CN114397333A - Electrolyte concentration sensor based on double electric layer principle, preparation method and application thereof - Google Patents
Electrolyte concentration sensor based on double electric layer principle, preparation method and application thereof Download PDFInfo
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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
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
-
- 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
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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Abstract
The invention discloses an electrolyte concentration sensor based on a double electric layer principle, a preparation method and application thereof. The method comprises the following steps: the method comprises the following steps: cleaning the substrate layer; step two: manufacturing a photoresist patterned glass sheet; step three: preparing an electrode pair; step four: and (6) integrated packaging. The electrolyte concentration sensor prepared by the method comprises a working electrode layer, an adhesion layer and a substrate layer, wherein the working electrode layer comprises a pair of electrode pairs with uncertain shapes, each electrode pair is led out by a metal wire in at least one direction, the tail end of the metal wire is provided with a welding point, and the welding point is used for welding a wire connected with a test device. The manufacturing process is simple, and the manufactured sensor is suitable for a low-voltage environment, can sensitively sense the change of the electrolyte concentration and has good performance.
Description
Technical Field
The invention belongs to the field of design and manufacture of advanced electronic components, and particularly relates to an electrolyte concentration sensor based on a double electric layer principle, a preparation method and application thereof.
Background
The sensor is a complex device for sensing external physical signals and chemical signals, and is divided into an electrical sensor, an optical sensor, a mechanical sensor and the like according to different principles. The electrochemical sensor is a special sensor in the field of sensors and can sense electrochemical signals, and the electrolyte concentration sensor is a special sensor in the field of electrochemical sensors and is used for detecting the concentration of ions in a solution, so that the electrochemical sensor can be applied to seawater salinity detection, sweat detection, body fluid detection and the like.
Most electrolyte concentration sensors on the market at present are mainly realized based on a method for measuring conductivity by chemical impedance analysis, and the sensors are not suitable for being combined with intelligent manipulators and the like due to large volume and mostly prepared based on rigid materials; in addition, there are electrolyte concentration sensors used for sweat composition analysis, which are complex to manufacture, require special materials, and are tasted along with electrochemical reactions during sensing, resulting in irreversible changes in sensor performance. Therefore, the electrolyte concentration sensor with simple structure, simple and convenient manufacturing process and excellent performance is developed, and has deeper application prospect.
The super capacitor is a capacitor with a very large capacitance value, and the super capacitor principle is used for manufacturing the sensor, so that the anti-interference capability of the sensor can be effectively enhanced. The electric double layer capacitor is a kind of super capacitor, which is characterized in that an electric double layer is generated in a sensitive region without electrochemical reaction. The application of the principle to the field of sensors is mainly focused on mechanical perception at present, and the application to electrolyte concentration sensors is in a vacant state at present.
Disclosure of Invention
In view of the above, the present invention is directed to an electrolyte concentration sensor based on the principle of electric double layer, a method for manufacturing the same, and an application thereof, so as to overcome the disadvantages of the prior art.
According to a first aspect of the invention, an electrolyte concentration sensor based on the double electric layer principle is provided, wherein the electrolyte concentration sensor comprises a working electrode layer, an adhesion layer and a substrate layer which are sequentially arranged from top to bottom, and is characterized in that the working electrode layer comprises a pair of electrode pairs with uncertain shapes, each electrode pair is led out by a metal lead in at least one direction, and the tail end of the metal lead is provided with a welding point which is used for welding a lead connected with a test device.
The working principle of the invention is an electrochemical double-electric-layer theory, and the change of the electric double-layer capacitance is caused by the change of the electrolyte concentration, so that the electrolyte concentration can be reversely deduced according to the capacitance.
Preferably, each of said electrode pairs is square or circular in shape with a side length of 3-8mm, preferably 5 mm. The sensing signal is weakened when the electrode is too small in size, and the performance of the sensor is reduced; the length of the side is too long, which is not beneficial to the utilization of the sensor in the occasions of human skin, and the like, therefore, the size of the sensor is selected to be about 5 mm.
Preferably, the line width of the metal wire is 0.2-0.5mm, and preferably 0.3 mm. The line width is too wide, so that the contact area between the lead and the electrolyte is too large, and lead signal interference is generated; too narrow a wire will increase the impedance in the circuit, which is detrimental to signal transmission.
Preferably, the electrode pair is made of an inert metal material, including but not limited to Au, Ag, Cu and Pt, preferably Au.
Preferably, the adhesion layer is made of a metal material capable of enhancing the adhesion between the inert metal material and the substrate material, including but not limited to Cr and Ti.
Preferably, the material of the substrate layer includes, but is not limited to, PI, PET and SiO2Preferably, PI is used. The PI is polyimide, the PET is polyethylene terephthalate, and the PI and the PET are both flexible materials, so that the manufactured sensor has certain flexibility and is convenient to combine with a manipulator; SiO 22The glass has certain rigidity, so that the manufactured sensor can be suitable for places with certain requirements on the structural strength of the sensor.
Preferably, the thickness of the working electrode layer is 50-150nm, preferably 100 nm; the thickness of the adhesion layer is 5-15nm, preferably 10 nm.
According to another aspect of the present invention, there is also provided a method of manufacturing an electrolyte concentration sensor based on the electric double layer principle, comprising the steps of:
the method comprises the following steps: cleaning a substrate layer, ultrasonically cleaning the substrate layer through at least one organic solvent, then cleaning the substrate layer through water, and blow-drying the substrate layer through an air gun, wherein the air blown out by the air gun is inert gas, preferably nitrogen;
step two: manufacturing a glass sheet with patterned photoresist, dropwise adding the photoresist on the cleaned substrate layer, spin-coating by a spin coater, and heating and curing by a hot plate at the heating temperature of 100-110 ℃, preferably 105 ℃; selecting a prepared mask plate, and developing after exposure by a photoetching machine to obtain a patterned photoresist substrate layer;
step three: preparing an electrode pair, and sequentially performing metal deposition on an adhesion layer metal and a working electrode layer metal on the substrate layer patterned by the photoresist obtained in the step two to obtain the electrode pair, wherein the metal deposition method comprises but is not limited to magnetron sputtering, thermal evaporation coating and electron beam evaporation coating, and magnetron sputtering is preferred;
step four: and (3) integrated packaging, namely packaging the lead part of the substrate layer with the electrode pair by PDMS, and connecting the lead to an LCR tester to complete the integrated packaging.
Preferably, the photoresist in the second step is 5350 photoresist, and the spin coating parameters of the spin coating machine are set as follows: the front rotation is 500rpm, and the rear rotation is 4000 rpm.
According to another aspect of the invention, the electrolyte concentration sensor based on the electric double layer principle is also provided to be applied to the occasions of human body sweating state detection, seawater concentration detection, electrolyte type analysis and the like.
Compared with the prior art, the invention has the following advantages:
(1) a new method is provided for making an electrolyte concentration sensor. The method comprises the following steps: the double-electric-layer theory is combined in the field of chemical sensors, and the change condition of the electrolyte concentration of the solution environment is sensed while chemical reaction is not generated under the low-voltage test condition.
(2) The sensor has simple manufacturing process, the electrodes are prepared by photoetching, and other processes such as silk-screen printing and the like can be selected.
(3) The sensor has simple and flexible structure and good performance, and the lowest concentration resolution ratio which can be detected is 0.01 mmol/L.
Drawings
Fig. 1 is a schematic view of the structure of an electrolyte concentration sensor of the present invention.
Fig. 2 is a capacitance-concentration characteristic curve of an electrolyte concentration sensor prepared in example 1 of the present invention.
Fig. 3 is a minimum concentration resolution curve for the electrolyte concentration sensor prepared in example 1.
Fig. 4 is a data point for the rigid substrate based electrolyte concentration sensor prepared in example 1 to detect different electrolyte species.
Fig. 5 is a graph of hand perspiration state detected by the PI flexible substrate-based electrolyte concentration sensor prepared in example 2.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific embodiments. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
In the following embodiments, the substrate layer may be made of flexible material or rigid material, including but not limited to PI (polyimide), PET (polyethylene terephthalate), and SiO2(glass), etc. The electrode pair is made of an inert metal material including, but not limited to, Au (gold), Ag (silver), Cu (copper), Pt (platinum), and the like. The adhesion layer is made of a metal material capable of enhancing the adhesion between the inert metal material and the substrate material, and includes but is not limited to Cr (chromium), Ti (titanium), and the like.
In the following examples, the metal deposition method used to prepare the electrode pair includes, but is not limited to, magnetron sputtering, thermal evaporation coating, and electron beam evaporation coating. In addition, screen printing can be used to produce the electrode pairs.
Example 1
The method comprises the following steps: and (5) cleaning the glass sheet. And ultrasonically cleaning the glass sheet by using acetone and isopropanol in sequence, then cleaning by using water, and finally drying by using a nitrogen gun to obtain a dry and clean glass sheet serving as a substrate layer.
Step two: and manufacturing the glass sheet with the patterned photoresist. And (3) dropwise adding 5350 photoresist on the glass sheet manufactured in the step one, spin-coating by a spin coater, wherein the spin coater has the following spin coating parameters: forward 500rpm, and then 4000 rpm; then thermally cured by a hot plate at 105 ℃; and selecting the prepared mask plate, and developing after exposure by adopting an MA6 photoetching machine to obtain the glass sheet with the patterned photoresist.
Step three: and preparing a test electrode pair. And C, carrying out magnetron sputtering on the glass sheet with the patterned photoresist obtained in the step two to sequentially deposit Cr and Au metals which are respectively used as an adhesion layer and an electrode layer, wherein the thickness of the deposited Cr is 10nm, and the thickness of the deposited Au is 100nm to obtain the electrode pair.
Step four: and (6) integrated packaging. And packaging the lead part of the glass sheet with the test electrode pair by PDMS, and connecting the lead to an LCR tester to complete integrated packaging.
The electrolyte concentration sensor structure prepared by the method is shown in figure 1 and comprises a working electrode layer, an adhesion layer and a substrate layer which are sequentially arranged from top to bottom, wherein the working electrode layer comprises a pair of electrode pairs with uncertain shapes, each electrode pair is led out by a metal lead in at least one direction, and the tail end of the metal lead is provided with a welding point. In this embodiment, the electrode pair is preferably a square structure, the side length of the square electrode pair is 5nm, and the width of the drawn metal wire is 0.3 nm. In other embodiments of the present invention, the shape of the electrode pair is not limited, and may be designed and modified according to actual requirements, such as a double semicircular electrode.
The electrolyte concentration sensor prepared in this example 1 was subjected to capacitance and concentration characteristic tests, and the obtained data were obtained by taking common logarithms for both sides, and the capacitance-concentration characteristic curve thereof, as shown in fig. 2, exhibited good linearity, and the linear slope thereof was close to theoretical analysis. When the sensor is applied to concentration detection, the concentration resolution is as low as 0.01mmol/L, as shown in FIG. 3.
The electrolyte concentration sensor shows better electrolyte species resolving power, and different electrolyte species show different capacitance signals under the same concentration as shown in figure 4. Wherein CaCl2、CaSO4、CuSO4、Na2SO4Have a higher signal, since these ions exhibit more ionic concentration and charge after electrolysis; lactic Acid (LA), urea, show lower signals because these electrolytes are weak electrolytes and only partially ionize in aqueous solutions; and water (H)2O) exhibits a very low capacitance signal due to H2O is an extremely weak electrolyte with an ion concentration of only 10 after ionization at room temperature- 7mol/L。
Example 2
In this embodiment, the manufacturing method of the electrolyte concentration sensor is substantially the same as that of embodiment 1, except that: the material of the substrate layer adopts flexible PI. Therefore, the electrolyte concentration sensor has certain flexibility, is convenient to combine with a manipulator, and can be flexibly applied to various scenes.
The prepared electrolyte concentration sensor can be applied to detect the sweating state of a human body as shown in fig. 5, which shows the sweating state of a human hand under a normal state, after sweating, and after washing hands.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (10)
1. The electrolyte concentration sensor is characterized in that the working electrode layer comprises a pair of electrode pairs with uncertain shapes, each electrode pair is led out by a metal lead in at least one direction, and the tail end of the metal lead is provided with a welding point which is used for welding a lead connected with a test device.
2. An electrolyte concentration sensor based on the electric double layer principle as claimed in claim 1, wherein each of the electrode pairs has a square shape with a side length of 3 to 8mm, preferably 5 mm.
3. An electrolyte concentration sensor based on the electric double layer principle according to claim 1 or 2, wherein the metal wire has a line width of 0.2 to 0.5mm, preferably 0.3 mm.
4. The double electric layer principle-based electrolyte concentration sensor according to claim 1 or 2, wherein the electrode pair is made of an inert metal material including but not limited to Au, Ag, Cu and Pt, preferably Au.
5. The sensor of claim 1 or 2, wherein the adhesion layer is made of a metal material capable of enhancing adhesion between the inert metal material and the substrate material, including but not limited to Cr and Ti.
6. An electric double layer principle based electrolyte concentration sensor according to claim 1 or 2, characterized in that the material of the substrate layer includes but is not limited to PI, parylene PET and SiO2Preferably, PI is used.
7. An electric double layer principle-based electrolyte concentration sensor according to claim 1 or 2, characterized in that the thickness of the working electrode layer is 50-150nm, preferably 100 nm; the thickness of the adhesion layer is 5-15nm, preferably 10 nm.
8. A preparation method of an electrolyte concentration sensor based on the principle of an electric double layer comprises the following steps:
the method comprises the following steps: cleaning the substrate layer, ultrasonically cleaning the substrate layer through at least one organic solvent, then cleaning the substrate layer through water, and drying the substrate layer through an air gun; the organic solvent includes but is not limited to acetone, isopropanol; the gas blown out by the air gun is inert gas, preferably nitrogen;
step two: manufacturing a glass sheet with patterned photoresist, dropwise adding the photoresist on the cleaned substrate layer, spin-coating by a spin coater, and heating and curing by a hot plate at the heating temperature of 100-110 ℃, preferably 105 ℃; selecting a prepared mask plate, and developing after exposure by a photoetching machine to obtain a patterned photoresist substrate layer;
step three: preparing an electrode pair, and sequentially performing metal deposition on an adhesion layer metal and a working electrode layer metal on the substrate layer patterned by the photoresist obtained in the step two to obtain the electrode pair, wherein the metal deposition method comprises but is not limited to magnetron sputtering, thermal evaporation coating and electron beam evaporation coating, and magnetron sputtering is preferred;
step four: and (3) integrated packaging, namely packaging the lead part of the substrate layer with the electrode pair by PDMS, and connecting the lead to an LCR tester to complete the integrated packaging.
9. The electric double layer principle-based electrolyte concentration sensor according to claim 1, wherein the photoresist in step two is 5350 photoresist, and the spin coating parameters of the spin coater are set as follows: the front rotation is 500rpm, and the rear rotation is 4000 rpm.
10. Use of the electrolyte concentration sensor according to any one of claims 1 to 7, wherein the electrolyte concentration sensor is used for human perspiration state detection, seawater concentration detection and electrolyte species analysis after being combined with a microporous membrane.
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