CN112504542A - Application of sensitive material in flexible vacuum pressure sensor - Google Patents
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- CN112504542A CN112504542A CN202011293898.8A CN202011293898A CN112504542A CN 112504542 A CN112504542 A CN 112504542A CN 202011293898 A CN202011293898 A CN 202011293898A CN 112504542 A CN112504542 A CN 112504542A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/02—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention relates to the technical field of flexible electronic materials, in particular to application of a sensitive material in a flexible vacuum pressure sensor. The sensitive material is highly sensitive to gas, the concentration of oxygen molecules in the atmosphere is in positive correlation with the gas pressure, when the sensitive material is exposed to a gas environment, the resistance of the sensitive material is obviously changed along with the change of the gas pressure, the sensitive material is applied to a flexible vacuum pressure sensor, the sensor responds to different pressure environments through the change of the resistance value, the sensitivity is high, the stability and the reliability of the flexible vacuum pressure sensor are good, the pressure change is exerted circularly, the resistivity of a device also shows cyclic change, the hysteresis is not obvious during pressure loading and unloading, and the sensitive material has good linear characteristics for different vacuum pressures. The conductive nano material of the flexible vacuum pressure sensor has a larger contact angle and shows super-hydrophobic performance. Therefore, the flexible pressure sensing device can be used for intelligent clothing and medical equipment and monitoring vacuum pressure in real time.
Description
Technical Field
The invention relates to the technical field of flexible electronic materials, in particular to application of a sensitive material in a flexible vacuum pressure sensor.
Background
Wearable electronics have attracted a great deal of attention due to their importance in disposable electronics, sensors, and health monitoring systems. These wearable devices are now very popular around the world, e.g. new marketed wristwatches, *** glasses, bracelets and glasses, all achieved by the miniaturization of current electronic components. In recent years, electronic textiles have attracted great scientific and commercial interest as a new generation of wearable electronics due to their potential applications in flexible electronics, sensors, and multifunctional smart apparel. By integrating advanced electronic functions into common and insulating textiles to form electronic textiles, the novel wearable electronic product has the advantages of light weight, low cost, stretchability, foldability and the like, and can be used for providing convenience for life services.
In addition, the sensor is required to have high sensitivity for monitoring human physiological signals, gases, light, and the like. In practical applications, there are many configurations of sensors, such as piezoresistive sensors, piezoelectric devices, capacitive sensors, field effect transistors, and the like. And all of the obtained information can be analyzed and compared to standard reference data and any abnormal signals sent to the physician for monitoring, alarming and further diagnosis. For different kinds of sensors, there are various sensing materials such as carbon, metal oxide nanowires, conductive elastomer composite, silicon nanowires, and the like. But the carbon nano tube and MXene two-dimensional materials are not applied to the vacuum pressure sensor at present.
Disclosure of Invention
In view of the above, the invention provides an application of a sensitive material in a flexible vacuum pressure sensor, in which a carbon nanotube and an MXene two-dimensional material in the sensitive material are highly sensitive to gas in the environment, and when the sensitive material is exposed to the gas environment, the resistance of the sensitive material is significantly changed.
The specific technical scheme is as follows:
the invention provides an application of a sensitive material in a flexible vacuum pressure sensor, wherein the sensitive material consists of a flexible substrate and a conductive nano material;
the flexible substrate is connected with the conductive nano material through ultrasonic welding;
the flexible substrate is made of a flexible high polymer material with the glass transition temperature of less than 81 ℃, and the conductive nano material is a carbon nano tube or MXene two-dimensional material.
It should be noted that only the flexible polymer material with the glass transition temperature of less than 81 ℃ can be melted in the ultrasonic welding process, so as to be fused with the conductive material, and the flexible polymer material has good stretchability, can be bent, and is suitable for being used as a substrate of a wearable device.
The sensitive material of the invention shows n-type semiconductor characteristics, and when the conductive nano material is a carbon nano tube, the carbon nano tube CNTs naturally absorb oxygen from the air, and have stronger electron affinity. At atmospheric pressure, a large number of oxygen molecules (O)2) Adsorbed to the exposed surface of CNTs, electrons (e-) in the conduction band can be trapped as negatively charged oxygen ions (O)2-) The number of free electrons in the air of the sensitive material is reduced, and the sensitive material presents a high resistance phenomenon. The concentration of oxygen molecules in the atmospheric pressure is constant, and as the atmospheric pressure decreases, the corresponding O2The number of free electrons in the air of the sensitive material is increased, and the resistance value of the sensitive material is reduced along with the reduction of the pressure. Sensitive material is applied to a flexible vacuum pressure sensor, and the sensor responds to different pressure environments through resistance value change, so that the sensor is flexibleThe flexible vacuum pressure sensor has high sensitivity, good stability and reliability, cyclic pressure variation, cyclic variation of device resistivity, insignificant hysteresis during pressure loading and unloading, and good linear characteristics for different vacuum pressures. The conductive nano material of the flexible vacuum pressure sensor has a larger contact angle and shows super-hydrophobic performance. Therefore, the flexible pressure sensing device can be used for intelligent clothing and medical equipment and monitoring vacuum pressure in real time.
The Mxene two-dimensional material belongs to a novel two-dimensional material, is sensitive to volatile organic compounds, and causes the concentration change of charge carriers on the surface layer of a two-dimensional material lamellar nanosheet when molecular gas is adsorbed on the surface layer of the two-dimensional material, so that the conductivity of the whole surface layer of the two-dimensional material is changed. The conductivity of the two-dimensional material is adjusted by the gas species.
In the invention, the flexible substrate is non-woven fabric, preferably non-woven fabric, polypropylene fiber or terylene made of polypropylene and viscose fiber; the glass transition temperature of polypropylene is 35 ℃, and the glass transition temperature of terylene is 67-81 ℃.
The flexible substrate is a pretreated flexible substrate, and the pretreatment specifically comprises the following steps:
ultrasonically cleaning a flexible substrate, soaking the flexible substrate in an isopropanol saturated solution, and drying the flexible substrate for later use;
the drying temperature of the ultrasonic cleaning is 50-80 ℃, preferably 60 ℃, the process parameters of the ultrasonic cleaning are that the maximum power is 150W, and the frequency range is 20-90 kHz; the drying time is 1-6 h, preferably 3 h;
the thickness of the flexible substrate is 140 μm to 160 μm, preferably 150 μm.
The conductive nano material is a carbon nano tube or MXene two-dimensional material, preferably a carbon nano tube, more preferably a carbon nano tube, and further preferably a multi-wall carbon nano tube; the outer diameter of the multi-walled carbon nano-tube is 10-15 nm, the length of the multi-walled carbon nano-tube is 0.1-10 mu m, and the purity of the multi-walled carbon nano-tube is 98%.
In the invention, the preparation method of the sensitive material comprises the following steps:
and immersing the flexible substrate in the dispersion liquid of the conductive nano material, and carrying out ultrasonic nano welding to obtain the sensitive material.
The flexible substrate is subjected to ultrasonic welding in the conductive nano material dispersion liquid, so that the flexible substrate is locally softened, the binding force between the conductive nano material and the flexible substrate is enhanced, the conductive nano material is not easy to fall off from the conductive substrate, and the electronic textile with durability and washability is formed.
The ultrasonic welding process used by the invention is simple and has lower cost.
The preparation method of the dispersion liquid of the conductive nano material comprises the following steps:
mixing a conductive nano material, a surfactant and a solvent, and then carrying out ultrasonic dispersion treatment to obtain a dispersion liquid of the conductive nano material;
the mass ratio of the conductive nano material to the surfactant is (5-10): 1, preferably 10: 1;
the surfactant sodium lauryl sulfate or polyacrylamide, preferably sodium lauryl sulfate;
the solvent is an isopropanol aqueous solution or an absolute ethyl alcohol aqueous solution, preferably an isopropanol aqueous solution, and the volume concentration of the solvent is 25-50%, preferably 25%;
the ultrasonic dispersion time is 15min-30min, preferably 30 min;
the concentration of the conductive nano material in the dispersion liquid of the conductive nano material is 0.1-0.5 mg/ml, and preferably 0.1 mg/ml.
The ultrasonic welding temperature is 0 ℃, the time is 3-30 min, the maximum output power is 2000W, the amplitude is 60%, and the frequency is 20 kHz.
In the invention, the sensitive material is required to be post-treated; the post-treatment specifically comprises the following steps: deionized water and isopropanol or absolute ethyl alcohol are adopted for washing, and then deionized water is adopted for ultrasonic cleaning and drying.
According to the invention, the copper wire and the sensitive material are tightly combined by using the conductive silver adhesive to prepare the flexible vacuum pressure sensor. The preparation of the flexible vacuum pressure sensor belongs to the prior art and is not described in detail here.
According to the technical scheme, the invention has the following advantages:
the invention provides an application of a sensitive material in a flexible vacuum pressure sensor, wherein the sensitive material consists of a flexible substrate and a conductive nano material; the flexible substrate is connected with the conductive nano material through ultrasonic welding; the flexible substrate is made of a flexible high polymer material with the glass transition temperature of less than 81 ℃, and the conductive nano material is a carbon nano tube or MXene two-dimensional material.
The sensitive material is highly sensitive to gas, the concentration of oxygen molecules in the atmosphere is in positive correlation with the gas pressure, when the sensitive material is exposed in a gas environment, the resistance of the sensitive material is obviously changed along with the change of the gas pressure, the sensitive material is applied to a flexible vacuum pressure sensor, the sensor responds to different atmospheric pressure environments through the change of the resistance value, the sensitivity is high, the flexible vacuum pressure sensor is good in stability and reliability, the pressure change is exerted circularly, the resistivity of a device also shows cyclic change, the hysteresis is not obvious during pressure loading and unloading, and the sensitive material has good linear characteristics for different vacuum pressures. The conductive nano material of the flexible vacuum pressure sensor has a larger contact angle and shows super-hydrophobic performance. Therefore, the flexible pressure sensing device can be used for intelligent clothing and medical equipment and monitoring vacuum pressure in real time.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
Fig. 1 is a flow chart of a process for preparing a carbon nanotube/nonwoven fabric according to embodiment 1 of the present invention;
FIG. 2 is a schematic view of ultrasonic welding of the carbon nanotube conductive nanomaterial of the present invention;
FIG. 3 is a scanning electron microscope image of the carbon nanotube/nonwoven fabric provided in example 1 of the present invention;
fig. 4 is a resistance value variation curve of the flexible vacuum pressure sensor provided in embodiment 1 of the present invention under different strain variations (the inset is a maximum uniaxial tensile strength and stress-strain curve of the flexible vacuum pressure sensor and an original non-woven fabric);
fig. 5 is a graph illustrating a variation of a resistance value of the flexible vacuum pressure sensor device according to embodiment 1 of the present invention under different pressures;
fig. 6 is a graph illustrating a resistance value variation of the flexible vacuum pressure sensor device according to embodiment 1 of the present invention during a cyclic pressure test;
fig. 7 is a graph of resistance change of the flexible vacuum pressure sensor device provided in embodiment 1 of the present invention at different washing times;
fig. 8 is a graph showing resistance value changes of the flexible vacuum pressure sensor device according to embodiment 1 before and after mechanical washing for 48 h.
Detailed Description
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it should be apparent that the embodiments described below are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The raw materials and reagents involved in the examples of the present invention are all commercially available.
Example 1
The embodiment is a flexible vacuum pressure sensor, and the specific preparation steps refer to fig. 1:
(1) pretreatment of non-woven fabrics (made of polypropylene and viscose): ultrasonic cleaning the non-woven fabric in deionized water for 5min at the frequency of 20 kHz; the isopropanol-saturated nonwoven was dried at 60 ℃ for 3h and the NWF having a thickness of 150 μm was cut into substrates of 3.0cm by 1.5cm for further use.
(2) Ultrasonic nano welding: firstly, weighing a mixture of 1: mixing 10 parts of sodium dodecyl sulfate and multi-walled carbon nanotubes (MWCNTs) (the outer diameter is 10-15 nm, the length is 0.1-10 mu m) in a beaker, then injecting a deionized water solvent with the volume fraction of 25% of isopropanol, and ultrasonically dispersing the whole system for 30min to obtain a multi-walled carbon nanotube dispersion liquid (0.1 mg/ml);
secondly, immersing the pretreated non-woven fabric fibers in a multi-walled carbon nanotube dispersion liquid, placing a solution system in an ice-water mixture at 0 ℃, then carrying out ultrasonic nano-welding at 0 ℃ for 15min, washing samples subjected to ultrasonic nano-welding respectively with deionized water and isopropanol until no black particles fall off, then placing the samples in the deionized water, and carrying out ultrasonic cleaning for 5min, wherein the used frequency is 20 kHz; and (3) placing the sample in a drying box at 60 ℃ for drying to obtain a sensitive material (carbon nano tube/non-woven fabric) which is marked as CNTs/NWF. Wherein the maximum output power of the ultrasonic nano-welder is 2000W, the amplitude is 60 percent and the frequency is 20 kHz.
(3) And fixing two copper wires on two sides of the carbon nano tube/non-woven fabric by using conductive silver paste for packaging to obtain the flexible vacuum pressure sensor.
FIG. 2 is a schematic view of ultrasonic welding of the carbon nanotube conductive nanomaterial of the present invention, wherein ultrasonic vibration generates a large amount of bubbles in the liquid, and the generated bubbles are broken to generate huge pressure and high temperature, so as to provide sufficient momentum and energy for the carbon nanotube to weld to the surface of the substrate and the internal structure, thereby forming a sensitive material.
Fig. 3 is an electron microscope image of example 1 with different resolutions, which shows that the carbon nanotubes in the carbon nanotube/nonwoven fabric sample are entangled with the nonwoven fabric fibers, and the carbon nanotubes are randomly and continuously distributed, even penetrate into the fabric, to form a conductive network structure. The method for welding the carbon nano tube to the non-woven fabric fiber by the ultrasonic welding technology has strong bonding force between the carbon nano tube and the non-woven fabric fiber, and the multi-wall carbon nano tube can be stably kept in the non-woven fabric, so that the sensor has washability and durability.
The flexible vacuum pressure sensor of example 1 was subjected to pressure using an Instron electronic universal material tester while measuring the resistance value across the device using a semiconductor parameter analyzer (Keithley 2400). Fig. 4 is a graph showing resistance value changes of the flexible vacuum pressure sensing device provided in embodiment 1 of the present invention under different strain changes, and as shown in fig. 4, when the strain is less than 9.4%, the resistance of the carbon nanotube/nonwoven fabric first decreases with decreasing strain and then increases with increasing strain, wherein the increase of the resistance is attributable to the unrecoverable fracture of the NWF fiber interconnection network structure. The result shows that the carbon nano tube/non-woven fabric has sensitive response to strain and can be used as a strain sensor; meanwhile, the flexible vacuum pressure sensor prepared by the ultrasonic nano welding technology has good conductivity, and the carbon nano tube non-woven fabric sensitive material is connected into a complete circuit by using a direct current power supply, so that the light-emitting diode can normally emit light.
The flexible vacuum pressure sensor device of example 1 and the raw nonwoven fabric were subjected to stress testing using an Instron electronic universal material tester and data analysis was performed using Bluehill 2.0 software. Fig. 4 is an inset of a graph showing a maximum uniaxial tensile strength and a stress-strain curve of the flexible vacuum pressure sensor and the original non-woven fabric, and as shown in the inset of fig. 4, in a range of tensile strain of 0-39.8%, the required stress of both the carbon nanotube-graphene/non-woven fabric and the original non-woven fabric increases with the increase of strain; within the range of 39.8-75% of tensile strain, the required stress is reduced along with the increase of the strain, which indicates that the deformation exceeds 39.8%, and the fiber interconnected network structure in the non-woven fabric is subjected to irreversible damage. Within the range of 0-45% of tensile strain, the same strain, the stress required by the carbon nanotube-graphene/non-woven fabric is larger than that of the original non-woven fabric, and the maximum tensile strain is 39.8%, which indicates that the mechanical property of the non-woven fabric is not changed by ultrasonic welding, the tensile strength and Young modulus of the non-woven fabric are almost the same as those of the original non-woven fabric, and even slightly higher than those of the original non-woven fabric.
Example 1 a flexible vacuum pressure sensor was placed in a chamber for measuring vacuum pressure sensing characteristics to apply different pressure conditions while the resistance of the sensor was measured in situ using a Keithley 2400Source-Meter SMU instrument. FIG. 5 provides examples 1 of the present inventionThe resistance value of the flexible vacuum pressure sensing device changes in a curve under different pressures, as shown in fig. 5, the device is 1000, 100, 10, 1, 2.4 x 10-2，6.5×10-3，5.2×10-4，7.3×10-5In millibar (mbar) pressure, corresponding to resistance values of 9766.5 Ω, 9717.1 Ω, 9579.6 Ω, 9536.1 Ω, 9501.3 Ω and 9467.5 Ω (ohm), it can be clearly observed that the flexible vacuum pressure sensor has sensitive response to different pressure environments, and the resistance value thereof decreases as the vacuum pressure decreases. This is attributed to the fact that the formed CNTs/NWF composite material exhibits n-type semiconductor characteristics, naturally absorbs oxygen from air, and has a strong electron affinity. At atmospheric pressure, a large number of oxygen molecules (O)2) Adsorbed to the exposed surface of CNTs, electrons (e-) in the conduction band can be trapped as negatively charged oxygen ions (O)2-) The CNTs/NWF composite material is reduced in the number of free electrons in air, and shows a high resistance phenomenon. The concentration of oxygen molecules in the atmospheric pressure is constant, and as the atmospheric pressure decreases, the corresponding O2The quantity of free electrons in the air of the CNTs/NWF composite material is increased, and the resistance value of the CNTs/NWF composite material is reduced along with the reduction of the pressure.
Example 1 a flexible vacuum pressure sensor was placed in a chamber for measuring vacuum pressure sensing characteristics to apply the same pressure conditions over a cycle while measuring the resistance of the sensor in situ using a Keithley 2400Source-Meter SMU instrument. Fig. 6 is a graph showing a resistance value variation of the flexible vacuum pressure sensor device provided in embodiment 1 of the present invention under a cyclic pressure, in which a test method is to apply a resistance value of 7.3 × 10 to CNTs/NWF cyclically-5The change in resistance was detected simultaneously with a gas pressure of 1000 mbar. Fig. 6 shows that the cyclic pressure variation and the resistance variation of the CNTs/NWF are also cyclic, and the hysteresis during pressure loading and unloading is not significant, which indicates that the resistance value of the prepared flexible vacuum pressure sensor has higher sensitivity and repeatability to air pressure.
The example 1 flexible vacuum pressure sensor was placed in DI water and DI water with detergent, stirred rapidly at 700rpm, and then dried. Fig. 7 is a resistance variation curve diagram of the flexible vacuum pressure sensor device provided in embodiment 1 of the present invention at different washing times, and the resistance values of the CNTs/NWF electronic textile sensor are obtained as the DI water and the detergent DI change with the washing time. As shown in fig. 7, after mechanical washing, the resistance of the CNTs/NWF electronic textile sensor with net resistances of 9.7k Ω and 9.9k Ω respectively increases first, and the resistivity thereof remains substantially unchanged after long-term washing due to the strong adhesion of the carbon nanotubes firmly inserted into the fibers, and only a small amount of carbon nanotubes fall off from the surface of the device under strong mechanical destruction and chemical action, which reflects that the CNTs/NWF flexible electronic textile vacuum pressure sensor prepared by the ultrasonic method has good washing fastness. In addition, it can be seen from the inset of fig. 7 that the CNTs/NWF flexible electronic textile vacuum pressure sensor exhibits superhydrophobic performance.
Fig. 8 is a graph showing a resistance value change curve of the flexible vacuum pressure sensor before and after 48h of mechanical washing in the embodiment 1 of the present invention under different pressures, and as can be obtained from fig. 8, the resistivity of the device increases after 48h of washing, and the resistance increases with the increase of the vacuum pressure. The flexible vacuum pressure sensor has good sensitivity to different air pressures before and after being mechanically washed for 48h, and generates good linear characteristic response to the pressure, which shows that the device has good repeatability, washability, durability and high sensitivity performance.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The application of the sensitive material in the flexible vacuum pressure sensor is characterized in that the sensitive material consists of a flexible substrate and a conductive nano material;
the flexible substrate is connected with the conductive nano material through ultrasonic welding;
the flexible substrate is made of a flexible high polymer material with the glass transition temperature of less than 81 ℃, and the conductive nano material is a carbon nano tube or MXene two-dimensional material.
2. Use according to claim 1, wherein the flexible substrate is a non-woven fabric.
3. Use according to claim 1, wherein the flexible substrate has a thickness of 140 μm to 160 μm.
4. The use according to claim 1, wherein the sensitive material is prepared by a method comprising the steps of:
and immersing the flexible substrate in the dispersion liquid of the conductive nano material, and carrying out ultrasonic nano welding to obtain the sensitive material.
5. The use according to claim 4, wherein the flexible substrate is a pretreated flexible substrate, the pretreatment being in particular:
and (3) ultrasonically cleaning the flexible substrate, soaking the flexible substrate in an isopropanol saturated solution, and drying the flexible substrate for later use.
6. The use according to claim 4, wherein the concentration of the conductive nanomaterial in the dispersion of conductive nanomaterials is 0.1 to 0.5 mg/ml.
7. The use according to claim 4, wherein the dispersion of conductive nanomaterial is prepared by a method comprising:
mixing a conductive nano material, a surfactant and a solvent, and then carrying out ultrasonic dispersion treatment to obtain a dispersion liquid of the conductive nano material.
8. Use according to claim 7, characterized in that the surfactant is sodium lauryl sulfate or polyacrylamide.
9. The application of claim 7, wherein the mass ratio of the conductive material to the surfactant is (5-10): 1.
10. the use according to claim 4, wherein the ultrasonic welding is carried out at a temperature of 0 ℃ for a time of 3-30 min, at a maximum output of 2000W and an amplitude of 60%, and at a frequency of 20 kHz.
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