CN112924512B - Alcohol hydrogel sensing device based on layered carbon nanosheets and method thereof - Google Patents
Alcohol hydrogel sensing device based on layered carbon nanosheets and method thereof Download PDFInfo
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Abstract
The invention relates to alcohol hydrogel sensing equipment based on layered carbon nanosheets, which comprises an electrolyte grid-controlled graphene transistor and hydrogel, wherein the electrolyte grid-controlled graphene transistor is fixedly arranged in the hydrogel; the electrolyte grid-controlled graphene transistor comprises a glass substrate, three metal electrodes, single-layer graphene and layered carbon nanosheets, wherein the layered carbon nanosheets are chlorella-derived layered carbon nanosheets; the hydrogel is prepared by polymerizing alcohol oxidase and polyacrylamide. The electrochemical detection platform based on the electrolyte grid-controlled graphene transistor is combined with the chlorella-derived layered carbon nanosheet and the alcohol oxidase-functionalized hydrogel to quickly detect the drinking condition in real time, and the real condition of whether drunk driving is carried out or not is predicted and evaluated by taking the alcohol content detected in the breath as a main index.
Description
Technical Field
The invention belongs to the technical field of alcohol detection, and particularly relates to alcohol hydrogel sensing equipment based on layered carbon nanosheets and a method thereof.
Background
In recent decades, malignant traffic accidents caused by drunk driving have frequently occurred, causing high attention and panic to people. According to the accident survey of the world health organization, about 50% to 60% of traffic accidents are related to drunk driving and have been listed as a major cause of death in car accidents. Therefore, in order to reduce the occurrence of accidents, inspection work has become an important part of prohibiting drunk driving.
The Blood Alcohol Concentration (BAC) test is currently the only formal determination and application of alcohol testing. However, in actual post-alcohol driving tests, on-site blood sampling is often impractical, which is time consuming and requires complex sample handling and specialized instrumentation. And it is non-real-time and cannot be concluded quickly.
In this regard, a portable alcohol breath tester has come to work, which is actually composed of an alcohol sensor (corresponding to a rheostat that varies with the alcohol concentration), whose resistance decreases with increasing alcohol concentration, and a voltmeter or ammeter, whose voltmeter representation increases if the driver breathes out alcohol at a higher concentration.
Heretofore, there have been various types of alcohol gas sensors such as semiconductor type gas sensors, single nanowire/nanorod type gas sensors, field effect transistor type gas sensors, and nano array type gas sensors, but these sensors have disadvantages such as low sensitivity, high cost, large manufacturing difficulty, and slow detection speed.
Disclosure of Invention
The invention aims to solve the problems and provide an alcohol hydrogel sensing device based on layered carbon nanosheets and a method thereof, wherein the alcohol hydrogel sensing device is simple in structure and reasonable in design.
The invention realizes the purpose through the following technical scheme:
the alcohol hydrogel sensing equipment based on the layered carbon nanosheets comprises electrolyte gate-controlled graphene transistors and hydrogel, wherein the electrolyte gate-controlled graphene transistors are fixedly arranged in the hydrogel;
the electrolyte grid-control graphene transistor comprises a glass substrate, three metal electrodes, single-layer graphene and layered carbon nanosheets, wherein the three metal electrodes are a source electrode, a drain electrode and a grid electrode respectively, the three metal electrodes are deposited on the glass substrate, the single-layer graphene is arranged on a graphene channel between the source electrode and the drain electrode, the layered carbon nanosheets are modified on the grid electrode, and the layered carbon nanosheets are derived from chlorella;
the hydrogel is prepared by polymerizing alcohol oxidase and polyacrylamide.
As a further optimization scheme of the invention, the device carries out real-time current monitoring through two Keithley digital source meters 2400 controlled by Labview software.
As a further optimized scheme of the invention, the electrolyte grid-controlled graphene transistor is packaged by waterproof glue, the electrolyte grid-controlled graphene transistor is half embedded in hydrogel, and the single-layer graphene and the layered carbon nanosheets are fully embedded in the hydrogel.
As a further optimization of the invention, the three metal electrodes are patterned electrodes comprising a gold layer and a chromium layer, the gold layer being coated on the outer surface of the chromium layer.
A manufacturing method of alcohol hydrogel sensing equipment based on layered carbon nanosheets comprises the following steps:
s1, manufacturing a substrate: adopting a glass sheet as a glass substrate, and ultrasonically cleaning the glass substrate;
s2, manufacturing a patterned electrode: the method comprises the following steps of drying a glass substrate by using nitrogen, fixing the glass substrate on a mask plate by using an adhesive tape, depositing a patterned chromium/gold electrode on the glass substrate by using magnetron sputtering, depositing a chromium layer firstly, and depositing a gold layer secondly, wherein the chromium layer mainly has the function of increasing the adhesion of gold and the glass substrate and avoiding the gold electrode from falling and being damaged;
s3, preparing single-layer graphene: by CH 4 And H 2 The mixed gas is synthesized into single-layer graphene through chemical vapor deposition, a Cu foil is used as a catalytic substrate, then a polymethyl methacrylate film is coated on the graphene in a spinning mode, and then the graphene is immersed into an etching solution to etch a Cu substrate and is washed for several times by distilled water;
s4, transferring graphene: transferring graphene between a source electrode and a drain electrode of a patterned substrate in water by using a wet transfer method, annealing, soaking the annealed substrate in acetone, replacing new acetone, soaking again, and repeating for multiple times;
s5, packaging of the device: protecting metal wires connecting the source electrode, the drain electrode and the grid electrode by using a waterproof siloxane layer so as to prevent short circuit caused by contact with an electrolyte in a sensor testing process;
s6, modifying the synthesized layered carbon nanosheets on bare gold electrodes of grids, drying, adding an acrylamide solution, an ethanol oxidase solution and a phosphate buffer solution into a container, uniformly stirring, polymerizing gel under N, N, N ', N' -tetramethyldiamine and ammonium persulfate, and semi-embedding an electrolyte grid-controlled graphene transistor and an air blowing pipe into the gel to obtain the hydrogel sensing equipment, wherein the whole process is carried out on ice, and the hydrogel sensing equipment is refrigerated for later use.
As a further optimization scheme of the invention, in the step S1, the glass substrate is sequentially subjected to ultrasonic cleaning by using acetone, ethanol and deionized water.
As a further optimization scheme of the invention, in step S3, polymethyl methacrylate is spin-coated on graphene by a two-step method, wherein the spin-coating is performed at a slow speed and at a fast speed, so that the polymethyl methacrylate is more uniformly spin-coated on graphene.
As a further optimization scheme of the invention, in the step S3, the etching solution comprises CuSO 4 、HCl、H 2 O, and CuSO 4 ：HCl：H 2 O＝10g：50mL：50mL。
A method for detecting alcohol blowing by using alcohol hydrogel sensing equipment based on layered carbon nanosheets judges the concentration of alcohol gas by measuring a channel current real-time response curve:
and measuring the change of the channel current along with time under the condition of fixed source voltage and grid voltage, taking the current value as initial current when the channel current is basically unchanged, then starting blowing air into the hydrogel, and enabling the current change value caused by expiration to correspond to the concentration of the alcohol gas.
The invention has the beneficial effects that:
1) The electrochemical detection platform based on the electrolyte grid-controlled graphene transistor is combined with the chlorella-derived layered carbon nanosheet and the alcohol oxidase-functionalized hydrogel to quickly detect the drinking condition in real time, and the real condition of whether drunk driving is carried out or not is predicted and evaluated by taking the alcohol content detected in breath as a main index, so that the electrolyte grid-controlled graphene transistor also has the advantages of low working voltage (generally less than 1V), quickness, real time, high sensitivity, low cost, easiness in manufacturing and the like, and the actual requirement of quickly detecting alcohol in real time, conveniently and accurately is met by combining the electrolyte grid-controlled graphene transistor with the hydrogel 7;
2) The alcohol hydrogel sensing equipment has the advantages of simple structure, low cost, easy manufacture and the like.
Drawings
Fig. 1 is a schematic diagram of an electrolyte gated graphene transistor of the present invention;
FIG. 2 is a flow chart of an electrolyte gated graphene transistor fabrication process of the present invention;
FIG. 3 is a diagram showing the effect of the detection method of the alcoholic hydrogel sensing device of the present invention.
In the figure: 1. a source electrode; 2. a drain electrode; 3. a gate electrode; 4. a glass substrate; 5. single-layer graphene; 6. a layered carbon nanosheet; 7. a hydrogel.
Detailed Description
The present application will now be described in further detail with reference to the drawings, and it should be noted that the following detailed description is given for purposes of illustration only and should not be construed as limiting the scope of the present application, as these numerous insubstantial modifications and variations can be made by those skilled in the art based on the teachings of the present application.
Example 1
As shown in fig. 1, an alcohol hydrogel sensing device based on layered carbon nanosheets comprises an electrolyte gated graphene transistor (SGGT) and a hydrogel 7, wherein the electrolyte gated graphene transistor is fixedly mounted in the hydrogel 7, and the electrolyte gated graphene transistor is a field effect transistor with a graphene transistor, and is connected with a channel by an electrolyte solution instead of an insulating layer, and is equivalent to a combination of a sensor and an amplifier;
the electrolyte grid-controlled graphene transistor comprises a glass substrate 4, three metal electrodes, a single-layer graphene 5 and a layered carbon nanosheet 6 (CNs), wherein the three metal electrodes are a source electrode 1, a drain electrode 2 and a grid electrode 3 respectively, the three metal electrodes are deposited on the glass substrate 4, the single-layer graphene 5 is arranged on a graphene channel between the source electrode 1 and the drain electrode 2, the layered carbon nanosheet 6 is modified on the grid electrode 3, and the layered carbon nanosheet 6 is a chlorella-derived layered carbon nanosheet 6;
the hydrogel 7 is prepared by polymerizing Alcohol Oxidase (AOX) and Polyacrylamide (PAM).
Further, the device was monitored for current in real time by two Keithley digital source meters 2400 controlled by Labview software.
Further, the electrolyte grid-controlled graphene transistor is applied to electrochemical detection of compounds in a solution system, and is different from a traditional field effect transistor, an electrolyte solution is contacted with a graphene channel and a grid 3, the change of channel current is regulated and controlled through the voltage of the grid 3, the voltage of the grid 3 is equivalent to that applied to two interfaces of the grid 3/electrolyte and the electrolyte/channel, each interface is provided with an electric double layer and is equivalent to a capacitor, the change of channel current can be regulated and controlled through the voltage of the grid, and each graphene transistor is equivalent to the combination of a sensor and an amplifier. The electrolyte grid-control graphene transistor also has the advantages of low working voltage (generally less than 1V), rapidness, real-time property, high sensitivity, low cost, easiness in manufacturing and the like, and the actual requirement of rapid, real-time, portable and high-accuracy alcohol detection is met by combining the electrolyte grid-control graphene transistor with the hydrogel 7.
Further, the electrolyte gate-controlled graphene transistor is half embedded in the hydrogel 7, and the single-layer graphene 5 and the layered carbon nanosheets 6 are fully embedded in the hydrogel 7.
Further, the three metal electrodes are patterned electrodes which comprise a gold layer and a chromium layer, and the gold layer covers the outer surface of the chromium layer.
As shown in fig. 2, the invention further provides a manufacturing method of the alcohol hydrogel sensing device based on the layered carbon nanosheets, which includes the following steps:
firstly, cutting and cleaning a glass substrate 4, then carrying out magnetron sputtering on the surface of the glass substrate with a patterned electrode through a mask plate, then preparing single-layer graphene 5 by an electrochemical vapor deposition method, transferring the single-layer graphene 5 to a channel between a source electrode 1 and a drain electrode 2, and finally packaging the graphene transistor by waterproof glue to prevent short circuit; a transistor with three electrodes, gate 3, source 1, drain 2 and a single layer graphene channel was mounted in a hydrogel 7 of 10mL size and monitored for current in real time by two Keithley digital source meters 2400 controlled by Labview software.
The method specifically comprises the following steps:
s1, manufacturing a substrate: cutting the glass slide into small glass sheets with the size of 1cm multiplied by 1cm by a glass knife to be used as a glass substrate 4, and carrying out ultrasonic cleaning on the glass substrate 4 for 20min by using acetone, ethanol and deionized water in sequence;
s2, manufacturing a patterned electrode: after the glass substrate 4 is dried by high-purity nitrogen, the glass substrate 4 is fixed on a mask plate by a high-temperature adhesive tape, a chromium/gold electrode patterned on the glass substrate 4 is deposited by magnetron sputtering, a chromium layer (10 nm) is deposited firstly, and then a gold layer (100 nm) is deposited, wherein the chromium layer mainly has the function of increasing the adhesion between gold and the glass substrate 4 and avoiding the gold electrode from falling off and being damaged;
s3, preparing single-layer graphene 5: by CH 4 (40 SCCM) and H 2 Synthesizing single-layer graphene 5 from the mixed gas of (20 SCCM) by Chemical Vapor Deposition (CVD) at 1000 ℃, using a Cu foil with the thickness of 25 mu m as a catalytic substrate, spin-coating a polymethyl methacrylate (PMMA) film on the graphene, then immersing the graphene in an etching solution to etch the Cu substrate, and washing the Cu substrate for several times by using distilled water;
in order to enable the polymethyl methacrylate (PMMA) to be more uniformly spin-coated on the graphene, a two-step method is adopted to spin-coat the polymethyl methacrylate (PMMA) on the graphene, wherein the slow spin-coating at 800rpm is firstly carried out for 10s, and then the fast spin-coating at 2000rpm is carried out for 20s;
in addition, the etching solution comprises CuSO 4 、HCl、H 2 O, and CuSO 4 ：HCl：H 2 O＝10g：50mL：50mL；
S4, transferring graphene: transferring graphene between a source electrode 1 and a drain electrode 2 of a patterned substrate in water by using a wet transfer method, annealing at 120 ℃ for 15min, soaking the annealed substrate in acetone at 50 ℃ for 1h, replacing new acetone, soaking again, and repeating for three times;
s5, packaging of the device: protecting metal wires connecting the source electrode 1, the drain electrode 2 and the grid electrode 3 with a waterproof siloxane layer to prevent short circuit caused by contact with electrolyte in the sensor testing process;
s6, modifying the synthesized layered carbon nanosheet 6 on a bare gold electrode of a grid 3, drying the electrode at room temperature, then adding 3mL of 30% acrylamide solution by mass ratio, 25 mu L of ethanol oxidase solution (AOX) with the volume of 52mg/mL and 7mL of Phosphate Buffered Saline (PBS) into a small square box and uniformly stirring, polymerizing gel under N, N, N ', N' -Tetramethyldiamine (TEMED) and ammonium persulfate with the mass ratio of 10%, and embedding an electrolyte gate control graphene transistor and an air blowing pipe into the gel in half to obtain the hydrogel sensing device, wherein the whole process is carried out on ice, and the hydrogel sensing device is placed in a refrigerator at 4 ℃ for later use.
As shown in figure 3, the invention also provides a method for detecting alcohol blowing by using the alcohol hydrogel sensing equipment based on the layered carbon nano-sheets, which is implemented by measuring a channel current real-time response curve (I) DS -t) judging the alcohol gas concentration:
at a fixed source 1 voltage (V) DS = 0.05V) and gate 3 voltage (V) G = 0.7V) was measured for the channel current I DS Change over time, until the channel current I DS When the current value is basically unchanged, the current value is taken as the initial current I 0 Then, blowing air into the hydrogel 7 is started, wherein each time interval is 25min, and the current change value I caused by expiration n The measurement results are shown in fig. 3 for the alcohol gas concentration.
From fig. 3 it can be found that: the alcohol hydrogel sensing equipment is high in sensitivity, fast and real-time, and meets the actual requirements of fast, real-time and high-accuracy alcohol detection.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (8)
1. The alcohol hydrogel sensing equipment based on the layered carbon nanosheets is characterized in that: the graphene-based photovoltaic cell comprises an electrolyte grid-control graphene transistor and hydrogel (7), wherein the electrolyte grid-control graphene transistor is fixedly arranged in the hydrogel (7);
the electrolyte grid-controlled graphene transistor comprises a glass substrate (4), three metal electrodes, a single-layer graphene (5) and a layered carbon nanosheet (6), wherein the three metal electrodes are a source electrode (1), a drain electrode (2) and a grid electrode (3) respectively, the three metal electrodes are deposited on the glass substrate (4), the single-layer graphene (5) is arranged on a graphene channel between the source electrode (1) and the drain electrode (2), the layered carbon nanosheet (6) is modified on the grid electrode (3), and the layered carbon nanosheet (6) is a chlorella-derived layered carbon nanosheet (6);
the hydrogel (7) is prepared by polymerizing alcohol oxidase and polyacrylamide;
the electrolyte grid-control graphene transistor is packaged by waterproof glue, the electrolyte grid-control graphene transistor is half embedded into hydrogel (7), the single-layer graphene (5) and the layered carbon nanosheets (6) are fully embedded into the hydrogel (7), and the alcohol hydrogel sensing equipment based on the layered carbon nanosheets judges the concentration of alcohol gas by measuring a channel current real-time response curve when detecting alcohol blowing: and measuring the change of the channel current along with time under the condition of fixing the voltage of the source electrode (1) and the voltage of the grid electrode (3), taking the current value as an initial current when the channel current is basically unchanged, then starting to blow air into the hydrogel (7), and enabling the current change value caused by expiration to correspond to the concentration of the alcohol gas.
2. The alcoholic hydrogel sensing device based on layered carbon nanosheets of claim 1, wherein: the device was monitored for real-time current by two Keithley digital source meters 2400 controlled by Labview software.
3. The alcoholic hydrogel sensing device based on layered carbon nanosheets of claim 1, wherein: the electrolyte grid-controlled graphene transistor is applied to electrochemical detection of compounds in a solution system, an electrolyte solution is contacted with a graphene channel and a grid (3), and the change of channel current is regulated and controlled through the voltage of the grid (3).
4. The alcoholic hydrogel sensing device based on layered carbon nanosheets of claim 1, wherein: the three metal electrodes are patterned electrodes comprising a gold layer and a chromium layer, the gold layer overlying the outer surface of the chromium layer.
5. A method for preparing the layered carbon nanoplate-based alcoholic hydrogel sensing device according to any one of claims 1 to 4, wherein: the method comprises the following steps:
s1, manufacturing a substrate: a glass sheet is used as a glass substrate (4), and the glass substrate (4) is ultrasonically cleaned;
s2, manufacturing a patterned electrode: drying the glass substrate (4) by using nitrogen, fixing the glass substrate on a mask plate by using an adhesive tape, depositing a patterned chromium/gold electrode on the glass substrate (4) by using magnetron sputtering, firstly depositing a chromium layer, and then depositing a gold layer;
s3, preparing single-layer graphene (5): by CH 4 And H 2 The mixed gas is synthesized into single-layer graphene (5) through chemical vapor deposition, a Cu foil is used as a catalytic substrate, a polymethyl methacrylate film is spin-coated on the graphene, and then the graphene is immersed in an etching solution to etch a Cu substrate and is washed for a plurality of times by distilled water;
s4, transferring graphene: transferring graphene between a source electrode (1) and a drain electrode (2) of a patterned substrate in water by using a wet transfer method, annealing, soaking the annealed substrate in acetone, replacing new acetone, soaking again, and repeating for multiple times;
s5, packaging of the device: protecting a metal wire connecting the source electrode (1), the drain electrode (2) and the grid electrode (3) by using a waterproof siloxane layer;
s6, modifying the synthesized layered carbon nanosheet (6) on a bare gold electrode of a grid (3), drying, adding an acrylamide solution, an ethanol oxidase solution and a phosphate buffer solution into a container, uniformly stirring, polymerizing gel under N, N, N ', N' -tetramethyl diamine and ammonium persulfate, and semi-embedding an electrolyte grid-control graphene transistor and an air blowing pipe into the gel to obtain the hydrogel sensing equipment, wherein the whole process is carried out on ice, and the hydrogel sensing equipment is refrigerated for later use.
6. The preparation method of the alcohol hydrogel sensing device based on the layered carbon nanosheets as claimed in claim 5, wherein: in the step S1, the glass substrate (4) is subjected to ultrasonic cleaning by using acetone, ethanol and deionized water in sequence.
7. The preparation method of the alcohol hydrogel sensing device based on the layered carbon nanosheets, as set forth in claim 5, wherein: in the step S3, polymethyl methacrylate is spin-coated on the graphene by adopting a two-step method, wherein the speed is slow firstly, and then the speed is fast, so that PMMA is spin-coated on the graphene more uniformly.
8. The preparation method of the alcohol hydrogel sensing device based on the layered carbon nanosheets, as set forth in claim 5, wherein: in step S3, the etching solution comprises CuSO 4 、HCl、H 2 O, and CuSO 4 ：HCl：H 2 O＝10g：50mL：50mL。
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