CN110429286B - Application of titanium nitride nanorod array in anode of microbial fuel cell - Google Patents

Application of titanium nitride nanorod array in anode of microbial fuel cell Download PDF

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CN110429286B
CN110429286B CN201910759571.6A CN201910759571A CN110429286B CN 110429286 B CN110429286 B CN 110429286B CN 201910759571 A CN201910759571 A CN 201910759571A CN 110429286 B CN110429286 B CN 110429286B
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anode
fuel cell
titanium nitride
microbial fuel
nanorod array
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CN110429286A (en
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颜美
刘达
果崇申
常庆环
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Harbin Institute of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/8663—Selection of inactive substances as ingredients for catalytic active masses, e.g. binders, fillers
    • H01M4/8673—Electrically conductive fillers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/16—Biochemical fuel cells, i.e. cells in which microorganisms function as catalysts
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M2004/8678—Inert electrodes with catalytic activity, e.g. for fuel cells characterised by the polarity
    • H01M2004/8689—Positive electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Abstract

The invention discloses an application of a titanium nitride nanorod array in a microbial fuel cell anode, which is characterized by excellent biocompatibility, good chemical stability, high conductivity, simple preparation, low price, nanorod array structure in-situ growth on carbon cloth and the like based on titanium nitrideGeobacter‑soliThe electrogenesis bacteria are efficiently enriched, the enrichment rate reaches 97.2 percent, and the output performance of the microbial fuel cell is further effectively improved. Titanium nitride nano anode pairGeobacter‑ soliThe efficient enrichment of the electrogenic bacteria fundamentally overcomes the defects of low output electric energy, unstable operation and the like of the current microbial fuel cell, and the pairGeobacter‑soliThe high enrichment rate of the electrogenic bacteria is also the highest among the anode materials studied at present. Therefore, the titanium nitride nanorod array can be applied to the anode of the microbial fuel cell, and the electricity generation power and the electric energy output stability of the cell are effectively improved.

Description

Application of titanium nitride nanorod array in anode of microbial fuel cell
Technical Field
The invention belongs to the technical field of materials, biology and environment, and relates to application of a titanium nitride nanorod array capable of efficiently enriching geobacillus in a microbial fuel cell anode.
Background
With the rapid development of economic globalization, the problem of water pollution becomes more and more severe, and a large amount of energy needs to be consumed in the sewage treatment process, and the microbial fuel cell can convert a large amount of energy contained in sewage into electric energy through the biocatalysis effect of the electricity-producing bacteria, so that the waste is changed into valuable, and the sewage treatment is changed from an energy consumption type to a self-supporting or energy-producing type. At present, the transfer mode of electrons between the electrogenic bacteria and the anode includes direct contact transfer of bacteria and the anode, nanowire-mediated rapid electron transfer and electron shuttle-mediated electron transfer, so that the anode is one of the key factors which restrict the performance of the microbial fuel cell. Researchers seek to improve the transfer efficiency of extracellular electrons and improve the performance of microbial fuel cells by developing different anode materials. However, whether the efficiency of transferring electrons out of cells is improved depends on the enrichment degree of the anode on the electrogenic bacteria,Geobacter(Geobacillus) is a classical Chinese vector of mixed floraThe type of the electrogenic bacteria has stronger electrogenesis capability. Researches show that when a plurality of bacterial strains are cultured as pure bacteria, the electrogenesis power density is much lower than that of mixed culture, the organic pollutants can be degraded in a grading way due to the respective advantages of a plurality of floras in the mixed culture, and then electrons are transferred to an anode by utilizing the electrogenesis bacteria, so that the electrons are transferred to a cathode through an external circuit to generate current, and in addition, the electrogenesis bacteria and a biomembrane automatically screened by the anode in the mixed floras are more stable under the system. Thus despite the knowledge thatGeobacterHas strong electrogenesis ability, but can not simply inoculate the mixed bacteria for pure bacteria culture for microbial fuel cells, but the mixed bacteria can be automatically screened by using anode materials during mixed inoculation, so that the mixed bacteria can be effectively enrichedGeobacterIs particularly important. So far, no efficient enrichment has been reportedGeobacterAn anode of a microbial fuel cell of electrogenesis bacteria. Therefore, a method capable of efficiently enrichingGeobacterThe anode material of the electrogenic bacteria is in need.
Disclosure of Invention
In order to overcome the defects that the conventional microbial fuel cell anode has low enrichment degree on electrogenic bacteria and limits the electrogenic performance of the microbial fuel cell, the invention provides the application of the titanium nitride nanorod array capable of efficiently enriching the geobacter in the microbial fuel cell anode.
The purpose of the invention is realized by the following technical scheme:
based on the characteristics of excellent biocompatibility of titanium nitride, better stability of transition metal nitride, simple preparation, low price, unique nanorod array structure and the like, the titanium nitride nanorod array capable of efficiently enriching the geobacter is used as the anode pair of the microbial fuel cell and grown in situ by taking carbon cloth as a substrateGeobacter-soliThe electrogenic bacteria are efficiently enriched, the enrichment rate reaches 97.2 percent, the performance of the battery can be effectively improved, and the power density output is high (4.025W/m)2) And (4) outputting current stably for a long time, and continuously discharging for 6 to 7 d in a single period.
A method for improving the electricity generation power and the electric energy output stability of a microbial fuel cell by utilizing the titanium nitride nanorod array anode comprises the following steps:
the method comprises the following steps: the method is characterized in that a titanium nitride nanorod array is used as an anode, a titanium wire is strung for the anode, a carbon fiber brush is used as a cathode, a microbial fuel cell reactor is used as an operation device, the effective volume of a cathode chamber is 100 ml, 80-90 ml anolyte is added into the anode chamber, 100 ml catholyte is added into the cathode chamber, and the formula of the anolyte is as follows: 1.5-2 g/L anode substrate (anhydrous sodium acetate, glucose, lactate or other substrates), 0.1 ml/L vitamin solution, 12.5 ml/L microelement, and the formula of the catholyte is as follows: 16.4 g/L K3[Fe(CN)6]，3.7 g/L KCl；
Step two: adding 10-20 ml of inoculation liquid into an anode chamber for inoculation, then adding a 1000 omega resistor, connecting a cathode and an anode to form a closed loop, placing the closed loop in a constant-temperature incubator at 37 ℃ to enable the closed loop to stably operate, using a DAQ6510 digital multimeter to monitor the voltage output condition in real time, and respectively replacing new cathode and anode liquids when the voltage is reduced to 0.05V;
step three: after the battery operates stably, the characteristics such as electrochemical impedance, power density, anode scanning electron microscope after inoculation, anode microbial community analysis and the like show that the titanium nitride nanorod array anode can be efficiently enrichedGeobacter-soliThe electricity generating bacteria can effectively improve the electric energy output and the operation stability of the microbial fuel cell.
In the present invention, the inoculum may be anaerobic sludge water, acclimated cell anode effluent, or a mixture of the two, such as: the inoculation liquid consists of 10-20 ml anaerobic sludge water and 10-15 ml acclimated battery anode effluent (namely the battery anode effluent which stably runs, specifically, 10-20 ml anaerobic sludge is used for inoculating a microbial fuel cell, and then the microbial fuel cell is placed in a 37 ℃ constant temperature incubator, and the anode liquid which continuously runs for 15-20 days can be used for starting and inoculating other batteries), wherein: anaerobic sludge comes from a Harbin Taiping sewage treatment plant. When the voltage is reduced to 0.05V after the battery runs for a period, the anolyte and the catholyte are respectively replaced, the anolyte is poured out of about 80-90 ml, the stock solution of about 10-20 ml is reserved in the anode chamber to facilitate the quick start of the battery, the anolyte is newly dispensed by adding about 80-90 ml, the catholyte is completely poured out, and the newly dispensed potassium ferricyanide solution is added.
In the invention, the electrochemical impedance spectrum test after the attachment of the bacterial membrane is to test in a mixed solution of 5 mM PBS solution and 5 mM potassium ferricyanide solution under a three-electrode system (a saturated calomel electrode is used as a reference electrode, and a platinum sheet is used as a counter electrode) when the battery continuously runs for about 20 d and a stable bacterial membrane is formed on the surface of an anode.
In the invention, the power density curve test shows that when the external resistor is replaced to calculate the corresponding current density and power density, the resistance value is reduced to be below 500 omega, and the reduction range of the resistance value is less than 50 omega, so that the power density curve is prevented from being folded back.
In the invention, after inoculation, a sample is observed and prepared by an anode scanning electron microscope, after bacterial immobilization and gradient dehydration, the sample is dried fully, and then, gold spraying treatment is carried out so as to have a clear object image under the scanning electron microscope, and the gold spraying time is about 2 min.
In the invention, the anode microbial community is analyzed, when the battery continuously and stably runs for about 30 d after inoculation, the microbes on the anode surface are fully attached to form a biological membrane, and then DNA extraction sequencing analysis is carried out.
Compared with the anode of the existing microbial fuel cell, the invention has the following advantages:
(1) The titanium nitride nanorod array anode can be efficiently enrichedGeobacter-soliIts percentage of occupancy in the anodic microbial community is up to 97.2%.
(2) Titanium nitride itself has excellent electric conductivity and biocompatibility, and its nanorod array structure that generates on the carbon cloth in situ can be fine improves the roughness on carbon cloth surface for the earth's bacillus utilizes cilium easily to snatch the array and adhere to, and it has the electric conductivity of class noble metal, can transmit the electron that is passed out by the bacterium through the metabolism to carbon cloth rapidly, thereby can the short-term delivery for outer circuit, promotes the electrogenesis efficiency of battery.
(3) The titanium nitride has precious metal-like property, good electrocatalytic activity, simple synthesis process and low cost.
(4) The titanium nitride has better stability, can be applied to the anode of the microbial fuel cell, and effectively improves the stability of long-term electric energy output of the microbial fuel cell.
(5) The invention is based on the characteristics of excellent biocompatibility, good chemical stability, high conductivity, simple preparation, low price, nanorod array structure in-situ growth on carbon cloth and the like of titanium nitride, and the invention is suitable for the field of electrochemical machiningGeobacter-soliThe electrogenic bacteria are efficiently enriched, the enrichment rate reaches 97.2 percent, the output performance of the microbial fuel cell is further effectively improved, and the maximum power density output is 4.025W/m22.2 times of the anode of the carbon cloth of the control group, and the single-period continuous discharge reaches 6 to 7 d.
(7) Titanium nitride nanorod array anode pairGeobacter-soliThe efficient enrichment of the electrogenic bacteria fundamentally overcomes the defects of low output electric energy, unstable operation and the like of the current microbial fuel cell, and the pairGeobacter-soliThe high enrichment rate of the electrogenic bacteria is also the highest in the anode materials studied at present. Therefore, the titanium nitride nanorod array can be applied to the anode of the microbial fuel cell, and the electricity generation power and the electric energy output stability of the cell are effectively improved.
Drawings
FIG. 1 is the X-ray diffraction pattern of the nano-rod array of titanium nitride;
FIG. 2 is a scanning electron microscope image of the titanium nitride nanorod array anode;
FIG. 3 is a scanning electron microscope image of the titanium nitride nanorod array anode with microorganisms attached thereon;
FIG. 4 is a scanning electron microscope image of bare carbon cloth with microbes attached to the anode;
FIG. 5 is a graph of voltage output for continuous operation;
FIG. 6 is a plot of polarization curve and power density;
FIG. 7 is the electrochemical impedance spectrum after the biofilm attachment on the anode;
FIG. 8 is a log plot of microorganisms on the anode at the seed level.
Detailed Description
The technical solutions of the present invention are further described below with reference to the drawings, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
The invention provides an application of a titanium nitride nanorod array capable of efficiently enriching geobacillus in a microbial fuel cell anode, which comprises the following specific application steps:
the method comprises the following steps: preparing a titanium nitride nanorod array anode, and preparing a carbon brush cathode, an anode chamber and a cathode chamber.
Step two: the mixed sludge is used for inoculation.
Step three: putting into a constant temperature incubator at 37 ℃ to ensure that the incubator operates stably.
Step four: and after the battery runs stably, performing battery performance test and analyzing the composition of the anode microbial community.
In the first step, the anode of the titanium nitride nanorod array is a nanorod array grown in situ on the surface of carbon cloth, and the material is prepared by entrusting eastern Dian scientific research platform (the related preparation method is also referred to in the literature: lu X, wang G, zhai T, et al. Stabilized TiN nanowire arrays for high-performance and flexible superparamers [ J ]. Nano Lett, 2012, 12 (10): 5376-81.). The X-ray diffraction test (figure 1) shows that the crystal form of the titanium nitride nanorod is cubic, and the titanium nitride nanorod is uniformly grown on the carbon fiber of the carbon cloth as can be seen from figure 2. The microbial fuel cell reactor used was of the two-compartment type and the volumes of the anode and cathode compartments were 100 ml.
In the second step, the anaerobic sludge comes from a Harbin Taiping sewage treatment plant, and the inoculation liquid is sludge water of 10-20 ml.
In the third step, when the battery runs in a constant temperature incubator at 37 ℃, a 1000-ohm resistor is additionally arranged, and the voltage output condition of the battery is monitored in real time by using a DAQ6510 digital multimeter. When the voltage of the battery is reduced to be below 0.05V, the battery is taken out, the anolyte and the catholyte are respectively replaced, the catholyte is completely poured out, 100 ml is added again to newly match the catholyte, the anolyte keeps about 10-20 ml stock solution, and about 80-90 ml is added to newly match the anolyte, so that the battery can be quickly started.
In the fourth step, the cell performance test includes an output voltage curve and a power density curve, and from the output voltage curve of fig. 5, the maximum output voltage of the titanium nitride anode is 0.655V, which is significantly higher than 0.535V of the carbon cloth, and the power output lasts for 6~7 days. The method for testing the power density of the battery comprises the following steps: when the anode liquid and the cathode liquid are replaced, the battery voltage is increased to the highest, the external resistor is removed to enable the open circuit to be 1 h, then the resistor box is connected, the resistors are sequentially decreased from 2000, 1000, 800, 700, 600, 550, 500, 450, 400, 350, 300 and 250 to 200 omega, the corresponding voltage value under each resistor is sequentially recorded, and the corresponding current and power are sequentially calculated through I = U/R and P = UI. Then, divided by 2 × 10-4 m2The corresponding current density and power density are obtained. From the power density curve of FIG. 6, the maximum power density of the titanium nitride anode is 4.025W/m2Of carbon cloth (1.872W/m)2) As much as 2.2 times.
Based on the reason of high electric energy output realized by the titanium nitride nanorod array anode, the invention respectively characterizes in three aspects of the attachment speed of microorganisms on the anode, the electrochemical impedance spectrum of the anode after the attachment of the bacterial membrane and the composition of the anode microbial community. FIG. 3 is a scanning electron microscope image of 2.5-3 d after titanium nitride anode inoculation, FIG. 4 is a scanning electron microscope image of 2.5-3 d after bare carbon cloth anode inoculation, it can be seen that a large amount of microorganisms have been attached to the surface of the titanium nitride anode, a thin bacterial film has been formed in a partial region, and only a small amount of bacteria are attached to the carbon cloth anode sparsely, which is consistent with the shorter voltage start time of the titanium nitride anode of FIG. 5. FIG. 7 is an electrochemical impedance spectrum measured when the cell operates stably at 25-30 d, and it can be seen that the charge transfer impedance (85.5 Ω) of the titanium nitride anode is significantly lower than that of the carbon cloth (385.8 Ω), which has excellent power output resultAre matched. FIG. 8 shows the sequencing results of the anode in 30 d stable cell operation, which can be seen on the titanium nitride anodeGeobacter-soliThe proportion of the electrogenic bacteria is up to 97.2 percent, and is obviously higher than that of a carbon cloth (70.7 percent) anode, and the titanium nitride nanorod array anode pairGeobacter-soliThe high-efficiency enrichment of the electrogenic bacteria enables the titanium nitride nanorod array-based anode to have stable high power output.
The invention will be further described with reference to the following specific examples, which are not intended to limit the invention:
example 1
The invention provides an application of a titanium nitride nanorod array capable of efficiently enriching geobacillus in a microbial fuel cell anode, which comprises the following specific application steps:
the method comprises the following steps: respectively shearing a titanium nitride nanorod array anode and a carbon cloth anode of 1 multiplied by 1 cm, penetrating and fixing the titanium nitride nanorod array anode and the carbon cloth anode from the middle by using a titanium wire, assembling a double-chamber microbial fuel cell reaction device, wherein the effective volume of a cathode chamber and an anode chamber is 100 ml, 80ml of anolyte is added into the anode chamber, 100 ml catholyte is added into the cathode chamber, and the formula of the anolyte is as follows: 2 g/L anhydrous sodium acetate, vitamin solution 0.1 ml/L, trace elements 12.5 ml/L, and a catholyte formula as follows: 16.4 g/L K3[Fe(CN)6]，3.7 g/L KCl。
Step two: taking 10 ml anaerobic sludge and 10 ml acclimatized anode chamber effluent as inoculation liquid, and using anhydrous sodium acetate as a substrate.
Step three: the assembled microbial fuel cell reactor was placed in a 37 ℃ incubator and its voltage output was monitored in real time using a DAQ6510 digital multimeter.
Example 2
The difference between this embodiment and embodiment 1 is that the clipping of the anode size is not limited to 1 × 1 cm, and can be performed as needed.
Example 3
This example is different from example 1 in that the microbial fuel cell reactor is not limited to the double chamber type reactor, but can be used for an air single chamber reactor and other types of reactors.
Example 4
The difference between this example and example 1 is that the inoculum solution is not limited to 10 ml anaerobic sludge +10 ml acclimatized anode effluent, and only a suitable amount of anaerobic sludge or a suitable amount of anode effluent of another acclimatized cell may be used. The addition of the acclimated anode effluent contributes to the rapid start-up of the cell, and therefore, the selection of the inoculation solution for the cell can be determined according to actual needs.
Example 5
This example differs from example 1 in that the anode substrate is not limited to anhydrous sodium acetate, but glucose or lactate and other substrates can be used.

Claims (7)

1. A method for improving the electricity generation power and the electric energy output stability of a microbial fuel cell by utilizing a titanium nitride nanorod array anode is characterized by comprising the following steps:
the method comprises the following steps: the method comprises the following steps of taking a titanium nitride nanorod array as an anode, a carbon fiber brush as a cathode, a microbial fuel cell reactor as an operation device, adding 80-90 ml anolyte into an anode chamber, and adding 100 ml catholyte into a cathode chamber, wherein the titanium nitride nanorod array is a titanium nitride nanorod array which grows in situ by taking carbon cloth as a substrate;
step two: adding 10-20 ml inoculation liquid into an anode chamber for inoculation, wherein the inoculation liquid is anaerobic sludge water, domesticated battery anode effluent water or a mixture of the anaerobic sludge water and the domesticated battery anode effluent water, then adding a 1000 omega resistor, connecting a cathode and an anode to form a closed loop, placing the closed loop in a 37 ℃ constant temperature incubator to enable the closed loop to stably operate, monitoring the voltage output condition in real time, and respectively replacing new cathode and anode liquid when the voltage is reduced to 0.05V;
step three: after the battery runs stably, the analysis and the characterization of electrochemical impedance, power density, anode scanning electron microscope after inoculation and anode microbial community show that the titanium nitride nanorod array anode can be efficiently enrichedGeobacter- soliThe enrichment rate of the electrogenic bacteria reaches 97.2 percent, thereby effectively improving the electric energy output and the operation stability of the microbial fuel cell.
2. The method for improving the power generation and the electric energy output stability of the microbial fuel cell by using the titanium nitride nanorod array anode as claimed in claim 1, wherein the effective volume of the cathode and anode chambers of the fuel cell reactor is 100 ml.
3. The method for improving the electricity generation power and the electric energy output stability of the microbial fuel cell by utilizing the titanium nitride nanorod array anode of claim 1, wherein the anolyte is prepared from the following components in percentage by weight: 1.5-2 g/L anode substrate, 0.1 ml/L vitamin solution and 12.5 ml/L microelement.
4. The method for improving the electrogenic power and the electric energy output stability of the microbial fuel cell by utilizing the titanium nitride nanorod array anode of claim 3, wherein the anode substrate is anhydrous sodium acetate, glucose or lactate.
5. The method for improving the electricity generation power and the electric energy output stability of the microbial fuel cell by utilizing the titanium nitride nanorod array anode as claimed in claim 1, wherein the catholyte formula is as follows: 16.4 g/L K3[Fe(CN)6]，3.7 g/L KCl。
6. The method for improving the power generation power and the electric energy output stability of the microbial fuel cell by using the titanium nitride nanorod array anode according to claim 1, wherein the acclimated cell anode effluent is obtained by a method comprising the following steps: inoculating the microbial fuel cell with 10-20 ml anaerobic sludge, then placing the microbial fuel cell into a 37 ℃ constant temperature incubator, and continuously operating the anolyte for 15-20 days to start and inoculate other cells.
7. The method for improving the generated power and the electric energy output stability of the microbial fuel cell by using the titanium nitride nanorod array anode according to claim 1, wherein when the voltage is reduced to 0.05V, the anolyte and the catholyte are respectively replaced, the anolyte is poured out of 80-90 ml, the stock solution of 10-20 ml is reserved in an anode chamber, then 80-90 ml is added for newly dispensing the anolyte, the catholyte is completely poured out, and the newly dispensed catholyte is added.
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