CN113101877A - Preparation method of MXene-based composite aerogel - Google Patents
Preparation method of MXene-based composite aerogel Download PDFInfo
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- CN113101877A CN113101877A CN202110368464.8A CN202110368464A CN113101877A CN 113101877 A CN113101877 A CN 113101877A CN 202110368464 A CN202110368464 A CN 202110368464A CN 113101877 A CN113101877 A CN 113101877A
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Abstract
The invention discloses a preparation method of MXene-based composite aerogel, which comprises the following steps: adding MXene into deionized water, and performing ultrasonic treatment and stirring to obtain MXene dispersion liquid; adding the functionalized nano-cellulose crystals into MXene dispersion liquid, stirring, performing molecular self-assembly, adding polyurethane, continuously stirring, performing chemical crosslinking, freezing by liquid nitrogen after the reaction is finished, and volatilizing ice crystals to obtain MXene-based composite aerogel; the method comprises the steps of taking functionalized nano-cellulose crystals as an assembling agent and a template, carrying out phase separation and self-assembly with MXene two-dimensional nanosheets, then carrying out chemical crosslinking reaction with waterborne polyurethane, and then carrying out directional freeze drying operation to obtain the MXene-based composite aerogel material with a three-dimensional directional internal pore channel structure, wherein the MXene-based composite aerogel material not only has super-elastic mechanical properties, but also has excellent electrochemical properties.
Description
Technical Field
The invention relates to the field of functional polymer aerogel materials, in particular to a preparation method of MXene-based composite aerogel.
Background
With the continuous progress of human society and the rapid development of industry, the worldwide demand for energy sources presents an explosive demand situation. However, traditional fossil fuel storage is limited and increasingly exhausted; meanwhile, a large amount of fossil fuels generate a large amount of greenhouse gases and toxic substances, such as carbon dioxide, carbon monoxide, volatile organic compounds and the like, during the combustion process, so that the global environment is irreversibly polluted and the climate is deteriorated, which has a great influence on human survival. Consequently, researchers are beginning to seek sustainable and renewable clean energy sources. Among them, electrochemical energy storage has been widely paid attention to by researchers as an important research direction in new energy technology. The super capacitor is an energy storage device for storing energy through surface ion adsorption or surface Faraday reaction, has high power density, long cycle life and high charging and discharging speed, and is widely applied to the fields of automobiles, energy storage power stations, aerospace and the like. The key material influencing the performance of the super capacitor is an electrode material, so that development of a structural electrode with high specific surface area, high capacitance and excellent mechanical properties is always the key point of scientific researchers.
In recent years, a new two-dimensional transition metal carbide or nitride (MXene) has received much attention from researchers. Compared with the traditional carbon material electrode, MXene has pseudo-capacitance characteristics due to surface functional groups introduced by etching, such as-OH, -F, -O and the like, so that the electrode has better electrochemical performance. In particular, MXene has excellent properties of electrical conductivity, hydrophilicity, abundant surface functional groups, high density, etc., making it a new generation of energy storage materials. However, as with other two-dimensional nanomaterials, MXene electrode reaction mostly occurs on the MXene surface and an interface constructed by the surface, and the electrochemical performance is limited by a severe lamellar stacking phenomenon, so that the MXene electrode reaction is far from the theory. Therefore, how to regulate and optimize the surface and structure of MXene, inhibit the stacking of MXene and construct MXene-based electrode materials with excellent electrochemical performance is the key. The stacked two-dimensional MXene material can be converted into a three-dimensional structure by a template method, freezing, intercalation and other methods, the stacking of the sheet layer can be effectively inhibited, the specific surface area is increased, and the electrochemical performance of the MXene electrode is improved. The aerogel is a kind of ultra-light material with a three-dimensional framework porous structure constructed by a freezing template method, and the aerogel can be used as an excellent electrode material due to the huge specific surface area and the porous channel structure.
To date, few reports have been made of the ability to synthesize MXene aerogels by gelation (e.g., ionic crosslinking, polymer crosslinking) and freeze templating. The most adopted method at present is to use graphene to promote gelation of MXene or composite polymer template material to directionally freeze-dry to construct a high-performance MXene-based aerogel material. However, the MXene aerogel has poor mechanical stability and an irregular three-dimensional pore channel structure, so that the MXene aerogel has poor structural durability. In addition, template-assisted techniques are used to build MXene composite aerogels, the presence of large amounts of templating agent (typically >20 wt%) severely reduces their conductivity, resulting in poor electrochemical performance. Since MXene is a rigid 2D sheet material, it remains a challenge to construct porous three-dimensional MXene aerogels with excellent mechanical properties combined with excellent electrochemical functionality.
Disclosure of Invention
The invention aims to provide a preparation method of MXene-based composite aerogel, and aims to solve the problems that the MXene-based composite aerogel prepared in the prior art has poor mechanical stability and poor electrochemical performance.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a preparation method of MXene-based composite aerogel, which comprises the following steps:
adding MXene into deionized water, and performing ultrasonic treatment and stirring to obtain MXene dispersion liquid;
adding the functionalized nano-cellulose crystal into MXene dispersion liquid, stirring, performing molecular self-assembly, adding polyurethane, continuously stirring, performing chemical crosslinking, freezing by liquid nitrogen after the reaction is finished, and volatilizing ice crystals to obtain the MXene-based composite aerogel.
Further, the mass-to-volume ratio of MXene, functionalized nanocellulose crystal, polyurethane and deionized water is 1:0.075:0.075:200 (g/g/g/mL).
Further, the time of chemical crosslinking reaction is 10-16 h; the freezing speed of the liquid nitrogen is 5-15 ℃/min; the process of volatilizing the ice crystals is carried out in a vacuum freeze dryer.
Further, the preparation method of MXene comprises the following steps: and (2) adding lithium fluoride into hydrochloric acid, stirring and mixing, adding the precursor MAX, continuously stirring and reacting, and after the reaction is finished, performing ultrasonic treatment and centrifugation to obtain an upper-layer suspension, and performing freeze drying to obtain MXene.
Further, the mass-to-volume ratio of lithium fluoride, MAX and hydrochloric acid is 1:1:20 (g/g/mL).
Further, the reaction temperature is 35 ℃ after the precursor MAX is added, and the reaction time is 24-48 h.
Further, the preparation method of the functionalized nano-cellulose crystal comprises the following steps: placing the nano-cellulose crystals into deionized water, stirring and performing ultrasonic treatment to obtain nano-cellulose crystal dispersion liquid;
adding a silane coupling agent into the nano-cellulose crystal dispersion liquid, adjusting the pH value, then placing the nano-cellulose crystal dispersion liquid into a hydrothermal kettle for hydrothermal reaction, centrifuging after the reaction is finished, taking the lower layer precipitate, washing and drying to obtain the functionalized nano-cellulose crystal.
Further, the mass-to-volume ratio of the nano-cellulose crystal, the deionized water and the silane coupling agent is 3:50:1(g/mL/mL), and the silane coupling agent is a perfluorosilane coupling agent.
Further, acetic acid is used for adjusting the pH value, and the pH value is adjusted to be 5; the temperature of the hydrothermal reaction is 80 ℃ and the time is 12 h.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the MXene-based composite aerogel provided by the invention comprises the steps of taking functionalized nano-cellulose crystals as an assembling agent and a template, carrying out phase separation and self-assembly with MXene two-dimensional nanosheets, then carrying out chemical crosslinking reaction with waterborne polyurethane, and then carrying out directional freeze-drying operation to obtain an MXene-based composite aerogel material with a three-dimensional directional internal pore channel structure, wherein the MXene-based composite aerogel material not only has super-elastic mechanical properties, but also has excellent electrochemical properties, so that the application field of MXene is further widened, and simultaneously, the MXene-based composite aerogel material also conforms to the concept of sustainable development of modern new energy sources;
according to the preparation method of the MXene-based composite aerogel, the content of MXene in the prepared MXene-based composite aerogel is high and can reach 85%, and compared with the traditional hybrid MXene aerogel, the MXene-based composite aerogel prepared by the invention can effectively inhibit stacking of MXene nano sheets, so that the electrochemical performance of the MXene-based composite aerogel is greatly improved;
according to the preparation method of the MXene-based composite aerogel, the prepared MXene-based composite aerogel has a directional pore channel structure inside and a divergent network structure on the surface, and test results show that the MXene-based composite aerogel can still show good compression recovery capacity after being circularly compressed for 100 times at 0 ℃, 80 ℃ and 150 ℃, and the recovery rate after being compressed for 100 times reaches more than 70%; in addition, the MXene-based composite aerogel has excellent energy storage performance, shows excellent mass specific capacitance of 225F/g (2mV/s sweep rate) when being used as a supercapacitor electrode, and can be applied to the field of supercapacitors.
Drawings
FIG. 1 is a compression rebound curve of MXene-based composite aerogel prepared in example 2 of the present invention at 0 ℃;
FIG. 2 is a compression rebound curve of MXene-based composite aerogel prepared in example 2 of the present invention at 80 ℃;
FIG. 3 is a compression rebound curve of MXene-based composite aerogel prepared in example 2 of the present invention at 150 ℃;
FIG. 4 is a cyclic voltammetry curve of MXene-based composite aerogel prepared in example 2 of the present invention;
FIG. 5 is a charging/discharging curve of MXene-based composite aerogel prepared in example 2 of the present invention;
fig. 6 is a mass specific capacitance curve of the MXene-based composite aerogel prepared in example 2 of the present invention at different sweeping speeds.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a preparation method of MXene-based composite aerogel comprises the following steps:
adding 1g of lithium fluoride into 20mL of hydrochloric acid (the concentration of the hydrochloric acid is 9mol/L), stirring for 30min, mixing, adding 1g of precursor MAX, continuously stirring and reacting at the temperature of 35 ℃ for 24h, performing ultrasonic treatment and centrifugation after the reaction is finished, wherein the centrifugation speed is 6000rpm, taking the upper-layer suspension, and performing freeze drying to obtain MXene;
putting 3g of nano-cellulose crystal into 50mL of deionized water, stirring for 6h, and carrying out ultrasonic treatment for 10min to obtain nano-cellulose crystal dispersion liquid;
adding 1mL of perfluorosilane coupling agent into the nano-cellulose crystal dispersion liquid, dropwise adding acetic acid to adjust the pH value to 5, then placing the mixture into a hydrothermal kettle to perform hydrothermal reaction at the temperature of 80 ℃ for 12 hours, centrifuging the mixture after the reaction is finished at the centrifugal speed of 8000rpm, taking the lower-layer precipitate, washing the precipitate for multiple times until the incompletely reacted perfluorosilane coupling agent is removed, and drying the precipitate to obtain the functionalized nano-cellulose crystal;
adding 0.5g of MXene into 100mL of deionized water, and carrying out ultrasonic treatment for 1h and stirring for 6h to obtain MXene dispersion liquid;
adding 0.0375g of functionalized nano-cellulose crystal into MXene dispersion liquid, stirring, performing molecular self-assembly, adding 0.0375g of polyurethane, continuously stirring, performing chemical crosslinking, wherein the chemical crosslinking reaction time is 10h, freezing by liquid nitrogen after the reaction is finished, the freezing speed of the liquid nitrogen is 5 ℃/min, volatilizing ice crystals to obtain the MXene-based composite aerogel, and volatilizing the ice crystals in a vacuum freeze dryer.
Example 2:
preparing MXene-based composite aerogel according to the method of the embodiment 1, except that 1g of precursor MAX is added, continuously stirring and reacting for 36 h; the time of the chemical crosslinking reaction is 13 h; the rate of liquid nitrogen freezing was 10 deg.C/min.
Example 3:
preparing MXene-based composite aerogel according to the method of the embodiment 1, except that 1g of precursor MAX is added, continuously stirring and reacting for 48 hours; the time of the chemical crosslinking reaction is 16 h; the rate of liquid nitrogen freezing was 15 deg.C/min.
The compression properties of the MXene-based composite aerogels obtained in examples 1 to 3 were tested, and the results are shown in table 1.
TABLE 1 compression Properties of MXene-based composite aerogels obtained in examples 1 to 3
As can be seen from table 1, the MXene-based composite aerogels prepared in examples 1 to 3 all have good compression resilience, and the recovery rate after 100 times of compression is over 70%.
Fig. 1 is a compression rebound curve of the MXene-based composite aerogel prepared in example 2 at 0 ℃, fig. 2 is a compression rebound curve of the MXene-based composite aerogel prepared in example 2 at 80 ℃, fig. 3 is a compression rebound curve of the MXene-based composite aerogel prepared in example 2 at 150 ℃, as can be seen from fig. 1 to fig. 3, the MXene-based composite aerogel prepared in example 2 can be circularly compressed for 100 times at 0 ℃, 80 ℃ and 150 ℃, and still can show better compression recovery capability, and experimental results show that the stability of the MXene-based composite aerogel prepared in example 2 has excellent temperature-resistant super-elastic characteristics.
Fig. 4 is a cyclic voltammetry curve of the MXene-based composite aerogel prepared in example 2, fig. 5 is a charging and discharging curve of the MXene-based composite aerogel prepared in example 2, as can be seen from fig. 4, the MXene-based composite aerogel prepared in example 2 has a good pseudocapacitance characteristic, as can be seen from fig. 5, the MXene-based composite aerogel prepared in example 2 has a fast charging and discharging characteristic, and an experimental result shows that the MXene-based composite aerogel prepared in example 2 can be used as a new generation of supercapacitor electrode material.
Fig. 6 is a mass specific capacitance curve of the MXene-based composite aerogel prepared in example 2 at different sweeping speeds, and it can be seen from fig. 6 that the mass specific capacitance of the MXene-based composite aerogel prepared in example 2 is much higher than that of the MXene film of the control group, and at a sweeping speed of 2mv/s, the mass specific capacitance of the MXene-based composite aerogel prepared in example 2 can reach 225F/g, at this time, the rate capability is very high, and the experimental result shows that the MXene-based composite aerogel prepared in example 2 has excellent mechanical stability and electrochemical performance.
The invention provides a preparation method of MXene-based composite aerogel, which comprises the steps of taking functionalized nano-cellulose crystals as an assembling agent and a template, carrying out phase separation and self-assembly with MXene two-dimensional nanosheets, then carrying out chemical crosslinking reaction with waterborne polyurethane, and then carrying out directional freeze-drying operation to obtain an MXene-based composite aerogel material with a three-dimensional directional internal pore channel structure.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (9)
1. The preparation method of the MXene-based composite aerogel is characterized by comprising the following steps: adding MXene into deionized water, and performing ultrasonic treatment and stirring to obtain MXene dispersion liquid;
adding the functionalized nano-cellulose crystal into MXene dispersion liquid, stirring, performing molecular self-assembly, adding polyurethane, continuously stirring, performing chemical crosslinking, freezing by liquid nitrogen after the reaction is finished, and volatilizing ice crystals to obtain the MXene-based composite aerogel.
2. The preparation method of the MXene-based composite aerogel according to claim 1, wherein the preparation method comprises the following steps: the mass-volume ratio of the MXene, the functionalized nano-cellulose crystal, the polyurethane and the deionized water is 1:0.075:0.075:200 (g/g/g/mL).
3. The preparation method of the MXene-based composite aerogel according to claim 1, wherein the preparation method comprises the following steps: the time of the chemical crosslinking reaction is 10-16 h; the freezing speed of the liquid nitrogen is 5-15 ℃/min; the volatilization process of the ice crystals is carried out in a vacuum freeze dryer.
4. The preparation method of the MXene-based composite aerogel according to claim 1, wherein the preparation method of the MXene comprises the following steps: and (2) adding lithium fluoride into hydrochloric acid, stirring and mixing, adding the precursor MAX, continuously stirring and reacting, and after the reaction is finished, performing ultrasonic treatment and centrifugation to obtain an upper-layer suspension, and performing freeze drying to obtain MXene.
5. The preparation method of the MXene-based composite aerogel according to claim 4, wherein the preparation method comprises the following steps: the mass-to-volume ratio of the lithium fluoride to the MAX to the hydrochloric acid is 1:1:20 (g/g/mL).
6. The preparation method of the MXene-based composite aerogel according to claim 4, wherein the preparation method comprises the following steps: the temperature of the reaction is 35 ℃ after the precursor MAX is added, and the reaction time is 24-48 h.
7. The preparation method of the MXene-based composite aerogel according to claim 1, wherein the preparation method of the functionalized nanocellulose crystal comprises: placing the nano-cellulose crystals into deionized water, stirring and performing ultrasonic treatment to obtain nano-cellulose crystal dispersion liquid;
adding a silane coupling agent into the nano-cellulose crystal dispersion liquid, adjusting the pH value, then placing the nano-cellulose crystal dispersion liquid into a hydrothermal kettle for hydrothermal reaction, centrifuging after the reaction is finished, taking the lower layer precipitate, washing and drying to obtain the functionalized nano-cellulose crystal.
8. The method for preparing MXene-based composite aerogel according to claim 7, wherein the method comprises the following steps: the mass-to-volume ratio of the nano-cellulose crystal, the deionized water and the silane coupling agent is 3:50:1(g/mL/mL), and the silane coupling agent is a perfluorinated silane coupling agent.
9. The method for preparing MXene-based composite aerogel according to claim 7, wherein the method comprises the following steps: the pH value is adjusted by using acetic acid, and the pH value is 5; the temperature of the hydrothermal reaction is 80 ℃, and the time is 12 h.
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