CN111040238B - Aramid nanofiber/MXene composite conductive aerogel and preparation method thereof - Google Patents

Aramid nanofiber/MXene composite conductive aerogel and preparation method thereof Download PDF

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CN111040238B
CN111040238B CN201911360559.4A CN201911360559A CN111040238B CN 111040238 B CN111040238 B CN 111040238B CN 201911360559 A CN201911360559 A CN 201911360559A CN 111040238 B CN111040238 B CN 111040238B
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CN111040238A (en
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杨斌
王琳
张美云
谭蕉君
宋顺喜
丁雪瑶
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Shaanxi University of Science and Technology
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Abstract

The invention discloses an aramid nano-fiber/MXene composite conductive aerogel and a preparation method thereof. The preparation method specifically comprises the steps of preparing an aramid nano fiber dispersion liquid, preparing an MXene dispersion liquid, preparing an aramid nano fiber/MXene composite dispersion liquid, preparing a gel-like aramid nano fiber/MXene composite material and the like, so that the aramid nano fiber/MXene composite conductive aerogel is obtained. The preparation process is simple and feasible, and the obtained aramid nanofiber/MXene composite conductive aerogel has wide application prospects in the fields of pressure sensing, intelligent sensors, wearable equipment and the like.

Description

Aramid nanofiber/MXene composite conductive aerogel and preparation method thereof
Technical Field
The invention belongs to the field of polymer nano materials and strain sensors, and particularly relates to an aramid nano fiber/MXene composite conductive aerogel and a preparation method thereof.
Background
The aerogel has the characteristics of high porosity, low density, controllable three-dimensional porous structure and the like, so that the aerogel has wide application prospects in the fields of adsorption, heat insulation, energy storage and the like. The conductive aerogel not only has the advantages of the aerogel, but also has great application potential in the fields of fuel cells, catalysis, supercapacitors, sensors, wearable equipment and the like due to excellent conductive performance. At present, most of conventional conductive aerogels are carbon-based aerogels obtained through high-temperature (>1000 ℃) pyrolysis, and although the carbon-based aerogels show excellent conductivity, the conventional conductive aerogels cannot be produced in batches due to the fact that harsh conditions such as high temperature, high pressure or strict oxygen-free conditions are required in the preparation process. In addition, conventional carbon-based aerogels tend to exhibit lower mechanical properties, greater brittleness, and poorer compression resilience due to high temperature pyrolysis treatment. Therefore, when the conventional carbon-based aerogel is applied to a sensor, the high sensitivity, the fast response performance, the long cycle time and the long service life are difficult to show, and the application requirements of the pressure sensor cannot be met. Aramid nano-fibers (ANFs) have unique nanoscale structures (the diameter is 3-30nm, the length can reach 10 mu m at most), large length-diameter ratio and specific surface area, and simultaneously retain excellent mechanical properties and temperature resistance of the Aramid fibers, so that the Aramid nano-fibers become a novel 'construction unit' with great potential for constructing macroscopic composite materials. The Chinese patent with application number 201710263470.0 discloses a preparation method of aramid nanofiber aerogel, the aramid nanofiber aerogel is obtained by the steps of extraction, preparation of aramid nanofiber dispersion liquid, preparation of aramid nanofiber hydrogel, vacuum filtration, freeze drying and the like, the initial decomposition temperature of the aerogel is 500 ℃, the aerogel has high heat resistance, the problem that the existing aerogel is poor in heat resistance can be solved, and the aramid nanofiber aerogel cannot conduct electricity due to the high insulation property of the fiber itself. Therefore, Ren Guangyuan et al reported that a nitrogen-doped carbon nanofiber aerogel is obtained by pyrolyzing aramid nanofibers at 1000 ℃ for 3 hours in a nitrogen atmosphere, and is expected to be applied to the fields of fuel cells or metal-air cells (Guangyuan Ren, et al, Journal of electrochemical Chemistry,2018,829: 177-183). However, the carbon nanofiber aerogel prepared by the method has lower strength and poorer compression resilience due to pyrolysis treatment at high temperature. In conclusion, simultaneously, due to the high pore structure of the aramid nanofiber aerogel, strong hydrogen bond acting force between fibers is weakened, the mechanical property and compression resilience of the aerogel are reduced, and the application of the aramid nanofiber aerogel in the field of pressure-sensitive sensors is limited to a great extent. In summary, no public reports on the preparation of the conductive aramid nanofiber aerogel and the application of the conductive aramid nanofiber aerogel in the field of sensors are found at present.
Disclosure of Invention
The invention aims to provide the aramid fiber nanofiber/MXene composite conductive aerogel and the preparation method thereof, so as to solve the problems that the existing aramid fiber nanofiber aerogel does not have conductivity and is poor in compression resilience and cannot be applied to the fields of pressure sensors and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
the aramid nano-fiber/MXene composite conductive aerogel is composed of aramid nano-fiber and MXene, and the mass ratio of the aramid nano-fiber to the MXene is (40-80) to (60-20); the density of the aramid nano fiber/MXene composite conductive aerogel is 20-40 mg/cm 3 。
A preparation method of aramid nanofiber/MXene composite conductive aerogel comprises the following steps:
the method comprises the following steps: preparing an aramid nanofiber dispersion liquid: mixing and sealing the aramid chopped fibers, potassium hydroxide, dimethyl sulfoxide and deionized water, and stirring at the rotating speed of 1200-1500 r/min for reaction for 2-4 h to obtain an aramid nanofiber dispersion liquid dispersed in the dimethyl sulfoxide;
step two: preparing MXene dispersion liquid: adding MAX raw materials and LiF into HCL solution, stirring at constant temperature to obtain MXene materials, washing with deionized water to neutrality, and dispersing in deionized water to obtain MXene dispersion liquid;
step three: preparing an aramid nano fiber/MXene composite dispersion liquid: injecting the MXene dispersion liquid obtained in the step two into the aramid nano-fiber dispersion liquid obtained in the step one under the stirring action of the stirring speed of 1500-2500 r/min to obtain an aramid nano-fiber/MXene composite dispersion liquid;
step four: preparing a gel-like aramid nanofiber/MXene composite material: preparing the gel-like aramid nano fiber/MXene composite material by carrying out vacuum filtration on the aramid nano fiber/MXene composite dispersion liquid obtained in the step three;
step five: preparing the aramid nano fiber/MXene composite conductive aerogel: and D, freezing the gel-like aramid nano-fiber/MXene composite material obtained in the fourth step, and then freezing and drying the frozen material to obtain the aramid nano-fiber/MXene composite conductive aerogel.
Further, in the first step, the proportion of the aramid chopped fibers, potassium hydroxide and dimethyl sulfoxide is 1 g: 1.5 g: 500mL, wherein the volume ratio of the deionized water to the dimethyl sulfoxide is 1: 50-1: 15.
Further, the aramid chopped fibers, the deionized water, the dimethyl sulfoxide and the potassium hydroxide are added in the following sequence: firstly adding potassium hydroxide and then adding deionized water, mixing and stirring for 5-20 min, and then sequentially adding aramid chopped fibers and dimethyl sulfoxide.
Further, the length of the aramid chopped fiber in the step one is 6 mm; the mass concentration of the obtained aramid nano-fiber dispersion liquid dispersed in dimethyl sulfoxide is 0.2%, wherein the diameter of the aramid nano-fiber is 12-15 nm, and the length of the aramid nano-fiber is 4-7 mu m.
Further, in the second step, the concentration of the HCL solution is 9mol/L, and the MAX raw material is Ti 3 AlC 2 And Ti 3 AlC 2 : the mass ratio of LiF is 1:1.6, and the mass concentration of the obtained MXene dispersion liquid is 1.0%.
Further, in the second step, the constant-temperature stirring temperature is 35 ℃, and the time is 35 hours.
Furthermore, the mass ratio of the aramid nano-fiber to the MXene in the third step is (40-80): 60-20.
Further, in the fourth step, the vacuum filtration time is 2-4 hours, and the water content of the obtained gel-like aramid nano fiber/MXene composite material is controlled to be 20-60%.
And further, placing the gel-like aramid fiber/MXene composite material obtained in the fourth step into an aluminum box, placing the aluminum box into a container filled with liquid nitrogen, freezing for 10-30 min, enabling the bottom of the aluminum box to be in contact with the upper plane of the liquid nitrogen when the liquid nitrogen is frozen, and then placing the frozen material into a freeze dryer for drying to obtain the aramid fiber/MXene composite conductive aerogel.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the aramid nanofiber/MXene composite conductive aerogel and the preparation method thereof, the aramid nanofiber/MXene composite conductive aerogel with low density, high strength and high compression elasticity is prepared by using the aramid nanofiber with a nanoscale structure, high strength, large length-diameter ratio and high temperature resistance as a matrix and using the MXene with excellent conductivity, good chemical stability and unique two-dimensional nano film structure as a conductive and filling coating material. The problems that the conventional aramid nanofiber aerogel is non-conductive, poor in compression resilience performance and low in strength, cannot be applied to the fields of pressure sensors and the like are solved, the preparation process is simple and feasible, and the application prospect in the fields of pressure sensors, intelligent sensors, wearable equipment and the like is wide.
According to the aramid nano-fiber/MXene composite conductive aerogel and the preparation method thereof, when the aramid nano-fiber dispersion liquid is prepared, deionized water with different proportions is added and the adding sequence of the components is regulated, so that the effective alkali concentration in the system can be improved, the reaction time of the aramid nano-fiber is effectively reduced, and the preparation efficiency is improved; when the aramid nano fiber/MXene composite dispersion liquid is prepared, the problem of flocculation caused by rapid protonation reduction of the aramid nano fiber can be avoided by a high-pressure injection mode of an injector, meanwhile, the aramid nano fiber serves as a MXene dispersing agent due to the rigid structure of the aramid nano fiber, the aramid nano fiber and the MXene can be stably dispersed under the action of electrostatic repulsion, and the aramid nano fiber/MXene composite dispersion liquid with an excellent dispersing effect is obtained; when the gel-like aramid nano fiber/MXene composite material is prepared, a tight coating structure is formed between the aramid nano fiber with large length-diameter ratio and the two-dimensional MXene with nanoscale by controlling the vacuum filtration time and the water content of the gel-like aramid nano fiber/MXene composite material, the aramid nano fiber/MXene composite fiber is formed, the composite fibers are tightly combined through strong intermolecular hydrogen bond acting force, the oriented distribution of the aramid nano fiber/MXene composite fiber is realized in the vacuum filtration process, the aramid nano fiber/MXene composite conductive aerogel has an obvious layered structure in the Z direction, the layered structure ensures that the aerogel exerts good strength performance of the aramid nano fiber, and when the material is compressed by external force, the multi-layered structure and the porous structure can well bear out-of-plane deformation through reversible deformation, endows the aramid nano fiber/MXene composite conductive aerogel with high strength, high compression modulus and excellent compression resilience; meanwhile, the excellent strength and compression resilience can ensure that the composite aerogel rapidly passes through the change of current signal feedback stress when being subjected to external pressure, so that the aramid nano-fiber/MXene composite conductive aerogel is endowed with high sensitivity.
According to the aramid nano-fiber/MXene composite conductive aerogel and the preparation method thereof, the components of the aramid nano-fiber and MXene have excellent temperature resistance, so that the composite aerogel is endowed with excellent heat resistance and thermal stability, and is expected to be applied to a sensor in a high-temperature environment, and the service life of the sensor is prolonged.
The aramid nano-fiber/MXene composite conductive aerogel and the preparation method thereof have the characteristics of low density, high mechanical strength, excellent compression resilience, good temperature resistance, high sensitivity, long cycle stability, long service life and the like, are expected to be applied to the fields of pressure sensors, human motion monitoring, wearable equipment and the like, expand the application fields of traditional single aramid nano-fiber and MXene, and realize diversified application and development of the aramid nano-fiber/MXene composite conductive aerogel.
Drawings
Fig. 1 is a Z-direction surface SEM image of the aramid nanofiber/MXene composite conductive aerogel obtained in example 3 of the present invention;
fig. 2 is a Z-direction cross-section SEM image of the aramid nanofiber/MXene composite conductive aerogel obtained in example 3 of the present invention;
fig. 3 is a compression curve of the aramid nanofiber/MXene composite conductive aerogel obtained in example 3 of the present invention;
fig. 4 is a thermogravimetric curve of the aramid nanofiber/MXene composite conductive aerogel obtained in embodiment 3 of the present invention in a nitrogen atmosphere;
fig. 5 is a current-time response curve of the aramid nanofiber/MXene composite conductive aerogel obtained in example 3 of the present invention when a pressure of 0.5kPa is applied thereto.
Detailed Description
Embodiments of the invention are described in further detail below:
the aramid fiber nanofiber/MXene composite conductive aerogel comprises aramid fiber nanofibers and MXene, wherein the mass ratio of the aramid fiber nanofibers to the MXene is (40-80) to (60-20); the mass of the aramid nano-fiber/MXene composite conductive aerogel is 200-600 mg, and the density is 20-40 mg/cm 3 。
A preparation method of aramid nanofiber/MXene composite conductive aerogel comprises the following steps:
the method comprises the following steps: preparing an aramid nano-fiber dispersion liquid, namely preparing 1g of aramid chopped fibers with the length of 6mm, 1.5g of potassium hydroxide, 500ml of dimethyl sulfoxide and a certain amount of deionized water, wherein the volume ratio of the deionized water to the dimethyl sulfoxide is (1: 50-1: 15); firstly adding potassium hydroxide, then adding deionized water, mixing and stirring for 5-20 min by using a magnetic stirrer, then sequentially adding aramid chopped fibers and dimethyl sulfoxide, placing the mixture into a sealed beaker, and stirring and reacting for 2-4 h at the rotating speed of 1200-1500 r/min by using the magnetic stirrer to obtain an aramid nano-fiber dispersion liquid with the mass concentration of 0.2% dispersed in the dimethyl sulfoxide, wherein the diameter of the aramid nano-fiber is 12-15 nm, and the length of the aramid nano-fiber is 4-7 mu m;
step two: preparation of MXene dispersion: 100ml of 9mol/L HCl solution is taken in a plastic container, 6.4g of LiF is slowly added,after stirring at 35 ℃ for 30min, 4g of MAX raw material (Ti) was slowly added 3 AlC 2 ) Continuously stirring the mixed solution at constant temperature (35 ℃) for 35 hours, controlling the rotating speed to be 3500r/min, centrifugally washing the mixed solution by deionized water until the pH value is 5, and dispersing the obtained sample in the deionized water to obtain MXene dispersion liquid with the mass concentration of 1.0%;
step three: preparing an aramid nano fiber/MXene composite dispersion liquid: injecting the MXene dispersion liquid obtained in the step two into the aramid fiber nanofiber dispersion liquid obtained in the step one under the stirring action of an injector at a stirring speed of 1500-2500 r/min according to the mass ratio of the aramid fiber nanofiber to the MXene of (40-80) to (20-60) to obtain the aramid fiber nanofiber/MXene composite dispersion liquid, wherein the absolute dry mass of the aramid fiber nanofiber/MXene in the dispersion liquid is 200-600 mg;
step four: preparing a gel-like aramid nanofiber/MXene composite material: placing the aramid fiber nanofiber/MXene composite dispersion liquid obtained in the third step into a sand core funnel, carrying out vacuum filtration for 2-4 h, washing by using deionized water in the vacuum filtration process, removing a dimethyl sulfoxide solvent in a system, and preparing to obtain a gel-like aramid fiber nanofiber/MXene composite material with the water content of 20-60%;
step five: preparing aramid nano fiber/MXene composite conductive aerogel: and (3) placing the gel-like aramid nanofiber/MXene composite material obtained in the fourth step into an aluminum box, placing the aluminum box into a container filled with liquid nitrogen, ensuring that the bottom of the aluminum box is in contact with the upper plane of the liquid nitrogen, freezing the liquid nitrogen for 10-30 min, and then placing the frozen material into a freeze dryer for drying to obtain the aramid nanofiber/MXene composite conductive aerogel which presents an obvious hierarchical structure in the Z direction.
According to the aramid nanofiber/MXene composite conductive aerogel and the preparation method thereof, the aramid nanofiber/MXene composite conductive aerogel with a low density, high strength and high pressure retraction elasticity is prepared by using the aramid nanofiber with a nanoscale structure, high strength, a large length-diameter ratio and high temperature resistance as a matrix and using the MXene with excellent conductivity, good chemical stability and a unique two-dimensional nano film structure as a conductive and filling coating material. The problems that the conventional aramid nanofiber aerogel is non-conductive, poor in compression resilience performance and low in strength due to a high-porosity structure of the conventional aramid nanofiber aerogel, cannot be applied to the fields of pressure sensors and the like are solved, the preparation process is simple and feasible, and the application prospect in the fields of pressure sensors, intelligent sensors, wearable equipment and the like is wide.
The present invention is described in further detail below with reference to examples:
example 1
The aramid nano-fiber/MXene composite conductive aerogel is composed of aramid nano-fiber and MXene, and the mass ratio of the aramid nano-fiber to the MXene is 40: 60; the mass of the aramid nano-fiber/MXene composite conductive aerogel is 600mg, and the density is 40mg/cm 3 。
A preparation method of aramid nanofiber/MXene composite conductive aerogel comprises the following steps:
the method comprises the following steps: preparing aramid nano-fiber dispersion liquid, namely mixing 1g of aramid chopped fibers with the length of 6mm, 1.5g of potassium hydroxide, 500ml of dimethyl sulfoxide and a certain amount of deionized water, wherein the volume ratio of the deionized water to the dimethyl sulfoxide is 1: 50; firstly adding potassium hydroxide, then adding deionized water, mixing and stirring for 5min by using a magnetic stirrer, then sequentially adding aramid chopped fibers and dimethyl sulfoxide, placing the mixture into a sealed beaker, and stirring and reacting for 4h at the rotating speed of 1200r/min by using the magnetic stirrer to obtain 0.2% aramid nano-fiber dispersion liquid dispersed in the dimethyl sulfoxide, wherein the diameter of the aramid nano-fiber is 12-15 nm, and the length of the aramid nano-fiber is 4-7 mu m;
step two: preparing MXene dispersion liquid: adding 6.4g LiF into 100ml 9mol/L HCl solution in a plastic container, stirring at 35 deg.C for 30min, and slowly adding 4g MAX raw material (Ti) 3 AlC 2 ) Continuously stirring the mixed solution at constant temperature (35 ℃) for 35 hours, controlling the rotating speed to be 3500r/min, centrifugally washing the mixed solution by deionized water until the pH value is 5, and dispersing the obtained sample in the deionized water to obtain MXene dispersion liquid with the mass concentration of 1.0%;
step three: preparing an aramid nano fiber/MXene composite dispersion liquid: injecting the MXene dispersion liquid obtained in the second step into the aramid fiber nanofiber dispersion liquid obtained in the first step at a mass ratio of 40:60 under the stirring action of a stirring speed of 2500r/min by using an injector to obtain an aramid fiber nanofiber/MXene composite dispersion liquid, wherein the absolute dry mass of the aramid fiber nanofiber/MXene in the dispersion liquid is 600 mg;
step four: preparing a gel-like aramid nanofiber/MXene composite material: placing the aramid nano-fiber/MXene composite dispersion liquid obtained in the third step into a sand core funnel, carrying out vacuum filtration for 4 hours, washing by using deionized water in the vacuum filtration process, removing a dimethyl sulfoxide solvent in a system, and preparing a gel-like aramid nano-fiber/MXene composite material with the water content of 60%;
step five: preparing the aramid nano fiber/MXene composite conductive aerogel: and (3) placing the gel-like aramid nanofiber/MXene composite material obtained in the fourth step into an aluminum box, placing the aluminum box into a container filled with liquid nitrogen, ensuring that the bottom of the aluminum box is in contact with the upper plane of the liquid nitrogen, freezing the liquid nitrogen for 30min, and then placing the frozen material into a freeze dryer for drying to obtain the aramid nanofiber/MXene composite conductive aerogel presenting an obvious hierarchical structure in the Z direction.
Example 2
The aramid fiber nanofiber/MXene composite conductive aerogel comprises aramid fiber nanofibers and MXene, wherein the mass ratio of the aramid fiber nanofibers to the MXene is 45: 55; the mass of the aramid nano-fiber/MXene composite conductive aerogel is 500mg, and the density is 30mg/cm 3 。
A preparation method of aramid nanofiber/MXene composite conductive aerogel comprises the following steps:
the method comprises the following steps: preparing aramid nano-fiber dispersion liquid, namely mixing 1g of aramid chopped fibers with the length of 6mm, 1.5g of potassium hydroxide, 500ml of dimethyl sulfoxide and a certain amount of deionized water, wherein the volume ratio of the deionized water to the dimethyl sulfoxide is 1: 40; firstly adding potassium hydroxide, then adding deionized water, mixing and stirring for 8min by using a magnetic stirrer, then sequentially adding aramid chopped fibers and dimethyl sulfoxide, placing the mixture into a sealed beaker, and stirring and reacting for 4h at the rotating speed of 1250r/min by using the magnetic stirrer to obtain 0.2% aramid nano-fiber dispersion liquid dispersed in the dimethyl sulfoxide, wherein the diameter of the aramid nano-fiber is 12-15 nm, and the length of the aramid nano-fiber is 4-7 mu m;
step two: preparing MXene dispersion liquid: adding 6.4g LiF into 100ml 9mol/L HCl solution in a plastic container, stirring at 35 deg.C for 30min, and slowly adding 4g MAX raw material (Ti) 3 AlC 2 ) Continuously stirring the mixed solution at constant temperature (35 ℃) for 35 hours, controlling the rotating speed to be 3500r/min, centrifugally washing the mixed solution by deionized water until the pH value is 5, and dispersing the obtained sample in the deionized water to obtain MXene dispersion liquid with the mass concentration of 1.0%;
step three: preparing an aramid nano fiber/MXene composite dispersion liquid: injecting the MXene dispersion liquid obtained in the second step into the aramid fiber nano fiber dispersion liquid obtained in the first step according to the mass ratio of aramid fiber nano fibers to MXene of 45:55 under the stirring action of a syringe at the stirring speed of 2400r/min to obtain aramid fiber nano fiber/MXene composite dispersion liquid, wherein the absolute dry mass of the aramid fiber nano fibers/MXene in the dispersion liquid is 500 mg;
step four: preparing a gel-like aramid nanofiber/MXene composite material: placing the aramid nano fiber/MXene composite dispersion liquid obtained in the third step into a sand core funnel, carrying out vacuum filtration for 4 hours, washing by using deionized water in the vacuum filtration process, removing a dimethyl sulfoxide solvent in a system, and preparing a gel-like aramid nano fiber/MXene composite material with the water content of 50%;
step five: preparing aramid nano fiber/MXene composite conductive aerogel: and (3) placing the gel-like aramid nanofiber/MXene composite material obtained in the fourth step into an aluminum box, placing the aluminum box into a container filled with liquid nitrogen, ensuring that the bottom of the aluminum box is in contact with the upper plane of the liquid nitrogen, freezing the liquid nitrogen for 28min, and then placing the frozen material into a freeze dryer for drying to obtain the aramid nanofiber/MXene composite conductive aerogel presenting an obvious hierarchical structure in the Z direction.
Example 3
The aramid fiber nanofiber/MXene composite conductive aerogel comprises aramid fiber nanofibers and MXene, wherein the mass ratio of the aramid fiber nanofibers to the MXene is 50: 50; the mass of the aramid nano-fiber/MXene composite conductive aerogel is 400mg, and the density is 25mg/cm 3 。
A preparation method of aramid nanofiber/MXene composite conductive aerogel comprises the following steps:
the method comprises the following steps: preparing aramid nano-fiber dispersion liquid, namely mixing 1g of aramid chopped fibers with the length of 6mm, 1.5g of potassium hydroxide, 500ml of dimethyl sulfoxide and a certain amount of deionized water, wherein the volume ratio of the deionized water to the dimethyl sulfoxide is 1: 30, of a nitrogen-containing gas; firstly adding potassium hydroxide, then adding deionized water, mixing and stirring for 10min by using a magnetic stirrer, then sequentially adding aramid chopped fibers and dimethyl sulfoxide, placing the mixture into a sealed beaker, and stirring and reacting for 3h at the rotating speed of 1300r/min by using the magnetic stirrer to obtain 0.2% aramid nano-fiber dispersion liquid dispersed in the dimethyl sulfoxide, wherein the diameter of the aramid nano-fiber is 12-15 nm, and the length of the aramid nano-fiber is 4-7 mu m;
step two: preparation of MXene dispersion: adding 6.4g LiF into 100ml 9mol/L HCl solution in a plastic container, stirring at 35 deg.C for 30min, and slowly adding 4g MAX raw material (Ti) 3 AlC 2 ) Continuously stirring the mixed solution for 35 hours at constant temperature (35 ℃), controlling the rotation speed to 3500r/min, centrifugally washing the mixed solution with deionized water until the pH value is 5, and dispersing the obtained sample in the deionized water to obtain MXene dispersion liquid with the mass concentration of 1.0%;
step three: preparing an aramid nano fiber/MXene composite dispersion liquid: injecting the MXene dispersion liquid obtained in the second step into the aramid fiber nano fiber dispersion liquid obtained in the first step by using an injector under the stirring action of the stirring speed of 2300r/min according to the mass ratio of the aramid fiber nano fiber to the MXene of 50:50 to obtain aramid fiber nano fiber/MXene composite dispersion liquid, wherein the absolute dry mass of the aramid fiber nano fiber/MXene in the dispersion liquid is 400 mg;
step four: preparing a gel-like aramid nanofiber/MXene composite material: placing the aramid nano fiber/MXene composite dispersion liquid obtained in the third step into a sand core funnel, carrying out vacuum filtration for 4 hours, washing by using deionized water in the vacuum filtration process, removing a dimethyl sulfoxide solvent in a system, and preparing a gel-like aramid nano fiber/MXene composite material with the water content of 40%;
step five: preparing the aramid nano fiber/MXene composite conductive aerogel: and (3) placing the gel-like aramid nanofiber/MXene composite material obtained in the fourth step into an aluminum box, placing the aluminum box into a container filled with liquid nitrogen, ensuring that the bottom of the aluminum box is in contact with the upper plane of the liquid nitrogen, freezing the liquid nitrogen for 25min, and then placing the frozen material into a freeze dryer for drying to obtain the aramid nanofiber/MXene composite conductive aerogel presenting an obvious hierarchical structure in the Z direction.
Example 4
The aramid fiber nanofiber/MXene composite conductive aerogel is composed of aramid fiber nanofibers and MXene, and the mass ratio of the aramid fiber nanofibers to the MXene is 55: 45; the mass of the aramid nano fiber/MXene composite conductive aerogel is 350mg, and the density is 25mg/cm 3 。
A preparation method of aramid nanofiber/MXene composite conductive aerogel comprises the following steps:
the method comprises the following steps: preparing an aramid nano-fiber dispersion liquid, namely preparing 1g of aramid chopped fibers with the length of 6mm, 1.5g of potassium hydroxide, 500ml of dimethyl sulfoxide and a certain amount of deionized water, wherein the volume ratio of the deionized water to the dimethyl sulfoxide is 1: 25; firstly adding potassium hydroxide, then adding deionized water, mixing and stirring for 10min by using a magnetic stirrer, then sequentially adding aramid chopped fibers and dimethyl sulfoxide, placing the mixture into a sealed beaker, and stirring and reacting for 3h at the rotating speed of 1350r/min by using the magnetic stirrer to obtain 0.2% aramid nano-fiber dispersion liquid dispersed in the dimethyl sulfoxide, wherein the diameter of the aramid nano-fiber is 12-15 nm, and the length of the aramid nano-fiber is 4-7 mu m;
step two: preparing MXene dispersion liquid: taking 100ml9mol/L HCL solution is put into a plastic container, 6.4g LiF is slowly added, after stirring for 30min at 35 ℃, 4g MAX raw material (Ti) is slowly added 3 AlC 2 ) Continuously stirring the mixed solution at constant temperature (35 ℃) for 35 hours, controlling the rotating speed to be 3500r/min, centrifugally washing the mixed solution by deionized water until the pH value is 5, and dispersing the obtained sample in the deionized water to obtain MXene dispersion liquid with the mass concentration of 1.0%;
step three: preparing an aramid nano fiber/MXene composite dispersion liquid: injecting the MXene dispersion liquid obtained in the second step into the aramid fiber nanofiber dispersion liquid obtained in the first step under the stirring action of a syringe at a stirring speed of 2100r/min according to the mass ratio of the aramid fiber nanofiber to the MXene of 55:45 to obtain an aramid fiber nanofiber/MXene composite dispersion liquid, wherein the absolute dry mass of the aramid fiber nanofiber/MXene in the dispersion liquid is 350 mg;
step four: preparing a gel-like aramid nanofiber/MXene composite material: placing the aramid fiber nanofiber/MXene composite dispersion liquid obtained in the third step into a sand core funnel, carrying out vacuum filtration for 3.5h, washing by using deionized water in the vacuum filtration process, removing a dimethyl sulfoxide solvent in a system, and preparing a gel-like aramid fiber nanofiber/MXene composite material with the water content of 40%;
step five: preparing the aramid nano fiber/MXene composite conductive aerogel: and (3) placing the gel-like aramid nanofiber/MXene composite material obtained in the fourth step into an aluminum box, placing the aluminum box into a container filled with liquid nitrogen, ensuring that the bottom of the aluminum box is in contact with the upper plane of the liquid nitrogen, freezing the liquid nitrogen for 25min, and then placing the frozen material into a freeze dryer for drying to obtain the aramid nanofiber/MXene composite conductive aerogel presenting an obvious hierarchical structure in the Z direction.
Example 5
The aramid nano-fiber/MXene composite conductive aerogel is composed of aramid nano-fiber and MXene, and the mass ratio of the aramid nano-fiber to the MXene is 60: 40; the mass of the aramid nano-fiber/MXene composite conductive aerogel is 300mg, and the density is 20mg/cm 3 。
A preparation method of aramid nanofiber/MXene composite conductive aerogel comprises the following steps:
the method comprises the following steps: preparing aramid nano-fiber dispersion liquid, namely mixing 1g of aramid chopped fibers with the length of 6mm, 1.5g of potassium hydroxide, 500ml of dimethyl sulfoxide and a certain amount of deionized water, wherein the volume ratio of the deionized water to the dimethyl sulfoxide is 1: 25; firstly adding potassium hydroxide, then adding deionized water, mixing and stirring for 15min by using a magnetic stirrer, then sequentially adding the aramid chopped fibers and dimethyl sulfoxide, placing the mixture into a sealed beaker, and stirring and reacting for 2.5h at the rotating speed of 1400r/min by using the magnetic stirrer to obtain 0.2% aramid nano-fiber dispersion liquid dispersed in the dimethyl sulfoxide;
step two: preparation of MXene dispersion: adding 6.4g LiF into 100ml 9mol/L HCl solution in a plastic container, stirring at 35 deg.C for 30min, and slowly adding 4g MAX raw material (Ti) 3 AlC 2 ) Continuously stirring the mixed solution for 35 hours at constant temperature (35 ℃), controlling the rotation speed to 3500r/min, centrifugally washing the mixed solution with deionized water until the pH value is 5, and dispersing the obtained sample in the deionized water to obtain MXene dispersion liquid with the mass concentration of 1.0%;
step three: preparing an aramid nano fiber/MXene composite dispersion liquid: injecting the MXene dispersion liquid obtained in the second step into the aramid fiber nanofiber dispersion liquid obtained in the first step under the stirring action of a syringe at a stirring speed of 1900r/min according to the mass ratio of the aramid fiber nanofiber to the MXene of 60:40 to obtain an aramid fiber nanofiber/MXene composite dispersion liquid, wherein the absolute dry mass of the aramid fiber nanofiber/MXene in the dispersion liquid is 300 mg;
step four: preparing a gel-like aramid nanofiber/MXene composite material: placing the aramid nano fiber/MXene composite dispersion liquid obtained in the third step into a sand core funnel, carrying out vacuum filtration for 3 hours, washing by using deionized water in the vacuum filtration process, removing a dimethyl sulfoxide solvent in a system, and preparing a gel-like aramid nano fiber/MXene composite material with the water content of 35%;
step five: preparing aramid nano fiber/MXene composite conductive aerogel: and (3) placing the gel-like aramid nanofiber/MXene composite material obtained in the fourth step into an aluminum box, placing the aluminum box into a container filled with liquid nitrogen, ensuring that the bottom of the aluminum box is in contact with the upper plane of the liquid nitrogen, freezing the liquid nitrogen for 20min, and then placing the frozen material into a freeze dryer for drying to obtain the aramid nanofiber/MXene composite conductive aerogel presenting an obvious hierarchical structure in the Z direction.
Example 6
The aramid nano-fiber/MXene composite conductive aerogel is composed of aramid nano-fiber and MXene, and the mass ratio of the aramid nano-fiber to the MXene is 70: 30; the mass of the aramid nano fiber/MXene composite conductive aerogel is 250mg, and the density is 20mg/cm 3 。
A preparation method of aramid nanofiber/MXene composite conductive aerogel comprises the following steps:
the method comprises the following steps: preparing aramid nano-fiber dispersion liquid, namely 1g of aramid chopped fibers with the length of 6mm, 1.5g of potassium hydroxide, 500ml of dimethyl sulfoxide and a certain amount of deionized water, wherein the volume ratio of the deionized water to the dimethyl sulfoxide is 1: 20; firstly adding potassium hydroxide, then adding deionized water, mixing and stirring for 17min by using a magnetic stirrer, then sequentially adding the aramid chopped fibers and dimethyl sulfoxide, placing the mixture into a sealed beaker, and stirring and reacting for 2.5h at the rotating speed of 1450r/min by using the magnetic stirrer to obtain 0.2% aramid nano-fiber dispersion liquid dispersed in the dimethyl sulfoxide, wherein the diameter of the aramid nano-fiber is 12-15 nm, and the length of the aramid nano-fiber is 4-7 mu m;
step two: preparation of MXene dispersion: 100ml of 9mol/L HCl solution was put in a plastic container, 6.4g LiF was slowly added, and after stirring at 35 ℃ for 30min, 4g MAX raw material (Ti) was slowly added 3 AlC 2 ) Continuously stirring the mixed solution for 35 hours at constant temperature (35 ℃), controlling the rotation speed to 3500r/min, centrifugally washing the mixed solution with deionized water until the pH value is 5, and dispersing the obtained sample in the deionized water to obtain MXene dispersion liquid with the mass concentration of 1.0%;
step three: preparing an aramid nano fiber/MXene composite dispersion liquid: injecting the MXene dispersion liquid obtained in the second step into the aramid fiber nano fiber dispersion liquid obtained in the first step at a mass ratio of aramid fiber nano fiber to MXene of 70:30 under the stirring action of a syringe at a stirring speed of 1700r/min to obtain aramid fiber nano fiber/MXene composite dispersion liquid, wherein the absolute dry mass of the aramid fiber nano fiber/MXene in the dispersion liquid is 250 mg;
step four: preparing a gel-like aramid nanofiber/MXene composite material: placing the aramid fiber nanofiber/MXene composite dispersion liquid obtained in the third step into a sand core funnel, carrying out vacuum filtration for 2.5h, washing by using deionized water in the vacuum filtration process, removing a dimethyl sulfoxide solvent in a system, and preparing a gel-like aramid fiber nanofiber/MXene composite material with the water content of 30%;
step five: preparing aramid nano fiber/MXene composite conductive aerogel: and (3) placing the gel-like aramid nanofiber/MXene composite material obtained in the fourth step into an aluminum box, placing the aluminum box into a container filled with liquid nitrogen, ensuring that the bottom of the aluminum box is in contact with the upper plane of the liquid nitrogen, freezing the liquid nitrogen for 15min, and then placing the frozen material into a freeze dryer for drying to obtain the aramid nanofiber/MXene composite conductive aerogel presenting an obvious hierarchical structure in the Z direction.
Example 7
The aramid fiber nanofiber/MXene composite conductive aerogel comprises aramid fiber nanofibers and MXene, wherein the mass ratio of the aramid fiber nanofibers to the MXene is 80: 20; the mass of the aramid nano fiber/MXene composite conductive aerogel is 200mg, and the density is 20mg/cm 3 。
A preparation method of aramid nanofiber/MXene composite conductive aerogel comprises the following steps:
the method comprises the following steps: preparing aramid nano-fiber dispersion liquid, namely 1g of aramid chopped fibers with the length of 6mm, 1.5g of potassium hydroxide, 500ml of dimethyl sulfoxide and a certain amount of deionized water, wherein the volume ratio of the deionized water to the dimethyl sulfoxide is 1: 15; firstly adding potassium hydroxide, then adding deionized water, mixing and stirring for 20min by using a magnetic stirrer, then sequentially adding the aramid chopped fibers and dimethyl sulfoxide, placing the mixture into a sealed beaker, and stirring and reacting for 2h at the rotating speed of 1500r/min by using the magnetic stirrer to obtain 0.2% aramid nano-fiber dispersion liquid dispersed in the dimethyl sulfoxide, wherein the diameter of the aramid nano-fiber is 12-15 nm, and the length of the aramid nano-fiber is 4-7 mu m;
step two: preparing MXene dispersion liquid: 100ml of 9mol/L HCl solution was put in a plastic container, 6.4g LiF was slowly added, and after stirring at 35 ℃ for 30min, 4g MAX raw material (Ti) was slowly added 3 AlC 2 ) Continuously stirring the mixed solution for 35 hours at constant temperature (35 ℃), controlling the rotation speed to 3500r/min, centrifugally washing the mixed solution with deionized water until the pH value is 5, and dispersing the obtained sample in the deionized water to obtain MXene dispersion liquid with the mass concentration of 1.0%;
step three: preparing an aramid nano fiber/MXene composite dispersion liquid: injecting the MXene dispersion liquid obtained in the second step into the aramid fiber nanofiber dispersion liquid obtained in the first step under the stirring action of a syringe at a stirring speed of 1500r/min according to the mass ratio of the aramid fiber nanofiber to the MXene of 80:20 to obtain an aramid fiber nanofiber/MXene composite dispersion liquid, wherein the absolute dry mass of the aramid fiber nanofiber/MXene in the dispersion liquid is 200 mg;
step four: preparing a gel-like aramid nanofiber/MXene composite material: placing the aramid nano fiber/MXene composite dispersion liquid obtained in the third step into a sand core funnel, carrying out vacuum filtration for 2 hours, washing by using deionized water in the vacuum filtration process, removing a dimethyl sulfoxide solvent in a system, and preparing a gel-like aramid nano fiber/MXene composite material with the water content of 20%;
step five: preparing the aramid nano fiber/MXene composite conductive aerogel: and (3) placing the gel-like aramid nanofiber/MXene composite material obtained in the fourth step into an aluminum box, placing the aluminum box into a container filled with liquid nitrogen, ensuring that the bottom of the aluminum box is in contact with the upper plane of the liquid nitrogen, freezing the liquid nitrogen for 10min, and then placing the frozen material into a freeze dryer for drying to obtain the aramid nanofiber/MXene composite conductive aerogel presenting an obvious hierarchical structure in the Z direction.
The aramid nano-fiber/MXene composite prepared in the embodiment 3 of the inventionThe conductive aerogel is detected and characterized, and part of indexes are as follows: 1. density: 25mg/cm -3 (ii) a 2. Compressive strength (50% strain): 51.5kPa, as shown in FIG. 3; 3. initial thermal decomposition temperature: 517 ℃ as shown in FIG. 4; 4. when the aramid nanofiber/MXene composite conductive aerogel is compressed at the pressure of 0.5kPa, obvious electric signal change can be generated, and the response speed is high, as shown in FIG. 5. The aramid nanofiber/MXene composite conductive aerogel prepared by the invention has good conductivity, excellent mechanical property and compression resilience, and excellent heat resistance. The aramid nano-fiber/MXene composite conductive aerogel with high strength and high sensitivity is developed and produced by adopting a novel process and a novel method, the production process is simple and feasible, the application of the aramid nano-fiber aerogel in the fields of pressure-sensitive sensors and the like is expanded, and the application prospect is wide.

Claims (9)

1. The aramid nano-fiber/MXene composite conductive aerogel is characterized by comprising aramid nano-fiber and MXene, wherein the mass ratio of the aramid nano-fiber to the MXene is (40-80) to (60-20); the density of the aramid nano fiber/MXene composite conductive aerogel is 20-40 mg/cm 3 ；
The aramid nano-fiber/MXene composite conductive aerogel is prepared by the following method:
the method comprises the following steps: preparing an aramid nanofiber dispersion liquid: mixing and sealing aramid chopped fibers, potassium hydroxide, dimethyl sulfoxide and deionized water, and stirring and reacting for 2-4 hours at the rotating speed of 1200-1500 r/min to obtain an aramid nanofiber dispersion liquid dispersed in the dimethyl sulfoxide;
step two: preparation of MXene dispersion: adding MAX raw materials and LiF into HCL solution, stirring at constant temperature to obtain MXene materials, washing with deionized water to neutrality, and dispersing in deionized water to obtain MXene dispersion liquid;
step three: preparing an aramid nano fiber/MXene composite dispersion liquid: injecting the MXene dispersion liquid obtained in the step two into the aramid nano-fiber dispersion liquid obtained in the step one under the stirring action of the stirring speed of 1500 r/min-2500 r/min to obtain an aramid nano-fiber/MXene composite dispersion liquid;
step four: preparing a gel-like aramid nanofiber/MXene composite material: preparing the gel-like aramid nano fiber/MXene composite material by carrying out vacuum filtration on the aramid nano fiber/MXene composite dispersion liquid obtained in the step three;
step five: preparing the aramid nano fiber/MXene composite conductive aerogel: and (3) placing the gel-like aramid nanofiber/MXene composite material obtained in the fourth step into an aluminum box, placing the aluminum box into a container filled with liquid nitrogen, freezing for 10-30 min, enabling the bottom of the aluminum box to be in contact with the upper plane of the liquid nitrogen when the liquid nitrogen is frozen, and then placing the frozen material into a freeze dryer for drying to obtain the aramid nanofiber/MXene composite conductive aerogel.
2. The preparation method of the aramid nanofiber/MXene composite conductive aerogel is characterized by comprising the following steps of:
the method comprises the following steps: preparing an aramid nanofiber dispersion liquid: mixing and sealing the aramid chopped fibers, potassium hydroxide, dimethyl sulfoxide and deionized water, and stirring and reacting for 2-4 hours at the rotating speed of 1200-1500 r/min to obtain an aramid nanofiber dispersion liquid dispersed in the dimethyl sulfoxide;
step two: preparation of MXene dispersion: adding MAX raw materials and LiF into HCL solution, stirring at constant temperature to obtain MXene materials, washing with deionized water to neutrality, and dispersing in deionized water to obtain MXene dispersion liquid;
step three: preparing an aramid nano fiber/MXene composite dispersion liquid: injecting the MXene dispersion liquid obtained in the step two into the aramid nano-fiber dispersion liquid obtained in the step one under the stirring action of the stirring speed of 1500-2500 r/min to obtain an aramid nano-fiber/MXene composite dispersion liquid;
step four: preparing a gel-like aramid nanofiber/MXene composite material: preparing a gel-like aramid nano fiber/MXene composite material from the aramid nano fiber/MXene composite dispersion liquid obtained in the third step through vacuum filtration;
step five: preparing the aramid nano fiber/MXene composite conductive aerogel: and (3) placing the gel-like aramid nanofiber/MXene composite material obtained in the fourth step into an aluminum box, placing the aluminum box into a container filled with liquid nitrogen, freezing for 10-30 min, enabling the bottom of the aluminum box to be in contact with the upper plane of the liquid nitrogen when the liquid nitrogen is frozen, and then placing the frozen material into a freeze dryer for drying to obtain the aramid nanofiber/MXene composite conductive aerogel.
3. The preparation method of the aramid nanofiber/MXene composite conductive aerogel according to claim 2, wherein in the first step, the proportion of the aramid chopped fibers, potassium hydroxide and dimethyl sulfoxide is 1 g: 1.5 g: 500mL, wherein the volume ratio of the deionized water to the dimethyl sulfoxide is 1: 50-1: 15.
4. The preparation method of the aramid nanofiber/MXene composite conductive aerogel according to claim 2, wherein the aramid chopped fiber, the deionized water, the dimethyl sulfoxide and the potassium hydroxide are added in the following sequence: firstly adding potassium hydroxide and then deionized water, mixing and stirring for 5-20 min, and then sequentially adding aramid chopped fibers and dimethyl sulfoxide.
5. The preparation method of the aramid nanofiber/MXene composite conductive aerogel according to claim 2, wherein in the first step, the length of the aramid chopped fiber is 6 mm; the mass concentration of the obtained aramid nano-fiber dispersion liquid dispersed in dimethyl sulfoxide is 0.2%, wherein the diameter of the aramid nano-fiber is 12-15 nm, and the length of the aramid nano-fiber is 4-7 mu m.
6. The preparation method of the aramid nanofiber/MXene composite conductive aerogel according to claim 2, wherein in the second step, the concentration of the HCL solution is 9mol/L, and the MAX raw material is Ti 3 AlC 2 And Ti 3 AlC 2 : the mass ratio of LiF is 1:1.6, and the mass concentration of the obtained MXene dispersion liquid is 1.0%.
7. The preparation method of the aramid nanofiber/MXene composite conductive aerogel according to claim 2, wherein in the second step, the constant-temperature stirring temperature is 35 ℃ and the time is 35 hours.
8. The preparation method of the aramid nanofiber/MXene composite conductive aerogel as claimed in claim 2, wherein the mass ratio of the aramid nanofiber to the MXene in the third step is (40-80): (60-20).
9. The preparation method of the aramid nanofiber/MXene composite conductive aerogel according to claim 2, wherein the vacuum filtration time in the fourth step is 2-4 hours, and the water content of the obtained gel-like aramid nanofiber/MXene composite material is controlled to be 20% -60%.
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