CN109742405B - Aperture-adjustable flexible electrode material and preparation method and application thereof - Google Patents
Aperture-adjustable flexible electrode material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a flexible electrode material with an adjustable aperture, which is a dual-network carbon structure, wherein the dual-network carbon structure comprises a primary porous network carbon skeleton, a secondary porous network carbon skeleton is filled in pores of the primary porous network carbon skeleton, and the aperture of the flexible electrode material is 10-1500 nm. The invention also correspondingly provides a preparation method and application of the aperture-adjustable flexible electrode material. The flexible electrode material has a double-network structure, can easily realize the adjustment of the pore size of the flexible electrode material, and provides a good foundation for further loading other high-activity substances on the electrode material. In addition, the flexible electrode material has excellent flexible folding capability, elastic performance and electrochemical performance.
Description
Technical Field
The invention belongs to the field of high-molecular functional materials, and particularly relates to a flexible electrode material and a preparation method and application thereof.
Background
In the modern society, as the updating speed of electronic products is increasing, flexible and bendable energy storage devices become hot spots for scientific research, and have the advantages of light weight, bending deformation, good stability and the like, and are gradually applied to the fields of foldable electronic equipment, aerospace, portable devices and the like. The current collector of the traditional battery is generally made of materials with higher strength, such as copper foil, aluminum foil and the like, and the active energy storage substances coated on the materials are easy to fall off and separate when the battery is bent, so that the electrochemical stability of the battery is influenced, and the current collector is not suitable for flexible batteries. Flexible batteries require that all materials in the battery be flexible and bendable, including electrode and separator materials, and also ensure that the flexible battery has excellent electrochemical performance and cycling stability.
In order to meet the special requirements of flexible batteries, new materials must be found or improvements must be made to the current materials to achieve flexible and foldable performance. At present, some flexible electrode materials are obtained by preparing composite films from materials such as graphene, carbon nanotubes and manganese dioxide through methods such as suction filtration and film formation, but the flexible electrode materials have some problems: (1) the flexible electrode material is easy to break after being bent and deformed for many times, and has great influence on the overall performance of the battery; (2) the pore size and dimension inside the flexible electrode material cannot be effectively controlled, and other high-efficiency active substance materials cannot be loaded inside the material. Therefore, the development of the flexible electrode material with adjustable aperture is of great significance to the development of flexible batteries.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background art, and provide a flexible electrode material with a multiple network structure and adjustable aperture, and a preparation method and application thereof. In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the utility model provides a flexible electrode material of aperture adjustable, flexible electrode material is dual network carbon structure, and dual network carbon structure includes one-level porous network carbon skeleton, it has second grade porous network carbon skeleton still to pack in the hole of one-level porous network carbon skeleton, flexible electrode material's aperture size is 10~ 1500 nm.
In the electrode material, preferably, the first-stage porous network carbon skeleton is formed by carbonizing melamine sponge, the aperture of the melamine sponge is 50-100 μm, and the second-stage porous network carbon skeleton is formed by carbonizing nano cellulose filled in the pores of the melamine sponge.
As a general technical concept, the present invention also provides a preparation method of the above aperture-adjustable flexible electrode material, comprising the following steps:
(1) immersing melamine sponge into the nano-cellulose solution, and extruding the melamine sponge for multiple times to obtain a nano-cellulose/melamine sponge composite material;
(2) freezing and vacuum drying the nano-cellulose/melamine sponge composite material obtained in the step (2) to obtain a nano-cellulose/melamine sponge base material;
(3) and (3) carrying out high-temperature carbonization treatment on the nano-cellulose/melamine sponge base material obtained in the step (2) in an inert atmosphere to obtain the flexible electrode material.
In the above preparation method, preferably, in the step (1), the preparation method of the nanocellulose solution includes the steps of: and (3) taking the nano-cellulose sol, preparing a nano-cellulose solution through ultrapure water, and then carrying out ultrasonic crushing in an ultrasonic crusher for 1-7 min to obtain the uniformly mixed nano-cellulose solution.
In the preparation method, preferably, in the step (1), the thickness of the melamine sponge is controlled to be 3-10 mm. Wherein, the thickness of melamine sponge is controlled to be 3-10 mm, so that the nano-cellulose can enter the interior of the melamine sponge conveniently.
In the preparation method, preferably, the mass fraction of the nano-cellulose solution is controlled to be 0.1-0.5%, and the pore size inside the flexible electrode material is 300-1500 nm; or the mass fraction of the nano-cellulose solution is controlled to be 0.5-1.0%, and the pore size inside the flexible electrode material is 10-300 nm. The mass concentration of the nano-cellulose has great influence on the aperture and the electrochemical performance of the flexible electrode material, the electrochemical performance of the material can be influenced if the mass fraction of the nano-cellulose solution is too low, the mass fraction is too high, the nano-cellulose is too viscous, and the nano-cellulose is difficult to enter the interior of the melamine sponge in the subsequent steps.
In the preparation method, preferably, the mass fraction of the nano-cellulose solution is controlled to be 0.85-1.0%, and the pore size inside the flexible electrode material is 10-80 nm. The mesoporous in the electrode material is important for the influence of the electrochemical performance of the carbon material, and for the flexible electrode material, when the mass fraction of the nanocellulose solution is controlled to be 0.85-1.0%, the content of mesoporous (2-50 nm) in pores in the electrode material is high, so that the electrochemical performance of the electrode material can be well improved.
In the preparation method, in the step (2), the freezing temperature is-50 to-30 ℃ and the freezing time is 5 to 9 hours during freezing and vacuum drying treatment, and the vacuum drying treatment is performed for 5 to 9 hours at the temperature of-40 to-20 ℃ and then for 12 to 24 hours at room temperature.
In the preparation method, preferably, the carbonization temperature is controlled to be 700-1000 ℃ during the high-temperature carbonization treatment. By carrying out thermal decomposition treatment on the nano-cellulose/melamine sponge base material in the temperature range, the nano-cellulose and the melamine sponge can be thermally decomposed into carbon materials, and the supercapacitor electrode material with flexibility, good conductivity and porosity is obtained. If the temperature is lower than the temperature, the obtained nano-cellulose/sponge composite matrix material is weakened in electrical conductivity and energy storage performance because the nano-cellulose/sponge composite matrix material cannot be completely carbonized; if the temperature is higher than the temperature, the nano-cellulose/sponge composite matrix material can be partially graphitized, so that the whole material becomes brittle and the flexible and bendable capacity of the composite matrix material is reduced.
In the preparation method, the process parameters of freezing, vacuum drying and high-temperature carbonization have great influence on the performance of the flexible electrode material, and the electrode material with high comprehensive performance can be obtained by controlling the process parameters.
As a general technical concept, the present invention further provides an application of the above flexible electrode material, wherein the flexible electrode material is used for loading a high activity substance to obtain a high activity electrode material, the high activity substance includes a metal, a metal oxide or a high molecular polymer (such as polyaniline), and the loading amount of the high activity substance is not less than 7% (i.e., after loading, the amount of the high activity substance accounts for not less than 7% of the total mass of the electrode). By regulating the aperture of the electrode material substrate, active substances with different sizes can be compounded or grown on the electrode material. When the aperture is small, polymer materials such as polyaniline and the like can be loaded, and when the aperture is large, metals, oxides and other materials with slightly large size can be adsorbed, so that the efficient adsorption and utilization of different active material materials by different apertures can be realized.
The nano-cellulose is a degradable pollution-free high polymer material obtained by nano-technology from cellulose in the nature, has strong renewable capability and excellent biodegradability, has strong chemical reaction activity due to large specific surface area and increased small-size effect, and still retains the properties after carbonization. The melamine sponge is a novel foam with a three-dimensional network structure with high aperture ratio, has special properties such as excellent elasticity, flexibility and high specific surface area, can be applied to numerous fields such as aviation, electromechanics and electronic products, and has wide market prospect. The nanocellulose is implanted into the melamine sponge in an extrusion adsorption mode, the nanocellulose is stabilized in the melamine through acting forces such as hydrogen bonds, van der waals force and the like to form a nanocellulose network structure, and the pore diameter in the composite material can be effectively regulated and controlled by controlling the mass fraction of the nanocellulose, so that the integrated nanoelectrode material with a dual network structure, adjustable pore diameter and excellent flexibility is obtained.
Compared with the prior art, the invention has the advantages that:
1. the flexible electrode material has a double-network structure, the nanocellulose is adsorbed in the melamine sponge, the nanocellulose network structure is constructed in the original network structure in the sponge, the network structure and the pore size of the nanocellulose in the sponge are regulated and controlled by controlling the concentration of the nanocellulose, the adjustment of the pore size of the flexible electrode material can be easily realized, and a good foundation is provided for further loading other high-activity substances for the electrode material.
2. According to the invention, the melamine sponge is used as a skeleton structure of the composite carbon material, the elasticity and flexibility of the carbon material subjected to high-temperature thermal decomposition are not damaged, and the melamine sponge still has excellent mechanical properties, so that the flexible electrode material has flexible and foldable capacity and excellent elastic properties.
3. The flexible electrode material disclosed by the invention has excellent electrochemical performance, the nano-cellulose carbon material is filled in the melamine sponge, the contact area between the electrode material and electrolyte is increased, and the internal conductivity can be improved by the mutual contact between carbon material frameworks, so that the electrochemical performance of the electrode material is more excellent. At a current density of 1A g-1The specific capacitance can reach 157.0 F.g at most-1The specific capacitance is improved by about 4 times compared with that of the melamine sponge carbon material, and the resistance value is very low, about 0.8 omega.
4. The preparation method disclosed by the invention is simple to operate, strong in controllability, wide in source of the raw plant fiber, low in cost and capable of meeting the strategic goal of green sustainable development.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a physical diagram of the flexible electrode material in example 1.
Fig. 2 is an electron micrograph of the microstructures of the flexible electrode materials prepared in example 3, comparative example 2, and example 4 (b, c, d correspond to example 3, comparative example 2, and example 4, respectively).
Fig. 3 is a flexible and foldable performance test chart of the flexible electrode material prepared in example 3.
FIG. 4 is a cyclic voltammetry test chart of the flexible electrode materials prepared in examples 1-4 and comparative example 1.
FIG. 5 shows MnO adsorption of the flexible electrode materials prepared in example 2 and comparative example 12Comparative figures for particles (a, b correspond to example 2 and comparative example 1, respectively).
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the utility model provides a flexible electrode material of aperture adjustable, this flexible electrode material is dual network carbon structure, and dual network carbon structure includes one-level porous network carbon skeleton, still packs in the hole of one-level porous network carbon skeleton and has second grade porous network carbon skeleton. The primary porous network carbon skeleton is formed by carbonizing melamine sponge, and the secondary porous network carbon skeleton is formed by carbonizing nano cellulose filled in pores of the melamine sponge. The aperture size of the flexible electrode material in this embodiment is about 500-1000 nm.
The preparation method of the aperture-adjustable flexible electrode material comprises the following steps:
(1) taking the nano-cellulose sol, blending the nano-cellulose solution with ultrapure water to obtain 0.1% by mass of the nano-cellulose solution, and then carrying out ultrasonic crushing for 5min in an ultrasonic crushing instrument to obtain the uniformly mixed nano-cellulose solution;
(2) the melamine sponge is sliced to obtain a melamine sponge sheet with the thickness of 7 mm;
(3) putting the melamine sponge sheet in the step (2) into the nano-cellulose solution prepared in the step (1), and extruding the sponge matrix for multiple times to enable nano-cellulose to enter the interior of the sponge, so as to obtain a nano-cellulose/melamine sponge composite material;
(4) placing the nano-cellulose/melamine sponge composite material obtained in the step (3) in a freeze dryer at-30 ℃ for freezing for 5h, then carrying out vacuum drying at-30 ℃ for 5h, and finally carrying out vacuum drying at room temperature for 12h to obtain a nano-cellulose/melamine sponge base material;
(5) and (4) placing the nano-cellulose/melamine sponge base material obtained in the step (4) in a tube furnace, introducing inert gas, performing high-temperature thermal decomposition treatment at 700 ℃, and obtaining the flexible electrode material with adjustable aperture after carbonization.
Fig. 1 is a real image of the flexible electrode material prepared in this example. As can be seen from the figure, the flexible electrode material has a regular shape and is easy to assemble into a super capacitor as an electrode material.
Example 2:
the utility model provides a flexible electrode material of aperture adjustable, this flexible electrode material is dual network carbon structure, and dual network carbon structure includes one-level porous network carbon skeleton, still packs in the hole of one-level porous network carbon skeleton and has second grade porous network carbon skeleton. The primary porous network carbon skeleton is formed by carbonizing melamine sponge, and the secondary porous network carbon skeleton is formed by carbonizing nano cellulose filled in pores of the melamine sponge. The aperture size of the flexible electrode material in this embodiment is about 20 to 300 nm.
The preparation method of the aperture-adjustable flexible electrode material comprises the following steps:
(1) taking the nano-cellulose sol, blending the nano-cellulose solution with ultrapure water to obtain 0.5% by mass of the nano-cellulose solution, and then carrying out ultrasonic crushing in an ultrasonic crusher for 3min to obtain the uniformly mixed nano-cellulose solution;
(2) the melamine sponge is sliced to obtain melamine sponge slices with the thickness of 5 mm;
(3) putting the melamine sponge sheet in the step (2) into the nano-cellulose solution prepared in the step (1), and extruding the sponge matrix for multiple times to enable nano-cellulose to enter the interior of the sponge, so as to obtain a nano-cellulose/melamine sponge composite material;
(4) placing the nano-cellulose/melamine sponge composite material obtained in the step (3) in a freeze dryer at-40 ℃ for freezing for 7h, then carrying out vacuum drying at-40 ℃ for 7h, and finally carrying out vacuum drying at room temperature for 18h to obtain a nano-cellulose/melamine sponge base material;
(5) and (4) placing the nano-cellulose/melamine sponge base material obtained in the step (4) in a tube furnace, introducing inert gas, performing high-temperature thermal decomposition treatment at 800 ℃, and carbonizing to obtain the flexible electrode material with adjustable aperture.
Example 3:
the utility model provides a flexible electrode material of aperture adjustable, this flexible electrode material is dual network carbon structure, and dual network carbon structure includes one-level porous network carbon skeleton, still packs in the hole of one-level porous network carbon skeleton and has second grade porous network carbon skeleton. The primary porous network carbon skeleton is formed by carbonizing melamine sponge, and the secondary porous network carbon skeleton is formed by carbonizing nano cellulose filled in pores of the melamine sponge. The aperture size of the flexible electrode material in this embodiment is about 20 to 200 nm.
The preparation method of the aperture-adjustable flexible electrode material comprises the following steps:
(1) taking the nano-cellulose sol, blending the nano-cellulose solution with ultrapure water to obtain 0.8% by mass of the nano-cellulose solution, and then carrying out ultrasonic crushing in an ultrasonic crusher for 7min to obtain the uniformly mixed nano-cellulose solution;
(2) the melamine sponge is sliced to obtain a melamine sponge sheet with the thickness of 3 mm;
(3) putting the melamine sponge sheet in the step (2) into the nano-cellulose solution prepared in the step (1), and extruding the sponge matrix for multiple times to enable nano-cellulose to enter the interior of the sponge, so as to obtain a nano-cellulose/melamine sponge composite material;
(4) placing the nano-cellulose/melamine sponge composite material obtained in the step (3) in a freeze dryer at-50 ℃ for freezing for 9h, then carrying out vacuum drying at-40 ℃ for 9h, and finally carrying out vacuum drying at room temperature for 24h to obtain a nano-cellulose/melamine sponge base material;
(5) and (3) placing the nano-cellulose/melamine sponge base material obtained in the step (4) in a tubular furnace, introducing inert gas, performing high-temperature thermal decomposition treatment at 1000 ℃, and carbonizing to obtain the flexible electrode material with adjustable aperture.
Fig. 2(b) is an electron microscope image of the microstructure of the flexible electrode material prepared in the example. As can be seen from the figure, a lamellar structure formed by nano-cellulose is arranged in the sponge framework, and the lamellar structure and the sponge framework structure form a sponge-nano-fiber dual structure.
Fig. 3 is a flexible and foldable performance test chart of the flexible electrode material prepared in this embodiment. The left drawing is a drawing for folding the flexible electrode material, and the right drawing is an expansion drawing of the folded flexible electrode material, so that the electrode material has no influence on the form through folding-unfolding, and the form is not changed through multiple folding-unfolding, so that the electrode material can be used on the flexible supercapacitor electrode material.
Example 4:
the utility model provides a flexible electrode material of aperture adjustable, this flexible electrode material is dual network carbon structure, and dual network carbon structure includes one-level porous network carbon skeleton, still packs in the hole of one-level porous network carbon skeleton and has second grade porous network carbon skeleton. The primary porous network carbon skeleton is formed by carbonizing melamine sponge, and the secondary porous network carbon skeleton is formed by carbonizing nano cellulose filled in pores of the melamine sponge. The aperture size of the flexible electrode material in this embodiment is about 10-80 nm.
The preparation method of the aperture-adjustable flexible electrode material comprises the following steps:
(1) taking the nano-cellulose sol, blending the nano-cellulose solution with ultrapure water to obtain 0.9% by mass of the nano-cellulose solution, and then carrying out ultrasonic crushing in an ultrasonic crusher for 7min to obtain the uniformly mixed nano-cellulose solution;
(2) the melamine sponge is sliced to obtain melamine sponge slices with the thickness of 9 mm;
(3) putting the melamine sponge sheet in the step (2) into the nano-cellulose solution prepared in the step (1), and extruding the sponge matrix for multiple times to enable nano-cellulose to enter the interior of the sponge, so as to obtain a nano-cellulose/melamine sponge composite material;
(4) placing the nano-cellulose/melamine sponge composite material obtained in the step (3) in a freeze dryer at-50 ℃ for freezing for 9h, then carrying out vacuum drying at-40 ℃ for 9h, and finally carrying out vacuum drying at room temperature for 24h to obtain a nano-cellulose/melamine sponge base material;
(5) and (3) placing the nano-cellulose/melamine sponge base material obtained in the step (4) in a tubular furnace, introducing inert gas, performing high-temperature thermal decomposition treatment at 950 ℃, and carbonizing to obtain the flexible electrode material with adjustable aperture.
Fig. 2(d) is an electron microscope image of the microstructure of the flexible electrode material prepared in the example. As can be seen from the figure, a lamellar structure formed by nano-cellulose is arranged in the sponge framework, and the lamellar structure and the sponge framework structure form a sponge-nano-fiber dual structure.
Comparative example 1:
in the comparative example, the melamine sponge sheet in example 1 was directly subjected to freezing, vacuum drying and high-temperature thermal decomposition to obtain a flexible electrode material. The aperture size of the flexible electrode material is 50-100 mu m.
FIG. 4 is a cyclic voltammetry test chart of the flexible electrode materials prepared in examples 1-4 and comparative example 1, and it can be seen that the current density of the flexible electrode materials in examples 1-4 and comparative example 1 is 1A · g-1The electrochemical performance data is shown in the following table 1, and the specific capacitance of the flexible electrode material regulated and controlled by the nano-cellulose is superior to that of an unregulated melamine sponge substrate.
Table 1: specific capacitance comparison table of flexible electrode materials of examples 1-4 and comparative example 1
| Sample (I) | Specific capacitance |
| Comparative example 1 | 31.5F/g |
| Example 1 | 129.7F/g |
| Example 2 | 117.6F/g |
| Example 3 | 134.1F/g |
| Example 4 | 157.0F/g |
FIG. 5(a) shows MnO loading by hydrothermal method using the flexible electrode material prepared in example 22An electron micrograph after granulation, and FIG. 5(b) is a view showing that MnO was supported by a hydrothermal method using the flexible electrode material prepared in this comparative example2As is clear from the electron micrograph after the granulation, MnO supporting in example 22The amount of particles (> 7%) is significantly greater than the amount loaded in this comparative example (around 3%), and the advantage of the flexible electrode material in example 2 during further use is even more significant.
Comparative example 2:
this comparative example differs from example 1 only in that the mass fraction of nanocellulose is 1.3%. The aperture size of the flexible electrode material is about 40-80 μm.
Fig. 2(c) is an electron microscope image of the microstructure of the flexible electrode material prepared in this comparative example. It can be seen from the figure that when the concentration of the nanocellulose is 1.3%, the nanocellulose is difficult to enter the sponge, so that the purpose of regulating and controlling the internal pore size cannot be achieved.
Claims (6)
1. A preparation method of a flexible electrode material with adjustable aperture is characterized by comprising the following steps:
(1) immersing melamine sponge into the nano-cellulose solution, and extruding the melamine sponge for multiple times to obtain a nano-cellulose/melamine sponge composite material; the thickness of the melamine sponge is controlled to be 3-10 mm, and the mass fraction of the nano cellulose solution is controlled to be 0.1-1.0%;
(2) freezing and vacuum drying the nano-cellulose/melamine sponge composite material obtained in the step (1) to obtain a nano-cellulose/melamine sponge base material;
(3) carrying out high-temperature carbonization treatment on the nano-cellulose/melamine sponge base material obtained in the step (2) in an inert atmosphere to obtain a flexible electrode material; and during high-temperature carbonization treatment, the carbonization temperature is controlled to be 700-1000 ℃.
2. The method according to claim 1, wherein in the step (1), the method for preparing the nanocellulose solution comprises the steps of: and (3) taking the nano-cellulose sol, preparing a nano-cellulose solution through ultrapure water, and then carrying out ultrasonic crushing in an ultrasonic crusher for 1-7 min to obtain the uniformly mixed nano-cellulose solution.
3. The preparation method of claim 1, wherein the mass fraction of the nanocellulose solution is controlled to be 0.1-0.5%, and the pore size inside the flexible electrode material is 300-1500 nm; or the mass fraction of the nano-cellulose solution is controlled to be 0.5-1.0%, and the pore size inside the flexible electrode material is 10-300 nm.
4. The preparation method according to claim 3, wherein the mass fraction of the nanocellulose solution is controlled to be 0.85-1.0%, and the pore size inside the flexible electrode material is 10-80 nm.
5. The preparation method according to any one of claims 1 to 4, wherein in the step (2), the freezing temperature is-50 to-30 ℃ and the freezing time is 5 to 9 hours during freezing and vacuum drying, and the vacuum drying is performed for 5 to 9 hours at-40 to-20 ℃ and then for 12 to 24 hours at room temperature.
6. The application of the flexible electrode material obtained by the preparation method according to any one of claims 1 to 5, wherein a high-activity substance is loaded on the flexible electrode material to obtain a high-activity electrode material, the high-activity substance comprises a metal, a metal oxide or a high molecular polymer, and the loading amount of the high-activity substance is not less than 7%.
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