CN107421995B - Based on AgVO3Nanowire respiration sensor and preparation method thereof - Google Patents

Based on AgVO3Nanowire respiration sensor and preparation method thereof Download PDF

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CN107421995B
CN107421995B CN201710614210.3A CN201710614210A CN107421995B CN 107421995 B CN107421995 B CN 107421995B CN 201710614210 A CN201710614210 A CN 201710614210A CN 107421995 B CN107421995 B CN 107421995B
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agvo
nanowire
sensor
electrode layer
flexible substrate
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CN107421995A (en
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林媛
廖非易
张尚杰
姚光
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University of Electronic Science and Technology of China
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    • 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
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance

Abstract

Based on AgVO3A nano-wire respiration sensor and a preparation method thereof belong to the technical field of functional material preparation. The respiration sensor comprises a four-layer structure, which is sequentially provided with a flexible substrate, an electrode layer and AgVO from bottom to top3Nanowire functional layer andthe sensor selects an organic material with the elastic modulus of 1 GPa-4 GPa as a flexible substrate, an electrode layer is formed on the flexible substrate by adopting a photoetching process, and then AgVO is coated on the electrode layer3And finally, packaging the nanowire functional layer by adopting medical dressing to obtain the flexible respiration sensor. The respiration sensor adopts a multilayer laminated structure, and the flexible substrate has bendability and tensile resistance, so that the stable performance of the sensor is ensured; meanwhile, compared with the existing respiration monitoring device, the respiration sensor has the advantages of large change range of the detected respiration intensity, high sensitivity, good process controllability and repeatability, and is favorable for realizing large-scale batch production.

Description

Based on AgVO3Nanowire respiration sensor and preparation method thereof
Technical Field
The invention relates to the technical field of functional material preparation, in particular to a functional material based on AgVO3Preparation method of nanowire material and AgVO-based nanowire material3The structure manufacturing of the nanowire respiration sensor and a method for testing the respiration of a human body.
Background
The silver vanadate material is a functional material widely applied to the aspects of optics, electricity, catalysis and the like, and different compositions and structures can be formed according to different proportions of silver, vanadium and oxygen, such as AgVO3、Ag3VO4、Ag2V4O11And the like. Wherein, AgVO3As a simpler compound in the silver vanadate series compounds, the preparation process is simple, and the formed phase is very stable, so that the silver vanadate series compounds have wide application prospects.
Respiration is the basis of human survival, and the strength, frequency and other information of human respiration are closely related to various physiological information of human bodies, for example, compared with patients, the respiratory frequency and respiratory intensity of normal human bodies are lower than those of the patients. The detection of the respiratory frequency and the intensity is proved, so that the detection of the change condition of the human health can be facilitated, and the early warning effect on diseases such as respiratory dysfunction and the like can be realized. Currently, common breath detection methods are: measuring the strain of the breathing telescopic action; measuring pressure changes in the breathing gas inlet and outlet; and temperature of breathing gasAnd (6) measuring the rows. AgVO3As a material with excellent performance, the material has great significance for monitoring the health of human bodies if being applied to a flexible gas sensor for respiratory monitoring.
Disclosure of Invention
The invention provides a method based on AgVO3The respiration sensor adopts a non-invasive respiration detection mode, does not cause discomfort caused by human foreign body sensation after long-term monitoring, and has monitoring effect on respiration frequency, respiration intensity and the like.
The technical scheme of the invention is as follows:
based on AgVO3The respiration sensor of the nano wire comprises a four-layer structure, and a flexible substrate, an electrode layer, a functional layer and a packaging layer are sequentially arranged from bottom to top, wherein the functional layer is AgVO3A nanowire.
Further, the flexible substrate is an organic material with an elastic modulus of 1GPa to 4GPa, specifically Polyimide (PI), polyethylene terephthalate (PET), and the like; the thickness of the flexible substrate is 20-50 mu m.
Furthermore, the electrode layers are interdigital electrodes, parallel electrodes and the like, and the distance between the electrodes is 50-200 mu m; the electrode layer is made of conductive materials such as gold and platinum, and the thickness of the electrode layer is 90-120 nm.
Further, the AgVO3The nanowire functional layer is prepared by the following steps: a. respectively preparing 0.02-0.03 mol/L ammonium metavanadate (NH)4VO3) The solution and 0.02-0.03 mol/L silver nitrate (AgNO)3) A solution; b. according to a molar ratio V: mixing an ammonium metavanadate solution and a silver nitrate solution according to the ratio of Ag to 1:1, and uniformly stirring in a water bath heating environment at 80-90 ℃; c. transferring the solution uniformly stirred in the step b into a reaction kettle, reacting at 180-190 ℃ for 12-24 h, and drying the taken sample at 60-80 ℃ to obtain AgVO3A nanowire; d. the AgVO obtained in the step c3Nanowires according to 0.5g AgVO3Adding the mixture into 10-15 mL of deionized water, and dispersing the mixture into the deionized water to form AgVO3And (3) uniformly coating the nanowire dispersion liquid on the electrode layer, and drying at 60-80 ℃ to obtain the functional layer of the breathing sensor.
Further, the packaging layer is a medical dressing, such as a polymeric film dressing, a hydrocolloid dressing and the like, which can transmit oxygen and water vapor and block particulate matters. As the medical dressing has the characteristics that gases such as oxygen, water vapor and the like can freely pass through but granular substances in the environment cannot pass through, AgVO can be well isolated3Nanowire functional layer and external environment for preventing AgVO3The damage caused by the inhalation of the nano wire by human body.
Based on AgVO3The preparation method of the nanowire breathing sensor comprises the following steps:
step 1, preparation of a flexible substrate: selecting an organic material with the elastic modulus of 1 GPa-4 GPa, such as Polyimide (PI), polyethylene terephthalate (PET) and the like as a flexible substrate;
step 2, preparing an electrode layer: preparing an interdigital electrode or a parallel electrode on a flexible substrate by adopting a photoetching process to serve as an electrode layer;
step 3, preparation of a functional layer: preparation of AgVO by hydrothermal method3The nanowires are prepared into dispersion liquid, coated on the electrode layer obtained in the step (2), and dried to form a functional layer of the breathing sensor;
step 4, packaging to obtain AgVO-based material3A nanowire respiration sensor.
Further, the preparation process of the functional layer in the step 3 specifically comprises the following steps: a. respectively preparing 0.02-0.03 mol/L ammonium metavanadate (NH)4VO3) The solution and 0.02-0.03 mol/L silver nitrate (AgNO)3) A solution; b. according to a molar ratio V: mixing an ammonium metavanadate solution and a silver nitrate solution according to the ratio of Ag to 1:1, and uniformly stirring in a water bath heating environment at 80-90 ℃; c. transferring the solution uniformly stirred in the step b into a reaction kettle, reacting at 180-190 ℃ for 12-24 h, and drying the taken sample at 60-80 ℃ to obtain AgVO3A nanowire; d. the AgVO obtained in the step c3Nanowires according to 0.5g AgVO3Adding intoDispersing 10-15 mL deionized water in proportion into the deionized water to form AgVO3And (3) uniformly coating the nanowire dispersion liquid on the electrode layer obtained in the step (2), and drying at the temperature of 60-80 ℃ to obtain the functional layer of the breathing sensor.
Further, the packaging in step 4 is made of medical dressing, such as polymeric film dressing, hydrocolloid dressing, etc. which can transmit oxygen and water vapor and block particulate matter.
The invention has the beneficial effects that:
the invention provides a flexible wearable respiration sensor and a preparation method thereof, wherein the sensor selects an organic material with the elastic modulus of 1 GPa-4 GPa as a flexible substrate, forms an electrode layer on the flexible substrate by adopting a photoetching process, and then coats AgVO on the electrode layer3And finally, packaging the nanowire functional layer by adopting medical dressing to obtain the flexible respiration sensor. The respiration sensor adopts a multilayer laminated structure, and the flexible substrate has bendability and tensile resistance, so that the stable performance of the sensor is ensured; meanwhile, compared with the existing respiration monitoring device, the respiration sensor has the advantages of large change range of the detected respiration intensity, high sensitivity, good process controllability and repeatability, and is favorable for realizing large-scale batch production.
Drawings
FIG. 1 shows AgVO-based data provided by the invention3A schematic structural diagram of a nanowire breathing sensor;
FIG. 2 is a schematic flow chart of a method for manufacturing a respiratory sensor according to an embodiment;
FIG. 3 is a resistance versus temperature curve for an exemplary respiration sensor;
FIG. 4 is a resistance-humidity curve of an embodiment respiration sensor;
FIG. 5 shows AgVO-based samples obtained in the example3The resistance change response curve of the breathing sensor of the nanowire to normal breathing;
FIG. 6 shows AgVO-based samples obtained in the examples3The resistance change response curve of the breathing sensor of the nano wire to the bradyrespiration and the tachypnea.
Detailed Description
The technical scheme of the invention is detailed below by combining the accompanying drawings and the embodiment.
Examples
Based on AgVO3The preparation method of the nanowire breathing sensor comprises the following steps:
step 1, preparing a flexible substrate:
a25 μm thick Polyimide (PI) film was cut to a size of 5 × 10mm2The PI film is attached to the glass sheet by using an adhesive tape, and the glass sheet is used as a hard substrate and plays a supporting role;
step 2, preparing an electrode layer:
preparing an interdigital electrode pattern on the PI film in the step 1 by adopting a photoetching process, wherein the electrode distance is 100 mu m, the interdigital index is 5, and the electrode size is 3 × 5mm2(ii) a Then, depositing a gold film with the thickness of 100nm by adopting a magnetron sputtering method, and cleaning by using acetone to obtain a gold interdigital electrode as an electrode layer;
step 3, preparing a functional layer of the breathing sensor:
a. respectively preparing 0.025mol/L ammonium metavanadate (NH) at normal temperature4VO3) Solution 240mL and 0.025mol/L silver nitrate (AgNO)3) 240mL of solution, mixing the two solutions at 80 ℃ and uniformly stirring; b. transferring the uniformly stirred solution into a reaction kettle, reacting for 16h at 180 ℃, and drying the taken sample at 70 ℃ to obtain AgVO3A nanowire; c. taking 0.5g of AgVO obtained in the step b3Grinding the nanowires into a powder structure, adding the powder structure into 10mL of deionized water, and carrying out ultrasonic treatment for 5min to form uniform AgVO3The nanowire dispersion is in a light yellow uniform solution state; d. placing the PI film with the gold interdigital electrode obtained in the step 2 on a baking table (JB-1B), keeping the temperature at 80 ℃, and placing the AgVO prepared in the previous step3And dripping 1mL of the nanowire dispersion liquid on a gold interdigital electrode, and drying at 70 ℃ to obtain a functional layer of the respiration sensor.
Step 4, packaging:
leading out interconnection wires from two ends of the gold interdigital electrode, and coating a polymeric membrane dressing (3M Tega)derm) cut to 5 × 10mm2The size of the flexible device covers the surface of the respiration sensor, and then the whole flexible device is taken down from a glass sheet, namely the AgVO-based device3A nanowire respiration sensor.
AgVO-based material obtained in the following examples3Analyzing the performance of the nano-wire breathing sensor;
AgVO-based on embodiment adopting Agilent B2901A source table3The respiration sensor of the nanowire measures the resistance change caused by the temperature change. As a result, as shown in fig. 3, the resistance of the respiration sensor gradually increases with the increase in temperature, and it can be seen that the resistance value of the device increases from 180M Ω to about 210M Ω when the ambient temperature changes from 20 ℃ to 70 ℃. AgVO-based on embodiment adopting Agilent B2901A source table3The resistance change of the nano wire respiration sensor caused by the humidity change is measured. As a result, as shown in fig. 4, the resistance of the respiration sensor decreases significantly with increasing humidity, and decreases approximately linearly, and the resistance decreases to 3.4M Ω for every 1% increase in humidity after linear fitting. In the breathing process of a human body, the changes of the exhaled air and the inhaled air mainly include temperature change, humidity change and air component proportion change, and the results show that the breathing sensor is mainly sensitive to the humidity change, and the response to the temperature change is relatively weak. Therefore, the experiment utilizes the temperature and humidity change in the respiration process, and the actual response of the human body in the respiration process is also tested, and the result is shown in fig. 5. When the human body breathes in, the resistance of the sensor is about 175M omega, when the human body breathes out the gas, the sensor is subjected to the comprehensive action of the humidity and the temperature of the exhaled gas, the resistance of the sensor is reduced to be about 1M omega, and when the human body breathes in the gas, the resistance of the sensor is restored to be about 175M omega; multiple breath tests show that the breathing sensor has good repeatability, the difference between the resistance values of the sensor during expiration and inspiration is more than 170 MOmega, and the breathing sensor can sensitively reflect the change conditions of the breathing frequency and the breathing intensity of a human body. In addition, the respiration sensor of the present invention, when used for respiration monitoring, has a sensitive response to both of the respiration and the tachycardia, as shown in FIG. 6,when a human body breathes quickly, the sensor can sensitively detect the change of breathing frequency, and the resistance value change range is reduced from 20M omega to about 1M omega; when the respiratory frequency of the human body is reduced, because the human body breathes slowly, more water vapor is exhaled by the human body, and meanwhile, the inspiration time is longer, so that the human body can bring the water vapor on the device back to the human body as much as possible during inspiration, and the resistance value change range of the device is larger. As can be seen from fig. 6, when the human body breathes slowly, the resistance value of the device ranges from about 80M Ω to about 1M Ω.

Claims (9)

1. Based on AgVO3The respiration sensor of the nano wire comprises a four-layer structure, and a flexible substrate, an electrode layer, a functional layer and a packaging layer are sequentially arranged from bottom to top, wherein the functional layer is AgVO3A nanowire.
2. AgVO-based according to claim 13The breathing sensor of the nano wire is characterized in that the flexible substrate is made of organic materials with the elastic modulus of 1 GPa-4 GPa.
3. AgVO-based according to claim 13The nanowire breathing sensor is characterized in that the thickness of the flexible substrate is 20-50 microns.
4. AgVO-based according to claim 13The nanowire respiration sensor is characterized in that the electrode layer is an interdigital electrode or a parallel electrode, the electrode layer is made of gold or platinum, and the thickness of the electrode layer is 90-120 nm.
5. AgVO-based according to claim 13A nanowire respiration sensor, characterized in that the AgVO3The nanowire functional layer is prepared by the following steps: a. respectively preparing 0.02-0.03 mol/L ammonium metavanadate solution and 0.02-0.03 mol/L silver nitrate solution; b. according to a molar ratio V: mixing an ammonium metavanadate solution and a silver nitrate solution according to the ratio of Ag to 1:1, and stirring in a water bath heating environment at the temperature of 80-90 DEG CUniformly stirring; c. transferring the solution uniformly stirred in the step b into a reaction kettle, reacting at 180-190 ℃ for 12-24 h, and drying the taken sample at 60-80 ℃ to obtain AgVO3A nanowire; d. the AgVO obtained in the step c3Nanowires according to 0.5g AgVO3Adding the mixture into 10-15 mL of deionized water, and dispersing the mixture into the deionized water to form AgVO3And (3) uniformly coating the nanowire dispersion liquid on the electrode layer, and drying at 60-80 ℃ to obtain the functional layer of the breathing sensor.
6. AgVO-based according to claim 13The respiration sensor of the nanowire is characterized in that the packaging layer is a thin film which is permeable to oxygen or water vapor and blocks particulate matters.
7. Based on AgVO3The preparation method of the nanowire breathing sensor comprises the following steps:
step 1, preparation of a flexible substrate: selecting an organic material with the elastic modulus of 1 GPa-4 GPa as a flexible substrate;
step 2, preparing an electrode layer: preparing an interdigital electrode or a parallel electrode on a flexible substrate by adopting a photoetching process to serve as an electrode layer;
step 3, preparation of a functional layer: preparation of AgVO by hydrothermal method3The nanowires are prepared into dispersion liquid, coated on the electrode layer obtained in the step (2), and dried to form a functional layer of the breathing sensor;
step 4, packaging to obtain AgVO-based material3A nanowire respiration sensor.
8. AgVO-based according to claim 73The preparation method of the nanowire breathing sensor is characterized in that the preparation process of the functional layer in the step 3 specifically comprises the following steps: a. respectively preparing 0.02-0.03 mol/L ammonium metavanadate solution and 0.02-0.03 mol/L silver nitrate solution; b. according to a molar ratio V: mixing an ammonium metavanadate solution and a silver nitrate solution according to the ratio of Ag to 1:1, and uniformly stirring in a water bath heating environment at 80-90 ℃; c. b, stirring the mixture evenlyTransferring the solution into a reaction kettle, reacting at 180-190 ℃ for 12-24 h, and drying the taken sample at 60-80 ℃ to obtain AgVO3A nanowire; d. the AgVO obtained in the step c3Nanowires according to 0.5g AgVO3Adding the mixture into 10-15 mL of deionized water, and dispersing the mixture into the deionized water to form AgVO3And (3) uniformly coating the nanowire dispersion liquid on the electrode layer obtained in the step (2), and drying at the temperature of 60-80 ℃ to obtain the functional layer of the breathing sensor.
9. AgVO-based according to claim 73The preparation method of the nanowire breathing sensor is characterized in that the encapsulation in the step 4 adopts a film which can be permeable to oxygen or water vapor and can block particulate matters.
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CN109557141B (en) * 2018-11-30 2021-01-15 湘潭大学 Titanium dioxide/silver vanadate nano heterojunction and preparation method and application thereof
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