CN108010733A - A kind of flower-shaped Cu2SnS3The preparation method of flexible super capacitor electrode material - Google Patents

A kind of flower-shaped Cu2SnS3The preparation method of flexible super capacitor electrode material Download PDF

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Publication number
CN108010733A
CN108010733A CN201711415674.8A CN201711415674A CN108010733A CN 108010733 A CN108010733 A CN 108010733A CN 201711415674 A CN201711415674 A CN 201711415674A CN 108010733 A CN108010733 A CN 108010733A
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China
Prior art keywords
super capacitor
sns
flower
shaped
electrode material
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Pending
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CN201711415674.8A
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Chinese (zh)
Inventor
王超
田瀚卿
姜晶
何欣芮
牛夷
张蕊
王楚珺
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University of Electronic Science and Technology of China
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University of Electronic Science and Technology of China
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Priority to CN201711415674.8A priority Critical patent/CN108010733A/en
Publication of CN108010733A publication Critical patent/CN108010733A/en
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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
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • 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)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

A kind of flower-shaped Cu of the disclosure of the invention2SnS3The preparation method of flexible super capacitor electrode material, belongs to synthesis and the preparing technical field of super capacitor material, and in particular to a kind of flower-shaped Cu2SnS3Flexible super capacitor production method.This method reaction prepares flower-shaped Cu2SnS3, preparation method is simple, good crystallinity, there is larger specific surface area and less mesoporous at the same time, more reactivity sites are provided for electrochemical reaction and shorten ion transmission path at the same time, in the aqueous solution of strong basicity, show the specific capacity of superelevation and its excellent high rate performance;Due to being the growth in situ on carbon cloth, the contact resistance of electrode material is reduced;And material crystallinity itself is high, specific capacity is higher, and energy density is excellent, is a kind of potential excellent electrode material for super capacitor.

Description

A kind of flower-shaped Cu2SnS3The preparation method of flexible super capacitor electrode material
Technical field
Synthesis and preparing technical field the invention belongs to super capacitor material, and in particular to a kind of flower-shaped Cu2SnS3 Flexible super capacitor production method.
Background technology
Ultracapacitor is a kind of new type of energy storage device between electrolytic capacitor and battery, has cycle life It is long, can high current charge-discharge the features such as, its application market is wide, is the research hotspot of new energy field.Compared to conventional secondary electricity Pond has many advantages such as power density is big, discharge and recharge is quick, good cycling stability and operating temperature range are wide.According to energy storage machine Ultracapacitor substantially can be divided into two major classes by reason:1 double layer capacitor, is mainly based upon porous electrode/electrolyte interface Accumulation stores electric charge.2 fake capacitance capacitors, are mainly based upon surface of active material and internal Reversible redox reaction To store electric charge.Therefore, electrode material is the core component of ultracapacitor.The extensive mainly various structures of research at present Carbon material, transition metal oxide and conducting polymer.At the same time, metal sulfide also result in the extensive interest of people. This is because common metal sulfide rich reserves and widely distributed in the earth, and material itself is nontoxic, suitable big rule Mould produces.Existing technology prepares Cu at present2SnS3All it is the preferential method using heat sputtering, but it is poor there are crystallinity, at the same time Complex manufacturing technology.
The content of the invention
The present invention is prepared for using high-performance carbon cloth as substrate, the Cu of growth in situ2SnS3Electrode, first Application is in super electricity On container.Many advantages, such as preparation method is simple, and crystallinity is high.
This method single step reaction prepares flower-shaped Cu2SnS3, preparation method is simple, good crystallinity, while has larger Specific surface area and less mesoporous, provides more reactivity sites for electrochemical reaction and shortens ion at the same time and transmit road Footpath, in the aqueous solution of strong basicity, shows the specific capacity of superelevation and its excellent high rate performance.Because the skill of the present invention Art scheme is:A kind of flower-shaped Cu2SnS3The preparation method of flexible super capacitor electrode material, this method include:
Step 1:By CuCl2.2H20、SnCl4, thioacetamide in molar ratio be 2:1:3 ratio after mixing, will Clean carbon cloth is immersed in mixed solution;
Step 2:It is 1 to add volume ratio:1 deionized water and ethylene glycol mixed solution, the deionized water and second two of addition The volume of mixed alkoxide solution is identical with the volume for the mixed solution that step 1 obtains, and is sufficiently mixed uniformly;
Step 3:The solution that step 2 is obtained is placed in high pressure, 200-260 DEG C of dry environment, dry 7-9 hour;
Step 4:After reaction, flower-shaped Cu is attached with carbon cloth2SnS3, using deionized water and washes of absolute alcohol, Carbon cloth after washing is placed in drying process in 60-80 DEG C of vacuum environment;
Step 5:The dry Cu completed2SnS3Positive and negative anodes of the carbon cloth as super capacitor.
This method reaction prepares flower-shaped Cu2SnS3, preparation method is simple, good crystallinity, while has larger ratio table Area and less mesoporous, provides more reactivity sites for electrochemical reaction and shortens ion transmission path at the same time, In the aqueous solution of strong basicity, the specific capacity of superelevation and its excellent high rate performance are shown;Due to being the original position on carbon cloth Growth, reduce the contact resistance of electrode material;And material crystallinity itself is high, specific capacity is higher, and energy density is excellent, is A kind of potential excellent electrode material for super capacitor.
Brief description of the drawings
Fig. 1 is electrode material production process figure of the present invention;
Fig. 2 is the SEM figures for the sample different amplification that instantiation 1 of the present invention is produced;
Fig. 3 is the SEM figures for the sample different amplification that instantiation 2 of the present invention is produced;
Fig. 4 sweeps the cyclic voltammetry curve under speed for electrode material difference of the present invention;
Fig. 5 is the constant current charge-discharge curve under electrode material difference current density of the present invention.
Embodiment
Embodiment 1
Step 1:Flower-shaped Cu2SnS3The synthesis of electrode material:By 4mmol CuCl2.2H20,2mmol SnCl4And 6mmol TAA (thioacetamide), is sufficiently mixed uniformly, 2 hours of strong mixing, are then 2cm*2cm carbon cloths by the area handled well It is put into reaction kettle.Transfer it in reaction kettle, be separately added into the deionized water and ethylene glycol (or poly- second two of equivalent Alcohol), it is 1 to make volume ratio both it:1, reaction kettle is transferred in insulating box, by temperature adjustment to 200 DEG C, keeps the temperature 9 hours. With other preparations Cu2SnS3Reaction is compared, and shortens the reaction time, reduces experimental period.
Step 2:After question response kettle is cooled to room temperature, obtained product deionized water and ethanol are distinguished into centrifuge washing three It is secondary, while obtained carbon cloth is rinsed with deionized water and absolute ethyl alcohol respectively, the product after washing and carbon cloth are placed in 70 DEG C Vacuum drying chamber drying 8 it is small when.
Step 3:The electrode handled well in step 2 is taken out, Cu is loaded with by what is dried2SnS3Carbon cloth be cut out two A quality is almost equal with volume and area is about 1cm2Electrode, separated with hydrophilic glass fibre diaphragm be assembled into it is symmetrical Electrode, instills in the KOH solution of suitable 3mol/L.So as to be made based on Cu2SnS3The flexible super capacitance of redox active Device.
Step 4:The ultracapacitor that step 3 is assembled, which is positioned on electrochemical operation platform, carries out chemical property Test.
Embodiment 2
Step 1:By CuCl2.2H20、SnCl4, thioacetamide in molar ratio be 2:1:3 ratio after mixing, will Clean carbon cloth is immersed in mixed solution;
Step 2:It is 1 to add volume ratio:1 deionized water and ethylene glycol mixed solution, the deionized water and second two of addition The volume of mixed alkoxide solution is identical with the volume for the mixed solution that step 1 obtains, and is sufficiently mixed uniformly;
Step 3:The solution that step 2 is obtained is placed in high pressure, 200 DEG C of dry environment, dry 7 hours;
Step 4:After reaction, flower-shaped Cu is attached with carbon cloth2SnS3, using deionized water and washes of absolute alcohol, Carbon cloth after washing is placed in drying process in 60 DEG C of vacuum environment;
Step 5:The dry Cu completed2SnS3Positive and negative anodes of the carbon cloth as super capacitor.
Fig. 2, Fig. 3:It is the SEM figures for having prepared material, is prepared as indicated by this EXPERIMENTAL EXAMPLE 1 and 2 method of embodiment Cu2SnS3, the flower-shaped structure that is made of nano-sheet.The loose porous structure of two dimension is more advantageous to electric transmission.
Fig. 4:Cu2SnS3Cyclic voltammetry curve under strong alkali solution, as figure shows the material have two it is obvious similar counterfeit The redox peaks of capacitance, in the case where difference sweeps speed, show good cycle performance.
Fig. 5:Cu2SnS3Constant current charge-discharge curve under strong alkali solution, under different current densities, shows good Good high rate performance.

Claims (1)

  1. A kind of 1. flower-shaped Cu2SnS3The preparation method of flexible super capacitor electrode material, this method include:
    Step 1:By CuCl2.2H20、SnCl4, thioacetamide in molar ratio be 2:1:3 ratio after mixing, will be clean Carbon cloth immerse mixed solution in;
    Step 2:It is 1 to add volume ratio:1 deionized water and ethylene glycol mixed solution, the deionized water and ethylene glycol of addition are mixed It is identical with the volume for the mixed solution that step 1 obtains to close the volume of solution, and is sufficiently mixed uniformly;
    Step 3:The solution that step 2 is obtained is placed in high pressure, 200-260 DEG C of dry environment, dry 7-9 hour;
    Step 4:After reaction, flower-shaped Cu is attached with carbon cloth2SnS3, using deionized water and washes of absolute alcohol, washing Carbon cloth afterwards is placed in drying process in 60-80 DEG C of vacuum environment;
    Step 5:The dry Cu completed2SnS3Positive and negative anodes of the carbon cloth as super capacitor.
CN201711415674.8A 2017-12-25 2017-12-25 A kind of flower-shaped Cu2SnS3The preparation method of flexible super capacitor electrode material Pending CN108010733A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110335757A (en) * 2019-04-22 2019-10-15 华南师范大学 A kind of copper and tin sulphur Cu2SnS3/ carbon quantum dot composite material and preparation method and the application in supercapacitor

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102094191A (en) * 2010-12-02 2011-06-15 山东建筑大学 Method for preparing copper tin sulfur film with preferred orientation
CN103977821A (en) * 2014-02-27 2014-08-13 上海大学 Cu3SnS4-graphene composite visible-light-driven photocatalyst and preparation method thereof
CN104773762A (en) * 2015-03-16 2015-07-15 浙江理工大学 NiCo2O4 mesoporous nanotube material grown on carbon fiber cloth and preparation method thereof
CN106207174A (en) * 2016-08-31 2016-12-07 电子科技大学 Cu2snS3nano material and preparation method thereof, lithium ion battery negative and lithium ion battery

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102094191A (en) * 2010-12-02 2011-06-15 山东建筑大学 Method for preparing copper tin sulfur film with preferred orientation
CN103977821A (en) * 2014-02-27 2014-08-13 上海大学 Cu3SnS4-graphene composite visible-light-driven photocatalyst and preparation method thereof
CN104773762A (en) * 2015-03-16 2015-07-15 浙江理工大学 NiCo2O4 mesoporous nanotube material grown on carbon fiber cloth and preparation method thereof
CN106207174A (en) * 2016-08-31 2016-12-07 电子科技大学 Cu2snS3nano material and preparation method thereof, lithium ion battery negative and lithium ion battery

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
CHAO WANG ET AL.: "Facile Synthesis of Different Morphologies of Cu2SnS3 for High-Performance Supercapacitors", 《ACS APPLIED MATERIALS & INTERFACES》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110335757A (en) * 2019-04-22 2019-10-15 华南师范大学 A kind of copper and tin sulphur Cu2SnS3/ carbon quantum dot composite material and preparation method and the application in supercapacitor
CN110335757B (en) * 2019-04-22 2021-07-16 华南师范大学 Copper tin sulfur Cu2SnS3/carbon quantum dot composite material, preparation method thereof and application thereof in super capacitor

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Application publication date: 20180508

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