CN105699455A - Preparation method of ionic liquid modified carbon paste electrode - Google Patents
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- 239000002608 ionic liquid Substances 0.000 title claims abstract description 42
- 150000001721 carbon Chemical class 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 15
- -1 hexafluorophosphate Chemical compound 0.000 claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 8
- 229940057995 liquid paraffin Drugs 0.000 claims abstract description 7
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 4
- 238000005498 polishing Methods 0.000 claims abstract description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 12
- 238000002484 cyclic voltammetry Methods 0.000 claims description 8
- 235000011164 potassium chloride Nutrition 0.000 claims description 6
- 239000001103 potassium chloride Substances 0.000 claims description 6
- 238000012512 characterization method Methods 0.000 claims description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 239000004576 sand Substances 0.000 claims 1
- 238000005056 compaction Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 abstract 1
- 238000004626 scanning electron microscopy Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 9
- 238000009792 diffusion process Methods 0.000 description 5
- 230000027756 respiratory electron transport chain Effects 0.000 description 5
- 238000003411 electrode reaction Methods 0.000 description 4
- 239000008151 electrolyte solution Substances 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- ONGZMKPEWCAXFS-UHFFFAOYSA-L [Cl+].[Cl-].[K+].[Cl-] Chemical compound [Cl+].[Cl-].[K+].[Cl-] ONGZMKPEWCAXFS-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008364 bulk solution Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004832 voltammetry Methods 0.000 description 1
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Abstract
本发明公开了N-丁基-N-甲基哌啶六氟磷酸盐离子液体与石墨粉和液体石蜡混合制得的一种新型离子液体修饰碳糊电极的制备方法。步骤如下：(1)一定质量比的离子液体、石墨粉和液体石蜡置于干净的研钵中充分研磨；(2)混合物装入玻璃管中，内嵌铜丝作为导线，用圆柱形金属棒压实；(3)使用前在抛光纸上充分打磨至镜面；(4)采用扫描电子显微镜对其表面形貌进行表征；(5)以铁氰化钾为电化学探针对该离子液体修饰碳糊电极的电化学行为进行比较研究。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 with graphite powder and liquid paraffin. The steps are as follows: (1) A certain mass ratio of ionic liquid, graphite powder and liquid paraffin is placed in a clean mortar and fully ground; (2) The mixture is put into a glass tube, embedded with copper wire as a wire, and a cylindrical metal rod is used to compaction; (3) fully polished to a mirror surface on polishing paper before use; (4) characterized its surface morphology by scanning electron microscopy; (5) modified the ionic liquid with potassium ferricyanide as an electrochemical probe The electrochemical behavior of carbon paste electrodes was studied comparatively.
Description
技术领域 technical field
本发明涉及化学修饰电极制备领域，其中探究了离子液体修饰碳糊电极的制备方法。 The invention relates to the field of preparation of chemically modified electrodes, in which a method for preparing ionic liquid modified carbon paste electrodes is explored.
背景技术 Background technique
离子液体具有导电率高，电化学窗口宽，高热稳定性，热容及热能储存密度高等优点，使其在电化学和电分析化学领域中具有很明显的优点，并且其酸碱性可调、挥发性小、溶解性好，使其在电化学的很多方向都具有很大的应用前景。 Ionic liquids have the advantages of high conductivity, wide electrochemical window, high thermal stability, high heat capacity and high thermal energy storage density, which make them have obvious advantages in the fields of electrochemistry and electroanalytical chemistry, and their acidity and alkalinity can be adjusted, Low volatility and good solubility make it have great application prospects in many directions of electrochemistry.
碳糊电极就是利用导电的石墨粉和憎水性的粘合剂混合制成糊状物，然后将其涂在电极棒上或填充入电极管中而制成的一类电极。虽然碳糊电极具有稳定性及重现性好、应用范围广、使用寿命长等优点，但其灵敏度和选择性受到限制。所以特效修饰剂的引入可以使其灵敏度和选择性有了进一步提高。 Carbon paste electrode is a type of electrode made by mixing conductive graphite powder and hydrophobic binder to form a paste, which is then coated on the electrode rod or filled into the electrode tube. Although the carbon paste electrode has the advantages of good stability and reproducibility, a wide range of applications, and a long service life, its sensitivity and selectivity are limited. Therefore, the introduction of specific modifiers can further improve the sensitivity and selectivity.
化学修饰碳糊电极具有制作简单、重现性好和表面容易更新的优势。离子液体修饰碳糊电极是化学修饰碳糊电极的一种，具有良好的电化学性能，有效地提高了各种有机/无机电活性物质的电子转移速率，可以增大界面导电性，并且降低生物分子的过电位值。 Chemically modified carbon paste electrodes have the advantages of simple fabrication, good reproducibility, and easy surface renewal. Ionic liquid modified carbon paste electrode is a kind of chemically modified carbon paste electrode, which has good electrochemical performance, effectively improves the electron transfer rate of various organic/inorganic electroactive substances, can increase the interface conductivity, and reduce the biological Molecular overpotential value.
发明内容 Contents of the invention
本发明目的在于克服现有碳糊电极的性质不足，通过使用一种离子液体作为粘合剂制成离子液体修饰碳糊电极，并对制备电极材料用量的优化，提供了一种灵敏度和选择性高，应用范围广的离子液体修饰碳糊电极制备方法。 The purpose of the present invention is to overcome the lack of properties of the existing carbon paste electrode, by using an ionic liquid as a binder to make an ionic liquid modified carbon paste electrode, and optimizing the amount of electrode material used to prepare the electrode, providing a sensitivity and selectivity A high-quality, wide-ranging method for the preparation of ionic liquid-modified carbon paste electrodes.
为了实现上述任务，本发明采取如下的技术解决方案： In order to realize above-mentioned task, the present invention takes following technical solution:
一种离子液体修饰碳糊电极的制备方法，其特征在于，包括以下步骤： A kind of preparation method of ionic liquid modified carbon paste electrode, it is characterized in that, comprises the following steps:
(1)石墨粉、离子液体和液体石蜡混合放入干净的研钵中，研磨2-3小时使之混合均匀； (1) Mix graphite powder, ionic liquid and liquid paraffin into a clean mortar, grind for 2-3 hours to make it evenly mixed;
(2)将细铜丝插入洗涤干净、长约为4-5cm、内径约为4mm、的玻璃管内，并将其固定； (2) Insert the thin copper wire into a cleaned glass tube with a length of about 4-5cm and an inner diameter of about 4mm, and fix it;
(3)将研钵中的混合物装入玻璃管中，用圆柱形金属棒将管内混合物压实，即得到离子液体修饰碳糊电极； (3) Put the mixture in the mortar into a glass tube, and compact the mixture in the tube with a cylindrical metal rod to obtain an ionic liquid modified carbon paste electrode;
(4)使用前，在抛光纸上打磨至镜面。 (4) Polish to a mirror finish on polishing paper before use.
所述离子液体为N-丁基-N-甲基哌啶六氟磷酸盐，其与石墨粉的质量均为0.8g，液体石蜡的体积为250μL。 The ionic liquid is N-butyl-N-methylpiperidine hexafluorophosphate, its mass and graphite powder are both 0.8 g, and the volume of liquid paraffin is 250 μL.
所述的离子液体修饰碳糊电极，采用扫描电子显微镜对其表面形貌进行表征。 The surface morphology of the carbon paste electrode modified by the ionic liquid is characterized by a scanning electron microscope.
所述的离子液体修饰碳糊电极，用离子液体修饰碳糊电极为工作电极，铂片为辅助电极，饱和甘汞电极为参比电极。在电位宽口为-0.7—0.3V范围内，对该修饰碳糊电极进行表征。 The carbon paste electrode modified by the ionic liquid is used as the working electrode, the platinum sheet is used as the auxiliary electrode, and the saturated calomel electrode is used as the reference electrode. The modified carbon paste electrode was characterized in the potential range of -0.7-0.3V.
所述的离子液体修饰碳糊电极，三电极系统在表征溶液中进行循环伏安扫描，研究离子液体修饰碳糊电极的电化学行为，包括对不同修饰电极的表征、在不同扫速下的循环伏安和不同修饰电极的阻抗。 The ionic liquid modified carbon paste electrode, the three-electrode system performs cyclic voltammetry scanning in the characterization solution, and studies the electrochemical behavior of the ionic liquid modified carbon paste electrode, including the characterization of different modified electrodes and the cycle at different scan rates Voltammetry and impedance of different modified electrodes.
所述表征溶液，研究不同扫速和阻抗时所用的溶液均为浓度为1.0mmol/L的铁氰化钾和0.1mol/L的氯化钾混合液。 The characterization solution used in the study of different scan rates and impedances is a mixture of potassium ferricyanide and 0.1mol/L potassium chloride with a concentration of 1.0mmol/L.
所述的离子液体修饰碳糊电极，扫速分别为0.05、0.06、0.07、0.08、0.09、0.1、0.15、0.2、0.25、0.3V/s。 The scanning speeds of the ionic liquid modified carbon paste electrodes are 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.15, 0.2, 0.25, 0.3 V/s respectively.
本发明的有益效果是：与现有技术相比，本发明提供了一种制备离子液体修饰碳糊电极的方法及其制备材料比例优化。与传统碳糊电极相比，石墨粉与离子液体质量比为1:1的离子液体修饰碳糊电极表面上发生的是扩散控制过程，对铁氰化钾氧化还原电位具有更高的电化学活性，具有更高的电子转移速率。本发明制备简单，电极表面容易更新，应用范围广，价格低廉，易于普及使用。 The beneficial effects of the invention are: compared with the prior art, the invention provides a method for preparing an ionic liquid-modified carbon paste electrode and the optimization of the preparation material ratio. Compared with the traditional carbon paste electrode, the ionic liquid modified carbon paste electrode surface with graphite powder and ionic liquid mass ratio of 1:1 is a diffusion-controlled process, which has higher electrochemical activity on the redox potential of potassium ferricyanide , with a higher electron transfer rate. The invention has the advantages of simple preparation, easy renewal of the electrode surface, wide application range, low price and easy popularization and use.
附图说明 Description of drawings
图1为不同质量比修饰电极的表面形貌图。A、B、C、D分别为石墨粉与离子液体质量比为1:1,2:1,3:1,1:2的修饰电极表面形貌。 Figure 1 is the surface topography of modified electrodes with different mass ratios. A, B, C, and D are the surface morphology of modified electrodes with mass ratios of graphite powder and ionic liquid of 1:1, 2:1, 3:1, and 1:2, respectively.
图2为不同质量比例的修饰电极的循环伏安图。a,b,c,d分别代表石墨粉与离子液体质量比为1:1,2:1,3:1,1:2,电解质溶液为1mmol/L的铁氰化钾和0.1mol/L的氯化钾混合液，扫速为100mV/s。 Figure 2 is the cyclic voltammograms of modified electrodes with different mass ratios. a, b, c, d respectively represent the mass ratio of graphite powder to ionic liquid is 1:1, 2:1, 3:1, 1:2, the electrolyte solution is 1mmol/L potassium ferricyanide and 0.1mol/L Potassium chloride mixture, the scan rate is 100mV/s.
图3为不同质量比例的修饰电极的阻抗图。a,b,c,d分别代表石墨粉与离子液体质量比为1:1,2:1,3:1,1:2，电解质溶液为1.0mmol/L的铁氰化钾和0.1mol/L的氯化钾混合液，扫速为100mV/s。 Figure 3 is the impedance diagram of modified electrodes with different mass ratios. a, b, c, d respectively represent the mass ratio of graphite powder to ionic liquid is 1:1, 2:1, 3:1, 1:2, the electrolyte solution is 1.0mmol/L potassium ferricyanide and 0.1mol/L Potassium chloride mixture, the scan rate is 100mV/s.
图4为石墨粉与离子液体质量比1:1下所制备的修饰电极在不同扫速下的循环伏安曲线图,电解质溶液为1.0mmol/L的铁氰化钾和0.1mol/L的氯化钾混合液，扫速为0.05、0.06、0.07、0.08、0.09、0.1、0.15、0.2、0.25、0.3V/s。 Figure 4 is the cyclic voltammetry curves of the modified electrode prepared at different scan rates at a mass ratio of graphite powder to ionic liquid of 1:1. The electrolyte solution is 1.0 mmol/L potassium ferricyanide and 0.1 mol/L chlorine Potassium chloride mixed solution, the scan rate is 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.15, 0.2, 0.25, 0.3V/s.
具体实施方式 detailed description
下面给出的实施例对本发明作进一步说明，但不超出本发明保护范围的限制。 The examples given below illustrate the present invention further, but do not go beyond the limitation of the protection scope of the present invention.
实施例1 Example 1
分别称量0.8g的N-丁基-N-甲基哌啶六氟磷酸盐和石墨粉，用移液枪量取250μL的液体石蜡充分混合，在干净的研钵中研磨2-3个小时；将打磨干净的细铜丝插入洗涤干净、长约为5-6cm、内径约为4mm的玻璃管内，并将其固定；将研钵中的混合物装入玻璃管中，然后从玻璃管的上方塞入适量的棉花，用圆柱形金属棒将管内混合物压实，即得到离子液体修饰碳糊电极；使用前，在抛光纸上打磨至镜面。按照上述方法，制备石墨粉和离子液体质量比分别为2:1,3:1,1:2修饰碳糊电极。 Weigh 0.8g of N-butyl-N-methylpiperidine hexafluorophosphate and graphite powder respectively, use a pipette gun to measure 250 μL of liquid paraffin and mix thoroughly, grind in a clean mortar for 2-3 hours ; Insert the polished thin copper wire into a clean glass tube with a length of about 5-6cm and an inner diameter of about 4mm, and fix it; put the mixture in the mortar into the glass tube, and then from the top of the glass tube Insert an appropriate amount of cotton, and compact the mixture in the tube with a cylindrical metal rod to obtain an ionic liquid-modified carbon paste electrode; before use, polish it to a mirror surface on polishing paper. According to the above method, the mass ratios of graphite powder and ionic liquid were 2:1, 3:1, and 1:2 to prepare modified carbon paste electrodes, respectively.
实施例2 Example 2
采用电子扫描显微镜对不同质量比的离子液体修饰碳糊电极进行表征，电极表面形貌如图1所示，A、B、C、D分别为石墨粉与离子液体质量比为1:1,2:1,3:1,1:2时的修饰电极表面形貌图。可以看出质量比为1:1条件下的修饰电极表面最为光滑、平整。 Electron scanning microscope was used to characterize the ionic liquid modified carbon paste electrodes with different mass ratios. The surface morphology of the electrodes is shown in Figure 1. :1, 3:1, 1:2 surface topography of the modified electrode. It can be seen that the surface of the modified electrode is the smoothest and evenest when the mass ratio is 1:1.
实施例3 Example 3
将制得的不同质量比的离子液体修饰碳糊电极置于浓度为1.0mmol/L的铁氰化钾和0.1mol/L的氯化钾混合液中进行循环伏安扫描。如图2所示，曲线a到d分别代表石墨粉和离子液体质量比1:1,2:1,3:1,1:2时的循环伏安曲线，可以看出，当质量比为1:1时，氧化还原峰电流值最大，即在此条件下电极表面的电子转移速率最快。 The prepared ionic liquid modified carbon paste electrodes with different mass ratios were placed in the mixed solution of potassium ferricyanide and 0.1mol/L potassium chloride with a concentration of 1.0mmol/L for cyclic voltammetry scanning. As shown in Figure 2, curves a to d represent respectively the cyclic voltammetry curves of graphite powder and ionic liquid mass ratio 1:1,2:1,3:1,1:2, as can be seen, when mass ratio is 1 :1, the redox peak current value is the largest, that is, the electron transfer rate on the electrode surface is the fastest under this condition.
实施例4 Example 4
考察了不同质量比的电极在1.0mmol/L的铁氰化钾和0.1mol/L的氯化钾混合液中的电化学阻抗谱，结果如图3所示。曲线a,b,c,d分别代表石墨粉和液体离子质量为1:1,2:1,3:1,1:2时的阻抗图，可以看出，四种不同修饰电极的电化学阻抗图谱有明显的不同。曲线a的阻抗值最小，曲线d的阻抗值最大。此结果和实施例3中不同修饰电极循环伏安结果一致，也充分证明了两者质量比为1:1时为最佳条件，此时修饰电极表面上的电子转移速率最快。 The electrochemical impedance spectroscopy of electrodes with different mass ratios in the mixture of 1.0mmol/L potassium ferricyanide and 0.1mol/L potassium chloride was investigated, and the results are shown in Figure 3. Curves a, b, c, and d represent the impedance diagrams when the mass of graphite powder and liquid ions are 1:1, 2:1, 3:1, and 1:2, respectively. It can be seen that the electrochemical impedance of four different modified electrodes The graphs are significantly different. The impedance value of curve a is the smallest, and the impedance value of curve d is the largest. This result is consistent with the cyclic voltammetry results of different modified electrodes in Example 3, and fully proves that the optimal condition is when the mass ratio of the two is 1:1, and the electron transfer rate on the surface of the modified electrode is the fastest at this time.
实施例5 Example 5
选取最佳质量比的离子液体修饰（石墨粉和液体离子质量比例1:1），考察了峰电流与扫速的关系。从图4中可以看出，随着扫速的增加，峰电流逐渐增大，在50~300mV/s范围内氧化峰电流和还原峰电流与v1/2呈良好的线性关系，说明该电极反应是扩散控制过程。说明电极反应过程是由扩散控制的。由于离子液体的存在极大的增加了界面导电效率，使到达电极表面的铁氰化钾能够快速完全的发生电极反应，即电子传递速率大于物质由本体溶液到达电极表面的扩散速度，所以电极反应过程由扩散过程控制。 The ionic liquid modification with the best mass ratio (mass ratio of graphite powder and liquid ion is 1:1) was selected, and the relationship between the peak current and the scan rate was investigated. It can be seen from Figure 4 that with the increase of scan rate, the peak current gradually increases, and the oxidation peak current and reduction peak current have a good linear relationship with v 1/2 in the range of 50~300mV/s, which shows that the electrode Reactions are diffusion controlled processes. It shows that the electrode reaction process is controlled by diffusion. Since the existence of ionic liquid greatly increases the interface conductivity efficiency, the potassium ferricyanide that reaches the electrode surface can quickly and completely undergo electrode reaction, that is, the electron transfer rate is greater than the diffusion rate of the substance from the bulk solution to the electrode surface, so the electrode reaction The process is controlled by the diffusion process.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610168460.4A CN105699455B (en) | 2016-03-23 | 2016-03-23 | A kind of preparation method of Ionic Liquid Modified carbon paste electrode |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 | 1-tert-butyl-3-methylimidazolium bromide ionic liquid modified electrode and its application |
| CN111403805A (en) * | 2020-04-28 | 2020-07-10 | 深圳先进技术研究院 | A composite solid electrolyte, its preparation method 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 |
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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 |
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| NOROUZ MALEKI等: ""High-Performance Carbon Composite Electrode Based on an Ionic Liquid as a Binder"", 《ANALYTICAL CHEMISTRY》 * |
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Cited By (4)
| 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 for highly sensitive detection of nonylphenol and preparation method thereof |
| CN109298054A (en) * | 2018-11-15 | 2019-02-01 | 湖南工程学院 | 1-tert-butyl-3-methylimidazolium bromide ionic liquid modified electrode and its application |
| CN111403805A (en) * | 2020-04-28 | 2020-07-10 | 深圳先进技术研究院 | A composite solid electrolyte, its preparation method and lithium ion battery |
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