CN109270148B - Anti-interference electrochemical transistor sensor and anti-interference method and application thereof - Google Patents

Anti-interference electrochemical transistor sensor and anti-interference method and application thereof Download PDF

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CN109270148B
CN109270148B CN201811209485.XA CN201811209485A CN109270148B CN 109270148 B CN109270148 B CN 109270148B CN 201811209485 A CN201811209485 A CN 201811209485A CN 109270148 B CN109270148 B CN 109270148B
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interference
electrochemical transistor
transistor sensor
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protective layer
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常钢
周扬
何云斌
何汉平
蔡志伟
马明宇
陶甜
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Hubei University
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Abstract

The invention relates to a method for improving the anti-interference performance of an electrochemical transistor sensor, wherein the electrochemical transistor sensor comprises a source electrode, a drain electrode and a grid electrode, and a channel of the electrochemical transistor sensor is arranged between the source electrode and the drain electrode. The optimization method of the electrochemical transistor sensor has the characteristic of shielding the response of the interfering substances while not influencing the response of the device to the substance to be measured.

Description

Anti-interference electrochemical transistor sensor and anti-interference method and application thereof
Technical Field
The invention relates to a method for improving the anti-interference performance of an electrochemical transistor sensor, belonging to the field of electrochemistry.
Background
In recent years, electrochemical transistor sensors, as a new electrochemical detection method, are considered to be a promising electrical analysis and detection method due to their inherent amplification characteristics and high sensitivity, while organic electrochemical transistors can be used in aqueous solutions with very stable performance and low operating voltage. Therefore, the organic electrochemical transistor has a wide application prospect in low-cost and high-sensitivity biosensors, such as glucose, dopamine, uric acid, ions, ascorbic acid, bacteria, cells, proteins and the like. However, poor selectivity and interference rejection of electrochemical transistor sensors have been problematic.
For example, in CN108593747A, "an enzyme-free electrochemical transistor sensor for glucose and a method for detecting glucose" thereof, an electrochemical transistor with graphene as a channel achieves highly sensitive detection of glucose, but the device has less ideal anti-interference performance for other substances in a solution. Therefore, it is very necessary to optimize the device immunity to interference. Considering that most of the interference is caused by the change of channel carrier concentration due to the diffusion of the interfering substance to the vicinity of the channel, and the response of the substance to be detected is mostly caused by the electrochemical reaction on the gate, which is different from the mechanism and position of the response caused by the interference.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for improving the anti-interference performance of an electrochemical transistor sensor, aiming at the above-mentioned shortcomings in the prior art, by shielding the response of the interfering substance by separating the channel from the gate, the response to the interfering substance is greatly reduced, and the response of the device to the object to be detected is not damaged.
The technical scheme adopted by the invention for solving the problems is as follows:
the method for improving the anti-interference performance of the electrochemical transistor sensor comprises a source electrode, a drain electrode and a grid electrode, wherein a channel of the electrochemical transistor sensor is arranged between the source electrode and the drain electrode.
The invention also provides an electrochemical transistor sensor, in particular of interference-resistant performance, comprising a source, a drain and a gate; the electrochemical transistor sensor channel is arranged between the source electrode and the drain electrode, the channel is single-layer graphene which is transferred by a wet method and grows in a physical vapor phase, and the grid electrode is a glassy carbon electrode which is modified by gold and graphene codeposition; the method is characterized in that a Nafion film protective layer and/or a glycan film protective layer is arranged on the channel, or a sand core glass tube with microporous ceramics at the lower end is sleeved outside the grid.
According to the scheme, the detection object of the anti-interference electrochemical transistor sensor is nitrite; the pH of the buffer solution is in the range of 5-8.
According to the scheme, the Nafion film protective layer is formed on the channel by a method of dripping Nafion solution. Wherein the Nafion solution is 0.1-5 wt% in a dosage of 3-50 μ L/3mm2。
According to the scheme, the chitosan film protective layer is formed on the channel by a method of dripping chitosan solution. Wherein the chitosan solution is prepared from 0.1-2% acetic acid solution with concentration of 50mg/mL and dosage of 3-20 μ L/mm2。
According to the determination of the anti-interference performance when the electrochemical transistor sensor detects nitrite, when a Nafion film protective layer and/or a glycan film protective layer is/are arranged on a channel, the electrochemical transistor sensor with the anti-interference performance is immersed into a buffer solution, a time current curve of the electrochemical transistor sensor is detected by using a digital source meter, a substance to be detected and an interference substance with the same concentration are respectively dripped at different time points, the magnitude of channel current changes accordingly, compared with a device which is not subjected to similar anti-interference treatment, if the current response value of the substance to be detected is obvious, the current response value of the interference substance is obviously reduced, and therefore the anti-interference performance of the device is determined to be improved; when a sand core glass tube with microporous ceramics at the lower end is sleeved outside the grid, a buffer solution containing a substance to be detected or an interference substance is respectively and directly dripped into the sand core glass tube of the anti-interference electrochemical transistor sensor at different time points, a time current curve of the transistor is detected by using a digital source meter, and the anti-interference performance of the device is also determined to be greatly improved by comparing current change values.
According to the scheme, the determination of the anti-interference performance and the V of the time current curveDS＝0.003-0.1V，VG＝0.6-1V。
According to the scheme, the anti-interference performance is determined, and the concentration ranges of the substance to be detected and the interfering substance in the buffer solution are both 10-1 mM.
According to the scheme, the determination of the anti-interference performance is carried out, and the interference substances are mainly common K+,Ca2+,Mg2+,NH4 +,Cl-,NO3-,SO4 2-,PO4 3-,CH3COO-And glucose solutions, and the like.
On the basis, the electrochemical transistor sensor with the anti-interference performance can be applied to the aspect of detecting nitrite waiting for detection substances. When the anti-interference electrochemical transistor sensor is provided with a Nafion film protective layer and/or a glycan film protective layer on a channel, immersing the anti-interference electrochemical transistor sensor into a buffer solution, dropwise adding nitrite standard solutions with different concentrations, detecting a time current curve of the electrochemical transistor sensor by using a digital source meter, drawing a standard curve through the change value of the current and the concentration of the nitrite standard solution, and further determining the content of nitrite in a sample to be detected; or when the sand core glass tube with the microporous ceramic at the lower end is sleeved outside the grid of the anti-interference electrochemical transistor sensor, directly dripping a buffer solution containing a substance to be detected into the sand core glass tube of the anti-interference electrochemical transistor sensor, dripping nitrite standard solutions with different concentrations, detecting a time current curve of the electrochemical transistor sensor by using a digital source meter, drawing a standard curve according to the change value of the current and the concentration of the nitrite standard solution, and further determining the content of nitrite in a sample to be detected.
Compared with the prior art, the invention has the beneficial effects that: the invention adopts a new idea to shield the response of the interfering substance by separating the channel from the grid so as to solve the anti-interference of the electrochemical transistor sensor, and has the characteristic of shielding the response of the interfering substance while not influencing the response of the device to the substance to be detected. The invention provides three methods for improving the anti-interference performance of the device. In the first method, a Nafion film is covered on a channel to separate the channel from interfering substances, and because the surface of the Nafion film is charged with negative charges, interference from anions is greatly shielded due to electrostatic interaction, so that the response of a device to the interference is remarkably reduced, particularly the anions; in the second method, a chitosan film is covered on the channel to separate the channel from the interfering substance; in the third method, a sand core glass tube with microporous ceramics at the lower end is sleeved outside the grid, so that the electrolyte contacting with the grid is separated from the electrolyte contacting with the channel; and the reactant is directly dripped into the glass tube, so that only the substance to be detected is allowed to be directly contacted with the grid electrode, meanwhile, the interference substance is difficult to diffuse to the vicinity of the channel, the response of the device to the interference is greatly reduced, and the selectivity of the device basically meets the requirement.
Drawings
FIG. 1 is a schematic diagram of an electrochemical transistor sensor with interference immunity;
FIG. 2 is a graph of interference testing of an electrochemical transistor sensor without interference rejection optimization as described in a comparative example;
FIG. 3 is a graph of the interference test of the electrochemical transistor sensor of example 1 for interference resistance;
FIG. 4 is a graph of the interference test of the electrochemical transistor sensor of example 2 for interference resistance;
FIG. 5 is an interference test plot of the electrochemical transistor sensor of example 3 for interference immunity;
FIG. 6 is a graph of the nitrite detection operation of the interference immunity electrochemical transistor sensor described in example 4.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the content of the present invention, but the present invention is not limited to the following examples.
The preparation method of the electrochemical transistor sensor mainly comprises the following steps:
plating a chromium layer and a gold layer on a substrate, wherein the gold layer is overlapped above the chromium layer and is used as an electrode of an electrochemical transistor sensor, a source electrode and a drain electrode are respectively selected, and a channel of the electrochemical transistor sensor is arranged between the source electrode and the drain electrode;
secondly, transferring the single-layer graphene onto the channel of the electrochemical transistor sensor obtained in the first step by adopting wet transfer to obtain a source electrode, a drain electrode and a channel of the electrochemical transistor sensor with the single-layer graphene as the channel;
thirdly, electrodepositing gold and graphene nano composite particles on the cleaned glassy carbon electrode by a cyclic voltammetry method to serve as a grid electrode of the electrochemical transistor sensor;
fourthly, a Nafion film protective layer and/or a glycan film protective layer is/are arranged on the channel, or a sand core glass tube with microporous ceramics at the lower end is sleeved outside the grid, and the channel or the grid is separated to shield the response of the electrochemical transistor sensor to interference substances, so that the electrochemical transistor sensor with the anti-interference function is obtained.
Of course, the present invention is not limited to the electrochemical transistor sensor, and any method suitable for resisting interference proposed by the present invention is within the protection scope of the present invention.
Comparative example
The electrochemical transistor sensor is prepared by the following specific preparation method:
the method comprises the steps of firstly, plating chromium and gold on a 1x1cm glass substrate in sequence by an evaporation coating method, wherein the thickness of the chromium is about 0.4nm, and the thickness of the gold is about 30nm, and the chromium and the gold are used as a source electrode and a drain electrode of a transistor;
secondly, uniformly coating a PMMA film on single-layer graphene of a copper substrate by a glue homogenizing method, etching the graphene on the back surface for 3min by using oxygen plasma, transferring a copper sheet to the surface of 0.7M ferric nitrate solution, cleaning the copper sheet for 3 times after the copper sheet is corroded, transferring the single-layer graphene to a channel of the transistor prepared in the first step, and then soaking the device in acetone at 60 ℃ to dissolve PMMA on the graphene to obtain the electrochemical transistor taking the graphene as the channel;
third, in 1mM HAuCl4Carrying out electrodeposition (electrodeposition adopts an electrical cyclic voltammetry method, the scanning speed is 50mV/s, and the number of scanning cycles is 10) on a glassy carbon electrode in 0.5mg/mL graphene oxide solution, wherein the gold and graphene nano composite particles are used as a grid electrode; and the grid electrode, the obtained source drain electrode and the obtained channel are jointly combined to obtain the electrochemical transistor sensor.
In order to examine the anti-interference performance of the electrochemical transistor sensor which is not optimized for anti-interference, the comparative example selects several common interference substances: k+、Ca2+、Mg2+、NH4 +、Cl-、NO3 -、SO4 2-、PO4 3-、CH3COO-And glucose, the specific method is as follows:
setting V of digital source meterDS＝0.05V、VGThe electrochemical transistor sensor was immersed in a buffer solution at 0.8V, and a 1mM sodium nitrite solution and a common interfering substance were sequentially added: k+,Ca2+,Mg2+,NH4 +,Cl-,NO3-,SO4 2-,PO4 3-,CH3COO-And glucose solution are respectively added into the buffer solution in drops at different time, the time current curve of the transistor is detected by a digital source meter, and the anti-interference performance of the device is determined by comparing the change value of the current, as shown in figure 2.
As can be seen from the time-current curve in fig. 2, the channel current variation caused by the interfering substance is very significant. This is because most of the electrochemical response interference is due to the change in channel carrier concentration caused by the diffusion of interfering species into the vicinity of the channel. If the selectivity of the sensor is poor, the electrical signal generated when detecting the actual sample is not only from the object to be detected, but also includes the response brought by other substances. Thus, the sensor cannot accurately obtain the concentration of the analyte, and the quantitative determination and the like are affected. Therefore, it is highly desirable to optimize the immunity of electrochemical transistor sensors to interference.
Example 1
An electrochemical transistor sensor with interference immunity which differs from the comparative example in that: a Nafion film protective layer is arranged on the channel, and the specific method comprises the following steps: a Nafion film protective layer is formed by dripping 10 mu L of Nafion solution with the mass concentration of 0.5 wt% on the graphene channel.
In order to verify the anti-interference performance of the anti-interference electrochemical transistor sensor, several common interference substances are also selected: k+、Ca2+、Mg2+、NH4 +、Cl-、NO3 -、SO4 2-、PO4 3-、CH3COO-And grapeThe sugar was tested for selectivity as follows:
setting V of digital source meterDS＝0.05V、VGThe electrochemical transistor sensor with interference-resistant properties was immersed in a buffer solution at 0.8V, and a 1mM sodium nitrite solution and a common interfering substance were sequentially added: k+,Ca2+,Mg2+,NH4 +,Cl-,NO3-,SO4 2-,PO4 3-,CH3COO-And glucose solution are respectively added into the buffer solution in drops at different time, the time current curve of the transistor is detected by a digital source meter, and the anti-interference performance of the device is determined by comparing the change value of the current, as shown in figure 3.
As can be seen from fig. 3, the response of the interference-resistant electrochemical transistor sensor to interfering substances, in particular anions, is significantly reduced. This is due to the negative charge on the surface of the Nafion membrane and the interference from anions is greatly shielded due to electrostatic interactions.
Example 2
An electrochemical transistor sensor with interference immunity which differs from the comparative example in that: the method for arranging the glycan film protective layer on the channel comprises the following steps: 15 mu L of chitosan solution with the mass concentration of 50mg/mL is dripped on the graphene channel, and a chitosan film protective layer is formed by a glue homogenizing method.
In order to verify the anti-interference performance of the anti-interference electrochemical transistor sensor, several common interference substances are also selected: k+、Ca2+、Mg2+、NH4 +、Cl-、NO3 -、SO4 2-、PO4 3-、CH3COO-And glucose, the specific method is as follows:
setting V of digital source meterDS＝0.05V、VGThe electrochemical transistor sensor with interference-resistant properties was immersed in a buffer solution at 0.8V, and a 1mM sodium nitrite solution and a common interfering substance were sequentially added: k+,Ca2+,Mg2+,NH4 +,Cl-,NO3-,SO4 2-,PO4 3-,CH3COO-And glucose solution are respectively added into the buffer solution in drops at different time, the time current curve of the transistor is detected by a digital source meter, and the anti-interference performance of the device is determined by comparing the change value of the current, as shown in figure 4.
As can be seen from fig. 4, the response of the electrochemical transistor sensor to interfering substances of this interference-resistant performance is slightly reduced. This is because a part of the interfering substance is blocked outside the channel due to the steric effect, but the response to the interfering substance is reduced less remarkably than in example 1.
Example 3
An electrochemical transistor sensor with interference immunity which differs from the comparative example in that: a layer of sand core glass tube with micropore ceramics at the lower end is sleeved outside the grid, and the concrete method comprises the following steps: a sand core glass tube with microporous ceramics at the lower end is sleeved outside the grid to separate the electrolyte contacting with the grid from the electrolyte contacting with the channel.
In order to verify the anti-interference performance of the anti-interference electrochemical transistor sensor, several common interference substances are also selected: k+、Ca2+、Mg2+、NH4 +、Cl-、NO3 -、SO4 2-、PO4 3-、CH3COO-And glucose, the specific method is as follows:
setting V of digital source meterDS＝0.05V、VGThe electrochemical transistor sensor with interference-resistant properties was immersed in a buffer solution at 0.8V, and a 1mM sodium nitrite solution and a common interfering substance were sequentially added: k+,Ca2+,Mg2+,NH4 +,Cl-,NO3-,SO4 2-,PO4 3-,CH3COO-And glucose solution are respectively and directly dripped into a sand core glass tube which is sleeved outside the grid and provided with microporous ceramics at the lower end, and a digital source meter is usedThe time current curve of the transistor is detected, and the anti-interference performance of the device is determined by comparing the change value of the current, as shown in fig. 5.
As can be seen from fig. 5, the response of the electrochemical transistor sensor with anti-interference performance to the interfering substance is greatly reduced, and the selectivity of the device basically meets the requirement.
Example 4
In order to verify the sensitivity of the electrochemical transistor sensor with the anti-interference performance, taking the electrochemical transistor sensor with the anti-interference performance described in embodiment 3 as an example, sodium nitrite solutions with different concentrations are detected, and the specific method is as follows:
setting V of digital source meterDS＝0.05V、VG0.8V, immersing the electrochemical transistor sensor with anti-interference performance in a buffer solution, sequentially dripping 0.1nM-10mM of sodium nitrite solution into a sand core glass tube sleeved at the lower end outside a grid and provided with microporous ceramics, detecting a time current curve of the transistor by using a digital source meter, and determining the concentration of nitrite according to the change value of current, as shown in figure 6.
As can be seen from FIG. 6, the electrochemical transistor sensor with anti-interference performance has extremely high sensitivity to nitrite, and the detection limit reaches 0.1 nM.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, many modifications and changes can be made without departing from the inventive concept of the present invention, and these modifications and changes are within the protection scope of the present invention.

Claims (7)

1. The method for improving the anti-interference performance of the electrochemical transistor sensor comprises a source electrode, a drain electrode and a grid electrode, wherein a channel of the electrochemical transistor sensor is arranged between the source electrode and the drain electrode, and the electrochemical transistor sensor is characterized in that a Nafion film protective layer and/or a chitosan film protective layer are arranged on the channel, or a sand core glass tube with microporous ceramics at the lower end is sleeved outside the grid electrode, and the channel or the grid electrode is separated to shield the response of the electrochemical transistor sensor to interference substances;
the Nafion film protective layer is formed by forming a Nafion film protective layer on the channel by a method of dripping Nafion solution; wherein the Nafion solution is 0.1-5 wt% in a dosage of 3-50 μ L/3mm2；
The chitosan film protective layer is formed on the channel by a method of dripping chitosan solution; wherein the chitosan solution takes 0.1-2 wt% acetic acid solution as solvent, the concentration is 40-60mg/mL, and the dosage is 3-20 μ L/mm2。
2. An electrochemical transistor sensor with anti-interference performance comprises a source electrode, a drain electrode and a grid electrode, and is characterized in that a Nafion film protective layer and/or a chitosan film protective layer are/is arranged on a channel, or a sand core glass tube with microporous ceramics at the lower end is sleeved outside the grid electrode;
the Nafion film protective layer is formed by forming a Nafion film protective layer on the channel by a method of dripping Nafion solution; wherein the Nafion solution is 0.1-5 wt% in a dosage of 3-50 μ L/3mm2；
The chitosan film protective layer is formed on the channel by a method of dripping chitosan solution; wherein the chitosan solution takes 0.1-2 wt% acetic acid solution as solvent, the concentration is 40-60mg/mL, and the dosage is 3-20 μ L/mm2。
3. The electrochemical transistor sensor with the anti-interference performance according to claim 2, wherein the source electrode and the drain electrode are arranged on a gold layer and a chromium layer, the gold layer is overlapped above the chromium layer, a channel of the electrochemical transistor sensor is arranged between the source electrode and the drain electrode, the channel is single-layer graphene grown in a physical vapor phase manner through wet transfer, and the grid electrode is a glassy carbon electrode modified by gold and graphene codeposition.
4. Use of the interference-tolerant electrochemical transistor sensor according to claim 2 for the quantitative analytical detection of nitrite.
5. The application of the sensor according to claim 4, wherein when the anti-interference electrochemical transistor sensor is provided with a Nafion film protective layer and/or a chitosan film protective layer on a channel, the anti-interference electrochemical transistor sensor is immersed in a buffer solution, nitrite standard solutions with different concentrations are dripped, a time current curve of the electrochemical transistor sensor is detected by using a digital source meter, a standard curve is drawn by the change value of the current and the concentration of the nitrite standard solution, and the content of nitrite in a sample to be detected is further determined; or when the sand core glass tube with the microporous ceramic at the lower end is sleeved outside the grid of the anti-interference electrochemical transistor sensor, directly dripping a buffer solution containing a substance to be detected into the sand core glass tube of the anti-interference electrochemical transistor sensor, dripping nitrite standard solutions with different concentrations, detecting a time current curve of the electrochemical transistor sensor by using a digital source meter, drawing a standard curve according to the change value of the current and the concentration of the nitrite standard solution, and further determining the content of nitrite in a sample to be detected.
6. The use according to claim 5, wherein the nitrite standard solution is present in a concentration of 0.1nM to 10 mM.
7. Use according to claim 5, characterised in that the V of the time current curveDS＝0.003-0.1V，VG＝0.6-1V。
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