CN114230378B - Preparation method of redox-driven super-assembly intelligent door control system - Google Patents
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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, adding an oxidizing agent and a reducing agent (hydrogen peroxide and ascorbic acid) with certain concentrations into the electrolyte, and performing 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 gating system.
Background
Redox reactions play 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 is due toThe ion source 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) 2 O 2 ) 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;
and 2, step: 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 H 2 O 2 Current of pre-Fc-MS/AAO;
and step 3: adding oxidant H into KCl solution in conductivity cell 2 O 2 Measuring 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 H 2 O 2 Effect of concentration and pH on gating 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 using the Anodic Aluminum Oxide (AAO) as a substrate through spin coating of a precursor solution and subsequent methods of interface super-assembly and evaporation-induced self-assembly to prepare an MS/AAO heterogeneous nanochannel;
step 1-2: soaking the MS/AAO heterojunction nano-channel in an excessive 5-10wt% 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 NH 2 -MS/AAO；
Step 1-3: reacting NH 2 -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 -6 The mol/L potassium chloride solution, the catholyte in the cathode pool is 0.1 to 10 -6 And 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 H 2 O 2 In a concentration of 0.1-10 -6 mol/L。
Further, in the step 4, the electrolyte KCl solution is 0.1-10 -6 mol/L, the concentration of the reducing agent AA is 0.1-10 -6 mol/L。
Further, in step 5, the method for exploring gated reversible cyclicity specifically comprises: repeating the step 3 and the step 4 to obtain different current curves; the exploration H 2 O 2 Specific methods of the effect of concentration and pH on gating properties include: multiple portions of H with different concentrations are prepared 2 O 2 And 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 serving as 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 and control of ions in a nano channel are realized, and the reversible change of 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 H 2 O 2 A 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 plot 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 an 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 H 2 O 2 Current 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 -6 The mol/L potassium chloride solution, the catholyte in the cathode pool is 0.1-10 - 6 A potassium chloride solution of mol/L; the anode electrode and the cathode electrode are Ag/AgCl electrodes; the test voltage is-1.6V to 1.6V;
and 3, step 3: 0.1-10 in the conductance cell -6 Adding 0.1-10 mol/LKCl solution -6 mol/L oxidant H 2 O 2 Measuring the current of Fc-MS/AAO after adding the oxidant;
and 4, step 4: 0.1-10 in the conductivity cell -6 Adding 0.1-10 mol/LKCl solution -6 mol/L reducing agent AA, and measuring the current of Fc-MS/AAO after adding the reducing agent AA;
and 5: exploration of gated reversible cyclicity, exploration of H 2 O 2 Effect of concentration and pH on gating properties.
The method for exploring gated reversible cyclicity comprises the following steps: repeating the steps 3 and 4 to obtainTo different current profiles; study H 2 O 2 Methods of influencing the gating properties by concentration and pH include: multiple portions of H with different concentrations are prepared 2 O 2 And KCl solutions with different pH values are used as electrolyte, and the corresponding current curve is obtained by adopting the method from the step 2 to the 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 -3 M 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 10 4 μm 2 Thickness of about 60 μm, and the addition of the oxidizing agent H was measured 2 O 2 Current of pre-Fc-MS/AAO;
3) The arrangement comprises 10 -3 MH 2 O 2 The 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 -3 The 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 (5) 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 H 2 O 2 Concentration: configuring H with different concentrations 2 O 2 The current is detected, as can be seen in FIG. 4, along with H 2 O 2 The 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 were prepared, and FIG. 5 shows that pH has little effect on Fc-MS/AAO currentHowever, pH affected the gating effect, as shown in the figure, hydrogen peroxide was the most effective in regulating Fc-MS/AAO ionic current at pH 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 ferrocenyl 2+ 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 acid 3+ 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 (4)
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, making the Fc-MS layer face the anode side, filling an electrolyte KCl solution in a conductivity cell, and measuring the addition of an oxidant H 2 O 2 Current of pre-Fc-MS/AAO;
and 3, step 3: adding oxidant H into KCl solution in conductivity cell 2 O 2 Measuring 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: h 2 O 2 The concentration is selected from one of 0.1 muM, 0.5 muM, 1 muM, 5 muM, 0.1mM and 1mM, and the pH is selected from one of 4,7 and 10, so as to obtain the optimal gate control reversible cyclicity;
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 an excessive 5-10wt% 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 NH 2 -MS/AAO；
Step 1-3: reacting NH 2 -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, an 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;
in step 3, the oxidant H 2 O 2 In a concentration of 0.1-10 -6 mol/L；
In step 4, the electrolyte KCl is dissolvedThe liquid is 0.1-10 -6 mol/L, the concentration of the reducing agent AA is 0.1-10 -6 mol/L。
2. 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.
3. The method of claim 2, wherein the anolyte in the anode tank is 0.1-10 -6 The mol/L potassium chloride solution, the catholyte in the cathode pool is 0.1-10 -6 And 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.
4. The method for preparing a redox-driven super-assembled intelligent gating system according to claim 3, 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 H 2 O 2 Specific methods of the effect of concentration and pH on gating properties include: preparing multiple portions of H with different concentrations 2 O 2 And 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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