CN110853935A - Molybdenum sulfide supercapacitor electrode and preparation method thereof - Google Patents

Molybdenum sulfide supercapacitor electrode and preparation method thereof Download PDF

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Publication number
CN110853935A
CN110853935A CN201911147458.9A CN201911147458A CN110853935A CN 110853935 A CN110853935 A CN 110853935A CN 201911147458 A CN201911147458 A CN 201911147458A CN 110853935 A CN110853935 A CN 110853935A
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mos
molybdenum sulfide
time
steps
supercapacitor electrode
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戚雯
刘玉峰
杨正春
翟娅琪
谢立强
张洪浩
赵心昊
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Beijing Collaborative Innovation Institute
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/24Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Electric Double-Layer Capacitors Or The Like (AREA)

Abstract

The invention discloses a molybdenum sulfide super capacitor electrode and a preparation method thereof, and MoS is prepared by adopting a new method2And MoS prepared by the new method2The method comprises the steps of adding acetylene black and polyvinylidene fluoride into an N-methyl pyrrolidone (NMP) solution for size mixing, then putting the size mixed slurry into an ultrasonic machine for ultrasonic treatment for 20 minutes, stirring the size uniformly after the ultrasonic treatment is finished, printing the size uniformly on carbon paper through screen printing, putting the carbon paper into a dryer for drying, and making an electrode after the drying is finished. According to the molybdenum sulfide supercapacitor electrode and the preparation method thereof, the MoS prepared by the novel method is adopted2The structure between layers is broken, so that the specific surface area of the internal structure is increased, the discharge time of the internal structure is increased, the charge time of the internal structure is shortened, and the improvement is achievedMoS2The energy storage efficiency is improved, and the performance of the molybdenum sulfide super capacitor electrode is improved obviously.

Description

Molybdenum sulfide supercapacitor electrode and preparation method thereof
Technical Field
The invention belongs to the technical field of microelectronic device materials, in particular to the technical field of electrode materials of super capacitors.
Background
Very serious problems facing the human society in the twenty-first century are energy problems and environmental problems. The focus of global attention has been the development and utilization of clean energy and the development and utilization of renewable energy. From the perspective of more reasonable and full utilization of electric energy, electric energy development and electric energy storage have the same important significance, so that research on various electrochemical energy storage properties is concerned to a great extent. With the drilling in of graphene-headed two-dimensional layered nanomaterials, graphene-like materials, e.g. MoS2The study of sulfide of transition metals has been also gradually noticed. MoS since the 90 s of the 20 th century2Due to the special layered structure and anisotropy, the application of the material in industrial production is gradually enlarged and the dosage is continuously increased, and the material is mainly applied to various fields of friction lubrication, catalytic refining super wave-absorbing material electronic probes, oxygen storage materials, electrode materials, photoelectrochemistry oxygen generation catalysts and the like.
By using MoS2Materials are receiving more and more attention to the production of supercapacitor electrodes. Conventional MoS2The materials can be produced by hydrothermal method, solution method, surfactant-assisted method, etc., and MoS produced by these methods2The material has the defects of higher reaction pressure, poorer crystallization, more impurities and the like, and is not beneficial to the production of the supercapacitor electrode.
Disclosure of Invention
(1) Solves the technical problem
The invention aims to provide a molybdenum sulfide supercapacitor electrode and a preparation method thereof, and aims to solve the problem of the existing MoS provided in the background technology2The material has the technical problems of high reaction pressure, poor crystallization, excessive impurities and the like, and is not beneficial to the production of the supercapacitor electrode.
(2) Technical scheme
In order to realize the purpose, the invention provides a preparation method of a molybdenum sulfide supercapacitor electrode, which comprises the following steps:
s1: mixing MoS2Adding an activating agent and deionized water into a vessel for fusion, and then fully stirring;
s2: after uniformly stirring, putting the vessel into an ultrasonic machine for fixing and slicing;
s3: taking out six clean small test tubes after the slicing treatment is finished, pouring the solution into the clean small test tubes, and carrying out four times of centrifugal operation on the solution;
s4: after the centrifugation in S3 is completed, the top layer of clear liquid is poured out, and a test tube is covered by a plurality of small holes, so that MoS remained on the wall of the test tube2Putting the mixture into a refrigerator for freeze-drying treatment;
s5: for the lyophilized MoS2Vacuumizing to obtain powdered MoS2And mixing the powdered MoS2Putting the mixture into a refrigerator, and obtaining the final MoS after the freezing is finished2Powder;
s6: mixing slurry;
s7: putting the mixed slurry into an ultrasonic machine for ultrasonic treatment for 20 minutes, and stirring the slurry uniformly after the ultrasonic treatment is finished;
s8: and (3) uniformly printing the slurry in the S7 on carbon paper by screen printing, putting the carbon paper into a dryer for drying, and preparing the electrode after drying.
As a preferable technical solution of the present invention, in the step S2, the ultrasonic power is 60W, the temperature is set to 20 degrees celsius, and the rotation speed of the high speed shearing machine is set to 7000 revolutions.
As a preferred embodiment of the present invention, the specific steps of performing four centrifugation operations on the solution in step S3 are as follows: when the centrifuge is put into the centrifuge for the first time, the rotating speed is set to 3000 revolutions, and the time is set to 30 minutes; after the completion, taking out six test tubes filled with the solution, pouring out the upper layer solution, and leaving solid substances on the walls of the test tubes; adding new deionized water, and performing second-time to fourth-time centrifugation, wherein the operation speed is set to 10000 revolutions and the time is set to 10 minutes in the second-time to fourth-time centrifugation.
In a preferred embodiment of the present invention, the time for the lyophilization process in step S4 is set to twenty-four hours.
As a preferred technical solution of the present invention, the slurry mixing process in step S6 is to mix MoS2Adding the powder, acetylene black and polyvinylidene fluoride (PVDF) into an N-methylpyrrolidone (NMP) solution; and wherein MoS2The mass ratio of the powder to the acetylene black to the polyvinylidene fluoride (PVDF) is 7-10:1-3: 1-3.
In a preferred embodiment of the present invention, in the step S7, the stirring method is to stir the mixture on the stirrer at a low speed for half an hour and at a high speed for one and half an hour.
As a preferable technical solution of the present invention, the temperature set when the dryer dries in step S8 is 90-120 ℃.
As a preferred embodiment of the present invention, the drying time of the dryer in the step S8 is two hours.
The invention also provides a molybdenum sulfide supercapacitor electrode, and the electrode manufactured by adopting any one of the preparation methods of the molybdenum sulfide supercapacitor electrode.
(3) Advantageous effects
Compared with the prior art, the invention has the beneficial effects that: the preparation method provided by the invention is used for treating powdery MoS by utilizing ultrasonic waves2Cutting to break the structure between layers, thereby increasing the specific surface area of the internal structure, further increasing the discharge time and shortening the charge time, compared with the MoS manufactured by the traditional methods such as a hydrothermal method, a solution method and the like2Remarkably improves MoS2The energy storage efficiency is improved, and the defects of low specific surface area, poor charge and discharge performance and poor cycle performance of the existing molybdenum sulfide are overcome; compared with the MoS manufactured by the traditional method2The electrode produced by the material solves the problem of the prior molybdenum sulfide super capacitorThe electrode has the problems of poor polar cyclicity and poor charge-discharge performance, and can effectively improve the cyclicity, high rate performance, specific capacity and the like of the conventional molybdenum sulfide supercapacitor electrode.
Drawings
FIG. 1 shows an example of an ultrasonically sheared MoS2Material is shown schematically in a Scanning Electron Microscope (SEM).
FIG. 2 shows MoS in comparative example2Material is shown schematically in a Scanning Electron Microscope (SEM).
FIG. 3 shows an example of an ultrasonically sheared MoS2Cyclic Voltammetry (CV) curve analysis of the material.
FIG. 4 shows MoS in comparative example2Cyclic Voltammetry (CV) curve analysis of the material.
FIG. 5 shows an example of an ultrasonically sheared MoS2Analysis graph of constant current charge and discharge (GCD) curve of material.
FIG. 6 shows MoS in comparative example2Analysis graph of constant current charge and discharge (GCD) curve of material.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
Examples
12 g of MoS2Adding 1ml of activating agent and 1200ml of deionized water into a vessel for fusion, and then fully stirring; after uniformly stirring, putting the vessel into an ultrasonic machine for fixing and slicing treatment, wherein the ultrasonic power is 60W, the temperature is set to be 20 ℃, and the rotating speed of a high-speed shearing machine is set to be 7000 revolutions; taking out six clean small test tubes after the slicing treatment is finished, pouring the solution into the clean small test tubes, and centrifuging the solution for four times, wherein specifically, the rotating speed is set to 3000 revolutions when the solution is placed into a centrifuge for the first time, and the time is set to 30 minutes; after completion, six test tubes filled with the solution were taken out, and the tube was taken outPouring out the upper layer solution to leave solid substances on the wall of the test tube; adding new deionized water, and centrifuging for the second time to the fourth time, wherein the running speed is set to 10000 revolutions and the time is set to 10 minutes during the second time to the fourth time of centrifugation; after the centrifugation is finished, pouring the topmost layer of clear liquid, and pricking a plurality of small holes on the test tube cover to retain the MoS on the wall of the test tube2Putting the mixture into a refrigerator for freeze-drying treatment, wherein the freeze-drying treatment time is set to be twenty-four hours; for the lyophilized MoS2Vacuumizing to obtain powdered MoS2And mixing the powdered MoS2Putting the mixture into a refrigerator, and obtaining the final MoS after the freezing is finished2Powder; taking the MoS2Adding 3 g of powder, 0.375 g of acetylene black and 0.375 g of polyvinylidene fluoride into 11.565 g of N-methyl pyrrolidone (NMP) solution for size mixing, putting the size mixed slurry into an ultrasonic machine for ultrasonic treatment for 20 minutes, and stirring the size uniformly after the ultrasonic treatment; and uniformly printing the slurry on carbon paper by screen printing, putting the carbon paper into a dryer for drying, wherein the drying set temperature is 100 ℃, the drying time is two hours, and the electrode can be prepared after the drying is finished.
Comparative example
Taking MoS manufactured by traditional method2Adding 3 g of powder, 0.375 g of acetylene black and 0.375 g of polyvinylidene fluoride into 11.565 g of N-methyl pyrrolidone (NMP) solution for size mixing, putting the size mixed slurry into an ultrasonic machine for ultrasonic treatment for 20 minutes, and stirring the size uniformly after the ultrasonic treatment; and uniformly printing the slurry on carbon paper by screen printing, putting the carbon paper into a dryer for drying, wherein the drying set temperature is 100 ℃, the drying time is two hours, and the electrode can be prepared after the drying is finished.
The invention can be seen from the analysis of fig. 1 and 2 that MoS is cut by ultrasonic wave2And MoS before ultrasonic cutting2Compared with the mutually separated laminated structure, the laminated parts are mutually stacked and the surface is loose. This shows that the ultrasonic-assisted mechanical shearing can effectively realize the separation of the layer-by-layer structure. It can be seen that the structure between the layers is broken.
The analysis of FIG. 3 and FIG. 4 shows thatThree-electrode MoS after ultrasonic cutting2The CV curve of (a) is relatively smooth. At 1mVs-1It can be seen that the graph appears as a rectangle, illustrating the MoS at low scan rates2The electrode exhibits good reversibility and capacitance characteristics. As the scan rate increases, the rectangle gradually deviates.
By the analysis of FIGS. 5 and 6, three-electrode MoS after cutting with ultrasound2GCD curve of (1), at 0.1mA cm-2The charging and discharging time is longest and can reach about 620s, and is delayed by 100s compared with that before cutting.
In summary, the ultrasonically sheared MoS in the examples2The electrode, as analyzed from fig. 3, showed a rectangular image at low speed scanning, indicating good reversibility. At high speed, the image deviates from a rectangle, which shows that the performance is poor, so the image is not suitable for being used as an electrode material under large current and is suitable for being used as an electrode material under small current, and the analysis of figure 5 shows that the voltage and the time are linear characteristics, the charging curve and the discharging curve are basically symmetrical, the image shows good reversibility, and the image is basically in triangular distribution. The discharge time can be prolonged after ultrasonic shearing, and the modification is obvious.
Therefore, the molybdenum sulfide two-dimensional material is subjected to ultrasonic shearing to manufacture an electrode material with more excellent performance, so that the defects of low surface area, poor charge and discharge performance and poor cycle performance of the existing molybdenum sulfide are overcome, and the performance of the molybdenum sulfide supercapacitor electrode is further remarkably improved.
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.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (9)

1. A preparation method of a molybdenum sulfide supercapacitor electrode is characterized by comprising the following steps: the method comprises the following steps:
s1: mixing MoS2Adding an activating agent and deionized water into a vessel for fusion, and then fully stirring;
s2: after uniformly stirring, putting the vessel into an ultrasonic machine for fixing and slicing;
s3: taking out six clean small test tubes after the slicing treatment is finished, pouring the solution into the clean small test tubes, and carrying out four times of centrifugal operation on the solution;
s4: after the centrifugation in S3 is completed, the top layer of clear liquid is poured out, and a test tube is covered by a plurality of small holes, so that MoS remained on the wall of the test tube2Putting the mixture into a refrigerator for freeze-drying treatment;
s5: for the lyophilized MoS2Vacuumizing to obtain powdered MoS2And mixing the powdered MoS2Putting the mixture into a refrigerator, and obtaining the final MoS after the freezing is finished2Powder;
s6: mixing slurry;
s7: putting the mixed slurry into an ultrasonic machine for ultrasonic treatment for 20 minutes, and stirring the slurry uniformly after the ultrasonic treatment is finished;
s8: and (3) uniformly printing the slurry in the S7 on carbon paper by screen printing, putting the carbon paper into a dryer for drying, and preparing the electrode after drying.
2. The method for preparing the molybdenum sulfide supercapacitor electrode according to claim 1, wherein the method comprises the following steps: in step S2, the ultrasonic power is 60W, the temperature is set to 20 degrees celsius, and the rotation speed of the high-speed shearing machine is set to 7000 revolutions.
3. The method for preparing the molybdenum sulfide supercapacitor electrode according to claim 2, wherein the method comprises the following steps: the specific steps of performing four centrifugation operations on the solution in step S3 are as follows: when the centrifuge is put into the centrifuge for the first time, the rotating speed is set to 3000 revolutions, and the time is set to 30 minutes; after the completion, taking out six test tubes filled with the solution, pouring out the upper layer solution, and leaving solid substances on the walls of the test tubes; adding new deionized water, and performing second-time to fourth-time centrifugation, wherein the operation speed is set to 10000 revolutions and the time is set to 10 minutes in the second-time to fourth-time centrifugation.
4. The method for preparing the molybdenum sulfide supercapacitor electrode according to claim 3, wherein the method comprises the following steps: the time for the freeze-drying process in said step S4 was set to twenty-four hours.
5. The method for preparing the molybdenum sulfide supercapacitor electrode according to claim 1, wherein the method comprises the following steps: the size mixing process in the step S6 is to mix MoS2Adding the powder, acetylene black and polyvinylidene fluoride (PVDF) into an N-methylpyrrolidone (NMP) solution; and wherein MoS2The mass ratio of the powder to the acetylene black to the polyvinylidene fluoride (PVDF) is 7-10:1-3: 1-3.
6. The method for preparing the molybdenum sulfide supercapacitor electrode according to claim 5, wherein the method comprises the following steps: in the step S7, the stirring method is to stir on the stirrer for half an hour at a low speed and for one and a half hours at a high speed.
7. The method for preparing the molybdenum sulfide supercapacitor electrode according to claim 6, wherein the method comprises the following steps: the temperature set when the dryer dries in the step S8 is 90-120 ℃.
8. The method for preparing the molybdenum sulfide supercapacitor electrode according to claim 7, wherein the method comprises the following steps: the drying time of the dryer in the step S8 is two hours.
9. A molybdenum sulfide supercapacitor electrode is characterized in that: an electrode made by the method of making a molybdenum sulfide supercapacitor electrode according to any one of claims 1 to 8.
CN201911147458.9A 2019-11-21 2019-11-21 Molybdenum sulfide supercapacitor electrode and preparation method thereof Pending CN110853935A (en)

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CN113415831A (en) * 2021-05-08 2021-09-21 湖南大学 A kind of Ni (OH)2Preparation method of/graphene composite material and preparation method of supercapacitor
CN116216780A (en) * 2023-03-01 2023-06-06 淮北师范大学 Broken shell-shaped MoS 2 Nanosphere material and preparation method and application thereof

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Application publication date: 20200228