CN110779956A - Humidity sensor and preparation method thereof - Google Patents
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Abstract
The invention discloses a humidity sensor and a preparation method thereof, wherein the humidity sensor comprises: a substrate; an adhesive layer disposed on the substrate, wherein the adhesive layer includes a first portion and a second portion; a first electrode layer disposed on the first portion; a linear piezoelectric material disposed laterally over the second portion and the first electrode layer, the linear piezoelectric material including a first end and a second end, wherein the first end is in contact with the first electrode layer; and a second electrode layer provided at a second end portion of the linear piezoelectric material.
Description
Technical Field
The embodiment of the invention relates to the technical field of sensing, in particular to a humidity sensor and a preparation method thereof.
Background
The humidity sensor has important significance in the fields of industrial and agricultural production, environmental protection, meteorological detection, aerospace and the like, and has higher requirements on sensing sensitivity, stability and reliability. In recent years, humidity sensors based on linear piezoelectric materials have received much attention.
The humidity sensor based on linear piezoelectric material in the prior art is generally configured to be connected to two electrodes (for example, vertically connected to an upper electrode and a lower electrode) along an axial direction, mainly considering a piezoelectric coefficient d
33The function of (1). However, the sensing of radial strain is also not negligible when considering the effect of external stress on the humidity performance of the humidity sensor, in particular for the absence of d
33The material of the piezoelectric coefficient requires different arrangements of the connection modes of the electrodes and the linear piezoelectric material. Therefore, it is necessary to study a humidity sensor in which a linear piezoelectric material is laterally disposed between upper and lower electrodes, so as to fill the blank of the study of the humidity sensor for radial strain sensing.
Disclosure of Invention
The embodiment of the invention aims to provide a radial strain sensing humidity sensor and a preparation method thereof.
According to an aspect of the present invention, there is provided a humidity sensor including: a substrate; an adhesive layer disposed on the substrate, wherein the adhesive layer includes a first portion and a second portion; a first electrode layer disposed on the first portion; a linear piezoelectric material disposed laterally over the second portion and the first electrode layer, the linear piezoelectric material including a first end and a second end, wherein the first end is in contact with the first electrode layer; and a second electrode layer provided at a second end portion of the linear piezoelectric material.
According to some embodiments, the linear piezoelectric material is perpendicular to a boundary line of the first electrode layer and the second portion.
According to some embodiments, the linear piezoelectric material comprises one of a nanowire, a microwire, a nanowire.
According to some embodiments, the linear piezoelectric material includes no d in trigonal 3m point group crystals
33The material having a piezoelectric coefficient is more preferably tellurium, α -quartz or AlPO
4、GaPO
4One kind of (1).
According to some embodiments, the linear piezoelectric material is in the shape of a hexagonal prism, and a single side edge of the hexagonal prism is located at the bottommost portion to contact the first electrode layer and the surface of the second portion.
According to some embodiments, the thickness of each of the first electrode layer and the second electrode layer is smaller than the radius of the linear piezoelectric material.
According to some embodiments, the substrate is a flexible substrate.
According to another aspect of the present invention, there is provided a method of manufacturing the humidity sensor described above, comprising: providing a substrate; providing an adhesive layer on a substrate, wherein the adhesive layer comprises a first portion and a second portion; providing a first electrode layer on the first portion; transversely arranging a linear piezoelectric material on the surfaces of the first electrode layer and the second part, wherein the linear piezoelectric material comprises a first end part and a second end part, and the first end part is in contact with the first electrode layer; and providing a second electrode layer at a second end portion of the linear piezoelectric material.
According to some embodiments, after the linear piezoelectric material is laterally disposed on the surfaces of the first electrode layer and the second portion, a glue layer is coated on the linear piezoelectric material such that the glue layer covers a middle portion of a side surface of the linear piezoelectric material, and then the second electrode layer is disposed.
According to some embodiments, further comprising: providing a temporary substrate; providing a linear piezoelectric material on a temporary substrate; covering a glue layer on the linear piezoelectric material, so that the glue layer covers the middle part of the side surface of the linear piezoelectric material; and peeling the linear piezoelectric material covered with the glue layer from the temporary substrate, arranging the linear piezoelectric material on the surfaces of the first electrode layer and the second part, and then arranging the second electrode layer.
In the humidity sensor according to the embodiment of the present invention, by disposing the linear piezoelectric material transversely between the first electrode layer and the second electrode layer, a radial strain sensing humidity sensor is provided, which is a novel structure different from the prior art, and the structure and type of the humidity sensor can be further improved, and is particularly suitable for the humidity sensor without d
33A material of piezoelectric coefficient; in addition, the humidity sensor of radial strain sensing can explore the influence of externally applied radial stress on the humidity performance of the humidity sensor, and adjust the humidity through the piezoelectric effect under the action of the radial stressThe gain of the sensor.
Drawings
Other objects and advantages of the present invention will become apparent from the following description of the invention which refers to the accompanying drawings, and may assist in a comprehensive understanding of the invention.
FIG. 1 illustrates a schematic structural view of a humidity sensor in accordance with an exemplary embodiment of the present invention;
FIG. 2 shows a scanning electron micrograph of a single tellurium line of a humidity sensor according to an exemplary embodiment of the present invention;
FIG. 3 shows a flow chart of a method of making the humidity sensor of FIG. 1;
FIG. 4 shows a schematic diagram of a process for making the humidity sensor of FIG. 1;
FIG. 5 shows a schematic diagram of another fabrication process of the humidity sensor of FIG. 1; and
FIG. 6 illustrates characterization results of humidity sensing of the humidity sensor of FIG. 1 under different humidity and stress effects.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to specific embodiments and the accompanying drawings. It should be noted that in the drawings or description, the same drawing reference numerals are used for similar or identical parts. Implementations not depicted or described in the drawings are of a form known to those of ordinary skill in the art. Additionally, while exemplifications of parameters including particular values may be provided herein, it is to be understood that the parameters need not be exactly equal to the respective values, but may be approximated to the respective values within acceptable error margins or design constraints. Directional phrases used in the embodiments, such as "upper," "lower," "front," "rear," "left," "right," and the like, refer only to the orientation of the figure. Accordingly, the directional terminology used is intended to be in the nature of words of description rather than of limitation.
Fig. 1 shows a schematic structural diagram of a humidity sensor 100 according to an exemplary embodiment of the present invention. As shown in FIG. 1, the humidity sensor 100 includesComprises the following steps: a substrate 1; an adhesive layer 2 disposed on the substrate 1, wherein the adhesive layer 2 includes a first portion 21 and a second portion 22; a first electrode layer 3 disposed on the first portion 21; a linear piezoelectric material 4 arranged transversely on the second portion 22 and the first electrode layer 3, the linear piezoelectric material 4 comprising a first end portion and a second end portion, wherein the first end portion is in contact with the first electrode layer 3; and a second electrode layer 5 provided at a second end portion of the linear piezoelectric material 4. That is, the humidity sensor 100 includes, in order from the bottom up, a substrate 1, an adhesive layer 2, a first electrode layer 3, a linear piezoelectric material 4, and a second electrode layer 5. In the humidity sensor 100 according to the embodiment of the present invention, by laterally disposing the linear piezoelectric material 4 between the first electrode layer 3 and the second electrode layer 5, a radial strain sensing humidity sensor is provided, which is a novel structure different from the prior art, and can further improve the structure and type of the humidity sensor, and is particularly suitable for the trigonal 3m point group crystal without d
33A material of piezoelectric coefficient; in addition, the humidity sensor with radial strain sensing can explore the influence of externally applied radial stress on the humidity performance of the humidity sensor, and the gain of the humidity sensor is adjusted through the piezoelectric effect under the action of the radial stress.
The substrate 1 may be a flexible substrate, which may be selected from PET or PI material, and may be provided with a thickness capable of withstanding a suitable mechanical bending and adapted to adjust the magnitude of the stress strain of the linear piezoelectric material 4, which may be, for example, 0.25mm to 0.8mm thick. The material of the adhesion layer 2 may be PMMA, and is disposed on the surface of the substrate 1 by spin coating, for example. The first electrode layer 3 is arranged on the first portion 21 of the adhesive layer 2, and the first portion 21 may occupy any suitable proportion of the area of the adhesive layer 2, for example the first electrode layer 3 may cover half the area of the adhesive layer 2. In this way, there is a boundary between the first electrode layer 3 and the second portion 22 of the adhesive layer 2 not covered by the first electrode layer 3.
The linear piezoelectric material 4 is laterally arranged on the surface of the first electrode layer 3 and the adhesion layer second portion 22, i.e. the linear piezoelectric material 4 intersects the boundary line between the first electrode layer 3 and the adhesion layer second portion 22. In some embodiments, the linear piezoelectric material 4 is a wire with a slitThe linear piezoelectric material 4 may include one of a nanowire, a microwire, and a nanowire, which may refer to a structure in which the radial length of the material is in the order of nanometers, micrometers, and millimeters and extends axially infinitely, for example, the aspect ratio of the material may be greater than 1000, and thus a rod-like or tubular structure may be included
4、GaPO
4The point group represents the symmetrical elements contained in the crystal, and the point group of 3m belongs to a trigonal system which comprises a third-order axis and a mirror surface which comprises the third-order axis and has an included angle of 60 DEG in pairs, because the crystal lattice groups of different piezoelectric materials have different piezoelectric coefficient directions, and the piezoelectric coefficients in the radial direction and the axial direction do not necessarily exist simultaneously, a proper piezoelectric material is selected according to the requirements of axial strain induction or radial strain induction when the device is prepared, and the arrangement position and the arrangement condition of the linear piezoelectric material 4 are also considered, which greatly influence the final result and determine the quality of output performance, tellurium, α -quartz, AlPO-quartz, AlPO- α -quartz, AlPO-III
4、GaPO
4The material having only d
11、d
14The piezoelectric strain coefficient is suitable for being transversely arranged between the upper electrode and the lower electrode to prepare a radial strain sensing humidity sensor. Since only at d
11And d
14The piezoelectric coefficient exists in the direction, and the contact arrangement of the material and the upper and lower electrodes is particularly important in the embodiment of the invention, tellurium, α -quartz, AlPO
4、GaPO
4The shape of the material may be a hexagonal prism, and a single side edge of the hexagonal prism is positioned at the bottommost portion (refer to fig. 3)C1) to contact the surface of the first electrode layer 3 and the second portion 22. The thickness of the second electrode layer 5 and the first electrode layer 3 on the upper and lower sides of the linear piezoelectric material 4 is smaller than the radius of the linear piezoelectric material 4, that is, half of the thickness. The linear piezoelectric material 4 can be prepared in a reaction vessel by a hydrothermal method. Fig. 2 shows a scanning electron micrograph of a single tellurium line of the humidity sensor according to an exemplary embodiment of the present invention, and referring to fig. 2, the scanning electron micrograph may clearly show the actual size of the tellurium line, which has a thickness of 30-40 μm.
Fig. 3 shows a flowchart of a method for manufacturing the humidity sensor 100 of fig. 1, and fig. 4 shows a schematic diagram of a manufacturing process of the humidity sensor 100 of fig. 1. Referring to fig. 3-4, the humidity sensor 100 may be prepared as follows:
s1, providing a substrate 1;
s2, disposing an adhesive layer 2 on the substrate 1, wherein the adhesive layer 2 includes a first portion 21 and a second portion 22; specifically, the adhesion layer 2 may be spin-coated on the upper surface of the substrate 1, the material of the adhesion layer 2 may be PMMA or PDMS11, the spin-coating speed may be 5000-;
s3, disposing the first electrode layer 3 on the adhesion layer first portion 21, for example, by spin coating; specifically, an isolation layer covers part of the area of the adhesion layer 2, a preservative film or other easily removable flexible films can be selected as the isolation layer, and after the electrode is subjected to spin coating, the isolation layer is removed;
s4, transversely disposing the linear piezoelectric material 4 on the surface of the first electrode layer 3 and the adhesion layer second part 22, the linear piezoelectric material 4 including a first end portion and a second end portion, such that the first end portion of the linear piezoelectric material 4 is in contact with the first electrode layer 3;
s5, the second electrode layer 5 is provided on the second end portion of the linear piezoelectric material 4.
The linear piezoelectric material 4 can be grown by a hydrothermal method, and a final product is adjusted and synthesized by controlling a precursor, the reaction temperature and the reaction time; the first electrode layer 3 and the second electrode layer 5 may be formed by spin coating or sputtering.
In some embodiments, the substrate 1 with the adhesive layer 2 is placed in a vacuum box for one minute in order to remove air in the adhesive layer, after the linear piezoelectric material 4 is laterally disposed on the surfaces of the first electrode layer 3 and the adhesive layer second portion 22, the linear piezoelectric material 4 is covered with the adhesive layer 6 so that the adhesive layer 6 covers the middle of the side surface of the linear piezoelectric material 4, and then the second electrode layer 5 is disposed. Specifically, the adhesive layer 6 may be a photoresist layer, and first covers an isolation layer above a contact position of the linear piezoelectric material 4 and the first electrode layer 3, and then coats the photoresist layer on the linear piezoelectric material 4, where there may be a certain gap for the isolation layer to cover, and in order to prevent the coated photoresist from penetrating, the first electrode layer 3 needs to be completely covered. The photoresist can be positive and negative photoresist such as SU-8, SUN, KPR, AZ, COP, etc., the spin coating speed is 800-. After the isolating layer film is removed, the isolating layer film is solidified in a vacuum drying oven, and a device structure of an upper electrode and a lower electrode can be formed. The material structure can be prevented from being oxidized by adjusting the curing temperature and time. Further, the electrode layers at the two ends can be led out by copper wires with the diameters of 0.8mm, 1.0mm and 1.2mm, in order to prevent the electrode layers from loosening, the electrode layers at the two ends can be fixed by resins, and then the humidity sensor 100 can be used for characterization measurement of humidity induction.
FIG. 5 is a schematic view illustrating another process for manufacturing the humidity sensor of FIG. 1, as shown in FIG. 5, the process for manufacturing the humidity sensor may include the steps of:
providing a temporary substrate;
providing a linear piezoelectric material 4 on a temporary substrate;
covering the linear piezoelectric material 4 with a glue layer 6, so that the glue layer 6 covers the middle part of the side surface of the linear piezoelectric material 4;
the linear piezoelectric material 4 covered with the glue layer 6 is peeled off from the temporary substrate and is provided on the surfaces of the first electrode layer 3 and the adhesive layer second portion 22, after which the second electrode layer 5 is provided.
The temporary substrate can be a silicon wafer, the adhesive layer 6 can be a spin-coated SU-8 adhesive layer, after the linear piezoelectric material 4 is covered by the SU-8 adhesive layer, the SU-8 adhesive layer and the temporary substrate are peeled off again through vacuum drying, the excess adhesive layer is removed in parallel by argon plasma to expose the upper part and the lower part of the linear piezoelectric material 4, and further electrode layers are arranged on the upper side and the lower side.
FIG. 6 illustrates characterization results of humidity sensing of the humidity sensor of FIG. 1 under different humidity and stress effects. Specifically, the prepared humidity sensor is placed in a closed container under constant temperature and constant pressure, and the external humidity of the humidity sensor is adjusted by using different saturated solutions (such as 98% concentrated sulfuric acid, NaCl solution and KCl solution) with different concentrations, so that the humidity is controlled to be 5% -80%. And applying different external radial stresses, the piezoelectric material 4 can be bent indirectly while bending the substrate 1. Specifically, the stress strain of the humidity sensor is adjusted by using a 3D displacement table with the resolution of micro-nano level. By controlling two different modes of tensile strain and compressive strain, induced charges with different signs are generated at two radial ends of the linear piezoelectric material 4 under stress strain, the induced potential generated by the induced charges can adjust the height of a potential barrier of a contact end of the metal semiconductor, further the signal output can be adjusted, and a final data graph can be obtained by utilizing a SCS4200 semiconductor test system. That is, the voltammetry curve of the linear piezoelectric material 4 under a certain compressive strain under different humidity; and a voltammogram of the linear piezoelectric material 4 under a certain humidity under different strains.
FIG. 6 is a top graph showing the voltammetric curve of a humidity sensor at a compressive strain of 0.22% at different humidities; the lower graph of fig. 6 shows the voltammogram of the humidity sensor at 38% humidity with RH representing relative humidity for different strains. It can be seen that when the compressive strain is fixed at 0.22%, the slope of the curve becomes smaller as the humidity increases; when the humidity was fixed at 38%, the slope of the curve became larger as the compression strain (absolute value) increased. It can be seen that the sensing result of the humidity sensor when sensing humidity has a great relationship with the radial stress condition, and the sensitivity of the sensor can be improved by adjusting the radial stress in practical use.
The following description is based on specific examples.
Example 1
A humidity sensor in which the linear piezoelectric material 4 is a tellurium wire is prepared.
Firstly, taking telluride as a precursor, obtaining a tellurium wire by adjusting reaction temperature and time under an alkaline environment, and then sequentially carrying out the following steps:
(a) spin-coating PMMA with the model number of A5 on a PET flexible substrate at the rotating speed of 6000rpm to prepare an adhesion layer with the film thickness of 2 mu m;
(b) coating a preservative film at the position of half PMMA on the substrate in a spin coating manner, brushing a layer of SPI conductive silver paste, and then uniformly spin-coating at the rotating speed of 1000rpm by using a spin coater to prepare a first electrode layer with the thickness of about 3 mu m;
(c) after the step (b), removing the preservative film, and placing tellurium wires which are prepared by hydrothermal growth and have the length of about 8mm and the thickness of about 40 mu m on the PMMA and the first electrode layer, so that the tellurium wires are perpendicular to the boundary line of the PMMA and the first electrode layer, and the placement form of the tellurium wires is ensured that a single side edge is arranged at the bottommost part;
(d) after the step (c), covering an isolating layer film on the first electrode layer, and spin-coating SU-8 photoresist at the rotating speed of 1000rpm, wherein the thickness of the photoresist layer is 35 mu m and the photoresist layer covers the whole tellurium wire;
(e) after the step (d), removing the SU-8 photoresist on the upper surface of the tellurium wire by using a normal-pressure radio frequency low-temperature plasma system at the flow rate of 300cc argon doped with 1% oxygen to expose the upper surface;
(f) and (e) covering a silver paste electrode at one end of the tellurium wire, which is not provided with the first electrode layer, to form a second electrode layer, removing the isolating layer film to form a device structure with an upper electrode and a lower electrode, drying in vacuum, leading out the electrodes by using copper wires with the diameter of 0.8mm, and coating and fixing the first electrode layer and the second electrode layer by using epoxy resin with the ratio of 1: 10.
Wherein, the step (b) can also be directly sputtering a layer of silver with the thickness of 1 μm under the high power of 150W by using a magnetron sputtering device to form the first electrode layer without covering the preservative film.
The humidity sensor provided by the embodiment of the invention at least has the following beneficial effects:
1. the method firstly grows the linear piezoelectric material in a reaction kettle by a hydrothermal method, then prepares the device structure by a simple operation method without complex and accurate material growth process control, and the manufactured structure is completely obtained by spin coating an adhesive layer and a glue layer at room temperature, so that the method is suitable for the condition that d does not exist
33Manufacturing a single-chain piezoelectric micro-nano structure material with piezoelectric coefficient; in addition, other equipment operation is not required to be introduced in the preparation process of the radial humidity-sensitive material, and the flow can be simplified.
2. The invention innovatively makes up for the prior sensing technology of simply using the electrodes at two axial sides, improves the equipment process of the humidity sensor by adopting the upper and lower electrodes and the transversely arranged linear piezoelectric material and introducing a radial strain applying mode, and can lay a certain foundation for the subsequent further-related radial strain sensing sensor.
3. The manufacturing method adopts a mature argon plasma photoresist removing process, the photoresist removing depth can be accurately controlled, the photoresist removing cleanliness is good, a micro-nano structure with a very clean side wall or top end can be obtained, and the surface definition of a single wire is good.
4. The manufacturing method is simple and easy to implement, has the advantages of controllable positions of the upper electrode and the lower electrode, easiness in manufacturing and the like, and is very suitable for application in the field of integrated systems such as micro-nano generators and self-driven sensors.
Although the present invention has been described in connection with the accompanying drawings, the embodiments disclosed in the drawings are intended to be illustrative of embodiments of the invention and should not be construed as limiting the invention.
It would be appreciated by those skilled in the art that changes may be made in these embodiments without departing from the principles and spirit of the general inventive concept, the scope of which is defined in the claims and their equivalents.
Claims (10)
1. A humidity sensor comprising:
a substrate;
an adhesive layer disposed on the substrate, wherein the adhesive layer includes a first portion and a second portion;
a first electrode layer disposed on the first portion;
a linear piezoelectric material disposed laterally over the second portion and the first electrode layer, the linear piezoelectric material including a first end and a second end, wherein the first end is in contact with the first electrode layer; and
and a second electrode layer provided at a second end portion of the linear piezoelectric material.
2. A humidity sensor according to claim 1, wherein the linear piezoelectric material is perpendicular to a boundary line of the first electrode layer and the second portion.
3. The humidity sensor of any of claims 1-2, wherein the linear piezoelectric material comprises one of a nanowire, a microwire, and a nanowire.
4. The humidity sensor according to any one of claims 1 to 3, wherein the linear piezoelectric material comprises a trigonal 3m point group crystal without d
33The material having a piezoelectric coefficient is more preferably tellurium, α -quartz or AlPO
4、GaPO
4One kind of (1).
5. The humidity sensor according to claim 4, wherein the linear piezoelectric material is in the shape of a hexagonal prism, and a single side edge of the hexagonal prism is located at the bottommost portion to contact the first electrode layer and the surface of the second portion.
6. A humidity sensor according to any of claims 1 to 5 in which the thickness of the first and second electrode layers are each less than the radius of the wire-like piezoelectric material.
7. A humidity sensor according to any of claims 1 to 6 wherein the substrate is a flexible substrate.
8. A method of making the humidity sensor of any one of claims 1-7, comprising:
providing a substrate;
providing an adhesive layer on a substrate, wherein the adhesive layer comprises a first portion and a second portion;
providing a first electrode layer on the first portion;
transversely arranging a linear piezoelectric material on the surfaces of the first electrode layer and the second part, wherein the linear piezoelectric material comprises a first end part and a second end part, and the first end part is in contact with the first electrode layer; and
and a second electrode layer is arranged at the second end part of the linear piezoelectric material.
9. The method according to claim 8, wherein after the linear piezoelectric material is laterally disposed on the surfaces of the first electrode layer and the second portion, the linear piezoelectric material is covered with a glue layer so that the glue layer covers the middle of the side surface of the linear piezoelectric material, and thereafter the second electrode layer is disposed.
10. The method of claim 8, further comprising:
providing a temporary substrate;
providing a linear piezoelectric material on a temporary substrate;
covering a glue layer on the linear piezoelectric material, so that the glue layer covers the middle part of the side surface of the linear piezoelectric material;
and peeling the linear piezoelectric material covered with the glue layer from the temporary substrate, arranging the linear piezoelectric material on the surfaces of the first electrode layer and the second part, and then arranging the second electrode layer.
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