CN113638128A - Preparation method of thin film material capable of realizing temperature and strain dual-function self-driven sensing - Google Patents
Preparation method of thin film material capable of realizing temperature and strain dual-function self-driven sensing Download PDFInfo
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
- D04H1/43835—Mixed fibres, e.g. at least two chemically different fibres or fibre blends
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
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Abstract
A method for preparing a film material capable of realizing temperature and strain dual-function self-driven sensing comprises the steps of taking PEDOT, PSS and water-soluble polyurethane (WPU) all-organic system composite stretchable thermoelectric fibers prepared by a wet spinning method as raw materials, dispersing the prepared stretchable thermoelectric fibers in a mixed solution of water and ethanol, and performing ultrasonic dispersion, vacuum filtration and mechanical pressing to obtain a two-dimensional porous reticular film structure. The porous network membrane realizes the detection of temperature based on the thermoelectric effect. Under the strain condition, the strain detection is realized based on the change of the point contact state between fibers in the fiber mesh film. When the temperature and strain excitation is simultaneously applied to one section of the film material, a voltage signal generated by temperature difference can be used as a signal source, and a power-containing testing device is not needed, so that the dual-function self-driven detection of the temperature and the strain is realized.
Description
Technical Field
The invention relates to the technical field of sensors, in particular to a preparation method of a thin film material capable of realizing temperature and strain dual-function self-driven sensing.
Background
In recent years, with the rapid development of the field of artificial intelligence and the increasing demand of people for health monitoring, the development of electronic skin or daily wearable micro electronic devices which are light and thin and can realize multi-function perception has gradually become a research hotspot in the current sensing field. From the standpoint of sensing functionality, strain sensing and temperature sensing are two important aspects.
In terms of strain sensing, the resistance-type strain sensing device has the advantages of high sensitivity, large detection range, strong structure designability, simple processing technology and the like, and is a strain/stress analysis sensitive element widely used at present. However, for the resistance type strain sensor, an external power supply is required to detect the resistance during detection, so that an additional energy supply device is required to be matched when the resistance type strain sensor is applied to electronic skin or wearable electronic devices.
For the temperature sensing part, the temperature sensors commonly used at present mainly include thermocouple sensors based on the thermoelectric effect, thermistor sensors using thermistors as elements, and infrared temperature sensors based on the black body radiation principle. The thermocouple sensor based on the thermoelectric effect is a self-generating sensor, has a simple structure, a wide temperature measurement range, high precision and quick response, and is the most commonly used contact type sensing temperature measuring device at present.
Although strain and temperature sensing technologies with single sensing function are well developed at present, materials and devices capable of simultaneously achieving temperature and strain sensing and self-driving without external energy are still rarely reported. Based on the development trend in the fields of electronic skins and wearable electronic devices, the preparation of flexible devices capable of realizing temperature and strain dual-function self-driven sensing is of great significance.
Disclosure of Invention
According to the technical problem that materials and devices which can simultaneously realize temperature and strain double-function sensing and can be self-driven without external energy supply are absent, the invention provides a preparation method of a film material which can realize temperature and strain double-function self-driven sensing.
The technical means adopted by the invention are as follows:
a preparation method of a thin film material capable of realizing temperature and strain dual-function self-driven sensing specifically comprises the following steps:
(a) adding ionic liquid into a PEDOT (PSS) aqueous solution, magnetically stirring under the condition of constant-temperature heating, and adjusting the viscosity of a mixed solution;
(b) further mixing the mixed solution prepared in the step (a) with an aqueous polyurethane dispersion;
(c) sucking the mixed solution prepared in the step (b) into an injector, mounting the injector on a micro-injection pump, immersing the outlet of a needle in an organic solvent coagulating bath, pushing the mixed solution out of the injector into the coagulating bath, and obtaining continuous PEDOT (PSS)/WPU (WPU) composite stretchable thermoelectric fiber in the coagulating bath; then, taking the PEDOT, PSS/WPU composite stretchable thermoelectric fiber out of the coagulation bath, and vertically hanging and drying the PEDOT, PSS/WPU composite stretchable thermoelectric fiber in a room-temperature environment;
(d) taking the PEDOT (PSS)/WPU (WPU) composite stretchable thermoelectric fiber dried in the step (c), and primarily shearing the PEDOT/PSS/WPU composite stretchable thermoelectric fiber; putting the primarily sheared fiber into a beaker, adding a mixed solution of water and ethanol, and vibrating and crushing the short fiber by using an ultrasonic vibration crushing technology to obtain a fiber suspension;
(e) collecting a fiber membrane with a porous net structure formed by PEDOT, PSS/WPU composite stretchable thermoelectric fibers on the surface of filter paper by vacuum filtration, and mechanically pressing the obtained fiber membrane.
Further, the polyurethane used is cationic, anionic or neutral polyurethane or polyurethane derivative.
Further, the organic solvent used in the coagulation bath in the step (c) is any one of isopropyl alcohol, ethanol, acetone, ethylene glycol, dimethyl sulfoxide, and a mixed solvent in which the above organic solvent is mixed with water.
Further, the diameter of the PEDOT/PSS/WPU composite stretchable thermoelectric fiber before the preliminary clipping ranges from 50nm to 100 μm.
Further, the thickness of the fibrous membrane having a porous network structure is 0.1 μm to 1 mm.
Compared with the prior art, the invention has the following advantages:
1. the preparation method of the film material capable of realizing the temperature and strain dual-function self-driven sensing utilizes the thermoelectric effect of PEDOT: PSS, the prepared composite fiber film material with the porous reticular structure generates voltage signals (delta V is S delta T, S is the Seebeck coefficient of the film material) under the condition that the temperature difference exists between two ends of the material (the temperature at the two ends is T1 and T2 respectively), the temperature difference value (delta T is T2-T1) can be obtained by detecting the voltage signals, and when the temperature excitation is applied to one end of the film and the other end is in a normal temperature state (for example, T1 is 298K), the temperature signal at the detection end can be calculated according to the temperature difference signals, so that the detection of the temperature can be realized (T2 is delta T298 + K).
2. According to the preparation method of the film material capable of realizing the temperature and strain dual-function self-driven sensing, the composite fiber film with the porous net-shaped structure is composed of a PEDOT (PolyEthyl Ether sulfonate)/WPU (PolyEthylene sulfonate) composite fiber structure, point contact is formed between fibers, the point contact state between different fibers is changed under a strain condition, and the resistance of the composite fiber film with the porous net-shaped structure is changed along with the change of the point contact state, so that the strain detection is realized.
3. According to the preparation method of the thin film material capable of realizing the temperature and strain dual-function self-driven sensing, provided by the invention, when the temperature and strain excitation is simultaneously applied to one section of the thin film material, a voltage signal generated by temperature difference can be used as a signal source, and the strain quantity is detected by using the ratio (I/I0) of the current (I) flowing in the thin film under the thermoelectric pressure to the current (I0) flowing in the thin film under the condition that only the temperature excitation exists and no strain exists, so that the thermoelectric pressure is used as the signal source in the testing process, and the dual-function self-driven detection of the temperature and the strain can be realized without any power supply testing device.
For the reasons, the invention can be widely popularized in the field of sensors.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a scanning electron microscope image of PEDOT, PSS/WPU composite fiber porous reticular film material.
FIG. 2 shows the resistance response of the porous reticular film of the PEDOT-PSS/WPU composite fiber under 1% strain.
FIG. 3 shows the resistance response of the porous reticular film of PEDOT PSS/WPU composite fiber under 10% strain.
FIG. 4 shows the resistance response of the porous reticular film of PEDOT PSS/WPU composite fiber under the strain of 15%.
FIG. 5 shows the resistance response of the porous reticulated film of PEDOT PSS/WPU composite fiber at 20% strain.
FIG. 6 is a voltammetry characteristic curve of the porous reticular film of the PEDOT/PSS/WPU composite fiber based on a self-driven working mode under the condition of 15K temperature difference.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
Example 1
The invention provides a preparation method of a film material capable of realizing temperature and strain dual-function self-driven sensing, which specifically comprises the following steps:
(a) adding 10 mass percent of 1-ethyl-3-methylimidazolium tricyanomethane ionic liquid into a PEDOT (Polytetrafluoroethylene-PSS) aqueous solution, magnetically stirring for 3 hours under the condition of oil bath at 60 ℃, and adjusting the viscosity of a mixed solution to 1000-10000 CPS;
(b) further mixing the mixed solution prepared in the step (a) with an aqueous polyurethane dispersion solution, wherein the mass ratio of PEDOT to PSS to polyurethane in the mixed solution is 6:4
(c) Sucking the mixed liquid prepared in the step (b) into an injector, selecting a needle head with the diameter of 25G to be assembled at the tail end of the injector, installing the injector on a micro-injection pump, immersing the outlet of the needle head in an organic solvent (ethanol) coagulation bath, setting the propelling speed of the micro-injection pump to be 3 mu L/h, pushing the mixed liquid out of the injector into the ethanol coagulation bath, connecting the lower part of the coagulation bath with a rotary table, adjusting the speed of the rotary table to be 2rad/min, and obtaining continuous PEDOT (PSS)/WPU (Poly ethylene propylene ether ketone) composite stretchable thermoelectric fiber in the coagulation bath; then, after the PEDOT, PSS/WPU composite stretchable thermoelectric fiber is placed in an ethanol coagulation bath for ten minutes, the PEDOT/PSU composite stretchable thermoelectric fiber is taken out of the coagulation bath, is vertically hung and dried in a room temperature environment, and a weight of 40mg is hung at the tail end of the PEDU composite stretchable thermoelectric fiber during drying so as to prevent the PEDU composite stretchable thermoelectric fiber from curling in a natural state;
(d) taking the PEDOT (PSS/WPU) composite stretchable thermoelectric fiber dried in the step (c), and primarily shearing the PEDOT/PSU composite stretchable thermoelectric fiber by using scissors; putting the primarily sheared fiber into a beaker, adding sufficient mixed solution of water and ethanol, and vibrating and crushing the short fiber by using an ultrasonic vibration crushing technology to obtain a fiber suspension;
(e) and collecting a fiber membrane with a porous net structure formed by PEDOT (PSS)/WPU (WPU) composite stretchable thermoelectric fibers on the surface of 0.45-micrometer filter paper by vacuum filtration, wherein the total mass of the PEDOT/PSS/WPU composite fibers is 10mg, and mechanically pressing the obtained fiber membrane by using a manual film pressing machine to ensure that the structure is firm and stable.
FIG. 1 is a scanning electron microscope image of PEDOT, PSS/WPU composite fiber porous reticular film material.
Further, the polyurethane used is cationic, anionic or neutral polyurethane or a polyurethane derivative (see patents CN106084162B, CN102993408B, etc. for polyurethane derivatives).
Further, the organic solvent used in the coagulation bath in the step (c) may be any one of isopropyl alcohol, acetone, ethylene glycol, dimethyl sulfoxide, and a mixed solvent of the above organic solvent and water.
Further, the diameter of the PEDOT/PSS/WPU composite stretchable thermoelectric fiber before the preliminary clipping ranges from 50nm to 100 μm.
Further, the thickness of the fibrous membrane having a porous network structure is 0.1 μm to 1 mm.
Further, temperature detection is carried out within the temperature range of 0-200 ℃ and with the detection accuracy of 0.01-2K: and (e) testing by using a film thermoelectric parameter testing system, wherein the Seebeck coefficient of the PEDOT/PSU composite fiber porous reticular film obtained in the step (e) is 20 muV/K, and a voltage signal of 20 muV is generated at two ends of the film material under the condition of every 1K temperature difference.
Further, strain detection is carried out in the strain detection range of 0.5% -50% and under the condition of the strain detection sensitivity factor of 5-50: and (e) coating silver paste on two ends of the PEDOT/WPU composite fiber porous reticular film obtained in the step (e), connecting copper wires, placing the film in a clamp clamped in a tensile machine, and performing strain test under the conditions that the initial length between two electrodes is 1cm and the strain loading rate is 2 mm/min.
Furthermore, under the condition that temperature and strain excitation is simultaneously applied to one section of the PEDOT, PSS/WPU composite fiber porous reticular film material, a voltage signal generated by temperature difference can be used as a signal source, and double-function self-driven detection of temperature and strain is realized.
FIGS. 2-5 show the response of the PEDOT PSS/WPU composite fiber porous reticular membrane to strain stimulus applied from the outside. The tensile strain applied by external stretching is directly reflected as the relative change of the resistance value of the porous reticular film. In the actual operation process, the tensile strain quantity applied to the film can be obtained by testing the relative change of the resistance values of the resistors at the two ends of the film. Fig. 2-5 demonstrate the sensing ability of the composite fibrous porous reticulated film to tensile strain. The tensile strain amount of 1% corresponds to a relative change in the electrical resistance of the film of 0.035. The tensile strain amount of 10% corresponds to a relative change in the electrical resistance of the film of 0.45. The tensile strain amount of 15% corresponds to a relative change in the electrical resistance of the film of 1.28. The tensile strain amount of 20% corresponds to a relative change in the electrical resistance of the film of 1.88.
FIG. 6 is a voltammetry characteristic curve of the PEDOT/PSS/WPU composite fiber porous reticular film based on a self-driven working mode under the temperature difference condition of 15K:
under the condition that temperature difference and strain exist at two ends of the film material at the same time, temperature sensing can be realized according to a voltage signal (delta V) generated by the temperature difference. There will be a voltage shift corresponding to the current-voltage characteristic of the film under this condition. The solid line in fig. 6 is a current-voltage characteristic curve of the thin film under an unstrained condition, corresponds to a current value (I0) of 10.84mA when the voltage is zero, and is a current value flowing through the thin film under an unstrained condition using a thermal voltage generated by temperature excitation as a signal source. As the strain gradually increases, the slope of the voltammogram curve in fig. 6 changes, meaning that the resistance value of the thin film material changes. The dashed, dotted and dashed lines in fig. 6 correspond to the strain conditions of 10%, 15% and 20% strain, respectively. Accordingly, when the voltage is zero, the current values (I) corresponding to the broken line, the dotted line, and the chain line are 7.26mA, 6.60mA, and 5.89mA, respectively. The strain is calculated as the ratio (I/I0) of the current (I) flowing through the film at this thermal voltage to the current (I0) flowing through the film in the absence of strain in the presence of temperature stimulus alone. Therefore, the thermal voltage is used as a signal source in the testing process, any testing device containing a power supply is not needed, and the dual-function self-driven detection of temperature and strain can be realized.
The above examples demonstrate that: the PEDOT/PSS/WPU composite fiber porous reticular film material prepared by the technical scheme provided by the invention can realize difunctional self-driven sensing of temperature and strain.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; 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 or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (5)
1. A preparation method of a thin film material capable of realizing temperature and strain dual-function self-driven sensing is characterized by comprising the following steps:
(a) adding ionic liquid into a PEDOT (PSS) aqueous solution, magnetically stirring under the condition of constant-temperature heating, and adjusting the viscosity of a mixed solution;
(b) further mixing the mixed solution prepared in the step (a) with an aqueous polyurethane dispersion;
(c) sucking the mixed solution prepared in the step (b) into an injector, mounting the injector on a micro-injection pump, immersing the outlet of a needle in an organic solvent coagulating bath, pushing the mixed solution out of the injector into the coagulating bath, and obtaining continuous PEDOT (PSS)/WPU (WPU) composite stretchable thermoelectric fiber in the coagulating bath; then, taking the PEDOT, PSS/WPU composite stretchable thermoelectric fiber out of the coagulation bath, and vertically hanging and drying the PEDOT, PSS/WPU composite stretchable thermoelectric fiber in a room-temperature environment;
(d) taking the PEDOT (PSS)/WPU (WPU) composite stretchable thermoelectric fiber dried in the step (c), and primarily shearing the PEDOT/PSS/WPU composite stretchable thermoelectric fiber; putting the primarily sheared fiber into a beaker, adding a mixed solution of water and ethanol, and vibrating and crushing the short fiber by using an ultrasonic vibration crushing technology to obtain a fiber suspension;
(e) collecting a fiber membrane with a porous net structure formed by PEDOT, PSS/WPU composite stretchable thermoelectric fibers on the surface of filter paper by vacuum filtration, and mechanically pressing the obtained fiber membrane.
2. The method for preparing the film material capable of achieving the temperature and strain dual-functional self-driven sensing according to claim 1, wherein the polyurethane is cationic, anionic or neutral polyurethane or polyurethane derivative.
3. The method for preparing a temperature and strain dual-functional self-driven sensing thin film material according to claim 1, wherein the organic solvent used in the coagulating bath in step (c) is any one of isopropyl alcohol, ethanol, acetone, ethylene glycol, dimethyl sulfoxide and a mixed solvent of the above organic solvent and water.
4. The preparation method of the film material capable of realizing the temperature and strain dual-function self-driven sensing is characterized in that the diameter of PEDOT/PSS/WPU composite stretchable thermoelectric fiber before the preliminary shearing is in the range of 50nm-100 μm.
5. The method for preparing the thin film material capable of realizing the temperature and strain dual-functional self-driven sensing, according to claim 1, is characterized in that the thickness of the fiber film with the porous net structure is 0.1 μm-1 mm.
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Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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