CN115287589B - Preparation method and application of gas sensor based on curled silicon nano film - Google Patents
Preparation method and application of gas sensor based on curled silicon nano film Download PDFInfo
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 13
- 239000010703 silicon Substances 0.000 title claims abstract description 13
- 239000002120 nanofilm Substances 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 67
- 239000007789 gas Substances 0.000 claims abstract description 35
- 238000000151 deposition Methods 0.000 claims abstract description 12
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000008021 deposition Effects 0.000 claims abstract description 10
- 238000005566 electron beam evaporation Methods 0.000 claims abstract description 8
- 239000011521 glass Substances 0.000 claims abstract description 5
- 239000010408 film Substances 0.000 claims description 34
- 238000001035 drying Methods 0.000 claims description 16
- 229920002120 photoresistant polymer Polymers 0.000 claims description 16
- 238000001259 photo etching Methods 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 7
- 239000010409 thin film Substances 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 238000004026 adhesive bonding Methods 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 238000007747 plating Methods 0.000 claims description 3
- 238000005096 rolling process Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000004528 spin coating Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000010894 electron beam technology Methods 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 5
- 230000035945 sensitivity Effects 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000010791 domestic waste Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- -1 such as In 2 O 3 Inorganic materials 0.000 description 1
- 238000000352 supercritical drying Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
- 108700012359 toxins Proteins 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/04—Coating on selected surface areas, e.g. using masks
- C23C14/042—Coating on selected surface areas, e.g. using masks using masks
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/26—Vacuum evaporation by resistance or inductive heating of the source
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
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- 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
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract
The invention belongs to the technical field of gas sensors, and relates to a preparation method and application of a gas sensor based on a curled silicon nano film, wherein an Si sensitive film grows on a glass substrate through an electron beam evaporation deposition technology, the Si sensitive film is curled through a proper method to form a film coil, then the film coil is manufactured into the gas sensor for detecting nitrogen dioxide gas, and the film with gas sensitivity is converted into a three-dimensional film coil device from a two-dimensional planar device, so that the specific surface area of the device is greatly improved, the film thickness is accurate and controllable, the film is suitable for preparing the gas sensor in batches, and the film coil has important value for development of gas sensitive materials and application of the gas sensor.
Description
Technical field:
the invention belongs to the technical field of gas sensors, and relates to a preparation method and application of a gas sensor based on a curled silicon nano film.
The background technology is as follows:
nitrogen dioxide is an important inorganic chemical raw material, and is also a common toxic industrial and domestic waste gas, such as exhaust of motor vehicles and exhaust of boilers, and the like, and the environmental effects brought by the nitrogen dioxide are various, including: the effects on competition and compositional changes between wetland and terrestrial plant species, reduced atmospheric visibility, acidification of surface water, eutrophication, and increased levels of toxins in the water body that are harmful to fish and other aquatic organisms. Therefore, the method has important application value for detecting the nitrogen dioxide.
The gas sensor has the advantages of small volume, high sensitivity, good stability, simple structure and the like, and is widely applied to the detection of high-hazard gas. Currently, gas sensor materials for nitrogen dioxide are mainly semiconductor metal oxides, such as In 2 O 3 、SnO 2 、Fe 2 O 3 For example, in order to further improve the detection sensitivity of the gas sensor, researchers have used noble metals such as Au, pt, etc. as sensitizers to enhance the surface sensitivity of metal oxide gas-sensitive materials.
However, since the thin film type gas sensor needs to be manufactured based on a substrate, the effective area for gas detection is necessarily limited, and there is an upper limit to the way to improve the performance by the material modification method. And as the demands of integrated circuits for device miniaturization become higher, the maximum utilization of the area on the wafer is also becoming a goal of researchers. Thus, there is an urgent need to develop a new structure of a sensitive thin film device to solve the above problems and achieve the corresponding objective.
The invention comprises the following steps:
the invention aims to overcome the defects of the prior art, and designs and provides a large-scale preparation method and application of a gas sensor based on a curled silicon nano film.
In order to achieve the above object, the present invention provides a method for growing a Si sensitive film on a glass substrate by electron beam evaporation deposition technique, and curling it by a proper method to form a film coil, and then forming a gas sensor for nitrogen dioxide gas detection, comprising the steps of:
(1) Taking a round glass substrate with the diameter of 2 inches and the thickness of 0.55mm as a substrate, and spin-coating a layer of photoresist on the surface of the substrate by using a spin coater;
(2) Photoetching the substrate obtained in the step (1) to etch out the sacrificial layer pattern;
(3) Evaporating a layer of Ge film on the substrate obtained in the step (2) by using an electron beam evaporation deposition mode, removing the photoresist, and oxidizing the film to obtain the substrate with the GeO sacrificial layer film;
(4) Repeating the gluing of the step (1) and the photoetching of the step (2) on the substrate with the GeO sacrificial layer film obtained in the step (3) to etch an electrode pattern;
(5) Evaporating a Cr/Au film on the substrate obtained in the step (4) by using a resistance thermal evaporation deposition mode to serve as a device electrode;
(6) Repeatedly gluing and photoetching the substrate obtained in the step (5) to etch a curled layer pattern;
(7) Evaporating a layer of Si film on the substrate obtained in the step (6) by using an electron beam evaporation deposition mode;
(8) Soaking the substrate obtained in the step (7) in 30% of H 2 O 2 Removing the GeO sacrificial layer in the solution for 12 hours, and rolling the Si film to form a coiled pipe;
(9) And (3) rapidly transferring the substrate obtained in the step (8) into a supercritical dryer, and performing supercritical drying on the substrate by using ethanol to obtain the gas sensor based on the curled silicon nano film.
The gas sensor based on the curled silicon nano film prepared by the invention can be directly used for detecting nitrogen dioxide.
Compared with the existing planar film sensor, the invention converts the film with gas sensitivity from a two-dimensional planar device to a three-dimensional film coiled tube device, greatly improves the specific surface area of the device, has accurate and controllable film thickness, is suitable for preparing the gas sensor in batches, and has important value for development of gas sensitive materials and application of the gas sensor.
Description of the drawings:
fig. 1 is a design drawing of a coating pattern of a Si thin film coil prepared in the embodiment of the present invention.
FIG. 2 is an optical micrograph of a Si film coil prepared according to an embodiment of the present invention.
FIG. 3 is a graph showing the gas-sensitive response recovery curve of a Si film coil prepared in the example of the present invention at 300℃for 20ppm nitrogen dioxide.
The specific embodiment is as follows:
the following is further illustrated by way of specific examples and with reference to the accompanying drawings.
Examples:
the specific process for preparing the gas sensor based on the curled silicon nano film in the embodiment is as follows:
(1) Taking a round glass substrate with the diameter of 2 inches and the thickness of 0.55mm as a substrate, and spin-coating a layer of photoresist on the surface of the substrate by using a 650Mz23N photoresist machine of Michao technology Co., ltd, wherein the photoresist model is ROL-7133 negative photoresist of Siebolding company, the low rotating speed of the photoresist machine is 600rpm, and the rotating time is 6 seconds; the high rotation speed is 2000rpm, the rotation time is 20 seconds, and then the substrate coated with the photoresist is placed on an electric hot plate and is pre-baked for 90 seconds at 110 ℃;
(2) Photoetching an array formed by rectangular patterns with the length of 320 mu m and the width of 300 mu m by using a URE-200/35 ultraviolet photoetching machine of a institute of photoelectric technology of Chinese academy of sciences, as shown in figure 1, placing a photoetched substrate on an electric plate, post-baking for 120s at 110 ℃, immersing in a 1% NaOH solution for developing for 45s, washing with deionized water, and drying by nitrogen flow to obtain the substrate etched with the sacrificial layer pattern;
(3) Electron beam evaporation deposition of Ge metal films was performed using AUTO500 e-beam plating system from HHV, uk: fixing the substrate etched with the sacrificial layer pattern on a sample holder to45nmGE metal is deposited, and then the deposited substrate is immersed into proper amount of acetone to dissolve photoresist, so that an array of rectangular Ge films is obtained on the substrate;
(4) O was applied to a substrate using a PDC-2G-2 plasma cleaning machine from Welch nanosystem, germany 2 Plasma cleaning for 5 minutes, putting the substrate into a baking oven at 150 ℃ to oxidize for 18 hours, and obtaining a GeO sacrificial layer film on the substrate;
(5) Repeating the gluing and pre-drying processes in the step (1) on the substrate obtained in the step (4), photoetching electrode patterns on the substrate by using the same method in the step (2), and repeating the post-drying, developing, cleaning and drying steps in the step (2) on the substrate after photoetching;
(6) Resistive evaporation deposition of Au thin films was performed using VZZ-300 high vacuum resistive evaporation coating equipment from Beijing micro-nano vacuum company: fixing the substrate obtained in the step (5) on a sample holder toThe method comprises the steps of (1) depositing 10nmCr metal and 40nmAu metal at a rate, immersing a deposited substrate in a proper amount of acetone to dissolve photoresist, and obtaining an array of film electrodes;
(7) Repeating the gluing and pre-baking processes in the step (1) on the substrate obtained in the step (6), and photoetching an array formed by rectangular patterns with the width of 300 mu m and the width of 320 mu m on the substrate by using the same method in the step (2). Repeating the steps of post-baking, developing, cleaning and drying in the step (2) on the substrate after photoetching;
(8) Electron beam evaporation deposition of Si thin films using AUTO500 e-beam plating system from HHV, uk: fixing the substrate obtained in the step (7) on a sample holder toIs deposited at a rate of 40nmSi. Immersing the deposited substrate into proper amount of acetone to dissolve photoresist, thus obtaining an array of rectangular Si films;
(9) Placing the substrate obtained in the step (8) into 30% H 2 O 2 Soaking in the solution for 12 hours, removing the GeO sacrificial layer film, rolling the Si film to form a curled film, rapidly transferring the substrate into a SAMDRI-PVT-3D supercritical dryer of Tousims company in the U.S., and drying to obtain the silicon curled film gas sensor after the drying process is finished, wherein the optical microscope photo is shown in figure 2.
This example uses the prepared Si-crimped silicon crimped film gas sensor for detecting nitrogen dioxide, whose response-recovery characteristics to nitrogen dioxide at a concentration of 20ppm are shown in fig. 3.
Claims (2)
1. The preparation method of the gas sensor based on the curled silicon nano film is characterized by comprising the following steps of:
(1) Taking a round glass substrate with the diameter of 2 inches and the thickness of 0.55mm as a substrate, and spin-coating a layer of photoresist on the surface of the substrate by using a spin coater, wherein the spin coater has the low rotating speed of 600rpm and the rotating time of 6 seconds; the high rotation speed is 2000rpm, the rotation time is 20 seconds, and then the substrate coated with the photoresist is placed on an electric hot plate and is pre-baked for 90 seconds at 110 ℃;
(2) Photoetching an array formed by rectangular patterns with the length of 320 microns and the width of 300 microns by using an ultraviolet photoetching machine, placing the photoetched substrate on an electric plate, post-baking for 120s at the temperature of 110 ℃, immersing the photoetched substrate into a 1% NaOH solution, developing for 45s, cleaning the photoetched substrate by using deionized water, and drying the photoetched substrate by using nitrogen flow to obtain a substrate etched with a sacrificial layer pattern;
(3) Electron beam evaporation deposition of the Ge metal film is carried out by using an electron beam coating system: fixing the substrate etched with the sacrificial layer pattern on a sample holder to45nmGE metal is deposited at the rate, and then the deposited substrate is immersed into acetone to dissolve photoresist, so that an array of rectangular Ge films is obtained on the substrate;
(4) O for substrate using plasma cleaning machine 2 Plasma cleaning for 5 minutes, putting the substrate into a baking oven at 150 ℃ to oxidize for 18 hours, and obtaining a GeO sacrificial layer film on the substrate;
(5) Repeating the gluing and pre-drying processes in the step (1) on the substrate obtained in the step (4), photoetching electrode patterns on the substrate by using the same method in the step (2), and repeating the post-drying, developing, cleaning and drying steps in the step (2) on the substrate after photoetching;
(6) And (3) performing resistance evaporation deposition of the Au thin film by using high-vacuum resistance evaporation coating equipment: fixing the substrate obtained in the step (5) on a sample holder toThe deposited substrate is immersed into acetone to dissolve photoresist, and an array of film electrodes is obtained;
(7) Repeating the gluing and pre-drying processes in the step (1) on the substrate obtained in the step (6), photoetching an array formed by rectangular patterns with the width of 300 mu m and the width of 320 mu m on the substrate by using the same method in the step (2), and repeating the post-drying, developing, cleaning and drying steps in the step (2) on the substrate after photoetching;
(8) Electron beam evaporation deposition of Si thin films using an electron beam plating system: fixing the substrate obtained in the step (7) on a sample holder toThe deposited substrate is immersed into proper amount of acetone to dissolve photoresist, and an array of rectangular Si films is obtained;
(9) Placing the substrate obtained in the step (8) into 30% H 2 O 2 Soaking in the solution for 12 hours, removing the GeO sacrificial layer film, rolling the Si film to form a curled film, then rapidly transferring the substrate into a supercritical dryer for drying, and obtaining the silicon curled film gas sensor after drying.
2. Use of a gas sensor based on a curled silicon nanomembrane prepared according to the method of claim 1, directly for the detection of nitrogen dioxide.
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