CN108735987A - A kind of tin vanadium cobalt manganese composite oxide nano particle and preparation method thereof - Google Patents
A kind of tin vanadium cobalt manganese composite oxide nano particle and preparation method thereof Download PDFInfo
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- CN108735987A CN108735987A CN201810345336.XA CN201810345336A CN108735987A CN 108735987 A CN108735987 A CN 108735987A CN 201810345336 A CN201810345336 A CN 201810345336A CN 108735987 A CN108735987 A CN 108735987A
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Abstract
The invention discloses a kind of tin vanadium cobalt manganese composite oxide nano particles and preparation method thereof, by a certain amount of manganese acetate in the present invention, cobalt acetate, vanadium acetylacetonate, ethanedioic acid dibutyl tin is dissolved in the n,N-Dimethylformamide and ethyl alcohol of certain volume, and suitable polyvinylpyrrolidone is then added, stirring, obtains the precursor mixture solution of brownish red；Then electrostatic spinning is carried out under certain voltage, flow rate and certain relative humidity atmosphere；Then electrostatic spinning product is sintered to obtain tin vanadium cobalt manganese composite oxide nano particle.Electrochemistry experiment proves tin vanadium cobalt manganese composite oxide nano particle prepared by this method, has broad application prospects as lithium ion battery negative material.Easy to operate in whole preparation process, cost of material is low, and equipment investment is few, suitable for mass production.
Description
Technical field
The invention belongs to Material Fields, and in particular to arrive a kind of tin vanadium cobalt manganese composite oxide nano particle and its preparation side
Method.
Background technology
Nano material has series of characteristics, such as quantum size effect, small-size effect, skin effect and quantum tunneling effect
It answers, thus brings dramatically different in light, electricity, magnetic, heat, sound or even superconduction etc. and macroscopic properties so that they are in magnetic material
The background of material, electronic material, optical material, novel battery etc. extensive application.
Nano material also has large specific surface area, high surface activity, ion diffusion path is short, wriggling is strong and plasticity is high etc.
Feature is applied to lithium ion battery electrode material and is remarkably improved de-/embedding lithium capacity and extends the recycling longevity of electrode
Life and improve electrode material and electrolyte solution wellability (Li Hong et al., lithium ion cell nano investigation of materials, electrochemistry,
2000,6(2):131-145；Yellow-study outstanding person et al., nanometer lithium storage materials and lithium ion battery, physics, 2002,31 (7):444-
449；Farrington G C et al., J.Electrochem.Soc., 1996,143,3590).Tin base cathode material theory specific volume
Amount is higher, and intercalation potential is relatively low in charge and discharge process, and there is no solvents to be total to imbedding problem, has a safety feature, while having more
High energy density per unit volume and specific energy, therefore the materials such as the oxide of tin, Sn-polymetallic orefield are by more and more
It pays close attention to (Wu Guoliang et al., the current situation and development of lithium ion battery negative material, battery, 2001,31,54-57).Tin-oxide
SnOXThough having very high Reversible lithium insertion capacity, irreversible capacity is higher for the first time, shows poor cycle performance.Vanadate
(V in compoundxOy) layer structure is typically comprised, it is very useful to Li+Insertion and abjection, simultaneously because vanadate has
Insoluble in electrolyte solution characteristic.Therefore, rely on the excellent chemical property of vanadate, as the research of lithium battery material,
Also gradually paid attention in recent years.Lee in 2014 steps on soldier et al. and is prepared for monodispersed M phase hypovanadic oxides nanometer using hydro-thermal method
Particle (preparation method of monodispersed M phase hypovanadic oxides nano particle, Publication No. CN104071843A).But vanadate chemical combination
For object during the circulating phase-change of deintercalation Li, irreversible transition therein will lead to the decaying of charging and discharging capabilities, and capacity is caused to damage
It loses (Jin K et al., Journal of power sources, 1999,83 (1), 79-83).Currently, cobalt system positive electrode and its
Modified material is still occupied an leading position on the market.2014, king was prepared for cobaltosic oxide class ball at drive et al. using hydro-thermal method
Type particle is used for the positive electrode of lithium ion battery, and has inquired into its chemical property (Wang Juncheng et al., oxidation of LITHIUM BATTERY four three
Cobalt process study, Metallic Functional Materials, 2014,21 (2):36-40).But the thermal stability of material still has to be hoisted.For
Manganese systems material, can be used as the manganese source for preparing lithium manganate having spinel structure has MnO2、Mn2O3、Mn3O4、MnCO3The compound of equal manganese.
2006, Fang et al. was prepared for LiNi with ball-milling method0.5Mn1.5O4, and probed into the material and filling after lithium ion battery is made
Discharge cycle performance (Fang et al., Mater Lett., 2006,60 (9-10):1273-1275).Chen Li cuckoos et al. are with manganese sulfate
For raw material, the mangano-manganic oxide product being prepared using air blast oxidizing process (use by Chen Lijuan et al., positive electrode material of lithium secondary cell
The preparation research of mangano-manganic oxide, using chemical industry, 2012,41 (3):473-479).But manganate is as lithium ion battery material
In application aspect, there is also recycle the problems such as number is not ideal enough.To further increase the electrochemistry of lithium ion battery
Can, the present invention is prepared for a kind of tin vanadium cobalt manganese composite oxide (SnO using electrostatic spinning technique2/VO2/CoO/Mn3O4) nanometer
Particle.
Invention content
The technical problem to be solved by the present invention is to be directed to the prior art, a kind of tin vanadium cobalt manganese composite oxide is provided
(SnO2/VO2/CoO/Mn3O4) nano particle and preparation method thereof.
The present invention solves the technical solution that above-mentioned technical problem is taken：A kind of tin vanadium cobalt manganese composite oxide nanometer
The preparation method of grain, it is main that the preparation method, which is used with manganese acetate, cobalt acetate, vanadium acetylacetonate, ethanedioic acid dibutyl tin,
Raw material, it is adhesive that suitable macromolecule, which is added, and electrostatic spinning technique is utilized under high voltage condition, prepares electrostatic spinning production
Product are then sintered in Muffle furnace, obtain a kind of tin vanadium cobalt manganese composite oxide (SnO2/VO2/CoO/Mn3O4) nanometer
Grain, specifically includes following steps：
1) a certain amount of manganese acetate (Mn (CH are weighed3COO)2), cobalt acetate (Co (CH3COO)2), vanadium acetylacetonate
(C15H21O6V), ethanedioic acid dibutyl tin (C12H24O4Sn) it is dissolved in the N,N-dimethylformamide (DMF) and ethyl alcohol of certain volume
(CH3CH2OH in), it is adhesive PVP (K-120, polyvinylpyrrolidone) that suitable macromolecule, which is then added, stirs 6~12h,
Obtain the precursor mixture solution of brownish red, the molar ratio of metallic element is Mn in mixture solution：Co：V：Sn=3：1：1：
1；2) by the precursor mixture solution of above-mentioned brownish red under 18~20kv voltages and 0.8~1.0mL/h flow rates, relative humidity
To carry out electrostatic spinning under 30~40% atmosphere；
3) the electrostatic spinning product of above-mentioned gained is placed in crucible, crucible is then positioned over 800-900 in Muffle furnace
DEG C sintering 5-7h, be then naturally cooling to room temperature, obtain a kind of tin vanadium cobalt manganese composite oxide SnO2/VO2/CoO/Mn3O4Nanometer
Particle.
The present invention also provides the purposes for the tin vanadium cobalt manganese composite oxide nano particle that the preparation method obtains, should
For nano particle as lithium ion battery negative material, first discharge specific capacity is 478.7mAh g-1, charge and discharge after recycling 85 times
Specific capacity is maintained at 390mAh g-1More than, efficiency for charge-discharge still keeps 99% or more after recycling 85 times.
Compared with prior art, the features of the present invention is as follows：
A kind of tin vanadium cobalt manganese composite oxide (SnO prepared by the present invention2/VO2/CoO/Mn3O4) nano particle performance is excellent
Different, it is 478.7mAh g that charge-discharge test, which shows the nano particle as cell negative electrode material first discharge specific capacity,-1, cycle 85
Charging and discharging capacity is maintained at 390mAh g after secondary-1More than, efficiency for charge-discharge still keeps 99% or more (Fig. 3) after recycling 85 times.
Description of the drawings
Fig. 1 is the XRD diagram of tin vanadium cobalt manganese composite oxide nano particle produced by the present invention；
Fig. 2 is that the SEM of tin vanadium cobalt manganese composite oxide nano particle produced by the present invention schemes；
Fig. 3 is chemical property of the tin vanadium cobalt manganese composite oxide nano particle produced by the present invention as battery material
Figure.
Specific implementation mode
Present invention is further described in detail with reference to embodiments.
Embodiment 1
Weigh the manganese acetate (Mn (CH of 3.0mmol (0.519g)3COO)2), 1.0mmol (0.177g) cobalt acetates (Co
(CH3COO)2), 1.0mmol (0.348g) vanadium acetylacetonates (C15H21O6) and 1.0mmol (0.351g) ethanedioic acid dibutyl tin V
(C12H24O4Sn it) is dissolved in the n,N-Dimethylformamide (DMF) and the ethyl alcohol of 10mL of 10mL, the PVP (K- of 3.0g is then added
120, polyvinylpyrrolidone), 6h is stirred, the precursor mixture solution of brownish red is obtained；By the presoma of above-mentioned brownish red
Mixture solution carries out electrostatic spinning under 18kv voltages and 0.8mL/h flow rates, under the atmosphere that relative humidity is 30%；It will be above-mentioned
The electrostatic spinning product of gained is placed in crucible, crucible is then positioned over 800 DEG C of sintering 5h in Muffle furnace, then Temperature fall
To room temperature, a kind of tin vanadium cobalt manganese composite oxide nano particle is obtained.The tin vanadium cobalt manganese composite oxide nano particle that will be obtained
Powder x-ray diffraction analysis (Fig. 1) is carried out, determines that the skeleton symbol of the composite oxides is SnO2/VO2/CoO/Mn3O4, scanning
It is nano particle shape (Fig. 2) that Electronic Speculum SEM, which observes its pattern, its performance (Fig. 3) is tested with electrochemical test.
Embodiment 2
Weigh the manganese acetate (Mn (CH of 1.5mmol (0.260g)3COO)2), 0.5mmol (0.0885g) cobalt acetates (Co
(CH3COO)2), 0.5mmol (0.174g) vanadium acetylacetonates (C15H21O6) and 0.5mmol (0.176g) ethanedioic acid dibutyl tin V
(C12H24O4Sn) it is dissolved in the N,N-dimethylformamide (DMF) of 10mL and the ethyl alcohol (CH of 10mL3CH2OH it in), is then added
The PVP (K-120, polyvinylpyrrolidone) of 2.5g stirs 12h, obtains the precursor mixture solution of brownish red；By above-mentioned palm fibre
Red precursor mixture solution carries out quiet under 19kv voltages and 0.9mL/h flow rates, under the atmosphere that relative humidity is 35%
Electrospun；The electrostatic spinning product of above-mentioned gained is placed in crucible, crucible is then positioned over 850 DEG C of sintering in Muffle furnace
Then 6h is naturally cooling to room temperature, obtain a kind of tin vanadium cobalt manganese composite oxide (SnO2/VO2/CoO/Mn3O4) nano particle.
Obtained tin vanadium cobalt manganese composite oxide nano particle is subjected to powder x-ray diffraction analysis and scanning electron microscope sem test, electricity consumption
Test chemical instrument tests its cycle performance and charge-discharge performance.
Embodiment 3
Weigh the manganese acetate (Mn (CH of 3.0mmol (0.519g)3COO)2), 1.0mmol (0.177g) cobalt acetates (Co
(CH3COO)2), 1.0mmol (0.348g) vanadium acetylacetonates (C15H21O6) and 1.0mmol (0.351g) ethanedioic acid dibutyl tin V
(C12H24O4Sn) it is dissolved in the N,N-dimethylformamide (DMF) of 10mL and the ethyl alcohol (CH of 10mL3CH2OH it in), is then added
The PVP (K-120, polyvinylpyrrolidone) of 3.2g stirs 8h, obtains the precursor mixture solution of brownish red；By above-mentioned palm fibre
Red precursor mixture solution carries out quiet under 20kv voltages and 1.0mL/h flow rates, under the atmosphere that relative humidity is 40%
Electrospun；The electrostatic spinning product of above-mentioned gained is placed in crucible, crucible is then positioned over 900 DEG C of sintering in Muffle furnace
Then 7h is naturally cooling to room temperature, obtain a kind of tin vanadium cobalt manganese composite oxide (SnO2/VO2/CoO/Mn3O4) nano particle.
Obtained tin vanadium cobalt manganese composite oxide nano particle is subjected to powder x-ray diffraction analysis and scanning electron microscope sem test, electricity consumption
Test chemical instrument tests its cycle performance and charge-discharge performance.
Claims (2)
1. a kind of preparation method of tin vanadium cobalt manganese composite oxide nano particle, which is characterized in that the tin vanadium cobalt manganese combined oxidation
Object nano particle chemical formula is SnO2/VO2/CoO/Mn3O4, the preparation method includes the following steps：
1) a certain amount of manganese acetate is weighed, cobalt acetate, vanadium acetylacetonate, ethanedioic acid dibutyl tin is dissolved in the N of certain volume, N- bis-
In methylformamide and ethyl alcohol, suitable PVP K-12 0 (referred to as PVP) is then added, stirs 6~12h, obtains
To the precursor mixture solution of brownish red, the molar ratio of metallic element is Mn in mixture solution：Co：V：Sn=3：1：1：1；
2) by the precursor mixture solution of obtained brownish red under 18~20kv voltages and 0.8~1.0mL/h flow rates, it is opposite
Electrostatic spinning is carried out under the atmosphere that humidity is 30~40%；
3) obtained electrostatic spinning product is placed in crucible, crucible is then positioned over 800~900 DEG C of sintering 5 in Muffle furnace
~7h, is then naturally cooling to room temperature, obtains a kind of tin vanadium cobalt manganese composite oxide nano particle.
2. a kind of purposes for the tin vanadium cobalt manganese composite oxide nano particle that preparation method as described in claim 1 obtains,
It is characterized in that, for the nano particle as lithium ion battery negative material, first discharge specific capacity is 478.7mAh g-1, cycle
Charging and discharging capacity is maintained at 390mAh g after 85 times-1More than, efficiency for charge-discharge still keeps 99% or more after recycling 85 times.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110854381A (en) * | 2019-11-27 | 2020-02-28 | 宁波大学 | Preparation method of carbon-doped tin-manganese composite oxide nanofiber modified by cobalt oxide |
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| KR20140036660A (en) * | 2012-09-17 | 2014-03-26 | (주)오렌지파워 | Active material for anode, method of fabricating the same and battery having the same |
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| CN110854381B (en) * | 2019-11-27 | 2022-03-08 | 宁波大学 | Preparation method of carbon-doped tin-manganese composite oxide nanofiber modified by cobalt oxide |
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