CN107389232B - Bio-based asymmetric flexible force-sensitive sensing material and preparation method thereof - Google Patents
Bio-based asymmetric flexible force-sensitive sensing material and preparation method thereof Download PDFInfo
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- CN107389232B CN107389232B CN201710450586.5A CN201710450586A CN107389232B CN 107389232 B CN107389232 B CN 107389232B CN 201710450586 A CN201710450586 A CN 201710450586A CN 107389232 B CN107389232 B CN 107389232B
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- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- G01L1/22—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges
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Abstract
The invention discloses a bio-based asymmetric flexible force-sensitive sensing material and a preparation method thereof, belonging to the field of preparation of advanced functional materials. The method comprises the following steps: (1) loading or assembling zero-dimensional, one-dimensional or two-dimensional conductive nano materials on the surface of the completely biodegradable fiber to prepare two pieces of conductive fiber cloth with different conductivities; (2) connecting a positive electrode and a negative electrode at two ends of the conductive fiber cloth with larger resistance; (3) and (3) attaching and packaging two pieces of conductive fiber cloth with different electric conductivities face to obtain the bio-based asymmetric flexible force-sensitive sensing material. The polymer framework material adopted by the invention is a completely biodegradable natural polymer material and has the characteristic of environmental friendliness; the sensitivity of the force-sensitive sensing material to pressure, bending deformation and distortion is superior to that of most piezoresistive flexible force-sensitive sensing materials reported at present, and the force-sensitive sensing material has super-strong stability, detection limit and excellent flexibility.
Description
Technical Field
The invention relates to the technical field of preparation of advanced functional materials, in particular to a bio-based asymmetric flexible force-sensitive sensing material and a preparation method thereof.
Background
With the rapid development of electronic technology, a flexible force-sensitive sensing material capable of meeting high performance of intelligent robots, electronic skins, wearable equipment and the like is urgently needed. The material can be attached to the surfaces of various irregular objects, can sense the acting force (compression, bending, stretching, distortion and the like) on the surface of the material, and converts external deformation signals into electric signals to realize the electronic functional material of force-sensitive sensing. The flexible conductive film is formed by compounding a high-molecular substrate (or called flexible substrate including rubber, plastic films, fiber fabrics and the like) with good flexibility and conductive elements (conductive fillers) in a certain mode, can be attached to various irregular surfaces, has the advantages of flexibility, compression, lightness, thinness, portability and the like, has wide application prospect in the fields of wearable equipment, intelligent robots, biomechanics, medical detection, flexible flat-panel displays and the like, and becomes a hotspot direction of current electronic material research.
In recent years, with the development of scientific technology, many sensing structures with high sensitivity, high stability, low detection limit and fast response have been designed and applied to flexible force-sensitive sensing materials. However, the flexible force-sensitive sensing materials are all designed symmetrically, that is, two completely consistent conductive surfaces with certain roughness are attached in a face-to-face mode, and the upper surface and the lower surface are respectively connected with electrodes and packaged; and the high molecular matrix used by the flexible force-sensitive sensing material is non-degradable thermosetting elastomers such as silicon rubber, natural rubber, styrene-butadiene rubber, cross-linked polyurethane and the like. As is well known, the update rate of current electronic products is very fast, and the non-biodegradable polymer matrix is obviously not suitable for the development trend of current electronic materials, so that there is a need to develop a flexible force-sensitive sensing material which has excellent sensing performance and can be biodegraded.
Disclosure of Invention
The invention aims to provide a flexible force-sensitive sensing material and a preparation method thereof, in particular to a bio-based asymmetric flexible force-sensitive sensing material and a preparation method thereof, which are beneficial to widening the research connotation and range of the current flexible force-sensitive sensing material.
The purpose of the invention is realized by the following technical scheme.
A preparation method of a bio-based asymmetric flexible force-sensitive sensing material comprises the following steps:
(1) loading or assembling zero-dimensional, one-dimensional or two-dimensional conductive nano materials on the surface of the completely biodegradable fiber to prepare two pieces of conductive fiber cloth with different conductivities;
(2) connecting a positive electrode and a negative electrode at two ends of the conductive fiber cloth with larger resistance;
(3) and (3) attaching and packaging two pieces of conductive fiber cloth with different electric conductivities face to obtain the bio-based asymmetric flexible force-sensitive sensing material.
Preferably, the fiber is a textile fiber obtained by spinning natural fibers or natural high molecular compounds of natural plants or animals from nature through chemical processing.
Preferably, the completely biodegradable natural fiber is natural plant or animal fiber derived from nature, and may be pure natural cotton fiber, hemp fiber, wool fiber, silk, spider silk, etc., or textile fiber obtained by spinning natural high molecular compounds such as cellulose, alginic acid, chitin, chitosan, starch, protein, etc. through chemical processing. The diameter of the single fiber is 100 nm-100 μm, and the length is 10 μm-5 cm.
Preferably, the thickness of the conductive fiber cloth is 1-400 μm.
Preferably, the zero-dimensional, one-dimensional or two-dimensional conductive nano material may be one or more of metal nanoparticles (such as silver nanoparticles, gold nanoparticles, copper nanoparticles, etc.), non-metal nanoparticles (such as acetylene black), metal nanowires (such as silver nanowires, gold nanowires, copper nanowires, etc.), carbon nanotubes, graphene, and doped metal oxides (such as aluminum-doped zinc oxide nanoparticles or nanowires).
Preferably, the conductive nanomaterial is supported and assembled on the surface of the fiber cloth by in-situ growth or by means of physical interaction (such as hydrogen bond, hydrophobic bond, etc.) to fix the conductive nanomaterial on the surface of the fiber.
Preferably, the diameter of the zero-dimensional conductive nano material is less than 100 nm, the length-diameter ratio of the one-dimensional nano material is 10-1000, the thickness of the two-dimensional nano material is 0.3-100 nm, and the sheet diameter is 100 nm-100 μm.
Preferably, the thickness of the conductive nano material on the surface of the fiber is 10 nm-10 μm, and the length and the width are both 1 cm-10 cm.
Preferably, the electrodes are metal electrodes such as copper electrodes, platinum electrodes, aluminum electrodes and the like, and the positive electrode and the negative electrode are fixed at two ends of the fiber cloth with larger resistance.
Preferably, the resistance ratio of the conductive fiber cloth with larger resistance to the fiber cloth with smaller resistance in the conductive fiber cloth is 1:1 to 50000: 1. The difference of the resistance values of the two pieces of conductive fiber cloth is the key for obtaining the high-sensitivity flexible force-sensitive sensing material, and on the premise of ensuring the conductive stability, the resistance ratio of the conductive fiber cloth with larger resistance to the fiber cloth with smaller resistance is larger (1), so that the higher the sensitivity of the obtained flexible force-sensitive sensing material is, the lower the detection limit is, and the faster the response time is.
Compared with the prior art, the invention has the following advantages:
1. the preparation method is simple and efficient, and has very wide application prospect.
2. The polymer framework material adopted by the invention is a completely biodegradable natural polymer material and has the characteristic of environmental friendliness;
3. the sensitivity of the force sensitive sensing material of the invention to pressure can reach 5-10 kPa-1The sensitivity to bending deformation can reach 0.5-2 Rad-1The sensitivity to distortion deformation can reach 0.05-0.1 degree, is superior to most of piezoresistive flexible force-sensitive sensing materials reported at present, and shows ultra-strong stability (>10000 cycles) and detection limit: (<5 mg) and excellent flexibility.
Drawings
FIG. 1 is a schematic structural diagram of a bio-based asymmetric flexible force-sensitive sensing material.
Detailed Description
The present invention will be described in more detail with reference to examples, but the present invention is not limited thereto.
The structure schematic diagram of the bio-based asymmetric flexible force-sensitive sensing material is shown in figure 1, and the material comprises an electrode 1, an encapsulating material 2, a small-resistance conductive fiber cloth 3 and a large-resistance conductive fiber cloth 4, wherein two ends of the large-resistance conductive fiber cloth are connected with the electrode, the small-resistance conductive fiber cloth is attached to the large-resistance conductive fiber cloth in a face-to-face mode, and the electrode, the small-resistance conductive fiber cloth and the large-resistance conductive fiber cloth are encapsulated through the encapsulating material.
Example 1
Soaking cotton fiber cloth with size of 1cm × 4cm × 1 μm in 3mg/ml graphene oxide water solution for 2min, drying at 80 deg.C for 30min to make the surface of the cotton fiber cloth coated with graphene oxide with thickness of 20 nm, and then at 80 deg.C, at concentration of 5mg/cm3Reducing the obtained product for 1h in hydrazine hydrate steam to obtain graphene-loaded cotton fiber cloth with the resistance of 5000 omega, and connecting copper electrodes at two ends of the cotton fiber cloth; soaking cotton fiber cloth with the size of 1cm multiplied by 4cm multiplied by 1 mu m in 3mg/ml absolute ethanol solution of gold nanowires for 2min, taking out, drying at 60 ℃ for 20min, assembling the gold nanowires with the thickness of 500 nm on the surface of the cotton fiber cloth, and obtaining the cotton fiber cloth loaded with the gold nanowires with the resistance of 0.1 omega; and then attaching the cotton fiber cloth loaded with the gold nanowires to the cotton fiber cloth loaded with the graphene, and packaging by using a 3M adhesive tape as a packaging material to obtain the flexible force-sensitive sensing material.
The sensitivity of the flexible force-sensitive sensing material prepared by the embodiment to pressure is 10 kPa-1Sensitivity to bending deformation of 1.1 Rad-1The sensitivity to distortion deformation is 0.09 degree per degree, which is superior to most of piezoresistive flexible force-sensitive sensing materials reported at present, and the piezoresistive flexible force-sensitive sensing material shows super stability (>10000 cycles) and detection limit: (<5 mg) and excellent flexibility.
Example 2
Soaking fibroin fiber cloth with the size of 1cm multiplied by 4cm multiplied by 400 mu m in a carbon nano tube aqueous solution with the size of 3mg/ml for 2min, taking out, drying at 80 ℃ for 30min, assembling industrial carbon nano tubes with the thickness of 100 nm on the surface of the fibroin fiber cloth to obtain carbon nano tube loaded fiber cloth with the resistance of 1500 omega, and connecting aluminum electrodes at two ends of the carbon nano tube loaded fiber cloth; soaking fibroin fiber cloth with size of 2 cm × 3 cm × 400 μm in water solution containing 20wt% silver nitrate and 5wt% PVP for 2min, taking out, and concentrating at 5mg/cm at 80 deg.C3Reducing in situ in hydrazine hydrate steam for 30min, thereby loading a layer of silver nanoparticles with the thickness of 400 nm on the surface of the fibroin fiber cloth, and obtaining the silver nanoparticle loaded fiber cloth with the resistance of 5 omega; then attaching the fiber cloth loaded with the silver nano particles on the fiber cloth loaded with the carbon nano tubes, and adopting a 3M adhesive tape as an encapsulating material for encapsulating to obtain the silver nano particle-loaded fiber clothTo flexible force sensitive sensing materials.
The sensitivity of the flexible force-sensitive sensing material prepared in the embodiment to pressure is 5 kPa-1Sensitivity to bending deformation of 0.8 Rad-1The sensitivity to distortion deformation is 0.06 degree, which is superior to most of piezoresistive flexible force-sensitive sensing materials reported at present, and the piezoresistive flexible force-sensitive sensing material has super stability (>10000 cycles) and detection limit: (<5 mg) and excellent flexibility.
Example 3
Soaking wool fiber cloth with the size of 1cm multiplied by 4cm multiplied by 200 mu m in a carbon nano tube aqueous solution of 3mg/ml for 2min, taking out, drying at 80 ℃ for 30min, assembling industrial-grade acetylene black with the thickness of 500 nm on the surface of the fiber cloth to obtain the acetylene black loaded wool fiber cloth with the resistance of 2000 omega, and connecting copper electrodes at two ends of the wool fiber cloth; soaking wool fiber cloth with size of 3 cm × 3 cm × 200 μm in aqueous solution containing 20wt% copper chloride and 5wt% PVP for 1min, taking out, and concentrating at 5mg/cm at 80 deg.C3Reducing in situ for 30min in hydrazine hydrate steam, thereby loading a layer of copper nanoparticles with the thickness of 1 mu m on the surface of the wool fiber cloth to obtain the wool fiber cloth loaded with the copper nanoparticles with the resistance of 10 omega; and then attaching the wool fiber cloth loaded with the copper nanoparticles to the wool fiber cloth loaded with the acetylene black, and packaging by using a 3M adhesive tape as a packaging material to obtain the flexible force-sensitive sensing material.
The sensitivity of the flexible force-sensitive sensing material prepared in the embodiment to pressure is 5 kPa-1Sensitivity to bending deformation of 0.6 Rad-1The sensitivity to distortion deformation is 0.09 degree per degree, which is superior to most of piezoresistive flexible force-sensitive sensing materials reported at present, and the piezoresistive flexible force-sensitive sensing material shows super stability (>10000 cycles) and detection limit: (<5 mg) and excellent flexibility.
Example 4
Soaking cotton fiber cloth with size of 1cm × 4cm × 100 μm in graphene oxide water solution of 3mg/ml for 2min, taking out, drying at 80 deg.C for 30min to make the surface of the fiber cloth be coated with graphene oxide with thickness of 20 nm, and coating the surface of the fiber cloth with graphene oxide of 5mg/cm3Reducing in hydrazine hydrate steam with concentration for 1h to obtain electricityThe conductive sodium alginate fiber cloth with the resistance of 1000 omega is connected with copper electrodes at two ends; soaking sodium alginate fiber cloth with size of 4cm × 4cm × 100 μm in water solution containing 20wt% silver nitrate and 5wt% PVP for 2min, taking out, and concentrating at 5mg/cm at 80 deg.C3Reducing in situ in hydrazine hydrate steam for 30min, thereby loading a layer of silver nano particles with the thickness of 400 nm on the surface of the sodium alginate fiber cloth, and obtaining the sodium alginate fiber cloth loaded with the silver nano particles and with the resistance of 10 omega; and then attaching the sodium alginate fiber cloth loaded with the silver nanoparticles to the conductive sodium alginate fiber cloth loaded with the graphene, and packaging by using a 3M adhesive tape as a packaging material to obtain the flexible force-sensitive sensing material.
The sensitivity of the flexible force-sensitive sensing material prepared by the embodiment to pressure is 8 kPa-1Sensitivity to bending deformation of 0.7 Rad-1The sensitivity to distortion deformation is 0.1 degree, is superior to most of piezoresistive flexible force-sensitive sensing materials reported at present, and shows ultra-strong stability (>10000 cycles) and detection limit: (<5 mg) and excellent flexibility.
Claims (7)
1. A preparation method of a bio-based asymmetric flexible force-sensitive sensing material is characterized by comprising the following steps:
(1) loading or assembling zero-dimensional, one-dimensional or two-dimensional conductive nano materials on the surface of the completely biodegradable fiber to prepare two pieces of conductive fiber cloth with different conductivities, namely fixing the conductive nano materials on the surface of the fiber by an in-situ growth or physical interaction method; the fiber is a textile fiber prepared by chemical processing and spinning of natural fibers or natural high molecular compounds of natural plants or animals from nature; the diameter of a single fiber in the fiber is 100 nm-100 mu m, and the length of the single fiber is 10 mu m-5 cm; the thickness of the conductive nano material on the surface of the fiber is 10 nm-10 mu m, and the length and the width of the conductive nano material are both 1 cm-10 cm; the thickness of the conductive fiber cloth is 1-400 μm;
(2) connecting the positive electrode and the negative electrode at two ends of the conductive fiber cloth with larger resistance;
(3) and (3) attaching and packaging two pieces of conductive fiber cloth with different electric conductivities face to obtain the bio-based asymmetric flexible force-sensitive sensing material.
2. The method for preparing a bio-based asymmetric flexible force-sensitive sensing material according to claim 1, wherein the natural fiber is cotton fiber, hemp fiber, wool fiber, silk or spider silk; the natural polymer compound is cellulose, alginic acid, chitin, chitosan, starch or protein.
3. The method for preparing a bio-based asymmetric flexible force-sensitive sensing material according to claim 1, wherein the zero-dimensional, one-dimensional or two-dimensional conductive nano material in step (1) is one or more of silver nano particles, gold nano particles, copper nano particles, acetylene black, silver nano wires, gold nano wires, copper nano wires, carbon nano tubes, graphene, aluminum-doped zinc oxide nano particles or nano wires.
4. The method for preparing a bio-based asymmetric flexible force-sensitive sensing material according to claim 1, wherein the diameter of the zero-dimensional conductive nano material in step (1) is less than 100 nm; the length-diameter ratio of the one-dimensional conductive nano material is 10-1000; the thickness of the two-dimensional conductive nano material is 0.3-100 nm, and the sheet diameter is 100 nm-100 μm.
5. The method for preparing a bio-based asymmetric flexible force sensing material according to claim 1, wherein the electrode in step (2) is a copper electrode, a platinum electrode or an aluminum electrode.
6. The method for preparing a bio-based asymmetric flexible force-sensitive sensing material according to claim 1, wherein the resistance ratio of the conductive fiber cloth with higher resistance to the fiber cloth with lower resistance in the conductive fiber cloth of step (3) is 1:1-50000: 1.
7. A bio-based asymmetric flexible force sensitive sensing material made by the method of any of claims 1-6.
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