CN115047046A - Electrode biological carrier for one-step electrodeposition cross-lamination modification of graphene/polyaniline and preparation method thereof - Google Patents
Electrode biological carrier for one-step electrodeposition cross-lamination modification of graphene/polyaniline and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 84
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 56
- 230000004048 modification Effects 0.000 title claims abstract description 28
- 238000012986 modification Methods 0.000 title claims abstract description 28
- 238000004070 electrodeposition Methods 0.000 title claims abstract description 23
- 238000003475 lamination Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- 238000002484 cyclic voltammetry Methods 0.000 claims description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 5
- 239000004917 carbon fiber Substances 0.000 claims description 5
- 239000003792 electrolyte Substances 0.000 claims description 5
- 229910052697 platinum Inorganic materials 0.000 claims description 5
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- 125000004122 cyclic group Chemical group 0.000 claims 2
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Abstract
The invention provides a preparation method of an electrode biological carrier for one-step electrodeposition cross-lamination modification of graphene/polyaniline, and relates to the technical field of bioelectrochemistry. The preparation method comprises the steps of preparing a graphene oxide/aniline mixed solution, constructing a three-electrode system and cross-laminating modified graphene/polyaniline to obtain the high-performance electrode bio-carrier for the cross-laminating modified graphene/polyaniline by one-step electrodeposition. Compared with an unmodified electrode, the electrode biological carrier with the graphene/polyaniline cross-laminated modified by one-step electrodeposition has the advantages that the electrochemical activity is remarkably improved, the charge transfer resistance is remarkably reduced, the electrochemical activity area is increased, and the biocompatibility is improved.
Description
Technical Field
The invention relates to the technical field of bioelectrochemistry, in particular to an electrode biological carrier for one-step electrodeposition cross-lamination modification of graphene/polyaniline and a preparation method thereof.
Background
The bioelectrochemical systems (BESs) are a novel water treatment technology which utilizes the catalytic action of microorganisms to synchronously realize pollutant degradation and energy recovery. Compared with the conventional non-biological electrode using noble metals such as platinum as a catalyst, the biological electrode has the advantages of low cost, corrosion resistance, and no need of chemical agent regeneration, and thus is one of the research hotspots. However, the biocompatibility of the electrode material and the ability of the electrode material to transfer electrons to microorganisms are major obstacles limiting the application of the bioelectrode in BESs. Therefore, there is a need to develop an electrode bio-carrier material with more excellent performance.
At present, the commonly used electrode materials mainly comprise various carbon materials, including carbon cloth, carbon brush, carbon felt and the like, and the carbon materials are considered to be good substrate materials for loading the biological membrane due to the advantages of large specific surface area, high porosity, good mechanical properties and the like. However, the unmodified carbon-based electrode has a large resistance, so that the extracellular electron transfer efficiency is severely limited, and further modification is required. Graphene is a two-dimensional lamellar structure formed by single-layer carbon atoms, has excellent conductivity, and is proved to be modified by graphene at present, so that the electrode performance of BESs can be effectively improved. The process of reducing graphene oxide to graphene (rGO) can be achieved by an electrochemical method while depositing on the surface of the electrode. However, the nano-sheet structure is easy to aggregate in the graphene modification process, and may have potential toxicity to microbial cells. Polyaniline (PANI) is a conductive high molecular material, is a nano-grade conjugated polymer, has stronger biocompatibility due to the positive charge, has the advantages of simple synthesis, good stability and the like, and is often used as a candidate material for modifying electrodes. However, polyaniline has the disadvantages of poor conductivity, relatively small specific surface area and the like, and is often used together with other materials for carrying out composite modification on the electrode.
In recent years, studies for compositely modifying carbon-based materials with rGO and PANI to overcome their limitations have been increasing. In the research of preparing the rGO/PANI composite modified bio-electrode carrier material, a cyclic voltammetry method is usually adopted to respectively realize the reduction of graphene oxide and the polymerization process of aniline monomers through two steps, so as to prepare a double-layer structure with a certain thickness of rGO and PANI accumulated on the surface of a substrate. The method needs to prepare two electrolytes, namely a GO dispersion solution and an aniline solution, sets two different scanning parameters to complete two depositions, so that the modification method is complex in process and long in required time, and the cyclic voltammetry involves two oxidation and reduction processes in one period, while the two steps of sequentially modifying rGO and PANI on the surface of an electrode mean that half of time and energy are wasted. More notably, reduced graphene oxide (rGO) is a graphene derivative which is easy to aggregate, so that aggregation is often inevitable in the first step of rGO deposition, the specific surface area of the rGO is reduced, and the electrochemical performance of the rGO is not fully exerted.
Disclosure of Invention
In order to overcome the problems that the existing two-step method is long in time for modifying a graphene/polyaniline electrode, more control steps are needed, and graphene sheets are easy to aggregate, the invention provides the electrode biological carrier for modifying the graphene/polyaniline by one-step electrodeposition and cross lamination and the preparation method thereof, the method not only can simultaneously retain respective advantages of two materials, but also can show the effect of '1 +1 > 2', the method is simple in modification step and short in time consumption, and the aggregation of the graphene sheets can be strictly inhibited by doping polyaniline particles, so that the technical effects of increasing the surface active sites of the electrode and improving the electron transfer efficiency of the electrode are realized. The preparation method of the electrode biological carrier for one-step electrodeposition cross-lamination modification of graphene/polyaniline comprises the following steps:
(1) preparing a graphene oxide/aniline mixed solution:
dispersing a graphene oxide aqueous solution by using a 0.1mol/L phosphate buffer solution with the pH of 8.0, and carrying out ultrasonic treatment at room temperature to eliminate the precipitation or agglomeration phenomenon generated at the bottom of the graphene oxide aqueous solution after the graphene oxide aqueous solution is placed for a long time;
then adding aniline into the dispersed graphene oxide solution, continuing to perform ultrasonic dispersion for 10-30min, and diluting the dispersed solution to obtain a graphene oxide/aniline blending solution;
(2) constructing a three-electrode system:
constructing a three-electrode system by taking a carbon-based electrode as a working electrode, a platinum mesh electrode as a counter electrode, Ag/AgCl as a reference electrode and an electrochemical workstation and taking the graphene oxide/aniline blended solution obtained in the step (1) as an electrolyte;
(3) cross-laminated modified graphene/polyaniline:
in a three-electrode system, graphene oxide is reduced to graphene in situ through cyclic voltammetry scanning, aniline is oxidized to polyaniline in situ, and graphene/polyaniline cross lamination modification on the surface of a working electrode is achieved.
Further, in the step (1), the ultrasonic treatment power is 180W, the ultrasonic treatment frequency is 40kHz, and the ultrasonic treatment time is 30-50 min.
Further, in the step (1), the ultrasonic dispersion power is 180W, the ultrasonic dispersion frequency is 40kHz, and the ultrasonic dispersion time is 10-30 min.
Further, in the step (1), the graphene concentration in the diluted graphene oxide/aniline blending solution is 0.3-0.8g/L, and the aniline concentration is 5-10 g/L.
Further, in the step (1), the graphene concentration in the diluted graphene oxide/aniline blending solution is 0.5g/L, and the aniline concentration is 9 g/L.
Further, the carbon-based electrode in the step (2) is one of a carbon fiber electrode, a carbon felt and a carbon cloth.
Further, in the step (3), the cyclic voltammetry scanning range is-1.4V-0.9V, the scanning rate is 50mV/s, and even sections are continuously scanned within the range of 20-40 sections.
Further, in the step (3), when the initial scanning direction of the cyclic voltammetry scanning is set to be the forward direction, graphene is modified on both the first layer and the last layer of the surface of the substrate electrode.
Further, in the step (3), when the initial scanning direction set by the cyclic voltammetry scanning is negative, polyaniline is modified on the first layer and the last layer of the surface of the substrate electrode.
The invention also aims to provide the electrode biological carrier for the one-step electrodeposition cross-lamination modification of graphene/polyaniline, which is prepared by the method.
Compared with the prior art, the invention has the beneficial technical effects that:
compared with an unmodified electrode, the electrode biological carrier with the graphene/polyaniline cross-laminated modified by one-step electrodeposition has the advantages that the electrochemical activity is remarkably improved, the charge transfer resistance is remarkably reduced, the electrochemical activity area is increased, and the biocompatibility is improved.
Drawings
The invention is further illustrated in the following description with reference to the drawings.
Fig. 1a shows a graphene/polyaniline cross-layered modification, and the initial scanning direction is negative, that is, a deposition curve of polyaniline on the outermost layer; fig. 1b is a graphene/polyaniline cross-laminated modification, and the initial scanning direction is the forward direction, that is, a deposition curve of graphene on the outermost layer;
fig. 2 is an SEM photograph of the electrode surface, where fig. 2a and 2b are carbon brush surface features of graphene/polyaniline cross-laminated modification and the outermost layer is polyaniline; fig. 2c and 2d are carbon brush surface morphologies of graphene/polyaniline cross lamination modification, and the outermost layer is graphene;
fig. 3 is a curve of a carbon fiber brush which is cross-layered and modified by graphene/polyaniline and has a surface layer of graphene and polyaniline, respectively, and an unmodified carbon fiber brush when cyclic voltammetry scanning is performed;
fig. 4 is an ac impedance spectrum of a carbon fiber brush and an unmodified carbon fiber brush, which are cross-laminated and modified with graphene/polyaniline and whose surface layers are graphene and polyaniline, respectively.
Detailed Description
The technical solution provided by the present invention is further illustrated by the following examples.
Example 1
A preparation process of an electrode biological carrier for one-step electro-deposition cross-laminated modification of graphene/polyaniline comprises the following steps:
(1) further dispersing the graphene oxide aqueous solution by using a 0.1mol/L phosphate buffer solution with the pH of 8.0, carrying out ultrasonic treatment at room temperature for 30min, adding analytically pure aniline into the graphene oxide buffer solution, and continuing the ultrasonic treatment for 10min to obtain a blended solution with the graphene oxide concentration of 0.5g/L and the aniline concentration of 9 g/L;
(2) constructing a three-electrode system, taking a carbon fiber brush electrode as a working electrode, a platinum mesh electrode as a counter electrode, Ag/AgCl as a reference electrode, and taking the graphene oxide/aniline blended solution as an electrolyte;
(3) under the condition of continuous stirring in a room temperature environment, modifying by using a cyclic voltammetry through an electrochemical workstation, setting a scanning range of-1.4V-0.9V and a scanning speed of 50mV/s, scanning 20 sections, wherein the starting direction of each cycle is negative scanning, namely sequentially performing three reactions in each cycle, namely the oxidation of aniline, the reduction of oxidized graphene and the oxidation of aniline, so as to prepare a cross laminated graphene/polyaniline modified bioelectrochemical system on the surface of a bioelectrode carrier, and the material of the outermost surface of the modified electrode is a polyaniline material.
SEM scanning is carried out on the electrode surface of the electrode biological carrier of the one-step electro-deposition cross-laminated modified graphene/polyaniline, and it can be observed that granular substances are gathered on the outermost layer of the electrode and distributed on the wrinkled sheet layer (fig. 2a and 2b), which illustrates that the idea of controlling the outermost layer to be polyaniline by controlling the initial scanning direction to be negative is successful.
Example 2
The difference from example 1 is that the initial scanning direction is negative, that is, three reactions, that is, the reduction of graphene oxide, the oxidation of aniline, and the reduction of graphene oxide, are performed in sequence in each cycle. SEM scanning of the electrode surface of the electrode bio-carrier modified with graphene/polyaniline by one-step electrodeposition and cross-lamination can observe that the outermost layer of the electrode is covered with a wrinkled graphene sheet layer and that the surface of a particle is covered with graphene (fig. 2c and 2d), which illustrates the success of the idea of controlling the outermost layer to be graphene by controlling the initial scanning direction to be the forward direction.
Test example 1
Electrochemical testing of the electrodes was performed on a three-electrode system using an electrochemical workstation (CHI 660E, chenhua, china):
(1) the electrodes prepared in examples 1 and 2 were compared with the unmodified electrode as the working electrode, respectively, and a platinum mesh electrode and an Ag/AgCl electrode were used as the counter electrode and the reference electrode, respectively;
(2) to pass through N 2 Aerating 1mol/L KCl solution for 30min as electrolyte, and performing cyclic voltammetry scanning at a scanning speed of 50mV/s from-0.4V to 0.6V;
(3) and (3) applying a sinusoidal alternating current wave with the amplitude of 5mV within the frequency range of 0.1-100000 Hz by taking the open-circuit potential as an initial potential, wherein in the obtained Nyquist diagram, the intersection value of a high-frequency range curve and a real axis is the ohmic internal resistance of the system, and the diameter value of a curve semicircle is the charge transfer resistance of the electrode.
As can be seen from fig. 3, under the same voltage, the oxidation and reduction currents of two cathode responses of graphene/polyaniline composite modification are both larger, which proves that the electrode of the invention has higher electrochemical activity;
as can be seen from fig. 4, compared with the unmodified electrode, the charge transfer resistance and the ohmic resistance of the cross laminated modified electrode are both significantly reduced, wherein the charge transfer resistance of the cross laminated modified electrode is significantly reduced, and the electrode with the graphene and polyaniline on the surface layer is 0.32 ohm and 1.49 ohm respectively, which are reduced by about 93% and 71%, which proves that the electrode resistance of the present invention is reduced and has higher conductivity.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. A preparation method of an electrode biological carrier for one-step electrodeposition cross-lamination modification of graphene/polyaniline is characterized by comprising the following steps:
(1) preparing a graphene oxide/aniline mixed solution:
dispersing a graphene oxide aqueous solution by using a 0.1mol/L phosphate buffer solution with the pH of 8.0, and carrying out ultrasonic treatment at room temperature to eliminate the precipitation or agglomeration phenomenon generated at the bottom of the graphene oxide aqueous solution after the graphene oxide aqueous solution is placed for a long time;
then adding aniline into the dispersed graphene oxide solution, continuing ultrasonic dispersion, and diluting the dispersed solution to obtain a graphene oxide/aniline blending solution;
(2) constructing a three-electrode system:
constructing a three-electrode system by taking a carbon-based electrode as a working electrode, a platinum mesh electrode as a counter electrode, Ag/AgCl as a reference electrode and an electrochemical workstation and taking the graphene oxide/aniline blended solution obtained in the step (1) as an electrolyte;
(3) cross-laminated modified graphene/polyaniline:
in a three-electrode system, graphene oxide is reduced to graphene in situ through cyclic voltammetry scanning, aniline is oxidized to polyaniline in situ, and graphene/polyaniline cross lamination modification on the surface of a working electrode is achieved.
2. The method for preparing the electrode bio-carrier for one-step electrodeposition cross-lamination modification of graphene/polyaniline according to claim 1, wherein in the step (1), the ultrasonic treatment power is 180W, the ultrasonic treatment frequency is 40kHz, and the ultrasonic treatment time is 30-50 min.
3. The preparation method of the electrode bio-carrier for one-step electrodeposition cross-lamination modification of graphene/polyaniline according to claim 1, wherein in the step (1), the ultrasonic dispersion power is 180W, the ultrasonic dispersion frequency is 40kHz, and the ultrasonic dispersion time is 10-30 min.
4. The method for preparing the electrode bio-carrier for one-step electrodeposition cross-lamination modification of graphene/polyaniline according to claim 1, wherein in the step (1), the graphene concentration in the diluted graphene oxide/aniline blended solution is 0.3-0.8g/L, and the aniline concentration is 5-10 g/L.
5. The method for preparing the electrode bio-carrier for one-step electrodeposition cross-lamination modification of graphene/polyaniline according to claim 1, wherein in the step (1), the graphene concentration in the diluted graphene oxide/aniline blended solution is 0.5g/L, and the aniline concentration is 9 g/L.
6. The method for preparing the electrode bio-carrier for one-step electrodeposition cross-lamination modification of graphene/polyaniline according to claim 1, wherein the carbon-based electrode in the step (2) is one of a carbon fiber electrode, a carbon felt and a carbon cloth.
7. The method for preparing the electrode bio-carrier for one-step electrodeposition cross-lamination modification of graphene/polyaniline, according to claim 1, wherein in the step (3), the cyclic voltammetry scan range is-1.4V-0.9V, the scan rate is 50mV/s, and the continuous scan even number segment is in the range of 20-40 segments.
8. The method for preparing the electrode bio-carrier for one-step electrodeposition cross-lamination modification of graphene/polyaniline as claimed in claim 1, wherein in step (3), when the initial scanning direction of the cyclic voltammetric scan is set to be the forward direction, graphene is modified on both the first layer and the last layer of the surface of the substrate electrode.
9. The method for preparing the electrode bio-carrier for one-step electrodeposition cross-lamination modification of graphene/polyaniline as claimed in claim 1, wherein in step (3), when the initial scanning direction of the cyclic voltammetric scan is set to be negative, polyaniline is modified on both the first layer and the last layer of the surface of the substrate electrode.
10. An electrode biological carrier for one-step electrodeposition cross-lamination modification of graphene/polyaniline, which is prepared by the method of any one of claims 1 to 9.
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