CN113520379A - One-way flow guide fabric-based wearable sweat sensor and preparation method thereof - Google Patents
One-way flow guide fabric-based wearable sweat sensor and preparation method thereof Download PDFInfo
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- CN113520379A CN113520379A CN202110623917.7A CN202110623917A CN113520379A CN 113520379 A CN113520379 A CN 113520379A CN 202110623917 A CN202110623917 A CN 202110623917A CN 113520379 A CN113520379 A CN 113520379A
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- 230000005661 hydrophobic surface Effects 0.000 claims abstract description 43
- 238000005507 spraying Methods 0.000 claims abstract description 36
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Images
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/145—Measuring characteristics of blood in vivo, e.g. gas concentration, pH value; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid, cerebral tissue
- A61B5/14507—Measuring characteristics of blood in vivo, e.g. gas concentration, pH value; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid, cerebral tissue specially adapted for measuring characteristics of body fluids other than blood
- A61B5/14517—Measuring characteristics of blood in vivo, e.g. gas concentration, pH value; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid, cerebral tissue specially adapted for measuring characteristics of body fluids other than blood for sweat
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/145—Measuring characteristics of blood in vivo, e.g. gas concentration, pH value; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid, cerebral tissue
- A61B5/1468—Measuring characteristics of blood in vivo, e.g. gas concentration, pH value; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid, cerebral tissue using chemical or electrochemical methods, e.g. by polarographic means
- A61B5/1477—Measuring characteristics of blood in vivo, e.g. gas concentration, pH value; Measuring characteristics of body fluids or tissues, e.g. interstitial fluid, cerebral tissue using chemical or electrochemical methods, e.g. by polarographic means non-invasive
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/68—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient
- A61B5/6801—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient specially adapted to be attached to or worn on the body surface
- A61B5/6802—Sensor mounted on worn items
Abstract
The invention relates to a one-way flow guide fabric-based wearable sweat sensor and a preparation method thereof, wherein the one-way flow guide fabric-based wearable sweat sensor comprises a sweat one-way flow guide layer and a sweat evaporation layer, wherein the substrates of the sweat one-way flow guide layer and the sweat evaporation layer are fabrics; one surface of the sweat one-way flow guide layer, which is attached to the sweat evaporation layer, is a hydrophilic surface, and the other surface of the sweat one-way flow guide layer is a hydrophobic surface; an electrode system woven by conductive fibers is embedded in the hydrophobic surface of the sweat one-way flow guide layer; the preparation method comprises the following steps: firstly, uniformly spraying a hydrophobic reagent on one side of a fabric, drying, uniformly spraying a hydrophilic reagent on the other side of the fabric, and carrying out UV (ultraviolet) photocuring to obtain a sweat one-way flow guide layer; preparing an electrode system; and weaving the electrode system into a hydrophobic surface embedded in the sweat one-way flow guide layer, and tightly attaching and sewing the hydrophilic fabric and the hydrophilic surface of the sweat one-way flow guide layer to prepare the one-way flow guide fabric-based wearable sweat sensor. The sweat sensor disclosed by the invention is combined with a sweat one-way flow guiding technology, so that the sweat in-situ real-time monitoring is realized, and the detection error is reduced.
Description
Technical Field
The invention belongs to the technical field of wearable sweat sensors, and relates to a one-way flow guide fabric-based wearable sweat sensor and a preparation method thereof.
Background
With the development of portable medical systems, real-time monitoring of various physiological markers related to human health is receiving much attention. Compared with conventional detection of blood, urine and saliva, the sweat sensor has the advantages of non-invasive and real-time continuous monitoring and the like, and various metabolites such as glucose, lactic acid, sodium ions, potassium ions and ammonium ions in sweat components can reflect the physiological health state of a human body in a relevant manner, so that the research of the wearable sweat sensor has important value and significance in the aspects of health monitoring disease prevention and the like.
Currently, the difficulty in research and development of wearable sweat sensors mainly lies in the aspects of selection of carrier substrates, acquisition of samples, preparation of electrode systems, design of signal transmission and the like, and requirements for wearable comfort, noninvasive continuous monitoring, wireless transmission, portable operation and the like need to be met.
The Chinese patent with the application number of 201810949363.8 provides a body surface sweat electrochemical sensor with a folded paper structure, which can collect, guide and evaporate sweat, and ensures real-time update of the sweat monitored by the electrochemical sensor. However, the sensor has a complex structure layer, and is difficult to bend, deform and repeatedly use for multiple times by taking a paper material as a substrate.
The chinese patent with application number 201810597277.5 provides a super-saturation sweat sensor to the sensor travelling comfort is given to flexible PET substrate, overcomes the collection of sweat and the not enough problem of immobilization monitoring. The sensor still uses the extensible PET material as a substrate, the stretching wearability and the air permeability are not good enough, and when sweat is detected in the super-hydrophilic micro-well detection area for a long time, the sweat can be stored and retained in the sensor, so that the detection result is inaccurate.
The Chinese patent with the application number of 2018114047835.3 provides a human body sweat real-time monitoring sensing system, through setting up the reactant in the multilayer micropore pipeline in the sensing chip, sweat reacts with the reactant of pipeline inner wall when flowing through the micropore pipeline to produce the signal of telecommunication. But when long-time detection is carried out, sweat can be accumulated on the surface of the sensor, and the wearing comfort and the detection accuracy are affected.
Although the research on existing wearable sweat sensors has been developed in different degrees, there are several problems in the prior art: 1. the existing sweat sensor carrier is mainly a polymer or a ductile substrate such as a chip array, and does not have the wearability of stretching, bending, deforming and the like in a true sense. 2. The long stagnation, accumulation and leaving of sweat on the sensor during the detection process can affect the accuracy of the detection result. 3. The sensor electrode directly contacts with skin, and sweat is accumulated on the skin surface during detection, and cannot be discharged in time after detection, so that a cool and dry detection and wearing comfort environment is difficult to create.
Therefore, it is necessary and important to develop a wearable sweat sensor based on unidirectional flow-guiding fabric, the fabric substrate and the conductive fibers can endow the sensor with natural flexibility and wearability, and the unidirectional flow-guiding function can reduce detection errors caused by sweat stagnation and create a fresh and dry detection environment.
Disclosure of Invention
The invention aims to solve the technical problems that in the prior art, a sweat sensor is poor in inherent flexibility of a substrate and an electrode material, inaccurate in detection due to the fact that sweat stagnates on the surface, poor in wearable comfort and the like, and provides a one-way flow guide fabric-based wearable sweat sensor and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a wearable sweat sensor based on a one-way flow guide fabric comprises a sweat one-way flow guide layer and a sweat evaporation layer which are mutually attached, wherein the substrates of the sweat one-way flow guide layer and the sweat evaporation layer are both fabrics;
one surface of the sweat one-way flow guide layer, which is attached to the sweat evaporation layer, is a hydrophilic surface, and the other surface of the sweat one-way flow guide layer is a hydrophobic surface; the hydrophilic surface faces inwards to be contacted with the sweat evaporation layer, the hydrophobic surface faces outwards to be contacted with the skin, and the sweat can be only led into the hydrophilic surface from the hydrophobic surface in a one-way mode after being secreted by the skin;
an electrode system woven by conductive fibers is embedded in the hydrophobic surface of the sweat one-way flow guide layer.
As a preferred technical scheme:
the wearable sweat sensor based on the unidirectional flow guide fabric is characterized in that the electrode system is provided with a port for connecting an electrochemical detection system;
the electrochemical detection system is a fixed electrochemical workstation, a miniature electrochemical workstation or an electrochemical detection chip.
In the wearable sweat sensor based on the unidirectional flow guide fabric, the hydrophilic surface of the sweat unidirectional flow guide layer is sewn with the evaporation layer.
According to the wearable sweat sensor based on the one-way flow guide fabric, the base fabric of the sweat one-way flow guide layer is more than one of cotton, terylene and nylon; the base fabric of the sweat evaporation layer is cotton fabric.
The wearable sweat sensor based on the unidirectional flow guide fabric is characterized in that the conductive fibers are more than one of commercial carbon fibers, graphene conductive fibers and carbon nanotube conductive fibers.
The wearable sweat sensor with the unidirectional flow guide fabric base is characterized in that the detection response time of the wearable sweat sensor with the unidirectional flow guide fabric base is 5-25s (a potential signal is suddenly increased from zero to a stable state within a certain time, the sudden increase time is the response time), the detection sensitivity is 80-110 mV/decade (the potential signal and the logarithm of the concentration of a detection liquid form a linear relation of a linear function, the slope of the linear function is the sensitivity), the linear correlation between an electric signal and the concentration of a detection reactant is 0.99-0.9999 (the linear correlation index is obtained by calculating and fitting the data between the concentration of a substance obtained by testing and the electric signal and is not obtained by directly testing an experiment, the linear correlation is usually used for representing the relation between the concentration of the detection substance of the sweat sensor and the strength of the electric signal, the closer the value of the linear correlation is to 1, the better the correlation is, to further assist in indicating the accuracy of the detection of the sensor).
A method of making a one-way flow guide fabric-based wearable sweat sensor as described above, comprising the steps of:
(1) preparing a sweat one-way flow guide layer;
firstly, uniformly spraying a hydrophobic reagent on one side of a fabric, drying, uniformly spraying a hydrophilic reagent on the other side of the fabric, and carrying out UV (ultraviolet) photocuring to obtain a sweat one-way flow guide layer; respectively spraying a hydrophobic reagent and a hydrophilic reagent on two sides of the fabric to construct asymmetric wettability, thereby realizing wettability gradient to endow the substrate fabric with a sweat one-way flow guide function;
(2) preparing an electrode system;
the electrode system consists of a working electrode, a counter electrode and a reference electrode, wherein the working electrode is Na+、K+、NH4 +Or a pH working electrode; the base material of the electrode system is conductive fiber;
the conductive fiber is functionally modified by a corresponding selective sensitive film to obtain Na+、K+、NH4 +Or a pH working electrode; coating and functionally modifying the conductive fiber with Ag/AgCl slurry (Ag/AgCl slurry appears in Chinese invention patents and documents, the functional modification is to improve the performance of a chemical biosensor by a common means, and different treatment methods are adopted according to different objects, wherein the treatment methods are modified by mixed solution of polyvinyl butyral, saturated sodium chloride, polyoxyethylene polyoxypropylene segmented copolymer F-127 and methanol) to obtain a reference electrode; directly taking the conductive fiber as a counter electrode or pretreating the conductive fiber in a mixed solvent of ethanol and acetone by using an ultrasonic cleaning machine to be used as the counter electrode;
(3) the electrode system in the step (2) is woven and embedded into the hydrophobic surface of the sweat one-way flow guide layer prepared in the step (1), meanwhile, the hydrophilic fabric and the hydrophilic surface of the sweat one-way flow guide layer are tightly attached and sewn to prepare the one-way flow guide fabric-based wearable sweat sensor, and when sweat flows through the electrode system from the hydrophobic surface to the hydrophilic surface rapidly and unidirectionally, Na in the sweat can be detected+、K+、NH4 +Or physiological substance electric signals such as pH value.
As a preferred technical scheme:
in the method, the step (1) of spraying the hydrophobic agent on one side of the fabric is specifically as follows: under the constant pressure of the spray gun of 1-5 kgf/cm2Then, keeping a vertical distance of 30-80 cm between a spray gun opening and the fabric, uniformly spraying a hydrophobic reagent on one side of the fabric, controlling the spraying amount of the hydrophobic reagent to be 20-100 mg, preheating, and baking for 40-80 min at the temperature of 100-150 ℃;
spraying a hydrophilic agent on the other side of the fabric specifically comprises the following steps: under the constant pressure of the spray gun of 1-5 kgf/cm2And keeping the vertical distance of 20-60 cm between the nozzle of the spray gun and the fabric, uniformly spraying a hydrophilic reagent on the other side of the fabric, controlling the spraying amount of the hydrophilic reagent to be 100-200 mg, and then placing the fabric under a UV (ultraviolet) photocuring instrument for photocatalysis for 40-80 min.
In the method, the hydrophobic reagent in the step (1) is a mixed solution of waterborne polyurethane, siloxane, micro-nano particles, a cross-linking agent and water; the water-based polyurethane is preferably modified polyurethane emulsion, and the modified polyurethane emulsion and the preparation method thereof refer to the preparation method in Chinese patent 201910998628.8; the siloxane is preferably a long carbon chain siloxane, more preferably hexadecyltrimethylsilane; the micro-nano particles are preferably silica nano particles; the crosslinking agent is preferably an isocyanate crosslinking agent, more preferably isophorone diisocyanate; the mass ratio of the waterborne polyurethane to the siloxane to the micro-nano particles to the cross-linking agent is 1.5-2.5: 2.5-3.5: 0.8-1.2, and the volume content of water in the hydrophobic reagent is 75-90%.
The hydrophilic reagent is a mixed solution of a hydrophilic monomer, a cross-linking agent, an organic solvent and a photoinitiator; the hydrophilic monomer is preferably an acrylate hydrophilic monomer, and more preferably methacrylic acid; the cross-linking agent is more than one of N-hydroxymethyl acrylamide, 2-hydroxyethyl methacrylate and polyethylene glycol diacrylate, and more preferably the polyethylene glycol diacrylate with hydrophilicity and bifunctional groups; the organic solvent is more than one of acetone, tetrahydrofuran and toluene, and acetone is more preferable; the photoinitiator is more than one of 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxycyclohexyl phenyl ketone and 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone, and is more preferably 2-hydroxy-2-methyl-1-phenyl-1-acetone; the mass ratio of the hydrophilic monomer to the cross-linking agent to the photoinitiator is 8-12: 1-3: 0.4-1, and the volume content of the organic solvent in the hydrophilic agent is 60-80%. .
In the method described above, the electrode system of step (2) is provided with a port.
The principle of the invention is as follows:
the one-way flow guide layer of the sweat sensor provides a place for one-way flow guide and sweat detection, and the sweat evaporation layer can quickly evaporate the detected sweat to the outside. After sweat is secreted by skin, the sweat is directly contacted with the hydrophobic surface of the unidirectional flow guide layer and is simultaneously contacted with the electrode system embedded in the hydrophobic surface, when the sweat penetrates from the hydrophobic surface to the hydrophilic surface in a unidirectional way, the electrode system can rapidly respond to corresponding physiological substance components in the sweat, corresponding potential or current signal intensity is generated according to different physiological substance concentrations, and the potential or current signal intensity and the concentration of the substance components in the sweat are in a near-linear relation, so that the sweat physiological substance components which are not in a normal concentration range can be judged, and reference information is provided for human body health monitoring disease prevention. It should be noted that, the base material of the unidirectional flow guiding layer, the sweat evaporating layer and the electrode system is fiber or fabric, which can endow the sensor with good wearability and comfort, and the detection system is on the hydrophobic surface, the sweat monitoring is completed in the unidirectional flow guiding real-time process, which can keep the skin contact surface dry and cool and improve the detection accuracy.
Has the advantages that:
(1) the sweat sensor selects the fabric with inherent flexibility as the substrate, selects the conductive fibers as the electrode material and is woven and embedded into the substrate to be integrated, and the sensor is endowed with good daily wearability such as stretching, deformation and bending.
(2) The sweat sensor disclosed by the invention is combined with a sweat one-way flow guiding technology, so that the sweat can be monitored in situ in real time in a dynamic process of unidirectionally transmitting sweat to the outside from a hydrophobic surface close to the skin, the detection error caused by sweat stagnation is reduced, and the sensor can be kept dry and cool in contact with the skin, so that the wearing comfort is improved.
(3) The sweat sensor provided by the invention adopts the all-fiber fabric as a raw material, and can be prepared by simply carrying out processing in ways of spraying, pouring or electropolymerization deposition and the like, so that the sweat sensor is low in cost, simple and easy to prepare, convenient to wear and unload, wide in monitoring concentration range of physiological substances in sweat components, high in signal sensitivity and good in repeatability.
Drawings
Fig. 1 is a schematic view of a one-way flow-directing textile-based wearable sweat sensor of embodiment 1 of the present invention;
fig. 2 is a unidirectional flow guide performance test of the unidirectional flow guide fabric substrate prepared in example 1 by using a contact angle meter;
FIG. 3 is a simulated sweat test of the sweat Na ion sensor prepared in example 1 using an electrochemical workstation;
FIG. 4 is a statistical analysis of the results of simulated sweat testing using an electrochemical workstation and comparative example 1;
FIG. 5 is a statistical analysis of the results of simulated sweat testing using an electrochemical workstation in accordance with example 1;
FIG. 6 shows the detection of anti-interference and ion-selective performance of the sweat Na-ion sensor prepared in example 1 using an electrochemical workstation;
FIG. 7 is a repeated measurement of the sweat Na ion sensor prepared in example 1 using an electrochemical workstation;
FIG. 8 is a simulated sweat test of the sweat potassium ion sensor prepared in example 2 using an electrochemical workstation;
FIG. 9 is a simulated sweat test using an electrochemical workstation on a sweat pH sensor prepared in example 3;
FIG. 10 shows the application of a mini electrochemical workstation to sweat NH prepared in example 44 +The sensor carries out simulated sweat detection;
wherein, 1-sweat single-direction flow guide layer, 2-sweat evaporation layer, 3-hydrophobic surface, 4-hydrophilic surface, 5-working electrode, 6-counter electrode and 7-reference electrode.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
A preparation method of a one-way flow guide fabric-based wearable sweat sensor comprises the following specific steps:
(1) preparing a sweat one-way flow guide layer;
at a constant lance pressure of 1kgf/cm2Then, keeping a vertical distance of 30cm between a spray gun opening and the cotton fabric, uniformly spraying a hydrophobic reagent on one side of the fabric, controlling the spraying amount of the hydrophobic reagent to be 20mg, preheating, and baking for 80min at the temperature of 100 ℃; then the pressure of the spray gun is constant and 1kgf/cm2Then, keeping a vertical distance of 20cm between a spray gun opening and the fabric, uniformly spraying a hydrophilic reagent on the other side of the fabric, controlling the spraying amount of the hydrophilic reagent to be 100mg, and then placing the fabric under a UV (ultraviolet) photocuring instrument for photocatalysis for 40min to obtain a sweat one-way diversion layer;
the hydrophobic reagent is a mixed solution of waterborne polyurethane (modified polyurethane emulsion, the preparation method refers to Chinese patent 201910998628.8), hexadecyltrimethylsilane, silicon dioxide nanoparticles, isophorone diisocyanate and water; the mass ratio of the waterborne polyurethane to the hexadecyl trimethyl siloxane to the silicon dioxide nano particles to the isophorone diisocyanate is 1.5:1.5:2.5:0.8, and the volume content of water in the hydrophobic reagent is 75%;
the hydrophilic reagent is a mixed solution of methacrylic acid, N-hydroxymethyl acrylamide, acetone and 2-hydroxy-2-methyl-1-phenyl-1-acetone; the mass ratio of the methacrylic acid to the N-hydroxymethyl acrylamide to the 2-hydroxy-2-methyl-1-phenyl-1-acetone is 8:3:0.4, and the volume content of the acetone in the hydrophilic reagent is 60 percent;
(2) preparing an electrode system;
the electrode system is operatedThe electrode, the reference electrode and the counter electrode are formed, and the working electrode is Na+A working electrode;
the substrate of the electrode system is commercial carbon fiber; the electrode system is provided with a port for connecting an electrochemical detection system; the electrochemical detection system is a fixed electrochemical workstation;
(3) and (3) weaving the electrode system obtained in the step (2) to be embedded into the hydrophobic surface of the sweat single-direction flow guide layer prepared in the step (1), and meanwhile, tightly attaching and sewing the cotton fabric and the hydrophilic surface of the sweat single-direction flow guide layer to obtain the one-direction flow guide fabric-based wearable sweat sensor.
The prepared one-way flow guide fabric-based wearable sweat sensor comprises a sweat one-way flow guide layer 1 and a sweat evaporation layer 2 (cotton fabric) which are sewn together, as shown in figure 1; one surface of the sweat one-way guiding layer 1 sewn together with the sweat evaporating layer 2 is a hydrophilic surface 4, and the other surface is a hydrophobic surface 3; the hydrophilic surface 4 is inwards contacted with the sweat evaporation layer 2, the hydrophobic surface 3 is outwards contacted with the skin, and the sweat can be unidirectionally led into the hydrophilic surface 4 from the hydrophobic surface 3 after being secreted by the skin; an electrode system (composed of a working electrode 5, a counter electrode 6 and a reference electrode 7) woven by conductive fibers is embedded in the hydrophobic surface 3 of the sweat one-way flow guide layer. As shown in fig. 2, the prepared unidirectional flow guide fabric substrate was subjected to unidirectional flow guide performance test using a contact angle meter; when the liquid drops are dripped from the hydrophobic surface, the hydrophobic surface initially shows the action of repelling the liquid drops, and the liquid drops gradually seep and penetrate to the hydrophilic surface along with the prolonging of time and finally are separated from the hydrophilic surface; when the liquid drops are dripped from the hydrophilic surface, the hydrophilic surface shows stronger lyophilic behavior at the beginning, and the liquid drops quickly spread out and wet the whole surface along with the prolonging of time; test results show that the prepared unidirectional flow guide fabric substrate has obvious unidirectional flow guide behavior, namely liquid drops can only be guided to a hydrophilic surface from a hydrophobic surface and cannot be reversely transported; an electrode system woven by conductive fibers is embedded in the hydrophobic surface of the sweat one-way flow guide layer.
Performing simulated sweat detection on the prepared one-way flow guide fabric-based wearable sweat sensor (a sweat sodium ion sensor), wherein the detection liquid is a sodium chloride solution, the detection concentration range is 10-160 mM, and the concentration covers the concentration range in real human sweat; simulating a real sweating scene, when the detection liquid is dripped into the hydrophobic surface of the unidirectional flow guide layer to be contacted with the fiber electrode, a potential signal can be generated, as shown in fig. 3, the concentration of the detection liquid is gradually increased from 10mM to 160mM every 50s, and the corresponding potential signal is also gradually increased in a step manner. The detection response time of the one-way flow guide fabric-based wearable sweat sensor is 5s, the detection sensitivity is 102mV/decade, and the linear correlation between the potential and the concentration of a detection reactant is 0.999.
Further, the sensor was tested for anti-interference and ion-selective performance in the presence of simulated multiple sweat components, with the results shown in fig. 6. The potential signals of 10mM potassium chloride, calcium chloride and ammonium chloride solutions added to 10mM sodium chloride solution, respectively, did not cause corresponding changes, whereas the potential signals increased significantly when 40mM sodium chloride solution was added. Therefore, the prepared one-way flow guide fabric-based wearable sweat sensor (sweat sodium ion sensor) has good sensitivity and selectivity for simulating sweat sodium ion detection.
Further, the one-way flow-guide fabric-based wearable sweat sensor (sweat sodium ion sensor) prepared in example 1 was subjected to a repeatability test, and the results are shown in fig. 7. After the first test, the corresponding tests are respectively carried out at intervals of 1 hour, one week and one month, and the voltage values tested at the same concentration and different time periods are similar. Therefore, the prepared sweat sensor has better stability and repeatability for simulating the detection of the sodium ions in the sweat.
Comparative example 1
A method of one-way flow guiding fabric-based wearable sweat sensor, which is substantially the same as example 1, except that in comparative example 1, a fabric without one-way flow guiding function is used as a substrate embedded with an electrode system woven by conductive fibers.
The simulated sweat detection data of the sweat sodium ion sensors prepared in example 1 and comparative example 1 were subjected to statistical analysis, and the results are shown in tables 1 to 4 and fig. 5 and 4, respectively. In FIG. 4, in comparative example 1, 10mM Na was added dropwise+After passing through a sectionThe voltage stabilized around 77.39mV with a standard deviation of 3.79 after the time response. And when sodium chloride solution with other concentration is subsequently dripped, the voltage cannot be kept stable and begins to fluctuate greatly. After the 20mM solution is added dropwise, the degree of transition of the voltage mean value is about 19.70mV, and the standard deviation reaches 16.90, which indicates that the reliability of the data is extremely low, the dispersion degree is too large, and the readability is not high. When sodium chloride solutions with the concentrations of 40mM, 80mM and 160mM are added dropwise at a constant speed of 1 μ L/s by a syringe through a syringe pump every 50s, the situation is also the same, the reading jumps greatly and the severity is expanded continuously, and the standard deviation is 18.96, 24.31 and 36.70 in sequence. Meanwhile, the average voltage difference among the concentrations is also small, and is respectively 7.18mV, 19.08mV and 10.22 mV. In fig. 5, the statistical data of example 1 shows relatively good stability. After sodium chloride solutions with different concentrations are added dropwise, the fluctuation situation and the rising trend of voltage values in a stable state are smaller under the same solution concentration, the standard deviations are within an acceptable range, the voltage mean values are respectively 75.53mV, 113.47mV, 148.49mV, 172.79mV and 199.79mV, the standard deviations under different solution concentrations are respectively 2.40, 1.56, 2.33, 1.37 and 1.84, the jump degrees are respectively 37.94mV, 35.02mV, 24.30mV and 27.01mV, and the differentiation degree of the voltage values under each concentration is better and more stable. The above results indicate that the accuracy of comparative example 1 is lower than that of example 1 because the base fabric of comparative example 1 does not have a unidirectional flow guide function, cannot guide the detection liquid to the non-detection area, and when the solution with different concentration contacts the detection area, it is mixed with the solution stored on the surface of the original detection area, so that the concentration fluctuation of the liquid to be detected actually changes, thereby affecting the detection accuracy.
Table 1 example 1 continuous monitoring of different concentrations of ion response by wearable sweat sensor
Continuation table (watch 1)
Table 2 example 1 statistical analysis of different concentrations of ion response for continuous monitoring by wearable sweat sensor
Table 3 different concentration ion response continuously monitored by the comparative example 1 wearable sweat sensor
Suzhong watch (Table 3)
Table 4 statistical analysis of different concentrations of ion response for continuous monitoring of wearable sweat sensor of comparative example 1
Example 2
A preparation method of a one-way flow guide fabric-based wearable sweat sensor comprises the following specific steps:
(1) preparing a sweat one-way flow guide layer;
at a constant lance pressure of 2kgf/cm2Then, keeping a vertical distance of 40cm between a spray gun opening and the polyester-cotton blended fabric with the mass ratio of 1:1, uniformly spraying a hydrophobic reagent on one side of the fabric, controlling the spraying amount of the hydrophobic reagent to be 40mg, preheating, and baking for 65min at 115 ℃; at a constant lance pressure of 2kgf/cm2Then, keeping a vertical distance of 30cm between a spray gun opening and the fabric, uniformly spraying a hydrophilic reagent on the other side of the fabric, controlling the spraying amount of the hydrophilic reagent to be 130mg, and then placing the fabric under a UV (ultraviolet) photocuring instrument for photocatalysis for 60min to obtain a sweat one-way diversion layer;
the hydrophobic reagent is a mixed solution of waterborne polyurethane (modified polyurethane emulsion, the preparation method refers to Chinese patent 201910998628.8), hexadecyltrimethylsilane, silicon dioxide nanoparticles, isophorone diisocyanate and water; in the mixed solution, the mass ratio of the waterborne polyurethane to the hexadecyltrimethylsilane to the silicon dioxide nano-particles to the isophorone diisocyanate is 2:2:3:1, and the volume content of water in the hydrophobic reagent is 80%;
the hydrophilic reagent is a mixed solution of methacrylic acid, 2-hydroxyethyl methacrylate, tetrahydrofuran and a photoinitiator (the mass ratio of 1:1 is 1:1, namely 1-hydroxycyclohexyl phenyl ketone and 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone); the mass ratio of the methacrylic acid to the 2-hydroxyethyl methacrylate to the photoinitiator is 10:1:0.55, and the volume content of tetrahydrofuran in the hydrophilic reagent is 70%;
(2) preparing an electrode system;
the electrode system consists of a working electrode, a counter electrode and a reference electrode, wherein the working electrode is a potassium ion working electrode;
the substrate of the electrode system is commercial carbon fiber; the electrode system is provided with a port for connecting an electrochemical detection system; the electrochemical detection system is a fixed electrochemical workstation;
(3) and (3) weaving the electrode system obtained in the step (2) to be embedded into the hydrophobic surface of the sweat single-direction flow guide layer prepared in the step (1), and meanwhile, tightly attaching and sewing the cotton fabric and the hydrophilic surface of the sweat single-direction flow guide layer to obtain the one-direction flow guide fabric-based wearable sweat sensor.
The prepared one-way flow guide fabric-based wearable sweat sensor comprises a sweat one-way flow guide layer and a sweat evaporation layer (cotton fabric) which are sewn together; one surface of the sweat one-way guiding layer sewn together with the sweat evaporating layer is a hydrophilic surface, and the other surface of the sweat one-way guiding layer is a hydrophobic surface; the hydrophilic surface faces inwards to be contacted with the sweat evaporation layer, the hydrophobic surface faces outwards to be contacted with the skin, and the sweat can be only led into the hydrophilic surface from the hydrophobic surface in a one-way mode after being secreted by the skin; an electrode system woven by conductive fibers is embedded in the hydrophobic surface of the sweat one-way flow guide layer.
Performing simulated sweat detection on the prepared one-way flow guide fabric-based wearable sweat sensor (sweat potassium ion sensor), wherein the detection liquid is a potassium chloride solution, the detection concentration range is 2-32 mM, and the concentration covers the concentration range in real human sweat; and simulating a real sweating scene, and generating a current signal when the detection liquid is dripped into the hydrophobic surface of the unidirectional current guide layer drop by drop and is contacted with the fiber electrode. As shown in FIG. 8, the concentration of the detection solution was gradually increased from 2mM to 32mM every 50 seconds, and the intensity of the corresponding current signal was also gradually increased in a stepwise manner. The detection response time of the one-way flow guide fabric-based wearable sweat sensor is 12s, the detection sensitivity is 83.3mV/decade, and the linear correlation between the potential and the concentration of a detection reactant is 0.9997. Therefore, the prepared sweat glucose sensor has better sensitivity and stability for simulating sweat glucose detection.
Example 3
A method for a one-way flow guide fabric-based wearable sweat sensor comprises the following specific steps:
(1) preparing a sweat one-way flow guide layer;
at a constant lance pressure of 4kgf/cm2Then, keeping a vertical distance of 50cm between a spray gun opening and the polyester fabric, uniformly spraying a hydrophobic reagent on one side of the fabric, controlling the spraying amount of the hydrophobic reagent to be 60mg, preheating, and baking at 130 ℃ for 50min; then the pressure of the spray gun is constant and 3kgf/cm2Then, keeping a vertical distance of 45cm between a spray gun opening and the fabric, uniformly spraying a hydrophilic reagent on the other side of the fabric, controlling the spraying amount of the hydrophilic reagent to be 160mg, and then placing the fabric under a UV (ultraviolet) photocuring instrument for photocatalysis for 70min to obtain a sweat one-way diversion layer;
the hydrophobic reagent is a mixed solution of waterborne polyurethane (modified polyurethane emulsion, the preparation method refers to Chinese patent 201910998628.8), hexadecyltrimethylsilane, silicon dioxide nanoparticles, isophorone diisocyanate and water; in the mixed solution, the mass ratio of the waterborne polyurethane to the hexadecyltrimethylsilane to the silicon dioxide nano-particles to the isophorone diisocyanate is 2.5:2.5:3:1, and the volume content of water in the hydrophobic reagent is 85%;
the hydrophilic agent is a mixed solution of methacrylic acid, polyethylene glycol diacrylate, acetone and 2-hydroxy-2-methyl-1-phenyl-1-acetone; the mass ratio of the methacrylic acid to the polyethylene glycol diacrylate to the 2-hydroxy-2-methyl-1-phenyl-1-acetone is 11:2.5:0.75, and the volume content of the acetone in the hydrophilic reagent is 75 percent;
(2) preparing an electrode system;
the electrode system consists of a working electrode, a reference electrode and a counter electrode, wherein the working electrode is a pH working electrode;
the base material of the electrode system is graphene conductive fiber; the electrode system is provided with a port for connecting an electrochemical detection system; the electrochemical detection system is a fixed electrochemical workstation;
(3) and (3) weaving the electrode system obtained in the step (2) to be embedded into the hydrophobic surface of the sweat single-direction flow guide layer prepared in the step (1), and meanwhile, tightly attaching and sewing the cotton fabric and the hydrophilic surface of the sweat single-direction flow guide layer to obtain the one-direction flow guide fabric-based wearable sweat sensor.
The prepared one-way flow guide fabric-based wearable sweat sensor comprises a sweat one-way flow guide layer and a sweat evaporation layer (cotton fabric) which are sewn together; one surface of the sweat one-way guiding layer sewn together with the sweat evaporating layer is a hydrophilic surface, and the other surface of the sweat one-way guiding layer is a hydrophobic surface; the hydrophilic surface faces inwards to be contacted with the sweat evaporation layer, the hydrophobic surface faces outwards to be contacted with the skin, and the sweat can be only led into the hydrophilic surface from the hydrophobic surface in a one-way mode after being secreted by the skin; an electrode system woven by conductive fibers is embedded in the hydrophobic surface of the sweat one-way flow guide layer.
As shown in fig. 9, the pH value was gradually changed from 7 to 3 every 50 seconds, and the corresponding current signal intensity was also gradually increased in a stepwise manner. The detection response time of the one-way flow guide fabric-based wearable sweat sensor is 18s, the detection sensitivity is 80mV/decade, and the linear correlation between the potential and the concentration of a detection reactant is 0.9999. Therefore, the prepared one-way flow guide fabric-based wearable sweat sensor (sweat pH sensor) has better sensitivity and stability for simulating sweat pH detection.
Example 4
A method for a one-way flow guide fabric-based wearable sweat sensor comprises the following specific steps:
(1) preparing a sweat one-way flow guide layer;
at a constant lance pressure of 5kgf/cm2Then, keeping a vertical distance of 60cm between a spray gun opening and the chinlon fabric, uniformly spraying a hydrophobic reagent on one side of the fabric, controlling the spraying amount of the hydrophobic reagent to be 80mg, preheating, and baking for 40min at 150 ℃; at a constant lance pressure of 5kgf/cm2Then, keeping a vertical distance of 60cm between a spray gun opening and the fabric, uniformly spraying a hydrophilic reagent on the other side of the fabric, controlling the spraying amount of the hydrophilic reagent to be 200mg, and then placing the fabric under a UV (ultraviolet) photocuring instrument for photocatalysis for 80min to obtain a sweat one-way diversion layer;
the hydrophobic reagent is a mixed solution of waterborne polyurethane (modified polyurethane emulsion, the preparation method refers to Chinese patent 201910998628.8), hexadecyltrimethylsilane, silicon dioxide nanoparticles, isophorone diisocyanate and water; in the mixed solution, the mass ratio of the waterborne polyurethane to the hexadecyltrimethylsilane to the silicon dioxide nano-particles to the isophorone diisocyanate is 2.5:2.5:3.5:1.2, and the volume content of water in the hydrophobic reagent is 90%;
the hydrophilic agent is a mixed solution of methacrylic acid, N-hydroxymethyl acrylamide, toluene and a photoinitiator (the mass ratio of 1:1 is 1:1, namely 1-hydroxycyclohexyl phenyl ketone and 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone); the mass ratio of the methacrylic acid to the N-hydroxymethyl acrylamide to the photoinitiator is 12:2:1, and the volume content of toluene in the hydrophilic reagent is 80%;
(2) preparing an electrode system;
the electrode system consists of a working electrode, a reference electrode and a counter electrode, wherein the working electrode is NH4 +A working electrode;
the base material of the electrode system is carbon nano tube conductive fiber; the electrode system is provided with a port for connecting an electrochemical detection system; the electrochemical detection system is a micro electrochemical workstation;
(3) and (3) weaving the electrode system obtained in the step (2) to be embedded into the hydrophobic surface of the sweat single-direction flow guide layer prepared in the step (1), and meanwhile, tightly attaching and sewing the cotton fabric and the hydrophilic surface of the sweat single-direction flow guide layer to obtain the one-direction flow guide fabric-based wearable sweat sensor.
The prepared one-way flow guide fabric-based wearable sweat sensor comprises a sweat one-way flow guide layer and a sweat evaporation layer (cotton fabric) which are sewn together; one surface of the sweat one-way guiding layer sewn together with the sweat evaporating layer is a hydrophilic surface, and the other surface of the sweat one-way guiding layer is a hydrophobic surface; the hydrophilic surface faces inwards to be contacted with the sweat evaporation layer, the hydrophobic surface faces outwards to be contacted with the skin, and the sweat can be only led into the hydrophilic surface from the hydrophobic surface in a one-way mode after being secreted by the skin; an electrode system woven by conductive fibers is embedded in the hydrophobic surface of the sweat one-way flow guide layer;
as shown in fig. 10, NH was applied every 50s4 +The concentration of the solution is gradually increased from 10mM to 160mM, and the corresponding potential signal intensity is also gradually increased in a step manner. The detection response time of the one-way flow guide fabric-based wearable sweat sensor is 25s, the detection sensitivity is 110mV/decade, and the linear correlation between the potential and the concentration of a detection reactant is 0.99. Thus, a one-way flow fabric-based wearable sweat sensor (sweat NH) was prepared4 +Sensor) to simulated sweat NH4 +The value detection has better sensitivity and stability.
Claims (10)
1. A wearable sweat sensor of one-way water conservancy diversion fabric base which characterized in that: the sweat single-direction flow guide layer and the sweat evaporation layer are attached to each other, and the substrates of the sweat single-direction flow guide layer and the sweat evaporation layer are both fabrics;
one surface of the sweat one-way flow guide layer, which is attached to the sweat evaporation layer, is a hydrophilic surface, and the other surface of the sweat one-way flow guide layer is a hydrophobic surface;
an electrode system woven by conductive fibers is embedded in the hydrophobic surface of the sweat one-way flow guide layer.
2. The one-way flow-through fabric-based wearable sweat sensor of claim 1, wherein the electrode system is ported for connection to an electrochemical detection system;
the electrochemical detection system is a fixed electrochemical workstation, a miniature electrochemical workstation or an electrochemical detection chip.
3. The wearable sweat sensor of claim 1, wherein the hydrophilic side of the sweat unitary wicking layer is stitched to the sweat evaporation layer.
4. The wearable sweat sensor with unidirectional flow guiding textile substrate of claim 1, wherein the base textile of the sweat unidirectional flow guiding layer is one or more of cotton, polyester and nylon; the base fabric of the sweat evaporation layer is cotton fabric.
5. The wearable sweat sensor of claim 1, wherein the conductive fibers are one or more of carbon fibers, graphene conductive fibers, and carbon nanotube conductive fibers.
6. The wearable sweat sensor with unidirectional flow guide fabric base as claimed in any of claims 1 to 5, wherein the wearable sweat sensor with unidirectional flow guide fabric base has a detection response time of 5 to 25s, a detection sensitivity of 80 to 110mV/decade, and a linear correlation between potential or current signal and detection reactant concentration of 0.99 to 0.9999.
7. A method of making a one-way flow-directing fabric-based wearable sweat sensor of any of claims 1-6 comprising the steps of:
(1) preparing a sweat one-way flow guide layer;
firstly, uniformly spraying a hydrophobic reagent on one side of a fabric, drying, uniformly spraying a hydrophilic reagent on the other side of the fabric, and carrying out UV (ultraviolet) photocuring to obtain a sweat one-way flow guide layer;
(2) preparing an electrode system;
the electrode system consists of a working electrode, a counter electrode and a reference electrode, wherein the working electrode is Na+、K+、NH4 +Or a pH value working electrode, wherein the base material of the electrode system is conductive fiber;
(3) and (3) weaving the electrode system obtained in the step (2) to be embedded into the hydrophobic surface of the sweat one-way flow guide layer prepared in the step (1), and meanwhile, tightly attaching and sewing the hydrophilic fabric and the hydrophilic surface of the sweat one-way flow guide layer to obtain the one-way flow guide fabric-based wearable sweat sensor.
8. The method according to claim 7, characterized in that the step (1) of spraying the hydrophobic agent on one side of the fabric is in particular: under the constant pressure of the spray gun of 1-5 kgf/cm2Then, keeping a vertical distance of 30-60 cm between a spray gun opening and the fabric, uniformly spraying a hydrophobic reagent on one side of the fabric, controlling the spraying amount of the hydrophobic reagent to be 20-80 mg, preheating, and baking for 40-80 min at the temperature of 100-150 ℃;
spraying a hydrophilic agent on the other side of the fabric specifically comprises the following steps: under the constant pressure of the spray gun of 1-5 kgf/cm2And keeping the vertical distance of 20-60 cm between the nozzle of the spray gun and the fabric, uniformly spraying a hydrophilic reagent on the other side of the fabric, controlling the spraying amount of the hydrophilic reagent to be 100-200 mg, and then placing the fabric under a UV (ultraviolet) photocuring instrument for photocatalysis for 40-80 min.
9. The method according to claim 7, wherein the hydrophobic reagent in step (1) is a mixed solution of aqueous polyurethane, siloxane, micro-nano particles, a cross-linking agent and water; the mass ratio of the waterborne polyurethane to the siloxane to the micro-nano particles to the cross-linking agent is 1.5-2.5: 2.5-3.5: 0.8-1.2, and the volume content of water in the hydrophobic reagent is 75-90%;
the hydrophilic reagent is a mixed solution of a hydrophilic monomer, a cross-linking agent, an organic solvent and a photoinitiator; the mass ratio of the hydrophilic monomer to the cross-linking agent to the photoinitiator is 8-12: 1-3: 0.4-1, and the volume content of the organic solvent in the hydrophilic agent is 60-80%.
10. The method of claim 7, wherein a port is left on the electrode system of step (2).
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