018-09-17 | 2020-03-24 | 中国科学院大连化学物理研究所 | Aniline sensor taking three-dimensional foamy graphene material as sensing film |
| CN111780901A (en) * | 2020-06-29 | 2020-10-16 | 复旦大学 | Spider-web-like flexible tactile sensor capable of simultaneously detecting force magnitude and direction |
| CN112730562A (en) * | 2020-12-22 | 2021-04-30 | 河南中泽生物工程有限公司 | Electrochemical immunosensor for detecting tiamulin antigen and preparation method thereof |
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| CN103076375A (en) * | 2012-12-21 | 2013-05-01 | 吉林大学 | Preparation method and application of coaxial entity/nano porous gold/Co3O4 compound electrode material |
| CN103257168A (en) * | 2013-01-31 | 2013-08-21 | 浙江工业大学 | Acetylcholine esterase electrode adopting foam nickel as carrier, and applications thereof |
| CN103257168B (en) * | 2013-01-31 | 2015-04-22 | 浙江工业大学 | Acetylcholine esterase electrode adopting foam nickel as carrier, and applications thereof |
| CN103424447B (en) * | 2013-08-22 | 2015-05-13 | 中国科学院上海微系统与信息技术研究所 | Nano-particle enhancement detection device based on non-modified monolayer graphene being used as working electrode and application thereof |
| CN103424447A (en) * | 2013-08-22 | 2013-12-04 | 中国科学院上海微系统与信息技术研究所 | Nano-particle enhancement detection device based on non-modified monolayer graphene being used as working electrode and application thereof |
| CN104760949B (en) * | 2014-01-08 | 2017-04-05 | 奈创科技股份有限公司 | Graphene generating means |
| CN104062339B (en) * | 2014-07-09 | 2016-08-31 | 华南师范大学 | [Ru (tatp) 3] 2+ modified electrode and the method being used for detecting glucose in blood, uric acid and ascorbic acid thereof |
| CN104062339A (en) * | 2014-07-09 | 2014-09-24 | 华南师范大学 | [Ru(tatp)3]<2+> modified electrode and method for detecting glucose, uric acid and ascorbic acid in blood by adopting electrode |
| CN104807861B (en) * | 2015-04-09 | 2017-05-24 | 山东师范大学 | Preparation method of spongy graphene-based stretchable gas sensor |
| CN104807861A (en) * | 2015-04-09 | 2015-07-29 | 山东师范大学 | Preparation method of spongy graphene-based stretchable gas sensor |
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| CN106525915A (en) * | 2016-09-30 | 2017-03-22 | 山东师范大学 | Support vector machine based foamed graphene sensor sample detection method and system |
| CN107462620A (en) * | 2017-08-23 | 2017-12-12 | 齐齐哈尔大学 | Glucose sensor electrode based on graphene/ZnO/ nickel foam nano composite materials |
| CN109239150A (en) * | 2018-08-07 | 2019-01-18 | 山东大学 | A kind of Co with high sensitivity3O4Porous nano-sheet non-enzymatic base glucose sensor and preparation method thereof |
| CN109239150B (en) * | 2018-08-07 | 2019-09-10 | 山东大学 | A kind of Co with high sensitivity3O4Porous nano-sheet non-enzymatic base glucose sensor and preparation method thereof |
| CN110907502A (en) * | 2018-09-17 | 2020-03-24 | 中国科学院大连化学物理研究所 | Aniline sensor taking three-dimensional foamy graphene material as sensing film |
| CN109975380A (en) * | 2019-03-28 | 2019-07-05 | 山东师范大学 | Magnetic control graphene field effect tube sensor and its production, measurement and detection method |
| CN110404544A (en) * | 2019-07-26 | 2019-11-05 | 华东理工大学 | A kind of bimetallic catalytic material and its preparation method and application method |
| CN110404544B (en) * | 2019-07-26 | 2022-04-26 | 华东理工大学 | Bimetallic catalytic material and preparation method and application method thereof |
| CN111780901A (en) * | 2020-06-29 | 2020-10-16 | 复旦大学 | Spider-web-like flexible tactile sensor capable of simultaneously detecting force magnitude and direction |
| CN111780901B (en) * | 2020-06-29 | 2022-01-28 | 复旦大学 | Spider-web-like flexible tactile sensor capable of simultaneously detecting force magnitude and direction |
| CN112730562A (en) * | 2020-12-22 | 2021-04-30 | 河南中泽生物工程有限公司 | Electrochemical immunosensor for detecting tiamulin antigen and preparation method thereof |
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Effective date of registration: 20161228 Address after: 210000 Gulou District, Jiangsu, Zhongshan North Road, No. 200, No. Patentee after: Nanjing Nan Wei Mingxin Mstar Technology Ltd Address before: Yuen Road Qixia District of Nanjing City, Jiangsu Province, No. 9 210046 Patentee before: Nanjing University of Posts and Telecommunications |
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