CN101851479A - Application of graphite conductive adhesive to prepare electrode-detection binder - Google Patents
Application of graphite conductive adhesive to prepare electrode-detection binder Download PDFInfo
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- CN101851479A CN101851479A CN201010173556A CN201010173556A CN101851479A CN 101851479 A CN101851479 A CN 101851479A CN 201010173556 A CN201010173556 A CN 201010173556A CN 201010173556 A CN201010173556 A CN 201010173556A CN 101851479 A CN101851479 A CN 101851479A
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Abstract
The invention discloses application of graphite conductive adhesive to prepare a chemically modified electrode or biosensor electrode binder for electrochemical biological sensing detection, wherein, the graphite conductive adhesive comprises the following components by weight percent: 40-60% of an epoxy resin, 20-40% of graphite powder, 10-30% of a diluent and 1.5-3% of an amine curing agent. The graphite conductive adhesive has excellent electrical conductivity, excellent adhesiveness, wide and flat electrochemical window, convenient use, and excellent application prospect in electrochemical biological detection.
Description
Technical field
The invention belongs to microelectronics and connect the material technology field, relate in particular to a kind of graphite conductive adhesive is used for the chemically modified electrode or the biological sensor electrode binding agent of electrochemica biological sensing detection in preparation application.
Background technology
Electrochemical test method is easy and simple to handle because of it, economical fast, instantaneity, high sensitivity etc. and be widely used in environmental protection and biological medicine monitoring, fields such as food sanitation monitoring and Materials science research.Wherein, the electrochemica biological sensing detection is the focus of current concern, also is the key areas that electro-chemical test is used.But biomolecules such as protein (amino acid), nucleic acid (DNA/RNA) and carbohydrate (glucose) etc. all are organic molecules, and electroconductibility is very poor, and biomolecules test system resistance is very big; And the electrochemical redox reaction of most of biomolecules takes place at very high positive potential and very low negative potential place usually, head and shoulders above the electrochemical window of common electrode, be subjected to the restriction at water oxygen peak, bring difficulty for the Electrochemical Detection of biomolecules.Therefore, exploitation is sensitive (resistance is little) as far as possible, and the wide as far as possible bio-sensing detecting electrode of electrochemical window could satisfy the application that electrochemica biological detects.
Usually, Electrochemical Detection is active material to be connected basal electrode (glass carbon, gold electrode, glass-carbon electrode, Graphite Electrodes, carbon paste electrode etc.) go up the realization of formation detecting electrode.That is to say that detecting electrode is the core component of electro-chemical test device; In the detecting electrode preparation, the bonding of detecting electrode active substance is fixing of crucial importance, and it directly influences the stability of electrode and the stable output of work-ing life and electrical signal.The binding agent that present described electrode is commonly used has polyvinyl alcohol (PVA), naphthols (Nafion), poly(vinylidene fluoride) (PVDF) and polytetrafluoroethylene (PTFE) etc.Counter electrode, active and resistance is most important two parameters that influence test electrode performance quality, the general requirement activity is high more good more, and resistance the smaller the better (tens ohm).As everyone knows, the above-mentioned non-conductive son of binders for electrodes is the main source of electrode resistance.These binding agent consumptions are many, can cause electrode conductivuty sharply to descend, and too much binding agent sticks on the active material simultaneously, and electrode activation is slack-off, also can cause the internal resistance of electrode and polarization to increase; If the binding agent consumption has lacked, the electrode bonding strength is not enough, and electrode active material easily comes off, and causes sensing electrode to lose efficacy.Therefore, existing electrode matrix material has been difficult to satisfy the requirement that current high precision Electrochemical Detection is used, and the electrode problem of being adhesively fixed has restricted the development of chemically modified electrode and biosensor.
Summary of the invention
At the deficiencies in the prior art, the problem to be solved in the present invention provides a kind of graphite conductive adhesive is used for the chemically modified electrode or the biological sensor electrode binding agent of electrochemica biological sensing detection in preparation application.
Graphite conductive adhesive of the present invention is used for the application of the chemically modified electrode or the biological sensor electrode binding agent of electrochemica biological sensing detection in preparation.
Wherein: described graphite conductive adhesive is made by following component by mass percent:
Resins, epoxy 40～60wt%
Graphite Powder 99 20～40wt%
Thinner 10～30wt%
Amine curing agent 1.5～3wt%;
Wherein: above-mentioned Resins, epoxy is E-44, E-12 or JF-220 Resins, epoxy, or the mixture of the two any weight ratio wherein; Above-mentioned Graphite Powder 99 is natural graphite or synthetic graphite, or the mixture of the two any weight ratio; Above-mentioned thinner is 1,4-butanediol diglycidyl ether, Terpineol 350 or butyl glycol ether amyl acetate, or the mixture of the two any weight ratio wherein; Above-mentioned solidifying agent is latent amine curing agent polyethylene polyamine (PEPA), trimethylhexamethylenediamine (TM D) or two amido sulfobenzides (DDS).
Above-mentioned graphite conductive adhesive is preferably made by following component by mass percent:
Resins, epoxy 48～52wt%
Graphite Powder 99 28～32wt%
Thinner 18～22wt%
Amine curing agent 2.0～2.5wt%
Wherein: the preferred E-44 of described Resins, epoxy, E-12 or JF-220 Resins, epoxy.
Wherein: described Graphite Powder 99 preferred natural graphite or synthetic graphite.
Wherein: described thinner is preferred 1,4-butanediol diglycidyl ether, Terpineol 350 or butyl glycol ether amyl acetate.
Wherein: the described preferred polyethylene polyamine of solidifying agent (PEPA), trimethylhexamethylenediamine (TM D) or the two amido sulfobenzides (DDS) stated.
The preparation of above-mentioned graphite conductive adhesive and application method are by surface treatment, batching, mixed grinding and roll-in film forming step are formed, wherein: described surface treatment is meant to be handled the graphite as conductive filler 30 minutes under 100 ℃ constant temperature with 0.5MKOH, cooling, filter, be washed with distilled water to neutrality; Use 0.5MHNO again
3According to above-mentioned same steps as re-treatment; Vacuum-drying under 120 ℃ of conditions then makes the activation of graphite cleaning, and is standby.Described batching is meant to be calculated raw material by mass percentage, and Resins, epoxy is that 40～60wt%, Graphite Powder 99 are that 20～40wt%, thinner are that 10～30wt% and amine curing agent are that 1.5～3wt% carries out proportioning.Described mixed grinding is meant elder generation with graphite and the full and uniform mixing of thinner, adds Resins, epoxy again and fully grinds in mortar, drips the latent amine curing agent then, obtains heavy-gravity glue cream after the mixing.Described roll-in film forming is meant when the graphite conductive adhesive with above-mentioned preparation is applied to electro-chemical test, earlier with its roll-in film forming, cut into the diaphragm of required area size, be bonded in basal electrode (glass carbon, gold electrode, glass-carbon electrode, Graphite Electrodes, carbon paste electrode etc.) on, the sensing that is adhesively fixed again active material carries out the electrochemica biological sensing detection.
Graphite conductive adhesive of the present invention is used for the application of the chemically modified electrode or the biological sensor electrode binding agent of electrochemica biological sensing detection in preparation, the preparation of electrode binder graphite conductive adhesive is simple and easy to do, described graphite conductive adhesive is applicable to being connected and fixed of basal electrode and active material when electrochemical detection electrode prepares, and is specially adapted to the bonding of chemically modified electrode and biological sensor electrode; The detecting electrode binding agent graphite conductive adhesive that experiment confirm provides has good electroconductibility and cementability, and electrochemical window is wide flat, easy to use, can satisfy electrochemica biological well and detect application.Further, graphite conductive adhesive of the present invention has following characteristics:
(1) preparation method is simple.
(2) have good conductive capability, specific conductivity is 2～3 Ω/square.
(3) wide flat (1.2～1.5V), background current is very little for electrochemical window.
(4) make the research electrode area controlled.
Description of drawings
Fig. 1 is graphite conductive adhesive (the Graphite ConductiveAdhesive that the embodiment of the invention 1 is related to, GCA), paste at glass-carbon electrode (Glass Carbon Electrode, GCE) on, with 0.025M simulated body fluid phosphate buffer solution (PBS, pH6.86) be electrolytic solution, saturated calomel electrode is under the reference electrode condition, the cyclic voltammetry curve of graphite conductive adhesive/glass-carbon electrode (GCA/GCE).As seen from the figure, GCA/GCE does not have water oxygen peak in-1.2～1.5V scope, occur behind the 1.8V analysing the oxygen peak, and electrochemical window is wide flat, and background current is very little.
Embodiment
The present invention will be further described below in conjunction with example, but the present invention protects content to be not limited only to this.
Embodiment 1:
E-12 Resins, epoxy (E-44 Resins, epoxy) 1.7 grams, Graphite Powder 99 (natural graphite) 1.0 grams, 1,4-butanediol diglycidyl ether 0.60 gram, polyethylene polyamine 0.07 gram, allocate by following step:
Get Graphite Powder 99 1.0 grams, put under 100 ℃ of conditions of 0.50MKOH and handled 30 minutes, cooling is filtered, and is washed with distilled water to neutrality; Use 0.50MHNO then
3According to the same steps as re-treatment; Vacuum-drying under 120 ℃ of conditions at last makes the activation of graphite cleaning, and is standby.
The Graphite Powder 99 of above-mentioned processing, 1,4-butanediol diglycidyl ether 0.60 gram after thorough mixing grinds in mortar, adds E-12 Resins, epoxy 1.7 grams again, and mixed grinding is even, drips polyethylene polyamine 0.07 gram then, and mixed grinding obtains graphite conductive adhesive.
With this graphite conductive adhesive roll-in film forming, cut into the diaphragm of required area size, on the bonding substrate glass-carbon electrode, prepared graphite conductive adhesive/glass-carbon electrode (GCA/GCE) is at 0.025M simulated body fluid phosphate buffer solution (PBS, pH6.86) in, saturated calomel electrode is cyclic voltammetry curve such as the Fig. 1 under the reference electrode condition.
Embodiment 2:
E-12 Resins, epoxy (JF-220 Resins, epoxy) 1.7 grams, Graphite Powder 99 (synthetic graphite) 1.3 grams, Terpineol 350 0.35 gram, trimethylhexamethylenediamine 0.07 gram, allocate by following step:
Get Graphite Powder 99 1.3 grams, put under 100 ℃ of conditions of 0.50MKOH and handled 30 minutes, cooling is filtered, and is washed with distilled water to neutrality; Use 0.50MHNO then
3According to the same steps as re-treatment; Vacuum-drying under 120 ℃ of conditions at last makes the activation of graphite cleaning, and is standby.
The Graphite Powder 99 of above-mentioned processing, Terpineol 350 0.35 gram after thorough mixing grinds in mortar, adds E-12 Resins, epoxy 1.7 grams again, and mixed grinding is even, drips trimethylhexamethylenediamine 0.07 gram then, and mixed grinding obtains graphite conductive adhesive.
With this graphite conductive adhesive roll-in film forming, cut into the diaphragm of required area size, on the bonding substrate glass-carbon electrode, prepared graphite conductive adhesive/glass-carbon electrode (GCA/GCE) is at 0.025M simulated body fluid phosphate buffer solution (PBS, pH6.86) in, saturated calomel electrode is that cyclic voltammetry curve and the Fig. 1 under the reference electrode condition is similar.
Embodiment 3:
E-12 Resins, epoxy (E-12 mixes with the JF-220 weight epoxy) 0.50 gram, Graphite Powder 99 (weight such as natural graphite and synthetic graphite are mixed) 0.30 gram, butyl glycol ether amyl acetate 0.17 restrains, and two amido sulfobenzides 0.03 restrain, and allocate by following step:
Get Graphite Powder 99 0.30 gram, put under 100 ℃ of conditions of 0.50MKOH and handled 30 minutes, cooling is filtered, and is washed with distilled water to neutrality; Use 0.50MHNO then
3According to the same steps as re-treatment; Vacuum-drying under 120 ℃ of conditions at last makes the activation of graphite cleaning, and is standby.
The Graphite Powder 99 of above-mentioned processing, butyl glycol ether amyl acetate 0.17 gram after thorough mixing grinds in mortar, adds E-12 Resins, epoxy 0.50 gram again, and mixed grinding is even, drips two amido sulfobenzides (DDS), 0.03 gram then, and mixed grinding obtains graphite conductive adhesive.
With this graphite conductive adhesive roll-in film forming, cut into the diaphragm of required area size, on the bonding substrate glass-carbon electrode, prepared graphite conductive adhesive/glass-carbon electrode (GCA/GCE) is at 0.025M simulated body fluid phosphate buffer solution (PBS, pH6.86) in, saturated calomel electrode is that cyclic voltammetry curve and the Fig. 1 under the reference electrode condition is similar.
Embodiment 4:
JF-220 Resins, epoxy 2.25 grams, Graphite Powder 99 1.22 grams, 1,4-butanediol diglycidyl ether 0.90 gram, two amido sulfobenzides, 0.13 gram, allocate by following step:
Get Graphite Powder 99 1.22 grams, put under 100 ℃ of conditions of 0.50MKOH and handled 30 minutes, cooling is filtered, and is washed with distilled water to neutrality; Use 0.50MHNO then
3According to the same steps as re-treatment; Vacuum-drying under 120 ℃ of conditions at last makes the activation of graphite cleaning, and is standby.
The Graphite Powder 99 of above-mentioned processing, 1.4-butanediol diglycidyl ether 0.90 gram is after thorough mixing grinds in mortar, add JF-220 Resins, epoxy 2.25 grams again, mixed grinding is even, drips two amido sulfobenzides, 0.13 gram then, mixed grinding obtains graphite conductive adhesive.
With this graphite conductive adhesive roll-in film forming, cut into the diaphragm of required area size, on the bonding substrate glass-carbon electrode, prepared graphite conductive adhesive/glass-carbon electrode (GCA/GCE) is at 0.025M simulated body fluid phosphate buffer solution (PBS, pH6.86) in, saturated calomel electrode is that cyclic voltammetry curve and the Fig. 1 under the reference electrode condition is similar.
Embodiment 5:
JF-220 Resins, epoxy 0.60 gram, Graphite Powder 99 0.60 gram, Terpineol 350 0.26 gram, two amido sulfobenzides, 0.04 gram, allocate by following step:
Get Graphite Powder 99 0.60 gram, put under 100 ℃ of conditions of 0.50MKOH and handled 30 minutes, cooling is filtered, and is washed with distilled water to neutrality; Use 0.50MHNO then
3According to the same steps as re-treatment; Vacuum-drying under 120 ℃ of conditions at last makes the activation of graphite cleaning, and is standby.
The Graphite Powder 99 of above-mentioned processing, Terpineol 350 0.26 gram after thorough mixing grinds in mortar, adds JF-220 Resins, epoxy 0.60 gram again, and mixed grinding is even, drips two amido sulfobenzides (DDS), 0.04 gram then, and mixed grinding obtains graphite conductive adhesive.
With this graphite conductive adhesive roll-in film forming, cut into the diaphragm of required area size, on the bonding substrate glass-carbon electrode, prepared graphite conductive adhesive/glass-carbon electrode (GCA/GCE) is at 0.025M simulated body fluid phosphate buffer solution (PBS, pH6.86) in, saturated calomel electrode is that cyclic voltammetry curve and the Fig. 1 under the reference electrode condition is similar.
Embodiment 6:
JF-220 Resins, epoxy 0.64 gram, Graphite Powder 99 0.45 gram, butyl glycol ether amyl acetate 0.48 gram, two amido sulfobenzides, 0.03 gram, allocate by following step:
Get Graphite Powder 99 0.45 gram, put under 100 ℃ of conditions of 0.50MKOH and handled 30 minutes, cooling is filtered, and is washed with distilled water to neutrality; Use 0.50MHNO then
3According to the same steps as re-treatment; Vacuum-drying under 120 ℃ of conditions at last makes the activation of graphite cleaning, and is standby.
The Graphite Powder 99 of above-mentioned processing, butyl glycol ether amyl acetate 0.48 gram is after thorough mixing grinds in mortar, add JF-220 Resins, epoxy 0.64 gram again, mixed grinding is even, drips two amido sulfobenzides (DDS), 0.03 gram then, mixed grinding obtains graphite conductive adhesive.
With this graphite conductive adhesive roll-in film forming, cut into the diaphragm of required area size, on the bonding substrate glass-carbon electrode, prepared graphite conductive adhesive/glass-carbon electrode (GCA/GCE) is at 0.025M simulated body fluid phosphate buffer solution (PBS, pH6.86) in, saturated calomel electrode is that cyclic voltammetry curve and the Fig. 1 under the reference electrode condition is similar.
Claims (6)
1. graphite conductive adhesive is used for the application of the chemically modified electrode or the biological sensor electrode binding agent of electrochemica biological sensing detection in preparation.
2. application as claimed in claim 1 is characterized in that: described graphite conductive adhesive is made by following component by mass percent:
Resins, epoxy 40～60wt%
Graphite Powder 99 20～40wt%
Thinner 10～30wt%
Amine curing agent 1.5～3wt%;
Wherein: above-mentioned Resins, epoxy is E-44, E-12 or JF-220 Resins, epoxy, or the mixture of the two any weight ratio wherein; Above-mentioned Graphite Powder 99 is natural graphite or synthetic graphite, or the mixture of the two any weight ratio; Above-mentioned thinner is 1,4-butanediol diglycidyl ether, Terpineol 350 or butyl glycol ether amyl acetate, or the mixture of the two any weight ratio wherein; Above-mentioned solidifying agent is latent amine curing agent polyethylene polyamine, trimethylhexamethylenediamine or two amido sulfobenzides.
3. application as claimed in claim 2 is characterized in that: described Resins, epoxy is E-44, E-12 or JF-220 Resins, epoxy.
4. application as claimed in claim 2 is characterized in that: described Graphite Powder 99 is natural graphite or synthetic graphite.
5. application as claimed in claim 2 is characterized in that: described thinner is 1,4-butanediol diglycidyl ether, Terpineol 350 or butyl glycol ether amyl acetate.
6. application as claimed in claim 2 is characterized in that: the described solidifying agent of stating is polyethylene polyamine, trimethylhexamethylenediamine or two amido sulfobenzides.
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| CN 201010173556 CN101851479B (en) | 2010-05-17 | 2010-05-17 | Application of graphite conductive adhesive to prepare electrode-detection binder |
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| CN 201010173556 CN101851479B (en) | 2010-05-17 | 2010-05-17 | Application of graphite conductive adhesive to prepare electrode-detection binder |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103199266A (en) * | 2013-03-15 | 2013-07-10 | 中国科学院城市环境研究所 | Electrode of bioelectrochemical system and manufacturing method of electrode |
| CN107069250A (en) * | 2017-01-23 | 2017-08-18 | 武汉昱仝科技有限公司 | A kind of carbon applies steel and preparation method thereof and purposes |
| CN107195923A (en) * | 2017-05-22 | 2017-09-22 | 上海弘枫实业有限公司 | A kind of high-efficiency fuel cell flow-guide double-pole plate |
| CN109135638A (en) * | 2018-06-26 | 2019-01-04 | 中国林业科学研究院林产化学工业研究所 | One kind is coupled hardness with softness epoxy conducting and preparation method thereof |
| CN110482845A (en) * | 2019-09-29 | 2019-11-22 | 深圳赛贝尔自动化设备有限公司 | The mold delivery device and method of curve glass forming apparatus |
| CN110519914A (en) * | 2019-08-28 | 2019-11-29 | 刘明炜 | A kind of conductive structure and its preparation method and application |
| CN112322246A (en) * | 2020-12-02 | 2021-02-05 | 句容市双诚电子有限公司 | Low-consumption temperature-resistant conductive adhesive for sensor and preparation method thereof |
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| CN1047685A (en) * | 1989-05-31 | 1990-12-12 | 谢志浩 | A kind of electrically conducting adhesive |
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2010
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Patent Citations (1)
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|---|---|---|---|---|
| CN1047685A (en) * | 1989-05-31 | 1990-12-12 | 谢志浩 | A kind of electrically conducting adhesive |
Non-Patent Citations (2)
| Title |
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| 《中国胶粘剂》 20080630 林韡等 石墨/环氧树脂导电胶的研究 4－9 1-6 第17卷, 第6期 * |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103199266A (en) * | 2013-03-15 | 2013-07-10 | 中国科学院城市环境研究所 | Electrode of bioelectrochemical system and manufacturing method of electrode |
| CN107069250A (en) * | 2017-01-23 | 2017-08-18 | 武汉昱仝科技有限公司 | A kind of carbon applies steel and preparation method thereof and purposes |
| CN107195923A (en) * | 2017-05-22 | 2017-09-22 | 上海弘枫实业有限公司 | A kind of high-efficiency fuel cell flow-guide double-pole plate |
| CN109135638A (en) * | 2018-06-26 | 2019-01-04 | 中国林业科学研究院林产化学工业研究所 | One kind is coupled hardness with softness epoxy conducting and preparation method thereof |
| CN110519914A (en) * | 2019-08-28 | 2019-11-29 | 刘明炜 | A kind of conductive structure and its preparation method and application |
| CN110482845A (en) * | 2019-09-29 | 2019-11-22 | 深圳赛贝尔自动化设备有限公司 | The mold delivery device and method of curve glass forming apparatus |
| CN110482845B (en) * | 2019-09-29 | 2023-05-12 | 深圳赛贝尔自动化设备有限公司 | Mould pushing mechanism and method of curved glass forming device |
| CN112322246A (en) * | 2020-12-02 | 2021-02-05 | 句容市双诚电子有限公司 | Low-consumption temperature-resistant conductive adhesive for sensor and preparation method thereof |
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