CN112281491A - Preparation and application of plant fiber-based reinforced carbon fiber network - Google Patents

Preparation and application of plant fiber-based reinforced carbon fiber network Download PDF

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CN112281491A
CN112281491A CN202011192916.3A CN202011192916A CN112281491A CN 112281491 A CN112281491 A CN 112281491A CN 202011192916 A CN202011192916 A CN 202011192916A CN 112281491 A CN112281491 A CN 112281491A
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fiber network
carbon fiber
plant
plant fiber
network
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CN112281491B (en
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刘温霞
李程龙
李国栋
于得海
王慧丽
宋兆萍
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Qilu University of Technology
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/16Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01LMEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L1/00Measuring force or stress, in general
    • G01L1/18Measuring force or stress, in general using properties of piezo-resistive materials, i.e. materials of which the ohmic resistance varies according to changes in magnitude or direction of force applied to the material
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/40Fibres of carbon

Abstract

The invention provides a plant fiber reinforced carbon fiber network, and belongs to the technical field of flexible pressure sensors. Adding plant fibers into a periodic acid solution to form a paper pulp suspension, and heating to react to obtain a plant fiber network; calcining the dried plant fiber network and then taking out the calcined plant fiber network to obtain a carbon fiber network; and (3) immersing the carbon fiber network into a dopamine hydrochloride solution, reacting, washing and drying to obtain the plant fiber-based reinforced carbon fiber network. The plant fiber reinforced carbon fiber network prepared by the invention is applied to the flexible piezoresistive pressure sensor, greatly improves the compression strength of the carbon fiber network, and has the advantages of short response time, large response current, low detection limit, wide working range and good fatigue resistance stability.

Description

Preparation and application of plant fiber-based reinforced carbon fiber network
Technical Field
The invention relates to preparation of a plant fiber-based reinforced carbon fiber network and application of the plant fiber-based reinforced carbon fiber network as a piezoresistive pressure sensor, and belongs to the technical field of flexible pressure sensors.
Background
Flexible pressure sensors have gained increasing attention in the fields of wearable electronics, health monitoring, intelligent robots, and the like. Piezoresistive flexible pressure sensors that convert external pressure into resistance signals have been widely studied due to the advantages of simple structure, low manufacturing cost, high sensitivity, and convenient signal collection. Piezoresistive flexible pressure sensors are typically composed of a flexible sensing component, electrodes, and wires. The flexible sensing component is a key part of the flexible pressure sensor, and is generally made of flexible, deformable elastic conductive composite material or conductive aerogel or sponge with deformable porous structure. Carbon aerogel with a three-dimensional porous structure is becoming a sensing material with great application potential due to its low density, easy deformation, strong conductivity, good chemical and thermal stability.
Currently, the carbon aerogel is mostly prepared by using graphene/graphene oxide, carbon nanotubes and carbon fibers/carbon nanofibers as building units and by using a freeze drying technology or using polymer sponge as a template. Most of the polymer sponges used as templates are synthetic polymers, and the production process is not environment-friendly; and the graphene/graphene oxide and the carbon nano tube have complex production process, high cost and high price. The carbon fiber/carbon nanofiber can be prepared using a synthetic fiber precursor derived from fossil resources, and also using a fiber precursor derived from biomass resources. Based on the problems of non-regenerability of fossil resources, pollution in the production process and the like, the carbon aerogel prepared by utilizing plant raw materials such as plant fibers which are low in cost, rich in reserves, sustainable, renewable and good in environmental compatibility has more significance. However, cellulose fibers are highly hydrophilic and tend to shrink significantly during carbonization, resulting in carbon fibers that are highly brittle and have poor mechanical properties, making it difficult to form an ideal carbon aerogel material. The sulfonic acid (CN 104428243A) is used as a dehydrating agent to remove water from the cellulose fiber, or sodium periodate (CN 110714352A) is used to oxidize the cellulose fiber to introduce aldehyde groups on the surface of the fiber, so that the hydration degree of the cellulose fiber can be reduced, the cellulose fiber is prevented from being sintered in the carbonization process, the appearance of the cellulose fiber material is maintained, and the porous carbon fiber network material with a paper-like structure is prepared. However, the carbon fiber network material prepared by the methods has poor bonding force among carbon fibers, does not have enough mechanical strength to bear repeated compression deformation, and has poor fatigue resistance when being used as a sensing material of a piezoresistive pressure sensor.
Disclosure of Invention
Aiming at the defects of the prior art for preparing carbon aerogel and the defects of low mechanical strength and poor compression deformation stability of the carbon aerogel prepared by using plant fibers, the invention provides a method for preparing an enhanced carbon fiber network by properly improving the bonding strength between the carbon fibers in the carbon fiber network by using in-situ synthesized conductive polymer polydopamine on the basis of selectively oxidizing the plant fibers by using sodium periodate and freeze-drying to keep the appearance of the carbonized fiber network.
A preparation method of a plant fiber-based enhanced carbon fiber network comprises the steps of dispersing sodium periodate in deionized water to form a sodium periodate solution with the concentration of 5%, adding plant fibers to form a paper pulp suspension with the concentration of 5%, heating the suspension to 30-40 ℃, reacting for 2-3 hours, dehydrating, centrifugally washing by using deionized water, filtering, forming, and freeze-drying to obtain the plant fiber network.
And heating the dried plant fiber network to 300 ℃ at the speed of 2-3 ℃/min in a tubular furnace under the protection of nitrogen, preserving heat for 2 hours, continuously heating to 800 ℃ at the speed of 2-3 ℃/min, preserving heat for 3 hours, taking out, and cooling to room temperature to obtain the carbon fiber network.
Dissolving dopamine hydrochloride in 0.01 mol/L aqueous solution of Tris (hydroxymethyl) aminomethane (Tris buffer), preparing 0.2-0.4% dopamine hydrochloride solution, adjusting the pH of the dopamine hydrochloride solution to 8.5 by using NaOH solution, immersing the carbon fiber network in the dopamine hydrochloride solution, reacting for 24 hours, taking out, washing with deionized water, and drying to obtain the enhanced carbon fiber network.
The plant fiber of the invention refers to cellulose fiber extracted from plant fiber raw materials, such as softwood pulp, hardwood pulp or cotton pulp.
The selective oxidation of the plant fiber by using the sodium periodate means that the plant fiber C is oxidized by using the sodium periodate with the concentration of 5 percent at the temperature of 30-40 DEG C2And C3The selective oxidation of hydroxyl group aims at introducing aldehyde group on the surface of the fiber to reduce the hydration degree of the plant fiber, is beneficial to reducing the shrinkage of the plant fiber in the subsequent carbonization process, maintaining the structural morphology of the obtained carbon fiber and improving the yield of the carbon fiber.
The carbonization refers to that the oxidized plant fiber is filtered, formed, frozen and dried to prepare a plant fiber network, and the plant fiber network is pre-carbonized at 300 ℃ and carbonized at 800 ℃ in the atmosphere of nitrogen or other inert gases to obtain the carbon fiber network. The diameter of the carbon fiber in the network is 11-23 μm, and the length of the carbon fiber is more than 500 μm (figure 1).
The invention relates to a method for properly improving the bonding strength between carbon fibers in a carbon fiber network by utilizing a conductive polymer polydopamine synthesized in situ, which is characterized in that polydopamine formed by in-situ oxidative polymerization of dopamine hydrochloride at 30 ℃ under an alkaline condition is used as an adhesive to properly increase the bonding strength between the fibers in the carbon fiber network, so that a reinforced carbon fiber network is obtained. The polydopamine contains a large number of catechol structures, has good adhesion to various interfaces, and greatly improves the compression deformation stability of the carbon fiber network on the basis of completely maintaining the morphology of the carbon fiber network by using the polydopamine as an adhesive (figure 2).
The invention also comprises a method for preparing the piezoresistive pressure sensor by using the reinforced carbon fiber network as a sensing material and bonding the reinforced carbon fiber network with the electrode and the lead together (figure 3). Specifically, the method comprises the following steps: the reinforced carbon fiber network with certain size is clamped between two metal foils coated with conductive silver adhesive, and metal foil strips or metal wires are adhered to the metal foils by the conductive silver adhesive, so that the piezoresistive pressure sensor is formed.
The invention has the beneficial effects
The invention provides a method for preparing a plant fiber-based reinforced carbon fiber network. The carbon fiber network prepared by the method has the advantages that the compression strength of the carbon fiber network is greatly improved, the carbon fiber network is impacted and compressed for 1000 times, and the intact elasticity and the network appearance are still maintained. When the enhanced carbon fiber network prepared by the method is used as a sensing material and assembled into a piezoresistive pressure sensor, the piezoresistive pressure sensor has the advantages of short response time, large response current, low detection limit, wide working range and good fatigue resistance stability.
Drawings
FIG. 1 is an SEM image of a reinforced carbon fiber network;
FIG. 2 (a, b) morphology of carbon fiber network before (a) and after (b) 1000 impact compressions; (c, d) the appearance of the enhanced carbon fiber network before (c) and after (d) 1000 times of impact compression;
fig. 3 is a pressure sensor using an enhanced carbon fiber network as a sensing material.
Detailed description of the preferred embodiment
The present invention is further illustrated with reference to the following specific examples, which are carried out on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are provided, but the scope of the present invention is not limited to the following examples; unless otherwise indicated, the parts described in the examples are parts by mass.
Example 1
Shredding a commercial needle-leaved wood pulp board, soaking the needle-leaved wood pulp board in deionized water overnight, defibering the needle-leaved wood pulp board for 10000 revolutions by using a defibrator, dissolving 5 parts of sodium periodate in 95 parts of deionized water, and preparing 100 parts of sodium periodate solution; and (3) dispersing 5 parts of softwood pulp in 100 parts of sodium periodate solution, heating the dispersion system to 40 ℃ after uniform dispersion, reacting for 2 hours, dehydrating, centrifugally washing for 3 times by using deionized water, filtering, forming, and freeze-drying to obtain a cellulose fiber network with the thickness of about 5 mm. And (3) placing the dried cellulose fiber network in a tubular furnace, introducing nitrogen, purging the air in the furnace, heating to 300 ℃ at the speed of 2 ℃/min under the protection of the nitrogen, preserving the heat for 2 hours, continuously heating to 800 ℃ at the speed of 2 ℃/min, preserving the heat for 3 hours, taking out, and cooling to room temperature to obtain the carbon fiber network material with the thickness of about 2.5 mm. The carbon fiber material is immersed in an aqueous solution containing 0.01 mol/L of tris (hydroxymethyl) aminomethane and 0.3 wt% of dopamine hydrochloride, the pH value is adjusted to 8.5 by using NaOH solution, the oxidative polymerization of polydopamine is initiated, and after full reaction is carried out for 24 hours, the reinforced carbon fiber network material with the thickness of about 2.2 mm is obtained by washing 3 times by using deionized water, wherein the diameter of the carbon fiber is about 17-23 μm, and the length of the carbon fiber is more than 500 μm. The height loss after rebound is still less than 15% after 1000 times of impact compression.
Cutting the carbon fiber network material into 2 x 4 cm2The block is clamped between two tinfoils coated with conductive silver adhesive, and tinfoil strips are respectively adhered to the surfaces of the two tinfoils to be used as leads, so that the piezoresistive pressure sensor is formed. When the digital source meter of GiTIMER 2425 is switched on, the initial current is about 0.2 mA under the fixed voltage of 1V. Applying a pressure of about 20 Pa to the sensor and the current rapidly increasing to about 2.1 mA; the output current increases with increasing pressure, and reaches a maximum value of 70 mA when the applied pressure reaches about 100 KPa, indicating that the working range of the pressure sensor is very wide. The initial current and the output current are very stable when the pressure of 20 Pa is repeatedly applied to the sensor, and the output current and the initial current are still not obviously changed after the pressure is repeatedly compressed to 1000 times, which shows that the fatigue resistance stability of the sensing material of the pressure sensor is very good.
Example 2
Shredding a commercial needle-leaved wood pulp board, soaking the needle-leaved wood pulp board in deionized water overnight, defibering the needle-leaved wood pulp board for 10000 revolutions by using a defibrator, dissolving 5 parts of sodium periodate in 95 parts of deionized water, and preparing 100 parts of sodium periodate solution; and (3) dispersing 5 parts of softwood pulp in 100 parts of sodium periodate solution, heating the dispersion system to 30 ℃ after uniform dispersion, reacting for 3 hours, dehydrating, centrifugally washing for 3 times by using deionized water, filtering, forming, and freeze-drying to obtain a cellulose fiber network with the thickness of about 5 mm. And (3) placing the dried cellulose fiber network in a tubular furnace, introducing nitrogen, purging the air in the furnace, heating to 300 ℃ at the speed of 3 ℃/min under the protection of the nitrogen, preserving the heat for 2 hours, continuously heating to 800 ℃ at the speed of 3 ℃/min, preserving the heat for 3 hours, taking out, and cooling to room temperature to obtain the carbon fiber network material with the thickness of about 2.5 mm. The carbon fiber material is immersed in an aqueous solution containing 0.01 mol/L of tris (hydroxymethyl) aminomethane and 0.4 wt% of dopamine hydrochloride, the pH value is adjusted to 8.5 by using NaOH solution, the oxidative polymerization of polydopamine is initiated, the polydopamine is fully reacted for 24 hours, then the polydopamine is washed for 3 times by using deionized water, and the carbon fiber material with the thickness of about 2.0 mm is obtained after drying, wherein the diameter of the carbon fiber is about 17-23 mu m, and the length of the carbon fiber is more than 500 mu m. The height loss after rebound is still less than 15% after 1000 times of impact compression.
Cutting the carbon fiber network material into 2 x 4 cm2The block is clamped between two tinfoils coated with conductive silver adhesive, and tinfoil strips are respectively adhered to the surfaces of the two tinfoils to be used as leads, so that the piezoresistive pressure sensor is formed. When the digital source meter of GiTIMER 2425 is switched on, the initial current is about 0.22 mA under the fixed voltage of 1V. Applying a pressure of about 20 Pa to the sensor and the current rapidly increased to about 2.7 mA; the output current increases with continued pressure increase, and reaches a maximum of 74 mA at an applied pressure of about 100 KPa, indicating a very wide operating range for the pressure sensor. The initial current and the output current are very stable when the pressure of 20 Pa is repeatedly applied to the sensor, and the output current and the initial current are still not obviously changed after the pressure is repeatedly compressed to 1000 times, which shows that the fatigue resistance stability of the sensing material of the pressure sensor is very good.
Example 3
Shredding a commercial needle-leaved wood pulp board, soaking the needle-leaved wood pulp board in deionized water overnight, defibering the needle-leaved wood pulp board for 10000 revolutions by using a defibrator, dissolving 5 parts of sodium periodate in 95 parts of deionized water, and preparing 100 parts of sodium periodate solution; and (3) dispersing 5 parts of softwood pulp in 100 parts of sodium periodate solution, heating the dispersion system to 40 ℃ after uniform dispersion, reacting for 2 hours, dehydrating, centrifugally washing for 3 times by using deionized water, filtering, forming, and freeze-drying to obtain a cellulose fiber network with the thickness of about 5 mm. And (3) placing the dried cellulose fiber network in a tubular furnace, introducing nitrogen, purging the air in the furnace, heating to 300 ℃ at the speed of 2 ℃/min under the protection of the nitrogen, preserving the heat for 2 hours, continuously heating to 800 ℃ at the speed of 2 ℃/min, preserving the heat for 3 hours, taking out, and cooling to room temperature to obtain the carbon fiber network material with the thickness of about 2.5 mm. The carbon fiber material is immersed in an aqueous solution containing 0.01 mol/L of tris (hydroxymethyl) aminomethane and 0.2 wt% of dopamine hydrochloride, the pH value is adjusted to 8.5 by using NaOH solution, the oxidative polymerization of polydopamine is initiated, the polydopamine is fully reacted for 24 hours, then the polydopamine is washed for 3 times by using deionized water, and the carbon fiber material with the thickness of about 2.3 mm is obtained after drying, wherein the diameter of the carbon fiber is about 17-23 mu m, and the length of the carbon fiber is more than 500 mu m. The height loss after rebound is still less than 15% after 1000 times of impact compression.
Cutting the carbon fiber network material into 2 x 4 cm2The block is clamped between two tinfoils coated with conductive silver adhesive, and tinfoil strips are respectively adhered to the surfaces of the two tinfoils to be used as leads, so that the piezoresistive pressure sensor is formed. When the digital source meter of GiTIMER 2425 is switched on, the initial current is about 0.17 mA under the fixed voltage of 1V. Applying a pressure of about 20 Pa to the sensor and the current rapidly increased to about 1.9 mA; the output current increases with increasing pressure, and reaches a maximum value of 63 mA when the applied pressure reaches about 100 KPa, indicating that the working range of the pressure sensor is very wide. The initial current and the output current are very stable when the pressure of 20 Pa is repeatedly applied to the sensor, and the output current and the initial current are still not obviously changed after the pressure is repeatedly compressed to 1000 times, which shows that the fatigue resistance stability of the sensing material of the pressure sensor is very good.
Example 4
Soaking cotton pulp in deionized water overnight, defibering for 10000 revolutions by using a defibrator, and dissolving 5 parts of sodium periodate in 95 parts of deionized water to prepare 100 parts of sodium periodate solution; and 5 parts of cotton fiber pulp is dispersed in 100 parts of sodium periodate solution, after uniform dispersion, the dispersion system is heated to 30 ℃, reacted for 3 hours, dehydrated, centrifugally washed for 3 times by deionized water, filtered, formed and freeze-dried to obtain a cellulose fiber network with the thickness of about 5 mm. And (3) placing the dried cellulose fiber network in a tubular furnace, introducing nitrogen, purging the air in the furnace, heating to 300 ℃ at the speed of 3 ℃/min under the protection of the nitrogen, preserving the heat for 2 hours, continuously heating to 800 ℃ at the speed of 3 ℃/min, preserving the heat for 3 hours, taking out, and cooling to room temperature to obtain the carbon fiber network material with the thickness of about 2.6 mm. The carbon fiber material is immersed in an aqueous solution containing 0.01 mol/L of tris (hydroxymethyl) aminomethane and 0.3 wt% of dopamine hydrochloride, the pH value is adjusted to 8.5 by using NaOH solution, the oxidative polymerization of polydopamine is initiated, the polydopamine is fully reacted for 24 hours, then the polydopamine is washed for 3 times by using deionized water, and the carbon fiber material with the thickness of about 2.2 mm is obtained after drying, wherein the diameter of the carbon fiber is about 11-18 mu m, and the length of the carbon fiber is more than 500 mu m. The height loss after rebound is still less than 15% after 1000 times of impact compression.
Cutting the carbon fiber network material into 2 x 4 cm2The block is clamped between two tinfoils coated with conductive silver adhesive, and tinfoil strips are respectively adhered to the surfaces of the two tinfoils to be used as leads, so that the piezoresistive pressure sensor is formed. When the digital source meter of GiTIMER 2425 is switched on, the initial current is about 0.23 mA under the fixed voltage of 1V. Applying a pressure of about 20 Pa to the sensor and the current rapidly increasing to about 2.4 mA; the output current increases with increasing pressure, and reaches a maximum of about 80 mA when the applied pressure reaches about 100 KPa, indicating that the operating range of the pressure sensor is very wide. The initial current and the output current are very stable when the pressure of 20 Pa is repeatedly applied to the sensor, and the output current and the initial current are still not obviously changed after the pressure is repeatedly compressed to 1000 times, which shows that the fatigue resistance stability of the sensing material of the pressure sensor is very good.
Example 5
Shredding a commercial hardwood pulp board, soaking the hardwood pulp board in deionized water overnight, defibering the hardwood pulp board for 10000 revolutions by using a defibrator, and dissolving 5 parts of sodium periodate in 95 parts of deionized water to prepare 100 parts of sodium periodate solution; and (2) dispersing 5 parts of hardwood pulp in 100 parts of sodium periodate solution, heating the dispersion system to 40 ℃ after uniform dispersion, reacting for 2 hours, dehydrating, centrifugally washing for 3 times by using deionized water, filtering, forming, and freeze-drying to obtain a cellulose fiber network with the thickness of about 5 mm. And (3) placing the dried cellulose fiber network in a tubular furnace, introducing nitrogen, purging the air in the furnace, heating to 300 ℃ at the speed of 2 ℃/min under the protection of the nitrogen, preserving the heat for 2 hours, continuously heating to 800 ℃ at the speed of 2 ℃/min, preserving the heat for 3 hours, taking out, and cooling to room temperature to obtain the carbon fiber network material with the thickness of about 2.4 mm. The carbon fiber material is immersed in an aqueous solution containing 0.01 mol/L of tris (hydroxymethyl) aminomethane and 0.4 wt% of dopamine hydrochloride, the pH value is adjusted to 8.5 by using NaOH solution, the oxidative polymerization of polydopamine is initiated, the polydopamine is fully reacted for 24 hours, then the polydopamine is washed for 3 times by using deionized water, and the carbon fiber material with the thickness of about 2.0 mm is obtained after drying, wherein the diameter of the carbon fiber is about 13-21 mu m, and the length of the carbon fiber is more than 500 mu m. The height loss after rebound is still less than 15% after 1000 times of impact compression.
Cutting the carbon fiber network material into 2 x 4 cm2The block is clamped between two tinfoils coated with conductive silver adhesive, and tinfoil strips are respectively adhered to the surfaces of the two tinfoils to be used as leads, so that the piezoresistive pressure sensor is formed. When the digital source meter of GiTIMER 2425 is switched on, the initial current is about 0.21 mA under the fixed voltage of 1V. Applying a pressure of about 20 Pa to the sensor and the current rapidly increasing to about 2.4 mA; the output current increases with increasing pressure, and reaches a maximum of 68 mA when the applied pressure reaches about 100 KPa, indicating that the operating range of the pressure sensor is very wide. The initial current and the output current are very stable when the pressure of 20 Pa is repeatedly applied to the sensor, and the output current and the initial current are still not obviously changed after the pressure is repeatedly compressed to 1000 times, which shows that the fatigue resistance stability of the sensing material of the pressure sensor is very good.
Comparative example 1
The method comprises the following steps of shredding a commercial softwood pulp board, soaking the softwood pulp board in deionized water overnight, defibering the softwood pulp board by a defibering machine for 10000 revolutions, dispersing 10 parts of softwood pulp in 200 parts of deionized water, filtering, forming and freeze-drying the dispersed softwood pulp board after uniform dispersion to obtain a cellulose fiber network with the thickness of about 7 mm. And (3) placing the dried cellulose fiber network in a tubular furnace, introducing nitrogen, purging the air in the furnace, heating to 300 ℃ at the speed of 2 ℃/min under the protection of the nitrogen, preserving the heat for 2 hours, continuously heating to 800 ℃ at the speed of 2 ℃/min, preserving the heat for 3 hours, taking out, and cooling to room temperature to obtain the carbon fiber network material with the thickness of about 2.5 mm. Wherein the diameter of the carbon fiber is about 17-23 μm, and the length is more than 500 μm. The height loss after rebound already exceeded 30% after 300 impact compressions.
The carbon fiber network material is cut into a square of 2 x 4 cm2, and is clamped between two tinfoils coated with conductive silver adhesive, and then tinfoil strips are respectively adhered to the surfaces of the two tinfoils to be used as leads, so that the piezoresistive pressure sensor is formed. The initial current was about 0.1 mA at a fixed 1V voltage on a digital source meter. Applying a pressure of about 20 Pa to the sensor and the current rapidly increasing to about 0.7 mA; continuously increasing the pressure, increasing the output current, and when the applied pressure reaches about 30KPa, the output current reaches the maximum value of 15 mA; the output current does not increase any more as the pressure continues to increase. The pressure of 20 Pa is repeatedly applied to the sensor, the initial current is gradually increased, the output current is gradually reduced, and the difference between the output current and the initial current is reduced by nearly 25 percent after the sensor is repeatedly compressed to about 200 times, which indicates that the sensing material of the pressure sensor is seriously damaged.
Comparative example 2
Shredding a commercial needle-leaved wood pulp board, soaking the needle-leaved wood pulp board in deionized water overnight, defibering the needle-leaved wood pulp board for 10000 revolutions by using a defibrator, dissolving 5 parts of sodium periodate in 95 parts of deionized water, and preparing 100 parts of sodium periodate solution; and (3) dispersing 5 parts of softwood pulp in 100 parts of sodium periodate solution, heating the dispersion system to 40 ℃ after uniform dispersion, reacting for 2 hours, dehydrating, centrifugally washing for 3 times by using deionized water, filtering, forming, and freeze-drying to obtain a cellulose fiber network with the thickness of about 5 mm. And (3) placing the dried cellulose fiber network in a tubular furnace, introducing nitrogen, purging the air in the furnace, heating to 300 ℃ at the speed of 2 ℃/min under the protection of the nitrogen, preserving the heat for 2 hours, continuously heating to 800 ℃ at the speed of 2 ℃/min, preserving the heat for 3 hours, taking out, and cooling to room temperature to obtain the carbon fiber network material with the thickness of about 2.5 mm. Wherein the diameter of the carbon fiber is about 17-23 μm, and the length is more than 500 μm. The height loss after rebound already exceeded 15% after 300 impact compressions.
Cutting the carbon fiber network material into 2 x 4 cm2The block is clamped between two tinfoils coated with conductive silver adhesive, and tinfoil strips are respectively adhered to the surfaces of the two tinfoils to be used as leads, so that the piezoresistive pressure sensor is formed. The initial current was 0.14 mA at a fixed voltage of 1V on a digital source meter. Applying a pressure of about 20 Pa to the sensor and the current rapidly increasing to about 1.2 mA; continue to increaseUnder high pressure, the output current is increased, and when the applied pressure reaches about 60KPa, the output current reaches the maximum value of about 24 mA; the output current does not increase any more as the pressure continues to increase. The pressure of 20 Pa is repeatedly applied to the sensor, the initial current is gradually increased, the output current is gradually reduced, and the difference between the output current and the initial current is reduced by nearly 25 percent after the pressure is repeatedly compressed to about 470 times, which indicates that the sensing material of the pressure sensor is seriously damaged.

Claims (7)

1. A preparation method of a plant fiber-based reinforced carbon fiber network is characterized by comprising the following steps:
1) adding plant fibers into a periodic acid solution to form a paper pulp suspension, heating the suspension to 30-40 ℃, reacting for 2-3 hours, dehydrating, centrifugally washing by using deionized water, filtering, forming, and freeze-drying to obtain a plant fiber network;
2) calcining the dried plant fiber network, taking out, and cooling to room temperature to obtain a carbon fiber network;
3) soaking the carbon fiber network into a dopamine hydrochloride solution, reacting for 24h, taking out, washing with deionized water, and drying to obtain a plant fiber-based reinforced carbon fiber network;
the prepared plant fiber-based reinforced carbon fiber network is applied to serving as a sensing material.
2. The method according to claim 1, wherein the concentration of the sodium periodate solution in the step 1) is 5wt% and the concentration of the pulp suspension is 3 to 5%.
3. The preparation method according to claim 1, wherein in the step 2), the calcination adopts two-step calcination, specifically: and heating the cellulose fiber network to 300 ℃ at the speed of 2-3 ℃/min under the protection of nitrogen, preserving heat for 2 hours, continuously heating to 800 ℃ at the speed of 2-3 ℃/min, and preserving heat for 3 hours.
4. The preparation method according to claim 1, wherein in the step 3), the dopamine hydrochloride solution is prepared by the following method: dissolving dopamine hydrochloride in 0.01 mol/L aqueous solution of trihydroxymethyl aminomethane to prepare 0.2-0.4% dopamine hydrochloride solution, and adjusting the pH of the dopamine hydrochloride solution to 8.5 by using NaOH solution.
5. The method according to claim 1, wherein the plant fiber is cellulose fiber extracted from plant fiber material, such as softwood pulp, hardwood pulp or cotton pulp.
6. The method according to claim 1, wherein the sensing material is a sensing material of a pressure sensor.
7. Use according to claim 6, wherein the pressure sensor is a flexible piezoresistive pressure sensor.
CN202011192916.3A 2020-10-30 2020-10-30 Preparation and application of plant fiber-based reinforced carbon fiber network Active CN112281491B (en)

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