CN112103485A - Preparation method of 0D/2D quantum dot/graphene nanocolloid heterostructure electrode material - Google Patents
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Abstract
The invention discloses a preparation method of a 0D/2D quantum dot/graphene nano roll heterostructure electrode material, which comprises the following steps: preparing Mxene quantum dots (MXene-QDs); b. preparing black phosphorus quantum dots (BP-QDs); c. preparing a Graphene Oxide (GO) nano roll; and d.0D/2D quantum dot/graphene nano roll heterostructure electrode material is prepared. The preparation method is simple, and the electrode material obtained by the method can be used in a battery to remarkably improve the electrochemical performance of LIB, such as larger interface area.
Description
Technical Field
The invention belongs to the technical field of electrode material preparation, and particularly relates to a preparation method of a 0D/2D quantum dot/graphene nanocolloid heterostructure electrode material.
Background
In recent years, Lithium Ion Batteries (LIBs), one of the most effective and practical electrochemical energy storage technologies, have been widely used as a main power source for various electronic products such as computers, mobile phones, camcorders, and wearable devices. This makes LIBs an essential component in many energy saving applications and changes lifestyle. To apply/integrate it into hybrid vehicles and help ameliorate the intermittency problem of renewable energy sources (e.g., wind and waves), LIBs do notIt is only necessary that the capacity is large and it is also necessary to have excellent rate capability and high stability. However, the relatively low capacity (372mAh g) of the current commercial graphite anode electrode-1) And the weak Li adsorption strength and rapid capacity reduction under rapid charge/discharge conditions limit its further applications. Under such circumstances, it is highly desirable to develop alternative anode electrode materials for next-generation LIBs, which have higher capacity, faster charge/discharge speed, longer cycle stability, and mass production to replace graphite.
Notably, two-dimensional (2D) materials, in particular black phosphorus, transition metal carbides and nitrides (MXenes), have become an attractive platform for designing and preparing functionally enhanced functional materials for various applications. In particular, they have recently attracted extensive research interest on lithium ion batteries due to their excellent electrical conductivity, high lithium storage capacity and surface hydrophilicity. However, re-stacking the resulting nanoplatelets by van der waals interactions and/or hydrogen bonding during the lift-off/electrode preparation process significantly limits ion transport and electrolyte penetration as well as the full utilization of its functional surface, thus resulting in unsatisfactory electrochemical performance. Thus, it remains a challenge to obtain satisfactory electrodes for a single 2D material (e.g., black phosphorus, MXenes), as none of them provides all of the performance needed to maximize energy density, power density, and cycle life.
To address the above disadvantages, integrating these nanoplatelets with a substrate to build a heterostructure may be an effective strategy that can provide a variety of synergistic strengths, resulting in superior performance of the resulting material. Among these substrates, graphene is of great interest due to its unique physicochemical properties, which promote rapid electron transport and Li+Diffusion of ions, thereby remarkably improving electrochemical performance. In addition, a size minimization strategy (length is as small as a few nanometers, such as quantum dots) is adopted, and the method is an effective method for improving the electrochemical performance of the electrode material due to the reduction of ion diffusion distance, the increase of active sites, and the large contact area between the electrode and the electrolyte, so that the electrode material is provided with the electrode materialThe unique advantages of the material. Thus, it is expected that stacking quantum dot graphene nanoplatelets based on 2D materials into heterostructures provides the opportunity to build high performance electrodes that will combine the collective advantages and synergistic performance of the individual components while eliminating the associated disadvantages. However, rational design and controlled synthesis of nano-heterostructure anode materials with excellent electrochemical performance via simple strategies remains a great challenge.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a 0D/2D quantum dot/graphene nano coil heterostructure electrode material. The electrode material obtained by the method can obviously improve the electrochemical performance when used in a battery.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme.
The invention provides a preparation method of a 0D/2D quantum dot/graphene nano roll heterostructure electrode material, which comprises the following steps:
preparation of Mxene quantum dots (MXene-QDs): uniformly dispersing MXene nano-sheets in DMF, transferring the obtained dispersion liquid into a high-pressure kettle, introducing nitrogen to remove oxygen, then carrying out vacuum drying, cooling to room temperature, filtering and evaporating the obtained suspension liquid to obtain a final product;
b. preparation of black phosphorus quantum dots (BP-QDs): uniformly dispersing the black phosphorus nanosheets in DMF, pouring the obtained dispersion liquid into an autoclave, introducing nitrogen to remove oxygen, then drying in vacuum, cooling, centrifuging the obtained dispersion liquid, collecting supernatant, and finally evaporating to obtain a final product;
c. preparing a Graphene Oxide (GO) nano roll: uniformly dispersing GO nano sheets in DDI water, heating an obtained GO dispersion liquid in a water bath, quickly immersing the GO nano sheets in liquid nitrogen until the GO nano sheets are completely frozen, and finally, obtaining graphene nano rolls through freeze drying;
d.0D/2D quantum dot/graphene nano coil heterostructure electrode material preparation: carrying out ultrasonic treatment on the GO nano-roll in 50ml DDI water containing 1 wt% of PDDA, then filtering and carrying out vacuum drying to obtain a PDDA modified GO nano-roll, and then carrying out ultrasonic treatment on MXene-QD (or BP-QDs) and the PDDA modified GO nano-roll according to the mass ratio of 3:1 in THF and the mixture was stirred at room temperature under argon for 3h, after which the mixture was centrifuged and washed with THF and heat treated under nitrogen atmosphere to give the final product.
Preferably, the vacuum drying temperature in the step a is 110-130 ℃, and the time is 24-48 h.
Preferably, the vacuum drying temperature in the step b is 140-180 ℃, and the time is 12-24 hours.
Preferably, the centrifugation conditions in step b are: the rotating speed is 5000-8000 rmp, and the time is 20-60 min.
Preferably, the water bath heating temperature in the step c is 70-80 ℃, and the time is 1-3 hours.
Preferably, the ultrasonic treatment time in the step d is 2-5 h.
Preferably, the vacuum drying temperature in the step d is 40-50 ℃ and the time is 12-24 hours.
Preferably, the heat treatment temperature in the step d is 300-400 ℃ and the time is 1 h.
The purpose of the invention and the technical problem to be solved are also realized by adopting the following technical scheme.
The invention also provides an application of the 0D/2D quantum dot/graphene nano coil heterostructure electrode material obtained by the preparation method in a lithium ion battery.
By the technical scheme, the invention at least has the following advantages: the invention provides a method for preparing a 0D/2D quantum dot/graphene nanocolloid heterostructure electrode material, which forms a new layered 0D/2D MXene quantum dot/graphene nanocolloid heterostructure by cold quenching, freeze drying and self-assembly, wherein two-dimensional (2D) graphene basic and zero-dimensional (0D) MXene (or black phosphorus) Quantum Dots (QDs) are encapsulated in a graphene nanocolloid. The 0D/2D quantum dot/graphene nano roll heterostructure electrode material has the advantages that in the heterostructure, the graphene nano roll with unique one-dimensional tubular shape and open inner cavity provides effective effectThe MXene (or black phosphorus) quantum dots have high capacity and abundant active sites encapsulated in the inner surface of graphene nano-coil, can reduce aggregation of single MXene (or black phosphorus) QDs and enhance electronic conductivity thereof, and maintain structural integrity during charge/discharge. Furthermore, the structural similarity of Mxene (or black phosphorus) DQ and graphene allows close surface-to-surface contact between Mxene (or black phosphorus) QD and graphene and provides a stable 0D/2D Mxene (or black phosphorus) QD/graphene heterostructure, thus facilitating efficient contact with the electrolyte and rapid ion transport. Furthermore, well-defined interfaces between MXene (or black phosphorus) QDs and graphene can reinforce each other, leading to unprecedented performance and triggering synergistic effects, making their ionic diffusion resistance lower, facilitating interfacial electron transport and maximizing Li+Storage potential of (2). Furthermore, a 0D/2D MXenes (or black phosphorus) QD/graphene heterostructure with well-defined morphology and high conductivity can be used as an adhesive-and conductor-free electrode for LIBs. In short, the unique bi-component heterostructure presented herein has many significant advantages as an electrode material to significantly improve the electrochemical performance of LIBs, such as large interfacial area, rapid insertion/extraction of lithium, short diffusion, and direct one-dimensional approach due to the synergistic effect of the components in the unique heterostructure, 0D/2D MXenes (or black phosphorus) QD/graphene nano rolling heterostructure electrode materials can be used as anodes for LIBs.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a flow chart of the preparation of a 0D/2D quantum dot/graphene nanocolloid heterostructure electrode material of the present invention;
fig. 2 is a battery discharge performance curve obtained by using the 0D/2D quantum dot/graphene nanocolloid heterostructure electrode material according to the present invention.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention and the accompanying drawings. 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
Preparation of Mxene quantum dots (MXene-QDs): MXene nanoplatelets are homogeneously dispersed in Dimethylformamide (DMF) by means of ultrasound. Next, the resulting dispersion was transferred to a teflon-lined autoclave, and bubbled with nitrogen for 30min to remove oxygen, followed by heat treatment at 120 ℃ for 24h in a vacuum oven. After cooling to room temperature, the suspension obtained was filtered through a microporous membrane and the filtrate was collected. Finally, the DMF solvent was removed by evaporation using a rotary evaporator to obtain the final product.
Preparation of black phosphorus quantum dots (BP-QDs): under vigorous stirring, the black phosphorus nanoplatelets are uniformly dispersed in DMF. Next, the obtained dispersion was poured into a teflon-lined autoclave, and bubbled with nitrogen for 30min to remove oxygen, and then kept at 140 ℃ for 12h in a vacuum oven. After cooling, the resulting dispersion was centrifuged at 5000rpm for 20 minutes, and the supernatant was collected by decanting. Finally, the solvent was evaporated using a rotary evaporator, and the remaining powder was collected to obtain a final product.
Preparing a Graphene Oxide (GO) nano roll: first, GO nanoplates were uniformly dispersed in DDI water by ultrasound. Next, the obtained GO dispersion was placed in a water bath at 80 ℃ for 1 h. The resulting GO dispersion was then quickly immersed in liquid nitrogen until completely frozen. And finally, obtaining the graphene nano-coil by freeze drying.
Preparing a 0D/2D quantum dot/graphene nano roll heterostructure electrode material: carrying out ultrasonic treatment on a GO nano-roll for 2 hours in 50ml of ultra-pure water containing 1 wt% of poly (diallyldimethylammonium chloride) (PDDA), carrying out non-covalent modification on the GO nano-roll by using the PDDA, then filtering and drying in a vacuum oven at 50 ℃ for 12 hours to obtain a PDDA modified GO nano-roll; then MXene-QD (or BP-QDs) and graphene nanocoils were mixed in Tetrahydrofuran (THF) in a mass ratio of 3:1, and the mixture was stirred at room temperature for 3 hours under argon protection. In this process, MXene-QD (or BP-QD) spontaneously assembles on graphene nanocoils by van der waals interactions. After that, the mixture was centrifuged and washed several times with THF. Treating at 300 deg.C for 1h under nitrogen protection gas to obtain the final product.
Example 2
Preparation of Mxene quantum dots (MXene-QDs): MXene nanoplatelets are homogeneously dispersed in Dimethylformamide (DMF) by means of ultrasound. Next, the resulting dispersion was transferred to a teflon-lined autoclave, and bubbled with nitrogen for 30min to remove oxygen, followed by heat treatment at 130 ℃ for 36h in a vacuum oven. After cooling to room temperature, the suspension obtained was filtered through a microporous membrane and the filtrate was collected. Finally, the DMF solvent was removed by evaporation using a rotary evaporator to obtain the final product.
Preparation of black phosphorus quantum dots (BP-QDs): under vigorous stirring, the black phosphorus nanoplatelets are uniformly dispersed in DMF. Next, the obtained dispersion was poured into a teflon-lined autoclave, and bubbled with nitrogen for 30min to remove oxygen, and then kept at 160 ℃ for 24h in a vacuum oven. After cooling, the resulting dispersion was centrifuged at 8000rpm for 40 minutes, and the supernatant was collected by decanting. Finally, the solvent was evaporated using a rotary evaporator, and the remaining powder was collected to obtain a final product.
Preparing a Graphene Oxide (GO) nano roll: first, GO nanoplates were uniformly dispersed in DDI water by ultrasound. Next, the obtained GO dispersion was placed in a water bath at 80 ℃ for 2 h. The resulting GO dispersion was then quickly immersed in liquid nitrogen until completely frozen. And finally, obtaining the graphene nano-coil by freeze drying.
Preparing a 0D/2D quantum dot/graphene nano roll heterostructure electrode material: carrying out ultrasonic treatment on a GO nano-roll for 2 hours in 50ml of ultra-pure water containing 1 wt% of poly (diallyldimethylammonium chloride) (PDDA), carrying out non-covalent modification on the GO nano-roll by using the PDDA, then filtering and drying in a vacuum oven at 40 ℃ for 18 hours to obtain a GO nano-roll modified by the PDDA; then MXene-QD (or BP-QDs) and graphene nanocoils were mixed in Tetrahydrofuran (THF) in a mass ratio of 3:1, and the mixture was stirred at room temperature for 3 hours under argon protection. In this process, MXene-QD (or BP-QD) spontaneously assembles on graphene nanocoils by van der waals interactions. After that, the mixture was centrifuged and washed several times with THF. Treating at 300 deg.C for 1h under nitrogen protection gas to obtain the final product.
Example 3
Preparation of Mxene quantum dots (MXene-QDs): MXene nanoplatelets are homogeneously dispersed in Dimethylformamide (DMF) by means of ultrasound. Next, the resulting dispersion was transferred to a teflon-lined autoclave, and bubbled with nitrogen for 30min to remove oxygen, followed by heat treatment at 110 ℃ for 48h in a vacuum oven. After cooling to room temperature, the suspension obtained was filtered through a microporous membrane and the filtrate was collected. Finally, the DMF solvent was removed by evaporation using a rotary evaporator to obtain the final product.
Preparation of black phosphorus quantum dots (BP-QDs): under vigorous stirring, the black phosphorus nanoplatelets are uniformly dispersed in DMF. Next, the obtained dispersion was poured into a teflon-lined autoclave, and bubbled with nitrogen for 30min to remove oxygen, and then kept at 180 ℃ for 12h in a vacuum oven. After cooling, the resulting dispersion was centrifuged at 7000rpm for 60 minutes, and the supernatant was collected by decanting. Finally, the solvent was evaporated using a rotary evaporator, and the remaining powder was collected to obtain a final product.
Preparing a Graphene Oxide (GO) nano roll: first, GO nanoplates were uniformly dispersed in DDI water by ultrasound. Next, the obtained GO dispersion was placed in a water bath at 80 ℃ for 3 h. The resulting GO dispersion was then quickly immersed in liquid nitrogen until completely frozen. And finally, obtaining the graphene nano-coil by freeze drying.
Preparing a 0D/2D quantum dot/graphene nano roll heterostructure electrode material: carrying out ultrasonic treatment on a GO nano-roll for 2 hours in 50ml of ultra-pure water containing 1 wt% of poly (diallyldimethylammonium chloride) (PDDA), carrying out non-covalent modification on the GO nano-roll by using the PDDA, then filtering and drying in a vacuum oven at 50 ℃ for 24 hours to obtain a PDDA modified GO nano-roll; then MXene-QD (or BP-QDs) and graphene nanocoils were mixed in Tetrahydrofuran (THF) in a mass ratio of 3:1, and the mixture was stirred at room temperature for 3 hours under argon protection. In this process, MXene-QD (or BP-QD) spontaneously assembles on graphene nanocoils by van der waals interactions. After that, the mixture was centrifuged and washed several times with THF. Treating at 400 ℃ for 1h under the protection of nitrogen to obtain the final product.
Test example 1 Performance test of electrode Material
The graphene nano-roll heterostructure electrode material obtained in the embodiment 1 is added into a positive electrode and a negative electrode of a lithium ion battery as an additive, for example, a ternary nickel-cobalt-manganese material positive electrode material and a carbon negative electrode material are added according to a proportion of 0.2%, slurry is prepared and coated on a commercial aluminum foil and a commercial copper foil respectively, and after drying, pole pieces of the lithium ion battery are prepared respectively. And finally, assembling the lithium ion battery by a conventional soft package battery process, and carrying out discharge capacity test and rate capability test at normal temperature, wherein the test result is shown in figure 2.
As can be seen from fig. 2, the maximum discharge capacity of the battery at normal temperature can reach more than 80% of the battery capacity when discharged at 20C rate, which is much higher than the rate performance of the commercial battery, indicating that the battery can realize large-rate discharge. The strong conductivity of the synthesized graphene nano coil material is used as an additive, so that the conductivity of an electrode of a lithium ion battery can be remarkably improved, and the high rate performance of the battery is further improved.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A method for preparing a 0D/2D quantum dot/graphene nanocolloid heterostructure electrode material, the method comprising the steps of:
preparation of Mxene quantum dots (MXene-QDs): uniformly dispersing MXene nano-sheets in DMF, transferring the obtained dispersion liquid into a high-pressure kettle, introducing nitrogen to remove oxygen, then carrying out vacuum drying, cooling to room temperature, filtering and evaporating the obtained suspension liquid to obtain a final product;
b. preparation of black phosphorus quantum dots (BP-QDs): uniformly dispersing the black phosphorus nanosheets in DMF, pouring the obtained dispersion liquid into an autoclave, introducing nitrogen to remove oxygen, then drying in vacuum, cooling, centrifuging the obtained dispersion liquid, collecting supernatant, and finally evaporating to obtain a final product;
c. preparing a Graphene Oxide (GO) nano roll: uniformly dispersing GO nano sheets in DDI water, heating an obtained GO dispersion liquid in a water bath, quickly immersing the GO nano sheets in liquid nitrogen until the GO nano sheets are completely frozen, and finally, obtaining graphene nano rolls through freeze drying;
d.0D/2D quantum dot/graphene nano coil heterostructure electrode material preparation: carrying out ultrasonic treatment on the GO nano-roll in 50ml DDI water containing 1 wt% of PDDA, then filtering and carrying out vacuum drying to obtain a PDDA modified GO nano-roll, and then carrying out ultrasonic treatment on MXene-QD (or BP-QDs) and the PDDA modified GO nano-roll according to the mass ratio of 3:1 in THF and the mixture was stirred at room temperature under argon for 3h, after which the mixture was centrifuged and washed with THF and heat treated under nitrogen atmosphere to give the final product.
2. The preparation method according to claim 1, wherein the vacuum drying temperature in the step a is 110-130 ℃ and the time is 24-48 h.
3. The preparation method according to claim 1, wherein the vacuum drying temperature in the step b is 140-180 ℃ and the time is 12-24 h.
4. The method of claim 1, wherein the centrifugation conditions in step b are: the rotating speed is 5000-8000 rmp, and the time is 20-60 min.
5. The preparation method of claim 1, wherein the water bath heating temperature in the step c is 70-80 ℃ and the time is 1-3 h.
6. The preparation method according to claim 1, wherein the ultrasonic treatment time in the step d is 2-5 h.
7. The preparation method according to claim 1, wherein the vacuum drying temperature in the step d is 40-50 ℃ and the time is 12-24 h.
8. The preparation method according to claim 1, wherein the heat treatment temperature in the step d is 300-400 ℃ and the time is 1 h.
9. Application of the 0D/2D quantum dot/graphene nanocolloid heterostructure electrode material obtained by the preparation method according to any one of claims 1 to 8 in lithium ion batteries.
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