CN105699455A - Preparation method of ionic liquid modified carbon paste electrode - Google Patents

Preparation method of ionic liquid modified carbon paste electrode Download PDF

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CN105699455A
CN105699455A CN201610168460.4A CN201610168460A CN105699455A CN 105699455 A CN105699455 A CN 105699455A CN 201610168460 A CN201610168460 A CN 201610168460A CN 105699455 A CN105699455 A CN 105699455A
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ionic liquid
electrode
carbon paste
modified carbon
paste electrode
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CN105699455B (en
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孙伟
闫丽君
牛学良
文作瑞
王文成
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Hainan Normal University
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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

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Abstract

The invention discloses a preparation method of a novel ionic liquid modified carbon paste electrode prepared by mixing N-butyl-N-methylpiperidine hexafluorophosphate ionic liquid, graphite powder and liquid paraffin wax. The preparation method comprises the following steps: (1) sufficiently grinding the ionic liquid, the graphite powder and the liquid paraffin wax in a clean mortar at a certain mass ratio; (2) putting the mixture into a glass tube; taking an embedded copper wire as a lead wire, and compacting by using a cylindrical metal rod; (3) before utilization, sufficiently polishing on polishing paper until a mirror surface is formed; (4) carrying out characterization on a surface shape by adopting a scanning electron microscope; (5) carrying out a comparative research on electrochemical behaviors of the ionic liquid modified carbon paste electrode by taking potassium ferricyanide as an electrochemical probe.

Description

A kind of preparation method of Ionic Liquid Modified carbon paste electrode
Technical field
The present invention relates to chemically modified electrode preparation field, the preparation method wherein having probed into Ionic Liquid Modified carbon paste electrode。
Background technology
Ionic liquid has conductivity height, electrochemical window width, high thermal stability, thermal capacitance and thermal energy storage density advantages of higher, it is made to have advantage clearly in electrochemistry and Electroanalytical Chemistry field, and its Acidity of Aikalinity is adjustable, volatility is little, dissolubility is good so that it is all have great application prospect in electrochemical a lot of directions。
Carbon paste electrode is exactly utilize the graphite powder of conduction and the binding agent of hydrophobicity to be mixed and made into pastel, is then coated on electrode bar or is packed into the class electrode made in electrode tube。Although carbon paste electrode has the advantage such as stability and favorable reproducibility, applied range, long service life, but its sensitivity and selectivity are restricted。So the introducing of specially good effect dressing agent can make its sensitivity and selectivity be further improved。
Chemically modified carbon paste electrode has and makes simple, favorable reproducibility and advantage that surface easily updates。Ionic Liquid Modified carbon paste electrode is the one of chemically modified carbon paste electrode, there is good chemical property, it is effectively improved the electron transfer rate of various organic/inorganic electroactive material, it is possible to increase interface conductivity, and reduce the overpotential value of biomolecule。
Summary of the invention
Present invention aim to overcome that the character of existing carbon paste electrode is not enough, by using a kind of ionic liquid to make Ionic Liquid Modified carbon paste electrode as binding agent, and to preparing the optimization of electrode material consumption, provide a kind of sensitivity and selectivity is high, the Ionic Liquid Modified carbon paste electrode preparation method of applied range。
In order to realize above-mentioned task, the present invention takes following technical solution:
The preparation method of a kind of Ionic Liquid Modified carbon paste electrode, it is characterised in that comprise the following steps:
(1) graphite powder, ionic liquid and liquid paraffin mixing are put in clean mortar, grind 2-3 hour so as to mix homogeneously；
(2) thin copper wire is inserted washes clean, be about for 4-5cm, internal diameter be about 4mm, glass tubing in, and be fixed；
(3) mixture in mortar is loaded in glass tubing, with cylindrical metal rod by interior for pipe mixture compacted, namely obtain Ionic Liquid Modified carbon paste electrode；
(4), before using, polishing paper is polishing to minute surface。
Described ionic liquid is N-butyl-N-methyl piperidine hexafluorophosphate, and its quality with graphite powder is 0.8g, and the volume of liquid paraffin is 250 μ L。
Described Ionic Liquid Modified carbon paste electrode, adopts scanning electron microscope that its surface topography is characterized。
Described Ionic Liquid Modified carbon paste electrode, is working electrode with Ionic Liquid Modified carbon paste electrode, and platinized platinum is auxiliary electrode, and saturated calomel electrode is reference electrode。It is within the scope of-0.7 0.3V at the wide mouth of current potential, this decorating carbon paste electrode is characterized。
Described Ionic Liquid Modified carbon paste electrode, three-electrode system is circulated voltammetric scan in characterizing solution, the electrochemical behavior of research Ionic Liquid Modified carbon paste electrode, including the impedance to the sign of different modifying electrode, the cyclic voltammetric under difference sweeps speed and different modifying electrode。
Described sign solution, research difference sweeps speed and solution used during impedance is the potassium chloride mixed liquor of the potassium ferricyanide that concentration is 1.0mmol/L and 0.1mol/L。
Described Ionic Liquid Modified carbon paste electrode, sweep speed respectively 0.05,0.06,0.07,0.08,0.09,0.1,0.15,0.2,0.25,0.3V/s。
The invention has the beneficial effects as follows: compared with prior art, the invention provides a kind of method preparing Ionic Liquid Modified carbon paste electrode and prepare material proportion optimization。Compared with conventional carbon paste electrode, graphite powder and ionic liquid mass ratio are happens is that diffusion controlled process on the Ionic Liquid Modified carbon paste electrode surface of 1:1, potassium ferricyanide oxidation-reduction potential is had higher electro-chemical activity, there is higher electron transfer rate。The present invention is prepared simply, and electrode surface easily updates, and applied range is cheap, it is easy to universal use。
Accompanying drawing explanation
Fig. 1 is the different quality surface topography map than modified electrode。A, B, C, D respectively graphite powder and ionic liquid mass ratio are the modified electrode surface topography of 1:1,2:1,3:1,1:2。
Fig. 2 is the cyclic voltammogram of the modified electrode of different quality ratio。It is 1:1 that a, b, c, d represent graphite powder and ionic liquid mass ratio respectively, 2:1,3:1,1:2, and electrolyte solution is the potassium chloride mixed liquor of the potassium ferricyanide of 1mmol/L and 0.1mol/L, sweeps speed for 100mV/s。
Fig. 3 is the impedance diagram of the modified electrode of different quality ratio。It is 1:1 that a, b, c, d represent graphite powder and ionic liquid mass ratio respectively, 2:1,3:1,1:2, and electrolyte solution is the potassium chloride mixed liquor of the potassium ferricyanide of 1.0mmol/L and 0.1mol/L, sweeps speed for 100mV/s。
Fig. 4 is graphite powder from modified electrode prepared under ionic liquid mass ratio 1:1 at the different cyclic voltammetry curve figure swept under speed, electrolyte solution is the potassium chloride mixed liquor of the potassium ferricyanide of 1.0mmol/L and 0.1mol/L, sweep speed be 0.05,0.06,0.07,0.08,0.09,0.1,0.15,0.2,0.25,0.3V/s。
Detailed description of the invention
The invention will be further described for example given below, but without departing from the restriction of scope。
Embodiment 1
Weighing N-butyl-N-methyl piperidine hexafluorophosphate and the graphite powder of 0.8g respectively, the liquid paraffin measuring 250 μ L with liquid-transfering gun is sufficiently mixed, and grinds 2-3 hour in clean mortar；The clean thin copper wire of polishing is inserted washes clean, is about and is about in the glass tubing of 4mm for 5-6cm, internal diameter, and be fixed；Mixture in mortar is loaded in glass tubing, then fills in appropriate Cotton Gossypii from the top of glass tubing, with cylindrical metal rod by interior for pipe mixture compacted, namely obtain Ionic Liquid Modified carbon paste electrode；Before using, polishing paper is polishing to minute surface。According to the method described above, graphite powder and ionic liquid mass ratio respectively 2:1,3:1,1:2 decorating carbon paste electrode are prepared。
Embodiment 2
Adopt electronic scanner microscope that the Ionic Liquid Modified carbon paste electrode of different quality ratio is characterized, electrode surface pattern is as it is shown in figure 1, A, B, C, D respectively graphite powder and ionic liquid mass ratio are 1:1,2:1, modified electrode surface topography map when 3:1,1:2。Can be seen that mass ratio is that modified electrode surface when 1:1 is the most smooth, smooth。
Embodiment 3
The Ionic Liquid Modified carbon paste electrode of prepared different quality ratio is placed in the potassium chloride mixed liquor of the potassium ferricyanide that concentration is 1.0mmol/L and 0.1mol/L and is circulated voltammetric scan。As in figure 2 it is shown, curve a to d represents graphite powder and ionic liquid mass ratio 1:1,2:1 respectively, cyclic voltammetry curve when 3:1,1:2, it can be seen that, when mass ratio is 1:1, oxidoreduction peak point current is maximum, and namely the electron transfer rate of electrode surface is the fastest with this understanding。
Embodiment 4
Having investigated the electrode of the different quality ratio electrochemical impedance spectroscopy in the potassium ferricyanide of 1.0mmol/L and the potassium chloride mixed liquor of 0.1mol/L, result is as shown in Figure 3。Curve a, b, c, d represent graphite powder respectively and liquid ions quality is impedance diagram when 1:1,2:1,3:1,1:2, it can be seen that the electrochemical impedance collection of illustrative plates of four kinds of different modifying electrodes has obvious difference。The resistance value of curve a is minimum, and the resistance value of curve d is maximum。This result is consistent with different modifying electrode cycle volt-ampere result in embodiment 3, and also fully demonstrating when both mass ratioes are 1:1 is optimum condition, and now the electron transfer rate on modified electrode surface is the fastest。
Embodiment 5
Choose the Ionic Liquid Modified (graphite powder and liquid ions mass ratio 1:1) of optimum quality ratio, the relation investigated peak current with swept speed。Figure 4, it is seen that along with the increase sweeping speed, peak current is gradually increased, at 50 ~ 300mV/s scope internal oxidition peak current and reduction peak current and v1/2In good linear relationship, illustrate that this electrode reaction is diffusion controlled process。Illustrate that electrode process is controlled by diffusion。Owing to the existence of ionic liquid significantly increases interfacial conductive efficiency, enable the generating electrodes reaction that the potassium ferricyanide of arrival electrode surface is quick and complete, namely electron transport rate is arrived the diffusion velocity of electrode surface more than material by bulk solution, so electrode process is by diffusion process control。

Claims (8)

1. the preparation method of an Ionic Liquid Modified carbon paste electrode, it is characterised in that comprise the following steps:
Graphite powder, ionic liquid and liquid paraffin mixing are put in clean mortar, grind 2-3 hour so as to mix homogeneously；
Thin copper wire is inserted washes clean, is about and is about in the glass tubing electrode of 4mm for 4-5cm, internal diameter, and is fixed；
Mixture in mortar is loaded in glass tubing, with cylindrical metal rod by interior for pipe mixture compacted, namely obtain Ionic Liquid Modified carbon paste electrode；
Before using, polishing paper is polishing to minute surface。
2. Ionic Liquid Modified carbon paste electrode according to claim 1, it is characterised in that: ionic liquid is N-butyl-N-methyl piperidine hexafluorophosphate, and its quality with graphite powder is 0.8g, and the consumption of liquid paraffin is 250 μ L。
3. Ionic Liquid Modified carbon paste electrode according to claim 1, it is characterised in that: adopt scanning electron microscope that electrode surface pattern is characterized。
4. Ionic Liquid Modified carbon paste electrode according to claim 2, it is characterised in that: being working electrode with Ionic Liquid Modified carbon paste electrode, platinized platinum is auxiliary electrode, and saturated calomel electrode is reference electrode。
5. regulation potential range is-0.7 0.3V。
6. Ionic Liquid Modified carbon paste electrode according to claim 4, it is characterized in that: three-electrode system is circulated voltammetric scan in characterizing solution, the electrochemical behavior of research Ionic Liquid Modified carbon paste electrode, including the impedance to the sign of modified electrode, the cyclic voltammetric under difference sweeps speed and different modifying electrode。
7. Ionic Liquid Modified carbon paste electrode according to claim 5, it is characterised in that: characterize solution, research difference solution used when sweeping speed and impedance and be the potassium chloride mixed liquor of the potassium ferricyanide that concentration is 1.0mmol/L and 0.1mol/L。
8. Ionic Liquid Modified carbon paste electrode according to claim 6, it is characterised in that: sweep speed respectively 0.05,0.06,0.07,0.08,0.09,0.1,0.15,0.2,0.25,0.3V/s。
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107192752A (en) * 2017-08-01 2017-09-22 信阳师范学院 A kind of chemically modified electrode for being used for highly sensitive detection nonyl phenol and preparation method thereof
CN109298054A (en) * 2018-11-15 2019-02-01 湖南工程学院 Bromination 1- tert-butyl -3- methylimidazole Ionic Liquid Modified electrode and application
CN111403805A (en) * 2020-04-28 2020-07-10 深圳先进技术研究院 Composite solid electrolyte, preparation method thereof and lithium ion battery

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CN101710093A (en) * 2009-12-28 2010-05-19 浙江大学 Novel carbon paste electrode and preparation method thereof
CN102269730A (en) * 2011-07-04 2011-12-07 中国科学院长春应用化学研究所 Carbon paste electrode and preparation method thereof
CN104237337A (en) * 2014-09-25 2014-12-24 普旭力 Biosensor sensitive membrane as well as preparation method and application thereof

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
CN101710093A (en) * 2009-12-28 2010-05-19 浙江大学 Novel carbon paste electrode and preparation method thereof
CN102269730A (en) * 2011-07-04 2011-12-07 中国科学院长春应用化学研究所 Carbon paste electrode and preparation method thereof
CN104237337A (en) * 2014-09-25 2014-12-24 普旭力 Biosensor sensitive membrane as well as preparation method and application thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107192752A (en) * 2017-08-01 2017-09-22 信阳师范学院 A kind of chemically modified electrode for being used for highly sensitive detection nonyl phenol and preparation method thereof
CN107192752B (en) * 2017-08-01 2019-07-05 信阳师范学院 A kind of chemically modified electrode and preparation method thereof for highly sensitive detection nonyl phenol
CN109298054A (en) * 2018-11-15 2019-02-01 湖南工程学院 Bromination 1- tert-butyl -3- methylimidazole Ionic Liquid Modified electrode and application
CN111403805A (en) * 2020-04-28 2020-07-10 深圳先进技术研究院 Composite solid electrolyte, preparation method thereof and lithium ion battery

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