CN107290241B - QCM humidity sensor and preparation method thereof - Google Patents
QCM humidity sensor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a QCM humidity sensor, which is characterized in that: the piezoelectric ceramic comprises a piezoelectric wafer, an insulating layer, a metal electrode layer and a humidity sensitive film layer; the metal electrode layer comprises a first metal electrode layer and a second metal electrode layer; the first metal electrode layer comprises two electrodes which are respectively arranged on two surfaces of the piezoelectric wafer, and an insulating layer is arranged on one surface of the electrode; the surface of the insulating layer is provided with a second metal electrode layer, and the surface of the second metal electrode layer is provided with a humidity sensitive film layer. The QCM humidity sensor has the structure of the bimetal electrode layer, can achieve high-sensitivity detection of low humidity, can enhance the stability of the sensor, has the advantages of low cost, large humidity detection range, high sensitivity, quick response, good repeatability and simple manufacturing process, and can be widely applied to the fields of low humidity detection and high-precision humidity detection.
Description
Technical Field
The invention relates to a humidity sensor, in particular to a QCM humidity sensor and a preparation method thereof.
Background
Humidity sensor is used as an important sensor and has very wide application in the fields of weather, agriculture, industrial control and the like. With the continuous development of technology, the demand of high-performance humidity sensors is increasing, and the traditional hair humidity sensor and the traditional dry and wet ball humidity sensor cannot meet the requirements of the industry, so that various types of electronic humidity sensors are appeared. In the last 60 th century, a Quartz Crystal Microbalance (QCM) type humidity sensor has emerged.
The QCM humidity sensor consists of a quartz crystal resonator and a humidity sensitive film layer modified on the surface of the resonator; the adsorption of water molecules by the humidity sensitive film deposited on the metal electrode causes an increase in the mass of the sensitive film (Deltam) and thus a frequency shift (Deltafm) is generated which is related to the molecular weight of the adsorbed water, as a function of the humidity to be measured in the environment, by the adsorption of water moleculesMeasuring the offset of the resonant frequency to obtain the humidity in the environment; the operating principle of the QCM humidity sensor is based on the following relation:
wherein f 0 Is the inherent fundamental frequency (in Hz) of the piezoelectric wafer, A is the area (in cm) of the metal electrode 2 )，ρ q 、μ q The density and shear modulus of the piezoelectric wafer, respectively. The QCM humidity sensor has the advantages of high sensitivity, low cost, simple testing device, easy realization of continuous field detection and the like, so that the QCM humidity sensor is widely applied to the field of humidity detection.
The detection sensitivity of the existing QCM humidity sensor is not high in a low humidity range (< 10% rh) because the content of water molecules in the air is low in the humidity range, which directly results in that the number of water molecules adsorbed on the humidity sensitive film layer is small, and thus the frequency offset of the QCM humidity sensor is small. In order to increase the detection sensitivity of QCM humidity sensors in the low humidity range, the sensitization methods that have been adopted by the industry are: (1) A humidity sensitive material with a nano structure is adopted to increase the specific surface area of the material; (2) A composite moisture sensitive material is adopted to enhance the hydrophilic characteristic of the material; (3) A large dose of moisture sensitive material is used to increase the water molecule adsorption sites. However, the sensitization methods of the three QCM humidity sensors in the low humidity range are all obtained on the premise that the humidity sensitive material adsorbs more water molecules. The adhesion of a large number of water molecules can greatly increase the viscosity of a humidity sensitive film deposited on a metal electrode of the QCM humidity sensor, so that abnormal phenomena such as abnormal fluctuation, vibration stopping and the like occur in the output frequency of the QCM humidity sensor, the stability of the sensor is greatly reduced, and the detection precision of the sensor is extremely unfavorable.
Disclosure of Invention
The invention aims at: aiming at the problems, by improving the structure of the existing QCM humidity sensor, a bimetal electrode layer structure is provided, a silicon dioxide film is sputtered on the surface of any metal electrode of the QCM humidity sensor, then an interdigital electrode is formed on the surface of the silicon dioxide film through an evaporation metal process, a photoetching process and an etching process, and a layer of water-absorbing medium humidity sensitive film is deposited on the surface of the interdigital electrode through methods such as air spraying, spin coating, drop coating and the like; and (5) preparing the QCM humidity sensor.
The technical scheme adopted by the invention is as follows:
the invention relates to a QCM humidity sensor, which comprises a piezoelectric wafer, an insulating layer, a metal electrode layer and a humidity sensitive film layer, wherein the piezoelectric wafer is arranged on the insulating layer; the metal electrode layer comprises a first metal electrode layer and a second metal electrode layer; the first metal electrode layer comprises two electrodes which are respectively arranged on two surfaces of the piezoelectric wafer, and an insulating layer is arranged on one surface of the electrode; the surface of the insulating layer is provided with a second metal electrode layer, and the surface of the second metal electrode layer is provided with a humidity sensitive film layer.
Further, the piezoelectric wafer is a piezoelectric quartz wafer, and is an AT cut.
Further, the fundamental frequency of the piezoelectric quartz wafer is 5-20 MHz.
Further, the metal electrode layer is made of gold or silver.
Further, the second metal electrode layer is an interdigital electrode structure.
Further, the interdigital electrode is respectively connected with a pin III and a pin IV; the first metal electrode layer comprises a first metal electrode and a second metal electrode; the second metal electrode is arranged between the piezoelectric wafer and the insulating layer and is connected with the second pin; the first metal electrode is connected with the first pin and is contacted with the piezoelectric chip.
Further, the humidity sensitive film layer is made of a water-absorbing medium material, and the dielectric constant is smaller than 5.
Further, the humidity-sensitive thin film layer is formed on the surface of the second metal electrode layer through an air spraying, spin coating or dripping method, and part of the humidity-sensitive thin film layer is filled in the electrode gap of the second metal electrode layer.
The invention relates to a preparation method of a QCM humidity sensor, which comprises the following steps:
s1: forming first metal electrode layers on two surfaces of a piezoelectric quartz wafer through an evaporation process;
s2: forming a silicon dioxide insulating layer with the thickness of 50nm on the surface of the first metal electrode layer through a sputtering process;
s3: forming a second metal electrode layer on the surface of the silicon dioxide insulating layer through an evaporation process;
s4: modifying the second metal electrode layer through a photoetching process and an etching process to form an interdigital electrode structure;
s5: cleaning with alcohol and deionized water, removing pollutants from the processed piezoelectric quartz wafer with the metal electrode, and drying;
s6: and forming a humidity-sensitive film layer on the surface of the second metal electrode layer by an air spraying, spin coating or dripping method, and drying.
According to the QCM humidity sensor, the second pin is connected with the third pin, the first pin and the fourth pin are used as two output ends of the sensor to be connected with two pins of an external vibration starting circuit, and under the condition that the pin configuration works, the QCM humidity sensor and the interdigital humidity-sensitive capacitor share a humidity-sensitive film layer, so that the humidity sensor device can be regarded as a serial structure of the QCM humidity sensor and the interdigital humidity-sensitive capacitor, and an equivalent circuit diagram of the humidity sensor device is shown in figure 3; in the equivalent circuit, the element resistance (R), inductance (L) and capacitance (C) reflect the mechanical loss, inertial mass and crystal elasticity of the QCM, respectively, the capacitance (C 0 ) Reflecting the inherent capacitance of the QCM; wherein, the adsorption of water molecules by the sensitive film layer of the QCM humidity sensor increases the inertial mass (i.e. L parameter) of the QCM, thereby generating a frequency shift Deltaf related to the mass of the adsorbed water molecules m ；
Equivalent humidity-sensitive capacitor C X The electrode III and the electrode IV are used as fringe capacitance electrodes, and the humidity sensitive film layer is used as a filling medium to form fringe humidity sensitive capacitance, when the sensitive film absorbs water molecules, the dielectric constant of the sensitive film is increased, so that C is caused X This increases, which results in a frequency shift Δf of the sensor that is related to the dielectric constant of the sensitive thin film layer ε The method comprises the steps of carrying out a first treatment on the surface of the Thus in a QCM humidity sensor according to the present inventionFrequency shift Δf=Δf of sensor due to water molecule adsorption m +Δf ε At the same time due to water adsorption resulting in Δf m And Δf ε All have negative values, so that a superposition effect is generated, and the aim of increasing the low humidity response sensitivity is fulfilled.
In summary, due to the adoption of the technical scheme, the beneficial effects of the invention are as follows:
1. the QCM humidity sensor manufactured by the invention introduces the structure of the bimetal electrode layer, is sensitive to the mass change and the dielectric constant change of the humidity sensitive film layer, and the mass and the dielectric constant change of the humidity sensitive film layer after the humidity sensitive film layer adsorbs water molecules can lead the QCM humidity sensor to generate frequency response sensitivity, thereby achieving the aim of detecting low humidity with high sensitivity under the condition of small amount of water molecules adsorption; meanwhile, the stability of the humidity sensor can not be reduced due to the change of the dielectric constant of the humidity sensitive film layer after water molecules are adsorbed, so that the stability of the sensor can be enhanced.
2. The QCM humidity sensor prepared by the invention has the advantages of low cost, large humidity detection range (0.1-100% RH), high sensitivity, quick response, good repeatability and simple manufacturing process, and can be widely applied to the fields of low humidity detection and high-precision humidity detection.
Drawings
The invention will now be described by way of example and with reference to the accompanying drawings in which:
fig. 1 is a schematic structural diagram of a QCM humidity sensor according to the present invention.
Fig. 2 is a top view of a QCM humidity sensor according to the present invention.
Fig. 3 is an equivalent circuit diagram of a QCM humidity sensor according to the present invention.
The marks in the figure: 1 is a piezoelectric wafer, 2 is an insulating layer, 3 is a metal electrode layer, 31 is a first metal electrode layer, 32 is a second metal electrode layer, and 4 is a humidity sensitive thin film layer.
Detailed Description
All of the features disclosed in this specification, or all of the steps in a method or process disclosed, may be combined in any combination, except for mutually exclusive features and/or steps.
Any feature disclosed in this specification (including any accompanying claims, abstract) may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise. That is, each feature is one example only of a generic series of equivalent or similar features, unless expressly stated otherwise.
Embodiment one:
as shown in fig. 1, the piezoelectric ceramic comprises a piezoelectric wafer 1, an insulating layer 2, a metal electrode layer 3 and a humidity sensitive film layer 4; the metal electrode layer 3 includes a first metal electrode layer 31 and a second metal electrode layer 32; the first metal electrode layer 31 comprises two electrodes respectively arranged on two surfaces of the piezoelectric wafer 1, and an insulating layer 2 is arranged on one surface of the electrode; the surface of the insulating layer 2 is provided with a second metal electrode layer 32, and the surface of the second metal electrode layer 32 is provided with a humidity sensitive film layer 4.
Embodiment two:
compared with the first embodiment, the present embodiment further discloses that the piezoelectric wafer 1 is a piezoelectric quartz wafer, and is an AT cut; the fundamental frequency of the piezoelectric quartz wafer is 5-20 MHz.
Embodiment III:
compared with the previous embodiment, this embodiment also discloses that the material of the metal electrode layer 3 is gold or silver.
Embodiment four:
as shown in fig. 2, compared with the previous embodiment, this embodiment also discloses that the second metal electrode layer 32 is an interdigital electrode structure.
The interdigital electrode is respectively connected with a pin III 323 and a pin IV 324; the first metal electrode layer 31 includes a first metal electrode and a second metal electrode; the second metal electrode is arranged between the piezoelectric wafer 1 and the insulating layer 2, and is connected with the second pin 312; the metal electrode is connected to the first pin 311 and contacts the piezoelectric chip 1.
Fifth embodiment:
compared with the previous embodiment, this embodiment also discloses that the humidity sensitive film layer 4 is made of a water-absorbing medium material, and has a dielectric constant less than 5.
The humidity sensitive film layer 4 is formed on the surface of the second metal electrode layer 32 by air spraying, spin coating or dripping method, and part of the sensitive film layer is filled in the electrode gap of the second metal electrode layer 32.
Example six:
compared with the previous embodiment, the embodiment also discloses a preparation method of the QCM humidity sensor, which comprises the following steps:
s1: forming first metal electrode layers 31 on both surfaces of the piezoelectric quartz wafer by an evaporation process;
s2: forming a silicon dioxide insulating layer 2 with the thickness of 50nm on the surface of the first metal electrode layer 31 through a sputtering process;
s3: forming a second metal electrode layer 32 on the surface of the silicon oxide insulating layer 2 by an evaporation process;
s4: modifying the second metal electrode layer 32 through a photolithography process and an etching process to form an interdigital electrode structure;
s5: cleaning with alcohol and deionized water, removing pollutants from the processed piezoelectric quartz wafer with the metal electrode, and drying;
s6: the humidity sensitive thin film layer 4 is formed on the surface of the second metal electrode layer 32 by an air-jet, spin-coating or drop-coating method, and dried.
The working principle of the QCM humidity sensor is as follows: the sensor is positioned in a detection environment, and the humidity sensitive film layer adsorbs water molecules in the environment, so that the humidity sensitive film layer is caused to change in two aspects:
(1) The humidity sensitive film layer absorbs water molecules to increase the mass, and the QCM humidity sensor generates a frequency shift delta f related to the mass of the absorbed water molecules according to the mass-frequency relation m ；
(2) The humidity sensitive film layer has a dielectric constant increased by adsorption of water molecules, which results in an interdigital humidity sensitive capacitor C formed between the third and fourth pins X The increase causes the sensor to generate a frequency shift delta f related to the dielectric constant of the sensitive film layer ε The method comprises the steps of carrying out a first treatment on the surface of the Due to the introduction of a frequency offset Deltaf related to the dielectric constant of the sensitive film layer ε This allows the sensor to operate in a low humidity range<10% RH) detection sensitivity can be greatly improved; meanwhile, the frequency stability of the QCM sensor is not reduced due to the dielectric constant change of the humidity sensitive film layer, so that the aim of detecting low humidity with high sensitivity and high precision can be realized very easily.
The invention is not limited to the specific embodiments described above. The invention extends to any novel one, or any novel combination, of the features disclosed in this specification, as well as to any novel one, or any novel combination, of the steps of the method or process disclosed.
Claims (7)
1. A QCM humidity sensor, characterized in that: comprises a piezoelectric wafer (1), an insulating layer (2), a metal electrode layer (3) and a humidity sensitive film layer (4); the metal electrode layer (3) comprises a first metal electrode layer (31) and a second metal electrode layer (32); the first metal electrode layer (31) comprises two electrodes which are respectively arranged on two surfaces of the piezoelectric wafer (1), and an insulating layer (2) is arranged on one surface of the electrode; a second metal electrode layer (32) is arranged on the surface of the insulating layer (2), and a humidity sensitive film layer (4) is arranged on the surface of the second metal electrode layer (32);
a method for preparing a QCM humidity sensor, comprising the steps of:
s1: forming first metal electrode layers (31) on both surfaces of a piezoelectric quartz wafer by an evaporation process;
s2: forming a silicon dioxide insulating layer (2) with the thickness of 50nm on the surface of the first metal electrode layer (31) through a sputtering process;
s3: forming a second metal electrode layer (32) on the surface of the silicon dioxide insulating layer (2) through an evaporation process;
s4: modifying the second metal electrode layer (32) through a photoetching process and an etching process to form an interdigital electrode structure;
s5: cleaning with alcohol and deionized water, removing pollutants from the processed piezoelectric quartz wafer with the metal electrode, and drying;
s6: and forming a humidity sensitive film layer (4) on the surface of the second metal electrode layer (32) by an air spraying, spin coating or dripping method, and drying.
2. The QCM humidity sensor of claim 1 wherein: the piezoelectric wafer (1) is a piezoelectric quartz wafer and is an AT cut.
3. The QCM humidity sensor of claim 2 wherein: the fundamental frequency of the piezoelectric quartz wafer is 5-20 MHz.
4. The QCM humidity sensor of claim 1 wherein: the metal electrode layer (3) is made of gold or silver.
5. The QCM humidity sensor of claim 1 wherein: the second metal electrode layer (32) is an interdigital electrode structure.
6. The QCM humidity sensor of claim 5 wherein: the interdigital electrode is respectively connected with a pin III (323) and a pin IV (324); the first metal electrode layer (31) comprises a first metal electrode and a second metal electrode; the second metal electrode is arranged between the piezoelectric wafer (1) and the insulating layer (2), and is connected with the second pin (312); a first metal electrode and a first connection pin (311) are contacted with the piezoelectric chip (1).
7. The QCM humidity sensor of claim 1 wherein: the humidity sensitive film layer (4) is made of a water-absorbing medium material, and the dielectric constant is smaller than 5.
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| CN108982277B (en) * | 2018-06-20 | 2020-05-19 | 华中科技大学 | Preparation method of quartz crystal microbalance humidity sensor and product |
| CN108896623B (en) * | 2018-07-11 | 2020-01-31 | 西南交通大学 | digital frequency type humidity sensor for measuring relative humidity of gas |
| CN109507059B (en) * | 2018-10-12 | 2020-08-18 | 华中科技大学 | Quartz crystal microbalance humidity sensor and preparation method thereof |
| CN112229878B (en) * | 2020-01-07 | 2021-08-10 | 南通大学 | Humidity sensor chip with three-electrode structure |
| CN112051307B (en) * | 2020-08-21 | 2022-04-22 | 华中科技大学 | Multi-sensor array based on quartz crystal microbalance and preparation method thereof |
| CN113390748A (en) * | 2021-06-16 | 2021-09-14 | 电子科技大学 | Humidity sensor based on quartz crystal microbalance and preparation method |
| CN114166935A (en) * | 2021-12-06 | 2022-03-11 | 西南交通大学 | QCM sensor and preparation method and application thereof |
| CN115165656A (en) * | 2022-07-28 | 2022-10-11 | 北京理工大学 | Small-size humidity transducer of high frequency quartz wafer microbalance and humidity measuring device |
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