CN113013421A - Preparation method and application of PDMS-based silver nanowire/nanogold/nano-nickel composite electrode - Google Patents
Preparation method and application of PDMS-based silver nanowire/nanogold/nano-nickel composite electrode Download PDFInfo
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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/nanogold/nano-nickel composite electrode. Taking Polydimethylsiloxane (PDMS) as a flexible substrate, modifying a hydrophilic surface layer on the flexible substrate by using a mixed solution of polyvinyl alcohol and glycerol, taking 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 PDMS-based silver nanowire/nano gold/nano nickel composite electrode; 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 high 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/nanogold/nano-nickel composite electrode.
Background
Fuel cells, while representative of new energy technologies, are not an emerging concept. The fuel cell directly catalyzes fuel to react with oxygen through a catalyst to convert chemical energy into electric energy, the energy efficiency is as high as 70%, and most of products are water, so that the environmental damage is extremely low. Fuel cells are classified into proton exchange membrane fuel cells, solid oxide fuel cells, molten carbonate fuel cells, alkaline fuel cells, and the like according to the electrolyte classification.
Although fuel cells have great advantages in some aspects, there are many problems in terms of life span, stability, etc., and it is a hot research problem to improve the life span and stability of fuel cells.
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/nanogold/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 fuel cells.
The above purpose of the invention is realized by the following technical scheme:
a preparation method of a PDMS-based silver nanowire/nanogold/nano-nickel composite electrode (NiNPs/AuNPs/AgNWs/PDMS electrode); taking Polydimethylsiloxane (PDMS) as a flexible substrate, modifying a hydrophilic surface layer on the flexible substrate by using a mixed solution of polyvinyl alcohol and glycerol, taking 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 PDMS-based silver nanowire/nano gold/nano nickel composite electrode; 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/nanogold/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 surface of a clean silicon wafer, shielding a mask plate containing an electrode pattern, and finally carrying out exposure and development to obtain a silicon wafer template; placing the silicon wafer template in a disposable culture dish, and pouring PDMS mixed solution with the mass ratio of 8-15: 1; then putting the mixture into a vacuum drier to pump out air bubbles in the PDMS mixed solution under negative pressure for 2-3 h; taking out, placing into a constant temperature oven at 60-100 deg.C, heating and curing for 1h, and cutting into 12 electrode substrates; treating the prepared electrode substrate with an adhesive tape (purchased from 3M company in America) to remove dust attached to the surface, and then putting the electrode substrate into an ultraviolet ozone cleaning machine to clean for 2-30min to obtain a PDMS substrate with a groove in a fixed shape;
(2) modifying the 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% of PVA and 5-7% of PVP in percentage by mass; preferably preparing a mixed aqueous solution of 4% of PVA and 7% of PVP in percentage by mass;
(b) soaking the prepared PDMS substrate in a mixed solution of PVA and PVP for 20-50min, and drying in a vacuum oven at 60-80 deg.C for 2 h; preferably, the prepared PDMS substrate is soaked in the mixed solution of PVA and PVP for 20min and then is dried in a vacuum oven at the temperature of 60-80 ℃ for 2 h;
(c) repeating step (b) once;
(d) placing the PDMS substrate into a vacuum oven with the temperature of 80-100 ℃ for thermal fixation for 20-30 min;
(e) repeating the steps (b) and (d) once to obtain the PDMS substrate modified by the surface hydrophilic layer;
(3) preparing AgNWs/PDMS plastic electrode
Mixing absolute ethyl alcohol and water according to the volume ratio of 9:1 to be used as a solvent, preparing 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 placing and drying the silver nanowire solution at room temperature for more than one day to prepare the AgNWs/PDMS plastic electrode;
(4) depositing flower-shaped nanogold to prepare an AuNPs/AgNWs/PDMS electrode;
using a three-electrode system, immersing 0.2M H AgNWs/PDMS plastic electrode2SO4And 4mg/m L KAuCl4In the mixture (2), a platinum electrode was used as a counter electrode and Ag/Ag Cl as a reference electrode. Setting the electrodeposition parameters of the electrochemical workstation by adopting a potential-time curve: setting the current at 0.2A for 1600s, and depositing. The deposited electrode is protected by nitrogen and is placed for standby after three days; preparing an AuNPs/AgNWs/PDMS electrode;
(5) preparing a PDMS-based silver nanowire/nanogold/nano-nickel composite electrode;
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 reference electrodes and a counter electrode, and putting the reference electrodes and the counter electrode into an electrolytic cell containing nickel sulfate solution; setting electrodeposition parameters of an electrochemical workstation by adopting a chronopotentiometry method: the upper limit voltage is minus 1V, the holding time is 300s, the lower limit voltage is minus 0.6V, the holding time is 100s, after deposition, the electrode is immediately taken out, is washed by deionized water for multiple times, is protected by nitrogen, and is placed for standby after three days; and preparing the PDMS-based silver nanowire/nano gold/nano nickel composite electrode.
Further, the step (1) of preparing the PDMS substrate is preferably: manufacturing a PDMS substrate by adopting a photoetching technology; spin-coating photoresist on the surface of a clean silicon wafer, shielding a mask plate containing an electrode pattern, and finally carrying out exposure and development 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 drier to pump out bubbles in the PDMS mixed solution under negative pressure, and taking 2 hours; taking out, placing into a constant-temperature oven at 80 ℃, heating and curing for 1h, and cutting into 12 electrode substrates; and (3) treating the prepared electrode substrate by using an adhesive tape (purchased from 3M company in America) to remove dust attached to the surface, and then putting the electrode substrate into an ultraviolet ozone cleaning machine to clean for 2min to obtain the PDMS substrate with the groove in a fixed shape.
The silver nanowire/nanogold/nano-nickel composite electrode (NiNPs/AuNPs/AgNWs/PDMS electrode) based on PDMS is applied to the construction of a lactose fuel cell by electrocatalytic oxidation of lactose solution. The method specifically comprises the following steps:
a three-electrode system is formed by taking a PDMS-based silver nanowire/nano-gold/nano-nickel composite electrode as a working electrode, an Ag/AgCl electrode as a reference electrode and a platinum wire as a counter electrode, and the three-electrode system is placed in a lactose solution taking a potassium hydroxide solution as an electrolyte to be combined into a lactose fuel cell.
Further, the electrolyte is 0.01-1mol/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 nano-wire 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 a base liquid.
The invention provides a method for preparing a PDMS substrate, which comprises the following steps: pouring a PDMS mixed solution with the mass ratio of 8-15: 1; then putting the mixture into a vacuum drier to pump out air bubbles in the PDMS mixed solution under negative pressure for 2-3 h; because the bubbles can not be eliminated in the time shorter than the time, the cost is increased and the efficiency is reduced if the time is too long; taking out, placing in a constant temperature oven at 60-100 deg.C, heating and curing for 1h, wherein the substrate obtained at a temperature below the range is too soft, and the substrate obtained at a temperature above the range is too hard.
The silver nanowire solution with the concentration of 5mg/mL is selected in the technical scheme provided by the invention, and the silver nanowire solution is uniformly spread and has good conductivity.
Drawings
FIG. 1 is a surface topography of a nano-Au/nano-Ni composite electrode based on PDMS silver nanowires.
FIG. 2 is a comparison of cyclic voltammograms of a lactose solution versus a blank solution.
FIG. 3 is a plot of cyclic voltammograms of different sweep rates of lactose solution.
FIG. 4 is a standard graph of lactose at different sweep rates.
Fig. 5 is a graph of the poisoning resistance of the nanogold/nano nickel composite electrode based on the PDMS silver nanowire.
Fig. 6 is a graph of spreading results of silver nanowire solutions of different concentrations. In the figure, the concentration of (a) is 1mg/mL, that of (b) is 3mg/mL, that of (c) is 5mg/mL, that of (d) is 7mg/mL, and that of (e) is 10 mg/mL.
Detailed Description
The invention is described in more detail below with reference to specific examples, without limiting the scope of the invention. Unless otherwise specified, the experimental methods adopted by the invention are all conventional methods, and experimental equipment, materials, reagents and the like used in the experimental method can be obtained from commercial sources.
Example 1
A preparation method of a PDMS-based silver nanowire/nanogold/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 surface of a clean silicon wafer, shielding a mask plate containing an electrode pattern, and finally carrying out exposure and development 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 drier to pump out bubbles in the PDMS mixed solution under negative pressure, and taking 2 hours; taking out, placing into a constant-temperature oven at 80 ℃, heating and curing for 1h, and cutting into 12 electrode substrates; treating the prepared electrode substrate with an adhesive tape (purchased from 3M company in America) to remove dust attached to the surface, and then putting the electrode substrate into an ultraviolet ozone cleaning machine to clean for 2min to obtain a PDMS substrate with a groove in a fixed shape;
(2) modifying the hydrophilic layer on the surface of the PDMS substrate; the method comprises the following specific steps:
(a) preparing a mixed aqueous solution of 4% of PVA and 7% of PVP in percentage by mass;
(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 2 h;
(c) repeating step (b) once;
(d) placing the PDMS substrate into a vacuum oven at 100 ℃ for thermal fixation of 20 min;
(e) repeating the steps (b) and (d) once to obtain the PDMS substrate modified by the surface hydrophilic layer;
(3) preparing AgNWs/PDMS plastic electrode
Mixing absolute ethyl alcohol and water according to the volume ratio of 9:1 to be used as a solvent, preparing 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 placing and drying the silver nanowire solution at room temperature for more than one day to prepare the AgNWs/PDMS plastic electrode;
(4) depositing flower-shaped nanogold to prepare an AuNPs/AgNWs/PDMS electrode;
using a three electrode system, a mixture of 0.2M H2SO4 and 4mg/m L KAuCl4 was immersed with an AgNWs/PDMS ductile electrode using a platinum electrode as the counter electrode and Ag/Ag Cl as the reference electrode. Setting the electrodeposition parameters of the electrochemical workstation by adopting a potential-time curve: the deposition was carried out with a current of 0.2A and a time of 1600 s. The deposited electrode is protected by nitrogen and is placed for standby after three days; preparing an AuNPs/AgNWs/PDMS electrode;
(5) preparing a PDMS-based silver nanowire/nanogold/nano-nickel composite electrode;
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 reference electrodes and a counter electrode, and putting the reference electrodes and the counter electrode into an electrolytic cell containing nickel sulfate solution; setting electrodeposition parameters of an electrochemical workstation by adopting a chronopotentiometry method: the upper limit voltage is minus 1V, the holding time is 300s, the lower limit voltage is minus 0.6V, the holding time is 100s, after deposition, the electrode is immediately taken out, is washed by deionized water for multiple times, is protected by nitrogen, and is placed for standby after three days; and preparing the PDMS-based silver nanowire/nano gold/nano nickel composite electrode.
The surface topography of the PDMS-based silver nanowire/nanogold/nano-nickel composite electrode is shown in figure 1, wherein the size and distribution of nano-particle on the electrode are uniform, and the electrocatalytic performance is particularly outstanding.
Application example 1
The PDMS-based silver nanowire/nanogold/nano-nickel composite electrode prepared in example 1 was used as a working electrode, an Ag/AgCl electrode was used as a reference electrode, and a platinum wire was used as a counter electrode to form a three-electrode system, which was then placed in a lactose solution using potassium hydroxide solution as an electrolyte to form a lactose fuel cell.
Further, the electrolyte is 1mol/LKOH, and the pH is 14.
The structured PDMS-based silver nanowire/nanogold/nano-nickel composite electrode anode is connected with a cathode through a lead, and is inserted into lactose solution to spontaneously react and oxidize lactose to realize conversion of biomass energy to electric energy, electrons generated by the anode are transferred to the cathode through the lead to reduce oxygen to hydroxyl ions, and the electric energy is stored.
Experimental study comparative application case 1
Comparison of Cyclic voltammograms for lactose solution and blank solution
The three-electrode system in application example 1 was used.
Firstly, placing a three-electrode system in a KOH solution with the pH of 14 and the concentration of 1mol/L, scanning within a potential range of-0.2-1.3V by using a cyclic voltammetry method, and recording a cyclic voltammetry curve of a blank solution; then, the three-electrode system is placed in 10mmol/L lactose solution to be detected containing 1mol/L KOH solution with pH of 14 as supporting electrolyte, and scanning is carried out in a potential range of-0.2-1.3V by using cyclic voltammetry, and the cyclic voltammetry curve of the lactose is recorded. As shown in fig. 2: the catalytic effect of the PDMS-based silver nanowire/nanogold/nano-nickel composite electrode at 10mmol/L lactose was tested at a scanning speed of 100 mV/s. It can be seen from fig. 2 that the PDMS-based silver nanowire/nanogold/nano-nickel composite electrode has good catalytic activity to lactose. The lactose fuel cell composed of the PDMS-based silver nanowire/nano-gold/nano-nickel composite electrode can efficiently convert the biological energy into the electric energy.
Experimental study comparative application case 2
PDMS-based cyclic voltammetric response of silver nanowire/nanogold/nano-nickel composite electrode to lactose with same concentration and different sweeping speeds
The three-electrode system in application example 1 was used.
Sequentially placing the three-electrode system in 10mm lactose solution to be detected containing 1mol/L KOH solution with pH of 14 as supporting electrolyte, testing the 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 were recorded at the same concentration. As shown in fig. 3 and 4: as can be seen from fig. 3 and 4, as the sweep rate is increased continuously, the oxidation current of the PDMS-based silver nanowire/nanogold/nano nickel composite electrode in the lactose solution is increased continuously, the oxidation peak is increased continuously, and a good linear response for catalyzing lactose is presented, so that it can be proved that the PDMS-based silver nanowire/nanogold/nano nickel composite electrode catalyzes lactose to be diffusion control.
Experimental study comparative application case 3
Silver nanowire/nanogold/nano nickel composite electrode anti-poisoning research based on PDMS
The three-electrode system in application example 1 was used.
First, the three-electrode system was placed in a 10mm lactose test solution containing 1mol/L KOH solution with pH 14 as a supporting electrolyte, and the time-current curve of lactose was recorded by the time-current method at a potential of 0.6V. 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 does not contain adsorbed lactose molecules. The adsorption of new lactose molecules then depends on the release of electrocatalytic sites by lactose oxidation, or on the occupation of electrode catalytically active sites by intermediate species such as CO, CHx, etc. formed in the first few minutes (rate determining step). Therefore, the slight decrease in current density is mainly due to the poisoning of the catalyst. Furthermore, the specific current experienced a rapid drop during the first 300 seconds throughout the test and was still a smooth and gentle change after the end of the test, with a decay of about 5%. Therefore, the silver nanowire/nanogold/nano-nickel composite electrode based on PDMS has strong anti-poisoning capacity and a stable structure.
The embodiments described above are merely preferred embodiments of the invention, rather than all possible embodiments of the invention. Any obvious modifications to the above would be obvious to those of ordinary skill in the art, but would not bring the invention so modified beyond the spirit and scope of the present invention.
Claims (4)
1. A preparation method of a PDMS-based silver nanowire/nanogold/nano-nickel composite electrode is characterized in that PDMS is used as a flexible substrate, a polyvinyl alcohol and glycerol mixed solution is used for modifying a hydrophilic surface layer on the flexible substrate, a silver nanowire ethanol solution is used as a conductive layer, nanogold-nickel particles are deposited on the conductive layer by an electrochemical deposition method, and the PDMS-based silver nanowire/nanogold/nano-nickel composite electrode is prepared; the nano nickel particles are deposited on the nano gold particles, and the nano gold particles are deposited on the silver nanowires.
2. The method for preparing a PDMS-based silver nanowire/nanogold/nano-nickel composite electrode according to claim 1, wherein the method comprises the following steps: (1) manufacturing a PDMS substrate;
manufacturing a PDMS substrate by adopting a photoetching technology; spin-coating photoresist on the surface of a clean silicon wafer, shielding a mask plate containing an electrode pattern, and finally carrying out exposure and development to obtain a silicon wafer template; placing the silicon wafer template in a disposable culture dish, and pouring PDMS mixed solution with the mass ratio of 8-15: 1; then putting the mixture into a vacuum drier to pump out air bubbles in the PDMS mixed solution under negative pressure for 2-3 h; taking out, placing into a constant temperature oven at 60-100 deg.C, heating and curing for 1h, and cutting into 12 electrode substrates; treating the prepared electrode substrate with an adhesive tape to remove dust attached to the surface, and then putting the electrode substrate into an ultraviolet ozone cleaning machine to clean for 2min to obtain a PDMS substrate with a groove in a fixed shape;
(2) modifying the 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% of PVA and 5-7% of PVP in percentage by mass;
(b) soaking the prepared PDMS substrate in a mixed solution of PVA and PVP for 20-50min, and drying in a vacuum oven at 60-80 deg.C for 2-3 h;
(c) repeating step (b) once;
(d) placing the PDMS substrate into a vacuum oven with the temperature of 80-100 ℃ for thermal fixation for 20-30 min;
(e) repeating the steps (b) and (d) once to obtain the PDMS substrate modified by the surface hydrophilic layer;
(3) preparing AgNWs/PDMS plastic electrode
Mixing absolute ethyl alcohol and water according to the volume ratio of 9:1 to be used as a solvent, preparing 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 placing and drying the silver nanowire solution at room temperature for more than one day to prepare the AgNWs/PDMS plastic electrode;
(4) depositing flower-shaped nanogold to prepare an AuNPs/AgNWs/PDMS electrode;
using a three-electrode system, immersing 0.2M H AgNWs/PDMS plastic electrode2SO4And 4mg/m L KAuCl4In the mixture (2), a platinum electrode was used as a counter electrode and Ag/Ag Cl as a reference electrode. Setting the electrodeposition parameters of the electrochemical workstation by adopting a potential-time curve: the deposition was carried out with a current of 0.2A and a time of 1600 s. The deposited electrode is protected by nitrogen and is placed for standby after three days; preparing an AuNPs/AgNWs/PDMS electrode;
(5) preparing a PDMS-based silver nanowire/nanogold/nano-nickel composite electrode;
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 reference electrodes and a counter electrode, and putting the reference electrodes and the counter electrode into an electrolytic cell containing nickel sulfate solution; setting electrodeposition parameters of an electrochemical workstation by adopting a chronopotentiometry method: the upper limit voltage is minus 1V, the holding time is 300s, the lower limit voltage is minus 0.6V, the holding time is 100s, after deposition, the electrode is immediately taken out, is washed by deionized water for multiple times, is protected by nitrogen, and is placed for standby after three days; and preparing the PDMS-based silver nanowire/nano gold/nano nickel composite electrode.
3. The use of a PDMS based silver nanowire/nanogold/nanonickel composite electrode of claim 1 or 2 in the construction of a lactose fuel cell by electrocatalytic oxidation of lactose solution.
4. The application of the composite electrode in the lactose solution electrocatalytic oxidation to construct the lactose fuel cell as claimed in claim 3, wherein the silver nanowire/nanogold/nano nickel composite electrode based on PDMS is used as a working electrode, the Ag/AgCl electrode is used as a reference electrode, the platinum wire is used as a counter electrode to form a three-electrode system, and the three-electrode system is placed in the lactose solution using potassium hydroxide solution as electrolyte to form the lactose fuel cell.
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| CN113937244A (en) * | 2021-08-30 | 2022-01-14 | 福州大学 | Method for preparing micron LED by transfer printing patterned electrode |
| CN113937244B (en) * | 2021-08-30 | 2023-08-04 | 福州大学 | Method for preparing micron LED by transferring patterned electrode |
| CN114583188A (en) * | 2022-03-04 | 2022-06-03 | 大连大学 | Method for constructing neutral glucose fuel cell electrode |
| CN114583183A (en) * | 2022-03-04 | 2022-06-03 | 大连大学 | Acidic glucose fuel cell electrode and preparation method thereof |
| CN114597364A (en) * | 2022-03-11 | 2022-06-07 | 西安电子科技大学 | Preparation method of polydimethylsiloxane and silver nanowire porous composite flexible lithium metal battery |
| CN114597364B (en) * | 2022-03-11 | 2024-01-16 | 西安电子科技大学 | Preparation method of polydimethylsiloxane and silver nanowire porous composite flexible lithium metal battery |
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