CN101447338A - SnS/MCNT nanometer combined electrode material for super capacitor and preparation method thereof - Google Patents
SnS/MCNT nanometer combined electrode material for super capacitor and preparation method thereof Download PDFInfo
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- CN101447338A CN101447338A CNA2008102014272A CN200810201427A CN101447338A CN 101447338 A CN101447338 A CN 101447338A CN A2008102014272 A CNA2008102014272 A CN A2008102014272A CN 200810201427 A CN200810201427 A CN 200810201427A CN 101447338 A CN101447338 A CN 101447338A
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Abstract
The invention relates to a SnS/MCNT nanometer combined electrode material for a super capacitor. The SnS/MCNT combined electrode material is prepared by ball milling and compound of SnS and MCNT. Sn powder and S powder are put in a high-energy ball milling pot according to mol ratio of 1 to 1, ethanol is added, the ball milling is carried out for 24 hours, SnS powder is obtained after drying and grinding; MCNT is put in mixed solution with the volume ratio of concentrated nitric acid and concentrated sulphuric acid of 1 to 3, and magnetic stirring and reaction is carried out for 30 minutes at the temperature of 80 DEG C; suction filtration and cleaning are carried out on the mixed solution after reaction repeatedly, and the processed MCNT is obtained after drying and grinding; the prepared SnS powder and the processed MCNT are mixed and put in the high-energy ball milling pot, the ethanol is added, and the ball milling is carried out for 1 hour; and the SnS/MCNT nanometer combined electrode material is obtained after drying and grinding powder. The invention has simple technique, and the obtained SnS/MCNT nanometer combined electrode material has high specific capacitance and good cyclical stability.
Description
Technical field
The present invention relates to a kind of SnS/MCNT nanometer combined electrode material that is used for ultracapacitor and preparation method thereof.
Background technology
Ultracapacitor can provide the specific energy higher than ordinary capacitor, than higher specific power of battery and longer cycle life, is considered to a kind of novel energy of highly effective, can be divided into electric double layer mechanism and pseudo capacitance mechanism according to energy storage mechanism.The electrode material for super capacitor of using electric double layer mechanism mainly comprises the material with carbon element of high-specific surface area, as [A.G.Pandolfo et.al such as active carbon, carbon aerogels, carbon nano-tube and carbon fibers, J.Power Sources 157 (2006) 11-27.], all be the desirable electrode material of ultracapacitor.Although the material with carbon element ultracapacitor is commercial applications tentatively, less because of its specific capacity, level of application thereby be very limited needs to seek new greatly than electric capacity, reliable and stable electrode material for super capacitor.In research in recent years, utilize metal oxide generation redox reaction and the pseudo capacitance that produces carries out the very big interest that the electrochemical capacitor of store energy has caused researcher.Wherein with RuO
2, IrO
2The research of pseudo-capacitance device that Deng metal oxide containing precious metals is electrode material is more.Although the ratio electric capacity of noble metal electrode material is greatly improved than material with carbon element, it costs an arm and a leg and is poisonous, therefore has bigger difficulty aspect commercially producing.Aboundresources, low-cost transition metal oxide MnO
2Deng having and RuO as electrode material for super capacitor
2Similar pseudo capacitance mechanism has bigger ratio electric capacity and specific power, has become one of the research focus in ultracapacitor field, but also has suitable distance apart from industrialization at present.
SnS is a kind of IV-VI family semi-conducting material of orthohormbic structure, is generally layer structure, the layer with layer between combine with Van der Waals force.SnS is at photovoltaic material [N.Sato et al., Sol.Energy Mater.Sol.Cells, 85 (2005) 153-165.B.Subramanian et al., Sol.Energy Mater.Sol.Cells, 79 (2003) 57-65.] and lithium ion battery negative material [X.-L.Gou et al., Mater.Chem.Phys., 93 (2005) 557-566.H.Mukaibo etal., J.Power Sources, 119-121 (2003) 60-63.] etc. the aspect correlative study is all arranged.But SnS is as a kind of potential electrode material for super capacitor, and its relevant exploration is also fewer.M.Jayalakshmi seminar [M.Jayalakshmiet al., Electrochem.Commun., 6 (2004) 1119-1122.] is to being that the ultracapacitor of electrode material has been done preliminary research with SnS.They with Hydrothermal Preparation the SnS nanometer rods, the ultracapacitor performance to SnS in 0.1M KOH and NaCl electrolyte solution is measured.The result shows that SnS possesses good electrochemistry cyclical stability and bigger ratio electric capacity, all is fit to as the electrode material for super capacitor with superperformance in alkalescence and neutral electrolyte.Because hydro thermal method need be implemented under specified temp and high pressure, and equipment is had certain requirement, therefore be unfavorable for applying on a large scale.
Summary of the invention
The present invention discloses a kind of SnS/MCNT nanometer combined electrode material that is used for ultracapacitor and preparation method thereof, adopt industrial widely used high-energy ball-milling process to carry out the compound of the preparation of SnS powder and SnS/MCNT, obtain the SnS/MCNT nanometer combined electrode material.Simple to operate, equipment requirements is not high, and is applied widely.Can be applicable to needs neutral electrolyte, high stability, high power density power supply occasion.
A kind of SnS/MCNT nanometer combined electrode material that is used for ultracapacitor is characterized in that: with the compound SnS/MCNT of the preparing combination electrode material of the same MCNT of SnS (stannous sulfide) (multi-walled carbon nano-tubes) ball milling.
A kind of preparation method who is used for the SnS/MCNT nanometer combined electrode material of ultracapacitor is characterized in that step is as follows:
A) high-energy ball milling prepares the SnS powder:
With Sn powder and S powder in molar ratio 1:1 put into the high-energy ball milling jar, add ethanol, 250 rev/mins of ball milling speed, ball milling 24 hours; The ball milling product is taken out and put into 85 ℃ of freeze-day with constant temperature of drying box 24 hours; Pitchy product powder ground in agate Yan Portland obtain ball milling SnS powder body material;
B) pre-treatment of multi-walled carbon nano-tubes:
MCNT is put into red fuming nitric acid (RFNA) and concentrated sulfuric acid volume ratio is the mixed solution of 1:3,80 ℃ of lower magnetic force stirring reactions 30 minutes; Reacted mixed solution is carried out repeatedly suction filtration, cleaning, and in drying box, dry product, grind the MCNT that obtains handling well after collecting;
C) the SnS powder with the high-energy ball milling preparation grinds the MCNT that obtains handling well after the collection together, puts into the high-energy ball milling jar after the mixing, adds ethanol, 150 rev/mins of ball milling speed, 1 hour ball milling time; After treating that ball grinder is cooled to room temperature, the ball milling product is taken out, 85 ℃ of freeze-day with constant temperature are 24 hours in drying box; At last, the product powder is ground in agate Yan Portland obtain the SnS/MCNT nanometer combined electrode material; Electrolyte is neutral solution.
Described Sn powder footpath is below 74 μ m, and S powder footpath is below 50 μ m.
High-energy ball milling prepares the SnS powder, and ball-milling medium is the agate ball of different-diameter, ratio of grinding media to material 20:1; Be mixed with the SnS/MCNT nano composite material, ball-milling medium is the agate ball of different-diameter, ratio of grinding media to material 5:1.
Be mixed with the SnS/MCNT nano composite material, the mass ratio of SnS and MCNT is 20:80, or 40:60, or 60:40 or 80:20.
Described neutral electrolyte is Na
2SO
4Solution.
The present invention adopts high-energy ball milling method to prepare nanometer SnS powder, it is mixed obtaining the SnS/MCNT nanometer combined electrode material by the low speed ball milling with the MCNT that handles well.SnS has bigger ratio electric capacity and good cyclical stability as the pseudo capacitance electrode material.In the SnS/MCNT compound system, the MCNT good electrical conductivity is that SnS discharges more pseudo capacitance and played important facilitation in the anodizing reduction process, the ratio electric capacity of the nano combined system of SnS/MCNT that has improved.
Advantage of the present invention and good effect are: abundant raw material, preparation technology are simple, do not need complex apparatus.The SnS/MCNT nanometer combined electrode material that obtains is than electric capacity height, good cycling stability; At neutral Na
2SO
4High specific capacity and stable operating state are arranged in the solution, and can be applicable to needs neutral electrolyte, high stability, high power density power supply occasion.
Description of drawings
Fig. 1 is the cyclic voltammetry scan figure of electrode material;
Fig. 2 is the constant current charge-discharge curve of electrode material.
(a)：20％SnS/80％MCNT；(b)：40％SnS/60％MCNT；
(c)：60％SnS/40％MCNT；(d)：80％SnS/20％MCNT。
As can be seen from Figure 1, the cyclic voltammetry curve profile similarity of different proportioning SnS/MCNT nanometer combined electrodes illustrates that their electrochemical reaction process has similitude.
As can be seen from Figure 2, every kind of electrode material all has typical ultracapacitor charging and discharging curve, and the time that discharges and recharges changes with the variation of compound proportioning.
Embodiment
Below in conjunction with drawings and Examples the present invention is done to describe in further detail, but present embodiment is not limited to the present invention, every employing similarity method of the present invention and similar variation thereof all should be listed protection scope of the present invention in.
Embodiment 1;
High-energy ball milling prepares the SnS powder.With particle diameter is that Sn powder and the particle diameter of 74 μ m is the S powder of 50 μ m, by etc. mol ratio put into high-energy planetary formula ball grinder; Ball-milling medium is the agate ball of different-diameter, ratio of grinding media to material 20:1; The ball grinder volume is 250ml; Add small amount of ethanol and prevent caking, 250 rev/mins of ball milling speed, ball milling is after 24 hours, and it is stand-by the ball milling product to be taken out and puts into 85 ℃ of freeze-day with constant temperature of drying box 24 hours.MCNT is put into the mixed solution of red fuming nitric acid (RFNA) and concentrated sulfuric acid volume ratio 1:3,80 ℃ of lower magnetic force stirring reactions 30 minutes.To reaction solution suction filtration, cleaning repeatedly, and the MCNT that oven dry obtains handling well in drying box.The SnS of preparation and the MCNT that handles well are put into high-energy planetary formula ball grinder according to mass ratio 20:80; Ball-milling medium is the agate ball of different-diameter, ratio of grinding media to material 5:1; The ball grinder volume is 250ml; Add small amount of ethanol and prevent caking, 150 rev/mins of ball milling speed, ball milling obtained the SnS/MCNT nanometer combined electrode material in 1 hour.
With the SnS/MCNT nanometer combined electrode material for preparing is work electrode, and the nickel sheet is an auxiliary electrode, and Ag/AgCl is a reference electrode, 0.1M Na
2SO
4Be electrolyte, form three electrode test systems and carry out electrochemical property test.Cyclic voltammetry scan speed 10mV/s, sweep interval-0.2～0.8V; The constant current charge-discharge electric current is 200mA/g, voltage range-0.2～0.8V.Nanometer combined electrode is 30.3F/g than electric capacity after 500 circulations, and enclosed pasture efficient remains on more than 90%.
Embodiment 2:
It is described to press embodiment 1, prepares the SnS/MCNT nanometer combined electrode material with SnS and MCNT mass ratio 40:60; With the SnS/MCNT nanometer combined electrode material for preparing is work electrode, and the nickel sheet is an auxiliary electrode, and Ag/AgCl is a reference electrode, 0.1MNa
2SO
4Be electrolyte, form three electrode test systems and carry out electrochemical property test.Cyclic voltammetry scan speed 10mV/s, sweep interval-0.2～0.8V; The constant current charge-discharge electric current is 200mA/g, voltage range-0.2～0.8V.Nanometer combined electrode is 43.8F/g than electric capacity after 500 circulations, and enclosed pasture efficient remains on more than 90%.
Embodiment 3:
It is described to press embodiment 1, prepares the SnS/MCNT nanometer combined electrode material with SnS and MCNT mass ratio 60:40; With the SnS/MCNT nanometer combined electrode material for preparing is work electrode, and the nickel sheet is an auxiliary electrode, and Ag/AgCl is a reference electrode, 0.1MNa
2SO
4Be electrolyte, form three electrode test systems and carry out electrochemical property test.Cyclic voltammetry scan speed 10mV/s, sweep interval-0.2～0.8V; The constant current charge-discharge electric current is 200mA/g, voltage range-0.2～0.8V.Nanometer combined electrode is 52.1F/g than electric capacity after 500 circulations, and enclosed pasture efficient remains on more than 90%.
Embodiment 4:
It is described to press embodiment 1, prepares the SnS/MCNT nanometer combined electrode material with SnS and MCNT mass ratio 80:20; With the SnS/MCNT nanometer combined electrode material for preparing is work electrode, and the nickel sheet is an auxiliary electrode, and Ag/AgCl is a reference electrode, 0.1M Na
2SO
4Be electrolyte, form three electrode test systems and carry out electrochemical property test.Cyclic voltammetry scan speed 10mV/s, sweep interval-0.2～0.8V; The constant current charge-discharge electric current is 200mA/g, voltage range-0.2～0.8V.Nanometer combined electrode is 62.5F/g than electric capacity after 500 circulations, and enclosed pasture efficient remains on more than 90%.
Claims (6)
1. a SnS/MCNT nanometer combined electrode material that is used for ultracapacitor is characterized in that: with the compound SnS/MCNT of the preparing combination electrode material of the same MCNT of SnS (stannous sulfide) (multi-walled carbon nano-tubes) ball milling.
2. preparation method who is used for the SnS/MCNT nanometer combined electrode material of ultracapacitor is characterized in that step is as follows:
A) high-energy ball milling prepares the SnS powder:
With Sn powder and S powder in molar ratio 1:1 put into the high-energy ball milling jar, add ethanol, 250 rev/mins of ball milling speed, ball milling 24 hours; The ball milling product is taken out and put into 85 ° of C freeze-day with constant temperature of drying box 24 hours; Pitchy product powder ground in agate Yan Portland obtain ball milling SnS powder body material;
B) pre-treatment of multi-walled carbon nano-tubes:
MCNT is put into red fuming nitric acid (RFNA) and concentrated sulfuric acid volume ratio is the mixed solution of 1:3,80 ° of C lower magnetic force stirring reactions 30 minutes; Reacted mixed solution is carried out repeatedly suction filtration, cleaning, and in drying box, dry product, grind the MCNT that obtains handling well after collecting;
C) the SnS powder with the high-energy ball milling preparation grinds the MCNT that obtains handling well after the collection together, puts into the high-energy ball milling jar after the mixing, adds ethanol, 150 rev/mins of ball milling speed, 1 hour ball milling time; After treating that ball grinder is cooled to room temperature, the ball milling product is taken out, 85 ° of C freeze-day with constant temperature are 24 hours in drying box; At last, the product powder is ground in agate Yan Portland obtain the SnS/MCNT nanometer combined electrode material; Electrolyte is neutral solution.
3. a kind of preparation method who is used for the SnS/MCNT nanometer combined electrode material of ultracapacitor according to claim 2 is characterized in that: Sn powder footpath is below 74 μ m, and S powder footpath is below 50 μ m.
4. a kind of preparation method who is used for the SnS/MCNT nanometer combined electrode material of ultracapacitor according to claim 2, it is characterized in that: high-energy ball milling prepares the SnS powder, and ball-milling medium is the agate ball of different-diameter, ratio of grinding media to material 20:1; Be mixed with the SnS/MCNT nano composite material, ball-milling medium is the agate ball of different-diameter, ratio of grinding media to material 5:1.
5. a kind of preparation method who is used for the SnS/MCNT nanometer combined electrode material of ultracapacitor according to claim 2, it is characterized in that: be mixed with the SnS/MCNT nano composite material, the mass ratio of SnS and MCNT is 20:80, or 40:60, or 60:40 or 80:20.
6. a kind of preparation method who is used for the SnS/MCNT nanometer combined electrode material of ultracapacitor according to claim 2, it is characterized in that: described neutral electrolyte is Na
2SO
4Solution.
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| CN102502791A (en) * | 2011-11-23 | 2012-06-20 | 陕西科技大学 | Method for preparing flower-cluster-shaped tin sulfide (SnS) nanometer particles by microwave hydrothermal method |
| CN106887578A (en) * | 2017-04-01 | 2017-06-23 | 中南大学 | A kind of artificial gold/CNT composite Nano negative material and preparation method thereof |
| CN107316989A (en) * | 2017-05-17 | 2017-11-03 | 华南理工大学 | A kind of tin sulfide/sulphur/few layer graphene composite and its preparation method and application |
| CN109638249A (en) * | 2018-12-10 | 2019-04-16 | 桂林理工大学 | Mineral/carbon/heat treatment carbonmaterials as anode preparation method for lithium ion battery |
| CN109659524A (en) * | 2018-12-10 | 2019-04-19 | 桂林理工大学 | Mineral/carbon compound cathode materials preparation method for lithium ion battery |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102502791A (en) * | 2011-11-23 | 2012-06-20 | 陕西科技大学 | Method for preparing flower-cluster-shaped tin sulfide (SnS) nanometer particles by microwave hydrothermal method |
| CN106887578A (en) * | 2017-04-01 | 2017-06-23 | 中南大学 | A kind of artificial gold/CNT composite Nano negative material and preparation method thereof |
| CN106887578B (en) * | 2017-04-01 | 2020-02-21 | 中南大学 | Tin sulfide/carbon nano tube composite nano negative electrode material and preparation method thereof |
| CN107316989A (en) * | 2017-05-17 | 2017-11-03 | 华南理工大学 | A kind of tin sulfide/sulphur/few layer graphene composite and its preparation method and application |
| CN107316989B (en) * | 2017-05-17 | 2020-05-22 | 华南理工大学 | Tin sulfide/sulfur/few-layer graphene composite material and preparation method and application thereof |
| CN109638249A (en) * | 2018-12-10 | 2019-04-16 | 桂林理工大学 | Mineral/carbon/heat treatment carbonmaterials as anode preparation method for lithium ion battery |
| CN109659524A (en) * | 2018-12-10 | 2019-04-19 | 桂林理工大学 | Mineral/carbon compound cathode materials preparation method for lithium ion battery |
| CN111416124A (en) * | 2020-03-27 | 2020-07-14 | 陕西科技大学 | Self-standing Sn-SnS/CNTs @ C flexible film and preparation and application thereof |
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Application publication date: 20090603 Assignee: Jiangsu Yueda New Material Technology Co., Ltd. Assignor: Shanghai No.2 Polytechnic Univ. Contract record no.: 2013320000263 Denomination of invention: Method for preparing SnS/MCNT nano composite electrode material used for super capacitor Granted publication date: 20120222 License type: Exclusive License Record date: 20130326 |
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