CN111941985B - Flexible strain sensing material and preparation method thereof - Google Patents

Flexible strain sensing material and preparation method thereof Download PDF

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CN111941985B
CN111941985B CN202010867254.9A CN202010867254A CN111941985B CN 111941985 B CN111941985 B CN 111941985B CN 202010867254 A CN202010867254 A CN 202010867254A CN 111941985 B CN111941985 B CN 111941985B
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waterborne polyurethane
silver
strain sensing
anionic
sensing material
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CN111941985A (en
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毕曙光
曾琪
姜会钰
冉建华
蔡光明
程德山
权衡
倪丽杰
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Wuhan Textile University
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Wuhan Textile University
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    • B32B27/00—Layered products comprising a layer of synthetic resin
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    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
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Abstract

The invention provides a flexible strain sensing material and a preparation method thereof. Above-mentioned flexible strain sensing material, silver nano wire/anion waterborne polyurethane mix conductive film layer has stronger adhesion, and through the bonding with the anion waterborne polyurethane rete on the flexible substrate layer, has greatly increased the bonding fastness between flexible substrate layer and the silver nano wire, is difficult to drop after repeated friction or deformation, and the durability is good. In addition, the silver nanowires are uniformly dispersed in the silver nanowire/anionic waterborne polyurethane mixed conductive film through prefabricating the silver nanowire/anionic waterborne polyurethane mixed conductive film, and the dispersion is more uniform, so that the conductivity uniformity of the silver nanowire/anionic waterborne polyurethane mixed conductive film is better.

Description

Flexible strain sensing material and preparation method thereof
Technical Field
The invention relates to the technical field of strain sensing materials, in particular to a flexible strain sensing material and a preparation method thereof.
Background
The flexible strain sensing material has great potential in the fields of wearable displays, intelligent clothing, health monitoring and the like. Silver nanowires (AgNWs) are widely used as conductive materials due to their high surface area, low resistance, low mass density, and high stability. The traditional flexible strain sensing material adopts silver nanowires to modify textiles, which can endow flexible fabric with conductivity, and the textiles are generally modified by a spraying or dipping method. In the using process, the silver nanowires are easy to fall off after repeated friction or deformation. Therefore, there is a pressing need for more efficient assembly methods to enhance the adhesion between the loaded conductive silver nanowires and the fibrous substrate. In addition, silver nanowires are prone to coagulation in aqueous solutions, which can affect the uniformity of conductivity. These disadvantages also limit the application of silver nanowires in the field of flexible strain sensing materials.
Disclosure of Invention
Based on this, the invention provides a flexible strain sensing material and a preparation method thereof, aiming at the technical problems that the fabric fiber of the traditional silver nanowire modified textile is lack of adhesiveness with the silver nanowire, so that the durability is poor, and the silver nanowire is easy to fall off after repeated friction or deformation in the using process.
The invention provides a flexible strain sensing material which comprises a flexible substrate layer, an anionic waterborne polyurethane film layer and a silver nanowire/anionic waterborne polyurethane mixed conductive film layer which are sequentially laminated.
On the basis of the technical scheme, the invention can further have the following specific selection or optimized selection.
In one embodiment, the thickness ratio of the flexible substrate layer, the anionic aqueous polyurethane film layer and the silver nanowire/anionic aqueous polyurethane mixed conductive film layer is (1.5:1) - (3: 1).
In one embodiment, when the stretching degree of the flexible strain sensing material is 0-60%, the resistance change value of the flexible strain sensing material is in an exponential relation with the stretching degree.
The invention also provides a preparation method of the flexible strain sensing material, which is characterized by comprising the following steps of:
pressing the anionic waterborne polyurethane film on the flexible substrate layer by a hot pressing method;
and pressing the silver nanowire/anionic waterborne polyurethane mixed conductive film on one side of the anionic waterborne polyurethane film of the flexible base material layer by a hot pressing method.
In one embodiment, the preparation method of the silver nanowire/anionic waterborne polyurethane mixed conductive film comprises the following steps:
mixing the silver nanowire water dispersion, anionic waterborne polyurethane, a foaming agent and a foam stabilizer to prepare a functional waterborne resin foaming agent;
and placing the functional aqueous resin foaming agent on a carrier plate after foaming treatment until the foam is completely eliminated, and drying the functional aqueous resin foaming agent for 1.0 to 3.0 hours at the temperature of between 60 and 80 ℃ to obtain the silver nanowire/anionic aqueous polyurethane mixed conductive film.
In one embodiment, the preparation method of the silver nanowire aqueous dispersion comprises the following steps:
providing a glycol solution of sodium chloride;
providing a glycol solution of an organic protective agent;
providing a glycol solution of a silver precursor;
mixing the glycol solution of the silver precursor with the glycol solution of the organic protective agent to obtain a first mixed solution;
mixing the ethylene glycol solution of sodium chloride with the first mixed solution to prepare a second mixed solution;
reacting the second mixed solution at the temperature of 110-150 ℃ for 6-10 h to prepare a solid-liquid mixture, and separating the solid-liquid mixture to remove the upper solution to prepare the silver nanowires;
dispersing the silver nanowires in deionized water to prepare the silver nanowire water dispersion;
the concentration of the silver nanowires in the silver nanowire water dispersion liquid is 1 g/L-10 g/L.
In one embodiment, the glycol solution of the silver precursor and the glycol solution of the organic protective agent are mixed in a manner that the glycol solution of the silver precursor is added dropwise into the glycol solution of the organic protective agent; the mixing mode of the ethylene glycol solution of sodium chloride and the first mixed solution is to drop the ethylene glycol solution of sodium chloride into the first mixed solution.
In one embodiment, the molar concentration of the ethylene glycol solution of sodium chloride is 30-37.5 mu mol/L.
In one embodiment, the mass concentration of the ethylene glycol solution of the organic protective agent is 2 g/L-10 g/L; the mass concentration of the glycol solution of the silver precursor is 2 g/L-10 g/L;
in one embodiment, the mass ratio of the organic protective agent to the silver precursor in the first mixed solution is (1:3) to (3: 1).
In one embodiment, the volume ratio of the ethylene glycol solution of sodium chloride to the first mixed solution is 1: 100.
In one embodiment, the silver nanowires have an average length of 30 to 120 μm.
In one embodiment, in the preparation method of the silver nanowire/anionic aqueous polyurethane mixed conductive film, the concentration of the anionic aqueous polyurethane is 1 g/L-10 g/L; the dry weight ratio of the silver nanowires to the anionic waterborne polyurethane is (1:9) - (3: 7).
In one embodiment, the foaming agent is any one or more of sodium dodecyl sulfate, lauryl betaine and dodecyl dimethyl benzyl ammonium chloride; the content of the foaming agent in the functional aqueous resin foaming agent is 0.1 g/L-1.0 g/L.
In one embodiment, the foam stabilizer is any one or more of sodium alginate, sodium carboxymethyl cellulose, polyvinyl alcohol, agar and guar gum; the content of the foam stabilizer in the functional aqueous resin foaming agent is 0.1-1.0 g/L.
In one embodiment, before the step of laminating the anionic waterborne polyurethane film on the flexible substrate layer by the hot pressing method, the method further comprises the following steps:
and pretreating the flexible base material layer by acetone.
In one embodiment, the acetone pretreatment is to place the flexible substrate layer in a soxhlet extractor containing acetone, circularly reflux the flexible substrate layer for 2.0 to 3.0 hours at the temperature of 60 to 70 ℃, take out the flexible substrate layer and dry the flexible substrate layer.
In one embodiment thereof, the method for preparing the anionic aqueous polyurethane film comprises the steps of:
placing the anionic waterborne polyurethane with the concentration of 10-30 g/L on a carrier plate, and drying for 1.0-2.0 h at the temperature of 60-80 ℃ to obtain the anionic waterborne polyurethane film.
In one embodiment, in the step of laminating the anionic waterborne polyurethane film on the flexible substrate layer by a hot pressing method, the hot pressing temperature is 150-170 ℃, and the hot pressing time is 1.0-3.0 min;
and in the step of laminating the silver nanowire/anionic waterborne polyurethane mixed conductive film on one side of the anionic waterborne polyurethane film of the flexible base material layer by a hot pressing method, the hot pressing temperature is 70-100 ℃, and the hot pressing time is 1.0-2.0 min.
Above-mentioned flexible strain sensing material, silver nano wire/anion waterborne polyurethane mix conductive film layer has stronger adhesion, and through the bonding with the anion waterborne polyurethane rete on the flexible substrate layer, has greatly increased the bonding fastness between flexible substrate layer and the silver nano wire, is difficult to drop after repeated friction or denaturation, and the durability is good. In addition, the silver nanowires are uniformly dispersed in the silver nanowire/anionic waterborne polyurethane mixed conductive film through prefabricating the silver nanowire/anionic waterborne polyurethane mixed conductive film, and the dispersion is more uniform, so that the conductivity uniformity of the silver nanowire/anionic waterborne polyurethane mixed conductive film is better.
Furthermore, the flexible strain sensing material has good electrical conductivity, and is large in strain range, high in sensitivity and good in stability through stretching in different degrees.
The preparation method of the flexible strain sensing material is simple to operate, mild in condition and low in cost. The prepared flexible strain sensing material has the advantages of good durability and good conductivity, and through stretching in different degrees, the flexible strain sensing material has the advantages of large strain range, high sensitivity and good stability.
Drawings
Fig. 1 is an XRD diffractogram of the silver nanowire/anionic waterborne polyurethane mixed conductive film prepared in embodiments 1 to 4 of the present invention;
FIG. 2 is an SEM micro-topography of a silver nanowire/anionic waterborne polyurethane mixed conductive film prepared in example 4 of the invention;
fig. 3 is a bar graph of silver nanowire loading-resistivity of the silver nanowire/anionic aqueous polyurethane hybrid conductive film prepared in examples 1 to 4 of the present invention;
FIG. 4 is a graph showing the tensile sensing relationship of flexible strain sensing materials prepared in examples 1 to 4 of the present invention;
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the detailed description and specific examples, while indicating the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
The reagents used in the present invention are commercially available, and the purity is chemical purity or higher.
The first aspect of the invention provides a flexible strain sensing material, which comprises a flexible substrate layer, an anionic waterborne polyurethane film layer and a silver nanowire/anionic waterborne polyurethane mixed conductive film layer which are sequentially laminated.
This flexible strain sensing material, silver nano wire/anion waterborne polyurethane mix conductive film layer have stronger adhesion, and through the anion waterborne polyurethane rete bonding with on the flexible substrate layer, have greatly increased the bonding fastness between flexible substrate layer and the silver nano wire, are difficult to drop after repeated friction or denaturation, and the durability is good. In addition, the silver nanowires are uniformly dispersed in the silver nanowire/anionic waterborne polyurethane mixed conductive film through prefabricating the silver nanowire/anionic waterborne polyurethane mixed conductive film, and the dispersion is more uniform, so that the conductivity uniformity of the silver nanowire/anionic waterborne polyurethane mixed conductive film is better.
In addition, the strain sensing material is expanded from the solution to the surface of the flexible substrate layer, so that the strain sensing material has the characteristics of good sensitivity and stable conductive capability, and the application range is widened. The flexible strain sensing material has great potential in the fields of wearable displays, intelligent clothing, health monitoring and the like.
Furthermore, the flexible strain sensing material has good conductivity, and is large in strain range, high in sensitivity and good in stability through stretching in different degrees.
Wherein, the flexible substrate layer is selected from wearable flexible materials, preferably elastic fabrics. The elastic fabric is selected as the flexible substrate layer because the elastic fabric has good strength, air permeability and wear resistance, light weight, good flexibility and deformability, and is comfortable to wear and soft in hand feeling.
As an optional embodiment, the thickness ratio of the flexible substrate layer, the anionic waterborne polyurethane film layer and the silver nanowire/anionic waterborne polyurethane mixed conductive film layer is (1.5:1) to (3: 1).
As an optional implementation mode, when the stretching degree of the flexible strain sensing material is 0-60%, the resistance change value of the flexible strain sensing material has an exponential relation with the stretching degree.
The second aspect of the present invention provides a method for preparing the above flexible strain sensing material, wherein the method comprises the following steps:
pressing the anionic waterborne polyurethane film on the flexible substrate layer by a hot pressing method;
and pressing the silver nanowire/anionic waterborne polyurethane mixed conductive film on one side of the anionic waterborne polyurethane film of the flexible substrate layer by a hot pressing method.
The preparation method of the flexible strain sensing material is simple to operate, mild in condition and low in cost. The prepared flexible strain sensing material has the advantages of good durability and good conductivity, and through stretching in different degrees, the flexible strain sensing material has a large strain range, high sensitivity and good stability.
As an alternative embodiment, the preparation method of the silver nanowire/anionic waterborne polyurethane mixed conductive film comprises the following steps:
mixing the silver nanowire water dispersion, anionic waterborne polyurethane, a foaming agent and a foam stabilizer to prepare a functional waterborne resin foaming agent;
and (2) placing the functional aqueous resin foaming agent on a carrier plate after foaming treatment until the foam is completely eliminated, and drying the functional aqueous resin foaming agent for 1.0 to 3.0 hours at the temperature of between 60 and 80 ℃ to obtain the silver nanowire/anionic aqueous polyurethane mixed conductive film.
Wherein the anionic waterborne polyurethane is carboxylic acid waterborne polyurethane, and the molecular weight range of the anionic waterborne polyurethane is 2W-5W.
Optionally, the functional aqueous resin foaming agent is foamed by using a foaming machine, and the silver nanowires can be uniformly distributed in the functional aqueous resin foaming agent through the foaming treatment, so that the silver nanowire/anionic aqueous polyurethane mixed conductive film prepared after drying has good conductive uniformity.
As an alternative embodiment, the method for preparing the aqueous dispersion of silver nanowires comprises the steps of:
providing a solution of sodium chloride in ethylene glycol;
providing a glycol solution of an organic protective agent;
providing a glycol solution of a silver precursor;
mixing a glycol solution of a silver precursor with a glycol solution of an organic protective agent to obtain a first mixed solution;
mixing a glycol solution of sodium chloride with the first mixed solution to prepare a second mixed solution;
reacting the second mixed solution at the temperature of 110-150 ℃ for 6-10 h to prepare a solid-liquid mixture, and separating the solid-liquid mixture to remove the upper solution to prepare the silver nanowires;
dispersing silver nanowires in deionized water to prepare a silver nanowire water dispersion;
the concentration of the silver nanowires in the silver nanowire water dispersion liquid is 1 g/L-10 g/L.
The preparation method of the silver nanowire has the characteristics of simplicity, mild reaction conditions, easiness in control and good repeatability, the silver nanowire is prepared by inducing the metal chloride, the average length of the prepared silver nanowire reaches more than 30 micrometers, even the silver nanowire with the length of about 120 micrometers can be prepared, and the prepared silver nanowire is controllable in length and uniform in size.
Further optionally, the mixing manner of the glycol solution of the silver precursor and the glycol solution of the organic protective agent is to drop the glycol solution of the silver precursor into the glycol solution of the organic protective agent; the mixing manner of the ethylene glycol solution of sodium chloride and the first mixed solution is to drop the ethylene glycol solution of sodium chloride into the first mixed solution.
Preferably, the molar concentration of the ethylene glycol solution of sodium chloride is 30 to 37.5. mu. mol/L.
Preferably, the mass concentration of the ethylene glycol solution of the organic protective agent is 2 g/L-10 g/L; the mass concentration of the glycol solution of the silver precursor is 2 g/L-10 g/L; preferably, the organic protective agent is polyvinylpyrrolidone.
Preferably, the mass ratio of the organic protective agent to the silver precursor in the first mixed solution is (1:3) to (3: 1).
Preferably, the volume ratio of the ethylene glycol solution of sodium chloride to the first mixed solution is 1: 100.
Preferably, the silver nanowires have an average length of 30 to 120 μm. More preferably, the silver nanowires have an average length of 80 to 120 μm.
In the preparation method of the silver nanowire/anionic waterborne polyurethane mixed conductive film as an optional embodiment, the concentration of the anionic waterborne polyurethane is 1 g/L-10 g/L; the dry weight ratio of the silver nanowires to the anionic waterborne polyurethane is (1:9) - (9: 1); preferably, the dry weight ratio of the silver nanowires to the anionic waterborne polyurethane is (1:9) - (3: 7); more preferably, the dry weight ratio of the silver nanowires to the anionic waterborne polyurethane is (1:9) - (2: 8).
Optionally, the foaming agent is any one or more of sodium dodecyl sulfate, lauryl betaine and dodecyl dimethyl benzyl ammonium chloride; the content of the foaming agent in the functional aqueous resin foaming agent is 0.1 g/L-1.0 g/L.
Optionally, the foam stabilizer is any one or more of sodium alginate, sodium carboxymethylcellulose, polyvinyl alcohol, agar and guar gum; the content of the foam stabilizer in the functional water-based resin foaming agent is 0.1-1.0 g/L.
Preferably, before the step of laminating the anionic waterborne polyurethane film on the flexible substrate layer by a hot pressing method, the method further comprises the following steps: and pretreating the flexible substrate layer by acetone.
Preferably, the acetone pretreatment is to place the flexible substrate layer in a Soxhlet extractor containing acetone, circularly reflux the flexible substrate layer for 2.0 to 3.0 hours at the temperature of between 60 and 70 ℃, take out the flexible substrate layer and dry the flexible substrate layer.
The silver nanowire/anion aqueous polyurethane mixed conductive film is combined with an anion aqueous polyurethane film of the flexible base material layer under the action of adhesive force through hot pressing, the flexible base material layer is pretreated through acetone, the adhesion amount of the silver nanowires on the surface of the flexible base material layer after hot pressing can be increased, so that the silver nanowire/anion aqueous polyurethane mixed conductive film forms a conductive layer on the surface of the flexible base material layer, the conduction of the flexible base material is facilitated, and the strain sensing capability of flexible collection is improved.
Preferably, the preparation method of the anionic aqueous polyurethane film comprises the following steps:
placing the anionic waterborne polyurethane with the concentration of 10 g/L-30 g/L on a carrier plate, and drying for 1.0-2.0 h at the temperature of 60-80 ℃ to obtain the anionic waterborne polyurethane film.
As an optional embodiment, in the step of laminating the anionic waterborne polyurethane film on the flexible substrate layer by a hot pressing method, the hot pressing temperature is 150-170 ℃, and the hot pressing time is 1.0-3.0 min;
in the step of laminating the silver nanowire/anionic waterborne polyurethane mixed conductive film on one side of the anionic waterborne polyurethane film of the flexible substrate layer by a hot pressing method, the hot pressing temperature is 70-100 ℃, and the hot pressing time is 1.0-2.0 min.
Example 1
1. Preparing a silver nanowire aqueous dispersion:
an ethylene glycol solution of sodium chloride having a molar concentration of 37.5. mu. mol/L, an ethylene glycol solution of polyvinylpyrrolidone having a mass concentration of 6g/L (average molecular weight of 1300000), and an ethylene glycol solution of silver nitrate having a mass concentration of 4g/L were prepared, respectively. 50mL of silver nitrate glycol solution is dripped into 50mL of ethylene glycol solution of vinyl pyrrolidone to prepare a first mixed solution, 1mL of sodium chloride glycol solution is dripped into the first mixed solution, and then the mixture reacts for 6 to 10 hours at the temperature of 130 ℃. And placing the solid-liquid mixture obtained after the reaction in a centrifuge, centrifuging for 5min at the rotating speed of 4000rpm, washing the solid with absolute ethyl alcohol for 2-3 times, removing the upper-layer liquid, dispersing the lower-layer precipitate, namely the silver nanowires in deionized water through ultrasonic dispersion for later use, and controlling the concentration of the silver nanowires to be 3 g/L. The detection shows that the yield of the prepared silver nanowires is 83.7%, the diameters of the prepared silver nanowires are uniform, the average length of the silver nanowires is 120 microns, and the proportion of the silver nanowires with the lengths of 115 microns-125 microns in the product is 97%.
2. Preparing a functional aqueous resin foaming agent:
and (2) mixing the silver nanowire dispersion liquid with anionic waterborne polyurethane with the concentration of 5g/L in proportion to ensure that the dry weight ratio of the silver nanowires to the anionic waterborne polyurethane is 0.2:9.8, and then adding a proper amount of foaming agent and foam stabilizer to uniformly mix to obtain the functional waterborne resin foaming agent.
3. Preparing a silver nanowire/anionic waterborne polyurethane mixed conductive film:
and (3) foaming the obtained functional aqueous resin foaming agent by using a foaming machine, placing the foaming agent in a polytetrafluoroethylene carrier plate, waiting for the elimination of foam until the foam is completely broken, and drying the polytetrafluoroethylene plate filled with the solution in an oven at the temperature of 70 ℃ for 2.0 h. Obtaining a silver nanowire/anionic waterborne polyurethane mixed conductive film;
4. preparing an anionic waterborne polyurethane film:
and (3) placing the anionic waterborne polyurethane with the concentration of 20g/L on a carrier plate, and drying for 1.5h at the temperature of 70 ℃ to obtain the anionic waterborne polyurethane film.
5. Preparing a flexible strain sensing material:
and hot-pressing the anionic waterborne polyurethane film on the elastic fabric pretreated by acetone at the temperature of 160 ℃ for 2.0 min. And hot-pressing the prepared silver nanowire/anionic waterborne polyurethane mixed conductive film on one side of the anionic waterborne polyurethane film of the elastic fabric at the hot-pressing temperature of 85 ℃ for 1.5min to finally prepare the flexible strain sensing material.
Wherein, this example needs to carry out acetone cleaning treatment to former fabric: putting the fabric into a Soxhlet extractor containing an acetone solution, heating to 65 ℃, carrying out reflux cleaning for 2.5 hours, and then transferring the fabric into a 60 ℃ drying oven for drying.
Example 2
The flexible strain sensing material of the present embodiment is the same as the preparation method of embodiment 1, except that the dry weight ratio of the silver nanowires to the anionic waterborne polyurethane in the functional waterborne resin foaming agent is silver nanowires: WPU is 0.5: 9.0.
Example 3
The flexible strain sensing material of the present embodiment is the same as the preparation method of embodiment 1, except that the dry weight ratio of the silver nanowires to the anionic waterborne polyurethane in the functional waterborne resin foaming agent is silver nanowire: WPU is 1.0: 9.0.
Example 4
The flexible strain sensing material of the present embodiment is the same as the preparation method of embodiment 1, except that the dry weight ratio of the silver nanowire to the anionic waterborne polyurethane in the functional waterborne resin foaming agent is silver nanowire: WPU is 2.0: 8.0.
As shown in fig. 1, the silver nanowire/anionic aqueous polyurethane mixed conductive films prepared in examples 1 to 4 have different ratios of silver nanowires to anionic aqueous polyurethane, and since the anionic aqueous polyurethane is an amorphous substance, the crystal form of the silver nanowire/anionic aqueous polyurethane mixture is not changed from that of the silver nanowire, and stronger diffraction peaks appear at 2 θ ═ 38.2 °, 44.38 °, 64.54 ° and 77.5 °.
As shown in fig. 2, it can be seen from the SEM micro-topography of the silver nanowire/anionic aqueous polyurethane mixed conductive film prepared in example 4 that the silver nanowires are embedded in the anionic aqueous polyurethane film under the adhesion of the anionic aqueous polyurethane, so that the anionic aqueous polyurethane film has conductivity to form a conductive film. And then, the silver nanowires are uniformly dispersed in the anionic aqueous polyurethane solution by adopting a foaming technology, so that the conductivity of the formed conductive film is more uniform.
As shown in fig. 3, the resistivity of the silver nanowire/anionic waterborne polyurethane mixed conductive film prepared in examples 1 to 4 was measured by a four-probe method to obtain a column trend graph of the change in the loading amount-resistivity of the silver nanowires in the silver nanowire/anionic waterborne polyurethane mixed conductive film, the resistivity was decreased with the increase in the proportion of the silver nanowires,when the loading amount of the silver nanowires is 20%, the minimum resistivity is measured to be 1.4x10 -5 Ω·m。
As shown in fig. 4, a fabric dynamic resistance tester is used to measure the real-time resistance value of the flexible strain sensing material prepared in embodiments 1 to 4 in the dynamic deformation process, so as to obtain a variation curve of the fabric resistance change rate along with the tensile strain, and as the proportion of the silver nanowires increases, the strain range of the flexible strain sensing material is larger, and the sensitivity is higher. The sensitivity value, i.e. the slope value of the curve, can reach up to 136 during the strain range of 60-70% extension. In addition, as can be seen from the figure, when the dry weight ratio of the silver nanowires to the anionic aqueous polyurethane in the functional aqueous resin foaming agent is silver nanowire: WPU is 2.0:8.0, the tensile degree of the flexible strain sensing material is 0 to 70%, and the resistance change value of the flexible strain sensing material has an exponential relationship with the tensile degree. The prepared flexible strain sensing material has the advantages that the bonding force between the conductive film and the elastic fabric is greatly enhanced due to the fact that the bonding film (the anionic waterborne polyurethane film) is thermally pressed on the elastic fabric substrate, and the resistance is not obviously changed when the flexible strain sensing material is repeatedly stretched for multiple times (more than 1000 times).
Example 5
1. Preparing a silver nanowire aqueous dispersion:
an ethylene glycol solution of sodium chloride having a molar concentration of 37.5. mu. mol/L, an ethylene glycol solution of polyvinylpyrrolidone having a mass concentration of 6g/L (average molecular weight of 1300000), and an ethylene glycol solution of silver nitrate having a mass concentration of 4g/L were prepared, respectively. 50mL of silver nitrate glycol solution is dripped into 50mL of ethylene glycol solution of vinyl pyrrolidone to prepare a first mixed solution, 1mL of sodium chloride glycol solution is dripped into the first mixed solution, and then the mixture reacts for 6 to 10 hours at the temperature of 140 ℃. And placing the solid-liquid mixture obtained after the reaction in a centrifuge, centrifuging for 5min at the rotating speed of 4000rpm, washing the solid with absolute ethyl alcohol for 2-3 times, removing the upper-layer liquid, dispersing the lower-layer precipitate, namely the silver nanowires in deionized water through ultrasonic dispersion for later use, and controlling the concentration of the silver nanowires to be 3 g/L. The detection shows that the yield of the prepared silver nanowires is 83.7%, the diameters of the prepared silver nanowires are uniform, the average length of the silver nanowires is 80 microns, and the proportion of the silver nanowires with the lengths of 75-85 microns in the product is 97%.
2. Preparing a functional aqueous resin foaming agent:
and (2) mixing the silver nanowire dispersion liquid with anionic waterborne polyurethane with the concentration of 5g/L in proportion to enable the dry weight ratio of the silver nanowires to the anionic waterborne polyurethane to be 0.2:9.8, and then adding a proper amount of foaming agent and foam stabilizer to be uniformly mixed to obtain the functional waterborne resin foaming agent.
3. Preparing a silver nanowire/anionic waterborne polyurethane mixed conductive film:
and (3) foaming the obtained functional aqueous resin foaming agent by using a foaming machine, placing the foaming agent in a polytetrafluoroethylene carrier plate, waiting for the elimination of foam until the foam is completely broken, and drying the polytetrafluoroethylene plate filled with the solution in an oven at the temperature of 70 ℃ for 2.0 h. Obtaining a silver nanowire/anionic waterborne polyurethane mixed conductive film;
4. preparing an anionic aqueous polyurethane film:
and (3) placing the anionic waterborne polyurethane with the concentration of 20g/L on a carrier plate, and drying for 1.5h at the temperature of 70 ℃ to obtain the anionic waterborne polyurethane film.
5. Preparing a flexible strain sensing material:
and (3) hot-pressing the anionic waterborne polyurethane film on the elastic fabric pretreated by acetone at the temperature of 160 ℃ for 2.0 min. And hot-pressing the prepared silver nanowire/anionic waterborne polyurethane mixed conductive film on one side of the anionic waterborne polyurethane film of the elastic fabric at the hot-pressing temperature of 85 ℃ for 1.5min to finally prepare the flexible strain sensing material.
Wherein, this example needs to carry out acetone cleaning treatment to former fabric: putting the fabric into a Soxhlet extractor containing an acetone solution, heating to 65 ℃, carrying out reflux cleaning for 2.5 hours, and then transferring the fabric into a 60 ℃ drying oven for drying.
Example 6
1. Preparing a silver nanowire water dispersion:
an ethylene glycol solution of sodium chloride having a molar concentration of 37.5. mu. mol/L, an ethylene glycol solution of polyvinylpyrrolidone having a mass concentration of 6g/L (average molecular weight of 1300000), and an ethylene glycol solution of silver nitrate having a mass concentration of 4g/L were prepared, respectively. 50mL of silver nitrate glycol solution is dripped into 50mL of ethylene glycol solution of vinyl pyrrolidone to prepare a first mixed solution, 1mL of sodium chloride glycol solution is dripped into the first mixed solution, and then the mixture reacts for 6 to 10 hours at the temperature of 150 ℃. And placing the solid-liquid mixture obtained after the reaction in a centrifuge, centrifuging for 5min at the rotating speed of 4000rpm, washing the solid with absolute ethyl alcohol for 2-3 times, removing the upper-layer liquid, dispersing the lower-layer precipitate, namely the silver nanowires in deionized water through ultrasonic dispersion for later use, and controlling the concentration of the silver nanowires to be 3 g/L. The detection shows that the yield of the prepared silver nanowires is 83.7%, the diameters of the prepared silver nanowires are uniform, the average length of the silver nanowires is 50 microns, and the proportion of the silver nanowires with the lengths of 35-55 microns in the product is 97%.
2. Preparing a functional aqueous resin foaming agent:
and (2) mixing the silver nanowire dispersion liquid with anionic waterborne polyurethane with the concentration of 5g/L in proportion to ensure that the dry weight ratio of the silver nanowires to the anionic waterborne polyurethane is 0.2:9.8, and then adding a proper amount of foaming agent and foam stabilizer to uniformly mix to obtain the functional waterborne resin foaming agent.
3. Preparing a silver nanowire/anionic waterborne polyurethane mixed conductive film:
and (3) foaming the obtained functional aqueous resin foaming agent by using a foaming machine, placing the foaming agent in a polytetrafluoroethylene carrier plate, waiting for the elimination of foam until the foam is completely broken, and drying the polytetrafluoroethylene plate filled with the solution in an oven at the temperature of 70 ℃ for 2.0 h. Obtaining a silver nanowire/anionic waterborne polyurethane mixed conductive film;
4. preparing an anionic aqueous polyurethane film:
and (3) placing the anionic waterborne polyurethane with the concentration of 20g/L on a carrier plate, and drying for 1.5h at the temperature of 70 ℃ to obtain the anionic waterborne polyurethane film.
5. Preparing a flexible strain sensing material:
and hot-pressing the anionic waterborne polyurethane film on the elastic fabric pretreated by acetone at the temperature of 160 ℃ for 2.0 min. And hot-pressing the prepared silver nanowire/anionic waterborne polyurethane mixed conductive film on one side of the anionic waterborne polyurethane film of the elastic fabric at the hot-pressing temperature of 85 ℃ for 1.5min to finally prepare the flexible strain sensing material.
Wherein, this example needs to carry out acetone cleaning treatment to former fabric: putting the fabric into a Soxhlet extractor containing an acetone solution, heating to 65 ℃, carrying out reflux cleaning for 2.5 hours, and then transferring the fabric into a 60 ℃ drying oven for drying.
Example 7
1. Preparing a silver nanowire aqueous dispersion:
an ethylene glycol solution of sodium chloride having a molar concentration of 37.5. mu. mol/L, an ethylene glycol solution of polyvinylpyrrolidone having a mass concentration of 6g/L (average molecular weight of 1300000), and an ethylene glycol solution of silver nitrate having a mass concentration of 4g/L were prepared, respectively. 50mL of silver nitrate glycol solution is dripped into 50mL of vinylpyrrolidone glycol solution to prepare a first mixed solution, 1mL of sodium chloride glycol solution is dripped into the first mixed solution, and then the mixture reacts for 6 to 10 hours at the temperature of 170 ℃. And placing the solid-liquid mixture obtained after the reaction in a centrifuge, centrifuging for 5min at the rotating speed of 4000rpm, washing the solid for 2-3 times by using absolute ethyl alcohol, removing the upper-layer liquid, dispersing the lower-layer precipitate, namely the silver nanowire in deionized water by using ultrasonic waves for later use, and controlling the concentration of the silver nanowire to be 3 g/L. The detection shows that the yield of the prepared silver nanowires is 83.7%, the diameters of the prepared silver nanowires are uniform, the average length of the silver nanowires is 40 micrometers, and the proportion of the silver nanowires with the lengths of 30 micrometers to 50 micrometers in the product is 97%.
2. Preparing a functional aqueous resin foaming agent:
and (2) mixing the silver nanowire dispersion liquid with anionic waterborne polyurethane with the concentration of 5g/L in proportion to enable the dry weight ratio of the silver nanowires to the anionic waterborne polyurethane to be 0.2:9.8, and then adding a proper amount of foaming agent and foam stabilizer to be uniformly mixed to obtain the functional waterborne resin foaming agent.
3. Preparing a silver nanowire/anionic waterborne polyurethane mixed conductive film:
and (3) foaming the obtained functional aqueous resin foaming agent by using a foaming machine, placing the foaming agent in a polytetrafluoroethylene carrier plate, waiting for the elimination of foam until the foam is completely broken, and drying the polytetrafluoroethylene plate filled with the solution in an oven at the temperature of 70 ℃ for 2.0 h. Obtaining a silver nanowire/anionic waterborne polyurethane mixed conductive film;
4. preparing an anionic aqueous polyurethane film:
and (2) placing the anionic waterborne polyurethane with the concentration of 20g/L on a carrier plate, and drying for 1.5h at the temperature of 70 ℃ to obtain the anionic waterborne polyurethane film.
5. Preparing a flexible strain sensing material:
and hot-pressing the anionic waterborne polyurethane film on the elastic fabric pretreated by acetone at the temperature of 160 ℃ for 2.0 min. And hot-pressing the prepared silver nanowire/anionic waterborne polyurethane mixed conductive film on one side of the anionic waterborne polyurethane film of the elastic fabric at the hot-pressing temperature of 85 ℃ for 1.5min to finally prepare the flexible strain sensing material.
Wherein, this example needs to carry out acetone cleaning treatment to former fabric: putting the fabric into a Soxhlet extractor containing an acetone solution, heating to 65 ℃, carrying out reflux cleaning for 2.5 hours, and then transferring the fabric into a 60 ℃ drying oven for drying.
The flexible strain sensor materials prepared in examples 4 to 7 were different in the average lengths of silver nanowires in the preparation of the functional aqueous resin foaming agent, which were 120 μm, 80 μm, 50 μm, and 40 μm, respectively.
The four-probe method was used to test the resistivity of the flexible strain sensing materials prepared in examples 4 to 7 before and after repeated stretching, and the measurement results are shown in table 1.
TABLE 1 resistivity of flexible strain sensing materials before and after repeated stretching
Example numbering Resistivity of flexible strain sensing material Resistivity after repeated stretching (1000 times)
Example 4 1.4x10 -5 (Ω·m) 4.2x10 -5 (Ω·m)
Example 5 1.9x10 -5 (Ω·m) 5.7x10 -5 (Ω·m)
Example 6 4.8x10 -5 (Ω·m) 1.4x10 -4 (Ω·m)
As can be seen from the test results of table 1, the longer the average length of the silver nanowires in the flexible strain sensing material is, the better the conductivity of the flexible strain sensing material is, and the better the durability is, the smaller the change in conductivity after repeated stretching is.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (8)

1. A preparation method of a flexible strain sensing material is characterized by comprising the following steps:
pressing the anionic waterborne polyurethane film on the flexible substrate layer by a hot pressing method;
pressing the silver nanowire/anionic waterborne polyurethane mixed conductive film on one side of the anionic waterborne polyurethane film of the flexible substrate layer by a hot pressing method;
the preparation method of the silver nanowire/anionic waterborne polyurethane mixed conductive film comprises the following steps:
mixing the silver nanowire water dispersion, anionic waterborne polyurethane, a foaming agent and a foam stabilizer to prepare a functional waterborne resin foaming agent;
and placing the functional aqueous resin foaming agent on a carrier plate after foaming treatment until the foam is completely eliminated, and drying the functional aqueous resin foaming agent for 1.0 to 3.0 hours at the temperature of between 60 and 80 ℃ to obtain the silver nanowire/anionic aqueous polyurethane mixed conductive film.
2. The method of preparing a flexible strain sensing material according to claim 1, wherein the method of preparing the aqueous dispersion of silver nanowires comprises the steps of:
providing a glycol solution of sodium chloride;
providing a glycol solution of an organic protectant;
providing a glycol solution of a silver precursor;
mixing the glycol solution of the silver precursor with the glycol solution of the organic protective agent to obtain a first mixed solution;
mixing the ethylene glycol solution of sodium chloride with the first mixed solution to prepare a second mixed solution;
reacting the second mixed solution at the temperature of 110-150 ℃ for 6-10 h to prepare a solid-liquid mixture, and separating the solid-liquid mixture to remove the upper solution to prepare the silver nanowires;
dispersing the silver nanowires in deionized water to prepare the silver nanowire water dispersion;
the concentration of the silver nanowires in the silver nanowire water dispersion liquid is 1 g/L-10 g/L.
3. The method for preparing a flexible strain sensing material according to claim 2, wherein the glycol solution of the silver precursor and the glycol solution of the organic protective agent are mixed in such a manner that the glycol solution of the silver precursor is added dropwise to the glycol solution of the organic protective agent; the mixing mode of the ethylene glycol solution of sodium chloride and the first mixed solution is to drop the ethylene glycol solution of sodium chloride into the first mixed solution.
4. The preparation method of the flexible strain sensing material according to claim 1, wherein in the preparation method of the silver nanowire/anionic waterborne polyurethane mixed conductive film, the concentration of the anionic waterborne polyurethane is 1 g/L-10 g/L; the dry weight ratio of the silver nanowires to the anionic waterborne polyurethane is (1:9) - (3: 7).
5. The method for preparing the flexible strain sensing material according to claim 1, wherein the foaming agent is any one or more of sodium dodecyl sulfate, lauryl betaine and dodecyl dimethyl benzyl ammonium chloride; the content of the foaming agent in the functional aqueous resin foaming agent is 0.1 g/L-1.0 g/L.
6. The preparation method of the flexible strain sensing material according to claim 1, wherein the foam stabilizer is any one or more of sodium alginate, sodium carboxymethylcellulose, polyvinyl alcohol, agar and guar gum; the content of the foam stabilizer in the functional aqueous resin foaming agent is 0.1-1.0 g/L.
7. The method of manufacturing a flexible strain sensing material according to any of claims 1 to 6,
in the step of laminating the anionic waterborne polyurethane film on the flexible substrate layer by a hot pressing method, the hot pressing temperature is 150-170 ℃, and the hot pressing time is 1.0-3.0 min;
and in the step of laminating the silver nanowire/anionic waterborne polyurethane mixed conductive film on one side of the anionic waterborne polyurethane film of the flexible substrate layer by a hot pressing method, the hot pressing temperature is 70-100 ℃, and the hot pressing time is 1.0-2.0 min.
8. A flexible strain sensing material, characterized in that the strain sensing material is prepared by the method for preparing a strain sensing material according to any one of claims 1 to 7.
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