CN109030564B - Transistor type formaldehyde sensor and manufacturing method thereof - Google Patents
Transistor type formaldehyde sensor and manufacturing method thereof Download PDFInfo
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- CN109030564B CN109030564B CN201810562889.0A CN201810562889A CN109030564B CN 109030564 B CN109030564 B CN 109030564B CN 201810562889 A CN201810562889 A CN 201810562889A CN 109030564 B CN109030564 B CN 109030564B
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Abstract
The invention discloses a transistor-type formaldehyde sensor and a manufacturing method thereof, wherein the transistor-type formaldehyde sensor comprises a substrate, a gate electrode arranged on the substrate, a dielectric layer arranged on the gate electrode, a composite film arranged on the dielectric layer, and a source electrode and a drain electrode arranged on the composite film, wherein the composite film is a zinc oxide film adsorbed with metal nano-particles. The transistor-type formaldehyde sensor provided by the invention has specific selectivity and strong anti-interference performance on formaldehyde, and solves the problem of poor stability and selectivity of the formaldehyde sensor in the prior art.
Description
Technical Field
The invention relates to the field of sensor devices, in particular to a transistor type formaldehyde sensor and a manufacturing method thereof.
Background
The formaldehyde sensor is an important gas-sensitive element in household environment detection as a semiconductor gas sensor, but the existing formaldehyde sensor has low selectivity, and although most of the semiconductor gas sensors have the advantages of simple manufacture, low cost, convenient use, easy matching with a test system, convenient replacement, capability of directly converting gas concentration into an electric signal and the like, the formaldehyde sensor also has the defects of poor stability and selectivity, complex sensitive mechanism, high working temperature, short service life and the like in practical application, and how to improve the comprehensive performance of the sensors becomes the work focus of researching the sensors.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention provides a transistor-type formaldehyde sensor and a method for manufacturing the same, which aims to solve the problem of poor stability and selectivity of the formaldehyde sensor in the prior art.
The technical scheme of the invention is as follows:
a transistor-type formaldehyde sensor comprises a substrate, a gate electrode arranged on the substrate, a dielectric layer arranged on the gate electrode, a composite film arranged on the dielectric layer, and a source electrode and a drain electrode arranged on the composite film, wherein the composite film is a zinc oxide film adsorbed with metal nano-particles.
In the transistor type formaldehyde sensor, metal nano particles in the composite film are adsorbed on the zinc oxide film through static electricity.
The transistor-type formaldehyde sensor is characterized in that the metal nanoparticles are one or more of gold nanoparticles, silver nanoparticles and platinum nanoparticles.
In the transistor-type formaldehyde sensor, the zinc oxide film is made of zinc oxide modified by doping alkali metal elements.
The transistor-type formaldehyde sensor is characterized in that in the zinc oxide film, the molar ratio of alkali metal elements to zinc oxide is 0.01: 1-0.15: 1.
the transistor-type formaldehyde sensor is characterized in that the substrate is a flexible substrate, the gate electrode is a metal gate electrode, and the dielectric layer is an aluminum oxide dielectric layer.
A method for manufacturing a transistor-type formaldehyde sensor comprises the following steps:
providing a substrate, and forming a gate electrode on the substrate;
depositing and preparing a dielectric layer on the gate electrode;
providing a zinc oxide solution, coating the zinc oxide solution on a dielectric layer, and annealing to form a zinc oxide film;
providing metal nano particles, performing charged modification on the zinc oxide film, and adsorbing the metal nano particles on the zinc oxide film through electrostatic action to obtain a composite film;
and depositing on the composite film to form a source electrode and a drain electrode to obtain the transistor-type formaldehyde sensor.
The manufacturing method of the transistor-type formaldehyde sensor comprises the following steps of coating the zinc oxide precursor solution on a gate electrode, and further comprises the following steps:
an alkali metal hydroxide is added to the zinc oxide solution.
The manufacturing method of the transistor-type formaldehyde sensor comprises the step of depositing aluminum oxide on the gate electrode by an atomic layer deposition method to prepare a dielectric layer.
The manufacturing method of the transistor-type formaldehyde sensor comprises the following steps of carrying out charged modification on a zinc oxide film, and comprises the following steps:
soaking the zinc oxide film by using a 3-aminopropyltriethoxysilane solution, washing the soaked zinc oxide film by using toluene, and drying in a nitrogen atmosphere.
Has the advantages that: according to the transistor type formaldehyde sensor provided by the invention, the composite film is arranged on the dielectric layer, then the source electrode and the drain electrode are arranged on the composite film, and the zinc oxide film with the metal nano particles is adsorbed on the composite film, so that the composite film can change the carrier concentration, the surface state and the device transportation capacity of the transistor, and the composite film has specific response to formaldehyde gas due to the modification of the metal nano particles, thereby realizing high selectivity and anti-interference of the device, and solving the problem that the formaldehyde sensor in the prior art is poor in stability and selectivity.
Drawings
FIG. 1 is a schematic structural diagram of a transistor-type formaldehyde sensor according to the present invention.
FIG. 2 is a flow chart of a method for manufacturing a transistor-type formaldehyde sensor according to a preferred embodiment of the present invention.
Detailed Description
The present invention provides a transistor-type formaldehyde sensor and a method for manufacturing the same, and the present invention will be described in further detail below in order to make the objects, technical solutions, and effects of the present invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A transistor-type formaldehyde sensor, suitable for detecting formaldehyde, wherein, as shown in fig. 1, comprises a substrate 100, a gate electrode 200 disposed on the substrate 100, a dielectric layer 300 disposed on the gate electrode 200, a composite film 400 disposed on the dielectric layer 300, a source electrode 500 and a drain electrode 600 disposed on the composite film 400, and the composite film 400 is a zinc oxide film 401 adsorbed with metal nanoparticles 402. According to the transistor type formaldehyde sensor, the zinc oxide film adsorbed with the metal nano particles is arranged between the dielectric layer and the source/drain electrode, and the metal nano particles modified on the zinc oxide film have a specific response effect on formaldehyde gas, so that the composite film can make a specific response on the formaldehyde gas, and a device generates a change of source leakage current when detecting the formaldehyde gas, thereby achieving a sensing effect, namely specifically identifying and detecting the formaldehyde gas.
Preferably, in the transistor-type formaldehyde sensor, in the composite film 400, the metal nanoparticles 402 are electrostatically adsorbed on the zinc oxide film 401. The electrostatic adsorption can fix the metal nanoparticles on the zinc oxide film, and the metal nanoparticles do not need to be modified or fixed by adding other groups, so that the damage to the specific formaldehyde gas response performance of the metal nanoparticles is avoided.
The metal nanoparticles 402 adsorbed on the zinc oxide film 401 may be gold nanoparticles, silver nanoparticles, platinum nanoparticles, or other metal nanoparticles having sensitive and specific response properties to formaldehyde gas.
Preferably, the zinc oxide film 401 is made of zinc oxide modified by doping of an alkali metal element, that is, zinc oxide used for manufacturing the zinc oxide film is modified by doping of an alkali metal, and the doping of the alkali metal can improve the field effect mobility of the zinc oxide, so that the performance of the prepared FET transistor is better.
More preferably, in the alkali metal doped and modified zinc oxide film, the molar ratio of alkali metal elements to zinc oxide is 0.01: 1-0.15: 1, the performance of the prepared FET transistor is excellent.
In the transistor-type formaldehyde sensor, the substrate 100 is a flexible substrate, the gate electrode 200 is a metal gate electrode and the dielectric layer 300 is an alumina dielectric layer, and the composite film 400 is also flexible, so that the whole device has excellent flexibility and high mechanical property of the device can be realized.
The performance of the transistor type formaldehyde sensor can be adjusted through different combinations of the types of metal nano particles, the doping concentration of zinc oxide, the thickness of an aluminum oxide dielectric layer, the thickness of a composite film and various parameters.
Preferably, the flexible substrate is a PDMS substrate; the gate electrode is a silver metal gate electrode; the dielectric layer is a 30 nanometer thick aluminum oxide layer; the zinc oxide nano film is a 30-nanometer thick zinc oxide nano film doped with alkali metal, is prepared on a substrate by a solution spin coating method, and then electrostatically adsorbs metal nano particles on the film; the gold source/drain electrodes will be deposited on the composite film by a reticle.
More preferably, the length of the channel of the gold source/drain electrode is 50 microns, the width of the channel of the gold source/drain electrode is 1000 microns, and the prepared sensor has excellent electrical properties.
The invention also provides a manufacturing method of the transistor-type formaldehyde sensor, as shown in fig. 2, wherein the manufacturing method comprises the following steps:
s1, providing a substrate, and forming a gate electrode on the substrate;
s2, depositing and preparing a dielectric layer on the gate electrode;
s3, providing a zinc oxide solution, coating the zinc oxide solution on the dielectric layer, and annealing to form a zinc oxide film;
s4, providing metal nano-particles, performing charged modification on the zinc oxide film, and adsorbing the metal nano-particles on the zinc oxide film through electrostatic action to obtain a composite film;
and S5, depositing and forming a source electrode and a drain electrode on the composite film to obtain the transistor type formaldehyde sensor.
Preferably, in the step S1, 20-30nm metal such as Ag is applied at a speed of 0.1nm/S at 10-6The gate electrode is formed on a flexible substrate such as PDMS by thermal evaporation in a vacuum degree of Torr.
In step S2, an aluminum oxide preparation dielectric layer is deposited on the gate electrode by an atomic layer deposition method. Preferably, the thickness of the aluminum oxide dielectric layer is 30 nm.
In step S3, the zinc oxide solution needs to be prepared first, preferably by a solution method, to reduce the manufacturing cost, and the specific steps are as follows: dissolving zinc oxide in ammonium hydroxide, refrigerating for 5 hours to increase the solubility of the zinc oxide, then spin-coating the zinc oxide solution on the dielectric layer, and annealing to form the zinc oxide film. Further, the spin coating speed of the zinc oxide film is 3000rpm, the spin coating time is 30s, the annealing temperature is 200 ℃, and the annealing time is 0.5 hour.
Preferably, the thickness of the zinc oxide film is controlled to be 30 nm.
More preferably, in step S3, an alkali metal hydroxide may be added to the zinc oxide solution to modify the doping of the zinc oxide, specifically, deionized water and hydroxide of lithium, sodium, potassium, etc. are added to the zinc oxide solution to improve the field effect mobility of the zinc oxide. Wherein, the molar ratio of the added alkali metal hydroxide to the added zinc oxide can be controlled to be 0.01: 1-0.15: 1.
in step S4, metal nanoparticles are prepared, and the aluminum oxide film in step S3 is modified with charges so that the metal nanoparticles are adsorbed on the zinc oxide film by electrostatic interaction, thereby preparing a composite film with metal nanoparticles, wherein the step of modifying the zinc oxide film with charges includes: soaking the zinc oxide film by using a 3-aminopropyltriethoxysilane solution, washing the soaked zinc oxide film by using toluene, and drying in a nitrogen atmosphere. The 3-aminopropyltriethoxysilane solution is a toluene solution of 3-aminopropyltriethoxysilane, after the zinc oxide film is soaked for 45mins, the zinc oxide film is washed for three times by toluene, redundant unreacted 3-aminopropyltriethoxysilane molecules are washed away, and then the whole device is placed in a nitrogen environment for drying, so that the electrification treatment of the zinc oxide film is completed; and then the whole device is soaked in the metal nano-particle solution for 12h, at the moment, because the zinc oxide film is provided with static electricity, the metal nano-particles can be adsorbed on the zinc oxide film through the action of the static electricity to form a target composite film, namely the zinc oxide film with the metal nano-particles.
The metal nano-particles are one or more of gold nano-particles, silver nano-particles and platinum nano-particles; the gold nanoparticles are prepared by heating a tetrachloroauric acid solution to 100 ℃, adding sodium citrate to react for 10-60 minutes (such as 30 minutes), and then cooling to room temperature, wherein preferably, the molar ratio of the sodium citrate to the tetrachloroauric acid is 3.78: 1; the silver nanoparticles are prepared by uniformly mixing sodium citrate and silver nitrate, adding sodium borohydride to react for 10-60 minutes (such as 30 minutes), and cooling to room temperature, wherein preferably, the molar ratio of the sodium citrate to the silver nitrate is 3.78: 1; the platinum nanoparticles are prepared by uniformly mixing sodium citrate and platinum tetravalent salt, adding sodium borohydride to react for 10-60 minutes (such as 30 minutes), and then cooling to room temperature, wherein preferably, the molar ratio of the sodium citrate to the platinum tetravalent salt is 3.78: 1.
in step S5, a metal of 20-30nm, such as Au, is thermally evaporated on the composite film at a rate of 0.1nm/S in a vacuum of 10-6Torr by using a mask to form a source electrode and a drain electrode, and a transistor-type formaldehyde sensor is obtained. Preferably, the length of the channel of the gold source/drain electrode is controlled to be 50 micrometers, the width of the channel is controlled to be 1000 micrometers, and the prepared sensor has excellent electrical properties.
The invention is illustrated in detail below by means of specific examples:
example 1
Forming a gate electrode on the flexible PDMS substrate through a mask in a thermal evaporation mode by silver, and preparing a 30-nanometer-thick aluminum oxide dielectric layer on the gate electrode by an atomic layer deposition method;
dissolving zinc oxide in ammonium hydroxide and refrigerating for 5 hours, and adding deionized water and hydroxides of lithium, sodium and potassium into the zinc oxide solution, wherein the molar ratio of the alkali metal hydroxide to the zinc oxide is 0.1: and 1, obtaining a zinc oxide film precursor solution. Spin-coating the zinc oxide film precursor solution on a dielectric layer at the rotation speed of 3000rpm for 30s, and annealing at 200 ℃ for 0.5h to obtain a nano zinc oxide film;
heating the tetrachloroauric acid solution to 100 ℃, and adding sodium citrate, wherein the molar ratio of the sodium citrate to the tetrachloroauric acid is 3.78: and 1, continuously reacting for 30 minutes, and finally cooling the solution to room temperature to obtain the nano gold particles. And (3) performing charged modification on the surface of the zinc oxide film, and adsorbing the prepared nano gold particles on the zinc oxide film through static electricity to obtain the nano gold particle-zinc oxide composite film.
And depositing gold on the composite film through a mask to form a source/drain electrode, wherein the length of a channel is 50 micrometers, the width of the channel is 1000 micrometers, and finally obtaining the transistor type formaldehyde sensor.
Example 2
Forming a gate electrode on the flexible PDMS substrate through a mask in a thermal evaporation mode by silver, and preparing a 30-nanometer-thick aluminum oxide dielectric layer on the gate electrode by an atomic layer deposition method;
dissolving zinc oxide in ammonium hydroxide and refrigerating for 5 hours, and adding deionized water and hydroxides of lithium, sodium and potassium into the zinc oxide solution, wherein the molar ratio of the alkali metal hydroxide to the zinc oxide is 0.01: and 1, obtaining a zinc oxide film precursor solution. Spin-coating the zinc oxide film precursor solution on a dielectric layer at the rotation speed of 3000rpm for 30s, and annealing at 200 ℃ for 0.5h to obtain a nano zinc oxide film;
mixing and stirring sodium citrate and silver nitrate at room temperature, wherein the molar ratio of the sodium citrate to the silver nitrate is 3.78: and 1, immediately adding sodium borohydride, continuously reacting for 20 minutes, and finally cooling the solution to room temperature to obtain the nano-silver particles. Performing charged modification on the surface of the zinc oxide film, and adsorbing the prepared nano silver particles on the zinc oxide film through static electricity to obtain a nano silver particle-zinc oxide composite film;
and depositing gold on the composite film through a mask to form a source/drain electrode, wherein the length of a channel is 50 micrometers, the width of the channel is 1000 micrometers, and finally obtaining the transistor type formaldehyde sensor.
Example 3
Forming a gate electrode on the flexible PDMS substrate through a mask in a thermal evaporation mode by silver, and preparing a 30-nanometer-thick aluminum oxide dielectric layer on the gate electrode by an atomic layer deposition method;
dissolving zinc oxide in ammonium hydroxide and refrigerating for 5 hours, and adding deionized water and hydroxides of lithium, sodium and potassium into the zinc oxide solution, wherein the molar ratio of the alkali metal hydroxide to the zinc oxide is 0.15: and 1, obtaining a zinc oxide film precursor solution. Spin-coating the zinc oxide film precursor solution on a dielectric layer at the rotation speed of 3000rpm for 30s, and annealing at 200 ℃ for 0.5h to obtain a nano zinc oxide film;
mixing and stirring sodium citrate and platinum quaternary salt at room temperature, wherein the molar ratio of the sodium citrate to the platinum quaternary salt is 3.78: and 1, immediately adding sodium borohydride, continuously reacting for 60 minutes, and finally cooling the solution to room temperature to obtain the nano platinum particles. Performing charged modification on the surface of the zinc oxide film, and adsorbing the prepared nano platinum particles on the zinc oxide film through static electricity to obtain a nano platinum particle-zinc oxide composite film;
and depositing gold on the composite film through a mask to form a source/drain electrode, wherein the length of a channel is 50 micrometers, the width of the channel is 1000 micrometers, and finally obtaining the transistor type formaldehyde sensor.
Example 4
The sensor prepared in the embodiment 1-3 is placed in a gas testing cavity, a probe is in contact with a grid electrode, a source electrode and a drain electrode of a device, source and drain current of a formaldehyde testing transistor device with a certain concentration is introduced for changing, and the result shows that the source and drain current change is obvious, namely the prepared transistor type formaldehyde sensor can specifically respond to formaldehyde gas.
Example 5
The bending resistance test is carried out on the sensors prepared in the embodiments 1-3, and the specific method comprises the following steps: and (3) constructing a sample stretching table by using a Linmot linear motor and a pneumatic vibration table to test the fatigue performance and the environmental stability of the flexible sensor. The electrical performance of the flexible sensor is tested after repeated compression and extension of the device through an order of magnitude of cycles. The result shows that the transistor-type formaldehyde sensor prepared by the invention still keeps good electrical properties after repeated compression and stretching, has excellent flexibility and can realize high mechanical property of devices.
In summary, according to the transistor-type formaldehyde sensor provided by the invention, the composite film is arranged on the dielectric layer, then the source electrode and the drain electrode are arranged on the composite film, and the zinc oxide film with the metal nanoparticles is adsorbed on the composite film, so that the composite film can change the carrier concentration, the surface state and the device transport capacity of the transistor, and the composite film has specific response to formaldehyde gas due to the modification of the metal nanoparticles, thereby realizing high selectivity and anti-interference of the device, and solving the problem that the formaldehyde sensor in the prior art is poor in stability and selectivity.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (4)
1. A transistor-type formaldehyde sensor is characterized by comprising a substrate, a gate electrode arranged on the substrate, a dielectric layer arranged on the gate electrode, a composite film arranged on the dielectric layer, and a source electrode and a drain electrode which are arranged on the composite film, wherein the composite film is a zinc oxide film adsorbed with metal nano-particles; in the composite film, metal nano particles are adsorbed on the zinc oxide film through static electricity; the zinc oxide film is made of zinc oxide modified by doping alkali metal elements; the metal nano-particles are one or more of gold nano-particles, silver nano-particles and platinum nano-particles; in the zinc oxide film, the molar ratio of alkali metal elements to zinc oxide is 0.01: 1-0.15: 1; the metal nano-particles modified on the zinc oxide film perform specific response to formaldehyde gas; the performance of the transistor-type formaldehyde sensor is adjusted through different combinations of the types of metal nano particles, the doping concentration of zinc oxide, the thickness of a dielectric layer and the thickness of a composite film.
2. The transistor-type formaldehyde sensor according to claim 1, wherein the substrate is a flexible substrate, the gate electrode is a metal gate electrode and the dielectric layer is an alumina dielectric layer.
3. A manufacturing method of a transistor-type formaldehyde sensor is characterized by comprising the following steps:
providing a substrate, and forming a gate electrode on the substrate;
depositing and preparing a dielectric layer on the gate electrode;
providing a zinc oxide solution, coating the zinc oxide solution on a dielectric layer, and annealing to form a zinc oxide film;
providing metal nano particles, performing charged modification on the zinc oxide film, and adsorbing the metal nano particles on the zinc oxide film through electrostatic action to obtain a composite film;
depositing on the composite film to form a source electrode and a drain electrode to obtain a transistor-type formaldehyde sensor;
before the step of coating the zinc oxide precursor solution on the gate electrode, the method further comprises the following steps:
adding an alkali metal hydroxide to the zinc oxide solution;
the step of performing charged modification on the zinc oxide film comprises the following steps:
soaking the zinc oxide film by using a 3-aminopropyltriethoxysilane solution, washing the soaked zinc oxide film by using toluene, and drying in a nitrogen atmosphere;
the metal nano-particles are one or more of gold nano-particles, silver nano-particles and platinum nano-particles; in the zinc oxide film, the molar ratio of alkali metal elements to zinc oxide is 0.01: 1-0.15: 1; the metal nano-particles modified on the zinc oxide film perform specific response to formaldehyde gas; the performance of the transistor-type formaldehyde sensor is adjusted through different combinations of the types of metal nano particles, the doping concentration of zinc oxide, the thickness of a dielectric layer and the thickness of a composite film.
4. The method of manufacturing the transistor-type formaldehyde sensor according to claim 3, wherein the dielectric layer is prepared by depositing aluminum oxide on the gate electrode by an atomic layer deposition method.
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| TWI740325B (en) * | 2018-12-28 | 2021-09-21 | 鴻海精密工業股份有限公司 | Gas sensor and method for making same |
| CN113640361A (en) * | 2021-07-19 | 2021-11-12 | 湘潭大学 | Grid sensitive FET gas sensor array for trace formaldehyde gas detection and preparation method thereof |
| CN113777147B (en) * | 2021-08-27 | 2022-11-18 | 同济大学 | Silver nanoparticle modified titanium carbide based field effect transistor gas sensor and preparation method and application thereof |
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