CN111847376A - Humidity sensor manufacturing method - Google Patents
Humidity sensor manufacturing method Download PDFInfo
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- CN111847376A CN111847376A CN202010633567.8A CN202010633567A CN111847376A CN 111847376 A CN111847376 A CN 111847376A CN 202010633567 A CN202010633567 A CN 202010633567A CN 111847376 A CN111847376 A CN 111847376A
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- graphene oxide
- humidity sensor
- dispersion liquid
- sensor according
- oxide dispersion
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- 238000004519 manufacturing process Methods 0.000 title claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 86
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 85
- 239000006185 dispersion Substances 0.000 claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000007710 freezing Methods 0.000 claims abstract description 13
- 230000008014 freezing Effects 0.000 claims abstract description 12
- 239000003990 capacitor Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000000151 deposition Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- 239000010408 film Substances 0.000 claims description 38
- 238000000034 method Methods 0.000 claims description 19
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000005530 etching Methods 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 9
- 238000004528 spin coating Methods 0.000 claims description 6
- 238000001548 drop coating Methods 0.000 claims description 4
- 238000010894 electron beam technology Methods 0.000 claims description 4
- 238000010884 ion-beam technique Methods 0.000 claims description 3
- 238000010329 laser etching Methods 0.000 claims description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000010409 thin film Substances 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 229920002120 photoresistant polymer Polymers 0.000 description 2
- 238000001020 plasma etching Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000004026 adhesive bonding Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B7/00—Microstructural systems; Auxiliary parts of microstructural devices or systems
- B81B7/02—Microstructural systems; Auxiliary parts of microstructural devices or systems containing distinct electrical or optical devices of particular relevance for their function, e.g. microelectro-mechanical systems [MEMS]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00349—Creating layers of material on a substrate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B2201/00—Specific applications of microelectromechanical systems
- B81B2201/02—Sensors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B2201/00—Specific applications of microelectromechanical systems
- B81B2201/02—Sensors
- B81B2201/0292—Sensors not provided for in B81B2201/0207 - B81B2201/0285
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C2201/00—Manufacture or treatment of microstructural devices or systems
- B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
- B81C2201/0101—Shaping material; Structuring the bulk substrate or layers on the substrate; Film patterning
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C2201/00—Manufacture or treatment of microstructural devices or systems
- B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
- B81C2201/0174—Manufacture or treatment of microstructural devices or systems in or on a substrate for making multi-layered devices, film deposition or growing
Abstract
The invention discloses a humidity sensor preparation method, which comprises the following steps: s01: providing a capacitor structure chip with an electrode and graphene oxide dispersion liquid; s02: depositing the graphene oxide dispersion onto the capacitor structure; s03: quickly freezing to solidify the graphene oxide dispersion liquid into a solid; s04: and reducing the pressure to sublimate the solvent in the graphene oxide dispersion liquid solid, and forming a three-dimensional spongy graphene oxide medium film between the electrodes. According to the invention, the contact area of the graphene oxide film and water molecules can be effectively increased, the adsorption capacity and the absorption effect of the graphene oxide film on the water molecules are greatly improved, the sensitivity of the graphene oxide capacitive humidity sensor is improved, and thus the performance of the graphene oxide humidity sensor is obviously improved.
Description
Technical Field
The invention relates to the technical field of sensors, in particular to a method for preparing a humidity sensor based on graphene oxide.
Background
The humidity sensor plays an important role in the fields of industry, agriculture, environmental detection and the like, and the core of the humidity sensor is to apply a sensitive material capable of converting humidity into other testable signals.
The humidity-sensitive material mainly comprises semiconductor oxide, high-molecular polymer and related composite materials, but a sensor using the humidity-sensitive material has the problems of small detection range, low sensitivity and the like.
Graphene oxide, as a graphene derivative, has a large specific surface area and rich oxygen-containing functional groups, and the oxygen-containing functional groups can be connected with water molecules through hydrogen bonds. Therefore, the graphene oxide is very suitable to be used as a sensitive material of a humidity sensor.
The capacitive humidity sensor mainly comprises a capacitance structure consisting of interdigital electrodes and a dielectric layer consisting of sensitive materials such as a graphene oxide film. Common methods for depositing graphene oxide on the interdigital electrode are as follows: spray coating, spin coating, drop coating, and ink jet printing.
However, the graphene oxide deposited by the above method has only the portion of the outermost surface of the film contacting with the outside, which effectively absorbs water molecules. And the graphene oxide in most films cannot absorb external water molecules, so that the graphene oxide film does not play a role of a sensitive material, the sensitivity of the humidity sensor is not high enough, and the waste of the graphene oxide material is also caused.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a humidity sensor preparation method.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a humidity sensor preparation method comprises the following steps:
s01: providing a capacitor structure chip with an electrode and graphene oxide dispersion liquid;
s02: depositing the graphene oxide dispersion onto the capacitor structure;
s03: quickly freezing to solidify the graphene oxide dispersion liquid into a solid;
s04: and reducing the pressure to sublimate the solvent in the graphene oxide dispersion liquid solid, and forming a three-dimensional spongy graphene oxide medium film between the electrodes.
Further, the method also includes step S05: and forming a downward groove on the surface of the graphene oxide dielectric film between the electrodes.
Further, the groove is formed by laser etching, ion beam etching or electron beam etching.
Further, in step S01, the mass fraction of graphene oxide in the graphene oxide dispersion liquid is 0.1% to 10%.
Further, the solvent is a mixture of water and an organic solvent, wherein the volume fraction of the water is 50-80%.
Further, the organic solvent includes one or more of ethanol, propanol, and isopropanol.
Further, in step S02, the graphene oxide dispersion is deposited by spin coating or drop coating.
Further, in step S02, the deposited graphene oxide dispersion liquid has a height of 1-500 μm.
Further, in step S03, the freezing temperature during quick freezing is-20 to-80 ℃; in step S04, the pressure is reduced to 500Pa or less when the pressure is reduced.
Further, in step S05, the occupation density of the trenches on the graphene oxide dielectric thin film is 20% to 80%.
The graphene oxide sensitive material film is loose and porous, the surface of the graphene oxide sensitive material film is uneven, the contact area of the graphene oxide film and water molecules can be effectively increased, the adsorption capacity and the absorption effect of the graphene oxide film on the water molecules are greatly improved, the sensitivity of the graphene oxide capacitive humidity sensor is improved, and therefore the performance of the graphene oxide humidity sensor is remarkably improved.
Drawings
FIG. 1 is a flow chart of a method for manufacturing a humidity sensor according to a preferred embodiment of the present invention.
Fig. 2-5 are schematic views of a process for fabricating a humidity sensor according to the method of fig. 1.
Detailed Description
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
In the following detailed description of the embodiments of the present invention, in order to clearly illustrate the structure of the present invention and to facilitate explanation, the structure shown in the drawings is not drawn to a general scale and is partially enlarged, deformed and simplified, so that the present invention should not be construed as limited thereto.
In the following description of the present invention, please refer to fig. 1, in which fig. 1 is a flowchart illustrating a method for manufacturing a humidity sensor according to a preferred embodiment of the present invention. As shown in fig. 1, a method for manufacturing a humidity sensor according to the present invention includes the following steps:
s01: and providing a capacitor structure chip with an electrode and a graphene oxide dispersion liquid.
Please refer to fig. 2. And finishing the structure required by the MEMS process on a chip for manufacturing the humidity sensor, and finishing the interdigital electrode in the capacitance structure of the humidity sensor. And depositing a graphene oxide film on the interdigital electrode as a sensitive material. The graphene oxide contains a large number of oxygen-containing groups, can adsorb water molecules, and has excellent humidity sensitivity.
S02: depositing the graphene oxide dispersion onto the capacitor structure.
Please refer to fig. 2. Preparing a graphene oxide dispersion liquid with a certain concentration. Mixing graphene oxide powder in a solvent to form a dispersion liquid, wherein the mass fraction of graphene oxide in the dispersion liquid is 0.1-10%.
The graphene oxide dispersion liquid with different concentrations can form three-dimensional spongy graphene oxide films with different porosities in the subsequent steps. The main components of the solvent in the dispersion liquid are water and an organic solvent, the volume fraction of the water is 50-80%, and the balance is the organic solvent. The organic solvent may specifically include one or more of ethanol, propanol, and isopropanol.
For example, the organic solvent may be composed of 60% by volume of deionized water, 20% by volume of ethanol, and 10% by volume of isopropyl alcohol. The organic solvent can also be composed of deionized water with volume fraction of 70% and isopropanol with volume fraction of 30%.
Then, the graphene oxide dispersion liquid can be deposited on the capacitor structure of the sensor by spin coating, drop coating and the like, and a graphene oxide water film is formed by using the surface tension of the liquid. Wherein the water film height is 1-500 μm.
S03: and (4) quick-freezing to solidify the graphene oxide dispersion liquid into a solid.
And (2) placing the interdigital electrode structure (chip) covered with the graphene oxide dispersion liquid into a vacuum freeze dryer (cavity) to quickly solidify the graphene oxide dispersion liquid into a solid, wherein the freezing temperature is-20 ℃ to-80 ℃.
S04: and (3) decompressing to sublimate the solvent in the graphene oxide dispersion liquid solid, and forming a three-dimensional spongy graphene oxide medium film between the electrodes.
The air pressure in the vacuum freeze dryer cavity is reduced, so that the solvent in the frozen graphene oxide film is sublimated to form a three-dimensional spongy graphene oxide film, as shown in fig. 3. Wherein, the air pressure of the cavity is reduced to be below 500 Pa.
Further, step S05 may also be included: and forming a downward groove on the surface of the graphene oxide dielectric film between the electrodes.
And etching the formed three-dimensional spongy graphene oxide film, and forming a groove structure on the surface of the graphene oxide film so as to further increase the contact area.
Wherein, the etching may be laser etching or electron beam etching, as shown in fig. 4. The etching may also be performed by photolithography in which a photoresist mask is formed on the surface of the graphene oxide film, as shown in fig. 5, and ion beam etching (plasma etching). Wherein, after etching, the occupation density of the formed groove on the whole film of the graphene oxide medium is 20-80% (area ratio).
Example one
A humidity sensor chip is provided on which the MEMS process has been completed and which includes interdigitated electrodes. Weighing 200mg of graphene oxide powder, weighing 60ml of deionized water, 30ml of ethanol and 10ml of isopropanol, fully mixing the above liquids, adding the graphene oxide powder, and fully stirring to form 2mg/ml graphene oxide dispersion liquid. And depositing the graphene oxide dispersion liquid on a capacitor structure of the sensor by using a dripping mode, and forming a graphene oxide water film by using the surface tension of the liquid, wherein the height of the water film is 20 mu m. And (3) putting the chip into a vacuum freeze dryer, wherein the freezing temperature is-60 ℃, so that the graphene oxide water film is rapidly solidified into a solid. And reducing the air pressure of the freezing cavity to 200Pa, and sublimating the solvent in the frozen graphene oxide film to form the three-dimensional spongy graphene oxide film. And etching the formed three-dimensional spongy graphene oxide film by using laser or electron beams to form a surface pit (groove) structure, wherein the density of the formed pits is 50%.
Example two
A humidity sensor chip is provided on which the MEMS process has been completed and which includes interdigitated electrodes. Weighing 800mg of graphene oxide powder, weighing 80ml of deionized water, 10ml of ethanol and 10ml of isopropanol, fully mixing the above liquids, adding the graphene oxide powder, and fully stirring to form 8mg/ml graphene oxide dispersion liquid. In order to facilitate the implementation of the subsequent gluing process, the graphene oxide dispersion liquid of the step needs to have higher concentration. And depositing the graphene oxide dispersion liquid on a capacitor structure of the sensor by using a spin coating mode, wherein the spin coating speed is 200rpm, and a graphene oxide water film is formed by using the surface tension of the liquid, and the height of the water film is 10 mu m. And (3) putting the chip into a vacuum freeze dryer, wherein the freezing temperature is-80 ℃, so that the graphene oxide water film is rapidly solidified into a solid. And reducing the air pressure of the freezing cavity to 400Pa, so that the solvent in the frozen graphene oxide film is sublimated to form the three-dimensional spongy graphene oxide film. And (3) coating and photoetching are carried out on the graphene oxide film, the formed three-dimensional spongy graphene oxide film is etched by utilizing plasma etching to form a surface pit (groove) structure, and the photoresist is removed at high temperature to complete the etching of the porous graphene oxide film. The pit density was 50%.
The above description is only for the preferred embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, so that all the equivalent structural changes made by using the contents of the description and the drawings of the present invention should be included in the scope of the present invention.
Claims (10)
1. A humidity sensor preparation method is characterized by comprising the following steps:
s01: providing a capacitor structure chip with an electrode and graphene oxide dispersion liquid;
s02: depositing the graphene oxide dispersion onto the capacitor structure;
s03: quickly freezing to solidify the graphene oxide dispersion liquid into a solid;
s04: and reducing the pressure to sublimate the solvent in the graphene oxide dispersion liquid solid, and forming a three-dimensional spongy graphene oxide medium film between the electrodes.
2. The method for manufacturing a humidity sensor according to claim 1, further comprising the step of S05: and forming a downward groove on the surface of the graphene oxide dielectric film between the electrodes.
3. The method of manufacturing a humidity sensor according to claim 2, wherein the trench is formed by laser etching, ion beam etching or electron beam etching.
4. The method for manufacturing a humidity sensor according to claim 1, wherein in step S01, the mass fraction of graphene oxide in the graphene oxide dispersion liquid is 0.1% to 10%.
5. The method of manufacturing a humidity sensor according to claim 1, wherein the solvent is a mixture of water and an organic solvent, wherein the volume fraction of water is 50% to 80%.
6. The method of manufacturing a humidity sensor according to claim 5, wherein the organic solvent comprises one or more of ethanol, propanol and isopropanol.
7. The method for preparing a humidity sensor according to claim 1, wherein in step S02, the graphene oxide dispersion is deposited by spin coating or drop coating.
8. The method for preparing a humidity sensor according to claim 1, wherein in step S02, the deposited graphene oxide dispersion liquid has a height of 1-500 μm.
9. The method for preparing a humidity sensor according to claim 1, wherein in step S03, the freezing temperature during quick freezing is-20 to-80 ℃; in step S04, the pressure is reduced to 500Pa or less when the pressure is reduced.
10. The method for preparing a humidity sensor according to claim 2, wherein in step S05, the occupation density of the trenches on the graphene oxide dielectric thin film is 20% to 80%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010633567.8A CN111847376A (en) | 2020-07-02 | 2020-07-02 | Humidity sensor manufacturing method |
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| CN202010633567.8A CN111847376A (en) | 2020-07-02 | 2020-07-02 | Humidity sensor manufacturing method |
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Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06128721A (en) * | 1992-10-19 | 1994-05-10 | Mitsubishi Electric Corp | Formation of sensitive thin film for gaseous nitrogen oxide sensor |
| KR20040092110A (en) * | 2003-04-25 | 2004-11-03 | 엘지전자 주식회사 | Method for manufacturing semiconductor gas sensor |
| CN201149495Y (en) * | 2008-01-04 | 2008-11-12 | 潘劲松 | Sensing device for measuring relative humiture |
| KR20140019642A (en) * | 2012-08-07 | 2014-02-17 | 정은아 | Manufacturing method of graphene oxide sponge using freezing drying method |
| US20150010825A1 (en) * | 2013-07-05 | 2015-01-08 | Graduate School At Shenzhen, Tsinghua University | Graphene composite material, methods for making graphene and graphene composite material, and lithium sulfur battery using the same |
| CN105806891A (en) * | 2014-12-31 | 2016-07-27 | 青岛中科软件股份有限公司 | Corrosion-resistant soil humidity sensor |
| CN106442629A (en) * | 2016-09-09 | 2017-02-22 | 浙江理工大学 | Preparation method of RGO (reduced graphene oxide) thin film moisture-sensitive sensor |
| WO2018018689A1 (en) * | 2016-07-29 | 2018-02-01 | 江苏大学 | Super-hydrophilic bionic sensor for moisture content of matrices and preparation method therefor |
| CN108083264A (en) * | 2018-02-26 | 2018-05-29 | 盐城科迈特新材料有限公司 | A kind of preparation method of three-dimensional grapheme |
| CN108414583A (en) * | 2018-03-05 | 2018-08-17 | 华中科技大学 | Humidity sensor and the improvement based on graphene oxide humidity sensor and preparation |
| CN109870489A (en) * | 2019-02-28 | 2019-06-11 | 上海集成电路研发中心有限公司 | A method of preparing graphene oxide in humidity sensor |
| KR20190126570A (en) * | 2018-05-02 | 2019-11-12 | 인하대학교 산학협력단 | Reduced graphene oxide/carbon nanotube composite material having a sponge structure and method for manufacturing the same |
-
2020
- 2020-07-02 CN CN202010633567.8A patent/CN111847376A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06128721A (en) * | 1992-10-19 | 1994-05-10 | Mitsubishi Electric Corp | Formation of sensitive thin film for gaseous nitrogen oxide sensor |
| KR20040092110A (en) * | 2003-04-25 | 2004-11-03 | 엘지전자 주식회사 | Method for manufacturing semiconductor gas sensor |
| CN201149495Y (en) * | 2008-01-04 | 2008-11-12 | 潘劲松 | Sensing device for measuring relative humiture |
| KR20140019642A (en) * | 2012-08-07 | 2014-02-17 | 정은아 | Manufacturing method of graphene oxide sponge using freezing drying method |
| US20150010825A1 (en) * | 2013-07-05 | 2015-01-08 | Graduate School At Shenzhen, Tsinghua University | Graphene composite material, methods for making graphene and graphene composite material, and lithium sulfur battery using the same |
| CN105806891A (en) * | 2014-12-31 | 2016-07-27 | 青岛中科软件股份有限公司 | Corrosion-resistant soil humidity sensor |
| WO2018018689A1 (en) * | 2016-07-29 | 2018-02-01 | 江苏大学 | Super-hydrophilic bionic sensor for moisture content of matrices and preparation method therefor |
| CN106442629A (en) * | 2016-09-09 | 2017-02-22 | 浙江理工大学 | Preparation method of RGO (reduced graphene oxide) thin film moisture-sensitive sensor |
| CN108083264A (en) * | 2018-02-26 | 2018-05-29 | 盐城科迈特新材料有限公司 | A kind of preparation method of three-dimensional grapheme |
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