CN110988057A - Sweat sensor, integrated electrode array and preparation method thereof - Google Patents
Sweat sensor, integrated electrode array and preparation method thereof Download PDFInfo
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Classifications
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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
- G01N27/27—Association of two or more measuring systems or cells, each measuring a different parameter, where the measurement results may be either used independently, the systems or cells being physically associated, or combined to produce a value for a further parameter
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/16—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements
-
- 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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- 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
- G01N27/333—Ion-selective electrodes or membranes
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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
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/333—Ion-selective electrodes or membranes
- G01N27/3335—Ion-selective electrodes or membranes the membrane containing at least one organic component
Abstract
The application relates to a sweat sensor, an integrated electrode array and a preparation method thereof, wherein the integrated electrode array of the sweat sensor comprises a first electrode group for detecting organic components in sweat and a second electrode group for detecting inorganic components in the sweat, the first electrode group and the second electrode group respectively comprise at least two working electrodes and at least one reference electrode, each reference electrode corresponds to at least one working electrode, and different working electrodes are used for detecting different sweat components. This application sets up the electrode that is used for detecting different sweat compositions in the sweat sensor, and every reference electrode corresponds at least one working electrode, and detection range is wide and the integrated level is high.
Description
Technical Field
The application relates to the technical field of sensors, in particular to a sweat sensor, an integrated electrode array and a preparation method of the sweat sensor.
Background
The wearable biosensor can realize continuous and noninvasive detection of various indexes of a human body, and plays an increasingly important role in modern medical treatment. Sweat is used as a biological fluid, contains rich biomarkers, can be used for monitoring physiological states and diagnosing related diseases, is convenient for noninvasive collection due to the fact that sweat is generated by sweat glands on the body surface, and has been widely applied to the fields of mobile health diagnosis, motion monitoring and the like. At present, researchers at home and abroad carry out a lot of work around wearable sweat sensors and obtain a series of achievements, but most of the wearable sweat sensors still have the problems of few detection components and low integration level.
Disclosure of Invention
In order to solve the technical problems, the application provides a sweat sensor, an integrated electrode array and a preparation method thereof, which can solve the problems of few detection components and low integration level of the existing sweat sensor.
In order to solve the above technical problem, the present application provides an integrated electrode array of a sweat sensor, comprising a first electrode set for detecting organic components in sweat and a second electrode set for detecting inorganic components in sweat, wherein the first electrode set and the second electrode set each comprise at least two working electrodes and at least one reference electrode, each of the reference electrodes corresponds to at least one of the working electrodes, and different working electrodes are used for detecting different sweat components.
The first electrode group comprises a first working electrode, a second working electrode and a first reference electrode, the first working electrode and the second working electrode respectively form a detection loop with the first reference electrode, and the first working electrode and the second working electrode are used for detecting different organic components in sweat.
The second electrode group comprises a third working electrode, a fourth working electrode and a second reference electrode, the third working electrode and the fourth working electrode respectively form a detection loop with the second reference electrode, and the third working electrode and the fourth working electrode are used for detecting different inorganic components in sweat.
The temperature detection device also comprises a temperature detection electrode which is a grid-shaped lead.
Wherein one of the working electrodes in the second electrode set is used for detecting hydrogen ions in sweat.
The electrode assembly further comprises a base layer and an encapsulation layer, wherein the first electrode group and the second electrode group are arranged on the base layer, and the encapsulation layer is arranged on the first electrode group and the second electrode group and exposes the corresponding working electrode and the corresponding reference electrode.
Wherein the integrated electrode array further comprises a plurality of through holes penetrating through the integrated electrode array in the thickness direction, the plurality of through holes are positioned at the working electrode and the reference electrode, and sweat entering the integrated electrode array is discharged through the plurality of through holes.
The present application also provides a method of making an integrated electrode array for a sweat sensor, comprising:
a. manufacturing a first patterned metal layer, wherein the first patterned metal layer comprises a first electrode group pattern and a second electrode group pattern, the first electrode group pattern and the second electrode group pattern respectively comprise at least two first electrode patterns and at least one second electrode pattern, and each second electrode pattern corresponds to at least one first electrode pattern;
b. manufacturing a second patterned metal layer, wherein the second patterned metal layer corresponds to the second electrode pattern below and has the same pattern, and forming a reference electrode without surface modification;
c. the method comprises the steps of surface modifying a first electrode pattern of the first electrode set pattern to form a working electrode for detecting different organic components in sweat, surface modifying a first electrode pattern of the second electrode set pattern to form a working electrode for detecting different inorganic components in sweat, and optionally surface modifying the reference electrode.
Wherein, step a, include:
the method comprises the steps of manufacturing a first patterned metal layer on a base layer, wherein the first patterned metal layer comprises a first electrode group pattern and a second electrode group pattern, and the first electrode group pattern and the second electrode group pattern respectively comprise at least two first electrode patterns and at least one second electrode pattern.
Wherein, before step b, further comprising:
d01. forming an encapsulation layer on the first patterned metal layer;
d02. and removing the part of the packaging layer covering the first electrode pattern and the second electrode pattern.
Wherein the first electrode pattern and the second electrode pattern each include a plurality of through holes, and step d02 further includes:
removing portions of the base layer corresponding to the plurality of through holes.
In step a, the first patterned metal layer further includes a pattern of a third electrode, the pattern of the third electrode is in a grid shape, and the third electrode is used for detecting temperature.
Wherein, step c, include:
and performing surface modification on one first electrode pattern in the second electrode group patterns to obtain a working electrode for detecting hydrogen ions in sweat.
The application also provides an integrated electrode array of the sweat sensor, which is prepared by the preparation method of the integrated electrode array of the sweat sensor.
The present application also provides a sweat sensor comprising an integrated electrode array of a sweat sensor as described above.
The application discloses integrated electrode array of sweat sensor, including the first electrode group that is arranged in detecting organic composition in the sweat and the second electrode group that is arranged in detecting inorganic composition in the sweat, first electrode group and second electrode group all include two at least working electrodes and at least one reference electrode, and different working electrodes are used for detecting different sweat compositions, through set up the electrode that is used for detecting different sweat compositions in the sweat sensor, and the quantity of reference electrode is less than the quantity of working electrode for the detection range of sweat sensor is wide and the integration is high.
The preparation method of the sweat sensor integrated electrode array comprises the steps of firstly manufacturing a first patterned metal layer, wherein the first patterned metal layer comprises a first electrode group pattern and a second electrode group pattern, the first electrode group pattern and the second electrode group pattern respectively comprise at least two first electrode patterns and at least one second electrode pattern, and each second electrode pattern corresponds to at least one first electrode pattern; then, a second patterned metal layer is manufactured, the second patterned metal layer corresponds to the second electrode pattern positioned below the second patterned metal layer, and the pattern of the second patterned metal layer is consistent with that of the second electrode pattern positioned below the second patterned metal layer, so that a reference electrode without surface modification is formed; finally, surface modification is carried out on the first electrode patterns in the first electrode group patterns to form working electrodes for detecting different organic components in sweat, surface modification is carried out on the first electrode patterns in the second electrode group patterns to form working electrodes for detecting different inorganic components in sweat, and surface modification is optionally carried out on the reference electrodes to finally obtain the integrated electrode array. The process is simple and the preparation cost is low.
Drawings
Fig. 1 is a schematic diagram of the structure of an integrated electrode array of a sweat sensor shown according to a first embodiment;
FIG. 2 is a schematic diagram of the structure of an integrated electrode array of a sweat sensor according to a second embodiment;
fig. 3 is a schematic flow diagram of a method of manufacturing an integrated electrode array for a sweat sensor according to a third embodiment;
fig. 4(a) to 4(e) are partial process schematic diagrams of a method of manufacturing an integrated electrode array of a sweat sensor according to a third embodiment.
Detailed Description
The following description of the embodiments of the present application is provided for illustrative purposes, and other advantages and capabilities of the present application will become apparent to those skilled in the art from the present disclosure.
In the following description, reference is made to the accompanying drawings that describe several embodiments of the application. It is to be understood that other embodiments may be utilized and that mechanical, structural, electrical, and operational changes may be made without departing from the spirit and scope of the present application. The following detailed description is not to be taken in a limiting sense, and the scope of embodiments of the present application is defined only by the claims of the issued patent. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.
Although the terms first, second, etc. may be used herein to describe various elements in some instances, these elements should not be limited by these terms. These terms are only used to distinguish one element from another.
Also, as used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context indicates otherwise. It will be further understood that the terms "comprises," "comprising," "includes" and/or "including," when used in this specification, specify the presence of stated features, steps, operations, elements, components, items, species, and/or groups, but do not preclude the presence, or addition of one or more other features, steps, operations, elements, components, species, and/or groups thereof. The terms "or" and/or "as used herein are to be construed as inclusive or meaning any one or any combination. Thus, "A, B or C" or "A, B and/or C" means "any of the following: a; b; c; a and B; a and C; b and C; A. b and C ". An exception to this definition will occur only when a combination of elements, functions, steps or operations are inherently mutually exclusive in some way.
First embodiment
Fig. 1 is a schematic diagram of the structure of an integrated electrode array of a sweat sensor shown according to a first embodiment. Referring to fig. 1, the integrated electrode array 10 of the sweat sensor of the present embodiment includes a first electrode set 11 and a second electrode set 12, in the present embodiment, the first electrode set 11 is used for detecting organic components in sweat, including but not limited to glucose and lactic acid, the second electrode set 12 is used for detecting inorganic components in sweat, including but not limited to sodium ions, potassium ions, calcium ions, chloride ions, and hydrogen ions, and the number of the first electrode set 11 and the second electrode set 12 is not limited to one.
First electrode set 11 and second electrode set 12 each include at least two working electrodes and at least one reference electrode, one corresponding to at least one working electrode, with different working electrodes being used to detect different sweat components. In the present embodiment, the first electrode group 11 includes a first working electrode 111, a second working electrode 112 and a first reference electrode 113, the second electrode group 12 includes a third working electrode 121, a fourth working electrode 122 and a second reference electrode 123, each working electrode is semicircular and has a diameter not less than 3mm, and each reference electrode is strip-shaped and is disposed between two corresponding working electrodes. It can be understood that the shape, size and arrangement of the electrodes can be adjusted according to the actual use requirement, and are not limited to the figures.
When the electrochemical workstation is used, the first working electrode 111 and the second working electrode 112 are respectively connected with two working electrode ends in the electrochemical workstation, the first reference electrode 113 is simultaneously connected with a reference electrode end and a counter electrode end of the electrochemical workstation, the third working electrode 121 and the fourth working electrode 122 are respectively connected with the other two working electrode ends of the electrochemical workstation, and the second reference electrode 123 is simultaneously connected with the other set of reference electrode end and the counter electrode end of the electrochemical workstation. When the integrated electrode array 10 works, a potential difference is formed between the working electrode and the corresponding reference electrode, and meanwhile, a conductive loop is formed between the working electrode and the corresponding reference electrode (which is also used as a counter electrode), that is, the first working electrode 111 and the second working electrode 112 respectively form a detection loop with the first reference electrode 113, and the third working electrode 121 and the fourth working electrode 122 respectively form a detection loop with the second reference electrode 123.
That is, in each electrode group, one reference electrode may correspond to at least two working electrodes, but the present invention is not limited to the form in which one reference electrode only corresponds to one working electrode may be additionally present in each electrode group, and by sharing the reference electrode, the electrode structure can be highly integrated, and the size of the device is not greatly increased while a large detection range and detection accuracy are ensured.
In this embodiment, the first working electrode 111 is used for detecting glucose in sweat, the second working electrode 112 is used for detecting lactate in sweat, and one of the working electrodes in the second electrode set 12 is used for detecting hydrogen ions in sweat, wherein one of the third working electrode 121 and the fourth working electrode 122 is used for detecting hydrogen ions in sweat, and the other of the third working electrode 121 and the fourth working electrode 122 is used for detecting sodium ions or potassium ions in sweat.
In this embodiment, a conductive layer such as gold (Au), copper (Cu), carbon, or the like is used for each working electrode, and a conductive layer such as silver/silver chloride (Ag/AgCl) is used for each reference electrode. The working electrodes for detecting glucose and lactic acid share the same group of Ag/AgCl electrodes as reference electrodes, the working electrodes for detecting sodium ions and hydrogen ions share the same group of Ag/AgCl electrodes modified by polyvinyl butyral (PVB) as reference electrodes, and then different working electrodes are functionally modified by using specific sensitive materials such as enzyme, ion selective membranes and the like, so that synchronous detection of different components in sweat is realized. Wherein, for the ion components in the sweat, such as sodium ions, hydrogen ions and the like, the corresponding working electrode can be modified by dripping a specific ion exchange membrane, such as sodium ion carriers and the like, so as to output the change curve of the membrane potential along with the ion concentration when detecting, and for the organic components in the sweat, such as glucose, lactic acid and the like, the corresponding working electrode can be modified by coating corresponding enzymes, such as glucose oxidase, lactic acid oxidase and the like, so as to output the change curve of the redox current along with the concentration of a target detection object when detecting.
Further, the integrated electrode array 10 of the sweat sensor may also include temperature sensing electrodes 13. In the present embodiment, the temperature detection electrode 13 is a grid-shaped wire, and the temperature of the skin or the environment can be known by detecting the change of the resistance value of the temperature detection electrode 13 with the temperature.
When one of the third working electrode 121 and the fourth working electrode 122 is used for detecting hydrogen ions in sweat, and the integrated electrode array 10 may further include the temperature detection electrode 13, by detecting the change of the concentration of hydrogen ions in sweat, the pH change of sweat may be known, by detecting the change of the resistance value of the temperature detection electrode 13 with temperature, the temperature of skin or environment may be known, and further, based on the response curve of the signals of different detection components with the change of temperature and pH, the detection signals of various sweat components may be calibrated in real time, so as to improve the accuracy of the detection result, and well solve the problem that the sweat sensor faces multi-component synchronous detection difficulty.
In order to make sweat smoothly pass through the integrated electrode array 10 and avoid the influence of the mixing of new and old sweat on the detection result, a passage for sweat to pass through is arranged in the integrated electrode array 10. In this embodiment, the integrated electrode array 10 further includes a plurality of through holes 15 penetrating the integrated electrode array 10 in the thickness direction, the plurality of through holes 15 being located at each of the working electrode and the reference electrode and penetrating each of the electrodes, so that sweat entering the integrated electrode array 10 can be discharged through the plurality of through holes 15. Thus, after various biomarkers in the sweat are detected by the specific electrodes, the sweat is continuously conveyed upwards through the through holes 15 on the surfaces of the electrodes and is discharged out of the body surface, and the problem that the new sweat and the old sweat are easy to mix is well solved.
The integrated electrode array of the sweat sensor of the present application comprises a first electrode set for detecting organic components in sweat and a second electrode set for detecting inorganic components in sweat, wherein the first electrode set and the second electrode set each comprise at least two working electrodes and at least one reference electrode, each reference electrode corresponds to at least one working electrode, and different working electrodes are used for detecting different sweat components. The sweat sensor is provided with the electrodes for detecting different sweat components, and each reference electrode corresponds to at least one working electrode, so that the sweat sensor is wide in detection range and high in integration level, and integration of the whole device is facilitated. In addition, a pH detection electrode and a temperature detection electrode are arranged, and the content of various components is corrected by utilizing the dependency among different detection signals, so that the synchronous measurement of various components in sweat is better realized.
Second embodiment
Fig. 2 is a schematic diagram of the structure of an integrated electrode array of a sweat sensor according to a second embodiment. Referring to fig. 2, the integrated electrode array of the present embodiment is mainly different from the first embodiment in that it further includes a substrate layer 16 and a packaging layer 17.
The first electrode set 11 and the second electrode set 12 are disposed on the substrate layer 16, the encapsulation layer 17 is disposed on the first electrode set 11 and the second electrode set 12 and exposes the corresponding working electrode and the reference electrode, and the encapsulation layer 17 covers the temperature detection electrode (refer to fig. 1) and a portion of the conductive wires. By providing the base layer 16 and the encapsulation layer 17, the overall strength and the service life of the integrated electrode array can be improved, and it can be understood that, in the integrated electrode array of the first embodiment, a thin film structure may be provided on at least one side of the first electrode group 11 and the second electrode group 12 to improve the overall strength.
In this embodiment, the integrated electrode array further includes a plurality of through holes (please refer to fig. 1) penetrating through the integrated electrode array along the thickness direction, the plurality of through holes are located at the working electrode and the reference electrode and penetrate through the electrodes, and simultaneously the plurality of through holes also penetrate through the base layer 16, when in use, one side of the encapsulation layer 17 is attached to the skin, sweat is directly contacted with the electrodes for detection after being discharged, and then is sequentially discharged from the electrodes and the base layer 16 through the through holes. Therefore, after various biomarkers in the sweat are detected by the specific electrodes, the sweat is continuously upwards transmitted through the through holes on the surfaces of the electrodes and is discharged out of the body surface, and the problem that the new sweat and the old sweat are easy to mix is well solved.
Third embodiment
Fig. 3 is a schematic flow diagram of a method of manufacturing an integrated electrode array for a sweat sensor according to a third embodiment. Referring to fig. 3, the method for manufacturing an integrated electrode array of a sweat sensor of the present embodiment includes:
In this embodiment, step 310 includes:
a first patterned metal layer is manufactured on a base layer, the first patterned metal layer comprises a first electrode group pattern and a second electrode group pattern, and the first electrode group pattern and the second electrode group pattern respectively comprise at least two first electrode patterns and at least one second electrode pattern.
Referring to fig. 4(a), firstly, a substrate 51, such as a silicon substrate, is spin-coated with polymethyl methacrylate (PMMA) and Polyimide (PI) as a sacrificial layer (not shown) and a base layer 52, respectively, and after heating and curing, referring to fig. 4(b), a chromium (Cr) layer with a thickness of 5-10nm and a gold (Au) layer with a thickness of 100-150nm are sequentially grown on the surface of the first encapsulation layer 52 by a magnetron sputtering method, so as to obtain a Cr/Au metal layer 53. Next, referring to fig. 4(c), the metal layer 53 is subjected to photolithography to obtain a first patterned metal layer, the first patterned metal layer includes a first electrode group pattern 531, a second electrode group pattern 532 and a third electrode pattern 535, in this embodiment, the third electrode pattern 535 is in a grid shape, the first electrode group pattern 531 includes two first electrode patterns 5311 and one second electrode pattern 5312, the second electrode group pattern 532 includes two first electrode patterns 5321 and one second electrode pattern 5322, the first electrode patterns 5311, the second electrode patterns 5321 and the second electrode patterns 5312, 5322 each include a plurality of through holes 533, and the plurality of through holes 533 penetrate through to the surface of the base layer 52.
In this embodiment, before step 320, the method may further include:
forming an encapsulation layer on the first patterned metal layer;
removing portions of the encapsulation layer covering the first and second electrode patterns, and removing portions of the base layer corresponding to the plurality of through holes.
Referring to fig. 4(d), spin-coating PI on the first patterned metal layer, curing to obtain a package layer 55, etching the package layer 55 with reactive ions (plasma beam), selectively removing portions of the package layer 55 covering the first electrode patterns 5311 and 5321 and the second electrode patterns 5312 and 5322, exposing regions of the first electrode patterns 5311 and 5321 and the second electrode patterns 5312 and 5322, and controlling the pattern diameters of the first electrode patterns 5311 and 5321 to be not less than 3mm, and selectively removing portions of the substrate layer 52 corresponding to the plurality of through holes 533 so that the plurality of through holes 533 penetrate through the upper and lower surfaces of the integrated electrode array.
Subsequently, referring to fig. 4(e), the entire surface of the regions of the first electrode patterns 5311, 5321 and the second electrode patterns 5312, 5322 is coated with a photoresist, the Ag growth regions of the second electrode patterns 5312, 5322 are exposed by exposure and development, then Ag with a thickness of 150-200nm is grown on the surfaces of the second electrode patterns 5312, 5322 by magnetron sputtering, the photoresist is removed to form Ag patterns corresponding to the second electrode patterns 5312, 5322, and then ferric chloride (FeCl) is dropped3) The solution etches the patterned Ag layer to obtain a second patterned metal layer 56, i.e., an Ag/AgCl layer, over the second electrode patterns 5312, 5322, the pattern of the second patterned metal layer 56 being identical to the pattern of the underlying second electrode patterns 5312, 5322, to obtain an Ag/AgCl reference electrode.
In practice, if the encapsulation layer 55 is not provided, a photoresist may be spin coated on the first patterned metal layer and removed after the second patterned metal layer 56 is obtained.
Wherein, each working electrode and each reference electrode are subjected to surface modification according to the sweat components and types to be detected to form different electrode groups, so as to obtain the integrated electrode array.
In the present embodiment, the surface modification is performed on one of the first electrode patterns 5311 in the first electrode group patterns 531 as follows:
dissolving glucose oxidase in phosphate buffer (pH)7.2), and then mixing with a 1% chitosan solution (the solvent is 2% acetic acid aqueous solution) according to a volume ratio of 1:2 to obtain a mixed enzyme solution; electrochemically depositing Prussian blue on the first electrode pattern (Cr/Au electrode), and dripping the enzyme solution on the area of the first electrode pattern with the dosage controlled at 10-50 μ L/cm2. Then, after drying at 4 ℃, crosslinking was performed at 30 ℃ for 1 hour using glutaraldehyde vapor to immobilize the enzyme, resulting in a working electrode for glucolase.
The other first electrode pattern 5311 of the first electrode group pattern 531 is surface-modified to obtain a working electrode for detecting lactic acid. In the present embodiment, the surface modification process of the other first electrode pattern 5311 in the first electrode group pattern 531 is similar to the above process, and only the glucose oxidase therein needs to be replaced with lactate oxidase.
The reference electrode 5312 in the first electrode set pattern 531 is the Ag/AgCl electrode described previously, i.e., is not modified.
In this embodiment, step 330 includes:
one of the first electrode patterns in the second electrode pattern 532 is surface modified to obtain a working electrode for detecting hydrogen ions in sweat.
Wherein, the surface modification of one of the first electrode patterns 5321 in the second electrode group pattern 532 is performed as follows:
poly (3, 4-ethylenedioxythiophene) -polystyrenesulfonic acid (PEDOT/PSS) was deposited on the corresponding first electrode pattern as an ion-electron conductive conversion element by electrochemical deposition using a mixed solution of 3, 4-ethylenedioxythiophene and poly (4-sodium styrenesulfonate) as an electrolyte. Then, sodium ionophore (Na ionophore X) is selected as an ion selective membrane to prepare an ion selective electrode as a sodium ion sensitive material. Specifically, Na ionophore X (1%), sodium tetrakis (3, 5-bis (trifluoromethyl) phenyl) borate (0.55%), polyvinyl chloride (33%), bis (2-ethylhexyl) sebacate (65.45%) were dissolved in tetrahydrofuran to prepare a solution with a concentration of 15%, and the solution was applied dropwise to the first electrode pattern on which PEDOT/PSS was deposited in an amount of 10-50. mu.L/cm2And drying at room temperature to obtain the working electrode for detecting sodium ions.
Alternatively, the surface modification is performed on one of the first electrode patterns 5321 in the second electrode group pattern 532 as follows:
poly (3, 4-ethylenedioxythiophene) -polystyrenesulfonic acid (PEDOT/PSS) was deposited on the corresponding first electrode pattern as an ion-electron conductive conversion element by electrochemical deposition using a mixed solution of 3, 4-ethylenedioxythiophene and poly (4-sodium styrenesulfonate) as an electrolyte. Subsequently, valinomycin (2%), sodium tetraphenylborate (0.5%), polyvinyl chloride (32.7%), bis (2-ethylhexyl) sebacate (64.7%) were dissolved in cyclohexanone, and the solution was applied dropwise to the first electrode pattern on which PEDOT/PSS was deposited, and dried at room temperature to obtain a working electrode for detecting potassium ions.
Surface modification is performed on the other first electrode pattern 5321 of the second electrode group pattern 532 as follows:
and electrochemically depositing Polyaniline (PANI) in the area corresponding to the first electrode pattern by using 0.1M aniline and 1M hydrochloric acid as electrolyte and scanning for 30-60 times at a rate of 0.1V/s in a range of-0.2-1V (VS Ag/AgCl) to obtain the working electrode for detecting hydrogen ions.
The second electrode patterns 5322 in the second electrode group patterns 532 are surface-modified by the following process:
dissolving polyvinyl butyral (79.1mg), sodium chloride (50mg), polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (2mg) and multi-walled carbon nanotubes (0.2mg) in 1ml of methanol, dropwise coating the solution on the second electrode pattern 5322 in the second electrode group pattern 532, and drying at room temperature.
After finishing the surface modification, the integrated electrode array is peeled off from the substrate 51 for standby by dissolving PMMA with acetone. In practice, if the base layer 52 and the encapsulation layer 55 are not provided, the electrode array can be transferred to a film for storage after finishing surface modification, and then directly attached to the skin by means of transfer when needed.
After the surface modification, when sweat contacts each electrode, ions such as sodium ions, hydrogen ions and the like in the sweat are detected on the corresponding ion selective electrode, and voltage signals corresponding to the ion concentration are output; the biomass such as glucose, lactic acid and the like are detected on corresponding enzyme electrodes, and current signals corresponding to the concentrations of the biomass are output. Simultaneously, through the hydrogen ion concentration change in the detection sweat, can learn the pH change of sweat, through the resistance value that detects the third electrode pattern along with the change of temperature, can learn the temperature of sweat or skin, and then can carry out real-time calibration to the detected signal of each sweat composition along with the response curve of temperature and pH change based on the signal of different detected components. Subsequently, sweat continues to be upwards transmitted through the through holes on the surface of the electrode and is discharged out of the body surface, and signal interference caused by mixing with newly generated sweat is avoided.
The preparation method of the sweat sensor integrated electrode array comprises the steps of firstly manufacturing a first patterned metal layer, wherein the first patterned metal layer comprises a first electrode group pattern and a second electrode group pattern, the first electrode group pattern and the second electrode group pattern respectively comprise at least two first electrode patterns and at least one second electrode pattern, and each second electrode pattern corresponds to at least one first electrode pattern; then, a second patterned metal layer is manufactured, the second patterned metal layer corresponds to the second electrode pattern positioned below the second patterned metal layer, and the pattern of the second patterned metal layer is consistent with that of the second electrode pattern positioned below the second patterned metal layer, so that a reference electrode without surface modification is formed; finally, surface modification is carried out on the first electrode patterns in the first electrode group patterns to form working electrodes for detecting different organic components in sweat, surface modification is carried out on the first electrode patterns in the second electrode group patterns to form working electrodes for detecting different inorganic components in sweat, and surface modification is optionally carried out on the reference electrodes to finally obtain the integrated electrode array. The high-integration sweat sensor electrode array is prepared by a micromachining process, the integration of the whole device is facilitated, various sweat components can be synchronously detected by modifying a specific functional layer and calibrating the specific functional layer by using environmental parameters such as temperature, pH and the like, and the high-integration sweat sensor electrode array is simple in process and low in cost.
The application also provides an integrated electrode array of the sweat sensor, which is prepared by the preparation method of the integrated electrode array of the sweat sensor according to the third embodiment.
The present application also provides a sweat sensor comprising an integrated electrode array according to the first embodiment, the second embodiment, or a method of manufacturing an integrated electrode array according to the third embodiment.
The above embodiments are merely illustrative of the principles and utilities of the present application and are not intended to limit the application. Any person skilled in the art can modify or change the above-described embodiments without departing from the spirit and scope of the present application. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical concepts disclosed in the present application shall be covered by the claims of the present application.
Claims (15)
1. An integrated electrode array for a sweat sensor comprising a first electrode set for detecting organic components in sweat and a second electrode set for detecting inorganic components in sweat, said first and second electrode sets each comprising at least two working electrodes and at least one reference electrode, each said reference electrode corresponding to at least one said working electrode, a different working electrode for detecting a different sweat component.
2. The integrated electrode array of a sweat sensor of claim 1, wherein the first electrode set includes a first working electrode, a second working electrode, and a first reference electrode, the first working electrode and the second working electrode each forming a detection circuit with the first reference electrode, the first working electrode and the second working electrode being configured to detect different organic components in sweat.
3. The integrated electrode array of a sweat sensor of claim 1 or 2, wherein the second electrode set includes a third working electrode, a fourth working electrode, and a second reference electrode, the third and fourth working electrodes forming a detection circuit with the second reference electrode, respectively, the third and fourth working electrodes being for detecting different inorganic components in sweat.
4. The integrated electrode array of a sweat sensor of claim 1 further comprising a temperature sensing electrode that is a grid-like wire.
5. The integrated electrode array of a sweat sensor of claim 1 or 4, wherein one of the working electrodes in the second electrode set is used to detect hydrogen ions in sweat.
6. The integrated electrode array of a sweat sensor of claim 1 further comprising a base layer and an encapsulation layer, the first and second electrode sets being disposed on the base layer, the encapsulation layer being disposed on the first and second electrode sets and exposing the corresponding working and reference electrodes.
7. The integrated electrode array of a sweat sensor of claim 1, further comprising a plurality of through-holes through the integrated electrode array in a thickness direction, the plurality of through-holes being located at the working electrode and the reference electrode, sweat entering the integrated electrode array being expelled through the plurality of through-holes.
8. A method of making an integrated electrode array for a sweat sensor, comprising:
a. manufacturing a first patterned metal layer, wherein the first patterned metal layer comprises a first electrode group pattern and a second electrode group pattern, the first electrode group pattern and the second electrode group pattern respectively comprise at least two first electrode patterns and at least one second electrode pattern, and each second electrode pattern corresponds to at least one first electrode pattern;
b. manufacturing a second patterned metal layer, wherein the second patterned metal layer corresponds to the second electrode pattern below and has the same pattern, and forming a reference electrode without surface modification;
c. the method comprises the steps of surface modifying a first electrode pattern of the first electrode set pattern to form a working electrode for detecting different organic components in sweat, surface modifying a first electrode pattern of the second electrode set pattern to form a working electrode for detecting different inorganic components in sweat, and optionally surface modifying the reference electrode.
9. The method of manufacturing an integrated electrode array for a sweat sensor of claim 8, wherein step a, comprises:
the method comprises the steps of manufacturing a first patterned metal layer on a base layer, wherein the first patterned metal layer comprises a first electrode group pattern and a second electrode group pattern, and the first electrode group pattern and the second electrode group pattern respectively comprise at least two first electrode patterns and at least one second electrode pattern.
10. The method of manufacturing an integrated electrode array for a sweat sensor of claim 9, wherein step b is preceded by the steps of:
d01. forming an encapsulation layer on the first patterned metal layer;
d02. and removing the part of the packaging layer covering the first electrode pattern and the second electrode pattern.
11. The method of manufacturing an integrated electrode array for a sweat sensor of claim 10 wherein said first electrode pattern and said second electrode pattern each include a plurality of through holes, step d02, further comprising:
removing portions of the base layer corresponding to the plurality of through holes.
12. The method of manufacturing an integrated electrode array for a sweat sensor of claim 8 wherein in step a, the first patterned metal layer further comprises a pattern of third electrodes, the pattern of third electrodes being grid-like, the third electrodes being used to detect temperature.
13. A method of manufacturing an integrated electrode array for a sweat sensor according to claim 8 or 12 wherein step c includes:
and performing surface modification on one first electrode pattern in the second electrode group patterns to obtain a working electrode for detecting hydrogen ions in sweat.
14. An integrated electrode array for a sweat sensor, prepared using the method of manufacturing an integrated electrode array for a sweat sensor according to any one of claims 8 to 13.
15. A sweat sensor comprising an integrated electrode array of the sweat sensor of any one of claims 1 to 7, 14.
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