CN107290241A - A kind of QCM humidity sensors and preparation method thereof - Google Patents
A kind of QCM humidity sensors and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of QCM humidity sensors, it is characterised in that：Including piezoelectric chip, insulating barrier, metal electrode layer and humidity sensitive film layer；The metal electrode layer includes the first metal electrode layer and the second metal electrode layer；First metal electrode layer includes two electrodes, is respectively arranged on two faces of piezoelectric chip, and one of electrode surface is provided with insulating barrier；The surface of insulating layer is provided with the second metal electrode layer, and the second metal electrode layer surface is provided with humidity sensitive film layer.QCM humidity sensors of the present invention have the structure of bimetallic electrode layer, high-sensitivity detection low humidity can be reached, the stability of sensor can be strengthened simultaneously, and cost is low, Humidity Detection scope is big, sensitivity is high, response is fast, reproducible, manufacture craft is simple, low humidity detection and high-precision Humidity Detection field can be widely applied to.
Description
Technical field
The present invention relates to humidity sensor, especially a kind of QCM humidity sensors and preparation method thereof.
Background technology
Humidity sensor has quite varied as the important sensor of a class in the field such as meteorology, agricultural, Industry Control
Application.With continuing to develop for science and technology, people are continuously increased to the demand of high-performance humidity sensor, traditional hair humidity
Sensor and wet and dry bulb humidity sensor can not meet the requirement of industry already, thus occur in that polytype electronic type humidity
Sensor.Eighties of last century sixties, occur in that a kind of QCM (QCM) formula humidity sensor.
QCM humidity sensors are with modifying the humidity sensitive film layer group in resonator surface by quartz-crystal resonator
Into；The humidity sensitive film adsorbed water molecule being deposited on metal electrode causes sensitive thin film quality to increase (Δ m), so as to produce
One frequency shift (FS) (Δ fm) related with adsorbed water molecule amount is led to because Water Molecular Adsorption amount is with treating that measuring moisture is relevant in environment
Cross the measurement of resonance frequency shift amount, you can obtain humidity in environment；The operation principle of QCM humidity sensors is based on following relation
Formula：Wherein f0For the intrinsic fundamental frequency (unit is Hz) of piezoelectric chip, A is metal electrode face
(unit is cm to product2), ρq、μqThe respectively density and modulus of shearing of piezoelectric chip.Due to qcm sensor have it is very high sensitive
Degree, lower cost are cheap, and test device is simple, be easily achieved many merits such as live continuous detection so that QCM humidity is passed
Sensor is widely used in Humidity Detection field.
Existing QCM humidity sensors in the range of low humidity (<10%RH) detection sensitivity is not generally high, because
The content of moisture in air is very low in this humidity range, and this directly results in the moisture being adsorbed onto on humidity sensitive film layer
Quantum count is also seldom, thus the frequency offset of QCM humidity sensors is also smaller.In order to increase QCM humidity sensors in low humidity
The detection sensitivity of scope is spent, the photosensitivity-enhancing method that industry personnel have used has：(1) using the humidity-sensitive material with nanostructured
To increase the specific surface area of material；(2) compound humidity-sensitive material is used with the water-wet behavior of reinforcing material；(3) using heavy dose
Humidity-sensitive material is to increase Water Molecular Adsorption point.But, photosensitivity-enhancing method of the above-mentioned three kinds of QCM humidity sensors in the range of low humidity
It is all based on what is obtained on the premise of humidity sensitive material adsorbs more hydrone numbers.And the Water Molecular Adsorption of a large amount of numbers
Humidity sensitive film viscosity on QCM humidity sensor metal electrodes can be deposited on to greatly increase, so as to cause QCM humidity to pass
There are the anomalies such as unusual fluctuations, failure of oscillation in the output frequency of sensor, and the stability of sensor is greatly reduced, and this is to sensor
Accuracy of detection is totally unfavorable.
The content of the invention
The goal of the invention of the present invention is：For above-mentioned problem, pass through the structure to existing QCM humidity sensors
It is improved, proposes a kind of bimetallic electrode Rotating fields, one layer two is sputtered in any surface of metal electrode of QCM humidity sensors
Silicon oxide film, then forms interdigital on silica membrane surface by evaporated metal technique, photoetching process and etching technics
Shape electrode is thin by the methods such as gas blowout, spin coating, drop coating one layer absorbent humidity of media sensitivity of deposition on interdigited electrode surface
Film；QCM humidity sensors are made.
The technical solution adopted by the present invention is as follows：
A kind of QCM humidity sensors of the present invention, including piezoelectric chip, insulating barrier, metal electrode layer and humidity sensitive film
Layer；The metal electrode layer includes the first metal electrode layer and the second metal electrode layer；First metal electrode layer includes two
Individual electrode, is respectively arranged on two faces of piezoelectric chip, and one of electrode surface is provided with insulating barrier；On the surface of insulating layer
Provided with the second metal electrode layer, the second metal electrode layer surface is provided with humidity sensitive film layer.
Further, the piezoelectric chip is piezoelectric quartz crystal plate, is AT cut types.
Further, the fundamental frequency of the piezoelectric quartz crystal plate is 5~20MHz.
Further, the metal electrode layer material is gold or silver.
Further, second metal electrode layer is interdigited electrode structure.
Further, the interdigited electrode connects pin three and pin four respectively；First metal electrode layer includes gold
Belong to electrode one and metal electrode two；Metal electrode two is arranged between piezoelectric chip and insulating barrier, the connection pin of metal electrode two
Two；Metal electrode one connects pin one, is contacted with piezoelectric chip.
Further, the humidity sensitive film layer is water imbibition dielectric material, and dielectric constant is less than 5.
Further, the humidity sensitive film layer is formed in the second metal electrode by gas blowout, spin coating or drop coating method
Layer surface, part sensitive thin film layer is filled in inside the electrode gap of the second metal electrode layer.
A kind of its preparation method of QCM humidity sensors of the present invention, comprises the following steps：
S1：Pass through evaporation process the first metal electrode layer of formation on two surfaces of piezoelectric quartz crystal plate；
S2：Pass through silicon dioxide insulating layer thick sputtering technology formation 50nm in the first metal electrode layer surface；
S3：Second metal electrode layer is formed on silicon dioxide insulating layer surface by evaporation process；
S4：The second metal electrode layer is modified by photoetching process and etching technics, interdigited electrode structure is formed；
S5：Cleaned with alcohol and deionized water, the piezoelectric quartz crystal plate with metal electrode of above-mentioned processing removes depollution
Thing, and dry；
S6：By gas blowout, spin coating or drop coating method in the second metal electrode layer surface formation humidity sensitive film layer, and
Dry.
QCM humidity sensors of the present invention, pin two is connected with pin three, and pin one and pin four are used as two of sensor
Two pins of the extraneous start-oscillation circuit of output end connection, under this pin configuration working condition, QCM humidity sensors and interdigital
Shape humicap share humidity sensitive film layer, therefore the humidity sensor device be considered as a QCM humidity sensor and
One interdigitated humicap cascaded structure form, its equivalent circuit diagram is as shown in Figure 3；In equivalent circuit, component resistance
(R), inductance (L) and electric capacity (C) reflect QCM mechanical loss, inertia mass and crystal elasticity, electric capacity (C respectively0) reflection
QCM natural capacity；Wherein, the sensitive thin film layer adsorbed water molecule meeting QCM of QCM humidity sensors inertia mass (that is to say L
Parameter) increase, so as to produce a frequency shift (FS) Δ f related to adsorption moisture protonatomic massm；
Equivalent humicap CXReflection be electrode three, electrode four as edge capacitance electrode, humidity sensitive film layer is made
The marginal mode humicap formed by filled media, after sensitive thin film adsorbed water molecule, its dielectric constant can increase, so that
So that CXIncrease, this causes sensor to produce a frequency shift (FS) Δ f related to sensitive thin film layer dielectric constantε；Therefore exist
In a kind of QCM humidity sensors that the present invention is announced, the frequency shift (FS) Δ f=Δs f that sensor is produced by Water Molecular Adsorptionm+
Δfε, simultaneously as water absorption causes Δ fmWith Δ fεIt is negative value, therefore produces a synergistic effect, reaches increase low humidity
The purpose of response sensitivity.
In summary, by adopting the above-described technical solution, the beneficial effects of the invention are as follows：
1st, the QCM humidity sensors obtained by the present invention introduce the structure of bimetallic electrode layer, while to humidity sensitive
The mass change and change in dielectric constant of film layer are sensitive, quality and dielectric constant after humidity sensitive film layer adsorbed water molecule
Change can cause QCM humidity sensors to produce frequency response sensitivity, so as under conditions of a small amount of adsorbed water molecule
Reach the purpose of high-sensitivity detection low humidity；Meanwhile, the change in dielectric constant after humidity sensitive film layer adsorbed water molecule will not
So that the stability of humidity sensor declines, thus the stability of sensor can be strengthened.
2nd, the QCM humidity sensors obtained by the present invention have that cost is low, Humidity Detection scope big (0.1-100%RH),
Sensitivity is high, it is simple to respond fast, reproducible, manufacture craft, can be widely applied to low humidity detection and high-precision humidity inspection
Survey field.
Brief description of the drawings
Examples of the present invention will be described by way of reference to the accompanying drawings, wherein：
Fig. 1 is a kind of structural representation of QCM humidity sensors of the invention.
Fig. 2 is a kind of top view of QCM humidity sensors of the invention.
Fig. 3 is a kind of equivalent circuit diagram of QCM humidity sensors of the invention.
Marked in figure：1 is piezoelectric chip, and 2 be insulating barrier, and 3 be metal electrode layer, and 31 be the first metal electrode layer, and 32 are
Second metal electrode layer, 4 be humidity sensitive film layer.
Embodiment
All features disclosed in this specification, or disclosed all methods or during the step of, except mutually exclusive
Feature and/or step beyond, can combine in any way.
Any feature disclosed in this specification (including any accessory claim, summary), unless specifically stated otherwise,
Replaced by other equivalent or with similar purpose alternative features.I.e., unless specifically stated otherwise, each feature is a series of
An example in equivalent or similar characteristics.
Embodiment one：
Such as Fig. 1, including piezoelectric chip 1, insulating barrier 2, metal electrode layer 3 and humidity sensitive film layer 4；The metal electrode
Layer 3 includes the first metal electrode layer 31 and the second metal electrode layer 32；First metal electrode layer 31 includes two electrodes, point
It is not arranged on 1 two faces of piezoelectric chip, one of electrode surface is provided with insulating barrier 2；The surface of insulating barrier 2 is provided with the
Two metal electrode layers 32, the surface of the second metal electrode layer 32 is provided with humidity sensitive film layer 4.
Embodiment two：
Compared with embodiment one, the present embodiment is also disclosed, and the piezoelectric chip 1 is piezoelectric quartz crystal plate, is AT cut types；
The fundamental frequency of the piezoelectric quartz crystal plate is 5~20MHz.
Embodiment three：
Compared with embodiment before, the present embodiment is also disclosed, and the material of metal electrode layer 3 is gold or silver.
Example IV：
Such as Fig. 2, compared with embodiment before, the present embodiment is also disclosed, and second metal electrode layer 32 is interdigital
Shape electrode structure.
The interdigited electrode connects pin 3 323 and pin 4 324 respectively；First metal electrode layer 31 includes gold
Belong to electrode one and metal electrode two；Metal electrode two is arranged between piezoelectric chip 1 and insulating barrier 2, and the connection of metal electrode two is drawn
Pin 2 312；Metal electrode one connects pin 1, is contacted with piezoelectric chip 1.
Embodiment five：
Compared with embodiment before, the present embodiment is also disclosed, and the humidity sensitive film layer 4 is water imbibition medium material
Material, dielectric constant is less than 5.
The humidity sensitive film layer 4 is by the formation of gas blowout, spin coating or drop coating method in the table of the second metal electrode layer 32
Face, part sensitive thin film layer is filled in inside the electrode gap of the second metal electrode layer 32.
Embodiment six：
Compared with embodiment before, the present embodiment is also disclosed, a kind of its preparation method of QCM humidity sensors, bag
Include following steps：
S1：Pass through evaporation process the first metal electrode layer 31 of formation on two surfaces of piezoelectric quartz crystal plate；
S2：Pass through silicon dioxide insulating layer 2 thick sputtering technology formation 50nm on the surface of the first metal electrode layer 31；
S3：Second metal electrode layer 32 is formed on the surface of silicon dioxide insulating layer 2 by evaporation process；
S4：The second metal electrode layer 32 is modified by photoetching process and etching technics, interdigited electrode knot is formed
Structure；
S5：Cleaned with alcohol and deionized water, the piezoelectric quartz crystal plate with metal electrode of above-mentioned processing removes depollution
Thing, and dry；
S6：Humidity sensitive film layer is formed on the surface of the second metal electrode layer 32 by gas blowout, spin coating or drop coating method
4, and dry.
A kind of operation principle of QCM humidity sensors of the present invention is as follows：Sensor is located in detection environment, humidity sensitive
Hydrone in film layer absorption environment, changes so as to cause humidity sensitive film layer to occur two aspects：
(1) humidity sensitive film layer adsorbed water molecule and cause its quality increase, it can be seen from mass-frequency relationship formula
QCM humidity sensors can produce a frequency shift (FS) Δ f related to adsorption moisture protonatomic massm；
(2) humidity sensitive film layer causes its dielectric constant to become big due to adsorbed water molecule, and this causes pin three and drawn
The interdigitated humicap C formed between pin fourXIncrease so that sensor can produce one it is normal with sensitive thin film layer dielectric
The related frequency shift (FS) Δ f of numberε；Due to introducing the frequency shift (FS) Δ f related to sensitive thin film layer dielectric constantε, this to pass
Sensor in the range of low humidity (<10%RH) detection sensitivity can be greatly improved；Simultaneously as humidity sensitive film layer
Change in dielectric constant will not generally cause the frequency stability of qcm sensor to decline, thus can very easily realize height
The purpose of sensitivity high precision test low humidity.
The invention is not limited in foregoing embodiment.The present invention, which is expanded to, any in this manual to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (9)
1. a kind of QCM humidity sensors, it is characterised in that：Including piezoelectric chip（1）, insulating barrier（2）, metal electrode layer（3）With
Humidity sensitive film layer（4）；The metal electrode layer（3）Including the first metal electrode layer（31）With the second metal electrode layer
（32）；First metal electrode layer（31）Including two electrodes, piezoelectric chip is respectively arranged at（1）On two faces, wherein one
Individual electrode surface is provided with insulating barrier（2）；The insulating barrier（2）Surface is provided with the second metal electrode layer（32）, the second metal electricity
Pole layer（32）Surface is provided with humidity sensitive film layer（4）.
2. QCM humidity sensors according to claim 1, it is characterised in that：The piezoelectric chip（1）It is brilliant for piezoelectric quartz
Piece, is AT cut types.
3. QCM humidity sensors according to claim 2, it is characterised in that：The fundamental frequency of the piezoelectric quartz crystal plate be 5~
20 MHz。
4. QCM humidity sensors according to claim 1, it is characterised in that：The metal electrode layer（3）Material for gold or
Person's silver.
5. QCM humidity sensors according to claim 1, it is characterised in that：Second metal electrode layer（32）For fork
Finger electrode structure.
6. QCM humidity sensors according to claim 5, it is characterised in that：The interdigited electrode connects pin respectively
Three（323）With pin four（324）；First metal electrode layer（31）Including metal electrode one and metal electrode two；Metal electricity
Pole two is arranged at piezoelectric chip（1）And insulating barrier（2）Between, the connection pin two of metal electrode two（312）；Metal electrode one is connected
Pin one（311）, with piezoelectric chip（1）Contact.
7. QCM humidity sensors according to claim 1, it is characterised in that：The humidity sensitive film layer（4）For water suction
Property dielectric material, dielectric constant be less than 5.
8. QCM humidity sensors according to claim 1, it is characterised in that：The humidity sensitive film layer（4）Pass through gas
Spray, spin coating or the formation of drop coating method are in the second metal electrode layer（32）Surface, part sensitive thin film layer is filled in the second metal
Electrode layer（32）Electrode gap inside.
9. a kind of its preparation method of the QCM humidity sensors based on described in one of claim 1-8, it is characterised in that：Including
Following steps：
S1：Pass through evaporation process the first metal electrode layer of formation on two surfaces of piezoelectric quartz crystal plate（31）；
S2：In the first metal electrode layer（31）Surface passes through silicon dioxide insulating layer thick 50 nm of sputtering technology formation（2）；
S3：By evaporation process in silicon dioxide insulating layer（2）The second metal electrode layer is formed on surface（32）；
S4：By photoetching process and etching technics to the second metal electrode layer（32）Modified, form interdigited electrode structure；
S5：Cleaned with alcohol and deionized water, the piezoelectric quartz crystal plate with metal electrode of above-mentioned processing, remove pollutant,
And dry；
S6：By gas blowout, spin coating or drop coating method in the second metal electrode layer（32）Surface forms humidity sensitive film layer
（4）, and dry.
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Cited By (7)
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| CN109507059A (en) * | 2018-10-12 | 2019-03-22 | 华中科技大学 | A kind of quartz crystal microbalance humidity sensor and preparation method thereof |
| CN112051307A (en) * | 2020-08-21 | 2020-12-08 | 华中科技大学 | Multi-sensor array based on quartz crystal microbalance and preparation method thereof |
| WO2021139206A1 (en) * | 2020-01-07 | 2021-07-15 | 南通大学 | Humidity sensor chip having three-electrode structure |
| 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 |
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| CN108982277A (en) * | 2018-06-20 | 2018-12-11 | 华中科技大学 | A kind of preparation method and product of quartz crystal microbalance humidity sensor |
| CN108982277B (en) * | 2018-06-20 | 2020-05-19 | 华中科技大学 | Preparation method of quartz crystal microbalance humidity sensor and product |
| CN108896623A (en) * | 2018-07-11 | 2018-11-27 | 西南交通大学 | It is a kind of for measuring the numerical frequency formula humidity sensor of gas relative humidity |
| 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 |
| CN109507059A (en) * | 2018-10-12 | 2019-03-22 | 华中科技大学 | A kind of quartz crystal microbalance humidity sensor and preparation method thereof |
| CN109507059B (en) * | 2018-10-12 | 2020-08-18 | 华中科技大学 | Quartz crystal microbalance humidity sensor and preparation method thereof |
| CN113588727A (en) * | 2020-01-07 | 2021-11-02 | 南通大学 | Humidity sensor chip without storage module |
| WO2021139206A1 (en) * | 2020-01-07 | 2021-07-15 | 南通大学 | Humidity sensor chip having three-electrode structure |
| CN113588727B (en) * | 2020-01-07 | 2022-04-05 | 南通大学 | Humidity sensor chip without storage module |
| CN112051307A (en) * | 2020-08-21 | 2020-12-08 | 华中科技大学 | Multi-sensor array based on quartz crystal microbalance and preparation method thereof |
| 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 |
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