CN115347251A - Preparation method of piezoelectric flexible self-powered sensor battery - Google Patents
Preparation method of piezoelectric flexible self-powered sensor battery Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
- H01M10/38—Construction or manufacture
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/16—Measuring force or stress, in general using properties of piezoelectric devices
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/18—Measuring 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/02—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning
- G01L9/06—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning of piezo-resistive devices
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/08—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of piezoelectric devices, i.e. electric circuits therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The application discloses a preparation method of a piezoelectric flexible self-powered sensor battery, which comprises the following steps: s101, adding graphene oxide into deionized water to form a graphene oxide suspension; s102, adding MXene solution into the graphene oxide suspension, stirring uniformly, and adding glucose to dissolve; s103, adding a certain mass fraction of cellulose suspension into deionized water, and stirring until the cellulose suspension is completely dissolved; s104, mixing and stirring the solution obtained in the step S103 and the solution obtained in the step S102 to obtain a mixed solution; s105, pouring the mixed solution into a prefabricated container, performing directional freezing through liquid nitrogen, and then drying in a freeze dryer; s106, putting the dried sample into a tube furnace, introducing nitrogen, keeping the sample at 300 ℃ for one hour, heating to 600-800 ℃ and keeping for one hour to obtain a finished product; and S107, assembling the battery by using the finished product.
Description
Technical Field
The application relates to the technical field of battery materials, in particular to a preparation method of a piezoelectric flexible self-powered sensor battery.
Background
The application relates to the technical field of battery materials, in particular to a preparation method of a piezoelectric flexible self-powered sensor battery. The rechargeable pressure sensor is used as a wearable intelligent device, has wide application prospect in the fields of artificial intelligence, medical appliances and the like, and arouses great research interest of people. Generally, the operation of the sensor depends on the support of an external power supply, which inevitably causes additional cost of the power supply, and the limitation of the volume of the additional power supply causes poor expandability. Thus, the spatial integration of the wearable sensor with the power source theoretically ensures that the pressure sensor achieves the inherent volume occupancy of the sensing device, but to date, little research has been done.
According to the existing research results, the construction of the nano generator based on the friction power generation mode is only explored, and the preparation of the self-powered sensor is mainly used. The nanogenerator provides a very small output current (typically in the range of 0-20 mua) due to the large internal resistance material necessary for the nanogenerator to operate, which affects the accurate measurement of micro-current. The piezoelectric flexible self-powered sensor mainly utilizes the piezoelectric effect caused by dielectric moment to realize the sensing of signals. The electric dipole moment is generated by deformation of oriented non-centrosymmetric crystal structure or porous polar body with persistent charges in the pore channels, and usually requires the use of harmful lead metal or organic ferroelectric compound materials. Moreover, such sensors can only be used to detect dynamic pressure signals, and cannot detect static pressure. The flexible pressure sensor can be mainly divided into a piezoresistive type, a capacitive type and a piezoelectric type according to a stimulation response mechanism, wherein the piezoresistive type sensor reflects impedance change belonging to state parameters, and has the capability of intuitively quantifying and visualizing external stress stimulation and even static pressure. However, the piezoresistive effect does not generate a charge, which provides a significant barrier to the design of a self-powered current source.
The flexible battery may be coupled to the pressure sensor in view of the large influence of the floating of the impedance on the output current when supplied by the regulated voltage source. Among various mainstream batteries, rechargeable zinc ion batteries are receiving attention because of their advantages of high energy density, safe discharge process, non-toxic and inexpensive battery materials, simple preparation process, etc. Therefore, designing a suitable zinc-ion battery system to operate in an affordable and scalable manner, with sustainable pressure sensing materials as one electrode, is expected to solve the above-mentioned problems,
flexible pressure sensors are typically composed of conductive electrodes, a force-sensitive layer, and a flexible substrate. Stability and sensitivity are important parameters for evaluating the performance of a sensor. Currently, hydrogels and aerogels with high porosity, excellent flexibility and electromechanical properties have been developed. However, hydrogel sensors tend to have hysteresis and volatility and low sensitivity, while aerogels tend to collapse under device deformation, becoming a circulation-stable stumbling stone. There is thus still a challenge in balancing sensitivity and stability. In addition, the positive electrode material of the zinc ion battery essentially ensures the efficient, rapid and stable storage of zinc, and realizes the smooth transmission of zinc ions, which puts more severe requirements on the cathode of the zinc ion mixed pressure sensor with dual identities.
Disclosure of Invention
In order to solve the technical problem, the application provides a preparation method of a piezoelectric flexible self-powered sensor battery, which is used for preparing a pressure sensor, reducing the space volume occupied by the pressure sensor and simultaneously improving the performance of the battery.
The preparation method of the piezoelectric flexible self-powered sensor battery provided by the application comprises the following steps:
s101, adding graphene oxide into deionized water, and stirring and oscillating to form a graphene oxide suspension;
s102, adding an MXene solution with a certain mass fraction into the graphene oxide suspension, uniformly stirring, adding glucose with a certain mass fraction, stirring and vibrating until the MXene solution is completely dissolved;
s103, adding the cellulose suspension with a certain mass fraction into deionized water, and stirring until the cellulose suspension is completely dissolved to obtain a cellulose solution;
s104, mixing and stirring the solution obtained in the step S103 and the solution obtained in the step S102 to obtain a mixed solution;
s105, pouring the mixed solution into a prefabricated container, performing directional freezing through liquid nitrogen, and then drying in a freeze dryer to obtain a dried sample;
s106, putting the dried sample into a tube furnace, introducing nitrogen, keeping the sample at 300 ℃ for one hour, heating to 600-800 ℃ and keeping for one hour to obtain a finished product;
and S107, assembling the battery by using the finished product.
Optionally, the MXene solution with a certain mass fraction is 0.2% -0.35% of the MXene solution with a certain mass fraction, and the cellulose suspension with a certain mass fraction is 2% -3% of the cellulose suspension with a certain mass fraction.
Optionally, in the mixed solution, the mass fraction of graphene oxide is 0.5-0.83%, the mass fraction of MXene is 0.08-0.125%, the mass fraction of glucose is 0.8-1.25%, and the mass fraction of cellulose is 0.8-1.25%.
Optionally, the graphene oxide in step S101 is synthesized by:
mixing concentrated sulfuric acid and phosphoric acid according to the proportion of 180;
slowly adding a certain amount of potassium permanganate into the container, and placing the container in a water bath kettle for magnetic stirring;
slowly adding hydrogen peroxide solution with a certain mass fraction into the container for multiple times until no bubbles are generated;
and when the preset reaction time is up, taking the container out of the water bath, slowly adding deionized water for many times for natural sedimentation, and taking out the precipitate in the container for freeze drying when the pH value of the supernatant is 6 to 7 to obtain the graphene oxide.
Optionally, the temperature of the water bath is 50 ℃, the stirring time is 6 hours, the mass fraction of the hydrogen peroxide solution is 15%, and the amount of the hydrogen peroxide solution added each time is 3.5 ml.
Optionally, the cellulose solution comprises: cellulose nanofiber, high-pressure uniform medium nanofiber, tempo oxidation high-pressure uniform nanofiber, lignin, CNF-P, CNF-C, cellulose nanocrystal and hydroxypropyl methyl cellulose.
Optionally, the heating rate when heating to 600 to 800 degrees celsius is 5 degrees celsius per minute.
Alternatively, the MXene solution is prepared by the following steps:
etching the Max phase of the titanium aluminum carbide by using hydrochloric acid for 48 hours to obtain a sample;
cleaning and ultrasonically oscillating the sample to obtain MXene; the MXene at least comprises an oxygen functional group, a hydroxide functional group and a fluorine functional group on the surface.
MXene solution was prepared using the MXene.
Optionally, the prefabricated container is an alumina container.
Optionally, in step S107, when the battery is assembled, the electrolyte is zinc trifluoromethanesulfonate.
According to the technical scheme, the method has the following advantages:
(1) The method provided by the application provides a new method for preparing the pressure sensor, the problem that the pressure sensor is required to be externally connected with an additional power supply is solved, the prepared battery can be directly used in the pressure sensor, and the space volume required by the pressure sensor is reduced.
(2) The finished product configuration prepared by the method has rich gap three-dimensional network, can effectively load various active materials, and can be used for assembling an ion battery.
(3) The pressure sensor prepared from the battery prepared by the method can adjust the content of MXene according to the current detection requirements of different pressure equipment. The pressure sensor can also be sized according to equipment requirements.
(4) The synthesis mode related to the method is simple, and the piezoelectric flexible self-supply sensor battery prepared by the method has excellent sensitivity and battery performance.
Drawings
In order to more clearly illustrate the technical solutions in the present application, the drawings required for the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings may be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic flow chart illustrating one embodiment of a method for making a piezoelectric flexible self-powered sensor cell of the present application;
fig. 2 is a schematic flow diagram of one embodiment of the preparation of graphene oxide provided herein;
fig. 3 is a capacity plot of a battery prepared by the method of the present application;
FIG. 4 is a graph of the cycling relationship between current and voltage for electrodes prepared by the methods of the present application.
Detailed Description
Flexible pressure sensors are typically composed of conductive electrodes, a force-sensitive layer, and a flexible substrate. Stability and sensitivity are important parameters for evaluating the performance of a sensor. Currently, hydrogels and aerogels with high porosity, excellent flexibility and electromechanical properties have been developed. However, hydrogel sensors tend to have hysteresis and volatility and low sensitivity, while aerogels tend to collapse under device deformation, becoming a circulation-stable stumbling stone. There is therefore still a challenge in balancing sensitivity and stability. In addition, the positive electrode material of the zinc ion battery essentially ensures the efficient, rapid and stable storage of zinc, and realizes the smooth transmission of zinc ions, which puts more severe requirements on the cathode of the zinc ion mixed pressure sensor with dual identities.
Transition metal carbides and nitrides (MXene, formula Mn +1XnTx, where M stands for transition metal, n = 1,2 or 3) are hot spot members of the two-dimensional (2D) family, which are advantageous for applications in the sensor and battery field due to their abundant surface functional groups (-OH, -O and-F), remarkable mechanical strength and extremely high "semi-metal" properties (> 6000S cm "1). The aerogel structure based on MXene has high porosity, low density and controllable three-dimensional porous structure, and shows huge potential in the fields of pressure sensing and batteries. In order to better match the pressure sensor to the zinc ion battery, the problem facing MXene-based aerogel structure is how to formulate the material selection and assembly rules to activate the dual function of the zinc ion hybrid pressure sensor.
MXene has excellent conductivity as well as graphene, and is a novel two-dimensional material with metal conductivity. However, MXene materials exist in powder or thin film form, and have high density due to extremely dense structure, and the structure is also extremely easy to break, and they do not have scalability, and MXene materials are not as flexible as graphene sheets, and are themselves difficult to form graphene aerogel with three-dimensional structure like graphene, and it is known from reported literature that graphene oxide is easy to form graphene aerogel with three-dimensional morphology. And the surface of the reduced graphene oxide contains rich oxygen-containing functional groups, and strong electrostatic repulsion exists between layers, so that the aqueous dispersion of the reduced graphene oxide is a colloid with negative electricity and can stably exist. MXene obtained by hydrochloric acid etching also contains hydrophilic groups such as hydroxyl group and epoxy group on the surface, and the aqueous dispersion thereof is negatively charged. Therefore, the reduced graphene oxide and MXene can be uniformly dispersed together, and stable colloid can be easily formed, so that favorable theoretical support is provided for the constructed MXene/graphene composite aerogel. However, the elastic property of the aerogel is lack of rigid support, the sensitivity of the aerogel in the aspect of pressure sensors is not enough, a substance with certain toughness needs to be filled into the aerogel so as to achieve better sensitivity, the selected cellulose has certain rigidity and can well play a supporting role, and the porous aerogel structure can effectively load different active materials to assemble different metal ion batteries.
Based on this, the present application provides a method for manufacturing a piezoelectric flexible self-powered sensor cell, and examples of the method will be described in detail below.
Referring to fig. 1, fig. 1 is a schematic flow chart of an embodiment of a method for manufacturing a piezoelectric flexible self-powered sensor battery provided in the present application, where the method includes:
s101, adding graphene oxide into deionized water, and stirring and oscillating to form a graphene oxide suspension;
s102, adding an MXene solution with a certain mass fraction into the graphene oxide suspension, uniformly stirring, adding glucose with a certain mass fraction, stirring and vibrating until the MXene solution is completely dissolved;
s103, adding the cellulose suspension with a certain mass fraction into deionized water, and stirring until the cellulose suspension is completely dissolved to obtain a cellulose solution;
s104, mixing and stirring the solution obtained in the step S103 and the solution obtained in the step S102 to obtain a mixed solution;
s105, pouring the mixed solution into a prefabricated container, performing directional freezing through liquid nitrogen, and then drying in a freeze dryer to obtain a dried sample;
s106, putting the dried sample into a tube furnace, introducing nitrogen, keeping the sample at 300 ℃ for one hour, heating to 600-800 ℃ and keeping for one hour to obtain a finished product;
and S107, assembling the battery by using the finished product.
In the above method provided by the present application, step S101 is used to prepare the graphene oxide suspension, and step S103 is used to prepare the cellulose solution, obviously, the time sequence between step S101 and step S103 may not be limited, that is, in practice, the graphene oxide suspension may be prepared first, the cellulose solution may be prepared first, or the graphene oxide suspension may be prepared simultaneously.
In the method that this application provided, synthesize MXene/oxidation graphite alkene aerogel earlier, be the aerogel of a three-dimensional structure, add the cellulose wherein again, improve its pressure sensitivity, and play crucial effect to three-dimensional structure's elasticity, use ultra-low temperature refrigeration technique, the aerogel network porosity that carries out directional freezing preparation through the liquid nitrogen promptly is abundant, the surface area is big, the carbon-based three-dimensional network that forms after calcining, be favorable to the transmission of electron, also be favorable to compressing the improvement of resilience performance equally, it is very big to battery performance and pressure performance's promotion, the voltage force transducer of this application method preparation still can be applied to the bracelet and detect the heartbeat, the motion, and aspects such as joint motion, can effectively detect pressure in real time. And the advantage of the pressure sensor of the same kind is that the pressure sensor can be self-powered and can provide the power required for the pressure detection of the same kind. Referring to fig. 3, fig. 3 is a graph of the capacity of a battery prepared by the method of the present application; FIG. 4 is a graph of the cycling relationship between current and voltage for electrodes prepared by the methods of the present application.
The graphene oxide used in step S101 may be directly prepared from a graphene oxide finished product, or may be prepared by itself, and the present application further provides an embodiment for preparing graphene oxide, which refers to fig. 2, and includes:
s201, mixing concentrated sulfuric acid and phosphoric acid according to the proportion of 180, adding a certain amount of graphite powder, and stirring and dissolving in a container;
s202, slowly adding quantitative potassium permanganate into the container, and placing the container in a water bath for magnetic stirring;
s203, slowly adding hydrogen peroxide solution with a certain mass fraction into the container for multiple times until no bubbles are generated;
and S204, taking the container out of the water bath pot after the preset reaction time is reached, slowly adding deionized water for many times for natural sedimentation, taking out the precipitate in the container for freeze drying until the pH value of the supernatant is 6-7, and obtaining the graphene oxide.
In view of the above method, the present application provides five embodiments for detailed description, which are:
the first embodiment is as follows:
(1) Adding graphene oxide into deionized water, and performing magnetic stirring and ultrasonic oscillation until suspension with the mass fraction of about 1.2-2% is formed;
the graphene oxide can be prepared by a hummer method, and the solution is deionized water.
(2) The method comprises the steps of pouring 0.2-0.35% by mass of MXene solution into 1.2-2% by mass of graphene oxide suspension for magnetic stirring, adding 2-3% by mass of glucose, and performing magnetic stirring and ultrasonic oscillation until the MXene solution is completely dissolved.
The glucose used in this step includes sucrose and glucose (D- (+) -glucopyranose, β -D-glucopyranose; α -D-glucopyranose; β -D-glucopyranose).
(3) And adding the cellulose suspension with the mass fraction of 2-3% into a beaker, and magnetically stirring until the cellulose suspension is dissolved to obtain a cellulose solution.
The cellulose used is: cellulose nano-fiber, high-pressure uniform medium nano-fiber, tempo oxidation high-pressure uniform nano-fiber, lignin, CNF-P, CNF-C, cellulose nanocrystal, hydroxypropyl methyl cellulose,
(4) And (3) mixing and stirring the solution obtained in the step (2) and the step (3) for 6 to 24 hours, wherein in the mixed solution, the mass fraction of graphene oxide is 0.5 to 0.83 percent, the mass fraction of MXene is 0.08 to 0.125 percent, the mass fraction of glucose is 0.8 to 1.25 percent, and the mass fraction of cellulose is 0.8 to 1.25 percent.
(5) Pouring the solution into a prefabricated container, and performing liquid nitrogen directional freezing, wherein the specific mode can be that the prefabricated container is placed above a precooled copper block (the bottom of the container is required to be smaller than the top of the copper block) and is placed in a freeze drying box overnight (the environment of the freeze drying box is-80 ℃, and 1000 pa). The prefabricated container used in this step may be an alumina crucible ark or other container of alumina material.
(6) And (3) placing the dried sample in a tube furnace, introducing nitrogen for 20 minutes, setting the annealing temperature, keeping the temperature at 300 ℃ for 1 hour, and keeping the temperature at about 700-800 ℃ for 1 hour, wherein the heating rate during heating is 5℃/min. In the step, annealing is carried out at the temperature of 300 ℃, and then the temperature is raised to 700 to 800 ℃.
The method of the present application corresponding to fig. 1 is described in detail below by means of four more specific examples:
example two:
(1) 140mg of graphene oxide was weighed and placed in a beaker A containing 6mL of deionized water, and magnetic stirring was performed for 0.5 hour and ultrasonic oscillation was performed for 0.5 hour until a stable suspension was formed.
(2) Pouring 6mL of MXene aqueous solution with the mass of 24mg into a beaker A, performing magnetic stirring for 0.5 hour to fully mix and dissolve the MXene aqueous solution, adding 200mg of glucose into the beaker A, performing magnetic stirring for 10 minutes, and performing ultrasonic oscillation for 0.5 hour.
(3) 280mg of cellulose was weighed and placed in a beaker B containing 12mL of deionized water, and stirred for 20 minutes to obtain a cellulose solution.
(4) The solution in beaker A was poured into beaker B and magnetically stirred rapidly for 6 hours.
(5) 2mL of the mixed solution was poured into a 30mm 20X 10 alumina square boat and placed on a 50X 20 copper block that had been pre-cooled with liquid nitrogen. After being completely frozen, the mixture is placed in a freeze dryer for drying.
(6) Placing the dried sample in a tube furnace, introducing nitrogen for 20 minutes, and setting the temperature interval as follows: the temperature is firstly preserved for one hour at 300 ℃, and then the temperature is raised to 800 ℃ and preserved for one hour. The heating rate was 5 ℃/min. And finally, assembling the battery. The electrolyte is zinc trifluoromethanesulfonate, the middle of the electrolyte is separated by a diaphragm, the diaphragm is used for separating the synthesized electrode from the zinc electrode, the positive electrode and the negative electrode of the battery are prevented from being separated, meanwhile, the electrolyte also has a good water retention function, and the loss of the electrolyte can be well reduced.
Example three:
(1) 120mg of graphene oxide was weighed, placed in a beaker A containing 6mL of deionized water, magnetically stirred for 0.5 hour, and ultrasonically shaken for 0.5 hour until a stable suspension was formed.
(2) Pouring 6mL of MXene aqueous solution containing 20mg of MXene into a beaker A, carrying out magnetic stirring for 0.5 hour to fully mix and dissolve, adding 240mg of glucose into the solution, carrying out magnetic stirring for 10 minutes, and carrying out ultrasonic oscillation for 0.5 hour.
(3) 240mg of cellulose was weighed and placed in a beaker B containing 12mL of deionized water, and stirred for 20 minutes to obtain a cellulose solution.
(4) The solution in beaker A was poured into beaker B and stirred magnetically for 6 hours rapidly.
(5) 2mL of the mixed solution was poured into a 30mm 20X 10 alumina square boat and placed on a 50X 20 copper block that had been pre-cooled with liquid nitrogen. After completely freezing, placing the mixture in a freeze dryer for drying.
(6) Placing the dried sample in a tube furnace, introducing nitrogen for 20 minutes, and setting the temperature interval as follows: the temperature is firstly preserved for one hour at 300 ℃, and then the temperature is raised to 600 ℃ and preserved for one hour. The heating rate was 5 ℃/min. And then the battery assembly is carried out. The electrolyte is zinc trifluoromethanesulfonate.
Example four:
(1) 100mg of graphene oxide was weighed and placed in a beaker A containing 6mL of deionized water, and magnetic stirring was carried out for 0.5 hour and ultrasonic oscillation was carried out for 0.5 hour until a stable suspension was formed.
(2) Pouring 6mL of MXene aqueous solution with the mass of 24mg into a beaker A, magnetically stirring for 0.5 hour to fully mix and dissolve, adding 260mg of glucose into the beaker, magnetically stirring for 10 minutes, and ultrasonically oscillating for 0.5 hour.
(3) 220mg of cellulose was weighed into a beaker B containing 12mL of deionized water and stirred for 20 minutes.
(4) The solution in beaker A was poured into beaker B and magnetically stirred rapidly for 6 hours.
(5) 2mL of the mixed solution was poured into a 30mm 20X 10 alumina square boat and placed on a 50X 20 copper block that had been pre-cooled with liquid nitrogen. After being completely frozen, the mixture is placed in a freeze dryer for drying.
(6) Placing the dried sample in a tube furnace, introducing nitrogen for 20 minutes, and setting the temperature interval as follows: the temperature is firstly preserved for one hour at 300 ℃, and then the temperature is raised to 700 ℃ and preserved for one hour. The heating rate was 5 ℃/min. And then the battery assembly is carried out. The electrolyte is zinc trifluoromethanesulfonate.
Example five:
(1) 150mg of graphene oxide was weighed and placed in a beaker A containing 6mL of deionized water, and magnetic stirring was performed for 0.5 hour and ultrasonic oscillation was performed for 0.5 hour until a stable suspension was formed.
(2) Pouring 6mL of MXene aqueous solution with the mass of 30mg into a beaker A, magnetically stirring for 0.5 hour to fully mix and dissolve, adding 220mg of glucose into the beaker, magnetically stirring for 10 minutes, and ultrasonically oscillating for 0.5 hour.
(3) 230mg of cellulose was weighed into a beaker B containing 12mL of deionized water and stirred for 20 minutes.
(4) The solution in beaker A was poured into beaker B and stirred magnetically for 6 hours rapidly.
(5) 2mL of the mixed solution was poured into a 30mm 20X 10 alumina square boat and placed on a 50X 20 copper block that had been pre-cooled with liquid nitrogen. After being completely frozen, the mixture is placed in a freeze dryer for drying.
(6) Placing the dried sample in a tube furnace, introducing nitrogen for 20 minutes, and setting the temperature interval as follows: the temperature is firstly preserved for one hour at 300 ℃, and then the temperature is raised to 800 ℃ and preserved for one hour. The heating rate was 5 ℃/min. And then the battery assembly is carried out. The electrolyte is zinc trifluoromethanesulfonate.
Claims (10)
1. A method for preparing a piezoelectric flexible self-powered sensor cell, the method comprising:
s101, adding graphene oxide into deionized water, and stirring and oscillating to form a graphene oxide suspension;
s102, adding an MXene solution with a certain mass fraction into the graphene oxide suspension, uniformly stirring, adding glucose with a certain mass fraction, stirring and vibrating until the MXene solution is completely dissolved;
s103, adding the cellulose suspension with a certain mass fraction into deionized water, and stirring until the cellulose suspension is completely dissolved to obtain a cellulose solution;
s104, mixing and stirring the solution obtained in the step S103 and the solution obtained in the step S102 to obtain a mixed solution;
s105, pouring the mixed solution into a prefabricated container, performing directional freezing through liquid nitrogen, and then drying in a freeze dryer to obtain a dried sample;
s106, putting the dried sample into a tube furnace, introducing nitrogen, keeping the sample at 300 ℃ for one hour, heating to 600-800 ℃ and keeping for one hour to obtain a finished product;
and S107, assembling the battery by using the finished product.
2. The method for preparing a piezoelectric flexible self-powered sensor battery as claimed in claim 1, wherein the certain mass fraction of MXene solution is 0.2% -0.35% of MXene solution, and the certain mass fraction of cellulose suspension is 2% -3% of cellulose suspension.
3. The method for preparing the piezoelectric flexible self-powered sensor battery as claimed in claim 2, wherein in the mixed solution, the mass fraction of graphene oxide is 0.5% -0.83%, the mass fraction of MXene is 0.08% -0.125%, the mass fraction of glucose is 0.8% -1.25%, and the mass fraction of cellulose is 0.8% -1.25%.
4. The method for manufacturing a piezoelectric flexible self-powered sensor cell as claimed in claim 1, wherein the graphene oxide in the step S101 is synthesized by:
mixing concentrated sulfuric acid and phosphoric acid according to the proportion of 180;
slowly adding a certain amount of potassium permanganate into the container, and placing the container in a water bath kettle for magnetic stirring;
slowly adding hydrogen peroxide solution with a certain mass fraction into the container for multiple times until no bubbles are generated;
and when the preset reaction time is up, taking the container out of the water bath, slowly adding deionized water for many times for natural sedimentation, and taking out the precipitate in the container for freeze drying when the pH value of the supernatant is 6 to 7 to obtain the graphene oxide.
5. The method for preparing a piezoelectric flexible self-powered sensor battery as claimed in claim 4, wherein the temperature of the water bath is 50 ℃, the stirring time is 6 hours, the mass fraction of the hydrogen peroxide solution is 15%, and the amount of the hydrogen peroxide solution added each time is 3.5 ml.
6. The method of making a piezoelectric flexible self-powered sensor cell as defined in claim 1 wherein the cellulose solution comprises: cellulose nanofiber, high-pressure uniform medium nanofiber, tempo oxidation high-pressure uniform nanofiber, lignin, CNF-P, CNF-C, cellulose nanocrystal and hydroxypropyl methyl cellulose.
7. The method of making a piezoelectric flexible self-powered sensor cell as in claim 1, wherein the heating rate to 600 to 800 degrees celsius is 5 degrees celsius per minute.
8. The method of making a piezoelectric flexible self-powered sensor cell as in claim 1, wherein the MXene solution is prepared by:
etching the Max phase of the titanium aluminum carbide by using hydrochloric acid for 48 hours to obtain a sample;
cleaning the sample and performing ultrasonic oscillation to obtain MXene; the surface of the MXene at least comprises an oxygen functional group, a hydroxide functional group and a fluorine functional group;
preparing MXene solution by using the MXene.
9. A method of making a piezoelectric flexible self-powered sensor cell as in claim 1 wherein the preformed container is an alumina container.
10. The method for manufacturing a piezoelectric flexible self-powered sensor cell as claimed in claim 1, wherein in step S107, the electrolyte is zinc trifluoromethanesulfonate during cell assembly.
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