CN114280108A - Aluminum-based porous alumina film humidity-sensitive sensor and preparation method thereof - Google Patents
Aluminum-based porous alumina film humidity-sensitive sensor and preparation method thereof Download PDFInfo
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 59
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 29
- 230000003647 oxidation Effects 0.000 claims abstract description 24
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 24
- 230000008569 process Effects 0.000 claims abstract description 19
- 238000000576 coating method Methods 0.000 claims abstract description 7
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- 230000008020 evaporation Effects 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 11
- 239000012528 membrane Substances 0.000 claims description 9
- 238000003466 welding Methods 0.000 claims description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- NGPGDYLVALNKEG-UHFFFAOYSA-N azanium;azane;2,3,4-trihydroxy-4-oxobutanoate Chemical compound [NH4+].[NH4+].[O-]C(=O)C(O)C(O)C([O-])=O NGPGDYLVALNKEG-UHFFFAOYSA-N 0.000 claims description 3
- CHKVPAROMQMJNQ-UHFFFAOYSA-M potassium bisulfate Chemical compound [K+].OS([O-])(=O)=O CHKVPAROMQMJNQ-UHFFFAOYSA-M 0.000 claims description 3
- 229910000343 potassium bisulfate Inorganic materials 0.000 claims description 3
- 239000010408 film Substances 0.000 claims 13
- 239000010409 thin film Substances 0.000 claims 4
- 239000004411 aluminium Substances 0.000 claims 2
- 230000004044 response Effects 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 6
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- 238000005259 measurement Methods 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical compound [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
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- 229920001721 polyimide Polymers 0.000 description 2
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
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- 239000000919 ceramic Substances 0.000 description 1
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- 238000009833 condensation Methods 0.000 description 1
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- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
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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
- 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
- G01N27/121—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 for determining moisture content, e.g. humidity, of the fluid
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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
- G01N27/22—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance
- G01N27/223—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance for determining moisture content, e.g. humidity
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Abstract
The invention relates to an aluminum-based porous alumina film humidity-sensitive sensor and a preparation method thereof, belonging to the technical field of sensors, wherein a main body of the sensor comprises an aluminum substrate, a porous alumina film growing on the surface of the aluminum substrate and a top electrode on the surface of the alumina film, and the preparation process of the sensor comprises the following steps: a primary oxidation process, a secondary oxidation process, an evaporation coating process and an electrode wire leading-out process. The porous alumina film prepared by the invention has low process power consumption, the surface of the film has larger aperture, and the film has higher response speed and recovery speed.
Description
Technical Field
The invention belongs to the technical field of sensors, and particularly relates to an aluminum-based porous alumina film humidity-sensitive sensor and a preparation method thereof.
Background
The humidity-sensitive sensor is widely researched and applied all the time, humidity can directly affect industrial production and daily life of human beings, and improvement of performance requirements of the humidity-sensitive sensor such as response speed, sensitivity and long-term stability is always the key point in the research direction of humidity measurement.
The measurement of humidity is mainly performed by a hair hygrometer measurement method, a dew point meter measurement method, a resistance-capacitance sensor measurement method, and the like.
The hair hygrometer uses specially processed hair as a humidity sensitive component, pores of the processed hair have good moisture absorption performance in a humidity environment, and the relative humidity of the measured air environment can be obtained through measurement and recording of the length and the shape of the hair because the change of the relative humidity in the air can affect the length and the shape of the hair.
The dew point instrument measurement method can directly measure the humidity of the air in the environment through a dew point instrument. The dew point temperature of the environmental gas can be measured by utilizing the characteristic that the dew point temperature of the water vapor in the environment is related to the humidity of the gas in the environment and the temperature values of the air with different humidity during dew formation are different, so that the humidity value corresponding to the measured gas can be obtained.
The resistance-capacitance method for measuring humidity is to place the prepared resistance-capacitance component in a humidity environment, and because the humidity-sensitive component has an adsorption effect on water molecules, and the electrical parameters of water and the electrical parameters of the surface material of the component are different, after the pores on the surface of the component adsorb the water molecules, the resistance and the capacitance of the humidity-sensitive component can be changed, and different resistance-capacitance values can be generated for different humidities.
Because the requirement of hair hygrometer to the environment is higher, can exert an influence to the measuring result under the great condition of air pollution, some air dust can directly lead to the hair hygrometer to obtain great error result moreover, can destroy the hair structure of hygrometer even, therefore need carry out routine maintenance in the normal use of hair hygrometer.
The dew point instrument is large in size, poor in portability and generally not suitable for measuring the humidity value of a cavity with small size, and the equipment is difficult to manufacture, so that the production cost is high and the price is high. In addition, the dew point meter needs to reduce the temperature to measure the dew point temperature of the ambient air, and the equipment needs a long time to reach the low temperature condition, so the dew point meter is not suitable for monitoring the ambient humidity in real time.
The humidity sensor manufactured by the resistance-capacitance method has small volume, is convenient to carry, has lower production cost, and can be suitable for some closed-cavity pipelines with small volume, so the resistance-capacitance method is a method with wider application range for humidity sensing at present.
Materials commonly used for measuring humidity by a resistance-capacitance method include polyimide materials and porous Al2O3 humidity sensitive ceramic films.
The polyimide material is used as a humidity-sensitive material, and the humidity-sensitive film absorbs a large amount of water molecules under a high-humidity environment and then generates a condensation phenomenon in the pores of the film, so that the humidity hysteresis is high and the stability is poor. The improvement of the moisture-sensitive property thereof is still required to be further studied due to the limitation of the material itself.
The porous Al2O3 humidity sensor has wide humidity sensing range, small device size, simple structure, low process power consumption and low production cost, and is suitable for various environments. The porous alumina film preparation technology can realize larger pore depth, which can obviously improve the specific surface area of the surface of the alumina film, and in addition, the porous alumina belongs to inorganic materials, has good insulating property and high temperature resistance, and can work at relatively higher environmental temperature, so that the porous Al2O3 humidity-sensitive sensor in the field of humidity-sensitive sensors is widely applied at present.
Disclosure of Invention
The invention aims to solve the technical problem of the product prepared by the prior art and provides an aluminum-based porous alumina film humidity-sensitive sensor and a preparation method thereof.
In order to solve the technical problem, the invention provides an aluminum-based porous alumina film humidity-sensitive sensor which comprises a substrate and a humidity-sensitive film, wherein the humidity-sensitive film covers the upper surface of the substrate, a bottom electrode lead is arranged on one side of the substrate and is fixedly connected to the substrate through screws, a top electrode is arranged in the center of the upper surface of the humidity-sensitive film, a top electrode lead is arranged on the top electrode, and the top electrode lead are fixedly connected through welding.
Preferably, the material of the humidity sensitive film is an alumina film.
Preferably, the substrate is an aluminum substrate.
Preferably, the top electrode is a gold electrode or an aluminum electrode.
A preparation method of an aluminum-based porous alumina film humidity-sensitive sensor comprises the following steps:
cleaning a high-purity aluminum sheet and then carrying out a primary oxidation process to prepare a porous aluminum oxide film;
cleaning the porous alumina film treated by the primary oxidation process and then carrying out a secondary oxidation process;
cleaning the porous alumina film treated by the secondary oxidation process, and then carrying out evaporation coating to prepare a top electrode on the surface of the porous alumina film;
after cleaning the porous alumina film humidity-sensitive sensor with the top electrode prepared by evaporation coating, perforating the substrate, and then fixing and leading out a bottom electrode wire by adopting a screw;
and welding the top electrode of the porous alumina film humidity-sensitive sensor after the bottom electrode wire is led out, and then leading out the top electrode wire.
Preferably, the primary oxidation process of the aluminum-based porous alumina film humidity-sensitive sensor is as follows: putting aluminum sheets into the molten KHSO4, and carrying out primary oxidation in the range of constant current 250-300mA by using the aluminum sheets as anodes, wherein the primary oxidation time is 2-3min, thus preparing the aluminum oxide film taking aluminum as a substrate.
Preferably, the secondary oxidation process of the aluminum-based porous alumina film humidity-sensitive sensor is as follows: putting an aluminum-based alumina film prepared by primary oxidation into an ammonium tartrate solution with the mass fraction of 3 percent by weight, and carrying out secondary oxidation by taking the aluminum-based alumina film as an anode at the constant voltage of 90-100V for 25-30 min.
Preferably, the evaporation coating process of the aluminum-based porous alumina film humidity-sensitive sensor comprises the following steps: fixing the mask plate and the aluminum-based alumina film, and preparing an electrode pattern on the aluminum-based alumina film by adopting gold or aluminum material.
Preferably, the aluminum-based porous alumina film humidity-sensitive sensor has the following electrode wire leading-out process: and perforating the aluminum substrate, connecting and fixing the aluminum substrate and the bottom electrode lead by screws, and then connecting and leading out the top electrode and the top electrode lead by welding.
The invention has the beneficial effects that: the porous alumina film humidity-sensitive sensor has the advantages of simple manufacturing process, convenient carrying of the prepared finished product and lower cost, and can be used for batch production. The prepared porous alumina film has good stability and high temperature resistance, so the porous alumina film is suitable for working environment temperature with a wider range. In addition, the porous alumina film prepared by the invention has larger pore diameter, is beneficial to the adsorption and desorption of water molecules, and has higher response speed and recovery speed.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a top electrode preparation mask pattern of the present invention;
in the drawings, the parts of the porous alumina membrane humidity-sensitive sensor represented by the respective reference numerals are listed below:
1. a substrate; 2. a moisture-sensitive film; 3. a top electrode; 4. a bottom electrode lead; 5. a screw; 6. a top electrode lead.
Detailed Description
The structure and process of the present invention are described below with reference to the accompanying drawings, which are provided as examples for explaining the present invention and not for limiting the scope of the present invention.
As shown in figure 1, the invention provides an aluminum-based porous alumina film humidity-sensitive sensor, which comprises a humidity-sensitive film 2, wherein the humidity-sensitive film 2 is positioned on the upper surface of a substrate 1, a bottom electrode lead 4 is arranged on the substrate 1, the substrate 1 and the bottom electrode lead 4 are fixedly connected through a screw 5, a top electrode 3 is arranged at the center of the surface of the humidity-sensitive film 2, a top electrode lead 6 is arranged on the top electrode 3, and the top electrode 3 and the top electrode lead 6 are fixedly connected through welding.
Further, the material of the humidity sensitive film 2 is an alumina film.
Further, the substrate 1 is an aluminum substrate.
Further, the top electrode 3 is a gold electrode or an aluminum electrode.
A preparation method of an aluminum-based porous alumina film humidity-sensitive sensor comprises the following steps:
designing a size structure of a high-purity aluminum sheet, and cutting the high-purity aluminum sheet into an aluminum sheet with the thickness of 0.6mm by using a cutting machine to obtain a substrate 1 which can be used for preparing an alumina film and is made of aluminum;
ultrasonically cleaning the cut aluminum sheet for 4min by using alcohol, then ultrasonically cleaning the aluminum sheet for 4min by using deionized water again, removing pollutants on the surface of the aluminum sheet, and finally drying the aluminum sheet by using nitrogen to obtain a substrate 1 with a clean and pollution-free surface;
in a high-temperature-resistant quartz glass beaker, taking molten KHSO4 as an electrolyte and a corrosion-resistant titanium rod as a cathode, and carrying out primary oxidation on a substrate 1 serving as an anode within the range of constant current of 250-300mA for 2-3min to prepare a humidity-sensitive film 2 made of Al2O 3;
in a common glass beaker, taking 3 percent of weight ammonium tartrate solution at normal temperature as electrolyte, taking a titanium rod as a cathode, and carrying out secondary oxidation on an aluminum-based alumina film (namely, a substrate 1 and a humidity-sensitive film 2) as an anode within the range of constant voltage of 90-100V, wherein the secondary oxidation time is 25-30 min;
the top electrode 3 made of gold or aluminum is prepared by using a mask and an evaporation coating mode, and the film thickness of the top electrode 3 is preferably controlled within hundreds of nanometers to prevent the thicker electrode film from blocking the holes on the surface of the humidity-sensitive film 2, and the pattern of the mask is shown in fig. 2.
In the primary oxidation process, the shape of the prepared humidity-sensitive film 2 is irregular due to the boiling phenomenon of the molten electrolyte, so that a cutter can be used for scraping part of the porous alumina to prepare the humidity-sensitive film 2 with the regular shape finally.
The substrate 1 is punched by a puncher, and then the bottom electrode (i.e. the substrate 1) and the bottom electrode lead 4 are connected and fixed by a screw 5 through a through hole.
And the top electrode lead 6 is welded and fixed to the top electrode 3 in a soldering mode and is led out.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. An aluminum-based porous alumina film humidity-sensitive sensor is characterized in that: the humidity-sensitive membrane electrode comprises a substrate (1) and a humidity-sensitive membrane (2), wherein the humidity-sensitive membrane (2) covers the upper surface of the substrate (1), a bottom electrode lead (4) is arranged on one side of the substrate (1), the bottom electrode lead (4) is fixedly connected onto the substrate (1) through a screw (5), a top electrode (3) is arranged at the center of the upper surface of the humidity-sensitive membrane (2), a top electrode lead (6) is arranged on the top electrode (3), and the top electrode (3) and the top electrode lead (6) are fixedly connected through welding.
2. The aluminum-based porous alumina membrane humidity-sensitive sensor according to claim 1, wherein the material of the humidity-sensitive membrane (2) is an alumina membrane.
3. An aluminium-based porous alumina membrane humidity sensor according to claim 1, wherein the substrate (1) is an aluminium substrate.
4. The humidity sensor according to claim 1, wherein the top electrode (3) is a gold electrode or an aluminum electrode.
5. The method for preparing an aluminum-based porous alumina thin film humidity sensor according to any one of claims 1 to 4, comprising the steps of:
step 1: carrying out a primary oxidation process on the high-purity aluminum sheet to prepare a porous aluminum oxide film with the aperture range of 500-600 nanometers;
step 2: carrying out secondary oxidation process on the porous alumina film treated in the step 1;
and step 3: carrying out evaporation coating on the porous alumina film treated in the step (2), and preparing a top electrode (3) on the surface of the porous alumina film;
and 4, step 4: perforating the substrate of the porous alumina film humidity-sensitive sensor treated in the step (3), and then fixing and leading out a bottom electrode wire by adopting a screw (5);
and 5: and (4) welding the top electrode (3) of the porous alumina thin film humidity sensor treated in the step (4), and then leading out a top electrode wire.
6. The method for preparing the aluminum-based porous alumina film humidity sensor according to claim 5, wherein the primary oxidation process in the step 1 is as follows: putting an aluminum sheet into the molten KHSO4, and carrying out primary oxidation in a constant current range of 250-300mA for 2-3min by using the aluminum sheet as an anode to prepare the porous aluminum oxide film taking aluminum as a substrate.
7. The method for preparing the aluminum-based porous alumina thin film humidity sensor according to claim 5, wherein the secondary oxidation process in the step 2 is as follows: and (2) putting the aluminum-based alumina film prepared by primary oxidation into an ammonium tartrate solution with the mass fraction of 3% by weight, and carrying out secondary oxidation by taking the aluminum-based alumina film as an anode at a constant voltage of 90-100V, wherein the secondary oxidation time is 25-30 min.
8. The method for preparing the aluminum-based porous alumina film humidity-sensitive sensor according to claim 5, wherein the evaporation coating process in the step 3 is as follows: fixing the mask plate and the aluminum-based alumina film, and preparing and forming an electrode pattern on the aluminum-based alumina film by adopting a gold or aluminum material.
9. The method for preparing the aluminum-based porous alumina thin film humidity sensor according to claim 5, wherein the electrode wire leading-out process in the steps 4 and 5 is as follows: the base (1) is perforated, the base (1) and the bottom electrode lead (4) are fixedly connected through a screw (5), and then the top electrode (3) and the top electrode lead (6) are connected and led out in a welding mode.
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| CN202111474405.5A CN114280108A (en) | 2021-12-03 | 2021-12-03 | Aluminum-based porous alumina film humidity-sensitive sensor and preparation method thereof |
| GB2218068.1A GB2614811B (en) | 2021-12-03 | 2022-12-01 | Aluminum-based porous alumina film humidity-sensitive sensor and manufacturing method thereof |
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| GB2614811A (en) * | 2021-12-03 | 2023-07-19 | Yangtze Delta Region Institute Of Univ Of Electronic Science And Technology Of China Huzhou | Aluminum-based porous alumina film humidity-sensitive sensor and manufacturing method thereof |
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| 史青: "α-Al2O3电容薄膜湿度传感器", 《电子科技大学学报》, pages 387 - 390 * |
| 葛澍蔚: "基氧化铝湿敏传感器制备及工艺研究", 《中国优秀硕士学位论文全文数据库信息科技辑》, pages 12 - 13 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2614811A (en) * | 2021-12-03 | 2023-07-19 | Yangtze Delta Region Institute Of Univ Of Electronic Science And Technology Of China Huzhou | Aluminum-based porous alumina film humidity-sensitive sensor and manufacturing method thereof |
| GB2614811B (en) * | 2021-12-03 | 2024-01-31 | Yangtze Delta Region Institute Of Univ Of Electronic Science And Technology Of China Huzhou | Aluminum-based porous alumina film humidity-sensitive sensor and manufacturing method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| GB202218068D0 (en) | 2023-01-18 |
| GB2614811B (en) | 2024-01-31 |
| GB2614811A (en) | 2023-07-19 |
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