CN102592839A - Graphene and silver sulfide nano composite material serving as supercapacitor electrode and preparation method for graphene and silver sulfide nano composite material - Google Patents

Graphene and silver sulfide nano composite material serving as supercapacitor electrode and preparation method for graphene and silver sulfide nano composite material Download PDF

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Publication number
CN102592839A
CN102592839A CN2012100661452A CN201210066145A CN102592839A CN 102592839 A CN102592839 A CN 102592839A CN 2012100661452 A CN2012100661452 A CN 2012100661452A CN 201210066145 A CN201210066145 A CN 201210066145A CN 102592839 A CN102592839 A CN 102592839A
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China
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graphene
composite material
silver sulfide
nano composite
sulfide nano
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陈玉金
李丽
朱春玲
王铁石
俞海龙
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Harbin Engineering University
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Harbin Engineering University
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    • 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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Abstract

The invention provides a graphene and silver sulfide nano composite material serving as a supercapacitor electrode and a preparation method for the graphene and silver sulfide nano composite material. The method comprises the following steps of: (1) adding 0.02 to 0.05g of AgNO3 into 15ml of distilled water, adding 0.02 to 0.05g of grapheme, performing ultrasonic treatment for 30 to 35 minutes to uniformly disperse reactants, adding 15 to 20ml of 0.2M ethanol solution of thioacetamide, and performing ultrasonic treatment again for 10 to 15 minutes to obtain reaction liquid; (2) transferring the reaction liquid into a 45ml polytetrafluoroethylene autoclave, reacting the mixture for 12 hours at 80 to 150 DEG C, performing suction filtration on the obtained product, and washing off the residual thioacetamide; and (3) drying the product for 12 hours at 40 DEG C in vacuum to obtain the graphene and silver sulfide nano composite material serving as the supercapacitor electrode. The specific capacity of the graphene and silver sulfide nano composite material is two times that of pure silver sulfide; moreover, the graphene and silver sulfide nano composite material has a stable charging and discharging platform. The composite material prepared by the method is light, facilitates industrial production and is wide in application range; and furthermore, the cost is reduced.

Description

Graphene and silver sulfide nano composite material and method for making as electrode of super capacitor
Technical field
The present invention relates to a kind of nano composite material, the present invention also relates to a kind of preparation method of nano composite material.Specifically a kind of Graphene and silver sulfide nano composite material as electrode of super capacitor and preparation method thereof.
Background technology
Become today of main body day by day in energy-conserving and environment-protective; Ultracapacitor is as a kind of novel energy storage device, has to discharge and recharge fast, environment is not polluted, and advantage such as have extended cycle life; Etc. characteristics and advantage; Can replace traditional storage battery in some field, become the new century new green power, its application more and more causes the attention of countries in the world.
As a kind of novel energy storage device, has super charge storage ability.On energy storage mechanism, it is highly reversible.Life-span is very long, can dash times without number for ten million time, discharge, and have very big electric current; Also have very wide voltage range and operating temperature range, it has the big electric current fast charging and discharging characteristic of traditional capacitor and the energy storage characteristic of battery concurrently, has filled up the blank of specific energy and specific power between ordinary capacitor and the battery; While is both defectives of customer service again, have both had the energy storage characteristic of battery, have and have the power characteristic of capacitor; It than the energy density of traditional electrochemical capacitor high thousands of times it can unconfined acceptance discharge many times and charge; But general ultracapacitor also has its weakness, is exactly that the energy filling rate is limited.
The per 0.4536 kilogram stored energy of high-end ultracapacitor on today market has only 1/25 of lithium battery.Research mainly contains metal sulfide and polymer as super capacitor anode material at present; Wherein ZnS/GO cyclic voltammetry specific capacity is about 114.6F/g; Active carbon has high specific capacity, after the KOH activation, and its specific capacity of cyclic voltammetry test 202.8F/g; The nitrogenous material with carbon element of melamine resin base after the activation, cyclic voltammetry gets specific capacity and also is merely 230.7F/g.
Therefore, how improving the specific capacity of nano composite material as super capacitor anode, improve the stability of material in cyclic process, is one of current main difficult technical.
Summary of the invention
The object of the present invention is to provide a kind of specific capacity high, the stable strong Graphene and the silver sulfide nano composite material of constant current charge-discharge as electrode of super capacitor.The present invention also aims to provide a kind of simple to operate, be suitable for suitability for industrialized production as the Graphene of electrode of super capacitor and the method for making of silver sulfide nano composite material.
The objective of the invention is to realize like this:
Graphene and silver sulfide nano composite material as electrode of super capacitor of the present invention is that 0.02-0.05 is restrained AgNO 3Add in 15 ml distilled waters, add 0.02-0.05 gram Graphene, sonicated 30-35 minute; Add 15-20ml concentration again and be ultrasonic again 10-15 minute of the ethanolic solution of 0.2M thioacetamide, put into autoclave, at 80-150 ℃ of reaction 12 hours down, suction filtration; At 12 hours resulting products of 40 ℃ of vacuumizes.
Graphene and the method for making of silver sulfide nano composite material as electrode of super capacitor of the present invention comprises the steps:
(1) 0.02-0.05 is restrained AgNO 3Add in 15 ml distilled waters, add 0.02-0.05 gram Graphene, sonicated 30-35 minute, reactant is uniformly dispersed, the ethanolic solution that adds 15-20ml concentration again and be the 0.2M thioacetamide obtained reactant liquor in ultrasonic again 10-15 minute;
(2) said reactant liquor is changed in the polytetrafluoroethylene autoclave of capacity 45ml, reacted 12 hours down at temperature 80-150 ℃, with the product suction filtration that obtains, the remaining thioacetamide of flush away;
(3) obtained Graphene and silver sulfide nano composite material in 12 hours 40 ℃ of vacuumizes as electrode of super capacitor.
Graphene of the present invention and silver sulfide nano composite material and preparation electrode of super capacitor; Its method is: Graphene/silver sulfide nano composite material prepares 80wt% Graphene/silver sulfide-conductive carbon-ptfe emulsion composite material; Smear; It is evenly coated in through on the nickel screen of purified treatment, and compressing tablet is tested after dry 12 hours.Assembling experiment capacitor at last utilizes blue electrical testing system to carry out cyclic voltammetric, impedance and time-measuring electric potential test.
The invention provides a kind of Graphene/silver sulfide nano composite material and method for making as electrode of super capacitor.Utilizing Graphene/silver sulfide-conductive carbon-ptfe emulsion composite material, is 1cm at its coating area 2The time, cyclic voltammetry records specific capacity can be stabilized in 289.23F/g, and chronoptentiometry records specific capacity and can be stabilized in more than the 220F/g.Graphene/silver sulfide nano composite material exceeds one times than the specific capacity of pure silver sulfide, and has stable charge and discharge platform.
Another advantage of the present invention is to use Graphene/silver sulfide nano composite material to do electrode; Reduced the consumption of silver sulfide when increasing specific capacity; And the price of silver is higher, therefore prepares AgNO in the process with this composite material than reducing Graphene/silver sulfide nano composite material greatly with pure silver sulfide cost 3Consumption is merely 20-40wt%, so materials still less, the composite material quality of making is lighter, more helps suitability for industrialized production, reduces cost, and uses also more extensive simultaneously.
Description of drawings
Fig. 1 is the transmission electron microscope picture of Graphene/silver sulfide nano composite material.
Fig. 2 is the XRD figure spectrum of Graphene/silver sulfide nano composite material.
Fig. 3 is that the cyclic voltammetry that contains 40wt% Graphene/silver sulfide-conductive carbon-ptfe emulsion composite material is measured curve.
Embodiment
For example the present invention is done in more detail below and describes:
Embodiment 1:
(1) gets the beaker of 100 milliliters of capacity, add 15 ml distilled waters, add 0.02-0.05 gram AgNO then 3, in solution, add 0.05 gram Graphene again, ultrasonic about 30 minutes, its dissolving is disperseed.The thioacetyl amine aqueous solution of preparation 0.2M takes by weighing the thioacetamide of about 0.235g, is dissolved in the 15ml ethanolic solution, and gained solution is joined in the former ultrasonic solution, continues ultrasonic about 10 minutes.
(2) after ultrasonic reactant liquor is changed in the polytetrafluoroethylene autoclave of capacity 45ml, put into drying box, the reaction 12 hours down of 120 ℃ of reaction temperatures, with the product suction filtration that obtains, the remaining thioacetamide of flush away.
Embodiment 2:
(1) gets the beaker of 100 milliliters of capacity, add 15 ml distilled waters, add 0.02-0.05 gram AgNO then 3, in solution, add 0.02 gram Graphene again, ultrasonic about 30 minutes, its dissolving is disperseed.The thioacetyl amine aqueous solution of preparation 0.2M takes by weighing the thioacetamide of about 0.235g, is dissolved in the 15ml ethanolic solution, and gained solution is joined in the former ultrasonic solution, continues ultrasonic about 10 minutes.
(2) after ultrasonic reactant liquor is changed in the polytetrafluoroethylene autoclave of capacity 45ml, put into drying box, the reaction 12 hours down of 100 ℃ of reaction temperatures, with the product suction filtration that obtains, the remaining thioacetamide of flush away.
Embodiment 3:
(1) gets the beaker of 100 milliliters of capacity, add 15 ml distilled waters, add 0.02-0.05 gram AgNO then 3, in solution, add 0.03 gram Graphene again, ultrasonic about 30 minutes, its dissolving is disperseed.The thioacetyl amine aqueous solution of preparation 0.2M takes by weighing the thioacetamide of about 0.235g, is dissolved in the 15ml ethanolic solution, and gained solution is joined in the former ultrasonic solution, continues ultrasonic about 10 minutes.
(2) after ultrasonic reactant liquor is changed in the polytetrafluoroethylene autoclave of capacity 45ml, put into drying box, the reaction 12 hours down of 150 ℃ of reaction temperatures, with the product suction filtration that obtains, the remaining thioacetamide of flush away.
At last, the product that obtains is carried out suction filtration, 40 ℃ of vacuumizes, Graphene/silver sulfide nano composite material is just made by top process.

Claims (2)

1. Graphene and silver sulfide nano composite material as an electrode of super capacitor is characterized in that it being that 0.02-0.05 is restrained AgNO 3Add in 15 ml distilled waters, add 0.02-0.05 gram Graphene, sonicated 30-35 minute; Add 15-20ml concentration again and be ultrasonic again 10-15 minute of the ethanolic solution of 0.2M thioacetamide, put into autoclave, at 80-150 ℃ of reaction 12 hours down, suction filtration; At 12 hours resulting products of 40 ℃ of vacuumizes.
2. one kind is used as the Graphene of electrode of super capacitor and the method for making of silver sulfide nano composite material, it is characterized in that comprising the steps:
(1) 0.02-0.05 is restrained AgNO 3Add in 15 ml distilled waters, add 0.02-0.05 gram Graphene, sonicated 30-35 minute, reactant is uniformly dispersed, the ethanolic solution that adds 15-20ml concentration again and be the 0.2M thioacetamide obtained reactant liquor in ultrasonic again 10-15 minute;
(2) said reactant liquor is changed in the polytetrafluoroethylene autoclave of capacity 45ml, reacted 12 hours down at temperature 80-150 ℃, with the product suction filtration that obtains, the remaining thioacetamide of flush away;
(3) obtained Graphene and silver sulfide nano composite material in 12 hours 40 ℃ of vacuumizes as electrode of super capacitor.
CN2012100661452A 2012-03-14 2012-03-14 Graphene and silver sulfide nano composite material serving as supercapacitor electrode and preparation method for graphene and silver sulfide nano composite material Pending CN102592839A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103413696A (en) * 2013-08-29 2013-11-27 电子科技大学 Method for manufacturing flexible electrode decorated by nano-silver colloid
CN104923260A (en) * 2015-05-12 2015-09-23 山东科技大学 Preparation method for silver sulfide-montmorillonite nanocomposite material
CN109364950A (en) * 2018-10-16 2019-02-22 湖南文理学院 A kind of graphene/metal sulfide multi-stage nano material and its green synthesis method

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101362947A (en) * 2008-08-11 2009-02-11 中国科学院长春应用化学研究所 Method for synthesizing near-infrared light argentic sulfide nanocrystalline coated by ligand

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101362947A (en) * 2008-08-11 2009-02-11 中国科学院长春应用化学研究所 Method for synthesizing near-infrared light argentic sulfide nanocrystalline coated by ligand

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ZUNLI MO ET AL.: "Graphene sheets/Ag2S nanocomposites: Synthesis and their application in supercapacitor materials", 《MATERIALS LETTERS》, 1 February 2012 (2012-02-01) *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103413696A (en) * 2013-08-29 2013-11-27 电子科技大学 Method for manufacturing flexible electrode decorated by nano-silver colloid
CN103413696B (en) * 2013-08-29 2015-12-23 电子科技大学 A kind of method manufacturing the flexible electrode that nano silver colloid is modified
CN104923260A (en) * 2015-05-12 2015-09-23 山东科技大学 Preparation method for silver sulfide-montmorillonite nanocomposite material
CN109364950A (en) * 2018-10-16 2019-02-22 湖南文理学院 A kind of graphene/metal sulfide multi-stage nano material and its green synthesis method

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Application publication date: 20120718