CN108511205B - Preparation method of (002) crystal face grown metal phase flexible molybdenum disulfide supercapacitor electrode material - Google Patents
Preparation method of (002) crystal face grown metal phase flexible molybdenum disulfide supercapacitor electrode material Download PDFInfo
- Publication number
- CN108511205B CN108511205B CN201810354978.6A CN201810354978A CN108511205B CN 108511205 B CN108511205 B CN 108511205B CN 201810354978 A CN201810354978 A CN 201810354978A CN 108511205 B CN108511205 B CN 108511205B
- Authority
- CN
- China
- Prior art keywords
- molybdenum disulfide
- electrode material
- metal phase
- supercapacitor electrode
- crystal face
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Classifications
-
- 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
-
- 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
-
- 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 discloses a metal phase molybdenum disulfide flexible supercapacitor electrode material with an exposed (002) crystal face synthesized by a hydrothermal method. According to the application, the metal phase molybdenum disulfide with the (002) crystal face exposed directly grows on the carbon fiber substrate, and the prepared electrode material of the super capacitor shows high specific capacitance and ultra-long circulation stability. And it has at the same time good flexibility properties. The supercapacitor electrode material disclosed by the invention is simple in experimental operation, low in production cost and wide in industrial application prospect.
Description
Technical Field
The invention belongs to the field of preparation of capacitor electrode materials, and particularly relates to a preparation method of a metal phase flexible molybdenum disulfide supercapacitor electrode material with a (002) crystal face growing.
Background
The super capacitor is also called as an electrochemical capacitor, is a novel energy storage device between a traditional capacitor and a secondary battery, which develops rapidly in recent years, and has the advantages of the traditional capacitor and the secondary battery, namely higher energy density than the traditional capacitor and higher power density than various secondary batteries. In addition, the typical advantages of supercapacitors, including fast charge rate, long cycle life, wide operating temperature range, maintenance-free, economical and environmentally friendly, have also prompted their use in many areas. With the development of intelligence, people have new requirements on supercapacitors, such as wearable portable flexible supercapacitor materials.
The transition metal molybdenum disulfide is used as a cheap electrode material and is widely applied to the super capacitor. However, as a semiconductor material, it has poor conductivity, which leads to problems of low practical capacity and poor cycle stability. Research proves that the molybdenum disulfide has three structures of a 1T phase, a 2H phase and a 3R phase. The metal 1T phase has very high conductivity, so that the preparation of the molybdenum disulfide with a high-purity phase structure is an effective means for improving the conductivity of the electrode material and further improving the actual capacity and the cycling stability of the electrode material. In addition, the edge part of the crystal face of the molybdenum disulfide (002) has good reaction activity, more active sites are exposed by controlling the growth of the mirror face, and the overall performance of the material can be effectively improved. Therefore, the carbon fiber is used as a substrate material to prepare the metal phase molybdenum disulfide flexible electrode material with a large amount of exposed (002) crystal face active sites, and the metal phase molybdenum disulfide flexible electrode material is applied to the super capacitor, meets the development requirements of the times, has the feasibility of industrial production, and is a valuable research subject.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a metal phase flexible molybdenum disulfide supercapacitor electrode material with a (002) crystal face growth, the preparation method is simple, the cost is low, the yield is high, and the prepared electrode material has high specific capacitance, good stability, long service life and good electrochemical activity.
The purpose of the invention is realized as follows:
a preparation method of a metal phase flexible molybdenum disulfide supercapacitor electrode material with a (002) crystal face growth is characterized by comprising the following steps:
(1) a sulfur source, a molybdenum source, ethanol and water are evenly stirred to prepare a precursor solution,
(2) adding the precursor solution into the inner container of the reaction kettle, and adding a piece of carbon fiber substrate material;
(3) putting the reaction kettle into an oven for reaction; and after the oven is cooled to room temperature, ultrasonically washing and drying the carbon fiber material. And obtaining the metal phase flexible molybdenum disulfide supercapacitor electrode material with the (002) crystal face growing.
Further:
(1) in the step (1), the molybdenum source is dodecahydrate and sodium molybdate, the sulfur source is L-cysteine, and the molar ratio of the molybdenum source to the sulfur source is 1: 10;
(2) the dosage of the molybdenum source in the step (1) is 0.5-2 millimoles, and the dosage of the L-cysteine is 5-20 millimoles;
(3) the volume ratio of the water to the ethanol in the step (1) is 1: 1 to 5: 1, the total volume is 60 milliliters;
(4) the reaction temperature in the step (3) is 180-220 ℃ and the reaction time is 24-36 hours.
Has the positive and beneficial effects that: the preparation method of the (002) crystal face growth metal phase flexible molybdenum disulfide supercapacitor electrode material prepared by the invention is simple to operate, the molybdenum disulfide flexible electrode material with complete structure and excellent performance can be prepared only in a short time, no complex equipment is needed, the cost is low, the synthesized molybdenum disulfide flexible nano material has large specific surface area and uniform distribution, has large-area exposed (002) active reaction sites and a metal phase structure with higher components, shows higher specific capacitance and stable electrochemical performance, has long cycle life, provides possibility for industrial production, is an excellent supercapacitor electrode material, and has good development prospect. The preparation method is simple and effective, low in cost and environment-friendly.
Drawings
FIG. 1 is an XRD (X-ray diffraction) spectrum of an electrode material of a (002) crystal face growth metal phase flexible molybdenum disulfide supercapacitor prepared in example 1 of the invention;
FIG. 2 is an XPS spectrum of an electrode material of a (002) crystal plane growth metal phase flexible molybdenum disulfide supercapacitor prepared in example 1 of the present invention;
FIG. 3 is an SEM image of (002) crystal plane growth metal phase flexible molybdenum disulfide supercapacitor electrode material prepared in example 1 of the present invention under different magnifications;
FIG. 4 is an HRTEM image of the (002) crystal plane growth metal phase flexible molybdenum disulfide supercapacitor electrode material prepared in example 1 of the present invention;
FIG. 5 is an SEM image of (002) crystal plane growth metal phase flexible molybdenum disulfide supercapacitor electrode material prepared in example 2 of the present invention under different magnifications;
fig. 6 is an SEM image of the (002) crystal plane growth metal phase flexible molybdenum disulfide supercapacitor electrode material prepared in example 3 of the present invention at different magnifications.
Detailed Description
The invention will be further described with reference to specific examples:
example 1
Soaking the carbon fiber material in aqua regia solution, heating at 100 ℃ for 2 hours, and then washing and drying for later use. 0.5 mmol of sodium molybdate and 5 mmol of L-cysteine are dissolved in 50 ml of water and 10 ml of absolute ethyl alcohol, and are stirred and dissolved to prepare a uniform solution. Then, the mixed solution is poured into a reaction kettle, a piece of treated carbon fiber substrate material (the size is 3 cm by 6 cm) is added, and the mixture is placed into an oven to react for 24 hours at the temperature of 200 ℃. And after the temperature of the oven is reduced to room temperature, taking out the carbon fiber composite material, carrying out ultrasonic cleaning, and carrying out vacuum drying at 60 ℃.
Through detection, a (002) crystal face is detected in the molybdenum disulfide supercapacitor electrode material prepared in the example.
Through detection, the electrode material of the molybdenum disulfide supercapacitor prepared by the example is molybdenum disulfide in a metal phase.
The molybdenum disulfide supercapacitor electrode material prepared by the preparation method shows good flexibility performance through detection, and the specific capacitance of the molybdenum disulfide supercapacitor electrode material is obviously changed through bending at different angles. And after repeated bending, the specific capacitance of the capacitor is not changed.
The molybdenum disulfide supercapacitor electrode material prepared by the method has good cycle performance, and 90% of first energy is still stored after 1000 cycles under the current density of 2 amperes per gram.
Example 2
Soaking the carbon fiber material in aqua regia solution, heating at 100 ℃ for 2 hours, and then washing and drying for later use. 1 mmol of sodium molybdate and 10 mmol of L-cysteine are dissolved in 50 ml of water and 10 ml of absolute ethyl alcohol, and are stirred and dissolved to prepare a uniform solution. Then, the mixed solution is poured into a reaction kettle, a piece of treated carbon fiber substrate material (the size is 3 cm by 6 cm) is added, and the mixture is placed into an oven to react for 24 hours at the temperature of 200 ℃. And after the temperature of the oven is reduced to room temperature, taking out the carbon fiber composite material, carrying out ultrasonic cleaning, and carrying out vacuum drying at 60 ℃.
Through detection, a (002) crystal face is detected in the molybdenum disulfide supercapacitor electrode material prepared in the example.
Through detection, the electrode material of the molybdenum disulfide supercapacitor prepared by the example is molybdenum disulfide in a metal phase.
The molybdenum disulfide supercapacitor electrode material prepared by the preparation method shows good flexibility performance through detection, and the specific capacitance of the molybdenum disulfide supercapacitor electrode material is obviously changed through bending at different angles. And after repeated bending, the specific capacitance of the capacitor is not changed.
The molybdenum disulfide supercapacitor electrode material prepared by the method has good cycle performance, and 86% of first energy is still stored after 1000 cycles under the current density of 2 amperes per gram.
Example 3
Soaking the carbon fiber material in aqua regia solution, heating at 100 ℃ for 2 hours, and then washing and drying for later use. 2 mmol of sodium molybdate and 20 mmol of L-cysteine are dissolved in 50 ml of water and 10 ml of absolute ethyl alcohol, and are stirred and dissolved to prepare a uniform solution. Then, the mixed solution is poured into a reaction kettle, a piece of treated carbon fiber substrate material (the size is 3 cm by 6 cm) is added, and the mixture is placed into an oven to react for 24 hours at the temperature of 200 ℃. And after the temperature of the oven is reduced to room temperature, taking out the carbon fiber composite material, carrying out ultrasonic cleaning, and carrying out vacuum drying at 60 ℃.
Through detection, a (002) crystal face is detected in the molybdenum disulfide supercapacitor electrode material prepared in the example.
Through detection, the electrode material of the molybdenum disulfide supercapacitor prepared by the example is molybdenum disulfide in a metal phase.
The molybdenum disulfide supercapacitor electrode material prepared by the preparation method shows good flexibility performance through detection, and the specific capacitance of the molybdenum disulfide supercapacitor electrode material is obviously changed through bending at different angles. And after repeated bending, the specific capacitance of the capacitor is not changed.
Through detection, the molybdenum disulfide supercapacitor electrode material prepared in the example has 79% of first energy preserved after 1000 cycles under the current density of 2 amperes per gram.
The preparation method of the (002) crystal face growth metal phase flexible molybdenum disulfide supercapacitor electrode material prepared by the invention is simple to operate, the molybdenum disulfide flexible electrode material with complete structure and excellent performance can be prepared only in a short time, no complex equipment is needed, the cost is low, the synthesized molybdenum disulfide flexible nano material has large specific surface area and uniform distribution, has large-area exposed (002) active reaction sites and a metal phase structure with higher components, shows higher specific capacitance and stable electrochemical performance, has long cycle life, provides possibility for industrial production, is an excellent supercapacitor electrode material, and has good development prospect. The preparation method is simple and effective, low in cost and environment-friendly.
Claims (3)
1. A preparation method of a metal phase flexible molybdenum disulfide supercapacitor electrode material with a (002) crystal face growth is characterized by comprising the following steps:
(1) uniformly stirring a sulfur source, a molybdenum source, ethanol and water to prepare a precursor solution;
(2) adding the precursor solution into the inner container of the reaction kettle, and adding a piece of carbon fiber substrate material;
(3) putting the reaction kettle into an oven for reaction; after the oven is cooled to room temperature, ultrasonically washing and drying the carbon fiber material to obtain a metal phase flexible molybdenum disulfide supercapacitor electrode material with a (002) crystal face growing; the material is mainly used for flexible supercapacitor electrode materials, and the shape of molybdenum disulfide is a nanosheet structure; in the step (1), the molybdenum source is dodecahydrate and sodium molybdate, the sulfur source is L-cysteine, and the molar ratio of the molybdenum source to the sulfur source is 1: 10; the carbon fiber substrate material is treated by soaking in aqua regia solution, heating at 100 ℃ for 2 hours, washing and drying; the dosage of the molybdenum source in the step (1) is 0.5-2 millimoles, and the dosage of the L-cysteine is 5-20 millimoles; the size of the carbon fiber substrate material was 3 cm by 6 cm.
2. The preparation method of the metal phase flexible molybdenum disulfide supercapacitor electrode material with the (002) crystal face growing according to claim 1, wherein the volume ratio of water to ethanol in the step (1) is 1: 1 to 5: 1, total volume 60 ml.
3. The preparation method of the metal phase flexible molybdenum disulfide supercapacitor electrode material with the (002) crystal face growth according to claim 1, wherein the reaction temperature in the step (3) is 180-220 ℃ and the time is 24-36 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810354978.6A CN108511205B (en) | 2018-04-19 | 2018-04-19 | Preparation method of (002) crystal face grown metal phase flexible molybdenum disulfide supercapacitor electrode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810354978.6A CN108511205B (en) | 2018-04-19 | 2018-04-19 | Preparation method of (002) crystal face grown metal phase flexible molybdenum disulfide supercapacitor electrode material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108511205A CN108511205A (en) | 2018-09-07 |
| CN108511205B true CN108511205B (en) | 2020-06-05 |
Family
ID=63382829
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810354978.6A Expired - Fee Related CN108511205B (en) | 2018-04-19 | 2018-04-19 | Preparation method of (002) crystal face grown metal phase flexible molybdenum disulfide supercapacitor electrode material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108511205B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110258104A (en) * | 2019-07-22 | 2019-09-20 | 信阳学院 | A method of synthesis 1T phase molybdenum disulfide/carbon cloth nanocomposite |
| CN111276676B (en) * | 2020-01-13 | 2022-10-14 | 信阳师范学院 | Preparation method of metal phase vanadium/molybdenum disulfide/carbon cloth sodium ion battery cathode material |
| CN112290003B (en) * | 2020-11-04 | 2021-07-23 | 齐鲁工业大学 | Molybdenum disulfide titanium dioxide cathode material of lithium ion battery and preparation method and application thereof |
| CN113981484B (en) * | 2021-10-25 | 2023-09-22 | 青海大学 | High-purity metal phase molybdenum disulfide array/carbon fiber cloth composite material and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105529448A (en) * | 2016-01-22 | 2016-04-27 | 西北工业大学 | Preparation method for flexible lithium ion battery cathode material |
| CN107285385A (en) * | 2017-07-03 | 2017-10-24 | 上海大学 | A kind of metallicity 1T molybdenum disulfide nano sheet arrays and its preparation method and application |
| CN107316979A (en) * | 2017-06-23 | 2017-11-03 | 湘潭大学 | A kind of molybdenum disulfide/carbon fiber network flexible electrode and its preparation method and application |
| CN107731567A (en) * | 2017-10-19 | 2018-02-23 | 天津工业大学 | Flexible carbon cloth load hollow ball-shape 1T MoS2The preparation method of electrode material for super capacitor |
-
2018
- 2018-04-19 CN CN201810354978.6A patent/CN108511205B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105529448A (en) * | 2016-01-22 | 2016-04-27 | 西北工业大学 | Preparation method for flexible lithium ion battery cathode material |
| CN107316979A (en) * | 2017-06-23 | 2017-11-03 | 湘潭大学 | A kind of molybdenum disulfide/carbon fiber network flexible electrode and its preparation method and application |
| CN107285385A (en) * | 2017-07-03 | 2017-10-24 | 上海大学 | A kind of metallicity 1T molybdenum disulfide nano sheet arrays and its preparation method and application |
| CN107731567A (en) * | 2017-10-19 | 2018-02-23 | 天津工业大学 | Flexible carbon cloth load hollow ball-shape 1T MoS2The preparation method of electrode material for super capacitor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108511205A (en) | 2018-09-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108511205B (en) | Preparation method of (002) crystal face grown metal phase flexible molybdenum disulfide supercapacitor electrode material | |
| CN106356525B (en) | A kind of preparation method of graphene growth in situ FeOOH nano-array lithium ion battery negative materials | |
| CN105280897B (en) | A kind of preparation method of lithium ion battery negative material C/ZnO/Cu composites | |
| CN106952737A (en) | A kind of preparation method of tungsten disulfide flake nano material | |
| CN110518235B (en) | Self-supporting trinickel disulfide electrode and preparation method and application thereof | |
| CN109065873B (en) | Preparation method and material of supported nano-copper mesoporous graphite carbon nitride negative electrode material | |
| CN106299344B (en) | A kind of sodium-ion battery nickel titanate negative electrode material and preparation method thereof | |
| CN107188230A (en) | A kind of molybdenum disulfide carbon is combined bouquet and its preparation method and application | |
| CN110010875A (en) | A kind of preparation method of flake cobalt sulfide composite and flexible carbon cloth electrode material | |
| CN105161690B (en) | The method that molybdenum disulfide charge and discharge cycles ability is improved by doped graphene and titanium dioxide | |
| CN109830657A (en) | A kind of MoS2/MoO2The preparation method of/three-dimensional carbon lithium ion battery negative material | |
| CN111933942A (en) | Sodium ion battery Na meeting high-rate discharge cycle performance2/3Mn1/2Fe1/4Co1/4O2Controllable regulation and control method of anode material | |
| CN103400980A (en) | Iron sesquioxide/nickel oxide core-shell nanorod array film as well as preparation method and application thereof | |
| CN105489899A (en) | Lithium ion battery cathode and preparation method thereof | |
| CN104495787A (en) | Preparation method of negative electrode nano carbon material of lithium ion battery | |
| CN106981626B (en) | A kind of preparation method of tungsten disulfide/Super P sodium-ion battery self-supporting cathode | |
| CN103107307A (en) | Water-solution lithium ion battery negative pole material and preparation method thereof | |
| CN109046418B (en) | Preparation method of nickel phosphide/nitrogen-doped reduced graphite oxide hydrogen evolution composite material | |
| CN110171828A (en) | A kind of FeS nano material and its preparation method and application based on carbon cloth oriented growth | |
| CN103296256B (en) | Method for preparing LiFePO4/C composite material by using sol-gel method | |
| CN113816425B (en) | MoS 2 Nitrogen-doped carbon/modified activated carbon sodium ion battery negative electrode material and preparation method thereof | |
| CN113097473B (en) | Nano-structure anatase titanium dioxide and preparation method and application thereof | |
| CN109950508B (en) | Carbon fiber cloth flexible lithium ion battery negative electrode material and preparation method thereof | |
| CN108963214B (en) | Preparation method of lithium ion battery negative electrode material | |
| CN112430089A (en) | ReO (ReO)3Shear structure MoNb6O18Method for producing materials and use thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20200605 Termination date: 20210419 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |