CN114388280B - Transparent supercapacitor based on MXene quantum dots processed by femtosecond laser - Google Patents

Transparent supercapacitor based on MXene quantum dots processed by femtosecond laser Download PDF

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Publication number
CN114388280B
CN114388280B CN202111612625.XA CN202111612625A CN114388280B CN 114388280 B CN114388280 B CN 114388280B CN 202111612625 A CN202111612625 A CN 202111612625A CN 114388280 B CN114388280 B CN 114388280B
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transparent
mxene
super capacitor
femtosecond laser
quantum dots
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CN114388280A (en
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姜澜
原永玖
李欣
马乐
张学强
许晨阳
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Beijing Institute of Technology BIT
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/54—Electrolytes
    • H01G11/56—Solid electrolytes, e.g. gels; Additives therein
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • 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
    • Y02E60/13—Energy storage using capacitors

Abstract

The invention relates to a manufacturing method for processing a transparent super capacitor based on femtosecond laser, and belongs to the field of novel energy storage electronic devices of nanometer quantum dots. According to the invention, a layer of MXene film of transparent gel electrolyte is covered above the femtosecond laser focusing processing with specific pulse delay, and the generated MXene quantum dots are deposited on the transparent gel electrolyte in advance by utilizing a plasma spraying effect, so that a complete patterned plane or sandwich transparent super capacitor is prepared. The electrode material prepared by the invention is novel, the preparation process is ingenious, the complete transparent super capacitor is processed in situ by a one-step method, a current collector and additional electrolyte are not needed, and meanwhile, the prepared transparent super capacitor has extremely high transparency and energy storage capacity, good stability and long cycle life.

Description

Transparent supercapacitor based on MXene quantum dots processed by femtosecond laser
Technical Field
The invention relates to a manufacturing method for processing a transparent super capacitor based on femtosecond laser, in particular to a method for adjusting and controlling the femtosecond laser to process MXene quantum dots and preparing the transparent super capacitor, and belongs to the field of novel energy storage electronic devices of nanometer quantum dots.
Background
In recent years, the trend in new electronic products has placed new demands on portable, lightweight, flexible and optically transparent devices. In order to provide energy to transparent electronic devices, the transparency, miniaturization and flexibility of the energy supply devices have become major considerations. The super capacitor has the advantages of quick charge/discharge, high power density, excellent multiplying power capability and long cycle life, and becomes an ideal energy storage device. However, the existing transparent super capacitor has contradiction between transparency and capacity of capacitor, and meanwhile, the preparation process is complex and the controllability is low, so that the development of the transparent super capacitor faces a small challenge.
Many methods for preparing high-performance transparent super-capacitors are proposed internationally at present, and the aim is to ensure the transparency and simultaneously realize high energy storage capacity. The skeleton porous material or the nano wire can be used as the electrode material to enhance the light transmittance of the electrode material by utilizing the gap between the skeleton porous material and the nano wire, and one of the key factors of the electrode material with high energy storage capacity is selected. On the basis, the quantum dot material has extremely high transparency due to the single-layer structure and the nano-scale diameter, and meanwhile, the quantum dot material has the characteristics of extremely high specific surface area and easiness in adsorbing and desorbing ions, so that the quantum dot material becomes an ideal electrode material in electrochemical energy storage. In addition, MXene has been widely accepted in the field of energy storage materials due to its unique high energy storage performance and the characteristics of two-dimensional materials. And the MXene quantum dot material combines high transparency and high energy storage capacity, so that the MXene quantum dot material becomes an ideal electrode material of the transparent super capacitor. However, the related report and the preparation process of the MXene quantum dot as the super capacitor electrode material have not been reported, and the electrode material combination form provides a new thought for the research of transparent super capacitors and the discussion of quantum effects in electrochemical energy storage, and the invention also provides a new technology for the synthesis of the MXene quantum dot and the preparation of the transparent super capacitors of the quantum dot.
Disclosure of Invention
The invention aims to solve the problems that the existing transparent super capacitor has low performance and low light transmittance and cannot meet the requirements, and provides a preparation method for processing the transparent super capacitor based on femtosecond laser; according to the method, the femtosecond laser capable of regulating and controlling the electron density under the specific laser pulse delay is utilized to process the MXene film covered with the transparent gel electrolyte, and the MXene quantum dots are excited to be attached to the transparent gel electrolyte above by utilizing the plasma eruption effect, so that the integrated processing and patterning of the transparent super capacitor of the MXene quantum dots are realized. By utilizing the method, the size and the distribution uniformity of the MXene quantum dots can be regulated and controlled by femtosecond laser, and the transparent super capacitor is directly prepared without other assembly processes, so that the obtained material has excellent performance and good repeatability, is suitable for large-scale preparation, and has good industrial prospect. The prepared transparent super capacitor has high transparency and high energy storage capacity.
The aim of the invention is achieved by the following technical scheme.
Step one, placing the prepared MXene film on a glass substrate, and covering a layer of transparent gel electrolyte on the glass substrate;
emitting femtosecond lasers with different pulse delays through a Michelson interferometer, focusing on an MXene film, and controlling laser energy by utilizing a continuous attenuation sheet;
and thirdly, emitting different pulse delays of femtosecond laser based on electronic dynamic regulation by using a Michelson interferometer, focusing on the MXene film, and controlling the laser energy by using a continuously-decaying piece. The femtosecond laser scanning path is controlled by a computer program, the MXene quantum dot material can be deposited in advance in a patterning way, the self-assembly process of the MXene quantum dot electrode material and the transparent gel electrolyte is realized after the processing is finished, and the patterned planar or sandwich transparent super capacitor is finished in one step.
The MXenx quantum dot material is densely and uniformly adhered on the surface of the transparent gel electrolyte, the size of the quantum dot is controllable, the uniformity is controllable, and the light transmittance of the quantum dot material is extremely high, so that the light transmittance of the whole transparent super capacitor is improved, the specific surface area of the MXene quantum dot is high, and the active sites are abundant, so that the electrochemical performance of the transparent super capacitor can be effectively increased.
The time domain shaping femtosecond laser pulse sequence is utilized, so that the delay of the pulse can be regulated and controlled to effectively control the electron density, thereby influencing the eruption of the plasma and improving the generation of the MXene quantum dots. According to the method provided by the invention, the MXene film is directly excited by the femtosecond laser, and the generated MXene quantum dots are directly attached to the transparent gel electrolyte, so that a complete transparent supercapacitor is directly constructed, and the transparent supercapacitor is prepared in situ in one step.
The transparent gel electrolyte described in the above steps includes: PVA/H 2 SO 4 、PVA/KCL、PEGDA/H 2 SO 4 、PEGDA/KCL。
The MXene film is mechanically stamped by MXene dispersion liquid, the thickness of the film is 20-40 mu m, and the size is 1cm 2 ～3*3cm 2 。
The size and the distribution uniformity of the MXene quantum dots can be regulated by dynamically regulating the pulse delay of the femtosecond laser through electrons; when the pulse delays are 5ps, 10ps and 1ps respectively, the sizes of the processed MXene quantum dots are 3nm, 5nm and 10nm respectively; the uniformity of distribution varies. The thickness of the single layer is about 2nm, and the light transmittance of the single layer can reach 99%.
Advantageous effects
1. The MXene quantum dot material is used as a novel super capacitor electrode material, has the characteristics of ultrahigh specific surface area and easiness in adsorbing and desorbing ions, and has extremely high electrochemical energy storage performance; meanwhile, due to the high light transmittance of the single-layer quantum dots, the whole super capacitor has high transparency, high energy storage and high transparency are realized, and the key problem of restricting the development of the transparent super capacitor is solved.
2. The invention realizes the in-situ preparation of the MXene quantum dot electrode material by using a femtosecond laser one-step method based on electronic dynamic regulation, realizes the complete assembly of the transparent super capacitor, and simultaneously designs the electrode material with any pattern by using laser patterning front deposition, thereby having strong individuation.
3. The method has the advantages of simple operation process, high efficiency, good repeatability, capability of selectively regulating and controlling the size and uniformity of the MXene quantum dots by changing parameters, no need of adding other chemical reagents in the whole process, green and pollution-free processing process, good large-scale application potential and good industrialization prospect. The method realizes the preparation of the high-performance transparent super low capacitor and provides a new idea for the selection of the electrode material of the transparent super capacitor and the processing technology.
4. The transparent supercapacitor of MXene quantum dots according to claim 2, further comprising: has excellent electrochemical performance, as high as 66.3mF cm -2 The area ratio capacitor is good in cycle life, the capacity of the capacitor is still 98% after 12000 cycles, meanwhile, the light transmittance of the transparent super capacitor device reaches more than 90%, and the transparent super capacitor device is good in flexibility and strong in bending resistance.
Drawings
FIG. 1 is a schematic illustration of the process of the present invention;
FIG. 2 is an electron microscope image of MXene quantum dots prepared in example 1 of the present invention;
FIG. 3 is a graph showing the CV curve of the MXene quantum dot transparent super capacitor prepared in example 1 of the present invention;
FIG. 4 is a graph showing the transparency of the MXene quantum dot transparent supercapacitor prepared in example 1 of the present invention;
FIG. 5 is a cycle life curve of the MXene quantum dot transparent supercapacitor prepared in example 1 of the present invention;
FIG. 6 is an electron microscope image of the MXene quantum dots prepared in example 2 of the present invention;
FIG. 7 is a graph showing the CV curve of the MXene quantum dot transparent super capacitor prepared in example 2 of the present invention;
FIG. 8 is a graph showing the transparency of the MXene quantum dot transparent supercapacitor prepared in example 2 of the present invention;
FIG. 9 is a cycle life curve of the MXene quantum dot transparent supercapacitor prepared in example 2 of the present invention;
FIG. 10 is an electron microscope image of MXene quantum dots prepared in example 3 of the present invention;
FIG. 11 is a graph showing the CV curve of the MXene quantum dot transparent super capacitor prepared in example 3 of the present invention;
FIG. 12 is a graph showing the transparency of the MXene quantum dot transparent supercapacitor prepared in example 3 of the present invention;
FIG. 13 is a cycle life curve of the MXene quantum dot transparent supercapacitor prepared in example 3 of the present invention.
Detailed Description
The inventive method of the present invention is described and illustrated in detail below in conjunction with specific examples. The content of which is to be interpreted as an explanation of the invention and not to limit the scope of the invention.
Example 1
The preparation method for processing the transparent super capacitor based on the femtosecond laser comprises the following steps:
step one, imprinting 0.5g of MXene nano-sheet into a rectangular block-shaped MXene film by using mechanical stress, transferring the rectangular block-shaped MXene film to a silicon dioxide substrate, and then placing a transparent gel electrolyte on the silicon dioxide substrate, wherein the length dimension of the transparent gel electrolyte is equal to that of the MXene film, and the thickness of the transparent gel electrolyte is 0.2cm;
emitting femtosecond laser with pulse delay based on electronic dynamic regulation by using a Michelson interferometer, controlling the laser power to be 12mw by using a continuous attenuation sheet by using the femtosecond laser with the pulse delay of 5ps, and focusing a laser focus on an MXene film;
step three, using a control program programmed in advance to control the electronic dynamic regulation femtosecond laser to perform patterning scanning, wherein the scanning speed is 200 mu m/s, the spraying of MXene plasma is initiated, the patterned MXene quantum dots are deposited on the transparent gel electrolyte above in front, the schematic diagram of the process is shown in figure 1, the electron microscope diagram of the quantum dots is shown in figure 2, the particle size is about 3nm, and the distribution is very uniform;
step four, taking out the transparent gel electrolyte after the pre-deposition in the step, and then performing electrochemical test and transparency test as a planar patterning or sandwich transparent super capacitor device without other current collectors and additional electrolyte, wherein FIG. 3 is a CV curve of the super capacitor, FIG. 4 is a transparency test, FIG. 5 is a 12000 cycle life curve, and the area specific capacitance reaches 66.3mF/cm 2 The transparency reaches 93 percent, and after 12000 times of circulation, 99 percent is still maintainedThe capacitor maintains the rate.
Example 2
This embodiment is substantially the same as the first embodiment, and is characterized in that:
in the present embodiment, the pulse delay based on the femtosecond laser in the second step is 10ps; in the third step, the electron microscope image of the quantum dots is shown in fig. 6, the particle size is about 5nm, and the distribution is relatively uniform; in the fourth step, FIG. 7 shows CV curve of the super capacitor, FIG. 8 shows transparency test, FIG. 9 shows 12000 cycle life curve, area specific capacitance of 38.5mF/cm 2 The transparency reaches 90%, and after 12000 times of circulation, the capacitance retention rate of 95% is still maintained.
Example 3
This embodiment is substantially the same as the first embodiment, and is characterized in that:
in the embodiment, the pulse delay of the femtosecond laser based on electronic dynamic regulation in the second step is 1ps; in the third step, the electron microscope image of the quantum dot is shown in fig. 10, the particle size is about 10nm, and the distribution is generally uniform; in the fourth step, FIG. 11 shows CV curve of the super capacitor, FIG. 12 shows transparency test, FIG. 13 shows 12000 cycle life curve, and area specific capacitance of the super capacitor reaches 29.7mF/cm 2 The transparency reached 87%, and after 12000 cycles, the capacitance retention of 89% was maintained.
While the foregoing is directed to embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.

Claims (3)

1. The preparation method of the transparent super capacitor based on the MXene quantum dot processed by the femtosecond laser is characterized by comprising the following steps:
step one, placing the prepared MXene film on a glass substrate, and covering a layer of transparent gel electrolyte on the glass substrate;
emitting different pulse delays of femtosecond laser based on electronic dynamic regulation through a Michelson interferometer, focusing on an MXene film, and controlling laser energy by utilizing a continuous attenuation sheet;
controlling a femtosecond laser scanning path through a computer program, enabling the femtosecond laser to penetrate through the transparent electrolyte, exciting quantum dot eruption, and attaching the quantum dots on the lower surface of the transparent electrolyte according to a pattern to form a transparent supercapacitor; the method realizes the patterning pre-deposition of the MXene quantum dot material, and the self-assembly process of the MXene quantum dot electrode material and the transparent gel electrolyte is realized after the processing is finished, so that the patterned planar transparent super capacitor is finished in one step.
2. The method of claim 1, wherein: the size of the MXene quantum dots is controllable along with the laser pulse delay, and when the pulse delay is 5ps, 10ps and 1ps respectively, the size of the processed MXene quantum dots is 3nm, 5nm and 10nm respectively.
3. The method of claim 1, wherein: the thickness of the film is 20-40 mu m, and the size is 1 x 1cm 2 ～3*3cm 2 The method comprises the steps of carrying out a first treatment on the surface of the The transparent gel electrolyte is as follows: PVA/H 2 SO 4 、PVA/KCL、PEGDA/H 2 SO 4 Or PEGDA/KCL.
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CN110272048A (en) * 2019-06-17 2019-09-24 西安电子科技大学 A kind of preparation method of two-dimensional layer nano material MXene quantum dot
CN113148987A (en) * 2021-04-08 2021-07-23 北京理工大学 Method for preparing MXene nanoflowers on graphene base in multi-dimensional mode
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