CN114230378A - Preparation method of redox-driven super-assembly intelligent door control system - Google Patents
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
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Abstract
The invention provides a preparation method of a redox-driven super-assembly intelligent door control system, which comprises the following steps: preparing and obtaining the Fc-MS/AAO heterojunction nanochannel based on a super-assembly and two-step modification method; and (3) building an electrochemical testing device, and adding an oxidizing agent and a reducing agent (hydrogen peroxide and ascorbic acid) with certain concentrations into the electrolyte to perform electrochemical testing. Compared with other gating methods, the ferrocene-modified mesoporous silica/anodic alumina heterojunction nano-channel prepared by the super-assembly method has the advantages of short time consumption, simple reaction process and the like, and has better reference value for the application of the intelligent nano-fluidic nano-channel device in the field of ion gating.
Description
Technical Field
The invention belongs to the technical field of nano ion channels, and particularly relates to a preparation method of a redox-driven super-assembly intelligent gate control system.
Background
Oxidation reduction reactionPlays a key messenger role in biological systems. Redox reactions also control biological processes such as cellular respiration and biological energy storage. In recent years, the bionic artificial nano ion channel has controllable ion transport performance, and is widely applied to the technical fields of sensing, gating, desalting, energy conversion and the like. Therefore, based on the redox reaction characteristics, hydrogen peroxide (H)2O2) Ion channels as triggers have great potential in the construction of biosensors, biological information transmitting receptors or devices. However, few studies of nanochannels based on redox-controlled ion transport are currently available. Therefore, the construction of an intelligent gating platform based on redox driving has important significance, and a new strategy is provided for the construction of a sensing and drug release platform.
Disclosure of Invention
The invention aims to solve the technical problems and provide a preparation method of a redox-driven super-assembly intelligent door control system.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a redox-driven super-assembly intelligent door control system comprises the following steps:
step 1: preparing and obtaining the Fc-MS/AAO heterojunction nanochannel based on a super-assembly and two-step modification method;
step 2: placing Fc-MS/AAO in a connecting channel between an anode pool and a cathode pool of an electrochemical testing device, enabling the Fc-MS layer to face to the anode side, filling an electrolyte KCl solution in a conductivity cell, and measuring the addition of an oxidant H2O2Current of pre-Fc-MS/AAO;
and step 3: adding oxidant H into KCl solution in conductivity cell2O2Measuring the current of Fc-MS/AAO after adding the oxidant;
and 4, step 4: adding a reducing agent AA into a KCl solution in a conductivity cell, and measuring the current of Fc-MS/AAO after adding the reducing agent AA;
and 5: exploration of gated reversible cyclicity, exploration of H2O2Concentration and pH vs. gatingThe influence of the properties.
Further, step 1 specifically includes the following steps:
step 1-1: constructing an ultrathin mesoporous silicon oxide layer on the surface of the anodic aluminum oxide by taking the Anodic Aluminum Oxide (AAO) as a substrate and adopting methods of spin coating of a precursor solution, subsequent interfacial super-assembly and evaporation-induced self-assembly to prepare an MS/AAO heterogeneous nano channel;
step 1-2: soaking the MS/AAO heterojunction nano-channel in 5-10 wt% of excessive 3-aminopropyltriethoxysilane solution for 12-14h at 40-50 ℃, taking out and washing, and performing heat treatment at 100-120 ℃ for 1-2h to obtain an amination-modified MS/AAO heterojunction nano-channel marked as NH2-MS/AAO；
Step 1-3: reacting NH2-MS/AAO is put into an excessive amount of 20-80mg/mL ferrocene formaldehyde ethanol solution, dipped for 5-7h at 30-70 ℃, washed by ethanol and isopropanol, the iso-channel is dipped into an excessive amount of 0.05-0.2mM sodium borohydride methanol solution for 0.5-2h, taken out and washed.
Further, in step 2, the electrochemical testing device includes an anode cell and a cathode cell which are arranged in parallel, a connecting channel for communicating the anode cell with the cathode cell, an anode electrode arranged in the anode cell, a cathode electrode arranged in the cathode cell, and a power supply and a picoammeter arranged between the anode electrode and the cathode electrode.
Further, the anolyte in the anode pool is 0.1-10-6The mol/L potassium chloride solution, the catholyte in the cathode pool is 0.1-10-6And in the mol/L potassium chloride solution, the anode electrode and the cathode electrode are Ag/AgCl electrodes, and the test voltage is-1.6V to 1.6V.
Further, in step 3, the oxidant H2O2In a concentration of 0.1-10-6mol/L。
Further, in the step 4, the electrolyte KCl solution is 0.1-10-6mol/L, the concentration of the reducing agent AA is 0.1-10-6mol/L。
Further, in step 5, the method for exploring gated reversible cyclicity specifically comprises: repeating step 3 and stepStep 4, obtaining different current curves; the exploration H2O2Specific methods of the effect of concentration and pH on gating properties include: multiple portions of H with different concentrations are prepared2O2And KCl solutions with different pH values are used as electrolyte, and corresponding current curves are obtained by adopting the methods of the step 2 and the step 3.
Changes in surface charge density and wettability are major factors affecting changes in ionic current. In the invention, ferrocene which is a redox active bistable molecule has different hydrophilicity and hydrophobicity and charge density in a redox state, and the two states can be reversibly switched in the presence of an oxidant and a reducing agent, so that reversible change of current is caused, and further, the transmission regulation of ions in a nano channel is realized, and the reversible change of the current is caused.
Compared with the prior art, the invention has the following beneficial effects:
the ferrocene-modified mesoporous silica/anodic alumina heterojunction nanochannel is prepared by a super-assembly method, the hydrophilicity and hydrophobicity and the charge density of an ion selective layer, namely an Fc-MS layer, of the system can be reversibly changed after redox of an oxidant and a reducing agent, and the reversible change of a current signal in the nanochannel is accompanied.
Drawings
FIG. 1 is a diagram of the gating mechanism of Fc-MS/AAO;
FIG. 2 is a schematic structural view of an electrochemical test device;
FIG. 3 is a graph of the reversible cyclicity of redox-driven gating in the examples;
FIG. 4 shows example H2O2A plot of the effect of concentration;
FIG. 5 is a graph showing the influence of the pH of the electrolyte in the examples;
FIG. 6 is a Zeta potential diagram of heterojunction nanochannels before and after redox reaction;
FIG. 7 is a contact angle test chart of heterojunction nanochannels before and after redox reaction;
the labels in the figure are: 1-anode pool, 2-cathode pool, 3-anode electrode, 4-cathode electrode, 5-power supply and 6-picoammeter.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
FIG. 1 is a diagram of the gating mechanism of Fc-MS/AAO.
A preparation method of a super-assembly intelligent gating platform for redox driving comprises the following steps:
step 1: preparing and obtaining the Fc-MS/AAO heterojunction nanochannel based on a super-assembly and two-step modification method;
step 2: placing Fc-MS/AAO in a connecting channel between an anode pool and a cathode pool of an electrochemical testing device, enabling the Fc-MS layer to face to the anode side, filling an electrolyte KCl solution in a conductivity cell, and measuring the addition of an oxidant H2O2Current of pre-Fc-MS/AAO;
the electrochemical testing device is shown in fig. 2 and comprises an anode pool 1 and a cathode pool 2 which are arranged in parallel, a connecting channel for communicating the anode pool 1 with the cathode pool 2, an anode electrode 3 arranged in the anode pool 1, a cathode electrode 4 arranged in the cathode pool 2, a power supply 5 and a picoammeter 6 which are arranged between the anode electrode 3 and the cathode electrode 4;
the anolyte in the anode pool is 0.1-10-6The mol/L potassium chloride solution and the catholyte in the cathode pool are 0.1 to 10- 6A potassium chloride solution of mol/L; the anode electrode and the cathode electrode are both Ag/AgCl electrodes; the test voltage is-1.6V to 1.6V;
and step 3: 0.1-10 in the conductance cell-6Adding 0.1-10 mol/LKCl solution-6mol/L oxidant H2O2Measuring the current of Fc-MS/AAO after adding the oxidant;
and 4, step 4: 0.1-10 in the conductance cell-6Adding 0.1-10 mol/LKCl solution-6mol/L reducing agent AA, and measuring the current of Fc-MS/AAO after adding the reducing agent AA;
and 5: exploring reversible cyclicity of gatingStudy H2O2Effect of concentration and pH on gating properties.
The method for exploring the gated reversible cyclicity comprises the following steps: repeating the step 3 and the step 4 to obtain different current curves; study H2O2Methods of influencing the gating properties by concentration and pH include: multiple portions of H with different concentrations are prepared2O2And KCl solutions with different pH values are used as electrolyte, and corresponding current curves are obtained by adopting the method of the same step 2-step 3.
The following is a specific application example:
an ion-gated application method for the preparation of Fc-MS/AAO comprising the steps of:
1) preparing and obtaining the Fc-MS/AAO heterojunction nanochannel based on a super-assembly and two-step modification method;
2) formulation 10-3M potassium chloride solution is respectively used as anolyte and catholyte, and electrochemical performance test (recording current value under voltage of-1.6V) is carried out by adopting an electrochemical test device (shown in figure 2, comprising a picometer and a pair of Ag/AgCl electrodes, and the details of the rest devices are the same) in CN202010640001.8, wherein Fc-MS/AAO is arranged at a connecting channel between an anode pool 1 and a cathode pool 2, the Fc-MS layer faces to one side of the anode, and the effective ion transport area is about 3 multiplied by 104μm2Thickness of about 60 μm, and the addition of the oxidizing agent H was measured2O2Current of pre-Fc-MS/AAO;
3) the arrangement comprises 10-3MH2O2The potassium chloride solution of (2) was added to the conductivity cell in step 1, and the current was measured, whereby it was found that the current was decreased.
4) The arrangement comprises 10-3The MAA potassium chloride solution was added to the conductivity cell in step 1, and the current was measured, indicating an increase in current.
5) And (4) exploring the gated reversible cyclicity, and repeating the steps 3 and 4 to obtain different current curves. As seen from FIG. 3, Fc-MS/AAO has good reversible cyclicity for regulating ion transport based on redox reaction. Study H2O2Concentration: configuring H with different concentrations2O2The current is detected, as can be seen in FIG. 4, along with H2O2The more the concentration increases, the more the current decreases. The effect of electrolyte pH on gating properties was explored: electrolyte solutions with pH values of 4, 7 and 10 are prepared, and as shown in figure 5, the pH value has little influence on the current of Fc-MS/AAO, but the pH value has influence on the gating effect, and as shown in the figure, the hydrogen peroxide has the best regulation effect on the current of Fc-MS/AAO ions at pH value of 7.
Further, as shown in FIG. 6, which is a Zeta potential diagram of the heterojunction nanochannel before and after oxidation-reduction, it can be seen from the diagram that the Zeta potential in the channel after oxidation by hydrogen peroxide was changed from-0.70 mV to +0.66mV, and the Zeta potential in the channel after reduction by ascorbic acid was changed to-0.73 mV.
As shown in fig. 7, which is a contact angle test chart of the heterojunction nanochannel before and after oxidation-reduction, it can be seen that the contact angle of the channel after oxidation by hydrogen peroxide is decreased from 89.12 ± 1.67 ° to 45.4 ± 0.47 °, and when ferrocenyl on the nanochannel is reduced, the contact angle is increased to 69.82 ± 1.42 °. It can be seen that changes in surface charge density and wettability are the main factors affecting changes in ionic current. The phenomenon of reduced current in Fc-MS/AAO may be due to Fe in ferrocenyl2+Oxidation, leading to hydrophilic channels, reduced charge density, modulated ion transport behavior, leading to lower ion currents since charge density dominates the current variations. And Fe after the reduction of the channel by ascorbic acid3+Is reduced, the channel becomes hydrophobic and the charge density increases, resulting in a recovery of the current.
In conclusion, the Fc-MS/AAO prepared by the embodiment of the invention can realize redox reaction driven ion gating.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (7)
1. A preparation method of a redox-driven super-assembly intelligent door control system is characterized by comprising the following steps:
step 1: preparing and obtaining the Fc-MS/AAO heterojunction nanochannel based on a super-assembly and two-step modification method;
step 2: placing Fc-MS/AAO in a connecting channel between an anode pool and a cathode pool of an electrochemical testing device, enabling the Fc-MS layer to face to the anode side, filling an electrolyte KCl solution in a conductivity cell, and measuring the addition of an oxidant H2O2Current of pre-Fc-MS/AAO;
and step 3: adding oxidant H into KCl solution in conductivity cell2O2Measuring the current of Fc-MS/AAO after adding the oxidant;
and 4, step 4: adding a reducing agent AA into a KCl solution in a conductivity cell, and measuring the current of Fc-MS/AAO after adding the reducing agent AA;
and 5: exploration of gated reversible cyclicity, exploration of H2O2Effect of concentration and pH on gating properties.
2. The method for preparing a redox-driven super-assembled intelligent gating system according to claim 1, wherein the step 1 specifically comprises the following steps:
step 1-1: constructing an ultrathin mesoporous silicon oxide layer on the surface of the anodic aluminum oxide by taking the Anodic Aluminum Oxide (AAO) as a substrate and adopting methods of spin coating of a precursor solution, subsequent interfacial super-assembly and evaporation-induced self-assembly to prepare an MS/AAO heterogeneous nano channel;
step 1-2: soaking the MS/AAO heterojunction nano-channel in 5-10 wt% of excessive 3-aminopropyltriethoxysilane solution for 12-14h at 40-50 ℃, taking out and washing, and performing heat treatment at 100-120 ℃ for 1-2h to obtain an amination-modified MS/AAO heterojunction nano-channel marked as NH2-MS/AAO；
Step 1-3: reacting NH2-MS/AAO is put into an excessive amount of 20-80mg/mL ferrocene formaldehyde ethanol solution, dipped for 5-7h at 30-70 ℃, washed by ethanol and isopropanol, and then the isopropanol is addedThe channel is immersed in an excess of 0.05-0.2mM sodium borohydride in methanol for 0.5-2h, removed and washed.
3. The method for preparing a redox-driven super-assembled intelligent gate control system according to claim 1, wherein in the step 2, the electrochemical testing device comprises an anode pool and a cathode pool which are arranged in parallel, a connecting channel for communicating the anode pool and the cathode pool, an anode electrode arranged in the anode pool, a cathode electrode arranged in the cathode pool, and a power supply and a picoammeter which are arranged between the anode electrode and the cathode electrode.
4. The method of claim 3, wherein the anolyte in the anode tank is 0.1-10-6The mol/L potassium chloride solution, the catholyte in the cathode pool is 0.1-10-6And in the mol/L potassium chloride solution, the anode electrode and the cathode electrode are Ag/AgCl electrodes, and the test voltage is-1.6V to 1.6V.
5. The method for preparing a redox-driven super-assembled intelligent gating system according to claim 4, wherein in the step 3, the oxidant H is2O2In a concentration of 0.1-10-6mol/L。
6. The method for preparing a redox-driven super-assembled intelligent door control system according to claim 4, wherein in the step 4, the electrolyte KCl solution is 0.1-10-6mol/L, the concentration of the reducing agent AA is 0.1-10- 6mol/L。
7. The method for preparing a redox-driven super-assembled intelligent gating system according to claim 4, wherein in the step 5, the method for exploring reversible cyclicity of gating specifically comprises: repeating the step 3 and the step 4 to obtain different current curves;
the exploration H2O2Specific methods of the effect of concentration and pH on gating properties include: multiple portions of H with different concentrations are prepared2O2And KCl solutions with different pH values are used as electrolyte, and corresponding current curves are obtained by adopting the methods of the step 2 and the step 3.
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| 方俊雄等: "β-FeOOH/U-g-C_3N_4异质结的制备及光电催化析氢性能", 《武汉工程大学学报》 * |
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