CN113013421B - Preparation method and application of PDMS-based silver nanowire/nano gold/nano nickel composite electrode - Google Patents
Preparation method and application of PDMS-based silver nanowire/nano gold/nano nickel composite electrode Download PDFInfo
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- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
- H01M4/8652—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites as mixture
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
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- H—ELECTRICITY
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention belongs to the technical field of fuel cell electrodes, and discloses a preparation method and application of a PDMS-based silver nanowire/nano-gold/nano-nickel composite electrode. Using Polydimethylsiloxane (PDMS) as a flexible substrate, using a mixed solution of polyvinyl alcohol and glycerol to modify a hydrophilic surface layer on the flexible substrate, using a silver nanowire ethanol solution as a conductive layer, and depositing nano gold-nickel particles on the conductive layer by using an electrochemical deposition method to prepare a silver nanowire/nano gold/nano nickel composite electrode based on PDMS; the nano nickel particles are deposited on the nano gold particles, and the nano gold particles are deposited on the silver nanowires. The fuel cell anode with higher catalytic activity and stability is obtained, the conversion rate of chemical energy is improved, and the development of the fuel cell is promoted.
Description
Technical Field
The invention belongs to the technical field of fuel cell electrodes, and relates to a preparation method and application of a PDMS-based silver nanowire/nano-gold/nano-nickel composite electrode.
Background
Fuel cells, while one of the representatives of new energy technologies, are not an emerging concept. The fuel cell directly catalyzes the reaction of fuel and oxygen through the catalyst to convert chemical energy into electric energy, the energy efficiency is up to 70%, and the product is mostly water with extremely low damage to the environment. Fuel cells can be classified into proton exchange membrane fuel cells, solid oxide fuel cells, molten carbonate fuel cells, alkaline fuel cells, and the like, according to electrolyte differentiation.
Although fuel cells have great advantages in some aspects, there are problems in terms of life, stability, etc., and improving the life and stability of fuel cells has become a hot spot research problem.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method and application of a PDMS-based silver nanowire/nano gold/nano nickel composite electrode, develops a non-enzymatic fuel cell anode, combines the advantages of nano materials, obtains a fuel cell anode with higher catalytic activity and stability, improves the conversion rate of chemical energy, and promotes the development of a fuel cell.
The above object of the present invention is achieved by the following technical solutions:
a preparation method of a silver nanowire/nano-gold/nano-nickel composite electrode (NiNPs/AuNPs/AgNWS/PDMS electrode) based on PDMS; using Polydimethylsiloxane (PDMS) as a flexible substrate, using a mixed solution of polyvinyl alcohol and glycerol to modify a hydrophilic surface layer on the flexible substrate, using a silver nanowire ethanol solution as a conductive layer, and depositing nano gold-nickel particles on the conductive layer by using an electrochemical deposition method to prepare a silver nanowire/nano gold/nano nickel composite electrode based on PDMS; the nano nickel particles are deposited on the nano gold particles, and the nano gold particles are deposited on the silver nanowires.
The preparation method of the PDMS-based silver nanowire/nano-gold/nano-nickel composite electrode (NiNPs/AuNPs/AgNWS/PDMS electrode) comprises the following specific preparation steps:
(1) Manufacturing a PDMS substrate;
manufacturing a PDMS substrate by adopting a photoetching technology; spin-coating photoresist on the clean surface of the silicon wafer, shielding a mask plate containing electrode patterns, and finally exposing and developing to obtain a silicon wafer template; placing a silicon wafer template in a disposable culture dish, and pouring a PDMS mixed solution with the mass ratio of 8-15:1; then putting the mixture into a vacuum dryer to suck bubbles in the PDMS mixed solution under negative pressure, and using the mixture for 2 to 3 hours; taking out, putting into a constant temperature oven at 60-100 ℃ for heating and curing for 1h, and cutting into 12 electrode substrates; the prepared electrode substrate is treated by an adhesive tape (purchased from 3M company in the United states) to remove dust attached to the surface, and then is put into an ultraviolet ozone cleaner to be cleaned for 2-30min, so as to obtain the PDMS substrate with the fixed-shape groove;
(2) Modification of a hydrophilic layer on the surface of the PDMS substrate; the method comprises the following specific steps:
(a) Preparing a mixed aqueous solution of 2-4% PVA and 5-7% PVP by mass percent; preferably, a mixed aqueous solution of 4% PVA and 7% PVP in percentage by mass is prepared;
(b) Soaking the prepared PDMS substrate in a mixed solution of PVA and PVP for 20-50min, and then drying in a vacuum oven at 60-80 ℃ for 2h; preferably, the prepared PDMS substrate is soaked in a mixed solution of PVA and PVP for 20min, and then is put into a vacuum oven at 60-80 ℃ for drying for 2h;
(c) Repeating step (b) once;
(d) Placing the PDMS substrate into a vacuum oven at 80-100 ℃ for heat fixing for 20-30min;
(e) Repeating the steps (b) and (d) once to obtain a PDMS substrate with a surface hydrophilic layer modified;
(3) Preparation of AgNWs/PDMS Plastic electrode
Mixing absolute ethyl alcohol and water according to the volume ratio of 9:1 as a solvent to prepare a silver nanowire solution with the concentration of 5mg/mL, uniformly spreading the silver nanowire solution in a groove on the surface of a PDMS substrate, and standing and drying at room temperature for more than one day to prepare an AgNWS/PDMS plastic electrode;
(4) Preparing an AuNPs/AgNWs/PDMS electrode by flower-shaped nano gold deposition;
immersion of AgNWs/PDMS Plastic electrode with three electrode System 0.2. 0.2M H 2 SO 4 And 4mg/m L KAuCl 4 A platinum electrode was used as a counter electrode and Ag/Ag Cl as a reference electrode. Setting electro-deposition parameters of an electrochemical workstation by adopting a potential-time curve: setting the current to 0.2A for 1600s, and carrying out deposition. The deposited electrode is protected by nitrogen, and is kept for three days for standby; preparing an AuNPs/AgNWs/PDMS electrode;
(5) Preparing a silver nanowire/nano-gold/nano-nickel composite electrode based on PDMS;
adopting a three-electrode system, taking AuNPs/AgNWs/PDMS with a nano structure as a working electrode, taking an Ag/AgCl electrode and a platinum wire electrode as a reference electrode and a counter electrode, and putting the electrodes into an electrolytic cell containing nickel sulfate solution; setting electro-deposition parameters of an electrochemical workstation by adopting a chronopotentiometry: the upper limit voltage is-1V, the holding time is 300s, the lower limit voltage is-0.6V, the holding time is 100s, the electrode is immediately taken out after deposition, the electrode is washed with deionized water for many times, the electrode is protected by nitrogen, and the electrode is kept for three days for standby; and preparing the PDMS-based silver nanowire/nano-gold/nano-nickel composite electrode.
Further, the PDMS substrate prepared in step (1) is preferably: manufacturing a PDMS substrate by adopting a photoetching technology; spin-coating photoresist on the clean surface of the silicon wafer, shielding a mask plate containing electrode patterns, and finally exposing and developing to obtain a silicon wafer template; placing a silicon wafer template in a disposable culture dish, and pouring a PDMS mixed solution with the mass ratio of 10:1; then putting the mixture into a vacuum dryer to suck bubbles in the PDMS mixed solution under negative pressure, and taking 2 hours; taking out, putting into a constant temperature oven at 80 ℃ for heating and curing for 1h, and cutting into 12 electrode substrates; the prepared electrode substrate was treated with an adhesive tape (purchased from 3M company in usa) to remove dust attached to the surface, and then put into an ultraviolet ozone cleaner to clean for 2min, thereby obtaining a PDMS substrate with a groove of a fixed shape.
The application of the PDMS-based silver nanowire/nano-gold/nano-nickel composite electrode (NiNPs/AuNPs/AgNWS/PDMS electrode) in lactose solution electrocatalytic oxidation construction of lactose fuel cells. The method comprises the following steps:
the method comprises the steps of forming a three-electrode system by taking a PDMS-based silver nanowire/nano gold/nano nickel composite electrode as a working electrode, a Ag/AgCl electrode as a reference electrode and a platinum wire as a counter electrode, and combining the three-electrode system with lactose solution taking potassium hydroxide solution as electrolyte as fuel to form the lactose fuel cell.
Further, the electrolyte is 0.01 to 1mol/LKOH, preferably 1mol/LKOH, and the pH is 14.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts PDMS and silver nanowires to prepare an electrode with high sensitivity to lactose, and the electrode has the advantages of good catalytic effect, high sensitivity, good selectivity, stable structure and the like when lactose is used as base solution.
The invention provides a method for preparing a PDMS substrate, which comprises the following steps: pouring PDMS mixed solution with the mass ratio of 8-15:1; then putting the mixture into a vacuum dryer to suck bubbles in the PDMS mixed solution under negative pressure, and using the mixture for 2 to 3 hours; because the bubbles cannot be eliminated when the time is shorter than the time, the cost is increased and the efficiency is reduced when the time is too long; and (3) taking out, putting into a constant-temperature oven at 60-100 ℃ for heating and curing for 1h, wherein the substrate obtained in the temperature range is too soft, and the substrate obtained in the temperature range is too hard.
According to the technical scheme provided by the invention, the silver nanowire solution with the concentration of 5mg/mL is selected, and the silver nanowire solution is uniformly spread and has good conductivity.
Drawings
FIG. 1 is a surface topography of a nano-gold/nano-nickel composite electrode based on PDMS silver nanowires.
FIG. 2 is a graph comparing cyclic voltammograms of lactose solution and blank solution.
FIG. 3 is a cyclic voltammogram of lactose solutions at different sweep rates.
Figure 4 is a standard graph of lactose at different sweep rates.
Fig. 5 is a graph of the anti-poisoning of a nano-gold/nano-nickel composite electrode based on PDMS silver nanowires.
Fig. 6 is a graph of spreading results of silver nanowire solutions of different concentrations. In the figure, (a) is 1mg/mL, (b) is 3mg/mL, (c) is 5mg/mL, (d) is 7mg/mL, and (e) is 10mg/mL.
Detailed Description
The present invention is described in detail below by way of specific examples, but the scope of the present invention is not limited thereto. Unless otherwise specified, the experimental methods used in the present invention are all conventional methods, and all experimental equipment, materials, reagents, etc. used can be obtained from commercial sources.
Example 1
The preparation method of the PDMS-based silver nanowire/nano-gold/nano-nickel composite electrode (NiNPs/AuNPs/AgNWS/PDMS electrode) comprises the following specific preparation steps:
(1) Manufacturing a PDMS substrate;
manufacturing a PDMS substrate by adopting a photoetching technology; spin-coating photoresist on the clean surface of the silicon wafer, shielding a mask plate containing electrode patterns, and finally exposing and developing to obtain a silicon wafer template; placing a silicon wafer template in a disposable culture dish, and pouring a PDMS mixed solution with the mass ratio of 10:1; then putting the mixture into a vacuum dryer to suck bubbles in the PDMS mixed solution under negative pressure, and taking 2 hours; taking out, putting into a constant temperature oven at 80 ℃ for heating and curing for 1h, and cutting into 12 electrode substrates; the prepared electrode substrate is treated by an adhesive tape (purchased from 3M company in the United states) to remove dust attached to the surface, and then is put into an ultraviolet ozone cleaner to be cleaned for 2min, so that a PDMS substrate with a groove with a fixed shape is obtained;
(2) Modification of a hydrophilic layer on the surface of the PDMS substrate; the method comprises the following specific steps:
(a) Preparing a mixed aqueous solution of 4% PVA and 7% PVP by mass percent;
(b) Soaking the prepared PDMS substrate in a mixed solution of PVA and PVP for 20min, and then drying in a vacuum oven at 60 ℃ for 2h;
(c) Repeating step (b) once;
(d) Placing the PDMS substrate into a vacuum oven at 100 ℃ for heat fixing to 20 min;
(e) Repeating the steps (b) and (d) once to obtain a PDMS substrate with a surface hydrophilic layer modified;
(3) Preparation of AgNWs/PDMS Plastic electrode
Mixing absolute ethyl alcohol and water according to the volume ratio of 9:1 as a solvent to prepare a silver nanowire solution with the concentration of 5mg/mL, uniformly spreading the silver nanowire solution in a groove on the surface of a PDMS substrate, and standing and drying at room temperature for more than one day to prepare an AgNWS/PDMS plastic electrode;
(4) Preparing an AuNPs/AgNWs/PDMS electrode by flower-shaped nano gold deposition;
a three electrode system was used, with an AgNWs/PDMS ductile electrode immersed in a mixture of 0.2M H2SO4 and 4mg/m L KAuCl4, using a platinum electrode as the counter electrode and Ag/Ag Cl as the reference electrode. Setting electro-deposition parameters of an electrochemical workstation by adopting a potential-time curve: setting the current to 0.2A for 1600s, and carrying out deposition. The deposited electrode is protected by nitrogen, and is kept for three days for standby; preparing an AuNPs/AgNWs/PDMS electrode;
(5) Preparing a silver nanowire/nano-gold/nano-nickel composite electrode based on PDMS;
adopting a three-electrode system, taking AuNPs/AgNWs/PDMS with a nano structure as a working electrode, taking an Ag/AgCl electrode and a platinum wire electrode as a reference electrode and a counter electrode, and putting the electrodes into an electrolytic cell containing nickel sulfate solution; setting electro-deposition parameters of an electrochemical workstation by adopting a chronopotentiometry: the upper limit voltage is-1V, the holding time is 300s, the lower limit voltage is-0.6V, the holding time is 100s, the electrode is immediately taken out after deposition, the electrode is washed with deionized water for many times, the electrode is protected by nitrogen, and the electrode is kept for three days for standby; and preparing the PDMS-based silver nanowire/nano-gold/nano-nickel composite electrode.
The surface morphology graph of the silver nanowire/nano gold/nano nickel composite electrode based on PDMS is shown in figure 1, the size and the distribution of nano particle particles on the electrode are uniform, and the electrocatalytic performance is particularly outstanding.
Application example 1
The three-electrode system is formed by taking the PDMS-based silver nanowire/nano gold/nano nickel composite electrode prepared in the embodiment 1 as a working electrode, taking an Ag/AgCl electrode as a reference electrode and taking a platinum wire as a counter electrode, and putting the three-electrode system in a lactose solution taking a potassium hydroxide solution as an electrolyte to be combined as a fuel to form the lactose fuel cell.
Further, the electrolyte was 1mol/LKOH, and the pH was 14.
The anode and the cathode of the constructed PDMS-based silver nanowire/nano gold/nano nickel composite electrode are connected through a lead, lactose is spontaneously reacted in lactose solution to realize conversion from biomass energy to electric energy, electrons generated by the anode are transferred to the cathode through the lead, and oxygen is reduced to hydroxyl ions to realize storage of electric energy.
Experimental study comparative application case 1
Comparison of cyclic voltammetry curves for lactose solutions and blank solutions
The three-electrode system was used as the three-electrode system in application example 1.
Firstly, placing a three-electrode system into a KOH solution with the pH value of 14 and the concentration of 1mol/L, scanning in a potential range of-0.2-1.3V by using cyclic voltammetry, and recording the cyclic voltammetry curve of a blank solution; then, the three-electrode system was placed in a lactose test solution containing 1mol/L KOH solution at pH 14 as a supporting electrolyte at 10mmol/L and scanned by cyclic voltammetry in a potential range of-0.2 to 1.3V, and the cyclic voltammetry of lactose was recorded. As shown in fig. 2: the catalytic effect of PDMS-based silver nanowires/gold/nickel nanowires composite electrodes was tested at a scan rate of 100mV/s at 10mmol/L lactose. From fig. 2, it can be seen that the PDMS-based silver nanowire/nanogold/nano nickel composite electrode has good catalytic activity to lactose. The lactose fuel cell composed of the silver nanowire/nano gold/nano nickel composite electrode based on PDMS can be used for converting bioenergy into electric energy efficiently.
Experimental study comparative application case 2
Cyclic voltammetric response of PDMS-based silver nanowires/gold/nickel nanowires composite electrodes to lactose of the same concentration at different sweep rates
The three-electrode system was used as the three-electrode system in application example 1.
Sequentially placing the three-electrode system into a lactose solution to be tested of 10mm, which contains KOH solution with the pH of 14 and 1mol/L as supporting electrolyte, and testing lactose solutions with different scanning speeds at the same concentration, wherein the scanning speeds are respectively 20m V/s, 40m V/s, 60m V/s, 80mV/s and 100m V/s, and scanning in a potential range of-0.2-1.3V by using a cyclic voltammetry. Cyclic voltammograms of lactose at different sweep rates for the same concentration were recorded. As shown in fig. 3 and 4: as can be seen from fig. 3 and fig. 4, as the sweeping speed increases, the oxidation current of the silver nanowire/nano gold/nano nickel composite electrode based on PDMS in lactose solution increases, the oxidation peak increases, and the linear response of lactose is well catalyzed, so that it can be proved that the silver nanowire/nano gold/nano nickel composite electrode based on PDMS catalyzes lactose to be diffusion control.
Experimental study comparative application case 3
Silver nanowire/nano gold/nano nickel composite electrode anti-poisoning research based on PDMS
The three-electrode system was used as the three-electrode system in application example 1.
First, a three-electrode system was placed in a 10mm lactose test solution containing 1mol/L KOH solution at pH 14 as a supporting electrolyte, and a time-current curve of lactose was recorded at a potential of 0.6V by a time-current method. However, the current density drops sharply at the beginning as shown in fig. 5. At the beginning of the reaction, it is a fast kinetic reaction, so the active site is free of adsorbed lactose molecules. The adsorption of new lactose molecules then depends on the release of the electrocatalytic sites by oxidation of lactose, or the formation of intermediate species such as CO, CHx, etc. in the first few minutes (rate determining step), the electrode catalytic active sites being occupied. Thus, the slight decrease in current density is mainly due to poisoning of the catalyst. Furthermore, the specific current experienced a rapid drop in the first 300 seconds throughout the test and remained a smooth and gentle change after the end of the test, with a decay of about 5%. Therefore, the silver nanowire/nano gold/nano nickel composite electrode based on PDMS has strong antitoxic capability and stable structure.
The above-described embodiments are only preferred embodiments of the invention, and not all embodiments of the invention are possible. Any obvious modifications thereof, which would be apparent to those skilled in the art without departing from the principles and spirit of the present invention, should be considered to be included within the scope of the appended claims.
Claims (3)
1. The preparation method of the PDMS-based silver nanowire/nano gold/nano nickel composite electrode is characterized by comprising the following specific steps:
(1) Manufacturing a PDMS substrate;
manufacturing a PDMS substrate by adopting a photoetching technology; spin-coating photoresist on the clean surface of the silicon wafer, shielding a mask plate containing electrode patterns, and finally exposing and developing to obtain a silicon wafer template; placing a silicon wafer template in a disposable culture dish, and pouring a PDMS mixed solution with the mass ratio of 8-15:1; then putting the mixture into a vacuum dryer to suck bubbles in the PDMS mixed solution under negative pressure, and using the mixture for 2 to 3 hours; taking out, putting into a constant temperature oven at 60-100 ℃ for heating and curing 1h, and cutting into 12 electrode substrates; the prepared electrode substrate is treated by an adhesive tape to remove dust attached to the surface, and then is put into an ultraviolet ozone cleaner to be cleaned for 2min, so as to obtain the PDMS substrate with the fixed-shape groove;
(2) Modification of a hydrophilic layer on the surface of the PDMS substrate; the method comprises the following specific steps:
(a) Preparing a mixed aqueous solution of PVA with the mass percentage of 2-4% and PVP with the mass percentage of 5-7%;
(b) Soaking the prepared PDMS substrate in a mixed solution of PVA and PVP for 20-50min, and then drying in a vacuum oven at 60-80 ℃ for 2-3h;
(c) Repeating step (b) once;
(d) Placing the PDMS substrate into a vacuum oven at 80-100 ℃ for heat fixing for 20-30min;
(e) Repeating the steps (b) and (d) once to obtain a PDMS substrate with a surface hydrophilic layer modified;
(3) Preparation of AgNWs/PDMS Plastic electrode
Mixing absolute ethyl alcohol and water according to the volume ratio of 9:1 as a solvent to prepare a silver nanowire solution with the concentration of 5mg/mL, uniformly spreading the silver nanowire solution in a groove on the surface of a PDMS substrate, and standing and drying at room temperature for more than one day to prepare an AgNWS/PDMS plastic electrode;
(4) Preparing an AuNPs/AgNWs/PDMS electrode by flower-shaped nano gold deposition;
immersing the electrode into the electrode of the AgNWS/PDMS plastic electrode by adopting a three-electrode system of 0.2MH 2 SO 4 And 4mg/m L KAuCl 4 Using a platinum electrode as a counter electrode and Ag/Ag Cl as a reference electrode; setting electro-deposition parameters of an electrochemical workstation by adopting a potential-time curve: setting the current to 0.2A for 1600s, and depositing; the deposited electrode is protected by nitrogen, and is kept for three days for standby; preparing an AuNPs/AgNWs/PDMS electrode;
(5) Preparing a silver nanowire/nano-gold/nano-nickel composite electrode based on PDMS;
adopting a three-electrode system, taking AuNPs/AgNWs/PDMS with a nano structure as a working electrode, taking an Ag/AgCl electrode and a platinum wire electrode as a reference electrode and a counter electrode, and putting the electrodes into an electrolytic cell containing nickel sulfate solution; setting electro-deposition parameters of an electrochemical workstation by adopting a chronopotentiometry: the upper limit voltage is-1V, the holding time is 300s, the lower limit voltage is-0.6V, the holding time is 100s, the electrode is immediately taken out after deposition, the electrode is washed with deionized water for many times, the electrode is protected by nitrogen, and the electrode is kept for three days for standby; and preparing the PDMS-based silver nanowire/nano-gold/nano-nickel composite electrode.
2. The use of a PDMS based silver nanowire/nanogold/nano nickel composite electrode according to claim 1 in the electrocatalytic oxidation of lactose solutions to construct lactose fuel cells.
3. The use of the composite electrode according to claim 2 in lactose fuel cell construction by electrocatalytic oxidation of lactose solution, wherein the three-electrode system is constructed by combining a silver nanowire/nano gold/nano nickel composite electrode based on PDMS as a working electrode, an Ag/AgCl electrode as a reference electrode, and a platinum wire as a counter electrode with lactose solution using potassium hydroxide solution as electrolyte as fuel.
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