CN112679964B - Silver nanowire/organic silicon elastomer self-repairing flexible material, preparation method thereof and flexible sensor - Google Patents
Silver nanowire/organic silicon elastomer self-repairing flexible material, preparation method thereof and flexible sensor Download PDFInfo
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Abstract
The invention relates to the technical field of flexible sensor materials, in particular to a silver nanowire/organic silicon elastomer self-repairing flexible material, a preparation method thereof and a flexible sensor. The invention adopts a strong and weak bond crosslinking mechanism and a physical blending method to realize the tight combination of the silver nanowires and the organic silicon elastomer; the surface of the silver nanowire is modified with polyvinylpyrrolidone, so that more hydrogen bonds can be formed with the synthesized self-repairing organic silicon elastomer, the repairing speed of the silver nanowire is improved, the dispersibility of the silver nanowire in a substrate is enhanced, and the conductivity and the sensing sensitivity of the flexible material are improved. The flexible sensor provided by the invention has excellent self-repairability, extensibility and high conductivity, can meet the performance requirements of multiple scenes on the flexible sensor, and can monitor the motion of each part of a human body.
Description
Technical Field
The invention relates to the technical field of flexible sensor materials, in particular to a silver nanowire/organic silicon elastomer self-repairing flexible material, a preparation method thereof and a flexible sensor.
Background
The flexible sensor is an electronic device which is prepared by utilizing flexible materials and has super strong environmental adaptability. Resistive strain sensors based on conductive elastomers are sensitive to changes in strain, which when an external strain is applied, results in a change in resistance. Compared with traditional sensors based on rigid semiconductors, metals and ceramics, flexible sensors have great advantages in terms of stretchability, which makes them have great application potential in the field of wearable devices. However, the flexible sensor is easy to age and damage, and accuracy and reliability of data information are affected. The flexible sensor with self-repairing performance can prolong the service life of electronic devices and improve the stability of collected information, so that high repairing efficiency becomes an ideal performance requirement of a new generation of flexible sensors.
The flexible sensor is generally composed of a flexible substrate and conductive fillers, the sensitivity and flexibility of the flexible sensor are greatly influenced by the selection of the substrate material, and the sensor taking an elastomer as the flexible substrate has great application potential. The conductive network can be constructed by filling conductive nano particles in the flexible substrate material, and the uniform conductive composite material can be formed by the good interface compatibility of the elastomer. However, the addition of most conductive fillers can seriously affect the comprehensive properties of flexibility, transparency and the like of the flexible sensor, thereby limiting the application of the flexible sensor in certain aspects. The sensor based on the silver nanowire-self-repairing elastomer conductive network is widely applied to the preparation of flexible sensing devices due to high conductivity and high transparency. For example, chinese patent CN111393651A discloses a stretchable electronic material using a self-repairing polysiloxane elastomer as a matrix, in which a conductive filler (multi-walled carbon nanotubes or silver nanowires, etc.) of the stretchable electronic material is attached to the surface of the polysiloxane elastomer in the form of a dispersion by spraying, and during the use of the stretchable electronic material, on one hand, the conductive network cannot be self-repaired after being damaged; on the other hand, the conductive network under tensile strain will break rapidly.
Therefore, the stretchability, the sensitivity, the repair performance and the like of the high-performance self-repairable strain sensor based on the silver nanowires have a great promotion space. There is an important need to develop a new type of flexible self-healing strain sensor.
Disclosure of Invention
In order to overcome the defects of the prior art, one of the purposes of the invention is to provide a preparation method of a silver nanowire/organic silicon elastomer self-repairing flexible material, a strong and weak bond crosslinking mechanism and a physical blending method are adopted to realize the tight combination of the silver nanowire and the organic silicon elastomer, and the prepared silver nanowire/organic silicon elastomer has excellent self-repairing property and high conductivity.
The second purpose of the invention is to provide a silver nanowire/organic silicon elastomer self-repairing flexible material prepared by the preparation method, which has excellent self-repairing performance and high conductivity.
Meanwhile, the invention also aims to provide a flexible sensor which is made of the silver nanowire/organic silicon elastomer self-repairing flexible material, has excellent self-repairing performance and high conductivity, can meet the performance requirements of multiple scenes on the flexible sensor, and can monitor the motion of each part of a human body.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a silver nanowire/organic silicon elastomer self-repairing flexible material comprises the steps of blending a self-repairing organic silicon elastomer solution and a silver nanowire dispersion liquid with the surface modified by polyvinylpyrrolidone, and then drying and forming to prepare the silver nanowire/organic silicon elastomer self-repairing flexible material.
Optionally, the solution is stirred for 3-5 hours under the blending condition of 30-50 ℃.
Optionally, the self-repairing silicone elastomer solution is prepared by dissolving a self-repairing silicone elastomer in an organic solvent; the silver nanowire dispersion liquid is prepared by dispersing silver nanowires in an organic solvent. Further, the organic solvent is tetrahydrofuran.
In the embodiment of the invention, the mass ratio of the self-repairing silicone elastomer to the silver nanowires is 100: 1 to 3.
The preparation method comprises the following steps of firstly preparing the self-repairing organic silicon elastomer: mixing amino-terminated polydimethylsiloxane and chloroform in an inert gas environment, adding a catalyst, and stirring for reaction under an ice bath condition to obtain a reaction mixed solution; dropwise adding a blending solution of diisocyanate raw materials and chloroform into the reaction mixed solution, continuously stirring under ice bath, and then stirring at normal temperature for reaction to obtain an elastomer product; adding terephthalyl alcohol into the elastomer product, stirring at normal temperature to react, cooling, removing unreacted micromolecule substances, and drying to obtain the self-repairing organic silicon elastomer.
Optionally, the diisocyanate raw material is selected from toluene diisocyanate, hexamethylene diisocyanate, isophorone diisocyanate, or diphenylmethane diisocyanate. Optionally, the inert gas environment is an argon or nitrogen environment. The self-repairing organic silicon elastomer with high elasticity, high repairing efficiency and high transparency is synthesized by adopting polydimethylsiloxane, diisocyanate raw materials and ethylene diamine serving as a chain extender under the ice bath condition.
The preparation method also comprises the following steps of preparing the silver nanowire with the surface modified with polyvinylpyrrolidone: dissolving silver nitrate in ethylene glycol to prepare a silver nitrate solution; dissolving sodium chloride and polyvinylpyrrolidone in ethylene glycol to prepare a mixed solution; dropwise adding the mixed solution into a silver nitrate solution at the temperature of 100-120 ℃ and the stirring speed of 500-800 rpm/min, uniformly mixing, heating to 160-180 ℃ in a high-pressure reaction kettle, keeping the temperature for 6-8 hours, naturally cooling to room temperature, washing, acetone precipitating, centrifuging and freeze-drying the product in sequence to obtain the silver nanowire with the surface modified with polyvinylpyrrolidone.
According to the preparation method of the silver nanowire/organic silicon elastomer self-repairing flexible material, the self-repairing organic silicon elastomer solution is blended with the silver nanowire dispersion liquid with the surface modified with polyvinylpyrrolidone, on one hand, a strong and weak bond crosslinking mechanism is matched with a physical blending method, so that the silver nanowire and the organic silicon elastomer are tightly combined, and the defect that a conductive network only exists on the surface of the material and cannot be self-repaired after the conductive network is damaged in the flexible material prepared by printing the silver wire on the surface in the prior art is overcome; and the conductive network of the silver wire can be rapidly broken under tensile strain, so that the strain detection range is generally lower than 50% and other technical defects are caused.
On the other hand, the surface of the silver nanowire is coated with polyvinylpyrrolidone, so that more hydrogen bonds are formed with the synthesized self-repairing organic silicon elastomer, the repairing speed of the silver nanowire is improved, and the dispersibility of the silver nanowire in the matrix is enhanced, so that the conductivity and the sensing sensitivity of the silver nanowire/organic silicon elastomer self-repairing flexible material are enhanced.
In a word, the preparation method is simple and convenient, and is easy for scale-up and mass production. The self-repairing organic silicon elastomer is based on reversible strong and weak multiple hydrogen bond repairing mechanism, the hydrogen bond effect is enhanced by the blending introduction of the silver nanowires with the surfaces modified with the polyvinylpyrrolidone, and the flexible material is endowed with excellent self-repairing property, conductivity, tensile property, high transparency and sensitive sensing performance. The flexible material prepared by the invention has a uniformly dispersed silver nanowire/organic silicon composite system, the tensile strain can reach 1000%, and the strain stability detection range exceeds 500%; and the multiple hydrogen bond action in the silver nanowire/organic silicon composite system ensures that the conductive network can still be perfectly self-repaired after being damaged, so that the original tensile and sensing performances of the material are recovered.
A silver nanowire/organic silicon elastomer self-repairing flexible material is prepared by the preparation method.
A flexible sensor is prepared from the silver nanowire/organic silicon elastomer self-repairing flexible material. The silver nanowire/organic silicon elastomer self-repairing flexible material prepared by the invention has good flexibility, tensile property and repairing property, leads can be directly connected to the two ends of the material externally, and strain sensing is realized by monitoring deformation by measuring the resistance value change in the material deformation process. The elastic membrane can also be used as a substrate to load the silver nanowire/organic silicon elastomer self-repairing flexible material to assemble a traditional resistance-type sensor; or dissolving the strain sensor by using an organic solvent (such as tetrahydrofuran, chloroform and dimethylformamide), coating the solution on a flexible substrate (such as a fabric surface), and externally connecting leads at two ends of the material in a drying process to obtain the wearable strain sensor integrated with the flexible substrate.
The repairing and sensing principle of the flexible strain sensor of the invention is as follows:
(1) the repair mechanism is as follows: reversible multiple hydrogen bonds formed in the elastomer self-repairing flexible material can not only quickly repair cracks, but also consume energy generated by strain, so that the silver nanowire/organic silicon elastomer self-repairing flexible material has excellent repairing performance and tensile performance. When the material is damaged by external force, the generated cracks gradually disappear along with the thermal motion of the molecular chain and the reconstruction of the reversible hydrogen bonds. The molecular chain motion degree of the silver nanowire/organic silicon elastomer is increased under the heating condition, so that the recombination of hydrogen bonds is facilitated, and the self-repairing speed and the repairing efficiency can be further improved;
(2) sensing principle: under the action of mechanical strain and the like, the silver nanowire/organic silicon elastomer conductive network in the sensor deforms, so that the resistance in the elastomer changes to a certain degree, and the change of the shape of the elastomer is converted into the change value of the resistance and the current. The multiple hydrogen bonds formed in the silver nanowires/organic silicon elastomer enhance the dispersibility and the conductivity of the silver nanowires and improve the sensing sensitivity of the composite elastomer.
Drawings
FIG. 1 is a comparison graph of self-repair efficiency detection results of silver nanowires/silicone elastomer self-repair flexible materials with different silver nanowire contents;
FIG. 2 is an I-T plot of a flexible sensor of the present invention for facial expression (drum cheek) sensing;
FIG. 3 is an I-T plot of a flexible sensor of the present invention for wrist joint bending sensing detection;
FIG. 4 is a graph comparing the sensing performance before and after repair of a flexible sensor according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The equipment and reagents used in the examples and the experimental examples were commercially available except as specifically indicated.
Example 1
The embodiment provides a silver nanowire/silicone elastomer self-repairing flexible material, and the preparation method specifically comprises the following operation steps:
s1, preparation of self-repairing organic silicon elastomer
The oxygen in the three-necked flask was removed by repeating the operation of introducing argon after vacuumizing three times, and then the three-necked flask was placed in an ice bath. 10.2ml of amino-terminated polydimethylsiloxane (H)2N–PDMS–H2N, Mn ═ 5000) were added in portions to a three-necked flask using a pipette. 10ml of the solution is added into a three-neck flaskChloroform as a solvent and 0.5ml of triethylamine as a catalyst, and mechanically stirring the mixed solution for 1h under the ice bath condition to obtain a reaction mixed solution;
0.4336g of toluene diisocyanate (TDI,0.0025mol, Mn. RTM. 174.16) was dissolved in 2ml of chloroform to prepare a mixed solution, and the mixed solution was added dropwise to the reaction mixture. Stirring in ice bath for 1h, stirring at normal temperature for 3h, and pouring out the viscous product (organic silicon elastomer) from the three-neck flask;
adding 0.37ml of terephthalyl alcohol into the viscous product, continuously stirring for 1h at normal temperature, slowly pouring the product into cold water, removing unreacted micromolecules, and fully drying to obtain a transparent colorless organic silicon elastomer;
s2. preparation of silver nanowires
Dissolving 0.68g of silver nitrate in 60ml of ethylene glycol to obtain a silver nitrate/ethylene glycol solution; then 4.6Mg of sodium chloride and 1.766g of polyvinylpyrrolidone (Mw is 1.3Mg/mol) are dissolved in 40ml of ethylene glycol to obtain a polyvinylpyrrolidone/sodium chloride/ethylene glycol mixed solution; stirring a silver nitrate/ethylene glycol solution at the speed of 600rpm/min at the temperature of 120 ℃, dropwise adding a polyvinylpyrrolidone/sodium chloride/ethylene glycol mixed solution into the silver nitrate/ethylene glycol solution at the speed of 5ml/min under vigorous stirring, mixing for 5min, transferring to a 125ml high-pressure kettle, heating to 160 ℃, keeping the temperature for 7h, cooling to room temperature, washing a resultant with methanol for 3 times, precipitating with acetone for 20h, centrifuging for 5 times at 5000rpm/min to obtain a glossy and filamentous silver nanowire solution, and freeze-drying to obtain silver nanowires;
s3, preparation of silver nanowire-organic silicon elastomer
Carrying out ultrasonic treatment on 30mg of silver nanowires in S2 for 10min to uniformly disperse the silver nanowires in 5ml of tetrahydrofuran solution; weighing 1g of the self-repairing silicone elastomer prepared in the step S1, and dissolving in 5ml of tetrahydrofuran to obtain a self-repairing silicone elastomer solution;
mixing the silver nanowire dispersion liquid with a self-repairing organic silicon elastomer solution, and stirring for 3 hours at 40 ℃ to obtain a nano composite solution, wherein the mass fraction of silver nanowires in the solution relative to the organic silicon elastomer is 3 wt%; and pouring the nano composite solution into a polytetrafluoroethylene mold for full drying to obtain the silver nanowire/organic silicon elastomer self-repairing flexible material containing 3 wt% of silver nanowires.
It should be understood that the stirring temperature for mixing the silver nanowire dispersion liquid and the self-repairing organic elastomer solution can be adjusted within the range of 30-50 ℃ in combination with the actual blending effect, and the stirring time can be adjusted within 3-5 hours.
Example 2
The embodiment provides a flexible sensor, which is manufactured by using the silver nanowire/silicone elastomer self-repairing flexible material prepared in the above embodiment 1, and a conventional resistive sensor is assembled by using an elastic film (for example, a stretchable adhesive tape) as a substrate and using the flexible material prepared in the embodiment 1 of the present invention as a conductive material.
It should be understood that organic solvents such as: tetrahydrofuran, chloroform and dimethylformamide are dissolved in the flexible material, and then the solution is coated on a flexible substrate (such as the surface of a fabric), and conducting wires are externally connected to two ends of the material in a drying process, so that the wearable sensor integrated with the flexible substrate is obtained.
Test example 1
Test subjects: the silver nanowire/silicone elastomer self-repairing flexible material with the mass fraction of silver nanowires of 3 wt% prepared in example 1, the silver nanowire/silicone elastomer self-repairing flexible material with the mass fraction of silver nanowires of 0 wt% respectively prepared in the same manner as in example 1, the silver nanowire/silicone elastomer self-repairing flexible material with the mass fraction of silver nanowires of 1 wt% respectively prepared in the same manner as in example 1, and the silver nanowire/silicone elastomer self-repairing flexible material with the mass fraction of silver nanowires of 2 wt% respectively prepared in the same manner as in example 1
Test methods and results:
1. detecting the self-repairing efficiency of different test objects for repairing for 9 hours at 60 ℃:
the self-repairing efficiency detection is characterized by the change of the tensile strength of the test material before and after self-repairing, and the repairing efficiency is that the tensile strength of the repaired sample/the tensile strength of the original sample is multiplied by 100 percent.
The test results are shown in fig. 1: the results shown in fig. 1 show that, with the increase of the content of the silver nanowires, the repair efficiency of the silver nanowire/silicone elastomer self-repair flexible material prepared by the method of the present invention is continuously improved, and the reason for analyzing the repair is that the silver nanowires modified with polyvinylpyrrolidone on the surface are embedded into the network structure of the silicone elastomer in a blending manner, and the silver nanowires subjected to surface modification treatment form more hydrogen bonds with the silicone elastomer, so that reversible strong and weak multiple hydrogen bond networks in the silicone elastomer are enriched, and the self-repair efficiency of the prepared flexible material is improved.
2. Detecting the mechanical property, the sensing sensitivity and the strain test range of different test objects:
the test method comprises the following steps:
mechanical properties: the tensile property is tested by adopting a universal mechanical property tester: the sample is stretched at a rate of 10mm/min until the sample breaks, and the tensile strength, tensile modulus and strain at break are obtained by tensile property testing;
sensing sensitivity: the method comprises the following steps of monitoring the relative resistance change value of a strain sensor on line in the stretching process of the strain sensor, wherein the sensitivity is the change rate of the relative resistance of the sensor, and the higher the change rate is, the more sensitive the sensor is;
strain test range: the strain monitoring range is the maximum strain monitoring range in which the relative resistance value of the sensor can keep good linear relation stability and sensing periodicity in the stretching and recovering process of the sensor, namely the strain monitoring range in which the sensor can stably work.
The test results are shown in table 1 below:
TABLE 1 mechanical properties, sensing sensitivity, Strain test Range for different silver nanowire content
| Silver wire content | Tensile modulus | Strain at break | Sensitivity of the probe | Range of |
| 0％ | 365kPa | 1200％ | - | - |
| 1％ | 505kPa | 1030％ | 0.82 | 0-700％ |
| 2％ | 723kPa | 929％ | 1.54 | 0-600％ |
| 3％ | 907kPa | 893％ | 2.06 | 0-500％ |
From the results shown in table 1, it can be seen that with the increase of the content of the silver nanowires, the comprehensive properties of the self-repairing flexible material prepared by the preparation method of the present invention, such as mechanical properties, sensing sensitivity, and strain test range, are all improved.
Test example 2 various performance tests of the flexible sensor provided in embodiment 2 of the present invention
1. The flexible sensor provided in embodiment 2 of the present invention is used for facial expression sensing detection and knee flexion sensing detection, and the results are shown in fig. 2 and fig. 3, respectively: the result shows that the flexible sensor made of the self-repairing flexible material can accurately monitor the facial expression and the bending change state of the knee in real time.
2. After the flexible sensor provided by embodiment 2 of the present invention is subjected to heat treatment at 40 ℃ for 6 hours, the sensing performance difference of the flexible sensor applied to wrist bending detection before and after the heat treatment is detected, and the result is shown in fig. 4, which shows that the sensing output signals before and after the heat treatment are consistent, so that it can be seen that the flexible sensor prepared by using the flexible material of the present invention still maintains good sensing performance after the heat treatment.
3. Compared with the repair efficiency of the flexible sensor prepared by the existing different materials, the results are shown in the following table 2:
TABLE 2 results of Flexible sensor research
From the results shown in table 2, it can be seen that the flexible sensor made of the flexible material prepared by the preparation method of the present invention has high repair efficiency compared with other existing flexible sensors.
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 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 (8)
1. A preparation method of a silver nanowire/organic silicon elastomer self-repairing flexible material is characterized by comprising the steps of blending a self-repairing organic silicon elastomer solution and a silver nanowire dispersion liquid with the surface modified with polyvinylpyrrolidone, and then drying and forming to prepare the silver nanowire/organic silicon elastomer self-repairing flexible material;
the self-repairing silicone elastomer is prepared as follows: mixing amino-terminated polydimethylsiloxane and chloroform in an inert gas environment, adding a catalyst, and stirring for reaction under an ice bath condition to obtain a reaction mixed solution; dropwise adding a blending solution of diisocyanate raw materials and chloroform into the reaction mixed solution, continuously stirring under ice bath, and then stirring at normal temperature for reaction to obtain an elastomer product; adding terephthalyl alcohol into an elastomer product, stirring at normal temperature for reaction, sequentially cooling, removing unreacted micromolecule substances, and drying to obtain the self-repairing organic silicon elastomer;
preparing silver nanowires with surfaces modified with polyvinylpyrrolidone: dissolving silver nitrate in ethylene glycol to prepare a silver nitrate solution; dissolving sodium chloride and polyvinylpyrrolidone in ethylene glycol to prepare a mixed solution; dropwise adding the mixed solution into a silver nitrate solution at the temperature of 100-120 ℃ and the stirring speed of 500-800 rpm/min, uniformly mixing, heating to 160-180 ℃ in a high-pressure reaction kettle, keeping the temperature for 6-8 hours, naturally cooling to room temperature, washing, acetone precipitating, centrifuging and freeze-drying the product in sequence to obtain the silver nanowire with the surface modified with polyvinylpyrrolidone.
2. The preparation method of the silver nanowire/silicone elastomer self-repairing flexible material of claim 1, wherein the solution blending is performed at 30-50 ℃ for 3-5 hours.
3. The preparation method of the silver nanowire/silicone elastomer self-repairing flexible material of claim 1, wherein the self-repairing silicone elastomer solution is prepared by dissolving a self-repairing silicone elastomer in an organic solvent; the silver nanowire dispersion liquid is prepared by dispersing silver nanowires in an organic solvent.
4. The method for preparing the silver nanowire/silicone elastomer self-repairing flexible material as claimed in claim 3, wherein the organic solvent is tetrahydrofuran.
5. The preparation method of the silver nanowire/silicone elastomer self-repairing flexible material as claimed in any one of claims 1 to 4, wherein the mass ratio of the self-repairing silicone elastomer to the silver nanowires is 100: 1 to 3.
6. The method for preparing the silver nanowire/silicone elastomer self-repairing flexible material according to claim 1, wherein the diisocyanate raw material is selected from toluene diisocyanate, hexamethylene diisocyanate, isophorone diisocyanate, or diphenylmethane diisocyanate.
7. A silver nanowire/silicone elastomer self-repairing flexible material is characterized by being prepared by the preparation method of any one of claims 1-6.
8. A flexible sensor, which is prepared from the silver nanowire/silicone elastomer self-repairing flexible material as claimed in claim 7.
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