CN110672666B - Electronic nose device and preparation method thereof - Google Patents
Electronic nose device and preparation method thereof Download PDFInfo
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- CN110672666B CN110672666B CN201911046298.9A CN201911046298A CN110672666B CN 110672666 B CN110672666 B CN 110672666B CN 201911046298 A CN201911046298 A CN 201911046298A CN 110672666 B CN110672666 B CN 110672666B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The invention discloses an electronic nose device and a preparation method thereof, and the electronic nose device comprises a substrate and N multiplied by M Field Effect Transistor (FET) type gas sensor arrays formed on the substrate, wherein each gas sensor in the arrays comprises a metal electrode arranged on the substrate and a patterned two-dimensional material conductive channel, the sensor arrays are modified in the same way according to rows, and the same grid voltage is applied according to columns. In the gas-sensitive test process, the response amplitude of each sensing unit is adjusted by changing the grid voltage, and the sensitivity to specific gas is enhanced or inhibited, so that the selectivity and the difference of the electronic nose device to different gases are realized. The method is used for detecting and identifying the low-concentration mixed gas, and has the technical advantages of high sensitivity, high reliability, strong noise resistance and the like.
Description
Technical Field
The invention relates to the field of semiconductor gas sensors, in particular to an electronic nose device and a preparation method thereof.
Background
With the rapid development of economy, industrial emission causes more and more serious atmospheric pollution, and atmospheric quality monitoring is increasingly important; in the production link, the concentration of flammable, explosive or toxic gas in the air is often required to be monitored so as to ensure safe production; in the food field, the quality, freshness and the like of products can be detected by a gas sensor; in the biomedical field, the detection of minute amounts of volatile organic gases (VOCs) in human breath can be used to assist medical diagnosis. However, a single component gas sensor is difficult to meet such application requirements. In addition, especially with the development of the internet of things, more gas sensors are needed in each link of production and logistics, and distributed sensing becomes a major development trend of production and life informatization in the future. Distributed sensing is expected to have smaller size and lower power consumption for future gas sensors. There is therefore a need to develop new gas sensors for ultra-low concentration, multi-component mixed gas identification.
A plurality of gas sensors with different gas sensitivity characteristics form an array, and gas components are judged through an image formed by response data of each device, and a gas sensing system based on the principle is generally called an electronic nose. Because most gas sensors have cross sensitivity, gas components and concentrations cannot be directly obtained from the response of one sensing unit in the array, and the odor is identified from the response image of the sensor array by a data fusion method, a neural network algorithm and other similar image identification methods. Based on this sensing principle, the selectivity of each sensing unit in the sensor array and its difference are the key to determine the gas resolution capability. In principle, the better the selectivity of each sensing unit, the larger the difference in selectivity is, the more beneficial the identification of gas is. The gas sensors in commercial electronic noses that are common today are mostly based on semiconducting metal oxides. Such devices currently fail to meet the requirements for distributed sensing: 1. the array is assembled by separate devices with different sensitive materials, so that the integration and the miniaturization of the devices are severely limited; 2. the temperature required by the contact reaction of the metal oxide and the gas is usually over 200 ℃, and the device needs to be heated to work, so that the power consumption of the device is difficult to reduce. The method finds a new gas sensitive material and a new device structure, greatly reduces the power consumption of the device, realizes the integration and miniaturization of the array, and has important significance for the future distributed gas sensing.
Disclosure of Invention
Aiming at the problem that the existing electronic nose device cannot meet the requirement of distributed sensing, the invention provides the electronic nose device and the preparation method thereof, the response amplitude of each sensing unit is adjusted by changing the gate voltage, and the sensitivity to specific gas is enhanced or inhibited, so that the selectivity and the difference of the FET type gas sensor array to different gases are realized.
The invention is realized by the following technical scheme:
an electronic nose device comprises a substrate and an N multiplied by M FET type gas sensor array arranged on the substrate, wherein the grid electrodes of the gas sensors in the same column apply the same voltage, the conductive channel materials of the gas sensors in the same row are modified in the same way, and the conductive channel materials of the gas sensors in different rows are modified in different ways.
Preferably, the conducting channel material is graphene, black phosphorus and MoS2One ofAnd (4) seed preparation.
Preferably, the conductive channel material of each gas sensor is modified by loading with nanoparticles.
Preferably, the nanoparticles are Pt, Pd, Au, Ag, Ni, Cu, SnO2、ZnO、TiO2、CuO、WS2CdS or Fe3O4。
Preferably, the FET type gas sensor is one of a back gate, a top gate, a side gate, and a wrap gate structure.
Preferably, in the FET-type gas sensor array, the same gate voltage is applied to the gates of the gas sensors in the same column, and different gate voltages are applied to different columns.
Preferably, the voltage applied to the grid electrode is-50V.
The invention also provides a preparation method of the electronic nose device, which comprises the following steps:
s1, preparing an N multiplied by M FET type gas sensor array on a substrate;
s2, conducting channel materials of the gas sensors in the same row are modified by the same nano particles, and conducting channel materials of the gas sensors in different rows are modified by different nano particles.
Preferably, the method of preparing the N × M FET-type gas sensor array in step S1 is as follows:
s1.1, photoetching is carried out on a substrate to form M grid patterns;
s1.2, depositing a metal electrode on the substrate in the step S1.1 to form a grid in the grid pattern area;
s1.3, depositing metal oxide on the metal electrode layer formed in the step S1.2 to form a dielectric layer;
s1.4, photoetching is carried out on the dielectric layer obtained in the step S1.3, and source electrode patterns and drain electrode patterns of N gas sensors are formed above each grid electrode;
s1.5, depositing a metal electrode on the surface of the substrate obtained in the step S1.4, and forming a source electrode and a drain electrode of the gas sensor in a source electrode and drain electrode pattern area;
s1.6, removing the photoresist protection area on the surface of the substrate, and reserving a source electrode, a drain electrode and a grid electrode of the gas sensor to obtain the N multiplied by M FET type gas sensor array.
Preferably, the modification method of the conductive channel in step S2 is specifically as follows:
firstly, transferring a channel material to a conductive channel region of a gas sensor, etching to form a conductive channel pattern, and then modifying nanoparticles on the conductive channel pattern;
or modifying the nano particles on the channel material, transferring the channel material to the conductive channel region, and etching to form a conductive channel pattern.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention provides an electronic nose device, which carries out the same modification on a sensor array of an electronic nose according to rows and applies the same gate voltage according to columns. In the gas-sensitive test process, the response amplitude of each sensing unit is adjusted by changing the grid voltage, and the sensitivity to specific gas is enhanced or inhibited, so that the selectivity and the difference of each sensing unit in the array device are realized, and the defects of high working temperature, high power consumption, low detection rate, poor sensitivity, single sensitive parameter and the like in the electronic nose based on metal oxide in the prior art are overcome.
The invention also provides a preparation method of the electronic nose device, and the N multiplied by M sensor array can be simply and efficiently obtained by preparing the grid electrode, the source electrode and the drain electrode. The channel material is modified in situ by methods such as sputtering, evaporation, dripping and the like, so that the electronic nose device is compatible with a mature photoetching process, a conductive channel with micron or even nano-scale size can be obtained, the possibility is provided for further reducing the size of the electronic nose device, and the integration level of the electronic nose device is further improved.
Drawings
FIG. 1 is a schematic diagram of a 3X 3FET type gas sensor array in an embodiment of the present invention;
FIG. 2 is a light mirror image of a graphene conducting channel in an embodiment of the invention;
FIG. 3 shows the magnetron sputtering repair of the present inventionDecorating TiO2SEM images of graphene channels of nanoparticles;
FIG. 4 is a data graph of the response curves of three conductive channels above the M2 column to 100ppm gas in example 1 of the present invention;
FIG. 5 is a graph of data on the selectivity of three conduction channels above the M2 column to 100ppm gas in example 1 of the present invention;
FIG. 6 shows SiO in the top of N2 line when the gate voltage of the electronic nose device of the present invention is 0V2The gas-sensitive response curves of three conductive channels modified by nano particles to 100ppm of gas A, gas B and gas propane respectively;
FIG. 7 shows SiO in the top of N2 lines when the gate voltage of the electronic nose device of the present invention is +5V, 0V and-5V, respectively2And the three conductive channels modified by the nano particles respectively have gas-sensitive response curves for 100ppm of gas A, gas B and gas propane.
In the figure: 1. a source electrode; 2. a gate electrode; 3. a drain electrode; 4. a dielectric layer; 5. a substrate; 6. a conductive channel.
Detailed Description
The present invention will now be described in further detail with reference to the attached drawings, which are illustrative, but not limiting, of the present invention.
Referring to fig. 1, an electronic nose device includes a substrate 5, and an N × M FET-type gas sensor array disposed on the substrate 5, in which conductive channel materials of the gas sensors in the same row are modified in the same manner, and conductive channel materials of the gas sensors in different rows are modified in different manners.
In the gas-sensitive test process of the electronic nose device provided by the invention, the response amplitude of each gas sensing unit is adjusted by changing the voltage of the grid 2, and the sensitivity to specific gas is enhanced or inhibited, so that the selectivity and the difference of the electronic nose device to different gases are realized.
Each gas sensor comprises a metal electrode and a patterned two-dimensional material conducting channel 6, wherein the metal electrode is arranged on a substrate 5 and comprises a source electrode 1 and a drain electrode 3, and the source electrode 1 and the drain electrode 3 are symmetrically arranged on two sides of a grid electrode 2 and are connected through the conducting channel 6.
The two-dimensional material of the conductive channel 6 is graphene, black phosphorus and MoS2One kind of (1).
The material of the conductive channel 6 of each gas sensor is modified by loading with nanoparticles.
The material of the conductive channels 6 in the N rows is modified in N different ways, and the conductive channels 6 of the gas sensors in each row are modified in the same way.
The nano particles are Pt, Pd, Au, Ag, Ni, Cu and SnO2、ZnO、TiO2、CuO、WS2、CdS、Fe3O4One kind of (1).
The FET type gas sensor is one or more of back gate, top gate, side gate and surrounding gate structures.
In the FET type gas sensor array, each gas sensor in the same column shares one grid 2, M columns apply M kinds of grid voltage values, and the range is-50V.
The invention also provides a preparation method of the electronic nose device, which comprises the following steps:
and S1, forming a patterned FET type metal electrode array on the substrate.
Processing a metal electrode array pattern on a substrate through photoresist, and depositing a metal electrode on the substrate through one of evaporation, sputtering, ion plating, laser pulse or molecular beam epitaxy methods, wherein the specific steps are as follows:
s1.1, carrying out first photoetching on a clean substrate by using negative photoresist to form M grid patterns;
s1.2, depositing a metal electrode on the substrate in the step S1.1 by adopting any one of evaporation plating, sputtering, ion plating, laser pulse or molecular beam epitaxy methods to form a grid 2 in a grid pattern area;
s1.3, depositing metal oxide on the metal electrode layer in the step S1.2 by using a shadow mask metal mask as a mask to form a dielectric layer 4;
s1.4, carrying out secondary photoetching on the dielectric layer 4 in the S1.3 by using negative photoresist, and forming source electrode and drain electrode patterns of N gas sensors above each grid electrode;
s1.5, depositing a metal electrode on the substrate in the step S1.4 by adopting any one of evaporation plating, sputtering, ion plating, laser pulse or molecular beam epitaxy methods, and forming a source electrode 1 and a drain electrode 3 of the gas sensor in a source electrode and drain electrode pattern area;
s1.6, removing the photoresist protection area on the substrate in acetone by using a Lift-off process, and reserving a source electrode 1, a drain electrode 3 and a grid electrode 2 of the gas sensor, wherein the area between the source electrode 1 and the drain electrode 3 and positioned on the top of the grid electrode 2 is a conductive channel 6.
In a preferred embodiment, the metal electrode and the dielectric layer in steps S1.2, S1.3 and S1.5 are deposited on the substrate by a magnetron sputtering method.
S2, transferring the conducting channel material and its modification onto the substrate and between the source 1 and drain 3 of each gas sensor, and patterning the conducting channel material.
Transferring the channel material and forming a pattern by plasma etching, and modifying the nanoparticles. The method comprises the following specific steps:
s2.1, transferring a conductive channel material in a conductive channel 6 of each gas sensor;
s2.2, photoetching and developing each conducting channel material of the S2.1 by adopting positive photoresist to form a conducting channel pattern;
s2.3, etching the substrate 5 obtained in the step S2.2 by using an oxygen plasma etching method, and reserving a conductive channel pattern;
and S2.4, using methods such as sputtering, evaporation, drop coating and the like to modify the conduction channels of the gas sensors in the same row in the same way, and modifying the gas sensors in different rows in different ways.
For example, the conductive channels of the M gas sensors in row N1 are all modified with Pt nanoparticles, the conductive channels of the M gas sensors in row N2 are all modified with Pd nanoparticles, and the conductive channels of the M gas sensors in row N3 are all modified with Cu nanoparticles.
Fig. 2 is a light mirror image of a patterned graphene channel.
FIG. 3 modification of TiO2SEM image of graphene channel of nanoparticles.
And S2.5, obtaining the NxM gas sensor array, and obtaining the electronic nose device.
Example one
Referring to fig. 1, an electronic nose device comprises a silicon oxide substrate, a back gate sputtered on the substrate, and Al sputtered on the back gate2O3A dielectric layer, and a final sputtering source drain electrode in a 3 × 3 array. And growing graphene by using a CVD method, transferring the graphene to a conductive channel region by using a wet method, and etching a conductive channel pattern by using oxygen plasma, wherein the channel length is 70 μm, and the width is 50 μm. Sputtering TiO on conductive channel of sensor array N1 line2Nanoparticles, N2 line Evaporation SiO2Nanoparticles, row N3, were not modified. In the gas sensitive test process, the grid voltage applied to the M1 column of the sensor array is-5V, the grid voltage of the M2 column is 0V, and the grid voltage of the M3 column is 5V.
Fig. 4 is a graph of the response of the three conductive channels above the columns of sensor array M2 to 100ppm of methane, ethane, propane, ethanol, acetone, and ammonia, and fig. 5 is a graph of the selectivity of the three conductive channels to the six gases.
Referring to fig. 4, it can be seen that when the gate voltage is 0V, the basic resistance of the graphene conducting channel is about 1.75K Ω, and the basic resistances of the graphene conducting channels modified with SiO2 and TiO2 nanoparticles are 2M Ω and 4.3M Ω, respectively, and the gas-sensitive response curves of the three conducting channels have higher signal-to-noise ratios.
Referring to fig. 5, it can be seen that the graphene conductive channel has a low gas-sensitive response to 100ppm of methane, ethane, propane, ethanol and acetone, and does not exhibit the gas-sensitive difference between the above five gases, i.e., does not exhibit selectivity; after the graphene conducting channel is modified with SiO2 and TiO2 nanoparticles, the gas-sensitive response of the conducting channel to the five gases is further improved, and meanwhile, the gas-sensitive response of the conducting channel to the five gases is obviously different. Fig. 6 is a graph showing the gas sensitive response curves of three conductive channels modified by SiO2 nanoparticles on the top row N2 for 100ppm methane, ethane and propane gases, respectively, when the gate voltage applied to columns M1, M2 and M3 is 0V. FIG. 7 is a graph showing the gas-sensitive response curves of three conducting channels modified by SiO2 nanoparticles on the upper row N2 to 100ppm of A, B and propane gases when gate voltages applied to columns M1, M2 and M3 are +5V, 0V and-5V, respectively.
Referring to fig. 6 and 7, it can be seen that when the gate voltage is 0V, the SiO2 nanoparticle modified graphene conduction channel cannot effectively distinguish methane, ethane, and propane gases; when +5V gate voltage and-5V gate voltage are applied through M1 columns and M3 columns respectively, the response amplitude of the graphene conducting channel modified by the SiO2 nanoparticles to methane is increased from 13.1% to 19.63%, and the response is obviously improved; and the amplitude of the response curve of the propane gas is reduced from 13.87% to 7.9%, and the response is obviously inhibited, so that three gases of A, B and propane can be well distinguished.
The low-dimensional nano material is one of the most promising gas sensitive materials at present, nano particles or molecules can provide more effective adsorption sites and improve the catalytic reaction activity, and the low-dimensional nano material itself provides high conductivity sensitivity, namely, the transferred charges caused by the adsorption of the gas molecules show significant change in conductivity through the high carrier mobility of the low-dimensional nano material. The synergistic effect between the loaded modifier and the low-dimensional nano material enables the low-dimensional nano material to become an ideal platform of the high-sensitivity and high-selectivity gas-sensitive material. Furthermore, the choice of device structure is also crucial. The sensitive resistance type is the most widely applied gas sensor at present, and the device has a simple structure and directly takes the change of the resistance value as the sensitive quantity. However, since only a single resistance change can be provided as the gas-sensitive parameter, the gas resolving power is greatly limited. The field-effect tube type gas sensor can provide more electrical parameters except for resistance as sensitive quantities, and the field-effect tube type gas sensor has important significance for improving the gas identification capability of the device.
The invention provides an electronic nose device, which carries out the same modification on a sensor array of an electronic nose according to rows and applies the same gate voltage according to columns. In the gas-sensitive test process, the response amplitude of each sensing unit is adjusted by changing the grid voltage, and the sensitivity to specific gas is enhanced or inhibited, so that the selectivity and the difference of each sensing unit in the array device are realized. The defects of high working temperature, high power consumption, low detection rate, poor sensitivity, single sensitive parameter and the like in the electronic nose based on metal oxide in the prior art are overcome. The invention is expected to develop an integrated low-dimensional semiconductor gas sensor array with high sensitivity and high identification capability, and provides a miniaturized high-performance gas sensor for a future distributed sensing network. The electronic nose device is used for detecting and identifying low-concentration mixed gas and has the technical advantages of high sensitivity, high reliability, strong noise resistance and the like.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (10)
1. An electronic nose device, comprising a substrate (5), and an N x M FET-type gas sensor array provided on the substrate (5), wherein the gates (2) of the gas sensors in the same column are applied with the same voltage, the conductive channel materials of the gas sensors in the same row are modified in the same manner, and the conductive channel materials of the gas sensors in different rows are modified in different manners.
2. The electronic nose device of claim 1, wherein the conductive channel material is graphene, black phosphorus, and MoS2One kind of (1).
3. The electronic nose device according to claim 1, wherein the conductive channel material of each gas sensor is modified by loading with nanoparticles.
4. The electronic nose device of claim 3 wherein the nanoparticles are Pt, Pd, Au, Ag, Ni, Cu, SnO2、ZnO、TiO2、CuO、WS2CdS or Fe3O4。
5. An electronic nose device according to claim 1, wherein the FET-type gas sensor is one of a back gate, top gate, side gate and wrap gate structure.
6. An electronic nose device according to claim 1, characterized in that the gate (2) of each gas sensor of the FET type gas sensor array, in the same column, is applied with the same gate voltage, and in different columns, is applied with different gate voltages.
7. An electronic nose device according to claim 6, characterized in that the voltage applied by the gate (2) is-50 to 50V.
8. A method of manufacturing an electronic nose device according to any one of claims 1 to 7, comprising the steps of:
s1, preparing an N multiplied by M FET type gas sensor array on a substrate;
s2, conducting channel materials of the gas sensors in the same row are modified by the same nano particles, and conducting channel materials of the gas sensors in different rows are modified by different nano particles.
9. The method for manufacturing an electronic nose device according to claim 8, wherein the method for manufacturing an N x M FET-type gas sensor array in step S1 is as follows:
s1.1, photoetching is carried out on a substrate to form M grid patterns;
s1.2, depositing a metal electrode on the substrate in the step S1.1 to form a grid (2) in the grid pattern area;
s1.3, depositing metal oxide on the metal electrode layer formed in the step S1.2 to form a dielectric layer (4);
s1.4, photoetching is carried out on the dielectric layer (4) obtained in the step S1.3, and source electrode patterns and drain electrode patterns of N gas sensors are formed above each grid electrode;
s1.5, depositing a metal electrode on the surface of the substrate obtained in the step S1.4, and forming a source electrode (1) and a drain electrode (3) of the gas sensor in a source electrode and drain electrode pattern area;
s1.6, removing the photoresist protection area on the surface of the substrate, and reserving a source electrode (1), a drain electrode (3) and a grid electrode (2) of the gas sensor to obtain the N multiplied by M FET type gas sensor array.
10. The method for preparing an electronic nose device according to claim 8, wherein the modification method of the conductive channel in step S2 is as follows:
firstly, transferring a channel material to a conductive channel region of a gas sensor, etching to form a conductive channel pattern, and then modifying nanoparticles on the conductive channel pattern;
or modifying the nano particles on the channel material, transferring the channel material to the conductive channel region, and etching to form a conductive channel pattern.
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